#------------------------------------------------------------------------------ #$Date: 2020-06-04 04:46:27 +0300 (Thu, 04 Jun 2020) $ #$Revision: 252629 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/06/7240610.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_7240610 loop_ _publ_author_name 'Gugin, Nikita' 'Presypkina, Eugenia V.' 'Virovets, Alexander Viktorovich' 'Davydova, Elena I.' 'Timoshkin, Alexey Y.' _publ_section_title ; Structural Variety of Aluminium and Gallium Coordination Polymers Based on Bis-pyridylethylene: From Molecular Complexes to Ionic Networks ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D0CE00541J _journal_year 2020 _chemical_formula_moiety 'C12 H10 Cl3 Ga N2' _chemical_formula_sum 'C12 H10 Cl3 Ga N2' _chemical_formula_weight 358.29 _chemical_properties_physical Air-sensitive,Moisture-sensitive _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-02-17 deposited with the CCDC. 2020-06-03 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90.785(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.92433(19) _cell_length_b 7.46902(18) _cell_length_c 26.5125(6) _cell_measurement_reflns_used 3119 _cell_measurement_temperature 90(2) _cell_measurement_theta_max 73.8820 _cell_measurement_theta_min 6.1290 _cell_volume 1371.04(6) _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution SHELXT _diffrn_ambient_temperature 90(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 4.2047 _diffrn_detector_type TitanS2 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.977 _diffrn_measurement_device_type 'Rigaku Oxford Diffraction SuperNova' _diffrn_measurement_method '\w scans' _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_unetI/netI 0.0343 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.977 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 6120 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.977 _diffrn_reflns_theta_full 67.500 _diffrn_reflns_theta_max 73.994 _diffrn_reflns_theta_min 3.334 _diffrn_source_type 'microfocus SuperNova source' _exptl_absorpt_coefficient_mu 7.977 _exptl_absorpt_correction_T_max 0.944 _exptl_absorpt_correction_T_min 0.501 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.736 _exptl_crystal_description 'elongated prism' _exptl_crystal_F_000 712 _exptl_crystal_recrystallization_method Sublimation _exptl_crystal_size_max 0.231 _exptl_crystal_size_mid 0.061 _exptl_crystal_size_min 0.029 _refine_diff_density_max 0.801 _refine_diff_density_min -0.472 _refine_diff_density_rms 0.086 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 163 _refine_ls_number_reflns 2728 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.965 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0279 _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^)+(0.0450P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0688 _refine_ls_wR_factor_ref 0.0705 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2268 _reflns_number_total 2728 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ce00541j2.cif _cod_data_source_block