#------------------------------------------------------------------------------ #$Date: 2020-10-06 11:52:33 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257544 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705284.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_7705284 loop_ _publ_author_name 'Guo, Yuan-Yuan' 'Lightfoot, Philip' _publ_section_title ; Structural diversity of lead halide chain compounds, APbX3, templated by isomeric molecular cations. ; _journal_issue 36 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 12767 _journal_page_last 12775 _journal_paper_doi 10.1039/d0dt02782k _journal_volume 49 _journal_year 2020 _chemical_formula_moiety 'Br3 Pb, C9 H8 N' _chemical_formula_sum 'C9 H8 Br3 N Pb' _chemical_formula_weight 577.08 _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 _atom_sites_solution_primary dual _atom_sites_solution_secondary dual _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-08-07 deposited with the CCDC. 2020-08-27 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 98.941(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 4.3397(2) _cell_length_b 22.5309(17) _cell_length_c 13.0048(10) _cell_measurement_reflns_used 951 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 2.4 _cell_volume 1256.12(15) _computing_molecular_graphics 'Ortep for Windows (Farrugia, 2012)' _computing_publication_material 'WinGX publication routines (Farrugia, 2012)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT-2018/2 (Sheldrick, 2015)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type ; Rigaku Mercury2 (2x2 bin mode) ; _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.1118 _diffrn_reflns_av_unetI/netI 0.0782 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 9972 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 24.994 _diffrn_reflns_theta_max 24.994 _diffrn_reflns_theta_min 2.405 _diffrn_source 'Sealed Tube' _exptl_absorpt_coefficient_mu 22.937 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.385 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 3.052 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Prism _exptl_crystal_F_000 1024 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _refine_diff_density_max 1.955 _refine_diff_density_min -1.922 _refine_diff_density_rms 0.317 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 127 _refine_ls_number_reflns 2192 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.944 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0349 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0249P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0767 _refine_ls_wR_factor_ref 0.0780 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1786 _reflns_number_total 2192 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02782k2.cif _cod_data_source_block shelx_CCDC2 _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 Adding full bibliography for 7705282--7705287.cif. ; _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7705284 _shelx_shelxl_version_number 2018/3 _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_res_file ; TITL shelxt_a.res in P21/n shelx.res created by SHELXL-2018/3 at 14:47:27 on 10-Jun-2020 CELL 0.71075 4.3397 22.5309 13.0048 90.000 98.941 90.000 ZERR 4 0.0002 0.0017 0.0010 0.000 0.006 0.000 LATT 1 SYMM 0.50000 - X , 0.50000 + Y , 0.50000 - Z SFAC Pb Br N C H UNIT 4 12 4 36 32 L.S. 5 FMAP 2 PLAN -20 ACTA OMIT -3 50 OMIT 0 2 4 OMIT -2 0 8 OMIT 1 6 0 OMIT -1 0 5 CONF BOND HTAB HTAB N1 Br1 WGHT 0.024900 FVAR 0.21003 RESI 0 PB1 1 0.703543 0.532441 0.857834 11.00000 0.01573 0.02225 = 0.01753 0.00087 0.00349 -0.00078 BR1 2 0.614673 0.510489 0.641441 11.00000 0.03081 0.02644 = 0.01922 -0.00220 0.00150 0.00589 BR2 2 1.193117 0.623410 0.828050 11.00000 0.01997 0.02240 = 0.03196 -0.00050 0.00596 -0.00157 BR3 2 0.225907 0.439241 0.892077 11.00000 0.02546 0.02138 = 0.02615 0.00141 0.00436 -0.00237 N1 3 0.192623 0.618460 0.514718 11.00000 0.02657 0.02456 = 0.04318 0.00678 0.01115 0.00702 AFIX 43 H1 5 0.262316 0.588990 0.553524 11.00000 -1.20000 AFIX 0 C1 4 -0.028537 0.608226 0.435981 11.00000 0.03228 0.03000 = 0.06349 -0.00771 0.01810 0.00467 AFIX 43 H2 5 -0.105110 0.569920 0.423492 11.00000 -1.20000 AFIX 0 C2 4 -0.149399 0.654530 0.370900 11.00000 0.02609 0.06320 = 0.03546 -0.01309 0.00363 0.01115 AFIX 43 H3 5 -0.303123 0.647226 0.314081 11.00000 -1.20000 AFIX 0 C3 4 -0.038579 0.711203 0.391702 11.00000 0.02974 0.03981 = 0.03281 0.00463 0.01295 0.01155 AFIX 43 H4 5 -0.121032 0.742520 0.349593 11.00000 -1.20000 AFIX 0 C4 4 0.197551 0.721942 0.475899 11.00000 0.02752 0.02833 = 0.03336 0.01083 0.01701 0.01020 C5 4 0.323192 0.778616 0.501658 11.00000 0.04563 0.02088 = 0.04850 0.01745 0.02257 0.01128 AFIX 43 H5 5 0.244243 0.811407 0.462791 11.00000 -1.20000 AFIX 0 C6 4 0.559874 0.785936 0.583158 11.00000 0.03752 0.02081 = 0.06521 -0.00042 0.01253 0.00637 AFIX 43 H6 5 0.643761 0.823403 0.599156 11.00000 -1.20000 AFIX 0 C7 4 0.675194 0.736535 0.642443 11.00000 0.02478 0.04382 = 0.03316 -0.00520 0.01059 0.00162 AFIX 43 H7 5 0.836023 0.742102 0.697797 11.00000 -1.20000 AFIX 0 C8 4 0.561339 0.680703 0.622300 11.00000 0.03419 0.02730 = 0.02980 0.00899 0.01965 0.00549 AFIX 43 H8 5 0.641893 0.648582 0.662700 11.00000 -1.20000 AFIX 0 C9 4 0.319162 0.673297 0.538801 11.00000 0.02721 0.01994 = 0.02829 0.00692 0.01666 0.01081 HKLF 4 1 -1.