#------------------------------------------------------------------------------ #$Date: 2024-03-06 01:35:49 +0200 (Wed, 06 Mar 2024) $ #$Revision: 290348 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/82/7248275.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_7248275 loop_ _publ_author_name 'Korobeynikov, Nikita A.' 'Usoltsev, Andrey N.' 'Sokolov, Maksim Nailyevich' 'Novikov, Alexander S.' 'Adonin, Sergey A.' _publ_section_title ; Polymeric polyiodo-chlorotellurates(IV): new supramolecular hybrids within the halometalate chemistry ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D4CE00088A _journal_year 2024 _chemical_formula_moiety 'I2, Cl6 Te, 2(C6 H8 N)' _chemical_formula_sum 'C12 H16 Cl6 I2 N2 Te' _chemical_formula_weight 782.37 _space_group_crystal_system tetragonal _space_group_IT_number 92 _space_group_name_Hall 'P 4abw 2nw' _space_group_name_H-M_alt 'P 41 21 2' _atom_sites_solution_hydrogens geom _audit_creation_date 2023-10-23 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _audit_update_record ; 2023-11-24 deposited with the CCDC. 2024-03-05 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.4279(2) _cell_length_b 9.4279(2) _cell_length_c 25.1636(7) _cell_measurement_reflns_used 9934 _cell_measurement_temperature 150.00 _cell_measurement_theta_max 31.43 _cell_measurement_theta_min 2.70 _cell_volume 2236.67(9) _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2017/1 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 150.00 _diffrn_detector PIXEL _diffrn_detector_area_resol_mean 7.41 _diffrn_detector_type 'Bruker PHOTON III area detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker D8 Venture diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_unetI/netI 0.0307 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 20945 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.516 _diffrn_reflns_theta_min 2.307 _diffrn_source 'Incoatec IuS3.0 microfocus X-ray tube' _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_voltage 50.0 _exptl_absorpt_coefficient_mu 4.806 _exptl_absorpt_correction_T_max 0.7462 _exptl_absorpt_correction_T_min 0.6396 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0727 before and 0.0605 after correction. The Ratio of minimum to maximum transmission is 0.8571. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'dark red' _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 2.323 _exptl_crystal_description block _exptl_crystal_F_000 1448 _exptl_crystal_size_max 0.062 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.035 _refine_diff_density_max 0.468 _refine_diff_density_min -0.770 _refine_diff_density_rms 0.094 _refine_ls_abs_structure_details ; Flack x determined using 1285 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.045(13) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 107 _refine_ls_number_reflns 3730 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all 0.0274 _refine_ls_R_factor_gt 0.0226 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0136P)^2^+0.1754P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0390 _reflns_Friedel_coverage 0.676 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 1.000 _reflns_number_gt 3422 _reflns_number_total 3730 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ce00088a2.cif _cod_data_source_block nk1018_a _cod_original_cell_volume 2236.67(11) _cod_database_code 7248275 _shelx_shelxl_version_number 2017/1 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.850 _shelx_estimated_absorpt_t_min 0.755 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C6(H6) 2.b Idealised Me refined as rotating group: C1(H1A,H1B,H1C) ; _shelx_res_file ; TITL NK1018_a.res in