#------------------------------------------------------------------------------ #$Date: 2025-03-22 01:36:20 +0200 (Sat, 22 Mar 2025) $ #$Revision: 298556 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/25/01/7250165.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_7250165 loop_ _publ_author_name 'van der Poll, Hendrik Johannes' 'Erasmus, Rudolph' 'Rademeyer, Melanie' _publ_section_title ; Structures and Band Gaps of Lead-Free Dabconium-Containing Hybrid Alkali-Metal Halide Perovskites ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D4CE00907J _journal_year 2025 _chemical_formula_moiety 'Br3 Cs, C6 H14 N2' _chemical_formula_sum 'C6 H14 Br3 Cs N2' _chemical_formula_weight 486.83 _space_group_crystal_system orthorhombic _space_group_IT_number 60 _space_group_name_Hall '-P 2n 2ab' _space_group_name_H-M_alt 'P b c n' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary difmap _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2025-02-17 deposited with the CCDC. 2025-03-21 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 9.8044(2) _cell_length_b 9.8273(3) _cell_length_c 27.3662(7) _cell_measurement_reflns_used 9474 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 31.0530 _cell_measurement_theta_min 2.4950 _cell_volume 2636.75(12) _computing_cell_refinement 'SAINT (Bruker, 2014)' _computing_data_collection 'APEX2 (Bruker, 2014)' _computing_data_reduction 'SAINT (Bruker, 2014)' _computing_molecular_graphics 'Mercury (Macrae et al., 2008)' _computing_publication_material 'Mercury (Macrae et al., 2008)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXTS (Sheldrick, 2015)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.964 _diffrn_measured_fraction_theta_max 0.777 _diffrn_measurement_device_type 'Bruker kappa, Photon 100 CMOS' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_unetI/netI 0.0312 _diffrn_reflns_Laue_measured_fraction_full 0.964 _diffrn_reflns_Laue_measured_fraction_max 0.777 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 20554 _diffrn_reflns_point_group_measured_fraction_full 0.964 _diffrn_reflns_point_group_measured_fraction_max 0.777 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.866 _diffrn_reflns_theta_min 2.077 _exptl_absorpt_coefficient_mu 11.862 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.30776 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker, 2014)' _exptl_crystal_colour Colourless _exptl_crystal_density_diffrn 2.453 _exptl_crystal_description Block _exptl_crystal_F_000 1792 _exptl_crystal_size_max 0.121 _exptl_crystal_size_mid 0.104 _exptl_crystal_size_min 0.077 _refine_diff_density_max 1.393 _refine_diff_density_min -1.523 _refine_diff_density_rms 0.188 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 124 _refine_ls_number_reflns 3387 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.052 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0344 _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^)+(0.0422P)^2^+6.3540P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0802 _refine_ls_wR_factor_ref 0.0832 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2981 _reflns_number_total 3387 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ce00907j2.cif _cod_data_source_block DCsBr3 _cod_database_code 7250165 _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 hj010b_lt2_auto_a.res in Pbcn shelx.res created by SHELXL-2018/3 at 15:15:01 on 17-Feb-2025 CELL 0.71073 9.8044 9.8273 27.3662 90.000 90.000 90.000 ZERR 8.00 0.0002 0.0003 0.0007 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, 1/2 - Y, 1/2 + Z SYMM - X, Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H BR CS N UNIT 48 112 24 8 16 MERG 2 TWIN 0.00 1.00 0.00 1.00 0.00 0.00 0.00 0.00 -1.00 2 MORE -1 EADP Br1A Br1B EADP Br2A Br2B EADP Br3A Br3B EQIV $9 x, y-1, z HTAB N2 Br3A_$9 HTAB N2 Br3B_$9 HTAB N1 Br1A HTAB N1 Br1B EQIV $5 -x+3/2, y-1/2, z HTAB C4 Br2A_$5 EQIV $3 -x+1, -y+2, -z+1 HTAB C4 Br3A_$3 HTAB C4 Br3B_$3 EQIV $6 -x+1, y, -z+1/2 HTAB C2 Br1A_$6 EQIV $10 -x+1/2, y-1/2, z HTAB C2 Br1A_$10 HTAB C2 Br1B_$10 HTAB C1 Br2A_$9 HTAB C1 Br2A_$5 HTAB C1 Br2B_$5 HTAB C6 Br2B_$10 HTAB C6 Br1B_$10 HTAB C6 Br3A_$3 HTAB C6 Br3B_$3 EQIV $11 x-1/2, -y+3/2, -z+1 HTAB C5 Br3B_$11 HTAB C5 Br2A_$9 HTAB C3 Br2A HTAB C3 Br2B HTAB N2 Br3A_$9 HTAB N2 Br3B_$9 HTAB N1 Br1A HTAB N1 Br1B HTAB C4 Br2A_$5 HTAB C4 Br3A_$3 HTAB C4 Br3B_$3 HTAB C2 Br1A_$6 HTAB C2 Br1A_$10 HTAB C2 Br1B_$10 HTAB C1 Br2A_$9 HTAB C1 Br2A_$5 HTAB C1 Br2B_$5 HTAB C6 Br2B_$10 HTAB C6 Br1B_$10 HTAB C6 Br3A_$3 HTAB C6 Br3B_$3 HTAB C5 Br3B_$11 HTAB C5 Br2A_$9 HTAB C3 Br2A HTAB C3 Br2B FMAP 2 PLAN 7 ACTA BOND $H CONF LIST 4 L.S. 10 TEMP -123.00 WGHT 0.042200 6.354001 BASF 0.06442 FVAR 0.82811 0.97117 0.97954 0.97615 CS1 4 0.500000 1.009372 0.250000 10.50000 0.01669 0.01468 = 0.01703 0.00000 0.00025 0.00000 CS2 4 0.500000 1.000000 0.500000 10.50000 0.01960 0.01752 = 0.01708 0.00110 0.00101 -0.00027 N2 5 0.566862 0.432625 0.404880 11.00000 0.02499 0.02477 = 0.02406 0.00484 -0.00059 0.00304 AFIX 13 H2 2 0.614273 0.379434 0.430993 11.00000 -1.20000 AFIX 0 N1 5 0.450156 0.564324 0.340169 11.00000 0.04030 0.02769 = 0.03045 0.00404 -0.00792 0.01004 AFIX 13 H1 2 0.403383 0.618658 0.314212 11.00000 -1.20000 AFIX 0 C4 1 0.592508 0.580667 0.412855 11.00000 0.02470 0.03333 = 0.03452 -0.01398 -0.00245 -0.00417 AFIX 23 H4A 2 0.691326 0.597325 0.417274 11.00000 -1.20000 H4B 2 0.544201 0.612137 0.442544 11.00000 -1.20000 AFIX 0 C2 1 0.534034 0.456555 0.316744 11.00000 0.03370 0.02711 = 0.02555 -0.00359 0.00163 -0.00380 AFIX 23 H2A 2 0.592517 0.496779 0.291033 11.00000 -1.20000 H2B 2 0.474151 0.387603 0.301403 11.00000 -1.20000 AFIX 0 C1 1 0.621937 0.390493 0.355838 11.00000 0.02151 0.01877 = 0.03391 -0.00439 0.00226 0.00191 AFIX 23 H1A 2 0.618891 0.290217 0.352549 11.00000 -1.20000 H1B 2 0.717845 0.420497 0.352380 11.00000 -1.20000 AFIX 0 C6 1 0.346174 0.502999 0.372634 11.00000 0.01911 0.06277 = 0.04321 -0.00533 -0.00056 0.00511 AFIX 23 H6A 2 0.276979 0.454275 0.352936 11.00000 -1.20000 H6B 2 0.299539 0.575021 0.391624 11.00000 -1.20000 AFIX 0 C5 1 0.417362 0.403869 0.407203 11.00000 0.02911 0.02856 = 0.04431 0.00203 0.01434 -0.00594 AFIX 23 H5A 2 0.383472 0.416461 0.440979 11.00000 -1.20000 H5B 2 0.398949 0.308889 0.397110 11.00000 -1.20000 AFIX 0 C3 1 0.541412 0.655916 0.368984 11.00000 0.06954 0.01542 = 0.04521 -0.00361 -0.00435 -0.00704 AFIX 23 H3A 2 0.490438 0.737890 0.379407 11.00000 -1.20000 H3B 2 0.619289 0.685418 0.348539 11.00000 -1.20000 PART 1 AFIX 0 BR3A 3 0.694774 1.305766 0.502028 21.00000 0.02257 0.02001 = 0.02633 0.00261 -0.00423 -0.00299 PART 2 BR3B 3 0.724955 1.276358 0.524866 -21.00000 0.02257 0.02001 = 0.02633 0.00261 -0.00423 -0.00299 PART 1 BR2A 3 0.530864 1.035369 0.375508 31.00000 0.02641 0.02415 = 0.01676 -0.00117 -0.00085 0.00024 PART 2 BR2B 3 0.532177 0.934941 0.376037 -31.00000 0.02641 0.02415 = 0.01676 -0.00117 -0.00085 0.00024 PART 1 BR1A 3 0.273961 0.735853 0.262155 41.00000 0.01967 0.01871 = 0.03300 0.00447 -0.00361 -0.00456 PART 2 BR1B 3 0.242661 0.753423 0.279193 -41.00000 0.01967 0.01871 = 0.03300 0.00447 -0.00361 -0.00456 HKLF 4 REM hj010b_lt2_auto_a.res in Pbcn REM wR2 = 0.0832, GooF = S = 1.052, Restrained GooF = 1.052 for all data REM R1 = 0.0344 for 2981 Fo > 4sig(Fo) and 0.0429 for all 3387 data REM 124 parameters refined using 0 restraints END WGHT 0.0422 6.3540 REM Highest difference peak 1.393, deepest hole -1.523, 1-sigma level 0.188 Q1 1 0.5000 1.1116 0.2500 10.50000 0.05 1.39 Q2 1 0.5013 1.0912 0.4996 11.00000 0.05 1.26 Q3 1 0.5353 1.1375 0.3701 11.00000 0.05 1.21 Q4 1 0.5436 1.0079 0.5175 11.00000 0.05 1.05 Q5 1 0.5450 1.0012 0.2327 11.00000 0.05 1.04 Q6 1 0.5000 0.9068 0.2500 10.50000 0.05 1.00 Q7 1 0.5454 1.0035 0.2660 11.00000 0.05 0.99 ; _shelx_res_checksum 80959 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, 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 Cs1 Cs 0.500000 1.00937(4) 0.250000 0.01613(11) Uani 1 2 d S T P . . Cs2 