#------------------------------------------------------------------------------ #$Date: 2013-08-29 16:37:19 +0100 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/13/2011334.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_2011334 loop_ _publ_author_name 'Wieczorrek, Carsten' _publ_section_title ; Tetraiodide von Tris(1,2-ethandiamin)komplexen der Metalle Zink und Nickel ; _journal_issue 9 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 1079 _journal_page_last 1081 _journal_volume 56 _journal_year 2000 _chemical_formula_iupac '[Zn(C2 H8 N2 )3 ][I3 ]I ' _chemical_formula_moiety 'C6 H24 N6 Zn 2+ , I3 - , I -' _chemical_formula_sum 'C6 H24 I4 N6 Zn' _chemical_formula_weight 753.28 _chemical_melting_point 457 _chemical_name_common Tris-Ethylendiamin-zinktetraiodid _chemical_name_systematic ; Tris(1,2-ethandiamin)zinktriiodid-iodid ; _space_group_IT_number 122 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall 'I -4 2bw' _symmetry_space_group_name_H-M 'I -4 2 d' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 14.7420(10) _cell_length_b 14.742 _cell_length_c 17.7910(10) _cell_measurement_reflns_used 5000 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.18 _cell_measurement_theta_min 2.76 _cell_volume 3866.5(3) _computing_cell_refinement ; IPDS-Programmsystem ; _computing_data_collection ; IPDS-Programmsystem (Stoe & Cie, 1996/97) ; _computing_data_reduction ; IPDS-Programmsystem ; _computing_molecular_graphics 'DIAMOND (Brandenburg, 1998)' _computing_publication_material ; WINGX (Farrugia, 1998), PARST95 (Nardelli, 1995), PLATON96 (Spek, 1996), CIFEDIT (Wieczorrek, 1999) ; _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 44.4 _diffrn_measured_fraction_theta_full .992 _diffrn_measured_fraction_theta_max .992 _diffrn_measurement_device_type 'Stoe & Cie. IPDS' _diffrn_measurement_method 'oszillation scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .0765 _diffrn_reflns_av_sigmaI/netI .0300 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 16727 _diffrn_reflns_theta_full 25.18 _diffrn_reflns_theta_max 25.18 _diffrn_reflns_theta_min 2.76 _exptl_absorpt_coefficient_mu 7.652 _exptl_absorpt_correction_T_max .232 _exptl_absorpt_correction_T_min .174 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; Die Absorptionskorrektur wurde unter WINGX V1.61 nach den Pyramidenfl\"achen <101> durchgef\"uhrt (Alcock 1970). ; _exptl_crystal_colour 'clear dark red' _exptl_crystal_density_diffrn 2.588 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'tetragonale Bipyramide nach <101>' _exptl_crystal_F_000 2752 _exptl_crystal_size_max .40 _exptl_crystal_size_mid .36 _exptl_crystal_size_min .36 _refine_diff_density_max .472 _refine_diff_density_min -.480 _refine_ls_abs_structure_details 'Flack (1983)' _refine_ls_abs_structure_Flack -.02(4) _refine_ls_extinction_coef .00167(5) _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)' _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 82 _refine_ls_number_reflns 1730 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.094 _refine_ls_R_factor_all .0218 _refine_ls_R_factor_gt .0196 _refine_ls_shift/su_max .001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+7.2246P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .0420 _reflns_number_gt 1631 _reflns_number_total 1730 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file jz1409.cif _[local]_cod_data_source_block I _cod_database_code 2011334 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x, -y+1/2, -z+1/4' '-x, y+1/2, -z+1/4' 'y, x+1/2, z+1/4' '-y, -x+1/2, z+1/4' '-y, x, -z' 'y, -x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1, -z+3/4' '-x+1/2, y+1, -z+3/4' 'y+1/2, x+1, z+3/4' '-y+1/2, -x+1, z+3/4' '-y+1/2, x+1/2, -z+1/2' 'y+1/2, -x+1/2, -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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol I1 .5000 .5000 .37741(3) .05352(15) Uani d S 1 . . I I2 .60152(2) .67050(2) .37813(2) .05671(12) Uani d . 