Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email FORNIESJ@UNIZAR.ES _publ_contact_author_name 'Prof Juan Fornies' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Quimica Inorganica Universidad de Zaragoza Facultad de Ciencias Zaragoza 50009 SPAIN ; _publ_section_title ; Synthesis and Characterisation of New Binuclear Complexes containing a quite strong Pt to Hg Donor Bond. Molecular Structure of Complex [Pt(C^P)(m-O2C CH3)2Hg (O2CCH3)]. ; loop_ _publ_author_name J.Fornies 'Irene Ara' 'Violeta Sicilia' 'J. Pablo Villarroya' data_ia47 _database_code_CSD 213988 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C27 H29 Hg O6 P Pt' _chemical_formula_weight 876.15 _chemical_melting_point ? _chemical_compound_source ? 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' 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' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 15.579(1) _cell_length_b 12.105(1) _cell_length_c 14.832(1) _cell_angle_alpha 90.00 _cell_angle_beta 93.50(1) _cell_angle_gamma 90.00 _cell_volume 2791.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 90 _cell_measurement_theta_min 12.0 _cell_measurement_theta_max 12.5 _exptl_crystal_description 'irregular block' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.084 _exptl_crystal_density_method ? _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 10.593 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.641 _exptl_absorpt_correction_T_max 0.902 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens P4 four-cicle automated diffractometer' _diffrn_measurement_method \w/2\q _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'no decay observed' _diffrn_reflns_number 6760 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0565 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4880 _reflns_number_observed 3681 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 351 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0592P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4529 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_obs 0.0432 _refine_ls_wR_factor_all 0.1071 _refine_ls_wR_factor_obs 0.0957 _refine_ls_goodness_of_fit_all 1.034 _refine_ls_goodness_of_fit_obs 1.087 _refine_ls_restrained_S_all 1.047 _refine_ls_restrained_S_obs 1.087 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Hg1 Hg 0.26606(3) -0.04460(3) 0.39676(3) 0.03065(14) Uani 1 d . . Pt1 Pt 0.19139(3) 0.11993(3) 0.30904(3) 0.02338(13) Uani 1 d . . P1 P 0.2213(2) 0.2409(2) 0.4194(2) 0.0247(6) Uani 1 d . . O1 O 0.1788(5) -0.1473(6) 0.2869(5) 0.037(2) Uani 1 d . . O2 O 0.1492(5) 0.0078(6) 0.2111(5) 0.038(2) Uani 1 d . . O3 O 0.3698(5) -0.0125(7) 0.2912(6) 0.044(2) Uani 1 d . . O4 O 0.3016(5) 0.1368(6) 0.2319(5) 0.032(2) Uani 1 d . . O5 O 0.3274(5) -0.1506(6) 0.4933(6) 0.038(2) Uani 1 d . . O6 