#------------------------------------------------------------------------------ #$Date: 2008-03-30 11:21:05 +0100 (Sun, 30 Mar 2008) $ #$Revision: 321 $ #$URL: svn://www.crystallography.net/cod/cif/2/2204345.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2204345 loop_ _publ_author_name 'Lerner, Hans-Wolfram' 'Bolte, Michael' _publ_section_title ; Dimethanoldiacetylacetonezinc(II) ; _journal_issue 10 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first m1468 _journal_page_last m1469 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '[Zn (C5 H7 O2) 2, (C H4 O) 2]' _chemical_formula_moiety 'C12 H22 O6 Zn' _chemical_formula_sum 'C12 H22 O6 Zn' _chemical_formula_weight 327.67 _chemical_name_systematic ; ; ; _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 69.184(10) _cell_angle_beta 81.385(11) _cell_angle_gamma 75.485(11) _cell_formula_units_Z 1 _cell_length_a 5.2986(7) _cell_length_b 7.4809(10) _cell_length_c 10.4575(15) _cell_measurement_reflns_used 23971 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.6 _cell_measurement_theta_min 3.9 _cell_volume 374.25(9) _computing_cell_refinement X-AREA _computing_data_collection 'X-AREA (Stoe & Cie, 2001)' _computing_data_reduction X-AREA _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material 'SHELXL97 and PLATON (Spek, 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997) ' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997) ' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_sigmaI/netI 0.0266 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 8019 _diffrn_reflns_theta_full 29.51 _diffrn_reflns_theta_max 29.51 _diffrn_reflns_theta_min 3.98 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.658 _exptl_absorpt_correction_T_max 0.698 _exptl_absorpt_correction_T_min 0.525 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(MULABS; Spek, 1990; Blessing, 1995)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 172 _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.22 _refine_diff_density_max 0.475 _refine_diff_density_min -0.725 _refine_ls_extinction_coef 0.028(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 96 _refine_ls_number_reflns 2077 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.093 _refine_ls_R_factor_all 0.0255 _refine_ls_R_factor_gt 0.0248 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0393P)^2^+0.0996P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.0688 _reflns_number_gt 2017 _reflns_number_total 2077 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file hb6092.cif loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Zn1 0.5000 0.5000 0.0000 0.01863(9) Uani d S 1 Zn O1 0.65903(19) 0.32771(15) 0.18068(10) 0.0227(2) Uani d . 1 O O2 0.17813(18) 0.61730(15) 0.10574(10) 0.02142(19) Uani d . 1 O O3 0.29930(19) 0.28079(15) 0.00127(11) 0.0236(2) Uani d D 1 O H3 0.154(3) 0.320(3) -0.030(2) 0.042(6) Uiso d D 1 H C1 0.7381(3) 0.2049(2) 0.41554(15) 0.0285(3) Uani d . 1 C H1A 0.7529 0.0691 0.4212 0.043 Uiso calc R 1 H H1B 0.6537 0.2233 0.5013 0.043 Uiso calc R 1 H H1C 0.9128 0.2337 0.4006 0.043 Uiso calc R 1 H C2 0.5755(3) 0.3419(2) 0.29710(14) 0.0215(2) Uani d . 1 C C3 0.3487(3) 0.4713(2) 0.32638(14) 0.0234(3) Uani d . 1 C H3A 0.3180 0.4733 0.4178 0.028 Uiso calc R 1 H C4 0.1646(3) 0.5974(2) 0.23274(14) 0.0207(2) Uani d . 1 C C5 -0.0747(3) 0.7184(2) 0.28444(15) 0.0247(3) Uani d . 