#------------------------------------------------------------------------------ #$Date: 2024-06-01 01:12:53 +0300 (Sat, 01 Jun 2024) $ #$Revision: 292132 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/17/1571737.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_1571737 loop_ _publ_author_name 'Giri, Indrajit' 'Chhetri, Shant' 'John P., Jesslyn' 'Mondal, Madalasa' 'Dey, Arka Bikash' 'Vijayaraghavan, Ratheesh K.' _publ_section_title ; Engineered solid-state aggregates in brickwork stacks of n-type organic semiconductors: a way to achieve high electron mobility ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC02339K _journal_year 2024 _chemical_formula_moiety 'C30 H34 Br4 N2 O4' _chemical_formula_sum 'C30 H34 Br4 N2 O4' _chemical_formula_weight 806.23 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2023-11-27 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _audit_update_record ; 2024-01-08 deposited with the CCDC. 2024-05-20 downloaded from the CCDC. ; _cell_angle_alpha 92.556(3) _cell_angle_beta 99.112(4) _cell_angle_gamma 90.114(4) _cell_formula_units_Z 1 _cell_length_a 5.2191(3) _cell_length_b 9.7042(4) _cell_length_c 14.6193(6) _cell_measurement_reflns_used 5763 _cell_measurement_temperature 99.97(15) _cell_measurement_theta_max 67.8750 _cell_measurement_theta_min 3.0300 _cell_volume 730.32(6) _computing_cell_refinement 'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 99.97(15) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix3000 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -79.00 1.00 0.50 1.57 -- -40.27 108.00 169.00 160 2 \w 21.00 79.00 0.50 1.57 -- 40.27-108.00 73.00 116 3 \w -150.00 -82.00 0.50 6.27 -- -82.50-108.00 73.00 136 4 \w -83.00 -15.00 0.50 6.27 -- -82.50 108.00 169.00 136 5 \w 29.00 108.00 0.50 6.27 -- 96.35-108.00 73.00 158 6 \w 103.00 164.00 0.50 6.27 -- 96.35 108.00 169.00 122 7 \w -24.00 35.00 0.50 1.57 -- -40.27 12.00 30.00 118 8 \w -24.00 35.00 0.50 1.57 -- -40.27 12.00 -30.00 118 9 \w -110.00 -26.00 0.50 1.57 -- -40.27 -25.00-150.00 168 10 \w -31.00 30.00 0.50 1.57 -- -40.27 25.00 150.00 122 11 \w -28.00 67.00 0.50 1.57 -- 40.27 -77.00-180.00 190 12 \w -35.00 24.00 0.50 1.57 -- 40.27 -12.00 -60.00 118 13 \w 25.00 107.00 0.50 1.57 -- 40.27 38.00 -30.00 164 14 \w -150.00 -58.00 0.50 6.27 -- -82.50 -68.00 -90.00 184 15 \w -84.00 -18.00 0.50 6.27 -- -82.50 117.00 60.00 132 16 \w -156.00 -83.00 0.50 6.27 -- -82.50 -96.00-180.00 146 17 \w -47.00 -15.00 0.50 6.27 -- -82.50 42.00-150.00 64 18 \w -153.00 -68.00 0.50 6.27 -- -82.50 -25.00-150.00 170 19 \w -47.00 -15.00 0.50 6.27 -- -82.50 42.00 60.00 64 20 \w 23.00 106.00 0.50 6.27 -- 96.35 -96.00 -60.00 166 21 \w 30.00 57.00 0.50 6.27 -- 96.35 -50.00 -30.00 54 22 \w 30.00 57.00 0.50 6.27 -- 96.35 -50.00 120.00 54 23 \w 80.00 164.00 0.50 6.27 -- 96.35 42.00 150.00 168 24 \w 28.00 105.00 0.50 6.27 -- 96.35 -77.00 -60.00 154 25 \w 33.00 110.00 0.50 6.27 -- 96.35-117.00-150.00 154 26 \w 99.00 160.00 0.50 6.27 -- 96.35 117.00 30.00 122 27 \w 28.00 68.00 0.50 6.27 -- 96.35 -59.00 60.00 80 28 \w 33.00 110.00 0.50 6.27 -- 96.35-117.00-180.00 154 29 \w 30.00 57.00 0.50 6.27 -- 96.35 -50.00 150.00 54 30 \w 23.00 106.00 0.50 6.27 -- 96.35 -96.00-120.00 166 31 \w 28.00 68.00 0.50 6.27 -- 96.35 -59.00 -60.00 80 32 \w 29.00 83.00 0.50 6.27 -- 96.35 -68.00 90.00 108 33 \w 83.00 164.00 0.50 6.27 -- 96.35 33.00-120.00 162 34 \w 83.00 164.00 0.50 6.27 -- 96.35 33.00 0.00 162 35 \w 28.00 105.00 0.50 6.27 -- 96.35 -77.00 150.00 154 36 \w 30.00 57.00 0.50 6.27 -- 96.35 -50.00 30.00 54 37 \w 99.00 160.00 0.50 6.27 -- 96.35 117.00 -90.00 122 38 \w 30.00 57.00 0.50 6.27 -- 96.35 -50.00-150.00 54 39 \w 75.00 165.00 0.50 6.27 -- 96.35 59.00 90.00 180 40 \w -109.00 -13.00 0.50 1.57 -- -40.27 -77.00-120.00 192 41 \w -31.00 30.00 0.50 1.57 -- -40.27 25.00 -60.00 122 42 \w -109.00 -13.00 0.50 1.57 -- -40.27 -77.00 150.00 192 43 \w -107.00 -21.00 0.50 1.57 -- -40.27 -50.00 150.00 172 44 \w -109.00 -13.00 0.50 1.57 -- -40.27 -77.00 0.00 192 45 \w -109.00 -13.00 0.50 1.57 -- -40.27 -77.00 90.00 192 46 \w -107.00 -21.00 0.50 1.57 -- -40.27 -50.00 30.00 172 47 \w -109.00 -13.00 0.50 1.57 -- -40.27 -77.00 30.00 192 48 \w 13.00 109.00 0.50 1.57 -- 40.27 77.00 -30.00 192 49 \w 13.00 109.00 0.50 1.57 -- 40.27 77.00-120.00 192 50 \w -151.00 -92.00 0.50 6.27 -- -82.50 -77.00-180.00 118 51 \w -151.00 -55.00 0.50 6.27 -- -82.50 -77.00 -30.00 192 52 \w -151.00 -55.00 0.50 6.27 -- -82.50 -77.00 30.00 192 53 \w -151.00 -55.00 0.50 6.27 -- -82.50 -77.00-150.00 192 54 \w -151.00 -55.00 0.50 6.27 -- -82.50 -77.00 120.00 192 55 \w 72.00 164.00 0.50 6.27 -- 96.35 68.00 60.00 184 56 \w 72.00 164.00 0.50 6.27 -- 96.35 68.00-180.00 184 57 \w 75.00 165.00 0.50 6.27 -- 96.35 59.00 -60.00 180 58 \w 75.00 165.00 0.50 6.27 -- 96.35 59.00 30.00 180 59 \w 72.00 164.00 0.50 6.27 -- 96.35 68.00 -90.00 184 60 \w 70.00 165.00 0.50 6.27 -- 96.35 77.00 150.00 190 61 \w 70.00 165.00 0.50 6.27 -- 96.35 77.00-120.00 190 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix3000' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0125055000 _diffrn_orient_matrix_UB_12 -0.1468909000 _diffrn_orient_matrix_UB_13 -0.0435050000 _diffrn_orient_matrix_UB_21 -0.0071570000 _diffrn_orient_matrix_UB_22 -0.0603312000 _diffrn_orient_matrix_UB_23 0.0952747000 _diffrn_orient_matrix_UB_31 -0.2986173000 _diffrn_orient_matrix_UB_32 -0.0061649000 _diffrn_orient_matrix_UB_33 -0.0210709000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_unetI/netI 0.0206 _diffrn_reflns_Laue_measured_fraction_full 0.985 _diffrn_reflns_Laue_measured_fraction_max 0.981 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 11478 _diffrn_reflns_point_group_measured_fraction_full 0.985 _diffrn_reflns_point_group_measured_fraction_max 0.981 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 67.966 _diffrn_reflns_theta_min 3.065 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 7.049 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.65729 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light red' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.833 _exptl_crystal_description plate _exptl_crystal_F_000 400 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.713 _refine_diff_density_min -1.490 _refine_diff_density_rms 0.222 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.454 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 193 _refine_ls_number_reflns 2618 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.457 _refine_ls_R_factor_all 0.1043 _refine_ls_R_factor_gt 0.0953 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2924 _refine_ls_wR_factor_ref 0.3137 