Cs 0.500000 1.000000 0.500000 0.01807(11) Uani 1 2 d S . P . . N2 N 0.5669(4) 0.4326(4) 0.40488(14) 0.0246(9) Uani 1 1 d . . . . . H2 H 0.614273 0.379434 0.430993 0.030 Uiso 1 1 calc R U . . . N1 N 0.4502(5) 0.5643(5) 0.34017(15) 0.0328(10) Uani 1 1 d . . . . . H1 H 0.403383 0.618658 0.314212 0.039 Uiso 1 1 calc R U . . . C4 C 0.5925(5) 0.5807(6) 0.41285(18) 0.0308(12) Uani 1 1 d . . . . . H4A H 0.691326 0.597325 0.417274 0.037 Uiso 1 1 calc R U . . . H4B H 0.544201 0.612137 0.442544 0.037 Uiso 1 1 calc R U . . . C2 C 0.5340(6) 0.4566(6) 0.31674(16) 0.0288(11) Uani 1 1 d . . . . . H2A H 0.592517 0.496779 0.291033 0.035 Uiso 1 1 calc R U . . . H2B H 0.474151 0.387603 0.301403 0.035 Uiso 1 1 calc R U . . . C1 C 0.6219(5) 0.3905(5) 0.35584(17) 0.0247(10) Uani 1 1 d . . . . . H1A H 0.618891 0.290217 0.352549 0.030 Uiso 1 1 calc R U . . . H1B H 0.717845 0.420497 0.352380 0.030 Uiso 1 1 calc R U . . . C6 C 0.3462(6) 0.5030(7) 0.3726(2) 0.0417(17) Uani 1 1 d . . . . . H6A H 0.276979 0.454275 0.352936 0.050 Uiso 1 1 calc R U . . . H6B H 0.299539 0.575021 0.391624 0.050 Uiso 1 1 calc R U . . . C5 C 0.4174(5) 0.4039(6) 0.4072(2) 0.0340(12) Uani 1 1 d . . . . . H5A H 0.383472 0.416461 0.440979 0.041 Uiso 1 1 calc R U . . . H5B H 0.398949 0.308889 0.397110 0.041 Uiso 1 1 calc R U . . . C3 C 0.5414(8) 0.6559(7) 0.3690(2) 0.0434(15) Uani 1 1 d . . . . . H3A H 0.490438 0.737890 0.379407 0.052 Uiso 1 1 calc R U . . . H3B H 0.619289 0.685418 0.348539 0.052 Uiso 1 1 calc R U . . . Br3A Br 0.69477(5) 1.30577(5) 0.50203(2) 0.02297(15) Uani 0.9712(15) 1 d . . P A 1 Br3B Br 0.7250(18) 1.2764(19) 0.5249(8) 0.02297(15) Uani 0.0288(15) 1 d . . P A 2 Br2A Br 0.53086(6) 1.03537(6) 0.37551(2) 0.02244(15) Uani 0.9795(13) 1 d . . P A 1 Br2B Br 0.532(3) 0.935(3) 0.3760(7) 0.02244(15) Uani 0.0205(13) 1 d . . P A 2 Br1A Br 0.27396(9) 0.73585(7) 0.26215(5) 0.0238(2) Uani 0.976(4) 1 d . . P A 1 Br1B Br 0.243(4) 0.753(3) 0.2792(17) 0.0238(2) Uani 0.024(4) 1 d . . P A 2 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 Cs1 0.0167(2) 0.0147(3) 0.01703(19) 0.000 0.00025(12) 0.000 Cs2 0.0196(2) 0.0175(3) 0.01708(19) 0.00110(12) 0.00101(13) -0.00027(14) N2 0.025(2) 0.025(3) 0.0241(19) 0.0048(16) -0.0006(16) 0.0030(16) N1 0.040(3) 0.028(3) 0.030(2) 0.0040(18) -0.008(2) 0.010(2) C4 0.025(3) 0.033(3) 0.035(3) -0.014(2) -0.002(2) -0.004(2) C2 0.034(3) 0.027(3) 0.026(2) -0.004(2) 0.002(2) -0.004(2) C1 0.022(2) 0.019(3) 0.034(3) -0.0044(19) 0.002(2) 0.0019(19) C6 0.019(3) 0.063(5) 0.043(4) -0.005(3) -0.001(2) 0.005(3) C5 0.029(3) 0.029(3) 0.044(3) 0.002(2) 0.014(2) -0.006(2) C3 0.070(5) 0.015(3) 0.045(3) -0.004(2) -0.004(3) -0.007(3) Br3A 