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 1.0000 0.0000 1.0000 REM shelxt_a.res in P21/n REM wR2 = 0.0780, GooF = S = 0.944, Restrained GooF = 0.944 for all data REM R1 = 0.0349 for 1786 Fo > 4sig(Fo) and 0.0408 for all 2192 data REM 127 parameters refined using 0 restraints END WGHT 0.0249 0.0000 REM Instructions for potential hydrogen bonds HTAB N1 Br1 EQIV $3 -x+1, -y+1, -z+1 HTAB C1 Br1_$3 HTAB C8 Br1 REM Highest difference peak 1.955, deepest hole -1.922, 1-sigma level 0.317 Q1 1 0.7062 0.5679 0.9013 11.00000 0.05 1.96 Q2 1 0.7331 0.5004 0.9006 11.00000 0.05 1.94 Q3 1 0.6640 0.4981 0.8069 11.00000 0.05 1.51 Q4 1 0.8489 0.5351 0.9557 11.00000 0.05 1.47 Q5 1 0.6902 0.5675 0.8172 11.00000 0.05 1.37 Q6 1 0.5491 0.5252 0.7551 11.00000 0.05 1.29 Q7 1 0.7627 0.5252 1.0626 11.00000 0.05 1.21 Q8 1 0.4926 0.5337 0.9422 11.00000 0.05 1.15 Q9 1 0.8971 0.5335 0.7751 11.00000 0.05 1.08 Q10 1 0.5644 0.4664 0.6351 11.00000 0.05 1.07 Q11 1 1.0584 0.5337 0.9010 11.00000 0.05 1.03 Q12 1 0.3181 0.6307 0.9167 11.00000 0.05 1.01 Q13 1 0.6194 0.5450 0.6748 11.00000 0.05 0.96 Q14 1 0.9124 0.5696 0.9595 11.00000 0.05 0.95 Q15 1 0.4855 0.5577 1.0805 11.00000 0.05 0.94 Q16 1 1.1428 0.5896 0.7765 11.00000 0.05 0.93 Q17 1 0.6785 0.4164 0.6530 11.00000 0.05 0.92 Q18 1 0.2561 0.3988 0.8600 11.00000 0.05 0.91 Q19 1 0.9664 0.5593 1.0355 11.00000 0.05 0.89 Q20 1 0.6194 0.5351 1.0157 11.00000 0.05 0.87 ; _shelx_res_checksum 48546 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 Pb1 Pb 0.70354(7) 0.53244(2) 0.85783(2) 0.01841(13) Uani 1 1 d . . . . . Br1 Br 0.6147(2) 0.51049(4) 0.64144(6) 0.0257(2) Uani 1 1 d . . . . . Br2 Br 1.19312(19) 0.62341(4) 0.82805(7) 0.0246(2) Uani 1 1 d . . . . . Br3 Br 0.2259(2) 0.43924(4) 0.89208(7) 0.0243(2) Uani 1 1 d . . . . . N1 N 0.1926(18) 0.6185(3) 0.5147(6) 0.0308(18) Uani 1 1 d . . . . . H1 H 0.262316 0.588990 0.553524 0.037 Uiso 1 1 calc R U . . . C1 C -0.029(2) 0.6082(5) 0.4360(9) 0.041(3) Uani 1 1 d . . . . . H2 H -0.105110 0.569920 0.423492 0.049 Uiso 1 1 calc R U . . . C2 C -0.149(2) 0.6545(5) 0.3709(8) 0.042(3) Uani 1 1 d . . . . . H3 H -0.303123 0.647226 0.314081 0.050 Uiso 1 1 calc R U . . . C3 C -0.039(2) 0.7112(5) 0.3917(7) 0.033(2) Uani 1 1 d . . . . . H4 H -0.121032 0.742520 0.349593 0.040 Uiso 1 1 calc R U . . . C4 C 0.198(2) 0.7219(4) 0.4759(7) 0.028(2) Uani 1 1 d . . . . . C5 C 0.323(2) 0.7786(4) 0.5017(8) 0.037(2) Uani 1 1 d . . . . . H5 H 0.244243 0.811407 0.462791 0.044 Uiso 1 1 calc R U . . . C6 C 0.560(2) 0.7859(5) 0.5832(9) 0.041(3) Uani 1 1 d . . . . . H6 H 0.643761 0.823403 0.599156 0.049 Uiso 1 1 calc R U . . . C7 C 0.675(2) 0.7365(4) 0.6424(8) 0.033(2) Uani 1 1 d . . . . . H7 H 0.836023 0.742102 0.697797 0.040 Uiso 1 1 calc R U . . . C8 C 0.561(2) 0.6807(4) 0.6223(7) 0.029(2) Uani 1 1 d . . . . . H8 H 0.641893 0.648582 0.662700 0.035 Uiso 1 1 calc R U . . . C9 C 0.319(2) 0.6733(4) 0.5388(7) 0.0238(19) 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 Pb1 0.01573(18) 