#------------------------------------------------------------------------------ #$Date: 2025-08-19 07:12:48 +0100 (Tue, 19 Aug 2025) $ #$Revision: 301798 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/13/2011335.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_2011335 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_paper_doi 10.1107/S0108270100008829 _journal_volume 56 _journal_year 2000 _chemical_formula_iupac '[Ni (C2 H8 N1 )3 ][I3 ] I' _chemical_formula_moiety 'C6 H24 N6 Ni 2+ , I3 - , I - ' _chemical_formula_sum 'C6 H24 I4 N6 Ni' _chemical_formula_weight 746.62 _chemical_melting_point 547 _chemical_name_common Tris-Ethylendiamin-nickeltetraiodid _chemical_name_systematic ; Tris(1,2-diaminoethan)nickeltriiodid-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 14.6700(10) _cell_length_b 14.670 _cell_length_c 17.754(2) _cell_measurement_reflns_used 5000 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26.12 _cell_measurement_theta_min 2.78 _cell_volume 3820.8(5) _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 .993 _diffrn_measured_fraction_theta_max .993 _diffrn_measurement_device_type 'IPDS (Stoe & Cie)' _diffrn_measurement_method 'oscillation 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 .0801 _diffrn_reflns_av_sigmaI/netI .0534 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _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 10875 _diffrn_reflns_theta_full 26.12 _diffrn_reflns_theta_max 26.12 _diffrn_reflns_theta_min 2.78 _exptl_absorpt_coefficient_mu 7.473 _exptl_absorpt_correction_T_max .350 _exptl_absorpt_correction_T_min .241 _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 2.596 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'tetragonale Bipyramide nach <101>' _exptl_crystal_F_000 2736 _exptl_crystal_size_max .35 _exptl_crystal_size_mid .28 _exptl_crystal_size_min .28 _refine_diff_density_max .742 _refine_diff_density_min -.639 _refine_ls_abs_structure_details 'Flack (1983)' _refine_ls_abs_structure_Flack .09(6) _refine_ls_extinction_coef .00019(3) _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)' _refine_ls_goodness_of_fit_ref .905 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 82 _refine_ls_number_reflns 1886 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all .905 _refine_ls_R_factor_all .0452 _refine_ls_R_factor_gt .0276 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0191P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .0516 _reflns_number_gt 1477 _reflns_number_total 1886 _reflns_threshold_expression I>2\s(I) _cod_data_source_file jz1409.cif _cod_data_source_block II _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_original_cell_volume 3820.8(6) _cod_database_code 2011335 _cod_database_fobs_code 2011335 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 -.37720(5) .04811(19) Uani d S 1 . . I I2 .32889(3) .39777(3) -.37798(4) .05060(15) Uani d . 1 . . I I3 .2500 .60145(4) -.1250 .04860(18) Uani d S 1 . . I Ni .22909(6) .7500 -.3750 .0260(2) Uani d S 1 . . Ni N1 .1311(4) .6813(4) -.3077(3) .0337(14) Uani d . 1 . . N H1A .1474 .6841 -.2589 .052(9) Uiso calc R 1 . . H H1B .0763 .7082 -.3128 .052(9) Uiso calc R 1 . . H C2 .1257(5) .5856(5) -.3321(5) .044(2) Uani d . 