O 0.2141(5) -0.1002(7) 0.5672(6) 0.047(2) Uani 1 d . . C1 C 0.1481(7) -0.0955(10) 0.2199(9) 0.036(3) Uani 1 d . . C2 C 0.1056(8) -0.1570(10) 0.1409(9) 0.049(3) Uani 1 d . . H2A H 0.1073(8) -0.2347(10) 0.1535(9) 0.073 Uiso 1 d R . H2B H 0.0469(8) -0.1334(10) 0.1315(9) 0.073 Uiso 1 d R . H2C H 0.1356(8) -0.1424(10) 0.0875(9) 0.073 Uiso 1 d R . C3 C 0.3634(7) 0.0669(9) 0.2375(8) 0.034(3) Uani 1 d . . C4 C 0.4328(7) 0.0835(11) 0.1723(9) 0.046(3) Uani 1 d . . H4A H 0.4760(7) 0.0275(11) 0.1821(9) 0.069 Uiso 1 d R . H4B H 0.4081(7) 0.0783(11) 0.1116(9) 0.069 Uiso 1 d R . H4C H 0.4584(7) 0.1549(11) 0.1816(9) 0.069 Uiso 1 d R . C5 C 0.2829(7) -0.1479(8) 0.5623(8) 0.029(2) Uani 1 d . . C6 C 0.3212(8) -0.2124(12) 0.6439(8) 0.052(3) Uani 1 d . . H6A H 0.2784(8) -0.2217(12) 0.6871(8) 0.077 Uiso 1 d R . H6B H 0.3406(8) -0.2834(12) 0.6251(8) 0.077 Uiso 1 d R . H6C H 0.3689(8) -0.1715(12) 0.6710(8) 0.077 Uiso 1 d R . C7 C 0.1254(6) 0.2384(8) 0.4826(7) 0.026(2) Uani 1 d . . C8 C 0.1117(7) 0.3096(9) 0.5541(7) 0.032(3) Uani 1 d . . H8A H 0.1553(7) 0.3617(9) 0.5736(7) 0.038 Uiso 1 d R . C9 C 0.0333(8) 0.3046(10) 0.5970(7) 0.038(3) Uani 1 d . . H9A H 0.0217(8) 0.3536(10) 0.6456(7) 0.046 Uiso 1 d R . C10 C -0.0264(7) 0.2257(9) 0.5665(8) 0.038(3) Uani 1 d . . H10A H -0.0799(7) 0.2206(9) 0.5951(8) 0.045 Uiso 1 d R . C11 C -0.0127(7) 0.1554(8) 0.4972(7) 0.028(2) Uani 1 d . . H11A H -0.0542(7) 0.0995(8) 0.4797(7) 0.034 Uiso 1 d R . C12 C 0.0641(6) 0.1645(8) 0.4514(7) 0.025(2) Uani 1 d . . C13 C 0.0786(7) 0.0963(8) 0.3692(7) 0.028(2) Uani 1 d . . H13A H 0.0752(7) 0.0200(8) 0.3858(7) 0.034 Uiso 1 d R . H13B H 0.0322(7) 0.1106(8) 0.3252(7) 0.034 Uiso 1 d R . C14 C 0.3119(6) 0.1978(9) 0.4960(7) 0.028(2) Uani 1 d . . C15 C 0.2939(7) 0.1474(9) 0.5761(8) 0.036(3) Uani 1 d . . H15A H 0.2349(7) 0.1420(9) 0.5911(8) 0.044 Uiso 1 d R . C16 C 0.3580(8) 0.1020(10) 0.6343(9) 0.048(3) Uani 1 d . . H16A H 0.3443(8) 0.0694(10) 0.6905(9) 0.058 Uiso 1 d R . C17 C 0.4399(9) 0.1078(12) 0.6097(11) 0.058(4) Uani 1 d . . H17A H 0.4847(9) 0.0767(12) 0.6490(11) 0.070 Uiso 1 d R . C18 C 0.4608(8) 0.1575(12) 0.5303(11) 0.058(4) Uani 1 d . . H18A H 0.5200(8) 0.1600(12) 0.5157(11) 0.069 Uiso 1 d R . C19 C 0.3982(8) 0.2023(11) 0.4704(8) 0.043(3) Uani 1 d . . C20 C 0.4247(8) 0.2600(13) 0.3860(9) 0.059(4) Uani 1 d . . H20A H 0.4856(8) 0.2526(13) 0.3813(9) 0.089 Uiso 1 d R . H20B H 0.3949(8) 0.2271(13) 0.3343(9) 0.089 Uiso 1 d R . H20C H 0.4099(8) 0.3368(13) 0.3889(9) 0.089 Uiso 1 d R . C21 C 0.2361(7) 0.3878(8) 0.3936(8) 0.035(3) Uani 1 d . . C22 C 0.2886(9) 0.4490(9) 0.4557(10) 0.053(4) Uani 1 d . . H22A H 0.3158(9) 0.4129(9) 0.5074(10) 0.064 Uiso 1 d R . C23 C 0.2999(12) 0.5605(12) 0.4439(12) 0.081(6) Uani 1 d . . H23A H 0.3397(12) 0.6024(12) 0.4821(12) 0.097 Uiso 1 d R . C24 C 0.2540(11) 0.6103(12) 0.3707(11) 0.070(5) Uani 