ayt58 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7240610 _shelx_shelxl_version_number 2018/3 _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_min 0.260 _shelx_estimated_absorpt_t_max 0.802 _shelx_res_file ; TITL ayt58 in P2(1)/n at 90K newGV noerr a58.res created by SHELXL-2018/3 at 16:00:57 on 06-Feb-2020 CELL 1.54178 6.92433 7.46902 26.51248 90.0000 90.7854 90.0000 ZERR 4.00 0.00019 0.00018 0.00064 0.0000 0.0023 0.0000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N CL GA UNIT 48 40 8 12 4 TEMP -183 L.S. 10 SIZE 0.231 0.061 0.029 PLAN 10 BOND $H FMAP 2 ACTA 135 OMIT 2 8 10 WGHT 0.045000 FVAR 0.13648 GA1 5 0.285018 0.779407 0.129434 11.00000 0.01330 0.01483 = 0.00790 -0.00023 -0.00073 0.00135 CL1 4 -0.009478 0.819122 0.157265 11.00000 0.01434 0.02518 = 0.01095 -0.00036 0.00103 0.00340 CL2 4 0.460707 1.004286 0.101423 11.00000 0.01975 0.01946 = 0.01252 0.00309 -0.00178 -0.00357 CL3 4 0.414133 0.510161 0.128611 11.00000 0.01939 0.01648 = 0.01356 -0.00093 -0.00178 0.00505 N1 3 0.397169 0.813041 0.205584 11.00000 0.01686 0.01681 = 0.00964 -0.00058 -0.00121 0.00106 N2 3 0.675476 0.759345 0.553008 11.00000 0.01592 0.01697 = 0.01085 -0.00051 -0.00269 0.00044 C1 1 0.563262 0.895262 0.217848 11.00000 0.01534 0.02245 = 0.01174 -0.00014 0.00049 0.00102 AFIX 43 H1 2 0.634428 0.951534 0.191888 11.00000 -1.20000 AFIX 0 C2 1 0.635773 0.901679 0.266932 11.00000 0.01386 0.02443 = 0.01528 -0.00106 -0.00161 -0.00063 AFIX 43 H2 2 0.754592 0.960802 0.273968 11.00000 -1.20000 AFIX 0 C3 1 0.533530 0.820936 0.305973 11.00000 0.01860 0.01764 = 0.01096 -0.00055 -0.00289 0.00141 C4 1 0.361326 0.733137 0.292636 11.00000 0.02317 0.01858 = 0.00799 0.00119 -0.00283 -0.00565 AFIX 43 H4 2 0.287169 0.674974 0.317677 11.00000 -1.20000 AFIX 0 C5 1 0.300501 0.731819 0.243011 11.00000 0.02194 0.01802 = 0.01310 0.00206 -0.00185 -0.00387 AFIX 43 H5 2 0.184226 0.670430 0.234669 11.00000 -1.20000 AFIX 0 C6 1 0.606418 0.827964 0.358048 11.00000 0.01938 0.02050 = 0.01136 -0.00078 -0.00355 -0.00129 AFIX 43 H6 2 0.733053 0.872940 0.363955 11.00000 -1.20000 AFIX 0 C7 1 0.504067 0.774374 0.397765 11.00000 0.01816 0.01776 = 0.01270 0.00059 -0.00527 -0.00167 AFIX 43 H7 2 0.377503 0.730739 0.390955 11.00000 -1.20000 AFIX 0 C8 1 0.567831 0.776300 0.450759 11.00000 0.01856 0.01561 = 0.01199 0.00080 -0.00238 0.00129 C9 1 0.757421 0.813525 0.466564 11.00000 0.01812 0.02032 = 0.01095 0.00162 0.00132 -0.00066 AFIX 43 H9 2 0.852615 0.845796 0.442753 11.00000 -1.20000 AFIX 0 C10 1 0.804054 0.802561 0.517485 11.00000 0.01741 0.02043 = 0.01158 -0.00043 -0.00268 -0.00213 AFIX 43 H10 2 0.933366 0.826806 0.527793 11.00000 -1.20000 AFIX 0 C11 1 0.492816 0.726554 0.538227 11.00000 0.01503 0.02476 = 0.01513 0.00143 -0.00025 -0.00220 AFIX 43 H11 2 0.400172 0.697017 0.562983 11.00000 -1.20000 AFIX 0 C12 1 0.434718 0.734351 0.487978 11.00000 0.01688 0.02724 = 0.01241 -0.00078 -0.00322 -0.00015 AFIX 43 H12 2 0.303926 0.711058 0.478893 11.00000 -1.20000 AFIX 0 HKLF 4 REM ayt58 in P2(1)/n at 90K newGV noerr REM wR2 = 0.0705, GooF = S = 