Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 # TITLE AND AUTHOR LIST _publ_section_title ; Crystal Structure of Lead(II) Acetylacetonate and the Structure of the Acetylacetone Solvated Lead(II) Ion in Solution Studied by Large Angle X-Ray Scattering. ; loop_ _publ_author_name _publ_author_address K.Lyczko ; Department of Radiochemistry Institute of Nuclear Chemistry and Technology Dorodna 16 03-195 Warsaw Poland ; J.Narbutt ; Department of Radiochemistry Institute of Nuclear Chemistry and Technology Dorodna 16 03-195 Warsaw Poland ; B.Paluchowska ; Institute of Atomic Energy 05-400 Otwock-\'Swierk Poland ; J.K.Maurin ; Institute of Atomic Energy 05-400 Otwock-\'Swierk Poland and National Institute of Public Health Che\/lmska 30/34 00-725 Warsaw Poland ; I.Persson ; Department of Chemistry Swedish University of Agricultural Sciences P.O. Box 7015 SE-750 07 Uppsala Sweden ; _publ_contact_author_name 'Krzysztof Lyczko' _publ_contact_author_email KML@ICHTJ.WAW.PL data_narpab _database_code_depnum_ccdc_archive 'CCDC 600005' _audit_creation_method SHELXL-97 _chemical_name_systematic ; catena-((\m~3~-Acetylacetonato-O,O,O',O')-(\m~2~-acetylacetonato-O,O,O')- lead(II)) ; _chemical_name_common ; catena-((mu!3$-Acetylacetonato-O,O,O',O')-(mu!2$- acetylacetonato-O,O,O')-lead(ii)) ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H14 O4 Pb' _chemical_formula_weight 405.40 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' Pb Pb -3.3944 10.1111 '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 8.083(2) _cell_length_b 7.830(2) _cell_length_c 18.940(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.74(3) _cell_angle_gamma 90.00 _cell_volume 1194.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description columnar _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.265 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 14.115 _exptl_absorpt_correction_type 'psi scan' _exptl_absorpt_correction_T_min 0.00131 _exptl_absorpt_correction_T_max 0.02148 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Kuma KM-4 \k-axis diffractometer' _diffrn_measurement_method 'separate scans for individual reflections' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% 0 _diffrn_reflns_number 1707 _diffrn_reflns_av_R_equivalents 0.0748 _diffrn_reflns_av_sigmaI/netI 0.0579 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 24.99 _reflns_number_total 1661 _reflns_number_gt 807 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kuma software (1991)' _computing_cell_refinement 'Kuma software (1991)' _computing_data_reduction 'Kuma software (1991)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Bruker-AXS, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 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^)+(0.0976P)^2^+3.7131P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1661 _refine_ls_number_parameters 136 _refine_ls_number_restraints 69 _refine_ls_R_factor_all 0.1337 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1723 _refine_ls_wR_factor_gt 0.1416 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.069 _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 Pb1 Pb 0.02971(8) 0.10170(6) 0.21976(3) 0.11205(18) Uani 1 1 d D . . O1 O 0.2349(6) 0.2952(8) 0.2583(3) 0.115(3) Uani 1 1 d D . . C2 C 0.3531(7) 0.2790(7) 0.3059(3) 0.111(4) Uani 1 1 d DU . . C1 C 0.4662(9) 0.3749(12) 0.2775(5) 0.117(4) Uani 1 1 d DU . . H11A H 0.4116 0.4595 0.2471 0.175 Uiso 1 1 calc R . . H11B H 0.5342 0.3040 0.2503 0.175 Uiso 1 1 calc R . . H11C H 0.5346 