0.0226(3) 0.0200(3) 0.0263(3) 0.00261(19) -0.0042(2) -0.00299(19) Br3B 0.0226(3) 0.0200(3) 0.0263(3) 0.00261(19) -0.0042(2) -0.00299(19) Br2A 0.0264(2) 0.0241(4) 0.0168(2) -0.00117(16) -0.00085(17) 0.0002(2) Br2B 0.0264(2) 0.0241(4) 0.0168(2) -0.00117(16) -0.00085(17) 0.0002(2) Br1A 0.0197(3) 0.0187(3) 0.0330(5) 0.0045(2) -0.0036(3) -0.0046(2) Br1B 0.0197(3) 0.0187(3) 0.0330(5) 0.0045(2) -0.0036(3) -0.0046(2) 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -0.3680 2.1192 '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' 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 Br2A Cs1 Br2A 171.52(2) . 3_655 ? Br2A Cs1 Br1B 96.8(8) . 6_666 ? Br2A Cs1 Br1B 77.3(8) 3_655 6_666 ? Br2A Cs1 Br1B 77.3(8) . 8_665 ? Br2A Cs1 Br1B 96.8(8) 3_655 8_665 ? Br1B Cs1 Br1B 92.6(10) 6_666 8_665 ? Br2A Cs1 Br1A 91.02(2) . . ? Br2A Cs1 Br1A 95.50(2) 3_655 . ? Br2A Cs1 Br1A 95.49(2) . 3_655 ? Br2A Cs1 Br1A 91.02(2) 3_655 3_655 ? Br1A Cs1 Br1A 79.64(4) . 3_655 ? Br2A Cs1 Br1A 88.87(2) . 6_666 ? Br2A Cs1 Br1A 85.75(2) 3_655 6_666 ? Br1A Cs1 Br1A 169.20(3) . 6_666 ? Br1A Cs1 Br1A 89.623(5) 3_655 6_666 ? Br2A Cs1 Br1A 85.75(2) . 8_665 ? Br2A Cs1 Br1A 88.87(2) 3_655 8_665 ? Br1A Cs1 Br1A 89.623(5) . 8_665 ? Br1A Cs1 Br1A 169.20(3) 3_655 8_665 ? Br1A Cs1 Br1A 101.14(3) 6_666 8_665 ? Br1B Cs1 Br2B 107.8(10) 6_666 . ? Br1B Cs1 Br2B 88.8(9) 8_665 . ? Br2A Cs1 Br2B 172.3(5) . 3_655 ? Br2A Cs1 Br2B 16.2(5) 3_655 3_655 ? Br1A Cs1 Br2B 83.0(5) . 3_655 ? Br1A Cs1 Br2B 78.8(5) 3_655 3_655 ? Br1A Cs1 Br2B 96.1(5) 6_666 3_655 ? Br1A Cs1 Br2B 98.9(5) 8_665 3_655 ? Br2A Cs1 Br1B 102.0(6) . 3_655 ? Br2A Cs1 Br1B 83.9(7) 3_655 3_655 ? Br1A Cs1 Br1B 85.9(7) . 3_655 ? Br1A Cs1 Br1B 9.1(8) 3_655 3_655 ? Br1A Cs1 Br1B 83.5(6) 6_666 3_655 ? Br1A Cs1 Br1B 171.1(4) 8_665 3_655 ? Br1B Cs1 Br1B 179.3(6) 6_666 . ? Br1B Cs1 Br1B 87.2(3) 8_665 . ? Br2B Cs1 Br1B 72.9(8) . . ? Br2B Cs1 Br1B 90.5(9) 3_655 . ? Br1B Cs1 Br1B 92.9(14) 3_655 . ? Br2A Cs2 Br2A 179.999(19) 5_676 . ? Br2A Cs2 Br2B 16.4(5) 5_676 5_676 ? Br2A Cs2 Br2B 163.6(5) . 5_676 ? Br2B Cs2 Br2B 180.0(8) 5_676 . ? Br2A Cs2 Br3B 79.3(3) 5_676 8_755 ? Br2A Cs2 Br3B 100.7(3) . 8_755 ? Br2A Cs2 Br3B 100.7(3) 5_676 4_476 ? Br2A Cs2 Br3B 79.3(3) . 4_476 ? Br2A Cs2 Br3A 90.248(13) 5_676 8_755 ? Br2A Cs2 Br3A 89.752(13) . 8_755 ? Br2A Cs2 Br3A 89.752(13) 5_676 4_476 ? Br2A Cs2 Br3A 90.248(13) . 4_476 ? Br3A Cs2 Br3A 180.0 8_755 4_476 ? Br2A Cs2 Br3A 96.723(13) 5_676 . ? Br2A Cs2 Br3A 83.277(13) . . ? Br3A Cs2 Br3A 90.081(4) 8_755 . ? Br3A Cs2 Br3A 89.919(4) 4_476 . ? Br2A Cs2 Br3A 83.277(13) 5_676 5_676 ? Br2A Cs2 Br3A 96.723(13) . 5_676 ? Br3A Cs2 Br3A 89.919(4) 8_755 5_676 ? Br3A Cs2 Br3A 90.081(4) 4_476 5_676 ? Br3A Cs2 Br3A 180.0 . 