#------------------------------------------------------------------------------ #$Date: 2020-06-04 04:46:27 +0300 (Thu, 04 Jun 2020) $ #$Revision: 252629 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/06/7240616.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_7240616 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 Br6 Ga2 N2' _chemical_formula_sum 'C12 H10 Br6 Ga2 N2' _chemical_formula_weight 801.12 _chemical_name_common alpha-polymorph _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 90.552(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 6.51032(16) _cell_length_b 12.2531(3) _cell_length_c 12.4379(3) _cell_measurement_reflns_used 1609 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 73.4310 _cell_measurement_theta_min 5.0650 _cell_volume 992.15(4) _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 0.991 _diffrn_measured_fraction_theta_max 0.952 _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 0.0355 _diffrn_reflns_av_unetI/netI 0.0411 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.952 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 3408 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.952 _diffrn_reflns_theta_full 67.500 _diffrn_reflns_theta_max 73.844 _diffrn_reflns_theta_min 5.067 _diffrn_source_type 'microfocus SuperNova source' _exptl_absorpt_coefficient_mu 17.459 _exptl_absorpt_correction_T_max 0.645 _exptl_absorpt_correction_T_min 0.474 _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 2.682 _exptl_crystal_description polyhedron _exptl_crystal_F_000 736 _exptl_crystal_recrystallization_method Sublimation _exptl_crystal_size_max 0.062 _exptl_crystal_size_mid 0.056 _exptl_crystal_size_min 0.035 _refine_diff_density_max 1.037 _refine_diff_density_min -0.610 _refine_diff_density_rms 0.182 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 100 _refine_ls_number_reflns 1914 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.999 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0332 _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^)+(0.0571P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0885 _refine_ls_wR_factor_ref 0.0927 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1554 _reflns_number_total 1914 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ce00541j2.cif _cod_data_source_block ayt65 _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7240616 _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 0.411 _shelx_estimated_absorpt_t_max 0.580 _shelx_res_file ; 65.res created by SHELXL-2014/7 TITL ayt65 in P2(1)/n at 123K newGV no err CELL 1.54178 6.51032 12.25313 12.43790 90.0000 90.5518 90.0000 ZERR 2.00 0.00016 0.00033 0.00029 0.0000 0.0022 0.0000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N GA BR UNIT 24 20 4 4 12 L.S. 10 PLAN 10 TEMP -150 BOND $H FMAP 2 ACTA 135 SIZE 0.062 0.056 0.035 WGHT 0.057100 FVAR 0.10942 BR1 5 1.395235 0.367747 0.424170 11.00000 0.02620 0.02899 = 0.02451 0.00409 0.00136 -0.00236 BR2 5 1.090571 0.477211 0.671551 11.00000 0.02774 0.01932 = 0.03491 -0.00462 0.00098 0.00250 BR3 5 1.525546 0.271794 0.711220 11.00000 0.02550 0.02474 = 0.02440 -0.00042 -0.00374 0.00418 GA1 4 1.277020 0.337806 0.595496 11.00000 0.02033 0.01678 = 0.02242 -0.00104 -0.00111 -0.00002 N1 3 1.067101 0.220609 0.574803 11.00000 0.02131 0.01545 = 0.02236 -0.00074 -0.00105 0.00008 C1 1 0.935099 0.230626 0.491605 11.00000 0.02556 0.01628 = 0.02386 0.00197 0.00049 -0.00206 AFIX 43 H1 2 0.949301 0.290982 0.444314 11.00000 -1.20000 AFIX 0 C2 1 0.780419 0.156675 0.472563 11.00000 0.02388 0.01833 = 0.02299 0.00296 -0.00309 0.00128 AFIX 43 H2 2 0.693254 0.164444 0.411347 11.00000 -1.20000 AFIX 0 C3 1 0.752061 0.069709 0.544030 11.00000 0.02411 0.01517 = 0.02450 0.00028 0.00147 -0.00331 C4 1 0.890958 0.059109 0.629055 11.00000 0.02570 0.01836 = 0.02427 0.00874 0.00270 -0.00147 AFIX 43 H4 2 0.878567 -0.000129 0.677840 11.00000 -1.20000 AFIX 0 C5 1 1.047396 0.134700 0.642837 11.00000 0.02570 0.01495 = 0.01793 0.00307 -0.00241 