#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/44/2014412.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_2014412 loop_ _publ_author_name 'Juan Granifo' 'Mar\'ia Teresa Garland' 'Ricardo Baggio' _publ_section_title ;Two one-dimensional zinc(II) coordination polymers: catena-poly[[bis(pentane-2,4-dionato-\k^2^O,O')zinc]-\m-1,4-bis(x-pyridyl)-2,3-diazabuta-1,3-diene] (x = 3, 4) ; _journal_coeditor_code SQ3002 _journal_issue 2 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m56 _journal_page_last m59 _journal_volume 62 _journal_year 2006 _chemical_formula_iupac '[Zn (C5 H7 O2)2 (C12 H10 N4)]' _chemical_formula_moiety 'C22 H24 N4 O4 Zn' _chemical_formula_sum 'C22 H24 N4 O4 Zn' _chemical_formula_weight 473.82 _chemical_name_systematic ; catena-poly[[bis(pentane-2,4-dionato-\k^2^O,O')zinc]-\m- 1,4-bis(4-pyridyl)-2,3-diazabuta-1,3-diene] ; _space_group_IT_number 2 _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 84.282(2) _cell_angle_beta 72.332(2) _cell_angle_gamma 89.558(2) _cell_formula_units_Z 1 _cell_length_a 6.3525(8) _cell_length_b 9.0459(11) _cell_length_c 10.3907(12) _cell_measurement_reflns_used 1870 _cell_measurement_temperature 273(2) _cell_measurement_theta_max 26.03 _cell_measurement_theta_min 3.34 _cell_volume 565.94(12) _computing_cell_refinement 'SAINT-NT (Bruker, 2000)' _computing_data_collection 'SMART-NT (Bruker, 2001)' _computing_data_reduction SAINT-NT _computing_molecular_graphics 'XP in SHELXTL-PC (Sheldrick, 2000 or 1994?)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 273(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.883 _diffrn_measurement_device_type 'Bruker SMART CCD area-detector' _diffrn_measurement_method '\f and \w scans' _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 0.0439 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 4727 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 27.99 _diffrn_reflns_theta_min 2.07 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.120 _exptl_absorpt_correction_T_max 0.84 _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Sheldrick, 1996) ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 246 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _refine_diff_density_max 0.402 _refine_diff_density_min -0.429 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 144 _refine_ls_number_reflns 2409 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.080 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0351 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0606P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0965 _refine_ls_wR_factor_ref 0.0971 _reflns_number_gt 2293 _reflns_number_total 2409 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file sq3002.cif _[local]_cod_data_source_block I _cod_database_code 2014412 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Zn1 0.5000 0.5000 0.5000 0.03504(14) Uani d S 1 . . Zn C1 -0.1060(3) 0.1952(2) 0.8561(2) 0.0407(4) Uani d . 