#------------------------------------------------------------------------------ #$Date: 2020-08-28 04:43:46 +0300 (Fri, 28 Aug 2020) $ #$Revision: 255702 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705283.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_7705283 loop_ _publ_author_name 'Guo, Yuanyuan' 'Lightfoot, Philip' _publ_section_title ; Structural Diversity of Lead Halide Chain Compounds, APbX3, Templated by Isomeric Molecular Cations ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02782K _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 _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 99.068(8) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 4.3634(4) _cell_length_b 22.5833(18) _cell_length_c 13.1074(11) _cell_measurement_reflns_used 952 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 2.4 _cell_volume 1275.46(19) _computing_molecular_graphics 'Ortep for Windows (Farrugia, 2012)' _computing_publication_material 'WinGX publication routines (Farrugia, 2012)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type ; Rigaku Mercury2 (2x2 bin mode) ; _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0609 _diffrn_reflns_av_unetI/netI 0.0482 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 12963 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.484 _diffrn_reflns_theta_min 2.394 _diffrn_source 'Sealed Tube' _exptl_absorpt_coefficient_mu 22.589 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.571 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 3.005 _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 1.295 _refine_diff_density_min -1.446 _refine_diff_density_rms 0.152 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.870 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 127 _refine_ls_number_reflns 2918 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.870 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0250 _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^)+(0.0210P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.0507 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2189 _reflns_number_total 2918 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02782k2.cif _cod_data_source_block shelx_CCDC1 _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_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7705283 _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 P2(1)/n shelx.res created by SHELXL-2018/3 at 14:36:36 on 10-Jun-2020 REM Old TITL RC14RTB REM SHELXT solution in P2(1)/n: R1 0.068, Rweak 0.004, Alpha 0.046 REM 0.188 for 82 systematic absences, Orientation as input REM Formula found by SHELXT: Pb Br3 N C9 CELL 0.71075 4.3634 22.5833 13.1074 90.000 99.068 90.000 ZERR 4.000 0.0004 0.0018 0.0011 0.000 0.008 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC PB BR N C H UNIT 4 12 4 36 32 L.S. 10 BOND HTAB HTAB N1 Br1 ACTA LIST 4 FMAP 2 PLAN 10 WGHT 0.021000 FVAR 0.19110 PB1 1 0.701912 0.532249 0.857410 11.00000 0.03085 0.03319 = 0.03028 0.00180 0.00409 -0.00108 BR1 2 0.609706 0.509917 0.642708 11.00000 0.05737 0.04089 = 