#------------------------------------------------------------------------------ #$Date: 2021-11-06 22:32:09 +0200 (Sat, 06 Nov 2021) $ #$Revision: 270486 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/09/7060958.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_7060958 loop_ _publ_author_name 'Kotov, Vitalii Yu.' 'Buikin, Pert A.' 'Ilyukhin, Andrey B.' 'Korlyukov, Alexander A.' 'Dorovatovskii, Pavel V.' _publ_section_title ; Synthesis and first-principles study of structural, electronic and optical properties of tetragonal hybrid halobismuthathes [Py2(XK)]2[Bi2Br10−xIx] ; _journal_issue 39 _journal_name_full 'New Journal of Chemistry' _journal_page_first 18349 _journal_page_last 18357 _journal_paper_doi 10.1039/D1NJ02390J _journal_volume 45 _journal_year 2021 _chemical_formula_moiety 'C18 H18 N2, 2(I3)' _chemical_formula_sum 'C18 H18 I6 N2' _chemical_formula_weight 1023.74 _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4.3 _audit_creation_date 2018-11-14T00:04:14-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_update_record ; 2021-02-22 deposited with the CCDC. 2021-08-31 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 94.1760(10) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.3297(2) _cell_length_b 8.3343(2) _cell_length_c 16.1878(3) _cell_measurement_reflns_used 9953 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 33.18 _cell_measurement_theta_min 2.19 _cell_volume 1255.37(5) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX3' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/1 (Sheldrick, 2018)' _computing_structure_solution 'SHELXS-2018 (Sheldrick, 2015)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.98 _diffrn_measured_fraction_theta_max 0.9 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_unetI/netI 0.0208 _diffrn_reflns_Laue_measured_fraction_full 0.98 _diffrn_reflns_Laue_measured_fraction_max 0.9 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 17611 _diffrn_reflns_point_group_measured_fraction_full 0.98 _diffrn_reflns_point_group_measured_fraction_max 0.9 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 33.201 _diffrn_reflns_theta_min 3.282 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 7.43 _exptl_absorpt_correction_T_max 0.2693 _exptl_absorpt_correction_T_min 0.1769 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 2.708 _exptl_crystal_description plate _exptl_crystal_F_000 916 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.724 _refine_diff_density_min -0.839 _refine_diff_density_rms 0.115 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.152 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 118 _refine_ls_number_reflns 4328 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.152 _refine_ls_R_factor_all 0.0235 _refine_ls_R_factor_gt 0.021 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+1.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.0506 _reflns_Friedel_coverage 0 _reflns_number_gt 4084 _reflns_number_total 4328 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1nj02390j2.cif _cod_data_source_block 4 _cod_depositor_comments 'Adding full bibliography for 7060957--7060960.cif.' _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7060958 _shelx_res_file ; TITL 1 in P2(1)/n shelx.res created by SHELXL-2018/1 at 00:03:48 on 14-Nov-2018 CELL 0.71073 9.3297 8.3343 16.1878 90.000 94.176 90.000 ZERR 2 0.0002 0.0002 0.0003 0.000 0.001 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N I UNIT 36 36 4 12 TEMP -123 OMIT 1 1 4 omit 0 1 1 OMIT -8 6 15 shel 8 .1 acta htab HTAB C1 I1 EQIV $2 -x+1/2, y-1/2, -z+1/2 HTAB C2 I3_$2 EQIV $3 -x, -y+1, -z HTAB C5 I2_$3 conf L.S. 4 BOND REM EXTI 0.010344 WGHT 0.020000 1.000000 FVAR 0.32963 I1 4 0.218632 0.488015 0.203883 11.00000 0.01870 0.02955 = 0.02818 0.00094 0.00490 -0.00254 I2 4 0.458182 0.637805 0.122125 11.00000 0.01747 0.02053 = 0.02592 0.00123 0.00010 -0.00044 I3 4 0.698628 0.751221 0.036656 11.00000 0.02378 0.03051 = 0.03141 -0.00200 0.00672 -0.00884 C1 1 -0.194379 0.374024 0.180148 11.00000 0.02187 0.02720 = 0.02437 -0.00187 -0.00105 -0.00149 AFIX 43 H1A 2 -0.110984 0.439069 0.188619 11.00000 -1.20000 AFIX 0 C2 1 -0.287607 0.361297 0.241914 11.00000 0.02950 0.03245 = 0.02410 -0.00174 0.00207 0.00138 AFIX 43 H2A 2 -0.268917 0.417266 0.292682 11.00000 -1.20000 AFIX 0 C3 1 -0.409018 0.266057 0.229351 11.00000 0.02763 0.02959 = 0.02372 0.00566 0.00709 0.00391 AFIX 43 H3A 2 -0.473803 0.254971 0.271629 11.00000 -1.20000 AFIX 0 C4 1 -0.434729 0.187313 0.154480 11.00000 0.02100 0.02482 = 0.03091 0.00462 0.00347 -0.00165 AFIX 43 H4A 2 -0.518206 0.122852 0.144636 11.00000 -1.20000 AFIX 0 C5 1 -0.338601 0.202923 0.094307 11.00000 0.02203 0.02064 = 0.02289 -0.00027 0.00169 -0.00291 AFIX 43 H5A 2 -0.355614 0.148489 0.042966 11.00000 -1.20000 AFIX 0 C6 1 -0.117061 0.309661 0.041934 11.00000 0.01932 0.02107 = 0.02388 0.00147 0.00670 -0.00184 AFIX 23 H6A 2 -0.037008 0.381590 0.061150 11.00000 -1.20000 H6B 2 -0.166829 0.358026 -0.008132 11.00000 -1.20000 AFIX 0 C7 1 -0.057591 0.148449 0.020243 11.00000 0.01506 0.02177 = 0.02049 0.00170 0.00377 -0.00087 C8 1 0.030517 0.064367 0.078764 11.00000 0.01791 0.02556 = 0.01815 0.00015 0.00094 0.00032 AFIX 43 H8A 2 0.051611 0.108260 0.132435 11.00000 -1.20000 AFIX 0 C9 1 0.087497 -0.083829 0.058490 11.00000 0.01755 0.02602 = 0.01997 0.00295 0.00046 0.00114 AFIX 43 H9A 2 0.146970 -0.141023 0.098514 11.00000 -1.20000 AFIX 0 N1 3 -0.219764 0.295646 0.108008 11.00000 0.01720 0.01738 = 0.02069 0.00154 0.00315 0.00115 HKLF 4 REM 1 in P2(1)/n REM R1 = 0.0210 for 4084 Fo > 4sig(Fo) and 0.0235 for all 4328 data REM 118 parameters refined using 0 restraints END WGHT 0.0093 1.1982 REM Instructions for potential hydrogen bonds HTAB C1 I1 HTAB C2 I3_$2 HTAB C5 I2_$3 HTAB C6 I1 HTAB C6 I2_$3 REM Highest difference peak 0.724, deepest hole -0.839, 1-sigma level 0.115 Q1 1 0.6647 0.8243 0.0164 11.00000 0.05 0.72 Q2 1 0.6560 0.6756 0.0199 11.00000 0.05 0.48 Q3 1 -0.2206 0.3329 0.1420 11.00000 0.05 0.48 Q4 1 0.7813 0.7087 -0.0007 11.00000 0.05 0.46 Q5 1 0.2165 0.5740 0.2330 11.00000 0.05 0.45 Q6 1 -0.0540 0.1066 -0.0120 11.00000 0.05 0.45 Q7 1 -0.2770 0.2778 0.1031 11.00000 0.05 0.43 Q8 1 -0.3132 0.0335 0.0377 11.00000 0.05 0.42 Q9 1 -0.3398 0.3150 0.2370 11.00000 0.05 0.41 Q10 1 -0.3651 0.1278 0.3010 11.00000 0.05 0.41 Q11 1 -0.3864 0.2150 0.1273 11.00000 0.05 0.40 Q12 1 0.3972 0.6178 0.1469 11.00000 0.05 0.40 Q13 1 0.4944 0.3925 0.0730 11.00000 0.05 0.39 Q14 1 0.1780 0.5545 0.1734 11.00000 0.05 0.39 Q15 1 0.7383 0.7790 0.0776 11.00000 0.05 0.39 Q16 1 -0.2559 0.4838 0.3792 11.00000 0.05 0.37 Q17 1 0.7057 0.8195 0.0718 11.00000 0.05 0.37 Q18 1 -0.0779 0.3668 0.0482 11.00000 0.05 0.36 Q19 1 -0.4218 0.2333 0.1891 11.00000 0.05 0.36 Q20 1 0.2938 0.5303 0.1705 11.00000 0.05 0.36 ; _shelx_res_checksum 28649 loop_ _symmetry_equiv_pos_as_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 I1 I 0.21863(2) 0.48802(2) 0.20388(2) 0.02532(4) Uani 1 1 d . . . . . I2 I 0.45818(2) 0.63781(2) 0.12212(2) 0.02138(4) Uani 1 1 d . . . . . I3 I 0.69863(2) 0.75122(2) 0.03666(2) 0.02834(5) Uani 1 1 d . . . . . C1 C -0.1944(3) 0.3740(3) 0.18015(15) 0.0246(4) Uani 1 1 d . . . . . H1A H -0.110984 0.439069 0.188619 0.03 Uiso 1 1 calc R U . . . C2 C -0.2876(3) 0.3613(3) 0.24191(16) 0.0287(5) Uani 1 1 d . . . . . H2A H -0.268917 0.417266 0.292682 0.034 Uiso 1 1 calc R U . . . C3 C -0.4090(3) 0.2661(3) 0.22935(16) 0.0267(5) Uani 1 1 d . . . . . H3A H -0.473803 0.254971 0.271629 0.032 Uiso 1 1 calc R U . . . C4 C -0.4347(3) 0.1873(3) 0.15448(16) 0.0255(5) Uani 1 1 d . . . . . H4A H -0.518206 0.122852 0.144636 0.031 Uiso 1 1 calc R U . . . C5 C -0.3386(2) 0.2029(3) 0.09431(14) 0.0218(4) Uani 1 1 d . . . . . H5A H -0.355614 0.148489 0.042966 0.026 Uiso 1 1 calc R U . . . C6 C -0.1171(2) 0.3097(3) 0.04193(14) 0.0212(4) Uani 1 1 d . . . . . H6A H -0.037008 0.38159 0.06115 0.025 Uiso 1 1 calc R U . . . H6B H -0.166829 0.358026 -0.008132 0.025 Uiso 1 1 calc R U . . . C7 C -0.0576(2) 0.1484(3) 0.02024(14) 0.0190(4) Uani 1 1 d . . . . . C8 C 0.0305(2) 0.0644(3) 0.07876(14) 0.0206(4) Uani 1 1 d . . . . . H8A H 0.051611 0.10826 0.132435 0.025 Uiso 1 1 calc R U . . . C9 C 0.0875(2) -0.0838(3) 0.05849(14) 0.0212(4) Uani 1 1 d . . . . . H9A H 0.14697 -0.141023 0.098514 0.025 Uiso 1 1 calc R U . . . N1 N -0.21976(19) 0.2956(2) 0.10801(12) 0.0183(3) Uani 1 1 d . . . . . 