0.0223(2) 0.01753(18) 0.00087(13) 0.00349(12) -0.00078(13) Br1 0.0308(5) 0.0264(5) 0.0192(4) -0.0022(3) 0.0015(3) 0.0059(4) Br2 0.0200(4) 0.0224(4) 0.0320(5) -0.0005(4) 0.0060(3) -0.0016(3) Br3 0.0255(4) 0.0214(4) 0.0261(4) 0.0014(4) 0.0044(3) -0.0024(4) N1 0.027(4) 0.025(4) 0.043(5) 0.007(4) 0.011(4) 0.007(3) C1 0.032(6) 0.030(6) 0.063(7) -0.008(5) 0.018(5) 0.005(5) C2 0.026(5) 0.063(8) 0.035(6) -0.013(5) 0.004(4) 0.011(5) C3 0.030(5) 0.040(6) 0.033(5) 0.005(5) 0.013(4) 0.012(4) C4 0.028(5) 0.028(5) 0.033(5) 0.011(4) 0.017(4) 0.010(4) C5 0.046(6) 0.021(5) 0.048(6) 0.017(5) 0.023(5) 0.011(4) C6 0.038(6) 0.021(5) 0.065(7) 0.000(5) 0.013(5) 0.006(4) C7 0.025(5) 0.044(6) 0.033(5) -0.005(5) 0.011(4) 0.002(4) C8 0.034(5) 0.027(5) 0.030(5) 0.009(4) 0.020(4) 0.005(4) C9 0.027(5) 0.020(4) 0.028(5) 0.007(4) 0.017(4) 0.011(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' 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' 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 Pb1 Br2 90.42(3) . 1_455 ? Br1 Pb1 Br2 88.91(3) . . ? Br2 Pb1 Br2 92.28(2) 1_455 . ? Br1 Pb1 Br3 91.97(3) . . ? Br2 Pb1 Br3 89.10(2) 1_455 . ? Br2 Pb1 Br3 178.36(3) . . ? Br1 Pb1 Br3 90.47(3) . 1_655 ? Br2 Pb1 Br3 179.09(3) 1_455 1_655 ? Br2 Pb1 Br3 87.97(2) . 1_655 ? Br3 Pb1 Br3 90.64(2) . 1_655 ? Pb1 Br2 Pb1 92.28(2) 1_655 . ? Pb1 Br3 Pb1 90.64(2) . 1_455 ? C1 N1 C9 123.8(9) . . ? N1 C1 C2 120.2(10) . . ? C3 C2 C1 119.2(9) . . ? C2 C3 C4 120.3(9) . . ? C3 C4 C5 123.5(9) . . ? C3 C4 C9 118.6(9) . . ? C5 C4 C9 117.9(9) . . ? C6 C5 C4 120.7(9) . . ? C5 C6 C7 119.5(10) . . ? C8 C7 C6 122.7(9) . . ? C7 C8 C9 117.8(9) . . ? N1 C9 C8 120.8(8) . . ? N1 C9 C4 117.7(8) . . ? C8 C9 C4 121.5(9) . . ? 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 Pb1 Br1 2.8241(9) . ? Pb1 Br2 2.9985(9) 1_455 ? Pb1 Br2 3.0201(9) . ? Pb1 Br3 3.0317(9) . ? Pb1 Br3 3.0713(9) 1_655 ? N1 C1 1.310(14) . ? N1 C9 1.368(12) . ? C1 C2 1.394(15) . ? C2 C3 1.376(15) . ? C3 C4 1.400(14) . ? C4 C5 1.408(14) . ? C4 C9 1.419(12) . ? C5 C6 1.366(15) . ? C6 C7 1.401(14) . ? C7 C8 1.362(13) . ? C8 C9 1.399(13) . ? 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 N1 H1 Br1 0.86 2.50 3.324(8) 161.9 . 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 C9 N1 C1 C2 -0.1(15) . . . . ? N1 C1 C2 C3 -1.4(15) . . . . ? C1 C2 C3 C4 1.4(14) . . . . ? C2 C3 C4 C5 179.7(9) . . . . ? C2 C3 C4 C9 0.0(13) . . . . ? C3 C4 C5 C6 -178.1(10) . . . . ? C9 C4 C5 C6 1.6(14) . . . . ? C4 C5 C6 C7 -0.9(15) . . . . ? C5 C6 C7 C8 0.1(16) . . . . ? C6 C7 C8 C9 -0.1(14) . . . . ? C1 N1 C9 C8 -178.1(9) . . . . ? C1 N1 C9 C4 1.5(13) . . . . ? C7 C8 C9 N1 -179.6(8) . . . . ? C7 C8 C9 C4 0.8(13) . . . . ? C3 C4 C9 N1 -1.5(12) . . . . ? C5 C4 C9 N1 178.8(8) . . . . ? C3 C4 C9 C8 178.2(8) . . . . ? C5 C4 C9 C8 -1.6(13) . . . . ?