P4(1)2(1)2 nk1018_a.res created by SHELXL-2017/1 at 15:10:12 on 23-Oct-2023 REM Old TITL NK1018 in P4(1)2(1)2 REM SHELXT solution in P4(1)2(1)2 REM R1 0.043, Rweak 0.019, Alpha 0.002, Orientation as input REM Flack x = -0.046 ( 0.013 ) from Parsons' quotients REM Formula found by SHELXT: C12 N2 Cl6 Te I2 CELL 0.71073 9.4279 9.4279 25.1636 90 90 90 ZERR 4 0.0002 0.0002 0.0007 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM 0.5-Y,0.5+X,0.25+Z SYMM 0.5+Y,0.5-X,0.75+Z SYMM 0.5-X,0.5+Y,0.25-Z SYMM 0.5+X,0.5-Y,0.75-Z SYMM +Y,+X,-Z SYMM -Y,-X,0.5-Z SFAC C H Cl I N Te UNIT 48 64 24 8 8 4 L.S. 10 PLAN 6 SIZE 0.062 0.04 0.035 TEMP -123.15 CONF LIST 4 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.013600 0.175400 FVAR 0.20517 I1 4 0.264897 0.071723 0.484461 11.00000 0.02697 0.02795 = 0.02546 -0.00289 0.00313 0.00288 TE1 6 0.640997 0.640997 0.500000 10.50000 0.01560 0.01560 = 0.01596 -0.00154 0.00154 0.00194 CL1 3 0.466490 0.816875 0.459488 11.00000 0.02865 0.02492 = 0.03321 0.00089 -0.00177 0.00727 CL2 3 0.827748 0.827748 0.500000 10.50000 0.02710 0.02710 = 0.03634 -0.00430 0.00430 -0.00843 CL3 3 0.566693 0.709651 0.593163 11.00000 0.03228 0.03129 = 0.01990 -0.00520 0.00490 0.00319 CL4 3 0.448941 0.448941 0.500000 10.50000 0.02528 0.02528 = 0.02991 -0.00131 0.00131 -0.00637 N1 5 0.526080 0.158073 0.604248 11.00000 0.02309 0.02919 = 0.01923 -0.00005 -0.00069 0.00113 C1 1 0.636780 0.107220 0.567833 11.00000 0.03112 0.04336 = 0.02952 -0.00862 0.00681 -0.00098 AFIX 137 H1A 2 0.618125 0.143301 0.531984 11.00000 -1.50000 H1B 2 0.636499 0.003284 0.567272 11.00000 -1.50000 H1C 2 0.729553 0.141155 0.579954 11.00000 -1.50000 AFIX 0 C2 1 0.525382 0.295756 0.618803 11.00000 0.02746 0.02385 = 0.02771 0.00037 -0.00188 -0.00403 AFIX 43 H2 2 0.596508 0.358491 0.606048 11.00000 -1.20000 AFIX 0 C3 1 0.420638 0.344712 0.652333 11.00000 0.03617 0.02299 = 0.03237 -0.00316 -0.00111 0.00053 AFIX 43 H3 2 0.419117 0.441648 0.662626 11.00000 -1.20000 AFIX 0 C4 1 0.318615 0.253531 0.670840 11.00000 0.02712 0.03706 = 0.02640 -0.00200 0.00216 0.00688 AFIX 43 H4 2 0.246649 0.286781 0.694145 11.00000 -1.20000 AFIX 0 C5 1 0.321266 0.113099 0.655358 11.00000 0.02411 0.03232 = 0.03104 0.00606 0.00018 -0.00109 AFIX 43 H5 2 0.250608 0.048893 0.667432 11.00000 -1.20000 AFIX 0 C6 1 0.427357 0.067877 0.622329 11.00000 0.02820 0.02390 = 0.02940 -0.00024 -0.00139 -0.00240 AFIX 43 H6 2 0.431086 -0.029009 0.612051 11.00000 -1.20000 AFIX 0 HKLF 4 REM NK1018_a.res in P4(1)2(1)2 REM R1 = 0.0226 for 3422 Fo > 4sig(Fo) and 0.0274 for all 3730 data REM 107 parameters refined using 0 restraints END WGHT 0.0136 0.1754 REM Highest difference peak 0.468, deepest hole -0.770, 1-sigma level 0.094 Q1 1 0.2435 0.1209 0.4610 11.00000 0.05 0.47 Q2 1 0.6161 0.6451 0.5964 11.00000 0.05 0.38 Q3 1 0.3189 0.5311 0.6670 11.00000 0.05 0.36 Q4 1 0.4017 0.2840 0.6750 11.00000 0.05 0.35 Q5 1 0.6923 0.7218 0.5982 11.00000 0.05 0.34 Q6 1 0.3558 0.2982 0.6531 11.00000 0.05 0.34 ; _shelx_res_checksum 10986 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -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_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 I1 I 0.26490(3) 0.07172(3) 0.48446(2) 0.02680(7) Uani 1 1 d . . . . . Te1 Te 0.64100(2) 0.64100(2) 0.500000 0.01572(7) Uani 1 2 d S T P . . Cl1 Cl 0.46649(10) 0.81688(10) 0.45949(4) 0.0289(2) Uani 1 1 d . . . . . Cl2 Cl 0.82775(9) 0.82775(9) 0.500000 0.0302(3) Uani 1 2 d S T P . . Cl3 Cl 0.56669(11) 0.70965(10) 0.59316(3) 0.0278(2) Uani 1 1 d . . . . . Cl4 Cl 0.44894(9) 0.44894(9) 0.500000 0.0268(3) Uani 1 2 d S T P . . N1 N 0.5261(3) 0.1581(3) 0.60425(11) 0.0238(7) Uani 1 1 d . . . . . C1 C 0.6368(4) 0.1072(5) 