1 d . . H24A H 0.2602(11) 0.6883(12) 0.3617(11) 0.084 Uiso 1 d R . C25 C 0.2010(8) 0.5537(10) 0.3127(9) 0.046(3) Uani 1 d . . H25A H 0.1692(8) 0.5915(10) 0.2646(9) 0.055 Uiso 1 d R . C26 C 0.1915(7) 0.4395(9) 0.3230(8) 0.034(3) Uani 1 d . . C27 C 0.1307(9) 0.3793(11) 0.2575(9) 0.055(4) Uani 1 d . . H27A H 0.1306(9) 0.3022(11) 0.2725(9) 0.082 Uiso 1 d R . H27B H 0.0738(9) 0.4087(11) 0.2611(9) 0.082 Uiso 1 d R . H27C H 0.1487(9) 0.3884(11) 0.1972(9) 0.082 Uiso 1 d 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 Hg1 0.0391(3) 0.0257(2) 0.0264(2) 0.0061(2) -0.0036(2) 0.0035(2) Pt1 0.0304(2) 0.0182(2) 0.0209(2) -0.0004(2) -0.0035(2) 0.0021(2) P1 0.0281(14) 0.0215(13) 0.0240(15) -0.0039(11) -0.0024(12) -0.0011(11) O1 0.043(5) 0.028(4) 0.039(5) 0.000(4) -0.014(4) 0.002(3) O2 0.058(5) 0.028(4) 0.028(4) -0.010(4) -0.002(4) 0.002(4) O3 0.041(5) 0.050(5) 0.041(5) 0.019(4) 0.007(4) 0.013(4) O4 0.047(4) 0.027(4) 0.023(4) 0.004(3) -0.003(3) 0.001(4) O5 0.044(5) 0.033(4) 0.037(5) 0.013(4) 0.001(4) 0.009(4) O6 0.031(4) 0.051(5) 0.058(6) 0.014(5) 0.001(4) 0.007(4) C1 0.028(6) 0.036(7) 0.043(8) -0.015(6) 0.004(5) -0.001(5) C2 0.051(8) 0.044(7) 0.049(8) -0.027(6) -0.016(7) -0.005(6) C3 0.032(6) 0.040(7) 0.030(6) 0.006(5) -0.008(5) -0.001(5) C4 0.032(6) 0.059(8) 0.047(8) 0.006(7) 0.006(6) 0.010(6) C5 0.030(6) 0.025(5) 0.033(7) 0.003(5) -0.002(5) 0.004(5) C6 0.053(8) 0.065(9) 0.036(8) 0.020(7) -0.001(6) 0.005(7) C7 0.028(5) 0.024(5) 0.025(6) -0.001(5) -0.011(5) 0.004(4) C8 0.038(6) 0.033(6) 0.023(6) 0.002(5) -0.004(5) 0.002(5) C9 0.060(8) 0.042(7) 0.013(6) 0.005(5) 0.001(5) 0.022(6) C10 0.033(6) 0.041(7) 0.039(7) 0.001(6) 0.002(5) 0.004(5) C11 0.031(6) 0.025(5) 0.028(6) 0.006(5) -0.008(5) -0.001(5) C12 0.028(6) 0.017(5) 0.028(6) 0.003(4) -0.009(5) 0.010(4) C13 0.041(6) 0.024(5) 0.019(6) 0.010(5) -0.006(5) 0.001(5) C14 0.028(6) 0.028(6) 0.027(6) -0.005(5) -0.005(5) 0.002(5) C15 0.034(6) 0.036(6) 0.037(7) -0.008(6) -0.016(5) 0.006(5) C16 0.062(9) 0.039(7) 0.043(8) -0.004(6) -0.008(7) 0.010(6) C17 0.048(8) 0.060(9) 0.064(10) -0.019(8) -0.016(7) 0.024(7) C18 0.022(6) 0.075(10) 0.074(11) -0.029(9) -0.010(7) 0.005(6) C19 0.046(7) 0.048(7) 0.038(7) -0.020(6) 0.018(6) -0.008(6) C20 0.035(7) 0.083(11) 0.060(10) -0.015(8) 0.006(7) -0.013(7) C21 0.046(7) 0.014(5) 0.044(7) 0.004(5) 0.003(6) 0.004(5) C22 0.077(10) 0.022(6) 0.057(9) 0.009(6) -0.014(8) -0.003(6) C23 0.116(14) 0.034(8) 0.088(14) -0.010(8) -0.034(12) -0.014(8) C24 0.115(14) 0.031(7) 0.063(11) -0.005(8) 0.001(10) -0.002(8) C25 0.062(8) 0.029(6) 0.047(8) 0.029(6) 0.005(7) 0.008(6) C26 0.046(7) 0.029(6) 0.028(6) 0.005(5) 0.010(5) -0.002(5) C27 0.064(9) 0.053(8) 0.047(8) 0.012(7) -0.007(7) -0.014(7) _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 Hg1 O5 2.107(7) . ? Hg1 O3 2.350(8) . ? Hg1 O1 2.404(7) . ? Hg1 Pt1 2.6131(6) . ? Hg1 C5 