1 . . I I3 .60136(3) 1.2500 .1250 .05170(14) Uani d S 1 . . I Zn .7500 1.22777(4) .3750 .03157(15) Uani d S 1 . . Zn N1 .6774(3) 1.1293(2) .3066(2) .0374(9) Uani d . 1 . . N H1A .6789 1.1462 .2580 .070(8) Uiso calc R 1 . . H H1B .7039 1.0745 .3107 .070(8) Uiso calc R 1 . . H C2 .5827(3) 1.1242(4) .3326(3) .0511(15) Uani d . 1 . . C H2A .5558 1.0674 .3162 .055(7) Uiso calc R 1 . . H H2B .5479 1.1735 .3109 .055(7) Uiso calc R 1 . . H C3 .5793(4) 1.1301(4) .4172(3) .0538(15) Uani d . 1 . . C H3A .5167 1.1302 .4340 .055(7) Uiso calc R 1 . . H H3B .6095 1.0779 .4390 .055(7) Uiso calc R 1 . . H N4 .6244(3) 1.2135(3) .4418(2) .0429(10) Uani d . 1 . . N H4A .6377 1.2102 .4911 .070(8) Uiso calc R 1 . . H H4B .5879 1.2616 .4342 .070(8) Uiso calc R 1 . . H N5 .8016(3) 1.3420(3) .4414(2) .0391(9) Uani d . 1 . . N H5A .7912 1.3322 .4906 .070(8) Uiso calc R 1 . . H H5B .8618 1.3479 .4345 .070(8) Uiso calc R 1 . . H C6 .7546(5) 1.4251(3) .4168(2) .0401(10) Uani d . 1 . . C H6A .7887 1.4780 .4327 .055(7) Uiso calc R 1 . . H H6B .6950 1.4280 .4397 .055(7) 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 I1 .0391(2) .0808(3) .0407(2) .0155(2) .000 .000 I2 .0615(2) .0646(2) .04400(19) .00266(16) .0059(2) -.01274 I3 .0348(2) .0841(3) .0363(2) .000 .000 .0055(3) Zn .0348(3) .0317(3) .0282(3) .000 -.0011(3) .000 N1 .042(2) .035(2) .035(2) -.0011(18) -.0024(17) -.0025(15) C2 .045(3) .050(3) .059(4) -.014(3) -.010(2) -.001(3) C3 .051(4) .063(4) .048(3) -.005(3) .010(2) .010(3) N4 .040(2) .053(2) .036(2) .0023(17) .0024(17) .0016(17) N5 .044(2) .043(2) .031(2) -.0016(18) -.0027(16) -.0017(17) C6 .051(3) .033(2) .037(2) .001(3) .005(2) -.0050(17) 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 I1 I2 . 2.9254(3) yes I1 I2 2_665 2.9254(3) no Zn N1 . 2.176(4) yes Zn N1 12_645 2.176(4) no Zn N5 . 2.193(4) yes Zn N5 12_645 2.193(4) no Zn N4 12_645 2.210(4) no Zn N4 . 2.210(4) yes N1 C2 . 1.472(6) no C2 C3 . 1.509(7) no C3 N4 . 1.464(7) no N5 C6 . 1.474(6) no C6 C6 12_645 1.492(8) no loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn .2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -.4742 1.8119 '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 I2 I1 I2 . 2_665 179.50(3) yes N1 Zn N1 . 12_645 96.3(2) no N1 Zn N5 . . 169.78(17) no N1 Zn N5 12_645 . 92.31(13) no N1 Zn N5 . 12_645 92.31(13) no N1 Zn N5 12_645 12_645 169.78(17) no N5 Zn N5 . 12_645 79.7(2) no N1 Zn N4 . 12_645 92.76(16) no N1 Zn N4 12_645 12_645 79.89(15) no N5 Zn N4 . 12_645 94.14(15) no N5 Zn N4 12_645 12_645 94.26(15) no N1 Zn N4 . . 79.89(15) no N1 Zn N4 12_645 . 92.76(16) no N5 Zn N4 . . 94.26(15) no N5 Zn N4 12_645 . 94.14(15) no N4 Zn N4 12_645 . 169.1(2) no C2 N1 Zn . . 109.0(3) no N1 C2 C3 . . 109.9(4) no N4 C3 C2 . . 109.4(5) no C3 N4 Zn . . 107.4(3) no C6 N5 Zn . . 108.4(3) no N5 C6 C6 . 12_645 109.8(3) no 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 _geom_hbond_publ_flag N1 H1A I3 . .90 3.04 3.855(4) 151 yes N1 H1B I3 16_465 .90 2.92 3.767(4) 159 yes N4 H4A I2 5 .90 2.96 3.765(4) 150 yes _cod_database_fobs_code 2011334