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2216 _reflns_number_total 2618 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc02339k2.cif _cod_data_source_block test3 _cod_database_code 1571737 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C30 H34 N4 O2 Br4' _chemical_oxdiff_usercomment 100K _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_max 0.539 _shelx_estimated_absorpt_t_min 0.333 _olex2_refinement_description ; 1. Rigid bond restraints C00A, Br02 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 2. Others Sof(H00K)=Sof(H00L)=Sof(H00M)=Sof(C0)=1-FVAR(1) Sof(H00H)=Sof(H00I)=Sof(H00J)=Sof(C1)=FVAR(1) 3.a Ternary CH refined with riding coordinates: C00G(H00G) 3.b Secondary CH2 refined with riding coordinates: C00D(H00A,H00B), C00E(H00C,H00D), C00F(H00E,H00F), C00I(H00N,H00O), C0(H0A,H0B) 3.c Idealised Me refined as rotating group: C00H(H00K,H00L,H00M), C00H(H00H,H00I,H00J), C00J(H00P,H00Q,H00R) ; _shelx_res_file ; TITL test3_a.res in P-1 test3.res created by SHELXL-2018/3 at 19:34:15 on 27-Nov-2023 REM Old TITL Test3 in P-1 REM SHELXT solution in P-1: R1 0.170, Rweak 0.008, Alpha 0.062 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C15 N O2 Br2 CELL 1.54184 5.2191 9.7042 14.6193 92.556 99.112 90.114 ZERR 1 0.0003 0.0004 0.0006 0.003 0.004 0.004 LATT 1 SFAC C H Br N O UNIT 30 34 4 2 4 DELU C00A Br02 L.S. 30 PLAN 5 SIZE 0.1 0.2 0.2 TEMP -173 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta OMIT -2 0 6 OMIT 0 -1 1 OMIT 0 2 5 OMIT 0 3 6 REM REM REM WGHT 0.200000 FVAR 0.39686 0.30861 BR01 3 0.005349 -0.332016 0.568413 11.00000 0.07751 0.05746 = 0.05835 -0.00028 0.00708 -0.00654 BR02 3 -0.023775 -0.074134 0.698904 11.00000 0.08560 0.10229 = 0.07246 0.00020 0.01051 0.00034 N003 4 0.444899 0.294669 0.646133 11.00000 0.06083 0.05015 = 0.04663 -0.01965 0.00167 0.00824 O004 5 0.116695 0.193954 0.703061 11.00000 0.07217 0.10448 = 0.10600 -0.06685 0.03386 -0.02223 C005 1 0.512089 -0.059875 0.472877 11.00000 0.04724 0.03889 = 0.03612 -0.00951 -0.00093 0.00337 O006 5 0.746501 0.404710 0.584831 11.00000 0.19785 0.05684 = 0.10882 -0.04211 0.08771 -0.05341 C007 1 0.316024 0.059363 0.595930 11.00000 0.04476 0.04683 = 0.03636 -0.01096 -0.00006 0.00046 C008 1 0.204873 -0.178960 0.549154 11.00000 0.05238 0.03656 = 0.04377 -0.00095 -0.00559 -0.00792 C009 1 0.362752 -0.180271 0.481262 11.00000 0.05180 0.03729 = 0.03907 -0.00826 0.00115 -0.00161 C00A 1 0.185128 -0.060466 0.606043 11.00000 0.04423 0.05096 = 0.04149 -0.00102 0.00265 0.00015 C00B 1 0.619874 0.300869 0.582626 11.00000 0.07622 0.04154 = 0.05592 -0.01548 0.01145 -0.00561 C00C 1 0.288465 0.186498 0.650974 11.00000 0.05514 0.05512 = 0.05485 -0.02216 0.00041 -0.00366 C00D 1 0.423152 0.422571 0.705474 11.00000 0.06704 0.04968 = 0.06221 -0.03203 0.00426 0.00013 AFIX 23 H00A 2 0.245433 0.427723 0.720992 11.00000 -1.20000 H00B 2 0.450819 0.504196 0.669825 11.00000 -1.20000 AFIX 0 C00E 1 0.594081 0.688681 0.827065 11.00000 0.08113 0.06261 = 0.08473 -0.03202 0.00179 0.00400 AFIX 23 H00C 2 0.497143 0.698589 0.763818 11.00000 -1.20000 H00D 2 0.781063 0.701187 0.824482 11.00000 -1.20000 AFIX 0 C00F 1 0.505819 0.802775 0.893990 11.00000 0.10797 0.06831 = 0.06740 -0.02427 0.00286 0.01503 AFIX 23 H00E 2 0.313920 0.804111 0.886061 11.00000 -1.20000 H00F 2 0.572036 0.781258 0.958994 11.00000 -1.20000 AFIX 0 C00G 1 0.615482 