#------------------------------------------------------------------------------ #$Date: 2020-06-04 04:46:27 +0300 (Thu, 04 Jun 2020) $ #$Revision: 252629 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/06/7240615.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_7240615 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 'beta polymorph' _chemical_properties_physical Air-sensitive,Moisture-sensitive _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 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 96.7181(19) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 6.56821(14) _cell_length_b 8.50459(16) _cell_length_c 18.1626(4) _cell_measurement_reflns_used 2621 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 73.6960 _cell_measurement_theta_min 5.7340 _cell_volume 1007.60(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 _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 0.999 _diffrn_measured_fraction_theta_max 0.976 _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 0.0244 _diffrn_reflns_av_unetI/netI 0.0271 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.976 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 3980 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.976 _diffrn_reflns_theta_full 67.500 _diffrn_reflns_theta_max 74.116 _diffrn_reflns_theta_min 4.903 _diffrn_source_type 'microfocus SuperNova source' _exptl_absorpt_coefficient_mu 17.192 _exptl_absorpt_correction_T_max 0.607 _exptl_absorpt_correction_T_min 0.389 _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 2.641 _exptl_crystal_description 'elongated prism' _exptl_crystal_F_000 736 _exptl_crystal_recrystallization_method Sublimation _exptl_crystal_size_max 0.114 _exptl_crystal_size_mid 0.062 _exptl_crystal_size_min 0.047 _refine_diff_density_max 0.534 _refine_diff_density_min -0.692 _refine_diff_density_rms 0.121 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 100 _refine_ls_number_reflns 2005 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.987 _refine_ls_R_factor_all 0.0298 _refine_ls_R_factor_gt 0.0243 _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^)+(0.0397P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.0627 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1701 _reflns_number_total 2005 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ce00541j2.cif _cod_data_source_block ayt64 _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 7240615 _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 0.245 _shelx_estimated_absorpt_t_max 0.499 _shelx_res_file ; 64.res created by SHELXL-2014/7 TITL ayt64 in P2(1)/c at 123K newGV no err CELL 1.54178 6.56821 8.50459 18.16260 90.0000 96.7181 90.0000 ZERR 2.00 0.00014 0.00016 0.00037 0.0000 0.0019 0.0000 LATT 1 SYMM -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 0.114 0.062 0.047 WGHT 0.039700 FVAR 0.12073 BR1 5 0.044718 0.543454 0.767105 11.00000 0.04959 0.02197 = 0.03551 0.00485 0.02672 0.00768 BR2 5 -0.024020 0.717611 0.571618 11.00000 0.02215 0.02880 = 0.02737 0.00160 0.00077 0.00331 BR3 5 0.468415 0.810821 0.696727 11.00000 0.02733 0.02302 = 0.03228 -0.00618 0.00082 -0.00341 GA1 4 0.207391 0.634549 0.670543 11.00000 0.02171 0.01531 = 0.02014 -0.00017 0.00598 0.00183 N1 3 0.334602 0.446276 0.629414 11.00000 0.02319 0.01625 = 0.02063 0.00184 0.00567 -0.00062 C1 1 0.515265 0.453447 0.601478 11.00000 0.02215 0.01990 = 0.03084 -0.00176 0.00860 -0.00357 AFIX 43 H1 2 0.591388 0.548621 0.606227 11.00000 -1.20000 AFIX 0 C2 1 0.593366 0.328236 0.566399 11.00000 0.02302 0.02560 = 0.02966 -0.00334 0.01362 -0.00226 AFIX 43 H2 2 0.721996 0.337200 0.547674 11.00000 -1.20000 AFIX 0 C3 1 0.483400 0.187335 0.558227 11.00000 0.02432 0.01877 = 0.02118 -0.00021 0.00182 0.00248 C4 1 0.299988 0.178387 0.590902 11.00000 0.02867 0.01668 = 0.02284 0.00055 0.00680 -0.00034 AFIX 43 H4 2 0.224093 0.083100 0.589148 11.00000 -1.20000 AFIX 0 C5 1 0.231622 0.308248 0.625296 11.00000 0.02688 0.01621 = 0.02028 