#------------------------------------------------------------------------------ #$Date: 2020-06-04 04:46:27 +0300 (Thu, 04 Jun 2020) $ #$Revision: 252629 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/06/7240612.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_7240612 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 Al2 Cl6 N2' _chemical_formula_sum 'C12 H10 Al2 Cl6 N2' _chemical_formula_weight 448.88 _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-2014/7 _audit_update_record ; 2020-02-17 deposited with the CCDC. 2020-06-03 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 91.122(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 6.5757(3) _cell_length_b 11.6146(4) _cell_length_c 12.0455(4) _cell_measurement_reflns_used 3066 _cell_measurement_temperature 90(2) _cell_measurement_theta_max 73.7810 _cell_measurement_theta_min 5.2740 _cell_volume 919.79(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-2014/7 (Sheldrick, 2014)' _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 0.987 _diffrn_measured_fraction_theta_max 0.972 _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 0.0286 _diffrn_reflns_av_unetI/netI 0.0292 _diffrn_reflns_Laue_measured_fraction_full 0.987 _diffrn_reflns_Laue_measured_fraction_max 0.972 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 6025 _diffrn_reflns_point_group_measured_fraction_full 0.987 _diffrn_reflns_point_group_measured_fraction_max 0.972 _diffrn_reflns_theta_full 67.500 _diffrn_reflns_theta_max 73.934 _diffrn_reflns_theta_min 5.291 _diffrn_source_type 'microfocus SuperNova source' _exptl_absorpt_coefficient_mu 9.418 _exptl_absorpt_correction_T_max 0.811 _exptl_absorpt_correction_T_min 0.690 _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 1.621 _exptl_crystal_description block _exptl_crystal_F_000 448 _exptl_crystal_recrystallization_method Sublimation _exptl_crystal_size_max 0.057 _exptl_crystal_size_mid 0.047 _exptl_crystal_size_min 0.032 _refine_diff_density_max 0.353 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.060 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.917 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 100 _refine_ls_number_reflns 1815 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.917 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0239 _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^)+(0.0387P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.0583 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1464 _reflns_number_total 1815 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ce00541j2.cif _cod_data_source_block ayt57 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7240612 _shelx_shelxl_version_number 2014/7 _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 0.616 _shelx_estimated_absorpt_t_max 0.753 _shelx_res_file ; a57.res created by SHELXL-2014/7 TITL ayt57 in P2(1)/n at 90K newGV noerr CELL 1.54178 6.57571 11.61460 12.04554 90.0000 91.1224 90.0000 ZERR 2.00 0.00028 0.00043 0.00037 0.0000 0.0032 0.0000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N AL CL UNIT 24 20 4 4 12 TEMP -183 L.S. 10 PLAN 10 BOND $H fmap 2 acta 135 OMIT 6 4 8 SIZE 0.057 0.047 0.032 WGHT 0.038700 FVAR 0.61759 AL1 4 -0.274900 0.344180 0.592068 11.00000 0.01673 0.01456 = 0.01259 -0.00089 0.00103 0.00050 CL1 5 -0.496381 0.277334 0.700013 11.00000 0.02058 0.02134 = 0.01566 -0.00127 0.00391 -0.00340 CL2 5 -0.110253 0.481348 0.667790 11.00000 0.02201 0.01536 = 0.02250 -0.00342 0.00008 -0.00192 CL3 5 -0.386828 0.373460 0.428685 11.00000 0.02145 0.02672 = 0.01467 0.00248 -0.00093 0.00379 N1 3 -0.071063 0.225851 0.573611 11.00000 0.01756 0.01232 = 0.01316 -0.00125 0.00043 -0.00068 C1 1 0.055512 0.235554 0.486126 11.00000 0.02153 0.01745 = 0.01414 0.00219 0.00221 -0.00027 AFIX 43 H1 2 0.033262 0.296122 0.434295 11.00000 -1.20000 AFIX 0 C2 1 0.213511 0.161351 0.470078 11.00000 0.01810 0.01783 = 0.01488 0.00075 0.00201 0.00045 AFIX 43 H2 2 0.297285 0.170304 0.407296 11.00000 -1.20000 AFIX 0 C3 1 0.252326 0.072462 0.545543 11.00000 0.01579 0.01473 = 0.01277 -0.00129 -0.00112 -0.00167 C4 1 0.118425 0.061568 0.634745 11.00000 0.02050 0.01437 = 0.01497 0.00228 -0.00113 -0.00263 AFIX 43 H4 2 0.136636 0.001122 0.687134 11.00000 -1.20000 AFIX 0 C5 1 -0.038092 0.138233 0.645870 11.00000 0.01868 0.01659 = 0.01447 0.00091 0.00028 -0.00295 AFIX 43 H5 2 -0.126880 0.129607 0.706584 11.00000 -1.20000 AFIX 0 C6 1 0.423611 -0.006185 0.536299 11.00000 0.01965 0.01461 = 0.01515 0.00036 -0.00206 -0.00082 AFIX 43 H6 2 0.428380 -0.070755 0.584692 11.00000 -1.20000 AFIX 0 HKLF 4 REM ayt57 in P2(1)/n at 90K newGV noerr REM R1 = 0.0239 for 1464 Fo > 4sig(Fo) and 0.0321 for all 1815 data REM 100 parameters refined using 0 restraints END WGHT 0.0386 0.0000 REM Highest difference peak 0.353, deepest hole -0.304, 1-sigma level 0.060 Q1 1 -0.1707 0.2787 0.5905 11.00000 0.05 0.35 Q2 1 -0.3939 0.3351 0.6876 11.00000 0.05 0.26 Q3 1 0.2152 0.0740 0.5852 11.00000 0.05 0.23 Q4 1 -0.1819 0.4146 0.6016 11.00000 0.05 0.22 Q5 1 -0.2417 0.3313 0.4681 11.00000 0.05 0.20 Q6 1 0.3299 0.0424 0.5344 11.00000 0.05 0.20 Q7 1 -0.4518 0.2649 0.5783 11.00000 0.05 0.20 Q8 1 -0.5803 0.3428 0.6835 11.00000 0.05 0.19 Q9 1 -0.3937 0.2762 0.5998 11.00000 0.05 0.19 Q10 1 -0.3716 0.2986 0.6232 11.00000 0.05 0.19 ; _shelx_res_checksum 25619 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 Al1 Al -0.27490(9) 0.34418(5) 0.59207(4) 0.01462(13) Uani 1 1 d . . . . . Cl1 Cl -0.49638(7) 0.27733(4) 0.70001(3) 0.01915(11) Uani 1 1 d . . . . . Cl2 Cl -0.11025(7) 0.48135(4) 0.66779(4) 0.01996(12) Uani 1 1 d . . . . . Cl3 Cl -0.38683(7) 0.37346(4) 0.42868(3) 