1 . . C H2C .0681 .5594 -.3163 .043(9) Uiso calc R 1 . . H H2D .1745 .5507 -.3091 .043(9) Uiso calc R 1 . . H C3 .1339(6) .5815(5) -.4177(5) .043(2) Uani d . 1 . . C H3C .1357 .5185 -.4342 .043(9) Uiso calc R 1 . . H H3D .0815 .6107 -.4407 .043(9) Uiso calc R 1 . . H N4 .2178(4) .6284(4) -.4403(3) .0388(15) Uani d . 1 . . N H4A .2156 .6422 -.4897 .052(9) Uiso calc R 1 . . H H4B .2663 .5922 -.4322 .052(9) Uiso calc R 1 . . H N5 .3389(4) .8025(4) -.4401(3) .0363(14) Uani d . 1 . . N H5A .3286 .7927 -.4894 .052(9) Uiso calc R 1 . . H H5B .3444 .8629 -.4326 .052(9) Uiso calc R 1 . . H C6 .4233(4) .7550(6) -.4161(3) .0360(15) Uani d . 1 . . C H6C .4263 .6954 -.4396 .043(9) Uiso calc R 1 . . H H6D .4762 .7897 -.4318 .043(9) 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 .0749(5) .0355(3) .0340(3) .0133(3) .000 .000 I2 .0600(3) .0567(3) .0351(2) .0006(2) -.0110(3) .0047(3) I3 .0844(5) .0323(3) .0291(3) .000 -.0046(5) .000 Ni .0290(6) .0303(5) .0186(5) .000 .000 .0018(5) N1 .038(3) .035(3) .028(3) -.001(3) .004(2) .000(3) C2 .046(5) .045(5) .040(5) -.020(4) .001(4) .009(4) C3 .057(5) .039(5) .032(5) -.007(4) -.006(4) -.007(3) N4 .052(4) .039(3) .025(3) .004(2) -.003(2) .001(3) N5 .042(3) .042(3) .025(3) -.003(3) -.001(3) .009(3) C6 .035(3) .041(4) .032(4) -.002(4) .004(3) -.007(4) 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' Ni Ni .3393 1.1124 '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 I3 I2 5 15_554 66.042(16) no I2 I1 I2 2_665 . 179.45(4) yes I1 I2 I3 . 13_444 177.606(19) no N1 Ni N1 3_564 . 94.8(3) no N1 Ni N5 3_564 3_564 172.0(2) no N1 Ni N5 . 3_564 92.02(19) no N1 Ni N5 3_564 . 92.02(19) no N1 Ni N5 . . 172.0(2) no N5 Ni N5 3_564 . 81.6(3) no N1 Ni N4 3_564 3_564 81.7(2) no N1 Ni N4 . 3_564 92.2(2) no N5 Ni N4 3_564 3_564 93.8(2) no N5 Ni N4 . 3_564 93.0(2) no N1 Ni N4 3_564 . 92.2(2) no N1 Ni N4 . . 81.7(2) no N5 Ni N4 3_564 . 93.0(2) no N5 Ni N4 . . 93.8(2) no N4 Ni N4 3_564 . 171.1(3) no C2 N1 Ni . . 108.9(4) no N1 C2 C3 . . 109.0(6) no N4 C3 C2 . . 108.7(7) no C3 N4 Ni . . 108.0(4) no C6 N5 Ni . . 107.8(4) no C6 C6 N5 3_564 . 109.4(5) no 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 I3 I2 5 3.9793(7) no I3 I2 15_554 3.9793(7) no I1 I2 2_665 2.9241(5) no I1 I2 . 2.9241(5) yes I2 I3 13_444 3.9793(7) no Ni N1 3_564 2.123(5) no Ni N1 . 2.123(5) yes Ni N5 3_564 2.127(6) no Ni N5 . 2.127(6) yes Ni N4 3_564 2.134(5) no Ni N4 . 2.134(5) yes N1 C2 . 1.472(9) no C2 C3 . 1.526(9) no C3 N4 . 1.466(9) no N5 C6 . 1.483(8) no C6 C6 3_564 1.467(12) 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 H1B I3 14_554 .90 2.90 3.753(6) 159 yes N4 H4A I2 14_554 .90 3.00 3.791(5) 148 yes 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 I2 I1 I2 I3 2_665 13_444 115.6(7) no N1 Ni N1 C2 3_564 . 103.8(5) no N5 Ni N1 C2 3_564 . -80.5(4) no N5 Ni N1 C2 . . -44.2(19) no N4 Ni N1 C2 3_564 . -174.3(4) no N4 Ni N1 C2 . . 12.2(4) no Ni N1 C2 C3 . . -38.5(8) no N1 C2 C3 N4 . . 54.7(9) no C2 C3 N4 Ni . . -42.2(7) no N1 Ni N4 C3 3_564 . -77.7(5) no N1 Ni N4 C3 . . 16.8(4) no N5 Ni N4 C3 3_564 . 108.4(4) no N5 Ni N4 C3 . . -169.8(4) no N4 Ni N4 C3 3_564 . -30.7(4) no N1 Ni N5 C6 3_564 . -170.7(5) no N1 Ni N5 C6 . . -23(2) no N5 Ni N5 C6 3_564 . 14.1(3) no N4 Ni N5 C6 3_564 . 107.5(5) no N4 Ni N5 C6 . . -78.4(5) no Ni N5 C6 C6 . 3_564 -40.9(9) no loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 PubChem 139057918