0.00190 0.00647 -0.00007 AFIX 43 H5 2 0.107278 0.301072 0.647057 11.00000 -1.20000 AFIX 0 C6 1 0.557567 0.059241 0.514852 11.00000 0.02656 0.02182 = 0.02545 -0.00168 0.00868 0.00291 AFIX 43 H6 2 0.698196 0.060329 0.507213 11.00000 -1.20000 AFIX 0 HKLF 4 REM ayt64 in P2(1)/c at 123K newGV no err REM R1 = 0.0243 for 1701 Fo > 4sig(Fo) and 0.0298 for all 2005 data REM 100 parameters refined using 0 restraints END WGHT 0.0397 0.0000 REM Highest difference peak 0.534, deepest hole -0.692, 1-sigma level 0.121 Q1 1 0.3575 0.6571 0.6912 11.00000 0.05 0.53 Q2 1 0.3114 0.7869 0.6781 11.00000 0.05 0.48 Q3 1 0.1938 0.7051 0.5583 11.00000 0.05 0.45 Q4 1 0.5035 0.5556 0.6720 11.00000 0.05 0.43 Q5 1 -0.1379 0.5775 0.5627 11.00000 0.05 0.41 Q6 1 -0.0051 0.6780 0.7989 11.00000 0.05 0.38 Q7 1 0.0645 0.5607 0.5553 11.00000 0.05 0.37 Q8 1 0.1419 0.8738 0.6769 11.00000 0.05 0.36 Q9 1 0.6653 0.9649 0.7428 11.00000 0.05 0.36 Q10 1 0.6121 0.8183 0.7157 11.00000 0.05 0.36 ; _shelx_res_checksum 65420 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 0.04472(7) 0.54345(4) 0.76710(2) 0.03397(13) Uani 1 1 d . . . . . Br2 Br -0.02402(6) 0.71761(5) 0.57162(2) 0.02627(11) Uani 1 1 d . . . . . Br3 Br 0.46841(6) 0.81082(4) 0.69673(2) 0.02776(11) Uani 1 1 d . . . . . Ga1 Ga 0.20739(6) 0.63455(5) 0.67054(2) 0.01877(11) Uani 1 1 d . . . . . N1 N 0.3346(5) 0.4463(3) 0.62941(16) 0.0198(6) Uani 1 1 d . . . . . C1 C 0.5153(6) 0.4534(4) 0.6015(2) 0.0239(7) Uani 1 1 d . . . . . H1 H 0.5914 0.5486 0.6062 0.029 Uiso 1 1 calc R U . . . C2 C 0.5934(6) 0.3282(4) 0.5664(2) 0.0253(7) Uani 1 1 d . . . . . H2 H 0.7220 0.3372 0.5477 0.030 Uiso 1 1 calc R U . . . C3 C 0.4834(6) 0.1873(4) 0.55823(19) 0.0215(7) Uani 1 1 d . . . . . C4 C 0.3000(6) 0.1784(4) 0.59090(19) 0.0224(7) Uani 1 1 d . . . . . H4 H 0.2241 0.0831 0.5891 0.027 Uiso 1 1 calc R U . . . C5 C 0.2316(6) 0.3082(4) 0.62530(19) 0.0208(7) Uani 1 1 d . . . . . H5 H 0.1073 0.3011 0.6471 0.025 Uiso 1 1 calc R U . . . C6 C 0.5576(6) 0.0592(4) 0.5149(2) 0.0242(7) Uani 1 1 d . . . . . H6 H 0.6982 0.0603 0.5072 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 0.0496(3) 0.02197(19) 0.0355(2) 0.00485(14) 0.02672(19) 0.00768(17) Br2 0.02215(18) 0.0288(2) 0.0274(2) 0.00160(14) 0.00077(14) 0.00331(14) Br3 0.0273(2) 0.0230(2) 0.0323(2) -0.00618(14) 0.00082(15) -0.00341(14) Ga1 0.0217(2) 0.0153(2) 0.0201(2) -0.00017(14) 0.00598(15) 0.00183(15) N1 0.0232(14) 0.0163(13) 0.0206(13) 0.0018(10) 0.0057(11) -0.0006(11) C1 0.0221(17) 0.0199(16) 0.0308(19) -0.0018(13) 0.0086(14) -0.0036(13) C2 0.0230(17) 0.0256(18) 0.0297(18) -0.0033(14) 0.0136(14) -0.0023(14) C3 0.0243(17) 0.0188(16) 0.0212(16) -0.0002(12) 0.0018(13) 0.0025(13) C4 0.0287(18) 0.0167(16) 0.0228(17) 0.0006(12) 0.0068(13) -0.0003(14) C5 0.0269(17) 0.0162(15) 0.0203(16) 0.0019(12) 0.0065(13) -0.0001(13) C6 0.0266(17) 0.0218(16) 0.0254(18) -0.0017(13) 0.0087(14) 0.0029(14) 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 111.90(2) . . ? Br3 Ga1 Br1 117.90(2) . . ? Br3 Ga1 Br2 111.62(2) . . ? N1 Ga1 Br1 105.59(8) . . ? N1 Ga1 Br2 102.69(9) . . ? N1 Ga1 Br3 105.55(9) . . ? C1 N1 Ga1 122.2(2) . . ? C1 N1 C5 118.4(3) . . ? C5 N1 Ga1 119.3(2) . . ? N1 C1 H1 118.8 . . ? N1 C1 C2 122.3(3) . . ? C2 C1 H1 118.8 . . ? C1 C2 H2 120.1 . . ? C1 C2 C3 119.9(3) . . ? C3 C2 H2 120.1 . . ? C2 C3 C4 117.3(3) . . ? C2 C3 C6 119.7(3) . . ? C4 C3 C6 122.9(3) . . ? C3 C4 H4 120.3 . . ? C5 C4 C3 119.4(3) . . ? C5 C4 H4 120.3 . . ? N1 C5 C4 122.4(3) . . ? N1 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? C3 C6 H6 117.6 . . ? C6 C6 C3 124.9(4) 3_656 . ? C6 C6 H6 117.6 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 2.2926(5) . ? Br2 Ga1 2.3235(5) . ? Br3 Ga1 2.2852(6) . ? Ga1 N1 1.991(3) . ? N1 C1 1.345(5) . ? N1 C5 1.352(5) . ? C1 H1 0.9500 . ? C1 C2 1.371(5) . ? C2 H2 0.9500 . ? C2 C3 1.398(5) . ? C3 C4 1.406(5) . ? C3 C6 1.461(5) . ? C4 H4 0.9500 . ? C4 C5 1.370(5) . ? C5 H5 0.9500 . ? C6 C6 1.335(8) 3_656 ? C6 H6 0.9500 . ?