Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_ZNDA _database_code_CSD 160057 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Anthony, S. Philip' 'Radhakrishnan, T. P.' _publ_contact_author_name 'Dr T P Radhakrishnan' _publ_contact_author_address ; Dr T P Radhakrishnan University of Hyderabad Hyderabad 500 046 INDIA ; _publ_contact_author_email 'tprsc@uohyd.ernet.in' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(acetylacetonato)(4-Dimethylamino-pyridine)Zinc(II) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C8.50 H12 N O2 Zn0.50' _chemical_formula_weight 192.88 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' 'N' 'N' 0.0061 0.0033 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Fdd2' #(No. 43) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 28.057(4) _cell_length_b 11.363(2) _cell_length_c 11.3253(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3610.6(10) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'Plate' _exptl_crystal_colour 'Colourless' _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 1.383 _exptl_absorpt_correction_type 'Empirical (using Psi-scan)' _exptl_absorpt_correction_T_min 0.9883 _exptl_absorpt_correction_T_max 0.9782 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3029 _diffrn_reflns_av_R_equivalents 0.0158 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 30.92 _reflns_number_total 1496 _reflns_number_gt 1353 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 w=1/[\s^2^(Fo^2^)+(0.0424P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.052(12) _refine_ls_number_reflns 1353 _refine_ls_number_parameters 117 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0257 _refine_ls_wR_factor_ref 0.0648 _refine_ls_wR_factor_gt 0.0626 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.001 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.0000 0.0000 0.98446(2) 0.03201(10) Uani 1 d S . . O8 O -0.04803(5) 0.13676(14) 0.9757(2) 0.0416(4) Uani 1 d . . . O12 O -0.04669(6) -0.10211(15) 0.89947(19) 0.0451(4) Uani 1 d . . . N2 N 0.0000 0.0000 1.1640(3) 0.0329(5) Uani 1 d S . . N6 N 0.0000 0.0000 1.5326(5) 0.0497(14) Uani 1 d S . . C3 C -0.00590(9) 0.0985(2) 1.2277(2) 0.0396(5) Uani 1 d . . . H3 H -0.0105 0.1686 1.1867 0.048 Uiso 1 calc R . . C4 C -0.00560(11) 0.1035(3) 1.3486(3) 0.0420(7) Uani 1 d . . . H4 H -0.0091 0.1754 1.3869 0.050 Uiso 1 calc R . . C5 C 0.0000 0.0000 1.4142(5) 0.0352(9) Uani 1 d S . . C7 C -0.00395(12) 0.1093(5) 1.6000(4) 0.0564(10) Uani 1 d . . . H7A H 0.0192 0.1649 1.5717 0.085 Uiso 1 calc R . . H7B H 0.0017 0.0935 1.6820 0.085 Uiso 1 calc R . . H7C H -0.0354 0.1414 1.5904 0.085 Uiso 1 calc R . . C9 C -0.08740(8) 0.1352(2) 0.9234(2) 0.0376(5) Uani 1 d . . . C10 C -0.10639(9) 0.0400(2) 0.8619(2) 0.0444(5) Uani 1 d . . . H10 H -0.1351 0.0518 0.8228 0.053 Uiso 1 calc R . . C11 C -0.08581(8) -0.0714(2) 0.8542(2) 0.0402(5) Uani 1 d . . . C13 