1 C H5A -0.0933 0.8562 0.2269 0.037 Uiso calc R 1 H H5B -0.0558 0.7051 0.3794 0.037 Uiso calc R 1 H H5C -0.2301 0.6724 0.2805 0.037 Uiso calc R 1 H C6 0.2964(3) 0.1029(2) 0.11373(17) 0.0297(3) Uani d . 1 C H6A 0.4689 0.0518 0.1512 0.045 Uiso calc R 1 H H6B 0.2537 0.0063 0.0818 0.045 Uiso calc R 1 H H6C 0.1648 0.1286 0.1852 0.045 Uiso calc R 1 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zn1 0.01482(12) 0.02238(13) 0.01722(12) -0.00315(8) -0.00139(7) -0.00524(8) O1 0.0201(4) 0.0264(5) 0.0189(4) -0.0022(4) -0.0034(3) -0.0053(4) O2 0.0167(4) 0.0269(5) 0.0200(4) -0.0031(3) -0.0009(3) -0.0081(4) O3 0.0181(4) 0.0240(5) 0.0277(5) -0.0049(4) -0.0049(4) -0.0058(4) C1 0.0300(7) 0.0300(7) 0.0214(6) -0.0020(6) -0.0074(5) -0.0044(5) C2 0.0220(6) 0.0228(6) 0.0196(6) -0.0080(5) -0.0041(5) -0.0036(5) C3 0.0234(6) 0.0287(7) 0.0180(6) -0.0073(5) -0.0008(5) -0.0069(5) C4 0.0183(5) 0.0234(6) 0.0221(6) -0.0081(5) 0.0011(5) -0.0079(5) C5 0.0205(6) 0.0302(7) 0.0248(6) -0.0054(5) 0.0020(5) -0.0123(5) C6 0.0280(7) 0.0244(6) 0.0338(8) -0.0058(5) -0.0030(6) -0.0057(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Zn1 O1 2_665 2.0354(10) ? Zn1 O1 . 2.0355(10) y Zn1 O2 . 2.0678(10) y Zn1 O2 2_665 2.0678(10) ? Zn1 O3 2_665 2.1621(10) ? Zn1 O3 . 2.1621(10) y O1 C2 . 1.2633(17) n O2 C4 . 1.2758(16) n O3 C6 . 1.4308(18) n O3 H3 . 0.826(10) ? C1 C2 . 1.5171(19) ? C1 H1A . 0.9800 ? C1 H1B . 0.9800 ? C1 H1C . 0.9800 ? C2 C3 . 1.412(2) n C3 C4 . 1.4033(19) n C3 H3A . 0.9500 ? C4 C5 . 1.5121(19) ? C5 H5A . 0.9800 ? C5 H5B . 0.9800 ? C5 H5C . 0.9800 ? C6 H6A . 0.9800 ? C6 H6B . 0.9800 ? C6 H6C . 0.9800 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Zn1 O1 2_665 . 180.0 ? O1 Zn1 O2 2_665 . 89.96(4) y O1 Zn1 O2 . . 90.04(4) y O1 Zn1 O2 2_665 2_665 90.04(4) ? O1 Zn1 O2 . 2_665 89.96(4) ? O2 Zn1 O2 . 2_665 180.0 ? O1 Zn1 O3 2_665 2_665 92.17(4) ? O1 Zn1 O3 . 2_665 87.83(4) ? O2 Zn1 O3 . 2_665 90.47(4) y O2 Zn1 O3 2_665 2_665 89.53(4) ? O1 Zn1 O3 2_665 . 87.83(4) y O1 Zn1 O3 . . 92.17(4) y O2 Zn1 O3 . . 89.53(4) y O2 Zn1 O3 2_665 . 90.47(4) ? O3 Zn1 O3 2_665 . 180.0 ? C2 O1 Zn1 . . 125.64(9) ? C4 O2 Zn1 . . 125.00(9) ? C6 O3 Zn1 . . 123.26(9) ? C6 O3 H3 . . 108.0(17) ? Zn1 O3 H3 . . 117.1(17) ? C2 C1 H1A . . 109.5 ? C2 C1 H1B . . 109.5 ? H1A C1 H1B . . 109.5 ? C2 C1 H1C . . 109.5 ? H1A C1 H1C . . 109.5 ? H1B C1 H1C . . 109.5 ? O1 C2 C3 . . 126.42(12) ? O1 C2 C1 . . 115.76(12) ? C3 C2 C1 . . 117.82(12) ? C4 C3 C2 . . 125.92(13) ? C4 C3 H3A . . 117.0 ? C2 C3 H3A . . 117.0 ? O2 C4 C3 . . 125.44(13) ? O2 C4 C5 . . 116.01(12) ? C3 C4 C5 . . 118.53(12) ? C4 C5 H5A . . 109.5 ? C4 C5 H5B . . 109.5 ? H5A C5 H5B . . 109.5 ? C4 C5 H5C . . 109.5 ? H5A C5 H5C . . 109.5 ? H5B C5 H5C . . 109.5 ? O3 C6 H6A . . 109.5 ? O3 C6 H6B . . 109.5 ? H6A C6 H6B . . 109.5 ? O3 C6 H6C . . 109.5 ? H6A C6 H6C . . 109.5 ? H6B C6 H6C . . 109.5 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion O2 Zn1 O1 C2 . -10.25(11) O2 Zn1 O1 C2 2_665 169.75(11) O3 Zn1 O1 C2 2_665 80.22(11) O3 Zn1 O1 C2 . -99.78(11) O1 Zn1 O2 C4 2_665 -166.98(11) O1 Zn1 O2 C4 . 13.02(11) O3 Zn1 O2 C4 2_665 -74.81(11) O3 Zn1 O2 C4 . 105.19(11) O1 Zn1 O3 C6 2_665 -174.15(11) O1 Zn1 O3 C6 . 5.85(11) O2 Zn1 O3 C6 . -84.17(11) O2 Zn1 O3 C6 2_665 95.83(11) Zn1 O1 C2 C3 . 3.8(2) Zn1 O1 C2 C1 . -176.16(9) O1 C2 C3 C4 . 5.2(2) C1 C2 C3 C4 . -174.86(13) Zn1 O2 C4 C3 . -9.52(19) Zn1 O2 C4 C5 . 171.79(9) C2 C3 C4 O2 . -1.8(2) C2 C3 C4 C5 . 176.82(13) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O3 H3 O2 2_565 0.826(10) 1.918(10) 2.7401(14) 173(2)