0.965, Restrained GooF = 0.965 for all data REM R1 = 0.0279 for 2268 Fo > 4sig(Fo) and 0.0357 for all 2728 data REM 163 parameters refined using 0 restraints END WGHT 0.0450 0.0000 REM Highest difference peak 0.801, deepest hole -0.472, 1-sigma level 0.086 Q1 1 0.1373 0.7942 0.1409 11.00000 0.05 0.80 Q2 1 0.4034 0.7861 0.1137 11.00000 0.05 0.64 Q3 1 0.1980 0.8427 0.1737 11.00000 0.05 0.43 Q4 1 0.5252 0.5381 0.1115 11.00000 0.05 0.41 Q5 1 0.3003 0.5204 0.1450 11.00000 0.05 0.38 Q6 1 0.3204 0.7954 0.3983 11.00000 0.05 0.36 Q7 1 0.5135 0.7424 0.1362 11.00000 0.05 0.32 Q8 1 0.7273 0.7293 0.5854 11.00000 0.05 0.32 Q9 1 0.4641 0.7431 0.5111 11.00000 0.05 0.32 Q10 1 0.5083 0.7573 0.4718 11.00000 0.05 0.31 ; _shelx_res_checksum 543 loop_ _space_group_symop_operation_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_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 Ga1 Ga 0.28502(4) 0.77941(4) 0.12943(2) 0.01202(10) Uani 1 1 d . . . . . Cl1 Cl -0.00948(8) 0.81912(8) 0.15726(2) 0.01681(13) Uani 1 1 d . . . . . Cl2 Cl 0.46071(8) 1.00429(8) 0.10142(2) 0.01726(13) Uani 1 1 d . . . . . Cl3 Cl 0.41413(8) 0.51016(8) 0.12861(2) 0.01649(13) Uani 1 1 d . . . . . N1 N 0.3972(3) 0.8130(3) 0.20558(7) 0.0145(4) Uani 1 1 d . . . . . N2 N 0.6755(3) 0.7593(3) 0.55301(7) 0.0146(4) Uani 1 1 d . . . . . C1 C 0.5633(4) 0.8953(4) 0.21785(9) 0.0165(5) Uani 1 1 d . . . . . H1 H 0.634428 0.951534 0.191888 0.020 Uiso 1 1 calc R U . . . C2 C 0.6358(4) 0.9017(4) 0.26693(9) 0.0179(5) Uani 1 1 d . . . . . H2 H 0.754592 0.960802 0.273968 0.021 Uiso 1 1 calc R U . . . C3 C 0.5335(4) 0.8209(3) 0.30597(9) 0.0158(5) Uani 1 1 d . . . . . C4 C 0.3613(4) 0.7331(3) 0.29264(9) 0.0166(5) Uani 1 1 d . . . . . H4 H 0.287169 0.674974 0.317677 0.020 Uiso 1 1 calc R U . . . C5 C 0.3005(4) 0.7318(3) 0.24301(9) 0.0177(5) Uani 1 1 d . . . . . H5 H 0.184226 0.670430 0.234669 0.021 Uiso 1 1 calc R U . . . C6 C 0.6064(4) 0.8280(3) 0.35805(9) 0.0171(5) Uani 1 1 d . . . . . H6 H 0.733053 0.872940 0.363955 0.021 Uiso 1 1 calc R U . . . C7 C 0.5041(4) 0.7744(3) 0.39776(9) 0.0163(5) Uani 1 1 d . . . . . H7 H 0.377503 0.730739 0.390955 0.020 Uiso 1 1 calc R U . . . C8 C 0.5678(4) 0.7763(3) 0.45076(9) 0.0154(5) Uani 1 1 d . . . . . C9 C 0.7574(4) 0.8135(3) 0.46656(9) 0.0165(5) Uani 1 1 d . . . . . H9 H 0.852615 0.845796 0.442753 0.020 Uiso 1 1 calc R U . . . C10 C 0.8041(4) 0.8026(3) 0.51748(9) 0.0165(5) Uani 1 1 d . . . . . H10 H 0.933366 0.826806 0.527793 0.020 Uiso 1 1 calc R U . . . C11 C 0.4928(4) 0.7266(4) 0.53823(10) 0.0183(5) Uani 1 1 d . . . . . H11 H 0.400172 0.697017 0.562983 0.022 Uiso 1 1 calc R U . . . C12 C 0.4347(4) 0.7344(4) 0.48798(10) 0.0189(5) Uani 1 1 d . . . . . H12 H 0.303926 0.711058 0.478893 0.023 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 Ga1 0.01330(15) 0.01483(16) 0.00790(15) -0.00023(10) -0.00073(10) 0.00135(11) Cl1 0.0143(3) 0.0252(3) 0.0110(3) -0.0004(2) 0.0010(2) 0.0034(2) Cl2 0.0198(3) 0.0195(3) 0.0125(3) 0.0031(2) -0.0018(2) -0.0036(2) Cl3 0.0194(3) 0.0165(3) 0.0136(3) -0.0009(2) -0.0018(2) 0.0050(2) N1 