#------------------------------------------------------------------------------ #$Date: 2020-05-07 00:15:04 +0300 (Thu, 07 May 2020) $ #$Revision: 251826 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/04/7240456.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_7240456 loop_ _publ_author_name 'Hachem, Hadi' 'Jeannin, olivier' 'Fourmigue, Marc' 'Barriere, Frederic' 'Lorcy, Dominique' _publ_section_title ; Halogen bonded metal bis(dithiolene) 2D frameworks ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D0CE00512F _journal_year 2020 _chemical_formula_moiety 'C4 I N O S3' _chemical_formula_sum 'C4 I N O S3' _chemical_formula_weight 301.13 _space_group_IT_number 14 _space_group_name_Hall '-P 2yab' _space_group_name_H-M_alt 'P 1 21/a 1' _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2yab' _symmetry_space_group_name_H-M 'P 1 21/a 1' _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4.3 _audit_creation_date 2017-07-17T17:26:30-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_update_record ; 2020-04-02 deposited with the CCDC. 2020-05-06 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 95.676(13) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.017(3) _cell_length_b 9.118(3) _cell_length_c 9.594(3) _cell_measurement_reflns_used 2531 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 27.18 _cell_measurement_theta_min 2.96 _cell_measurement_wavelength 0.71073 _cell_volume 784.9(4) _computing_cell_refinement 'Bruker APEX2 (Bruker, 2014)' _computing_data_collection 'Bruker APEX2 (Bruker, 2014)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2014)' _computing_molecular_graphics 'Ortep for Windows (Farrugia, 2012)' _computing_publication_material 'WinGX publication routines (Farrugia, 2012)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SIR-92 (Altomare et al., 1994)' _diffrn_ambient_temperature 296(2) _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.942 _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_orient_matrix_UB_11 0.076202 _diffrn_orient_matrix_UB_12 -0.072924 _diffrn_orient_matrix_UB_13 -0.024259 _diffrn_orient_matrix_UB_21 0.061602 _diffrn_orient_matrix_UB_22 0.081255 _diffrn_orient_matrix_UB_23 -0.034045 _diffrn_orient_matrix_UB_31 0.053107 _diffrn_orient_matrix_UB_32 0.010384 _diffrn_orient_matrix_UB_33 0.096041 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0578 _diffrn_reflns_av_unetI/netI 0.063 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.942 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 4843 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.942 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.209 _diffrn_reflns_theta_min 3.089 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 4.803 _exptl_absorpt_correction_T_max 0.825 _exptl_absorpt_correction_T_min 0.379 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.548 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 560 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.04 _refine_diff_density_max 1.435 _refine_diff_density_min -0.886 _refine_diff_density_rms 0.184 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 