#------------------------------------------------------------------------------ #$Date: 2016-03-26 18:27:35 +0200 (Sat, 26 Mar 2016) $ #$Revision: 180430 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/20/99/7209978.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_7209978 loop_ _publ_author_name 'W\;ec\/lawik, Magdalena' 'G\;agor, Anna' 'Piecha, Anna' 'Jakubas, Ryszard' 'Medycki, Wojciech' _publ_section_title ; Synthesis, crystal structure and phase transitions of a series of imidazolium iodides ; _journal_issue 28 _journal_name_full CrystEngComm _journal_page_first 5633 _journal_paper_doi 10.1039/c3ce40559a _journal_volume 15 _journal_year 2013 _chemical_formula_sum 'C3 H5 I N2' _chemical_formula_weight 195.99 _chemical_name_systematic ; ? ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 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 106.647(6) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 7.8732(5) _cell_length_b 15.4592(7) _cell_length_c 9.6771(6) _cell_measurement_reflns_used 11100 _cell_measurement_temperature 110(2) _cell_measurement_theta_max 25.68 _cell_measurement_theta_min 3.0 _cell_volume 1128.47(12) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 110(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _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 0.0923 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 11100 _diffrn_reflns_theta_full 25.68 _diffrn_reflns_theta_max 25.68 _diffrn_reflns_theta_min 3.00 _exptl_absorpt_coefficient_mu 5.534 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.77653 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_density_diffrn 2.307 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _refine_diff_density_max 4.839 _refine_diff_density_min -1.538 _refine_diff_density_rms 0.474 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.276 _refine_ls_matrix_type full _refine_ls_number_parameters 109 _refine_ls_number_reflns 2123 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.276 _refine_ls_R_factor_all 0.0683 _refine_ls_R_factor_gt 0.0624 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+4.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1320 _refine_ls_wR_factor_ref 0.1342 _reflns_number_gt 1878 _reflns_number_total 2123 _reflns_threshold_expression >2sigma(I) _cod_data_source_file c3ce40559a.txt _cod_data_source_block 5 _cod_original_cell_volume 1128.47(11) _cod_original_sg_symbol_H-M P2(1)/n _cod_database_code 7209978 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 I1 I 0.23838(7) 0.01081(4) 0.21078(6) 0.0175(2) Uani 1 1 d . I2 I 0.47291(8) 0.23997(4) 0.98632(5) 0.0188(2) Uani 1 1 d . N1 N 0.2816(11) 0.0376(6) 0.8369(9) 0.0263(18) Uani 1 1 d . H1 H 0.3086 0.0709 0.9112 0.032 Uiso 1 1 calc R N3 N 0.2273(11) -0.0757(6) 0.7094(10) 0.032(2) Uani 1 1 d . H3 H 0.2133 -0.1292 0.6843 0.038 Uiso 1 1 calc R C2 C 0.2454(12) 0.0651(8) 0.7002(11) 0.031(2) Uani 1 1 d . H2 H 0.2459 0.1220 0.6695 0.038 Uiso 1 1 calc R C4 C 0.2703(13) -0.0469(7) 0.8419(11) 0.027(2) Uani 1 1 d . H4 H 0.2894 -0.0803 0.9248 0.033 Uiso 1 1 calc R C5 C 0.2079(16) -0.0060(8) 0.6158(13) 0.041(3) Uani 1 1 d . H5 H 0.1758 -0.0078 0.5156 0.049 Uiso 1 1 calc R N6 N 0.0003(9) 0.1831(6) -0.0012(8) 0.0242(19) Uani 1 1 d . H6 H 0.0119 0.1294 0.0230 0.029 Uiso 1 1 calc R N8 N -0.0522(11) 0.2978(5) -0.1285(9) 0.0286(19) Uani 1 1 d . H8 H -0.0812 0.3315 -0.2022 0.034 Uiso 1 1 calc R C7 C -0.0467(13) 0.2125(6) -0.1338(10) 0.026(2) Uani 1 1 d . H7 H -0.0718 0.1791 -0.2171 0.031 Uiso 1 1 calc R C9 C 0.0277(16) 0.2511(8) 0.0924(11) 0.040(3) Uani 1 1 d . H9 H 0.0622 0.2478 0.1926 0.048 Uiso 1 1 calc R C10 C -0.0046(12) 0.3244(8) 0.0123(11) 0.032(3) Uani 1 1 d . H10 H 0.0037 0.3810 0.0460 0.039 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 0.0204(3) 0.0145(3) 0.0164(3) 0.00040(19) 0.0035(2) -0.00062(19) I2 0.0245(3) 0.0142(3) 0.0182(3) 0.00084(19) 0.0071(2) 0.0000(2) N1 0.027(4) 0.024(4) 0.029(4) -0.012(4) 0.010(3) 0.001(4) N3 0.024(4) 0.021(5) 0.055(6) -0.016(4) 0.018(4) -0.008(3) C2 0.020(5) 0.029(6) 0.044(7) 0.014(5) 0.010(4) -0.004(4) C4 0.028(5) 0.030(5) 0.027(5) 0.004(4) 0.014(4) 0.004(4) C5 0.030(6) 0.075(10) 0.021(5) 0.003(5) 0.012(5) 0.007(5) N6 0.021(4) 0.020(4) 0.033(5) 0.012(3) 0.010(4) 0.004(3) N8 0.028(4) 0.020(4) 0.035(5) 0.012(3) 0.005(4) 0.001(3) C7 0.032(5) 0.027(5) 0.022(5) -0.007(4) 0.011(4) -0.006(4) C9 0.028(6) 0.074(9) 0.021(5) -0.007(6) 0.012(4) -0.004(5) C10 0.019(5) 0.028(6) 0.050(7) -0.019(5) 0.010(5) -0.003(4) 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 C4 N1 C2 110.8(8) C4 N1 H1 124.6 C2 N1 H1 124.6 C4 N3 C5 108.9(9) C4 N3 H3 125.5 C5 N3 H3 125.5 C5 C2 N1 106.7(9) C5 C2 H2 126.7 N1 C2 H2 126.7 N1 C4 N3 107.7(9) N1 C4 H4 126.1 N3 C4 H4 126.1 C2 C5 N3 105.9(10) C2 C5 H5 127.1 N3 C5 H5 127.1 C7 N6 C9 109.2(9) C7 N6 H6 125.4 C9 N6 H6 125.4 C7 N8 C10 109.6(8) C7 N8 H8 125.2 C10 N8 H8 125.2 N8 C7 N6 108.2(8) N8 C7 H7 125.9 N6 C7 H7 125.9 C10 C9 N6 107.2(9) C10 C9 H9 126.4 N6 C9 H9 126.4 C9 C10 N8 105.8(9) C9 C10 H10 127.1 N8 C10 H10 127.1 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N1 C4 1.311(15) N1 C2 1.339(13) N1 H1 0.8600 N3 C4 1.307(13) N3 C5 1.388(15) N3 H3 0.8600 C2 C5 1.350(16) C2 H2 0.9300 C4 H4 0.9300 C5 H5 0.9300 N6 C7 1.311(11) N6 C9 1.364(14) N6 H6 0.8600 N8 C7 1.320(13) N8 C10 1.368(12) N8 H8 0.8600 C7 H7 0.9300 C9 C10 1.355(16) C9 H9 0.9300 C10 H10 0.9300 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 H1 I2 0.86 2.91 3.591(8) 136.9 . N3 H3 I2 0.86 2.75 3.533(8) 151.5 2_546 N6 H6 I1 0.86 2.83 3.551(8) 143.1 . N8 H8 I1 0.86 2.83 3.525(8) 139.6 4_565