#------------------------------------------------------------------------------ #$Date: 2023-12-08 16:16:31 +0200 (Fri, 08 Dec 2023) $ #$Revision: 288183 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/64/1556446.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1556446 loop_ _publ_author_name 'Van Megen, M.' 'Reiss, G.J.' _publ_section_title ; I62- Anion Composed of Two Asymmetric Triiodide Moieties: A Competition between Halogen and Hydrogen Bond ; _journal_name_full Inorganics _journal_page_first 3 _journal_page_last 13 _journal_paper_doi 10.3390/inorganics1010003 _journal_volume 1 _journal_year 2013 _chemical_formula_moiety 'C8 H22 N2, 2(I3)' _chemical_formula_sum 'C8 H22 I6 N2' _chemical_formula_weight 907.68 _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _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 _cell_angle_alpha 76.531(2) _cell_angle_beta 78.842(2) _cell_angle_gamma 84.574(2) _cell_formula_units_Z 1 _cell_length_a 6.20008(14) _cell_length_b 7.0452(2) _cell_length_c 12.5770(3) _cell_measurement_reflns_used 12262 _cell_measurement_temperature 100(1) _cell_measurement_theta_max 32.2744 _cell_measurement_theta_min 2.9668 _cell_volume 523.46(2) _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 100(1) _diffrn_detector_area_resol_mean 16.2711 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\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 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0183 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 5489 _diffrn_reflns_theta_full 28.99 _diffrn_reflns_theta_max 28.99 _diffrn_reflns_theta_min 2.98 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 8.888 _exptl_absorpt_correction_T_max 0.850 _exptl_absorpt_correction_T_min 0.102 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid (Clark & Reid, 1995). ; _exptl_crystal_colour black-brown _exptl_crystal_density_diffrn 2.879 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 402 _exptl_crystal_size_max 0.4973 _exptl_crystal_size_mid 0.2828 _exptl_crystal_size_min 0.0180 _refine_diff_density_max 1.530 _refine_diff_density_min -1.058 _refine_diff_density_rms 0.265 _refine_ls_extinction_coef 0.0022(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.668 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 87 _refine_ls_number_reflns 5489 _refine_ls_number_restraints 9 _refine_ls_restrained_S_all 1.667 _refine_ls_R_factor_all 0.0355 _refine_ls_R_factor_gt 0.0341 _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^)+(0.015P)^2^+2.5P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0885 _refine_ls_wR_factor_ref 0.0888 _reflns_number_gt 5185 _reflns_number_total 5489 _reflns_threshold_expression >2sigma(I) _cod_data_source_file inorganics-01-00003-s002.cif _cod_data_source_block DAOHI _cod_depositor_comments ; The following automatic conversions were performed: data name '_atom_site_symetry_multiplicity' was replaced with '_atom_site_symmetry_multiplicity' as specified in the replacement file 'data/replacement-values/replacement_tags.lst'. Automatic conversion script Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas ; _cod_original_sg_symbol_H-M P-1 _cod_database_code 1556446 