2.753(11) . ? Pt1 C13 2.039(10) . ? Pt1 O2 2.066(7) . ? Pt1 O4 2.131(8) . ? Pt1 P1 2.224(3) . ? P1 C7 1.812(11) . ? P1 C14 1.834(10) . ? P1 C21 1.837(10) . ? O1 C1 1.246(14) . ? O2 C1 1.258(14) . ? O3 C3 1.248(13) . ? O4 C3 1.280(12) . ? O5 C5 1.271(13) . ? O6 C5 1.224(12) . ? C1 C2 1.507(15) . ? C3 C4 1.51(2) . ? C5 C6 1.531(15) . ? C7 C12 1.369(14) . ? C7 C8 1.393(14) . ? C8 C9 1.41(2) . ? C9 C10 1.39(2) . ? C10 C11 1.362(15) . ? C11 C12 1.415(15) . ? C12 C13 1.500(14) . ? C14 C15 1.38(2) . ? C14 C19 1.420(15) . ? C15 C16 1.39(2) . ? C16 C17 1.35(2) . ? C17 C18 1.38(2) . ? C18 C19 1.39(2) . ? C19 C20 1.51(2) . ? C21 C26 1.37(2) . ? C21 C22 1.40(2) . ? C22 C23 1.37(2) . ? C23 C24 1.40(2) . ? C24 C25 1.34(2) . ? C25 C26 1.40(2) . ? C26 C27 1.50(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 O5 Hg1 O3 104.6(3) . . ? O5 Hg1 O1 111.1(3) . . ? O3 Hg1 O1 91.0(3) . . ? O5 Hg1 Pt1 166.4(2) . . ? O3 Hg1 Pt1 81.1(2) . . ? O1 Hg1 Pt1 80.8(2) . . ? O5 Hg1 C5 26.3(3) . . ? O3 Hg1 C5 129.6(3) . . ? O1 Hg1 C5 112.9(3) . . ? Pt1 Hg1 C5 143.7(2) . . ? C13 Pt1 O2 88.3(4) . . ? C13 Pt1 O4 173.2(3) . . ? O2 Pt1 O4 85.3(3) . . ? C13 Pt1 P1 85.2(3) . . ? O2 Pt1 P1 173.3(2) . . ? O4 Pt1 P1 101.1(2) . . ? C13 Pt1 Hg1 92.6(3) . . ? O2 Pt1 Hg1 87.9(2) . . ? O4 Pt1 Hg1 89.5(2) . . ? P1 Pt1 Hg1 93.92(7) . . ? C7 P1 C14 107.7(5) . . ? C7 P1 C21 104.0(5) . . ? C14 P1 C21 107.6(5) . . ? C7 P1 Pt1 103.2(3) . . ? C14 P1 Pt1 112.8(3) . . ? C21 P1 Pt1 120.5(4) . . ? C1 O1 Hg1 117.0(7) . . ? C1 O2 Pt1 125.8(8) . . ? C3 O3 Hg1 121.4(7) . . ? C3 O4 Pt1 121.9(7) . . ? C5 O5 Hg1 106.5(6) . . ? O1 C1 O2 125.2(11) . . ? O1 C1 C2 120.1(11) . . ? O2 C1 C2 114.7(11) . . ? O3 C3 O4 125.5(11) . . ? O3 C3 C4 118.7(10) . . ? O4 C3 C4 115.8(10) . . ? O6 C5 O5 125.7(10) . . ? O6 C5 C6 119.6(11) . . ? O5 C5 C6 114.7(9) . . ? O6 C5 Hg1 78.6(7) . . ? O5 C5 Hg1 47.2(5) . . ? C6 C5 Hg1 161.5(8) . . ? C12 C7 C8 121.7(10) . . ? C12 C7 P1 114.6(8) . . ? C8 C7 P1 123.6(8) . . ? C7 C8 C9 119.6(10) . . ? C10 C9 C8 117.5(10) . . ? C11 C10 C9 122.9(11) . . ? C10 C11 C12 119.3(10) . . ? C7 C12 C11 118.8(10) . . ? C7 C12 C13 119.9(10) . . ? C11 C12 C13 121.4(9) . . ? C12 C13 Pt1 117.1(7) . . ? C15 C14 C19 119.6(10) . . ? C15 C14 P1 118.0(8) . . ? C19 C14 P1 121.9(9) . . ? C14 C15 C16 122.1(12) . . ? C17 C16 C15 117.8(14) . . ? C16 C17 C18 122.0(13) . . ? C17 C18 C19 121.5(12) . . ? C18 C19 C14 116.9(12) . . ? C18 C19 C20 119.5(12) . . ? C14 C19 C20 123.4(12) . . ? C26 C21 C22 120.5(10) . . ? C26 C21 P1 122.4(9) . . ? C22 C21 P1 116.7(9) . . ? C23 C22 C21 120.6(13) . . ? C22 C23 C24 117.3(14) . . ? C25 C24 C23 122.8(13) . . ? C24 C25 C26 119.9(12) . . ? C21 C26 C25 118.8(11) . . ? C21 C26 C27 122.8(10) . . ? C25 C26 C27 118.4(11) . . ? _refine_diff_density_max 1.902 _refine_diff_density_min -1.729 _refine_diff_density_rms 0.213