1 . . C C2 -0.1242(3) 0.2353(2) 0.7280(2) 0.0398(4) Uani d . 1 . . C H2 -0.2467 0.2042 0.7056 0.048 Uiso calc R 1 . . H C3 0.0393(3) 0.3210(2) 0.6346(2) 0.0386(4) Uani d . 1 . . C H3 0.0235 0.3474 0.5492 0.046 Uiso calc R 1 . . H N4 0.2212(3) 0.36882(18) 0.65938(17) 0.0387(4) Uani d . 1 . . N C5 0.2371(4) 0.3299(3) 0.7834(2) 0.0535(6) Uani d . 1 . . C H5 0.3619 0.3616 0.8030 0.064 Uiso calc R 1 . . H C6 0.0812(4) 0.2465(3) 0.8826(2) 0.0558(6) Uani d . 1 . . C H6 0.0996 0.2239 0.9677 0.067 Uiso calc R 1 . . H C7 -0.2679(4) 0.1010(2) 0.9614(2) 0.0466(5) Uani d . 1 . . C H7 -0.2476 0.0824 1.0464 0.056 Uiso calc R 1 . . H N8 -0.4348(3) 0.0437(2) 0.94153(17) 0.0470(4) Uani d . 1 . . N C9 0.2218(5) 0.9280(3) 0.6075(3) 0.0703(8) Uani d . 1 . . C H9A 0.2524 0.9743 0.5163 0.106 Uiso calc R 1 . . H H9B 0.2607 0.9956 0.6626 0.106 Uiso calc R 1 . . H H9C 0.0673 0.9021 0.6438 0.106 Uiso calc R 1 . . H C10 0.3558(4) 0.7890(2) 0.6072(2) 0.0454(5) Uani d . 1 . . C C11 0.4947(4) 0.7751(2) 0.6895(2) 0.0524(5) Uani d . 1 . . C H11 0.5043 0.8559 0.7364 0.063 Uiso calc R 1 . . H C12 0.6197(3) 0.6526(2) 0.7082(2) 0.0418(4) Uani d . 1 . . C C13 0.7438(5) 0.6523(3) 0.8102(3) 0.0672(7) Uani d . 1 . . C H13A 0.6896 0.5717 0.8800 0.101 Uiso calc R 1 . . H H13B 0.7228 0.7447 0.8500 0.101 Uiso calc R 1 . . H H13C 0.8983 0.6402 0.7660 0.101 Uiso calc R 1 . . H O14 0.6379(2) 0.53697(15) 0.64704(14) 0.0391(3) Uani d . 1 . . O O15 0.3299(2) 0.69470(15) 0.53251(15) 0.0437(3) Uani d . 1 . . O 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 0.0363(2) 0.03266(19) 0.0397(2) 0.00054(12) -0.01659(14) -0.00451(13) C1 0.0394(11) 0.0405(10) 0.0403(10) -0.0059(8) -0.0102(8) -0.0007(8) C2 0.0328(10) 0.0432(10) 0.0450(11) -0.0021(8) -0.0146(8) -0.0024(8) C3 0.0343(10) 0.0419(10) 0.0400(10) 0.0005(8) -0.0137(8) 0.0015(8) N4 0.0364(9) 0.0398(8) 0.0408(9) -0.0044(7) -0.0140(7) 0.0002(7) C5 0.0512(13) 0.0625(14) 0.0499(12) -0.0218(11) -0.0238(10) 0.0078(11) C6 0.0578(14) 0.0729(16) 0.0399(11) -0.0206(12) -0.0237(10) 0.0091(11) C7 0.0490(12) 0.0512(12) 0.0367(10) -0.0086(10) -0.0106(9) 0.0021(9) N8 0.0454(10) 0.0503(10) 0.0402(9) -0.0142(8) -0.0080(8) 0.0049(8) C9 0.0771(19) 0.0475(13) 0.090(2) 0.0209(13) -0.0280(15) -0.0169(13) C10 0.0458(12) 0.0386(10) 0.0478(12) 0.0039(9) -0.0086(9) -0.0039(9) C11 0.0645(14) 0.0454(12) 0.0536(13) 0.0061(10) -0.0224(11) -0.0204(10) C12 0.0414(11) 0.0477(11) 0.0365(10) -0.0057(9) -0.0119(8) -0.0059(8) C13 0.0767(18) 0.0750(17) 0.0669(17) 0.0055(14) -0.0426(15) -0.0228(14) O14 0.0406(7) 0.0385(7) 0.0429(7) -0.0008(6) -0.0193(6) -0.0049(6) O15 0.0456(8) 0.0397(7) 0.0511(8) 0.0076(6) -0.0218(7) -0.0069(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 O14 2_666 2.0328(13) ? Zn1 O14 . 2.0328(13) y Zn1 O15 . 2.0617(13) y Zn1 O15 2_666 2.0617(13) ? Zn1 N4 . 2.2689(17) y Zn1 N4 2_666 2.2689(17) ? C1 C2 . 1.383(3) ? C1 C6 . 1.392(3) ? C1 C7 . 1.458(3) ? C2 C3 . 1.369(3) ? C2 H2 . 0.9300 ? C3 N4 . 1.341(2) ? C3 H3 . 0.9300 ? N4 C5 . 1.335(3) ? C5 C6 . 1.360(3) ? C5 H5 . 0.9300 ? C6 H6 . 0.9300 ? C7 N8 . 1.264(3) ? C7 H7 . 0.9300 ? N8 N8 2_457 1.413(3) ? C9 C10 . 1.512(3) ? C9 H9A . 0.9600 ? C9 H9B . 0.9600 ? C9 H9C . 0.9600 ? C10 O15 . 1.252(2) ? C10 C11 . 1.400(3) ? C11 C12 . 1.390(3) ? C11 H11 . 0.9300 ? C12 O14 . 1.264(2) ? C12 C13 . 1.501(3) ? C13 H13A . 0.9600 ? C13 H13B . 0.9600 ? C13 H13C . 0.9600 ? 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' 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 O14 Zn1 O14 2_666 . 180.0 ? O14 Zn1 O15 2_666 . 90.49(5) ? O14 Zn1 O15 . . 89.51(5) y O14 Zn1 O15 2_666 2_666 89.51(5) ? O14 Zn1 O15 . 2_666 90.49(5) ? O15 Zn1 O15 . 2_666 180.0 ? O14 Zn1 N4 2_666 . 90.78(6) ? O14 Zn1 N4 . . 89.22(6) y O15 Zn1 N4 . . 91.29(6) y O15 Zn1 N4 2_666 . 88.71(6) ? O14 Zn1 N4 2_666 2_666 89.22(6) ? O14 Zn1 N4 . 2_666 90.78(6) ? O15 Zn1 N4 . 2_666 88.71(6) ? O15 Zn1 N4 2_666 2_666 91.29(6) ? N4 Zn1 N4 . 2_666 180.00(7) ? C2 C1 C6 . . 116.99(19) ? C2 C1 C7 . . 123.68(18) ? C6 C1 C7 . . 119.32(19) ? C3 C2 C1 . . 119.51(18) ? C3 C2 H2 . . 120.2 ? C1 C2 H2 . . 120.2 ? N4 C3 C2 . . 123.53(18) ? N4 C3 H3 . . 118.2 ? C2 C3 H3 . . 118.2 ? C5 N4 C3 . . 116.54(18) ? C5 N4 Zn1 . . 120.20(13) ? C3 N4 Zn1 . . 123.20(13) ? N4 C5 C6 . . 123.7(2) ? N4 C5 H5 . . 118.2 ? C6 C5 H5 . . 118.2 ? C5 C6 C1 . . 119.7(2) ? C5 C6 H6 . . 120.1 ? C1 C6 H6 . . 120.1 ? N8 C7 C1 . . 122.54(19) ? N8 C7 H7 . . 118.7 ? C1 C7 H7 . . 118.7 ? C7 N8 N8 . 2_457 111.8(2) ? C10 C9 H9A . . 109.5 ? C10 C9 H9B . . 109.5 ? H9A C9 H9B . . 109.5 ? C10 C9 H9C . . 109.5 ? H9A C9 H9C . . 109.5 ? H9B C9 H9C . . 109.5 ? O15 C10 C11 . . 125.56(19) ? O15 C10 C9 . . 115.9(2) ? C11 C10 C9 . . 118.5(2) ? C12 C11 C10 . . 126.54(19) ? C12 C11 H11 . . 116.7 ? C10 C11 H11 . . 116.7 ? O14 C12 C11 . . 125.66(19) ? O14 C12 C13 . . 115.30(19) ? C11 C12 C13 . . 119.04(19) ? C12 C13 H13A . . 109.5 ? C12 C13 H13B . . 109.5 ? H13A C13 H13B . . 109.5 ? C12 C13 H13C . . 109.5 ? H13A C13 H13C . . 109.5 ? H13B C13 H13C . . 109.5 ? C12 O14 Zn1 . . 126.31(13) ? C10 O15 Zn1 . . 125.78(13) ? _journal_paper_doi 10.1107/S0108270106000540