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.20401(5) 0.24805(5) 0.45477(3) 0.01542(8) Uani 1 1 d . . . I2 I -0.12127(5) 0.34587(4) 0.28037(3) 0.01450(8) Uani 1 1 d . . . I3 I -0.39664(5) 0.42562(5) 0.12413(3) 0.01893(9) Uani 1 1 d . . . N1 N 0.6391(7) 0.2404(7) 0.6075(4) 0.0194(9) Uani 1 1 d D . . H11 H 0.672(7) 0.362(2) 0.604(3) 0.028(11) Uiso 1 1 d D . . H12 H 0.516(4) 0.239(7) 0.582(3) 0.028(11) Uiso 1 1 d D . . H13 H 0.752(5) 0.177(6) 0.572(3) 0.028(11) Uiso 1 1 d D . . C1 C 0.6047(8) 0.1366(7) 0.7276(4) 0.0166(9) Uani 1 1 d D . . H1A H 0.5795 0.0001 0.7346 0.020 Uiso 1 1 calc R . . H1B H 0.4767 0.1949 0.7685 0.020 Uiso 1 1 calc R . . C2 C 0.8077(8) 0.1533(7) 0.7748(4) 0.0163(9) Uani 1 1 d . . . H2A H 0.8274 0.2901 0.7701 0.020 Uiso 1 1 calc R . . H2B H 0.9357 0.1029 0.7299 0.020 Uiso 1 1 calc R . . C3 C 0.7938(8) 0.0416(7) 0.8962(4) 0.0152(9) Uani 1 1 d . . . H3A H 0.6678 0.0933 0.9416 0.018 Uiso 1 1 calc R . . H3B H 0.7723 -0.0951 0.9014 0.018 Uiso 1 1 calc R . . C4 C 1.0020(8) 0.0584(7) 0.9405(4) 0.0163(9) Uani 1 1 d . . . H4A H 1.0197 0.1949 0.9377 0.020 Uiso 1 1 calc R . . H4B H 1.1283 0.0124 0.8926 0.020 Uiso 1 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 I1 0.01413(14) 0.01612(15) 0.01710(15) -0.00260(11) -0.00606(11) -0.00209(10) I2 0.01453(14) 0.01358(14) 0.01581(15) -0.00280(11) -0.00365(11) -0.00186(10) I3 0.02241(16) 0.01722(15) 0.01926(16) -0.00324(12) -0.01030(12) 0.00015(11) N1 0.019(2) 0.018(2) 0.022(2) -0.0003(17) -0.0105(17) -0.0029(16) C1 0.018(2) 0.012(2) 0.018(2) -0.0003(17) -0.0037(18) -0.0028(16) C2 0.013(2) 0.017(2) 0.021(2) -0.0061(18) -0.0040(18) -0.0020(16) C3 0.015(2) 0.017(2) 0.013(2) -0.0008(17) -0.0020(17) -0.0036(17) C4 0.015(2) 0.021(2) 0.012(2) -0.0015(18) -0.0004(17) -0.0044(17) 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' I I -0.4742 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 C1 N1 H11 107(3) . . C1 N1 H12 108(3) . . H11 N1 H12 111(3) . . C1 N1 H13 107(3) . . H11 N1 H13 110(3) . . H12 N1 H13 112(3) . . N1 C1 C2 108.8(4) . . N1 C1 H1A 109.9 . . C2 C1 H1A 109.9 . . N1 C1 H1B 109.9 . . C2 C1 H1B 109.9 . . H1A C1 H1B 108.3 . . C1 C2 C3 112.9(4) . . C1 C2 H2A 109.0 . . C3 C2 H2A 109.0 . . C1 C2 H2B 109.0 . . C3 C2 H2B 109.0 . . H2A C2 H2B 107.8 . . C4 C3 C2 111.6(4) . . C4 C3 H3A 109.3 . . C2 C3 H3A 109.3 . . C4 C3 H3B 109.3 . . C2 C3 H3B 109.3 . . H3A C3 H3B 108.0 . . C3 C4 C4 113.0(5) . 2_757 C3 C4 H4A 109.0 . . C4 C4 H4A 109.0 2_757 . C3 C4 H4B 109.0 . . C4 C4 H4B 109.0 2_757 . H4A C4 H4B 107.8 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 I2 I3 2.7739(4) . N1 C1 1.500(6) . N1 H11 0.893(8) . N1 H12 0.885(8) . N1 H13 0.891(8) . C1 C2 1.516(6) . C1 H1A 0.9700 . C1 H1B 0.9700 . C2 C3 1.537(7) . C2 H2A 0.9700 . C2 H2B 0.9700 . C3 C4 1.526(6) . C3 H3A 0.9700 . C3 H3B 0.9700 . C4 C4 1.528(9) 2_757 C4 H4A 0.9700 . C4 H4B 0.9700 . loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H12 I1 0.885(8) 2.727(13) 3.592(4) 166(4) . N1 H11 I1 0.893(8) 2.810(12) 3.688(4) 168(4) 2_666 N1 H13 I1 0.891(8) 2.93(3) 3.653(5) 139(4) 1_655 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 N1 C1 C2 C3 -176.8(4) . . . . C1 C2 C3 C4 179.0(4) . . . . C2 C3 C4 C4 -177.5(5) . . . 2_757