5_676 ? Br2B Cs2 Br3B 74.3(6) 5_676 . ? Br2B Cs2 Br3B 105.7(6) . . ? Br3B Cs2 Br3B 88.00(14) 8_755 . ? Br3B Cs2 Br3B 92.00(14) 4_476 . ? Br2A Cs2 Br3B 93.3(3) 5_676 5_676 ? Br2A Cs2 Br3B 86.7(3) . 5_676 ? Br3A Cs2 Br3B 96.6(3) 8_755 5_676 ? Br3A Cs2 Br3B 83.4(3) 4_476 5_676 ? Br3A Cs2 Br3B 167.9(4) . 5_676 ? Br3A Cs2 Br3B 12.1(4) 5_676 5_676 ? C4 N2 C5 110.1(4) . . ? C4 N2 C1 109.8(4) . . ? C5 N2 C1 109.8(4) . . ? C4 N2 H2 109.1 . . ? C5 N2 H2 109.1 . . ? C1 N2 H2 109.1 . . ? C6 N1 C2 110.5(5) . . ? C6 N1 C3 109.9(4) . . ? C2 N1 C3 109.0(5) . . ? C6 N1 H1 109.1 . . ? C2 N1 H1 109.1 . . ? C3 N1 H1 109.1 . . ? N2 C4 C3 107.9(4) . . ? N2 C4 H4A 110.1 . . ? C3 C4 H4A 110.1 . . ? N2 C4 H4B 110.1 . . ? C3 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? N1 C2 C1 108.3(4) . . ? N1 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? N1 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? H2A C2 H2B 108.4 . . ? N2 C1 C2 107.9(4) . . ? N2 C1 H1A 110.1 . . ? C2 C1 H1A 110.1 . . ? N2 C1 H1B 110.1 . . ? C2 C1 H1B 110.1 . . ? H1A C1 H1B 108.4 . . ? N1 C6 C5 108.5(4) . . ? N1 C6 H6A 110.0 . . ? C5 C6 H6A 110.0 . . ? N1 C6 H6B 110.0 . . ? C5 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? N2 C5 C6 107.5(4) . . ? N2 C5 H5A 110.2 . . ? C6 C5 H5A 110.2 . . ? N2 C5 H5B 110.2 . . ? C6 C5 H5B 110.2 . . ? H5A C5 H5B 108.5 . . ? N1 C3 C4 109.0(5) . . ? N1 C3 H3A 109.9 . . ? C4 C3 H3A 109.9 . . ? N1 C3 H3B 109.9 . . ? C4 C3 H3B 109.9 . . ? H3A C3 H3B 108.3 . . ? Cs2 Br3A Cs2 154.905(17) 4_576 . ? Cs2 Br3B Cs2 155.0(6) 4_576 . ? Cs2 Br2A Cs1 165.761(19) . . ? Cs2 Br2B Cs1 155.1(10) . . ? Cs1 Br1A Cs1 164.632(19) . 6_556 ? Cs1 Br1B Cs1 154.1(15) 6_556 . ? 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 Cs1 Br2A 3.4574(4) . ? Cs1 Br2A 3.4575(4) 3_655 ? Cs1 Br1B 3.47(2) 6_666 ? Cs1 Br1B 3.47(2) 8_665 ? Cs1 Br1A 3.4996(6) . ? Cs1 Br1A 3.4996(6) 3_655 ? Cs1 Br1A 3.5042(6) 6_666 ? Cs1 Br1A 3.5042(6) 8_665 ? Cs1 Br2B 3.54(2) . ? Cs1 Br2B 3.54(2) 3_655 ? Cs1 Br1B 3.65(3) 3_655 ? Cs1 Br1B 3.65(3) . ? Cs2 Br2A 3.4378(4) 5_676 ? Cs2 Br2A 3.4379(4) . ? Cs2 Br2B 3.466(19) 5_676 ? Cs2 Br2B 3.467(19) . ? Cs2 Br3B 3.545(17) 8_755 ? Cs2 Br3B 3.545(17) 4_476 ? Cs2 Br3A 3.5500(5) 8_755 ? Cs2 Br3A 3.5500(5) 4_476 ? Cs2 Br3A 3.5608(5) . ? Cs2 Br3A 3.5608(5) 5_676 ? Cs2 Br3B 3.564(17) . ? Cs2 Br3B 3.564(17) 5_676 ? N2 C4 1.492(7) . ? N2 C5 1.494(7) . ? N2 C1 1.505(6) . ? N2 H2 1.0000 . ? N1 C6 1.480(7) . ? N1 C2 1.486(7) . ? N1 C3 1.494(8) . ? N1 H1 1.0000 . ? C4 C3 1.496(8) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C2 C1 1.519(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C6 C5 1.527(8) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? 