0.4304 0.3145 0.175 Uiso 1 1 calc R . . C3 C 0.3866(10) 0.1406(6) 0.3488(4) 0.109(4) Uani 1 1 d DU . . H2A H 0.4831 0.1467 0.3791 0.163 Uiso 1 1 calc R . . C4 C 0.2944(7) -0.0072(7) 0.3526(3) 0.088(3) Uani 1 1 d DU . . C5 C 0.3366(15) -0.1061(11) 0.4083(4) 0.120(4) Uani 1 1 d DU . . H13A H 0.2653 -0.2042 0.4072 0.179 Uiso 1 1 calc R . . H13B H 0.3254 -0.0429 0.4511 0.179 Uiso 1 1 calc R . . H13C H 0.4497 -0.1425 0.4069 0.179 Uiso 1 1 calc R . . O2 O 0.1692(7) -0.0558(8) 0.3121(3) 0.121(3) Uani 1 1 d D . . O1' O 0.1466(8) 0.1631(8) 0.1122(2) 0.102(3) Uani 1 1 d D . . C2' C 0.1972(11) 0.0756(6) 0.0611(3) 0.096(3) Uani 1 1 d DU . . C1' C 0.2518(12) 0.1628(11) 0.0060(4) 0.080(3) Uani 1 1 d DU . . H22A H 0.2343 0.2829 0.0126 0.121 Uiso 1 1 calc R . . H22B H 0.1918 0.1262 -0.0372 0.121 Uiso 1 1 calc R . . H22C H 0.3681 0.1414 0.0035 0.121 Uiso 1 1 calc R . . C3' C 0.1970(11) -0.1004(5) 0.0657(4) 0.075(3) Uani 1 1 d DU . . H22D H 0.2434 -0.1508 0.0275 0.113 Uiso 1 1 calc R . . C4' C 0.1453(10) -0.2208(6) 0.1126(3) 0.070(3) Uani 1 1 d DU . . C5' C 0.1641(18) -0.3880(8) 0.0989(7) 0.125(5) Uani 1 1 d DU . . H22E H 0.1219 -0.4545 0.1360 0.187 Uiso 1 1 calc R . . H22F H 0.2797 -0.4129 0.0963 0.187 Uiso 1 1 calc R . . H22G H 0.1041 -0.4158 0.0545 0.187 Uiso 1 1 calc R . . O2' O 0.0978(7) -0.1654(6) 0.1703(3) 0.072(2) Uani 1 1 d D . . 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 Pb1 0.1724(4) 0.0466(2) 0.1225(3) -0.0004(3) 0.0447(3) -0.0074(3) O1 0.113(5) 0.110(7) 0.130(6) -0.008(5) 0.054(4) -0.015(6) C2 0.096(8) 0.132(6) 0.102(8) -0.003(5) -0.015(6) 0.002(6) C1 0.115(8) 0.133(8) 0.101(8) -0.020(6) 0.004(6) -0.023(7) C3 0.129(9) 0.092(5) 0.105(7) -0.025(4) 0.004(7) 0.017(5) C4 0.086(7) 0.124(5) 0.048(4) -0.045(4) -0.036(5) -0.008(5) C5 0.096(9) 0.125(7) 0.131(8) 0.011(6) -0.030(7) 0.012(8) O2 0.140(7) 0.116(7) 0.107(5) 0.032(5) 0.016(5) -0.022(6) O1' 0.124(5) 0.072(5) 0.114(5) 0.021(4) 0.041(4) 0.006(5) C2' 0.113(8) 0.087(4) 0.087(6) 0.004(5) 0.001(6) -0.044(6) C1' 0.088(7) 0.067(5) 0.086(6) -0.011(4) 0.006(5) -0.016(6) C3' 0.059(6) 0.097(4) 0.069(5) 0.017(4) -0.010(5) -0.011(6) C4' 0.048(6) 0.072(4) 0.087(6) 0.015(4) -0.013(5) -0.002(5) C5' 0.138(11) 0.078(4) 0.155(12) 0.025(7) -0.006(9) 0.035(8) O2' 0.068(4) 0.059(4) 0.087(4) -0.015(4) 0.000(3) -0.001(4) _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 Pb1 O1 2.319(5) . ? Pb1 O2 2.351(5) . ? Pb1 O1' 2.365(5) . ? Pb1 O2' 2.375(4) . ? O1 C2 1.264(6) . ? C2 C1 1.330(8) . ? C2 C3 1.369(6) . ? C3 C4 1.381(6) . ? C4 O2 1.276(6) . ? C4 C5 1.330(8) . ? O1' C2' 1.280(6) . ? C2' C1' 1.352(7) . ? C2' C3' 1.380(5) . ? C3' C4' 1.383(6) . ? C4' O2' 1.265(6) . ? C4' C5' 1.345(7) . ? 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 Pb1 O2 79.7(2) . . ? O1 Pb1 O1' 79.2(2) . . ? O2 Pb1 O1' 123.1(2) . . ? O1 Pb1 O2' 121.1(2) . . ? O2 Pb1 O2' 73.7(2) . . ? O1' Pb1 O2' 73.6(2) . . ? C2 O1 Pb1 129.6(5) . . ? O1 C2 C1 99.2(6) . . ? O1 C2 C3 127.1(6) . . ? C1 C2 C3 125.3(7) . . ? C2 C3 C4 127.8(7) . . ? O2 C4 C5 116.2(7) . . ? O2 C4 C3 128.5(6) . . ? C5 C4 C3 115.1(7) . . ? C4 O2 Pb1 126.8(5) . . ? C2' O1' Pb1 135.9(4) . . ? O1' C2' C1' 117.3(6) . . ? O1' C2' C3' 119.0(6) . . ? C1' C2' C3' 123.7(6) . . ? C2' C3' C4' 136.3(6) . . ? O2' C4' C5' 123.3(8) . . ? O2' C4' C3' 116.8(5) . . ? C5' C4' C3' 119.6(8) . . ? C4' O2' Pb1 137.7(4) . . ? _diffrn_measured_fraction_theta_max 0.788 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.788 _refine_diff_density_max 0.776 _refine_diff_density_min -0.854 _refine_diff_density_rms 0.185