#------------------------------------------------------------------------------ #$Date: 2016-02-20 03:06:23 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176774 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/52/2205242.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_2205242 loop_ _publ_author_name 'Helena Elengoz' 'Rinat Shoshnik' 'Israel Goldberg' _publ_section_title ; Tris(biacetyl dihydrazone-\k^2^N,N')zinc(II) bis(perchlorate) at 110K ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m538 _journal_page_last m540 _journal_paper_doi 10.1107/S1600536805004757 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac '[Zn (C4 H10 N4)3] (Cl O4)2' _chemical_formula_moiety 'C12 H30 N12 Zn 2+, 2Cl O4 -' _chemical_formula_sum 'C12 H30 Cl2 N12 O8 Zn' _chemical_formula_weight 606.75 _chemical_name_systematic ; Tris(biacetyl dihydrazone-\k^2^N,N')zinc(II) bis(perchlorate) ; _space_group_IT_number 165 _symmetry_cell_setting trigonal _symmetry_space_group_name_Hall '-P 3 2"c' _symmetry_space_group_name_H-M 'P -3 c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 2 _cell_length_a 9.4496(4) _cell_length_b 9.4496(4) _cell_length_c 15.3237(4) _cell_measurement_reflns_used 1664 _cell_measurement_temperature 110(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 2.49 _cell_volume 1185.01(8) _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997)' _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_data_reduction DENZO _computing_molecular_graphics ; ORTEPIII (Burnett & Johnson, 1996) and MERCURY (Bruno et al., 2002) ; _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _diffrn_ambient_temperature 110(2) _diffrn_detector_area_resol_mean '56 microns' _diffrn_measured_fraction_theta_full 0.977 _diffrn_measured_fraction_theta_max 0.977 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \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 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 6818 _diffrn_reflns_theta_full 27.48 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_min 2.49 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.328 _exptl_absorpt_correction_T_max 0.8787 _exptl_absorpt_correction_T_min 0.6536 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_crystal_colour 'light yellow' _exptl_crystal_density_diffrn 1.700 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Needle _exptl_crystal_F_000 628 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.364 _refine_diff_density_min -0.417 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 57 _refine_ls_number_reflns 893 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.982 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0354 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0348P)^2^+2.7971P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0814 _refine_ls_wR_factor_ref 0.0897 _reflns_number_gt 705 _reflns_number_total 893 _reflns_threshold_expression I>2\s(I)' _cod_data_source_file ci6528.cif _cod_data_source_block I _cod_database_code 2205242 _cod_database_fobs_code 2205242 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'y, x, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-y, -x, z-1/2' 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 0.0000 0.0000 0.2500 0.0108(2) Uani d S 1 Zn N2 0.2321(3) 0.1259(3) 0.08856(12) 0.0166(5) Uani d . 