0.0169(10) 0.0168(10) 0.0096(9) -0.0006(7) -0.0012(7) 0.0011(8) N2 0.0159(10) 0.0170(10) 0.0108(10) -0.0005(8) -0.0027(8) 0.0004(8) C1 0.0153(12) 0.0225(12) 0.0117(11) -0.0001(9) 0.0005(9) 0.0010(10) C2 0.0139(11) 0.0244(13) 0.0153(12) -0.0011(10) -0.0016(9) -0.0006(10) C3 0.0186(12) 0.0176(12) 0.0110(11) -0.0006(9) -0.0029(9) 0.0014(10) C4 0.0232(13) 0.0186(12) 0.0080(11) 0.0012(9) -0.0028(9) -0.0056(10) C5 0.0219(13) 0.0180(12) 0.0131(12) 0.0021(9) -0.0019(10) -0.0039(10) C6 0.0194(12) 0.0205(12) 0.0114(11) -0.0008(9) -0.0035(9) -0.0013(10) C7 0.0182(12) 0.0178(12) 0.0127(12) 0.0006(9) -0.0053(9) -0.0017(9) C8 0.0186(12) 0.0156(11) 0.0120(12) 0.0008(9) -0.0024(9) 0.0013(9) C9 0.0181(12) 0.0203(12) 0.0110(11) 0.0016(9) 0.0013(9) -0.0007(10) C10 0.0174(12) 0.0204(13) 0.0116(12) -0.0004(9) -0.0027(9) -0.0021(10) C11 0.0150(12) 0.0248(13) 0.0151(12) 0.0014(10) -0.0002(9) -0.0022(10) C12 0.0169(12) 0.0272(13) 0.0124(12) -0.0008(10) -0.0032(9) -0.0002(10) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga -1.2846 0.7763 '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 N1 Ga1 N2 178.88(8) . 4_575 ? N1 Ga1 Cl1 89.65(6) . . ? N2 Ga1 Cl1 91.00(6) 4_575 . ? N1 Ga1 Cl3 88.55(6) . . ? N2 Ga1 Cl3 90.33(6) 4_575 . ? Cl1 Ga1 Cl3 120.36(3) . . ? N1 Ga1 Cl2 91.90(6) . . ? N2 Ga1 Cl2 88.54(6) 4_575 . ? Cl1 Ga1 Cl2 121.87(3) . . ? Cl3 Ga1 Cl2 117.77(3) . . ? C1 N1 C5 117.4(2) . . ? C1 N1 Ga1 125.06(17) . . ? C5 N1 Ga1 117.26(16) . . ? C11 N2 C10 118.0(2) . . ? C11 N2 Ga1 124.31(17) . 4_676 ? C10 N2 Ga1 117.33(16) . 4_676 ? N1 C1 C2 122.8(2) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C1 C2 C3 119.9(2) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C2 C3 C4 116.9(2) . . ? C2 C3 C6 120.7(2) . . ? C4 C3 C6 122.4(2) . . ? C5 C4 C3 119.5(2) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? N1 C5 C4 123.5(2) . . ? N1 C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? C7 C6 C3 123.5(2) . . ? C7 C6 H6 118.3 . . ? C3 C6 H6 118.3 . . ? C6 C7 C8 126.5(2) . . ? C6 C7 H7 116.7 . . ? C8 C7 H7 116.7 . . ? C12 C8 C9 117.3(2) . . ? C12 C8 C7 118.8(2) . . ? C9 C8 C7 123.9(2) . . ? C10 C9 C8 119.0(2) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? N2 C10 C9 123.3(2) . . ? N2 C10 H10 118.4 . . ? C9 C10 H10 118.4 . . ? N2 C11 C12 122.2(2) . . ? N2 C11 H11 118.9 . . ? C12 C11 H11 118.9 . . ? C11 C12 C8 120.2(2) . . ? C11 C12 H12 119.9 . . ? C8 C12 H12 119.9 . . ? 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 Ga1 N1 2.168(2) . ? Ga1 N2 2.173(2) 4_575 ? Ga1 Cl1 2.1982(6) . ? Ga1 Cl3 2.2010(6) . ? Ga1 Cl2 2.2085(7) . ? N1 C1 1.340(3) . ? N1 C5 1.349(3) . ? N2 C11 1.342(3) . ? N2 C10 1.344(3) . ? C1 C2 1.389(3) . ? C1 H1 0.9500 . ? C2 C3 1.399(4) . ? C2 H2 0.9500 . ? C3 C4 1.402(4) . ? C3 C6 1.464(3) . ? C4 C5 1.376(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.339(4) . ? C6 H6 0.9500 . ? C7 C8 1.467(3) . ? C7 H7 0.9500 . ? C8 C12 1.395(4) . ? C8 C9 1.400(4) . ? C9 C10 1.386(3) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.388(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ?