#------------------------------------------------------------------------------ #$Date: 2020-04-21 04:57:05 +0300 (Tue, 21 Apr 2020) $ #$Revision: 250973 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/03/7240357.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_7240357 loop_ _publ_author_name 'Mehring, Michael' 'Preda, Ana Maria' 'Scholz, Sebastian' 'Krasowska, Malgorzata' 'Bhattacharyya, Kalishankar' 'Toma, Ana Maria' 'Silvestru, Cristian' 'Korb, Marcus' 'Rueffer, Tobias' 'Lang, Heinrich' 'Auer, Alexander A.' _publ_section_title ; Evaluation of bismuth-based dispersion energy donors -- synthesis, structure and theoretical study of 2-biphenylbismuth(III) derivatives ; _journal_name_full 'Physical Chemistry Chemical Physics' _journal_paper_doi 10.1039/C9CP06924K _journal_year 2020 _chemical_formula_moiety 'C12 H9 Bi Cl2' _chemical_formula_sum 'C12 H9 Bi Cl2' _chemical_formula_weight 433.07 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2013 _audit_update_record ; 2020-04-03 deposited with the CCDC. 2020-04-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.6237(7) _cell_length_b 9.0462(8) _cell_length_c 17.6540(17) _cell_measurement_reflns_used 4660 _cell_measurement_temperature 100 _cell_measurement_theta_max 25.5754 _cell_measurement_theta_min 3.2241 _cell_volume 1217.52(19) _computing_cell_refinement 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_data_collection 'APEX3 v2017.3-0' _computing_data_reduction 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)' _diffrn_ambient_temperature 100 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'bruker venture d8' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_unetI/netI 0.0565 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 5829 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 25.574 _diffrn_reflns_theta_min 3.531 _exptl_absorpt_coefficient_mu 14.883 _exptl_absorpt_correction_T_max 0.32 _exptl_absorpt_correction_T_min 0.14 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.363 _exptl_crystal_description block _exptl_crystal_F_000 792 _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _refine_diff_density_max 1.000 _refine_diff_density_min -0.785 _refine_diff_density_rms 0.139 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.021(11) _refine_ls_extinction_coef 0.0022(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 0.818 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 138 _refine_ls_number_reflns 2249 _refine_ls_number_restraints 111 _refine_ls_restrained_S_all 0.801 _refine_ls_R_factor_all 0.0224 _refine_ls_R_factor_gt 0.0204 _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^)] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.0457 _reflns_Friedel_coverage 0.706 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.999 _reflns_number_gt 2150 _reflns_number_total 2249 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cp06924k2.cif _cod_data_source_block shelx_CCDC5 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_database_code 7240357 _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 0.318 _shelx_estimated_absorpt_t_max 0.318 _shelxl_version_number 2013-4 _shelx_res_file ; TITL mo_ss_ma_006_0m_a.res in P2(1)2(1)2(1) CELL 0.71073 7.6237 9.0462 17.6540 90.000 90.000 90.000 ZERR 4.00 0.0007 0.0008 0.0017 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H BI CL UNIT 48 36 4 8 MERG 2 OMIT 1 0 1 OMIT 1 1 0 OMIT 0 5 8 OMIT -2 5 7 OMIT 0 1 3 TWIN RIGU FMAP 2 PLAN 20 SIZE 0.100 0.100 0.100 ACTA 50.00 BOND $H LIST 6 L.S. 10 TEMP -173.15 WGHT 0.000000 EXTI 0.002188 BASF 0.02108 FVAR 0.11283 C1 1 1.173143 0.602379 0.295957 11.00000 0.01036 0.00737 = 0.01808 -0.00242 -0.00326 0.00013 C2 1 1.315947 0.669458 0.259682 11.00000 0.01041 0.01200 = 0.02150 -0.00047 0.00222 0.00416 AFIX 43 H2 2 1.336285 0.653111 0.207257 11.00000 -1.20000 AFIX 0 C3 1 1.427405 0.760002 0.301054 11.00000 0.00882 0.01482 = 0.03341 -0.00205 -0.00276 0.00103 AFIX 43 H3 2 1.524631 0.806134 0.277093 11.00000 -1.20000 AFIX 0 C4 1 1.396022 0.782839 0.377751 11.00000 0.01351 0.01739 = 0.03185 -0.00862 -0.00671 -0.00311 AFIX 43 H4 2 1.471701 0.845922 0.405729 11.00000 -1.20000 AFIX 0 C5 1 1.258193 0.716129 0.413624 11.00000 0.02009 0.01568 = 0.02114 -0.00772 -0.00233 0.00220 AFIX 43 H5 2 1.240180 0.731598 0.466278 11.00000 -1.20000 AFIX 0 C6 1 1.141941 0.623758 0.372289 11.00000 0.01427 0.00730 = 0.01728 -0.00255 -0.00060 0.00423 C7 1 0.996679 0.548987 0.411534 11.00000 0.01712 0.01302 = 0.01234 -0.00262 -0.00054 0.00355 C8 1 1.026858 0.456766 0.474236 11.00000 0.02688 0.01607 = 0.01163 -0.00168 -0.00181 0.00580 AFIX 43 H8 2 1.143445 0.442931 0.491863 11.00000 -1.20000 AFIX 0 C9 1 0.892555 0.386827 0.510258 11.00000 0.03512 0.01537 = 0.01876 0.00269 0.00366 -0.00031 AFIX 43 H9 2 0.917349 0.325714 0.552689 11.00000 -1.20000 AFIX 0 C10 1 0.721542 0.402744 0.486524 11.00000 0.02960 0.01685 = 0.02130 -0.00192 0.00848 -0.00284 AFIX 43 H10 2 0.629274 0.354702 0.513022 11.00000 -1.20000 AFIX 0 C11 1 0.684757 0.489764 0.423400 11.00000 0.01945 0.01607 = 0.02249 -0.00062 0.00616 0.00364 AFIX 43 H11 2 0.567924 0.498155 0.405186 11.00000 -1.20000 AFIX 0 C12 1 0.820435 0.564118 0.387355 11.00000 0.01898 0.01062 = 0.01218 0.00133 0.00092 0.00411 AFIX 43 H12 2 0.794501 0.626525 0.345550 11.00000 -1.20000 AFIX 0 BI1 3 0.979038 0.466637 0.232029 11.00000 0.01129 0.00939 = 0.01207 -0.00122 0.00030 -0.00151 CL1 4 0.840227 0.727077 0.190583 11.00000 0.01591 0.00800 = 0.01260 0.00033 -0.00238 0.00163 CL2 4 1.162639 0.456424 0.116430 11.00000 0.01996 0.01784 = 0.01298 -0.00168 0.00459 0.00139 HKLF 4 REM mo_ss_ma_006_0m_a.res in P2(1)2(1)2(1) REM R1 = 0.0204 for 2150 Fo > 4sig(Fo) and 0.0224 for all 2249 data REM 138 parameters refined using 111 restraints END WGHT 0.0000 0.0000 REM Highest difference peak 1.000, deepest hole -0.785, 1-sigma level 0.139 Q1 1 0.9774 0.5697 0.2335 11.00000 0.05 1.00 Q2 1 0.9741 0.3743 0.2332 11.00000 0.05 0.72 Q3 1 0.8706 0.4698 0.1318 11.00000 0.05 0.62 Q4 1 0.9719 0.7947 0.2340 11.00000 0.05 0.57 Q5 1 0.9704 0.4679 0.1844 11.00000 0.05 0.56 Q6 1 1.3182 0.7347 0.2727 11.00000 0.05 0.51 Q7 1 0.9973 0.4658 0.2903 11.00000 0.05 0.49 Q8 1 0.7776 0.4968 0.1772 11.00000 0.05 0.46 Q9 1 1.0014 0.7918 0.3805 11.00000 0.05 0.45 Q10 1 1.0068 0.6600 0.2655 11.00000 0.05 0.43 Q11 1 1.1812 0.5180 0.1220 11.00000 0.05 0.42 Q12 1 0.9059 0.5308 0.3826 11.00000 0.05 0.42 Q13 1 1.1532 0.4603 0.1562 11.00000 0.05 0.42 Q14 1 1.1949 0.5273 0.1765 11.00000 0.05 0.42 Q15 1 1.0224 0.7825 0.1699 11.00000 0.05 0.41 Q16 1 1.0030 0.6411 0.1183 11.00000 0.05 0.41 Q17 1 1.0258 0.7698 0.3665 11.00000 0.05 0.40 Q18 1 1.1915 0.4919 0.2984 11.00000 0.05 0.40 Q19 1 1.6602 0.8034 0.2237 11.00000 0.05 0.38 Q20 1 0.9878 0.3758 0.1559 11.00000 0.05 0.38 ; _shelx_res_checksum 19873 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 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 C1 C 1.1731(9) 0.6024(7) 0.2960(5) 0.0119(14) Uani 1 1 d . U . . . C2 C 1.3159(8) 0.6695(7) 0.2597(6) 0.0146(16) Uani 1 1 d . U . . . H2 H 1.3363 0.6531 0.2073 0.018 Uiso 1 1 calc R U . . . C3 C 1.4274(10) 0.7600(8) 0.3011(6) 0.0190(17) Uani 1 1 d . U . . . H3 H 1.5246 0.8061 0.2771 0.023 Uiso 1 1 calc R U . . . C4 C 1.3960(10) 0.7828(8) 0.3778(6) 0.0209(18) Uani 1 1 d . U . . . H4 H 1.4717 0.8459 0.4057 0.025 Uiso 1 1 calc R U . . . C5 C 1.2582(10) 0.7161(8) 0.4136(6) 0.0190(18) Uani 1 1 d . U . . . H5 H 1.2402 0.7316 0.4663 0.023 Uiso 1 1 calc R U . . . C6 C 1.1419(9) 0.6238(7) 0.3723(5) 0.0129(15) Uani 1 1 d . U . . . C7 C 0.9967(9) 0.5490(7) 0.4115(5) 0.0142(14) Uani 1 1 d . U . . . C8 C 1.0269(10) 0.4568(8) 0.4742(5) 0.0182(15) Uani 1 1 d . U . . . H8 H 1.1434 0.4429 0.4919 0.022 Uiso 1 1 calc R U . . . C9 C 0.8926(11) 0.3868(8) 0.5103(6) 0.0231(18) Uani 1 1 d . U . . . H9 H 0.9173 0.3257 0.5527 0.028 Uiso 1 1 calc R U . . . C10 C 0.7215(11) 0.4027(9) 0.4865(6) 0.0226(18) Uani 1 1 d . U . . . H10 H 0.6293 0.3547 0.5130 0.027 Uiso 1 1 calc R U . . . C11 C 0.6848(10) 0.4898(8) 0.4234(5) 0.0193(18) Uani 1 1 d . U . . . H11 H 0.5679 0.4982 0.4052 0.023 Uiso 1 1 calc R U . . . C12 C 0.8204(10) 0.5641(7) 0.3874(5) 0.0139(17) Uani 1 1 d . U . . . H12 H 0.7945 0.6265 0.3455 0.017 Uiso 1 1 calc R U . . . Bi1 Bi 0.97904(3) 0.46664(3) 0.23203(2) 0.01092(11) Uani 1 1 d . U . . . Cl1 Cl 0.8402(2) 0.72708(17) 0.19058(12) 0.0122(4) Uani 1 1 d . U . . . Cl2 Cl 1.1626(2) 0.4564(2) 0.11643(12) 0.0169(4) Uani 1 1 d . 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 C1 0.010(3) 0.007(3) 0.018(4) -0.002(3) -0.003(3) 0.000(3) C2 0.010(3) 0.012(3) 0.022(4) 0.000(3) 0.002(3) 0.004(2) C3 0.009(3) 0.015(3) 0.033(4) -0.002(3) -0.003(3) 0.001(3) C4 0.014(3) 0.017(4) 0.032(5) -0.009(3) -0.007(3) -0.003(3) C5 0.020(4) 0.016(4) 0.021(4) -0.008(3) -0.002(3) 0.002(3) C6 0.014(3) 0.007(3) 0.017(4) -0.003(3) -0.001(3) 0.004(2) C7 0.017(3) 0.013(3) 0.012(4) -0.003(3) -0.001(3) 0.004(3) C8 0.027(3) 0.016(3) 0.012(4) -0.002(3) -0.002(3) 0.006(3) C9 0.035(4) 0.015(4) 0.019(5) 0.003(4) 0.004(3) 0.000(3) C10 0.030(4) 0.017(3) 0.021(5) -0.002(4) 0.008(3) -0.003(3) C11 0.019(3) 0.016(4) 0.022(5) -0.001(3) 0.006(3) 0.004(3) C12 0.019(3) 0.011(4) 0.012(4) 0.001(3) 0.001(3) 0.004(2) Bi1 0.01129(14) 0.00939(13) 0.01207(16) -0.00122(12) 0.00030(11) -0.00151(10) Cl1 0.0159(8) 0.0080(8) 0.0126(10) 0.0003(8) -0.0024(8) 0.0016(6) Cl2 0.0200(8) 0.0178(8) 0.0130(11) -0.0017(9) 0.0046(7) 0.0014(9) 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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 C6 C1 C2 121.2(7) . . ? C6 C1 Bi1 117.2(5) . . ? C2 C1 Bi1 121.5(6) . . ? C3 C2 C1 119.4(9) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 119.7(8) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 121.2(7) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C4 C5 C6 120.1(9) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C1 C6 C5 118.4(7) . . ? C1 C6 C7 121.6(7) . . ? C5 C6 C7 119.9(8) . . ? C8 C7 C12 116.8(7) . . ? C8 C7 C6 121.4(7) . . ? C12 C7 C6 121.9(7) . . ? C9 C8 C7 121.4(7) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C8 C9 C10 121.4(9) . . ? C8 C9 H9 119.3 . . ? C10 C9 H9 119.3 . . ? C9 C10 C11 119.5(8) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 119.4(7) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C11 C12 C7 121.5(7) . . ? C11 C12 H12 119.3 . . ? C7 C12 H12 119.3 . . ? C1 Bi1 Cl2 93.6(2) . . ? C1 Bi1 Cl1 85.20(19) . . ? Cl2 Bi1 Cl1 91.77(6) . . ? C1 Bi1 Cl1 81.85(19) . 3_745 ? Cl2 Bi1 Cl1 95.25(6) . 3_745 ? Cl1 Bi1 Cl1 165.61(4) . 3_745 ? Bi1 Cl1 Bi1 109.82(7) . 3_755 ? 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 C1 C6 1.382(13) . ? C1 C2 1.401(10) . ? C1 Bi1 2.230(7) . ? C2 C3 1.388(11) . ? C2 H2 0.9500 . ? C3 C4 1.390(14) . ? C3 H3 0.9500 . ? C4 C5 1.367(12) . ? C4 H4 0.9500 . ? C5 C6 1.420(11) . ? C5 H5 0.9500 . ? C6 C7 1.471(10) . ? C7 C8 1.405(11) . ? C7 C12 1.416(10) . ? C8 C9 1.361(11) . ? C8 H8 0.9500 . ? C9 C10 1.377(12) . ? C9 H9 0.9500 . ? C10 C11 1.393(13) . ? C10 H10 0.9500 . ? C11 C12 1.388(11) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? Bi1 Cl2 2.476(2) . ? Bi1 Cl1 2.6844(16) . ? Bi1 Cl1 2.9088(18) 3_745 ? Cl1 Bi1 2.9088(18) 3_755 ?