#------------------------------------------------------------------------------ #$Date: 2020-06-04 04:46:27 +0300 (Thu, 04 Jun 2020) $ #$Revision: 252629 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/06/7240611.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_7240611 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 Cl6 Ga2 N2' _chemical_formula_sum 'C12 H10 Cl6 Ga2 N2' _chemical_formula_weight 534.36 _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 90.8579(17) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 6.51299(12) _cell_length_b 11.7499(3) _cell_length_c 12.0716(2) _cell_measurement_reflns_used 2969 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 73.8640 _cell_measurement_theta_min 5.2360 _cell_volume 923.70(3) _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 (Sheldrick, 2014)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 123(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 4.2047 _diffrn_detector_type TitanS2 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'Rigaku Oxford Diffraction SuperNova' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_unetI/netI 0.0205 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_number 4197 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 67.500 _diffrn_reflns_theta_max 73.997 _diffrn_reflns_theta_min 5.253 _diffrn_source_type 'microfocus SuperNova source' _exptl_absorpt_coefficient_mu 11.530 _exptl_absorpt_correction_T_max 0.589 _exptl_absorpt_correction_T_min 0.430 _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 1.921 _exptl_crystal_description polyhedron _exptl_crystal_F_000 520 _exptl_crystal_recrystallization_method Sublimation _exptl_crystal_size_max 0.122 _exptl_crystal_size_mid 0.108 _exptl_crystal_size_min 0.065 _refine_diff_density_max 0.444 _refine_diff_density_min -0.501 _refine_diff_density_rms 0.070 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 100 _refine_ls_number_reflns 1851 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.985 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_gt 0.0217 _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^)+(0.0396P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0557 _refine_ls_wR_factor_ref 0.0567 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1641 _reflns_number_total 1851 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ce00541j2.cif _cod_data_source_block ayt68 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7240611 _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 0.334 _shelx_estimated_absorpt_t_max 0.521 _shelx_res_file ; 68.res created by SHELXL-2014/7 TITL ayt68 in P2(1)/n at 123K newGV no err model CELL 1.54178 6.51299 11.74994 12.07163 90.0000 90.8579 90.0000 ZERR 2.00 0.00012 0.00025 0.00021 0.0000 0.0017 0.0000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N CL GA UNIT 24 20 4 12 4 L.S. 10 PLAN 10 TEMP -150 BOND $H FMAP 2 ACTA 135 SIZE 0.122 0.108 0.065 WGHT 0.039600 FVAR 0.18038 GA1 5 0.220533 0.152758 0.592787 11.00000 0.02083 0.02009 = 0.01628 0.00078 0.00024 -0.00067 CL1 4 0.391405 0.016059 0.670289 11.00000 0.02767 0.02168 = 0.02948 0.00440 -0.00157 0.00206 CL2 4 0.110199 0.123689 0.426267 11.00000 0.02729 0.03660 = 0.01896 -0.00339 -0.00256 -0.00450 CL3 4 -0.008195 0.219889 0.702255 11.00000 0.02678 0.03010 = 0.02064 0.00148 0.00418 0.00516 N1 3 0.430008 0.272953 0.573443 11.00000 0.02231 0.01865 = 0.01732 0.00073 -0.00045 0.00073 C1 1 0.459086 0.359281 0.645604 11.00000 0.02579 0.02282 = 0.01733 -0.00136 0.00003 0.00368 AFIX 43 H1 2 0.368479 0.367037 0.706084 11.00000 -1.20000 AFIX 0 C2 1 0.616630 0.436640 0.634103 11.00000 0.02553 0.02001 = 0.02018 -0.00289 -0.00166 0.00134 AFIX 43 H2 2 0.633686 0.496524 0.686309 11.00000 -1.20000 AFIX 0 C3 1 0.751165 0.426730 0.545447 11.00000 0.02164 0.01819 = 0.01863 0.00161 -0.00332 0.00220 C4 1 0.715038 0.338365 0.469965 11.00000 0.02463 0.02424 = 0.01775 -0.00285 0.00179 -0.00022 AFIX 43 H4 2 0.800278 0.330233 0.407282 11.00000 -1.20000 AFIX 0 C5 1 0.557417 0.263720 0.486192 11.00000 0.02682 0.02388 = 0.01847 -0.00388 0.00127 -0.00126 AFIX 43 H5 2 0.536535 0.203511 0.434721 11.00000 -1.20000 AFIX 0 C6 1 0.922562 0.505808 0.535927 11.00000 0.02501 0.01966 = 0.01902 -0.00123 -0.00387 -0.00081 AFIX 43 H6 2 0.925183 0.570018 0.583751 11.00000 -1.20000 AFIX 0 HKLF 4 REM ayt68 in P2(1)/n at 123K newGV no err model REM R1 = 0.0217 for 1641 Fo > 4sig(Fo) and 0.0251 for all 1851 data REM 100 parameters refined using 0 restraints END WGHT 0.0396 0.0000 REM Highest difference peak 0.444, deepest hole -0.501, 1-sigma level 0.070 Q1 1 0.2908 0.0773 0.6525 11.00000 0.05 0.44 Q2 1 0.3292 0.0903 0.6015 11.00000 0.05 0.44 Q3 1 0.3356 0.2173 0.5859 11.00000 0.05 0.44 Q4 1 0.1002 0.2085 0.6073 11.00000 0.05 0.36 Q5 1 0.1070 0.0964 0.5993 11.00000 0.05 0.29 Q6 1 0.8314 0.4594 0.5327 11.00000 0.05 0.27 Q7 1 0.4795 -0.0388 0.6605 11.00000 0.05 0.27 Q8 1 0.0807 0.2781 0.7043 11.00000 0.05 0.25 Q9 1 0.5514 0.4049 0.6397 11.00000 0.05 0.25 Q10 1 0.6637 0.4413 0.5674 11.00000 0.05 0.24 ; _shelx_res_checksum 51418 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 0.22053(3) 0.15276(2) 0.59279(2) 0.01907(9) Uani 1 1 d . . . . . Cl1 Cl 0.39141(7) 0.01606(4) 0.67029(4) 0.02630(12) Uani 1 1 d . . . . . Cl2 Cl 0.11020(8) 0.12369(5) 0.42627(4) 0.02765(12) Uani 1 1 d . . . . . Cl3 Cl -0.00819(7) 0.21989(4) 0.70225(4) 0.02580(12) Uani 1 1 d . . . . . N1 N 0.4300(2) 0.27295(14) 0.57344(13) 0.0194(3) Uani 1 1 d . . . . . C1 C 0.4591(3) 0.35928(17) 0.64560(15) 0.0220(4) Uani 1 1 d . . . . . H1 H 0.3685 0.3670 0.7061 0.026 Uiso 1 1 calc R U . . . C2 C 0.6166(3) 0.43664(17) 0.63410(15) 0.0219(4) Uani 1 1 d . . . . . H2 H 0.6337 0.4965 0.6863 0.026 Uiso 1 1 calc R U . . . C3 C 0.7512(3) 0.42673(16) 0.54545(15) 0.0195(4) Uani 1 1 d . . . . . C4 C 0.7150(3) 0.33837(17) 0.46997(16) 0.0222(4) Uani 1 1 d . . . . . H4 H 0.8003 0.3302 0.4073 0.027 Uiso 1 1 calc R U . . . C5 C 0.5574(3) 0.26372(18) 0.48619(16) 0.0231(4) Uani 1 1 d . . . . . H5 H 0.5365 0.2035 0.4347 0.028 Uiso 1 1 calc R U . . . C6 C 0.9226(3) 0.50581(17) 0.53593(16) 0.0213(4) Uani 1 1 d . . . . . H6 H 0.9252 0.5700 0.5838 0.026 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 0.02083(13) 0.02009(14) 0.01628(13) 0.00078(8) 0.00024(9) -0.00067(9) Cl1 0.0277(2) 0.0217(2) 0.0295(2) 0.00440(18) -0.00157(18) 0.00206(18) Cl2 0.0273(2) 0.0366(3) 0.0190(2) -0.00339(18) -0.00256(17) -0.0045(2) Cl3 0.0268(2) 0.0301(3) 0.0206(2) 0.00148(17) 0.00418(17) 0.00516(19) N1 0.0223(7) 0.0187(8) 0.0173(7) 0.0007(6) -0.0005(6) 0.0007(6) C1 0.0258(9) 0.0228(10) 0.0173(8) -0.0014(7) 0.0000(7) 0.0037(8) C2 0.0255(9) 0.0200(9) 0.0202(8) -0.0029(7) -0.0017(7) 0.0013(8) C3 0.0216(8) 0.0182(9) 0.0186(8) 0.0016(7) -0.0033(7) 0.0022(8) C4 0.0246(9) 0.0242(10) 0.0178(9) -0.0028(7) 0.0018(7) -0.0002(8) C5 0.0268(10) 0.0239(10) 0.0185(9) -0.0039(7) 0.0013(7) -0.0013(8) C6 0.0250(9) 0.0197(9) 0.0190(8) -0.0012(7) -0.0039(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' 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 Cl2 Ga1 Cl1 116.71(2) . . ? Cl2 Ga1 Cl3 113.99(2) . . ? Cl3 Ga1 Cl1 111.29(2) . . ? N1 Ga1 Cl1 103.30(5) . . ? N1 Ga1 Cl2 102.95(5) . . ? N1 Ga1 Cl3 107.16(5) . . ? C1 N1 Ga1 123.41(13) . . ? C1 N1 C5 118.73(17) . . ? C5 N1 Ga1 117.75(13) . . ? N1 C1 H1 119.1 . . ? N1 C1 C2 121.88(18) . . ? C2 C1 H1 119.1 . . ? C1 C2 H2 120.1 . . ? C1 C2 C3 119.86(18) . . ? C3 C2 H2 120.1 . . ? C2 C3 C4 117.33(18) . . ? C2 C3 C6 119.77(17) . . ? C4 C3 C6 122.89(18) . . ? C3 C4 H4 119.9 . . ? C5 C4 C3 120.16(17) . . ? C5 C4 H4 119.9 . . ? N1 C5 C4 122.02(18) . . ? N1 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C3 C6 H6 117.7 . . ? C6 C6 C3 124.6(2) 3_766 . ? C6 C6 H6 117.7 3_766 . ? 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 Cl1 2.1593(5) . ? Ga1 Cl2 2.1519(5) . ? Ga1 Cl3 2.1556(5) . ? Ga1 N1 1.9799(17) . ? N1 C1 1.349(3) . ? N1 C5 1.355(2) . ? C1 H1 0.9500 . ? C1 C2 1.379(3) . ? C2 H2 0.9500 . ? C2 C3 1.398(3) . ? C3 C4 1.399(3) . ? C3 C6 1.458(3) . ? C4 H4 0.9500 . ? C4 C5 1.367(3) . ? C5 H5 0.9500 . ? C6 C6 1.347(4) 3_766 ? C6 H6 0.9500 . ?