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 N2 H2 Br3A^a 1.00 2.22 3.193(4) 164.1 1_545 yes N2 H2 Br3B^b 1.00 2.97 3.94(2) 165.3 1_545 yes N1 H1 Br1A^a 1.00 2.23 3.222(4) 172.4 . yes N1 H1 Br1B^b 1.00 2.27 3.22(3) 158.4 . yes C4 H4A Br2A^a 0.99 3.02 3.857(5) 143.5 8_755 yes C4 H4B Br3A^a 0.99 2.91 3.822(5) 154.3 5_676 yes C4 H4B Br3B^b 0.99 2.99 3.817(18) 141.3 5_676 yes C2 H2A Br1A^a 0.99 3.06 3.967(6) 153.2 3_655 yes C2 H2B Br1A^a 0.99 3.05 4.007(6) 163.2 8_655 yes C2 H2B Br1B^b 0.99 2.57 3.52(5) 160.1 8_655 yes C1 H1A Br2A^a 0.99 2.72 3.642(5) 154.7 1_545 yes C1 H1B Br2A^a 0.99 2.78 3.729(5) 160.0 8_755 yes C1 H1B Br2B^b 0.99 2.54 3.46(3) 155.4 8_755 yes C6 H6A Br2B^b 0.99 3.10 3.77(3) 126.0 8_655 yes C6 H6A Br1B^b 0.99 2.83 3.65(5) 140.6 8_655 yes C6 H6B Br3A^a 0.99 3.14 3.932(6) 138.2 5_676 yes C6 H6B Br3B^b 0.99 2.72 3.613(19) 149.9 5_676 yes C5 H5A Br3B^b 0.99 2.62 3.19(2) 116.2 4_466 yes C5 H5B Br2A^a 0.99 3.04 3.887(6) 144.1 1_545 yes C3 H3A Br2A^a 0.99 2.95 3.735(6) 136.7 . yes C3 H3A Br2B^b 0.99 1.98 2.75(3) 132.7 . yes N2 H2 Br3A^a 1.00 2.22 3.193(4) 164.1 1_545 yes N2 H2 Br3B^b 1.00 2.97 3.94(2) 165.3 1_545 yes N1 H1 Br1A^a 1.00 2.23 3.222(4) 172.4 . yes N1 H1 Br1B^b 1.00 2.27 3.22(3) 158.4 . yes C4 H4A Br2A^a 0.99 3.02 3.857(5) 143.5 8_755 yes C4 H4B Br3A^a 0.99 2.91 3.822(5) 154.3 5_676 yes C4 H4B Br3B^b 0.99 2.99 3.817(18) 141.3 5_676 yes C2 H2A Br1A^a 0.99 3.06 3.967(6) 153.2 3_655 yes C2 H2B Br1A^a 0.99 3.05 4.007(6) 163.2 8_655 yes C2 H2B Br1B^b 0.99 2.57 3.52(5) 160.1 8_655 yes C1 H1A Br2A^a 0.99 2.72 3.642(5) 154.7 1_545 yes C1 H1B Br2A^a 0.99 2.78 3.729(5) 160.0 8_755 yes C1 H1B Br2B^b 0.99 2.54 3.46(3) 155.4 8_755 yes C6 H6A Br2B^b 0.99 3.10 3.77(3) 126.0 8_655 yes C6 H6A Br1B^b 0.99 2.83 3.65(5) 140.6 8_655 yes C6 H6B Br3A^a 0.99 3.14 3.932(6) 138.2 5_676 yes C6 H6B Br3B^b 0.99 2.72 3.613(19) 149.9 5_676 yes C5 H5A Br3B^b 0.99 2.62 3.19(2) 116.2 4_466 yes C5 H5B Br2A^a 0.99 3.04 3.887(6) 144.1 1_545 yes C3 H3A Br2A^a 0.99 2.95 3.735(6) 136.7 . yes C3 H3A Br2B^b 0.99 1.98 2.75(3) 132.7 . 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 C5 N2 C4 C3 -69.9(5) . . . . ? C1 N2 C4 C3 51.0(6) . . . . ? C6 N1 C2 C1 -69.2(5) . . . . ? C3 N1 C2 C1 51.7(6) . . . . ? C4 N2 C1 C2 -68.9(5) . . . . ? C5 N2 C1 C2 52.2(5) . . . . ? N1 C2 C1 N2 14.2(6) . . . . ? C2 N1 C6 C5 51.7(6) . . . . ? C3 N1 C6 C5 -68.7(6) . . . . ? C4 N2 C5 C6 51.5(5) . . . . ? C1 N2 C5 C6 -69.5(5) . . . . ? N1 C6 C5 N2 15.0(6) . . . . ? C6 N1 C3 C4 50.7(7) . . . . ? C2 N1 C3 C4 -70.6(6) . . . . ? N2 C4 C3 N1 15.7(7) . . . . ?