0.02096(12) Uani 1 1 d . . . . . N1 N -0.0711(3) 0.22585(13) 0.57361(12) 0.0143(3) Uani 1 1 d . . . . . C1 C 0.0555(3) 0.23555(17) 0.48613(15) 0.0177(4) Uani 1 1 d . . . . . H1 H 0.0333 0.2961 0.4343 0.021 Uiso 1 1 calc R U . . . C2 C 0.2135(3) 0.16135(17) 0.47008(15) 0.0169(4) Uani 1 1 d . . . . . H2 H 0.2973 0.1703 0.4073 0.020 Uiso 1 1 calc R U . . . C3 C 0.2523(3) 0.07246(16) 0.54554(14) 0.0144(3) Uani 1 1 d . . . . . C4 C 0.1184(3) 0.06157(16) 0.63475(14) 0.0166(4) Uani 1 1 d . . . . . H4 H 0.1366 0.0011 0.6871 0.020 Uiso 1 1 calc R U . . . C5 C -0.0381(3) 0.13823(16) 0.64587(14) 0.0166(4) Uani 1 1 d . . . . . H5 H -0.1269 0.1296 0.7066 0.020 Uiso 1 1 calc R U . . . C6 C 0.4236(3) -0.00618(16) 0.53630(15) 0.0165(4) Uani 1 1 d . . . . . H6 H 0.4284 -0.0708 0.5847 0.020 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 Al1 0.0167(3) 0.0146(3) 0.0126(2) -0.00089(19) 0.00103(19) 0.0005(2) Cl1 0.0206(2) 0.0213(2) 0.0157(2) -0.00127(16) 0.00391(16) -0.00340(18) Cl2 0.0220(2) 0.0154(2) 0.0225(2) -0.00342(16) 0.00008(17) -0.00192(17) Cl3 0.0214(2) 0.0267(2) 0.01467(19) 0.00248(16) -0.00093(16) 0.00379(19) N1 0.0176(8) 0.0123(7) 0.0132(7) -0.0013(5) 0.0004(6) -0.0007(6) C1 0.0215(10) 0.0175(9) 0.0141(8) 0.0022(7) 0.0022(7) -0.0003(8) C2 0.0181(9) 0.0178(9) 0.0149(8) 0.0007(7) 0.0020(7) 0.0004(8) C3 0.0158(9) 0.0147(8) 0.0128(8) -0.0013(6) -0.0011(6) -0.0017(7) C4 0.0205(9) 0.0144(8) 0.0150(8) 0.0023(7) -0.0011(7) -0.0026(7) C5 0.0187(9) 0.0166(9) 0.0145(8) 0.0009(7) 0.0003(7) -0.0030(7) C6 0.0197(9) 0.0146(9) 0.0151(8) 0.0004(6) -0.0021(7) -0.0008(7) 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' Al Al 0.2130 0.2455 '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' 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 Al1 Cl2 111.25(3) . . ? Cl3 Al1 Cl1 113.52(3) . . ? Cl3 Al1 Cl2 116.39(3) . . ? N1 Al1 Cl1 107.23(5) . . ? N1 Al1 Cl2 103.52(5) . . ? N1 Al1 Cl3 103.68(5) . . ? C1 N1 Al1 117.76(13) . . ? C5 N1 Al1 124.22(12) . . ? C5 N1 C1 117.88(17) . . ? N1 C1 H1 118.8 . . ? N1 C1 C2 122.40(17) . . ? C2 C1 H1 118.8 . . ? C1 C2 H2 119.9 . . ? C1 C2 C3 120.28(16) . . ? C3 C2 H2 119.9 . . ? C2 C3 C4 117.02(18) . . ? C2 C3 C6 123.10(16) . . ? C4 C3 C6 119.88(17) . . ? C3 C4 H4 120.0 . . ? C5 C4 C3 119.91(17) . . ? C5 C4 H4 120.0 . . ? N1 C5 C4 122.48(17) . . ? N1 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? C3 C6 H6 117.7 . . ? C6 C6 C3 124.6(2) 3_656 . ? C6 C6 H6 117.7 3_656 . ? 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 Al1 Cl1 2.1187(7) . ? Al1 Cl2 2.1222(7) . ? Al1 Cl3 2.1151(7) . ? Al1 N1 1.9356(17) . ? N1 C1 1.360(2) . ? N1 C5 1.354(2) . ? C1 H1 0.9500 . ? C1 C2 1.367(3) . ? C2 H2 0.9500 . ? C2 C3 1.396(3) . ? C3 C4 1.408(2) . ? C3 C6 1.456(3) . ? C4 H4 0.9500 . ? C4 C5 1.369(3) . ? C5 H5 0.9500 . ? C6 C6 1.352(4) 3_656 ? C6 H6 0.9500 . ?