1 N H2A 0.3403 0.1815 0.0697 0.033(9) Uiso d R 1 H H2B 0.1830 0.1944 0.0801 0.033(9) Uiso d R 1 H N3 0.2168(3) 0.0698(2) 0.17354(13) 0.0127(5) Uani d . 1 N C4 0.3231(3) 0.0379(3) 0.20537(15) 0.0128(5) Uani d . 1 C C5 0.4754(3) 0.0701(3) 0.15924(18) 0.0191(6) Uani d . 1 C H5A 0.4553 0.0573 0.0962 0.029 Uiso calc R 1 H H5B 0.5084 -0.0075 0.1794 0.029 Uiso calc R 1 H H5C 0.5627 0.1818 0.1718 0.029 Uiso calc R 1 H Cl6 0.3333 0.6667 0.07464(6) 0.0156(2) Uani d S 1 Cl O7 0.2608(3) 0.5007(2) 0.04370(12) 0.0295(5) Uani d . 1 O O8 0.3333 0.6667 0.16832(19) 0.0192(7) Uani d S 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 0.0124(4) 0.012 0.0077(3) 0.006 0.000 0.000 N2 0.0182(11) 0.0221(12) 0.0094(10) 0.0100(10) 0.0036(8) 0.0053(8) N3 0.0139(11) 0.0141(10) 0.0083(10) 0.0057(8) 0.0018(8) 0.0016(7) C4 0.0132(13) 0.0092(11) 0.0142(12) 0.0041(10) 0.0010(9) -0.0016(9) C5 0.0160(13) 0.0172(14) 0.0229(14) 0.0075(12) 0.0051(10) 0.0016(11) Cl6 0.0175(5) 0.021 0.0093(5) 0.011 0.000 0.000 O7 0.0348(13) 0.0251(11) 0.0253(11) 0.0124(10) -0.0036(9) -0.0135(8) O8 0.0253(16) 0.025 0.0070(14) 0.012 0.000 0.000 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' N N 0.0061 0.0033 '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' Cl Cl 0.1484 0.1585 '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 N3 Zn1 N3 6 4 93.31(7) ? N3 Zn1 N3 6 5 93.31(7) ? N3 Zn1 N3 4 5 93.31(7) y N3 Zn1 N3 6 . 102.24(11) y N3 Zn1 N3 4 . 74.33(11) yes N3 Zn1 N3 5 . 160.52(11) ? N3 Zn1 N3 6 3 160.52(11) y N3 Zn1 N3 4 3 102.24(11) ? N3 Zn1 N3 5 3 74.33(11) ? N3 Zn1 N3 . 3 93.30(7) y N3 Zn1 N3 6 2 74.33(11) ? N3 Zn1 N3 4 2 160.52(11) ? N3 Zn1 N3 5 2 102.24(11) ? N3 Zn1 N3 . 2 93.30(7) ? N3 Zn1 N3 3 2 93.30(7) ? N3 N2 H2A . . 112.5 ? N3 N2 H2B . . 112.7 ? H2A N2 H2B . . 109.7 ? C4 N3 N2 . . 120.3(2) ? C4 N3 Zn1 . . 117.25(16) ? N2 N3 Zn1 . . 121.89(16) ? N3 C4 C5 . . 124.2(2) ? N3 C4 C4 . 4 115.54(14) ? C5 C4 C4 . 4 120.31(14) ? 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 ? O8 Cl6 O7 . 3_565 109.21(9) ? O8 Cl6 O7 . 2_665 109.20(9) ? O7 Cl6 O7 3_565 2_665 109.76(9) ? O8 Cl6 O7 . . 109.20(9) ? O7 Cl6 O7 3_565 . 109.75(9) ? O7 Cl6 O7 2_665 . 109.71(9) ? 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 N3 6 2.158(2) ? Zn1 N3 4 2.158(2) ? Zn1 N3 5 2.158(2) ? Zn1 N3 . 2.158(2) yes Zn1 N3 3 2.158(2) ? Zn1 N3 2 2.158(2) ? N2 N3 . 1.386(3) yes N2 H2A . 0.93 ? N2 H2B . 0.98 ? N3 C4 . 1.281(3) yes C4 C5 . 1.492(3) yes C4 C4 4 1.502(5) yes C5 H5A . 0.98 ? C5 H5B . 0.98 ? C5 H5C . 0.98 ? Cl6 O8 . 1.435(3) ? Cl6 O7 3_565 1.441(2) ? Cl6 O7 2_665 1.442(2) ? Cl6 O7 . 1.442(2) ? 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_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag N3 Zn1 N3 C4 6 . 91.09(19) ? N3 Zn1 N3 C4 4 . 1.07(14) ? N3 Zn1 N3 C4 5 . -51.11(18) ? N3 Zn1 N3 C4 3 . -100.7(2) ? N3 Zn1 N3 C4 2 . 165.77(19) ? N3 Zn1 N3 N2 6 . -97.69(19) ? N3 Zn1 N3 N2 4 . 172.3(2) ? N3 Zn1 N3 N2 5 . 120.11(18) ? N3 Zn1 N3 N2 3 . 70.49(15) ? N3 Zn1 N3 N2 2 . -23.01(18) ? N2 N3 C4 C5 . . 5.4(4) yes Zn1 N3 C4 C5 . . 176.80(19) ? N2 N3 C4 C4 . 4 -174.1(2) yes Zn1 N3 C4 C4 . 4 -2.7(3) ?