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 I1 0.01870(7) 0.02955(8) 0.02818(8) 0.00094(5) 0.00490(6) -0.00254(5) I2 0.01747(7) 0.02053(8) 0.02592(8) 0.00123(5) 0.00010(5) -0.00044(4) I3 0.02378(8) 0.03051(9) 0.03141(9) -0.00200(6) 0.00672(6) -0.00884(6) C1 0.0219(10) 0.0272(12) 0.0244(11) -0.0019(8) -0.0011(8) -0.0015(8) C2 0.0295(12) 0.0324(13) 0.0241(12) -0.0017(9) 0.0021(9) 0.0014(9) C3 0.0276(12) 0.0296(12) 0.0237(11) 0.0057(8) 0.0071(9) 0.0039(9) C4 0.0210(10) 0.0248(12) 0.0309(12) 0.0046(9) 0.0035(9) -0.0016(8) C5 0.0220(10) 0.0206(10) 0.0229(11) -0.0003(8) 0.0017(8) -0.0029(8) C6 0.0193(10) 0.0211(11) 0.0239(11) 0.0015(8) 0.0067(8) -0.0018(7) C7 0.0151(9) 0.0218(10) 0.0205(10) 0.0017(7) 0.0038(7) -0.0009(7) C8 0.0179(9) 0.0256(11) 0.0182(10) 0.0001(7) 0.0009(7) 0.0003(7) C9 0.0175(9) 0.0260(11) 0.0200(10) 0.0029(8) 0.0005(8) 0.0011(7) N1 0.0172(8) 0.0174(8) 0.0207(9) 0.0015(6) 0.0031(6) 0.0012(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 I3 I2 I1 174.110(7) . . ? N1 C1 C2 120.9(2) . . ? C1 C2 C3 119.4(2) . . ? C4 C3 C2 119.2(2) . . ? C5 C4 C3 119.6(2) . . ? N1 C5 C4 120.3(2) . . ? N1 C6 C7 111.37(18) . . ? C9 C7 C8 119.7(2) 3 . ? C9 C7 C6 120.4(2) 3 . ? C8 C7 C6 119.9(2) . . ? C9 C8 C7 120.1(2) . . ? C7 C9 C8 120.3(2) 3 . ? C1 N1 C5 120.6(2) . . ? C1 N1 C6 120.21(19) . . ? C5 N1 C6 119.17(19) . . ? 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 I1 I2 2.9556(2) . ? I2 I3 2.8796(2) . ? C1 N1 1.344(3) . ? C1 C2 1.376(4) . ? C2 C3 1.386(4) . ? C3 C4 1.384(4) . ? C4 C5 1.377(3) . ? C5 N1 1.356(3) . ? C6 N1 1.492(3) . ? C6 C7 1.505(3) . ? C7 C9 1.393(3) 3 ? C7 C8 1.397(3) . ? C8 C9 1.393(3) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C1 H1A I1 0.95 3.09 3.960(2) 152.3 . yes C2 H2A I3 0.95 3.12 3.734(3) 124.2 2_545 yes C5 H5A I2 0.95 3.3 3.836(2) 118.1 3_565 yes loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 0.1(4) . . . . ? C1 C2 C3 C4 -0.8(4) . . . . ? C2 C3 C4 C5 0.9(4) . . . . ? C3 C4 C5 N1 -0.4(4) . . . . ? N1 C6 C7 C9 115.4(2) . . . 3 ? N1 C6 C7 C8 -65.9(3) . . . . ? C9 C7 C8 C9 -0.3(4) 3 . . . ? C6 C7 C8 C9 -179.0(2) . . . . ? C7 C8 C9 C7 0.3(4) . . . 3 ? C2 C1 N1 C5 0.4(3) . . . . ? C2 C1 N1 C6 -179.5(2) . . . . ? C4 C5 N1 C1 -0.3(3) . . . . ? C4 C5 N1 C6 179.7(2) . . . . ? C7 C6 N1 C1 120.5(2) . . . . ? C7 C6 N1 C5 -59.4(3) . . . . ?