C -0.11632(12) 0.2469(2) 0.9308(4) 0.0588(8) Uani 1 d . . . H13A H -0.1256 0.2605 1.0112 0.088 Uiso 1 calc R . . H13B H -0.1443 0.2394 0.8825 0.088 Uiso 1 calc R . . H13C H -0.0975 0.3119 0.9033 0.088 Uiso 1 calc R . . C14 C -0.11159(11) -0.1667(2) 0.7870(3) 0.0561(7) Uani 1 d . . . H14A H -0.0905 -0.2003 0.7294 0.084 Uiso 1 calc R . . H14B H -0.1389 -0.1336 0.7480 0.084 Uiso 1 calc R . . H14C H -0.1218 -0.2268 0.8409 0.084 Uiso 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 Zn1 0.03099(14) 0.03362(15) 0.03142(14) 0.000 0.000 0.00243(17) O8 0.0408(7) 0.0366(7) 0.0475(9) -0.0022(8) -0.0082(8) 0.0061(6) O12 0.0432(9) 0.0379(8) 0.0543(12) -0.0079(8) -0.0097(8) 0.0015(7) N2 0.0346(12) 0.0291(12) 0.0351(12) 0.000 0.000 0.0029(9) N6 0.083(4) 0.033(2) 0.0330(18) 0.000 0.000 -0.0066(15) C3 0.0557(12) 0.0259(9) 0.0372(11) 0.0020(8) -0.0034(12) 0.0049(8) C4 0.0642(17) 0.0229(11) 0.0388(15) -0.0049(10) -0.0002(12) 0.0009(10) C5 0.043(2) 0.035(2) 0.0272(16) 0.000 0.000 -0.0044(12) C7 0.077(2) 0.055(2) 0.0376(17) -0.0121(14) -0.0007(15) -0.0058(15) C9 0.0390(10) 0.0414(11) 0.0325(11) 0.0051(9) -0.0011(8) 0.0080(9) C10 0.0375(11) 0.0562(14) 0.0396(12) -0.0013(11) -0.0076(10) 0.0040(10) C11 0.0376(10) 0.0494(12) 0.0335(11) -0.0039(9) -0.0007(9) -0.0061(9) C13 0.0575(17) 0.0576(17) 0.0612(18) -0.0008(14) -0.0131(15) 0.0251(13) C14 0.0534(14) 0.0588(16) 0.0559(16) -0.0109(14) -0.0089(13) -0.0103(13) _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 Zn1 O12 1.9972(17) . ? Zn1 O12 1.9972(17) 2 ? Zn1 N2 2.033(3) . ? Zn1 O8 2.0593(15) . ? Zn1 O8 2.0593(15) 2 ? O8 C9 1.253(3) . ? O12 C11 1.261(3) . ? N2 C3 1.342(3) . ? N2 C3 1.342(3) 2 ? N6 C5 1.341(5) . ? N6 C7 1.462(5) . ? N6 C7 1.462(5) 2 ? C3 C4 1.371(5) . ? C4 C5 1.400(5) . ? C5 C4 1.400(5) 2 ? C9 C10 1.392(3) . ? C9 C13 1.509(3) . ? C10 C11 1.394(4) . ? C11 C14 1.508(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 O12 Zn1 O12 122.37(13) . 2 ? O12 Zn1 N2 118.81(6) . . ? O12 Zn1 N2 118.81(6) 2 . ? O12 Zn1 O8 89.20(7) . . ? O12 Zn1 O8 88.15(8) 2 . ? N2 Zn1 O8 92.75(6) . . ? O12 Zn1 O8 88.15(8) . 2 ? O12 Zn1 O8 89.20(7) 2 2 ? N2 Zn1 O8 92.75(6) . 2 ? O8 Zn1 O8 174.50(13) . 2 ? C9 O8 Zn1 126.05(16) . . ? C11 O12 Zn1 127.32(17) . . ? C3 N2 C3 115.0(3) . 2 ? C3 N2 Zn1 122.51(15) . . ? C3 N2 Zn1 122.51(15) 2 . ? C5 N6 C7 121.5(3) . . ? C5 N6 C7 121.5(3) . 2 ? C7 N6 C7 117.1(6) . 2 ? N2 C3 C4 124.8(3) . . ? C3 C4 C5 119.8(3) . . ? N6 C5 C4 122.1(3) . . ? N6 C5 C4 122.1(3) . 2 ? C4 C5 C4 115.9(5) . 2 ? O8 C9 C10 125.8(2) . . ? O8 C9 C13 115.8(2) . . ? C10 C9 C13 118.4(2) . . ? C9 C10 C11 125.3(2) . . ? O12 C11 C10 125.9(2) . . ? O12 C11 C14 115.1(2) . . ? C10 C11 C14 119.0(2) . . ? _diffrn_measured_fraction_theta_max 0.258 _diffrn_reflns_theta_full 30.92 _diffrn_measured_fraction_theta_full 0.258 _refine_diff_density_max 0.52 _refine_diff_density_min -0.24 _refine_diff_density_rms 0.06