91 _refine_ls_number_reflns 1819 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.091 _refine_ls_R_factor_all 0.0843 _refine_ls_R_factor_gt 0.0521 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+6.7839P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1214 _refine_ls_wR_factor_ref 0.1477 _reflns_Friedel_coverage 0 _reflns_number_gt 1278 _reflns_number_total 1819 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ce00512f2.cif _cod_data_source_block C4INOS3 _cod_original_sg_symbol_H-M 'P 21/a' _cod_database_code 7240456 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL SIR92 run in space group P 21/a CELL 0.71073 9.0170 9.1180 9.5940 90.000 95.676 90.000 ZERR 2.00 0.0030 0.0030 0.0030 0.000 0.013 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, - Z SFAC C N S I O UNIT 16 4 12 4 4 MERG 2 FMAP 2 PLAN 25 ACTA BOND $H CONF L.S. 10 TEMP 23.00 WGHT 0.035500 6.783899 FVAR 0.49197 C1 1 0.095279 0.438122 0.861307 11.00000 0.06580 0.04250 = 0.05857 -0.01239 0.02118 -0.01601 C2 1 0.062654 0.159368 0.829024 11.00000 0.04960 0.03310 = 0.04360 -0.00134 0.00373 0.00008 C3 1 -0.034770 0.219824 0.727181 11.00000 0.05067 0.02346 = 0.04114 -0.00066 0.00557 0.00474 C4 1 -0.085271 -0.007158 0.680771 11.00000 0.05315 0.02892 = 0.03752 -0.00293 0.00486 0.00101 N1 2 -0.116999 0.127042 0.642143 11.00000 0.05308 0.03189 = 0.04221 0.00465 0.00160 0.00054 S1 3 -0.039354 0.412327 0.717737 11.00000 0.07256 0.02772 = 0.07053 0.00321 0.00111 -0.00099 S2 3 0.169644 0.275366 0.942671 11.00000 0.06078 0.05282 = 0.05055 -0.00993 -0.00751 -0.00739 S3 3 0.049699 -0.027577 0.819495 11.00000 0.06597 0.03438 = 0.04917 0.00279 -0.00766 0.00689 I1 4 -0.189332 -0.188919 0.581408 11.00000 0.06317 0.03480 = 0.05910 -0.00749 0.00723 -0.00677 O1 5 0.135632 0.557996 0.904960 11.00000 0.10099 0.05061 = 0.08119 -0.01937 0.01799 -0.03043 HKLF 4 REM SIR92 run in space group P 21/a REM R1 = 0.0521 for 1278 Fo > 4sig(Fo) and 0.0843 for all 1819 data REM 91 parameters refined using 0 restraints END WGHT 0.0330 7.1756 REM Highest difference peak 1.435, deepest hole -0.886, 1-sigma level 0.184 Q1 1 -0.0841 -0.1817 0.5614 11.00000 0.05 1.43 Q2 1 -0.0644 0.3083 0.7340 11.00000 0.05 1.27 Q3 1 -0.1897 -0.1015 0.5360 11.00000 0.05 1.03 Q4 1 -0.2931 -0.1663 0.6060 11.00000 0.05 1.03 Q5 1 -0.1518 -0.1844 0.6816 11.00000 0.05 1.02 Q6 1 -0.0693 0.4697 0.6563 11.00000 0.05 1.01 Q7 1 -0.2149 -0.1619 0.4567 11.00000 0.05 0.85 Q8 1 0.0936 -0.0935 0.8820 11.00000 0.05 0.71 Q9 1 0.0465 0.6442 0.8215 11.00000 0.05 0.70 Q10 1 -0.1977 -0.2821 0.5173 11.00000 0.05 0.69 Q11 1 0.0420 -0.2156 0.7790 11.00000 0.05 0.61 Q12 1 -0.1484 -0.2974 0.5396 11.00000 0.05 0.60 Q13 1 0.1732 0.4709 0.9795 11.00000 0.05 0.56 Q14 1 -0.0704 0.2550 0.6031 11.00000 0.05 0.54 Q15 1 0.1366 -0.1433 0.9637 11.00000 0.05 0.53 Q16 1 0.1165 0.7600 0.9751 11.00000 0.05 0.51 Q17 1 -0.2582 -0.0811 0.6384 11.00000 0.05 0.51 Q18 1 0.0293 0.2939 0.6771 11.00000 0.05 0.49 Q19 1 -0.1876 -0.0656 0.6545 11.00000 0.05 0.48 Q20 1 0.0575 0.5302 0.8382 11.00000 0.05 0.47 Q21 1 0.1063 0.2216 0.8841 11.00000 0.05 0.46 Q22 1 0.0653 -0.0247 0.7154 