0.03323 -0.00433 0.00095 0.01034 BR2 2 1.191380 0.622858 0.827779 11.00000 0.03772 0.03201 = 0.05530 -0.00060 0.00764 -0.00184 BR3 2 0.225709 0.439808 0.893657 11.00000 0.04649 0.03248 = 0.04571 0.00336 0.00636 -0.00361 N1 3 0.198214 0.618533 0.516914 11.00000 0.05565 0.03499 = 0.07531 0.01026 0.01213 0.00879 AFIX 43 H1 5 0.266802 0.589514 0.556523 11.00000 -1.20000 AFIX 0 C1 4 -0.020625 0.607963 0.437763 11.00000 0.05230 0.05480 = 0.09966 -0.02886 0.01498 -0.00076 AFIX 43 H2 5 -0.093507 0.569547 0.425033 11.00000 -1.20000 AFIX 0 C2 4 -0.143485 0.653627 0.373171 11.00000 0.07118 0.09578 = 0.05608 -0.00969 0.00663 0.02276 AFIX 43 H3 5 -0.300208 0.646181 0.317881 11.00000 -1.20000 AFIX 0 C3 4 -0.031785 0.709281 0.391804 11.00000 0.06353 0.06276 = 0.05304 0.01307 0.01249 0.02029 AFIX 43 H4 5 -0.110452 0.740028 0.348190 11.00000 -1.20000 AFIX 0 C4 4 0.199600 0.720969 0.475566 11.00000 0.04732 0.04339 = 0.04668 0.01373 0.01846 0.01323 C5 4 0.323912 0.778039 0.499849 11.00000 0.06251 0.03384 = 0.09327 0.02128 0.02716 0.01518 AFIX 43 H5 5 0.245493 0.810587 0.460737 11.00000 -1.20000 AFIX 0 C6 4 0.556548 0.785123 0.579903 11.00000 0.06240 0.03847 = 0.11702 -0.00363 0.03178 -0.00111 AFIX 43 H6 5 0.640945 0.822558 0.594554 11.00000 -1.20000 AFIX 0 C7 4 0.672079 0.737097 0.640936 11.00000 0.05393 0.05803 = 0.06543 -0.00240 0.01092 0.00326 AFIX 43 H7 5 0.830820 0.743223 0.696165 11.00000 -1.20000 AFIX 0 C8 4 0.558446 0.681720 0.621643 11.00000 0.05492 0.04868 = 0.04824 0.01403 0.01425 0.00939 AFIX 43 H8 5 0.637342 0.649963 0.662765 11.00000 -1.20000 AFIX 0 C9 4 0.321248 0.673567 0.538940 11.00000 0.04705 0.03208 = 0.04992 0.00893 0.02299 0.01088 HKLF 4 REM shelxt_a.res in P2(1)/n REM wR2 = 0.0507, GooF = S = 0.870, Restrained GooF = 0.870 for all data REM R1 = 0.0250 for 2189 Fo > 4sig(Fo) and 0.0407 for all 2918 data REM 127 parameters refined using 0 restraints END WGHT 0.0210 0.0000 REM Instructions for potential hydrogen bonds HTAB N1 Br1 EQIV $3 -x+1, -y+1, -z+1 HTAB C1 Br1_$3 REM Highest difference peak 1.295, deepest hole -1.446, 1-sigma level 0.152 Q1 1 0.6989 0.5763 0.8585 11.00000 0.05 1.30 Q2 1 0.7109 0.4894 0.8577 11.00000 0.05 1.25 Q3 1 0.6631 0.5314 0.7919 11.00000 0.05 1.00 Q4 1 0.7366 0.5326 0.9233 11.00000 0.05 0.99 Q5 1 0.9313 0.5717 0.8349 11.00000 0.05 0.84 Q6 1 0.4979 0.4906 0.8822 11.00000 0.05 0.81 Q7 1 0.8801 0.4936 0.8185 11.00000 0.05 0.74 Q8 1 0.2267 0.4374 0.8289 11.00000 0.05 0.68 Q9 1 0.5436 0.5676 0.8927 11.00000 0.05 0.64 Q10 1 1.1820 0.6234 0.8927 11.00000 0.05 0.59 ; _shelx_res_checksum 84823 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 0.70191(4) 0.53225(2) 0.85741(2) 0.03152(7) Uani 1 1 d . . . . . Br1 Br 0.60971(14) 0.50992(3) 0.64271(4) 0.04450(15) Uani 1 1 d . . . . . Br2 Br 1.19138(12) 0.62286(3) 0.82778(5) 0.04164(14) Uani 1 1 d . . . . . Br3 Br 0.22571(13) 0.43981(3) 0.89366(4) 0.04166(14) Uani 1 1 d . . . . . N1 N 0.1982(12) 0.6185(2) 0.5169(4) 0.0551(14) Uani 1 1 d . . . . . H1 H 0.266802 0.589514 0.556523 0.066 Uiso 1 1 calc R U . . . C1 C -0.0206(15) 0.6080(3) 0.4378(6) 0.069(2) Uani 1 1 d . . . . . H2 H -0.093507 0.569547 0.425033 0.082 Uiso 1 1 calc R U . . . C2 C -0.1435(18) 0.6536(4) 0.3732(6) 0.075(2) Uani 1 1 d . . . . . H3 H -0.300208 0.646181 0.317881 0.090 Uiso 1 1 calc R U . . . C3 C -0.0318(15) 0.7093(4) 0.3918(5) 0.0594(18) Uani 1 1 d . . . . . H4 H -0.110452 0.740028 0.348190 0.071 Uiso 1 1 calc R U . . . C4 C 0.1996(13) 0.7210(3) 0.4756(5) 0.0446(15) Uani 1 1 d . . . . . C5 C 0.3239(16) 0.7780(3) 0.4998(6) 0.0616(19) Uani 1 1 d . . . . . H5 H 0.245493 0.810587 0.460737 0.074 Uiso 1 1 calc R U . . . C6 C 0.5565(17) 0.7851(3) 0.5799(7) 0.071(2) Uani 1 1 d . . . . . H6 H 0.640945 0.822558 0.594554 0.085 Uiso 1 1 calc R U . . . C7 C 0.6721(16) 0.7371(3) 0.6409(5) 0.0590(18) Uani 1 1 d . . . . . H7 H 0.830820 0.743223 0.696165 0.071 Uiso 1 1 calc R U . . . C8 C 0.5584(14) 0.6817(3) 0.6216(5) 0.0500(16) Uani 1 1 d . . . . . H8 H 0.637342 0.649963 0.662765 0.060 Uiso 1 1 calc R U . . . C9 C 0.3212(13) 0.6736(3) 0.5389(5) 0.0414(14) 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 0.03085(10) 0.03319(12) 0.03028(11) 0.00180(9) 0.00409(7) -0.00108(9) Br1 0.0574(3) 0.0409(3) 0.0332(3) -0.0043(2) 0.0009(3) 0.0103(3) Br2 0.0377(3) 0.0320(3) 0.0553(4) -0.0006(3) 0.0076(3) -0.0018(2) Br3 0.0465(3) 0.0325(3) 0.0457(3) 0.0034(3) 0.0064(2) -0.0036(3) N1 0.056(3) 0.035(3) 0.075(4) 0.010(3) 0.012(3) 0.009(3) C1 0.052(4) 0.055(5) 0.100(6) -0.029(4) 0.015(4) -0.001(4) C2 0.071(5) 0.096(7) 0.056(5) -0.010(5) 0.007(4) 0.023(5) C3 0.064(4) 0.063(5) 0.053(4) 0.013(4) 0.012(3) 0.020(4) C4 0.047(3) 0.043(4) 0.047(4) 0.014(3) 0.018(3) 0.013(3) C5 0.063(4) 0.034(4) 0.093(6) 0.021(4) 0.027(4) 0.015(3) C6 0.062(5) 0.038(4) 0.117(7) -0.004(4) 0.032(5) -0.001(4) C7 0.054(4) 0.058(5) 0.065(5) -0.002(4) 0.011(3) 0.003(4) C8 0.055(4) 0.049(4) 0.048(4) 0.014(3) 0.014(3) 0.009(3) C9 0.047(3) 0.032(3) 0.050(4) 0.009(3) 0.023(3) 0.011(3) 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 90.374(18) . 1_455 ? Br1 Pb1 Br2 89.166(19) . . ? Br2 Pb1 Br2 92.681(18) 1_455 . ? Br1 Pb1 Br3 92.27(2) . . ? Br2 Pb1 Br3 88.667(18) 1_455 . ? Br2 Pb1 Br3 178.024(17) . . ? Br1 Pb1 Br3 91.053(18) . 1_655 ? Br2 Pb1 Br3 178.562(17) 1_455 1_655 ? Br2 Pb1 Br3 87.509(17) . 1_655 ? Br3 Pb1 Br3 91.107(18) . 1_655 ? Pb1 Br2 Pb1 92.681(18) 1_655 . ? Pb1 Br3 Pb1 91.108(18) . 1_455 ? C1 N1 C9 122.9(6) . . ? N1 C1 C2 120.6(7) . . ? C3 C2 C1 119.1(7) . . ? C2 C3 C4 120.8(7) . . ? C3 C4 C9 118.7(6) . . ? C3 C4 C5 123.6(6) . . ? C9 C4 C5 117.7(6) . . ? C6 C5 C4 119.8(6) . . ? C5 C6 C7 120.9(7) . . ? C8 C7 C6 121.5(7) . . ? C7 C8 C9 118.3(6) . . ? N1 C9 C8 120.4(6) . . ? N1 C9 C4 117.9(6) . . ? C8 C9 C4 121.7(6) . . ? 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 2.8247(6) . ? Pb1 Br2 3.0046(6) 1_455 ? Pb1 Br2 3.0267(6) . ? Pb1 Br3 3.0352(6) . ? Pb1 Br3 3.0766(6) 1_655 ? N1 C1 1.316(9) . ? N1 C9 1.367(8) . ? C1 C2 1.387(10) . ? C2 C3 1.356(10) . ? C3 C4 1.395(9) . ? C4 C9 1.407(8) . ? C4 C5 1.415(9) . ? C5 C6 1.350(10) . ? C6 C7 1.394(10) . ? C7 C8 1.354(9) . ? C8 C9 1.388(8) . ? 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 2.49 3.321(5) 161.8 . yes