0.00102 AFIX 43 H5 2 1.142245 0.126262 0.700763 11.00000 -1.20000 AFIX 0 C6 1 0.580614 -0.006995 0.532447 11.00000 0.02473 0.01804 = 0.03093 -0.00083 0.00211 -0.00418 AFIX 43 H6 2 0.585038 -0.071666 0.574535 11.00000 -1.20000 AFIX 0 HKLF 4 REM ayt65 in P2(1)/n at 123K newGV no err REM R1 = 0.0332 for 1554 Fo > 4sig(Fo) and 0.0441 for all 1914 data REM 100 parameters refined using 0 restraints END WGHT 0.0573 0.0000 REM Highest difference peak 1.037, deepest hole -0.610, 1-sigma level 0.182 Q1 1 1.0436 0.4797 0.5932 11.00000 0.05 1.04 Q2 1 1.5206 0.3744 0.4354 11.00000 0.05 0.84 Q3 1 1.2438 0.3630 0.4042 11.00000 0.05 0.77 Q4 1 1.6151 0.2727 0.7815 11.00000 0.05 0.74 Q5 1 1.2149 0.4791 0.7193 11.00000 0.05 0.69 Q6 1 1.5643 0.4998 0.3452 11.00000 0.05 0.67 Q7 1 1.0922 0.4747 0.7645 11.00000 0.05 0.67 Q8 1 1.1204 0.4785 0.4758 11.00000 0.05 0.66 Q9 1 1.1444 0.3362 0.5561 11.00000 0.05 0.65 Q10 1 1.6475 0.4846 0.4589 11.00000 0.05 0.63 ; _shelx_res_checksum 12384 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 Br1 Br 1.39523(9) 0.36775(5) 0.42417(5) 0.02656(17) Uani 1 1 d . . . . . Br2 Br 1.09057(9) 0.47721(5) 0.67155(5) 0.02732(18) Uani 1 1 d . . . . . Br3 Br 1.52555(9) 0.27179(5) 0.71122(5) 0.02491(17) Uani 1 1 d . . . . . Ga1 Ga 1.27702(10) 0.33781(6) 0.59550(5) 0.01985(18) Uani 1 1 d . . . . . N1 N 1.0671(7) 0.2206(4) 0.5748(4) 0.0197(9) Uani 1 1 d . . . . . C1 C 0.9351(9) 0.2306(5) 0.4916(5) 0.0219(11) Uani 1 1 d . . . . . H1 H 0.9493 0.2910 0.4443 0.026 Uiso 1 1 calc R U . . . C2 C 0.7804(9) 0.1567(5) 0.4726(4) 0.0218(11) Uani 1 1 d . . . . . H2 H 0.6933 0.1644 0.4113 0.026 Uiso 1 1 calc R U . . . C3 C 0.7521(9) 0.0697(5) 0.5440(4) 0.0213(11) Uani 1 1 d . . . . . C4 C 0.8910(9) 0.0591(5) 0.6291(4) 0.0228(12) Uani 1 1 d . . . . . H4 H 0.8786 -0.0001 0.6778 0.027 Uiso 1 1 calc R U . . . C5 C 1.0474(9) 0.1347(4) 0.6428(4) 0.0195(11) Uani 1 1 d . . . . . H5 H 1.1422 0.1263 0.7008 0.023 Uiso 1 1 calc R U . . . C6 C 0.5806(9) -0.0070(5) 0.5324(5) 0.0246(12) Uani 1 1 d . . . . . H6 H 0.5850 -0.0717 0.5745 0.029 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 Br1 0.0262(3) 0.0290(4) 0.0245(3) 0.0041(2) 0.0014(2) -0.0024(2) Br2 0.0277(3) 0.0193(3) 0.0349(3) -0.0046(2) 0.0010(2) 0.0025(2) Br3 0.0255(3) 0.0247(3) 0.0244(3) -0.0004(2) -0.0037(2) 0.0042(2) Ga1 0.0203(3) 0.0168(4) 0.0224(3) -0.0010(3) -0.0011(3) 0.0000(3) N1 0.021(2) 0.015(2) 0.022(2) -0.0007(18) -0.0010(17) 0.0001(18) C1 0.026(3) 0.016(3) 0.024(3) 0.002(2) 0.000(2) -0.002(2) C2 0.024(3) 0.018(3) 0.023(3) 0.003(2) -0.003(2) 0.001(2) C3 0.024(3) 0.015(3) 0.024(3) 0.000(2) 0.001(2) -0.003(2) C4 0.026(3) 0.018(3) 0.024(3) 0.009(2) 0.003(2) -0.001(2) C5 0.026(3) 0.015(3) 0.018(2) 0.003(2) -0.002(2) 0.001(2) C6 0.025(3) 0.018(3) 0.031(3) -0.001(2) 0.002(2) -0.004(2) 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' Ga Ga -1.2846 0.7763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 '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 Br1 Ga1 Br2 116.36(4) . . ? Br3 Ga1 Br1 113.30(4) . . ? Br3 Ga1 Br2 111.94(3) . . ? N1 Ga1 Br1 103.28(14) . . ? N1 Ga1 Br2 102.91(14) . . ? N1 Ga1 Br3 107.69(14) . . ? C1 N1 Ga1 117.7(4) . . ? C1 N1 C5 119.1(5) . . ? C5 N1 Ga1 123.1(4) . . ? N1 C1 H1 118.8 . . ? N1 C1 C2 122.3(5) . . ? C2 C1 H1 118.8 . . ? C1 C2 H2 120.2 . . ? C1 C2 C3 119.6(5) . . ? C3 C2 H2 120.2 . . ? C2 C3 C6 122.0(5) . . ? C4 C3 C2 117.7(5) . . ? C4 C3 C6 120.3(5) . . ? C3 C4 H4 119.9 . . ? C5 C4 C3 120.2(5) . . ? C5 C4 H4 119.9 . . ? N1 C5 C4 121.0(5) . . ? N1 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C3 C6 H6 117.5 . . ? C6 C6 C3 125.0(7) 3_656 . ? C6 C6 H6 117.5 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 Br1 Ga1 2.3020(9) . ? Br2 Ga1 2.3039(9) . ? Br3 Ga1 2.3020(9) . ? Ga1 N1 1.997(5) . ? N1 C1 1.344(7) . ? N1 C5 1.357(7) . ? C1 H1 0.9500 . ? C1 C2 1.374(8) . ? C2 H2 0.9500 . ? C2 C3 1.401(8) . ? C3 C4 1.391(8) . ? C3 C6 1.465(8) . ? C4 H4 0.9500 . ? C4 C5 1.386(8) . ? C5 H5 0.9500 . ? C6 C6 1.329(12) 3_656 ? C6 H6 0.9500 . ?