11.00000 0.05 0.45 Q23 1 -0.3817 -0.0680 0.5801 11.00000 0.05 0.44 Q24 1 0.0219 0.3933 0.6912 11.00000 0.05 0.43 Q25 1 -0.0005 0.1886 0.8510 11.00000 0.05 0.43 ; _shelx_res_checksum 25708 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0953(11) 0.4381(11) 0.8613(10) 0.055(2) Uani 1 1 d . . . . . C2 C 0.0627(10) 0.1594(9) 0.8290(9) 0.0422(19) Uani 1 1 d . . . . . C3 C -0.0348(10) 0.2198(8) 0.7272(9) 0.0384(17) Uani 1 1 d . . . . . C4 C -0.0853(10) -0.0072(9) 0.6808(8) 0.0398(18) Uani 1 1 d . . . . . N1 N -0.1170(8) 0.1270(8) 0.6421(7) 0.0426(16) Uani 1 1 d . . . . . S1 S -0.0394(3) 0.4123(2) 0.7177(3) 0.0573(6) Uani 1 1 d . . . . . S2 S 0.1696(3) 0.2754(3) 0.9427(3) 0.0556(6) Uani 1 1 d . . . . . S3 S 0.0497(3) -0.0276(2) 0.8195(2) 0.0507(6) Uani 1 1 d . . . . . I1 I -0.18933(7) -0.18892(6) 0.58141(7) 0.0523(3) Uani 1 1 d . . . . . O1 O 0.1356(10) 0.5580(8) 0.9050(8) 0.077(2) Uani 1 1 d . . . . . 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 C1 0.066(6) 0.043(5) 0.059(6) -0.012(4) 0.021(5) -0.016(4) C2 0.050(5) 0.033(4) 0.044(4) -0.001(3) 0.004(4) 0.000(3) C3 0.051(5) 0.023(4) 0.041(4) -0.001(3) 0.006(4) 0.005(3) C4 0.053(5) 0.029(4) 0.038(4) -0.003(3) 0.005(4) 0.001(3) N1 0.053(4) 0.032(4) 0.042(4) 0.005(3) 0.002(3) 0.001(3) S1 0.0726(17) 0.0277(11) 0.0705(16) 0.0032(10) 0.0011(13) -0.0010(10) S2 0.0608(15) 0.0528(15) 0.0505(13) -0.0099(11) -0.0075(11) -0.0074(11) S3 0.0660(15) 0.0344(11) 0.0492(12) 0.0028(9) -0.0077(11) 0.0069(10) I1 0.0632(4) 0.0348(4) 0.0591(4) -0.0075(3) 0.0072(3) -0.0068(3) O1 0.101(6) 0.051(5) 0.081(5) -0.019(4) 0.018(5) -0.030(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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' O O 0.0106 0.006 '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 _geom_angle_publ_flag O1 C1 S1 123.4(9) . . ? O1 C1 S2 120.9(9) . . ? S1 C1 S2 115.7(5) . . ? C3 C2 S3 109.2(6) . . ? C3 C2 S2 118.7(6) . . ? S3 C2 S2 132.0(5) . . ? N1 C3 C2 117.2(7) . . ? N1 C3 S1 126.0(6) . . ? C2 C3 S1 116.8(7) . . ? N1 C4 S3 116.1(6) . . ? N1 C4 I1 122.7(6) . . ? S3 C4 I1 121.2(4) . . ? C4 N1 C3 109.0(7) . . ? C3 S1 C1 94.7(4) . . ? C2 S2 C1 94.0(4) . . ? C2 S3 C4 88.4(4) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.213(11) . ? C1 S1 1.759(11) . ? C1 S2 1.777(11) . ? C2 C3 1.364(12) . ? C2 S3 1.710(8) . ? C2 S2 1.741(9) . ? C3 N1 1.346(11) . ? C3 S1 1.758(8) . ? C4 N1 1.302(10) . ? C4 S3 1.722(8) . ? C4 I1 2.088(8) . ? 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 _geom_torsion_publ_flag S3 C2 C3 N1 -0.7(10) . . . . ? S2 C2 C3 N1 -179.2(6) . . . . ? S3 C2 C3 S1 -179.8(5) . . . . ? S2 C2 C3 S1 1.6(10) . . . . ? S3 C4 N1 C3 -1.7(10) . . . . ? I1 C4 N1 C3 178.7(6) . . . . ? C2 C3 N1 C4 1.5(11) . . . . ? S1 C3 N1 C4 -179.5(7) . . . . ? N1 C3 S1 C1 179.7(8) . . . . ? C2 C3 S1 C1 -1.2(8) . . . . ? O1 C1 S1 C3 -178.8(9) . . . . ? S2 C1 S1 C3 0.5(6) . . . . ? C3 C2 S2 C1 -1.0(8) . . . . ? S3 C2 S2 C1 -179.2(7) . . . . ? O1 C1 S2 C2 179.4(9) . . . . ? S1 C1 S2 C2 0.1(6) . . . . ? C3 C2 S3 C4 -0.2(7) . . . . ? S2 C2 S3 C4 178.1(7) . . . . ? N1 C4 S3 C2 1.1(7) . . . . ? I1 C4 S3 C2 -179.2(5) . . . . ?