0.56783(15) 0.0347(10) Uani 1 1 d . . . . . H1A H 0.618125 0.143301 0.531984 0.052 Uiso 1 1 calc R U . . . H1B H 0.636499 0.003284 0.567272 0.052 Uiso 1 1 calc R U . . . H1C H 0.729553 0.141155 0.579954 0.052 Uiso 1 1 calc R U . . . C2 C 0.5254(4) 0.2958(4) 0.61880(14) 0.0263(8) Uani 1 1 d . . . . . H2 H 0.596508 0.358491 0.606048 0.032 Uiso 1 1 calc R U . . . C3 C 0.4206(5) 0.3447(4) 0.65233(15) 0.0305(9) Uani 1 1 d . . . . . H3 H 0.419117 0.441648 0.662626 0.037 Uiso 1 1 calc R U . . . C4 C 0.3186(4) 0.2535(5) 0.67084(14) 0.0302(9) Uani 1 1 d . . . . . H4 H 0.246649 0.286781 0.694145 0.036 Uiso 1 1 calc R U . . . C5 C 0.3213(4) 0.1131(5) 0.65536(15) 0.0292(9) Uani 1 1 d . . . . . H5 H 0.250608 0.048893 0.667432 0.035 Uiso 1 1 calc R U . . . C6 C 0.4274(4) 0.0679(4) 0.62233(13) 0.0272(8) Uani 1 1 d . . . . . H6 H 0.431086 -0.029009 0.612051 0.033 Uiso 1 1 calc R U . . . 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 0.02697(14) 0.02795(14) 0.02546(11) -0.00289(10) 0.00313(9) 0.00288(11) Te1 0.01560(9) 0.01560(9) 0.01596(12) -0.00154(8) 0.00154(8) 0.00194(13) Cl1 0.0286(5) 0.0249(5) 0.0332(4) 0.0009(4) -0.0018(4) 0.0073(4) Cl2 0.0271(4) 0.0271(4) 0.0363(6) -0.0043(4) 0.0043(4) -0.0084(5) Cl3 0.0323(5) 0.0313(5) 0.0199(4) -0.0052(3) 0.0049(4) 0.0032(4) Cl4 0.0253(4) 0.0253(4) 0.0299(5) -0.0013(4) 0.0013(4) -0.0064(5) N1 0.0231(17) 0.0292(18) 0.0192(13) -0.0001(12) -0.0007(12) 0.0011(15) C1 0.031(2) 0.043(3) 0.0295(18) -0.0086(17) 0.0068(17) -0.001(2) C2 0.027(2) 0.024(2) 0.0277(18) 0.0004(15) -0.0019(15) -0.0040(16) C3 0.036(2) 0.023(2) 0.0324(18) -0.0032(16) -0.0011(17) 0.0005(19) C4 0.027(2) 0.037(2) 0.0264(18) -0.0020(17) 0.0022(15) 0.0069(19) C5 0.024(2) 0.032(2) 0.0310(19) 0.0061(17) 0.0002(15) -0.0011(17) C6 0.028(2) 0.0239(19) 0.0294(17) -0.0002(15) -0.0014(16) -0.0024(18) 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' Cl Cl 0.1484 0.1585 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 '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 Cl1 Te1 Cl1 179.59(5) . 7_556 ? Cl1 Te1 Cl4 90.21(2) 7_556 . ? Cl1 Te1 Cl4 90.21(2) . . ? Cl2 Te1 Cl1 89.79(2) . . ? Cl2 Te1 Cl1 89.79(2) . 7_556 ? Cl2 Te1 Cl3 90.85(2) . 7_556 ? Cl2 Te1 Cl3 90.85(2) . . ? Cl2 Te1 Cl4 180.000(14) . . ? Cl3 Te1 Cl1 88.55(3) . 7_556 ? Cl3 Te1 Cl1 88.55(3) 7_556 . ? Cl3 Te1 Cl1 91.46(3) 7_556 7_556 ? Cl3 Te1 Cl1 91.46(3) . . ? Cl3 Te1 Cl3 178.29(5) . 7_556 ? Cl3 Te1 Cl4 89.15(2) . . ? Cl3 Te1 Cl4 89.15(2) 7_556 . ? C2 N1 C1 119.1(3) . . ? C6 N1 C1 119.9(3) . . ? C6 N1 C2 121.0(3) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2 120.3 . . ? N1 C2 C3 119.5(4) . . ? C3 C2 H2 120.3 . . ? C2 C3 H3 120.0 . . ? C4 C3 C2 120.0(4) . . ? C4 C3 H3 120.0 . . ? C3 C4 H4 120.2 . . ? C3 C4 C5 119.5(4) . . ? C5 C4 H4 120.2 . . ? C4 C5 H5 120.5 . . ? C6 C5 C4 118.9(4) . . ? C6 C5 H5 120.5 . . ? N1 C6 C5 121.1(4) . . ? N1 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? 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 I1 I1 2.6917(5) 7_556 ? Te1 Cl1 2.5486(9) 7_556 ? Te1 Cl1 2.5486(9) . ? Te1 Cl2 2.4900(13) . ? Te1 Cl3 2.5310(8) 7_556 ? Te1 Cl3 2.5309(8) . ? Te1 Cl4 2.5607(13) . ? N1 C1 1.469(5) . ? N1 C2 1.349(5) . ? N1 C6 1.340(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2 0.9500 . ? C2 C3 1.378(5) . ? C3 H3 0.9500 . ? C3 C4 1.372(5) . ? C4 H4 0.9500 . ? C4 C5 1.380(6) . ? C5 H5 0.9500 . ? C5 C6 1.369(5) . ? C6 H6 0.9500 . ? 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 N1 C2 C3 C4 0.3(6) . . . . ? C1 N1 C2 C3 179.0(3) . . . . ? C1 N1 C6 C5 -178.6(3) . . . . ? C2 N1 C6 C5 1.2(5) . . . . ? C2 C3 C4 C5 -0.4(6) . . . . ? C3 C4 C5 C6 0.9(6) . . . . ? C4 C5 C6 N1 -1.3(6) . . . . ? C6 N1 C2 C3 -0.7(5) . . . . ?