0.427174 0.793810 11.00000 0.16778 0.05890 = 0.06401 -0.03678 -0.01844 0.03645 PART 2 AFIX 13 H00G 2 0.785923 0.451327 0.775343 11.00000 -1.20000 AFIX 0 PART 0 C00H 1 0.895777 0.308892 0.922657 11.00000 0.06317 0.11754 = 0.05696 -0.00834 -0.00301 0.00215 PART 2 AFIX 137 H00K 2 1.052940 0.323941 0.895449 -21.00000 -1.50000 H00L 2 0.913074 0.223816 0.956716 -21.00000 -1.50000 H00M 2 0.871818 0.386974 0.965246 -21.00000 -1.50000 AFIX 137 PART 1 H00H 2 1.083241 0.294774 0.927546 21.00000 -1.50000 H00I 2 0.808575 0.219882 0.924998 21.00000 -1.50000 H00J 2 0.860658 0.370111 0.974283 21.00000 -1.50000 AFIX 0 PART 0 C00I 1 0.549746 0.550982 0.857245 11.00000 0.15949 0.06239 = 0.05839 -0.03020 0.00199 0.01411 AFIX 23 H00N 2 0.364600 0.543013 0.864004 11.00000 -1.20000 H00O 2 0.653268 0.541980 0.919529 11.00000 -1.20000 AFIX 0 C00J 1 0.608404 0.946105 0.873952 11.00000 0.13502 0.06953 = 0.11201 -0.04470 0.01484 0.00475 AFIX 137 H00P 2 0.557691 0.963330 0.808034 11.00000 -1.50000 H00Q 2 0.798043 0.948541 0.889696 11.00000 -1.50000 H00R 2 0.534504 1.017300 0.911423 11.00000 -1.50000 AFIX 0 PART 2 C0 1 0.662332 0.296396 0.845971 -21.00000 0.05296 0.06729 = 0.05397 -0.02138 0.00351 -0.00397 AFIX 23 H0A 2 0.690198 0.219412 0.801978 11.00000 -1.20000 H0B 2 0.506253 0.274174 0.873322 11.00000 -1.20000 AFIX 0 PART 1 C1 1 0.781782 0.382224 0.819671 21.00000 0.09934 0.04604 = 0.04298 -0.01822 0.01589 0.00680 HKLF 4 REM test3_a.res in P-1 REM wR2 = 0.3137, GooF = S = 1.454, Restrained GooF = 1.457 for all data REM R1 = 0.0953 for 2216 Fo > 4sig(Fo) and 0.1043 for all 2618 data REM 193 parameters refined using 1 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 1.713, deepest hole -1.490, 1-sigma level 0.222 Q1 1 0.0638 -0.0594 0.6394 11.00000 0.05 1.71 Q2 1 0.1168 -0.2649 0.5583 11.00000 0.05 1.52 Q3 1 0.1563 -0.3792 0.6023 11.00000 0.05 1.48 Q4 1 -0.1424 -0.2992 0.5269 11.00000 0.05 1.23 Q5 1 0.0052 -0.1631 0.6777 11.00000 0.05 1.20 ; _shelx_res_checksum 5940 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.429 _oxdiff_exptl_absorpt_empirical_full_min 0.730 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -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 Br01 Br 0.00535(17) -0.33202(9) 0.56841(5) 0.0649(5) Uani 1 1 d . . . . . Br02 Br -0.0238(2) -0.07413(14) 0.69890(8) 0.0871(5) Uani 1 1 d . U . . . N003 N 0.4449(13) 0.2947(6) 0.6461(4) 0.0539(15) Uani 1 1 d . . . . . O004 O 0.1167(14) 0.1940(9) 0.7031(6) 0.094(3) Uani 1 1 d . . . . . C005 C 0.5121(13) -0.0599(7) 0.4729(4) 0.0419(13) Uani 1 1 d . . . . . O006 O 0.747(2) 0.4047(8) 0.5848(6) 0.116(3) Uani 1 1 d . . . . . C007 C 0.3160(12) 0.0594(7) 0.5959(4) 0.0437(14) Uani 1 1 d . . . . . C008 C 0.2049(13) -0.1790(6) 0.5492(4) 0.0458(14) Uani 1 1 d . . . . . C009 C 0.3628(13) -0.1803(6) 0.4813(4) 0.0437(14) Uani 1 1 d . . . . . C00A C 0.1851(13) -0.0605(7) 0.6060(4) 0.0461(14) Uani 1 1 d . U . . . C00B C 0.6199(17) 0.3009(8) 0.5826(5) 0.0583(18) Uani 1 1 d . . . . . C00C C 0.2885(15) 0.1865(8) 0.6510(5) 0.0567(18) Uani 1 1 d . . . . . C00D C 0.4232(16) 0.4226(8) 0.7055(6) 0.0613(19) Uani 1 1 d . . . . . H00A H 0.245433 0.427723 0.720992 0.074 Uiso 1 1 calc R U . . . H00B H 0.450819 0.504196 0.669825 0.074 Uiso 1 1 calc R U . . . C00E C 0.594(2) 0.6887(10) 0.8271(7) 0.078(3) Uani 1 1 d . . . . . H00C H 0.497143 0.698589 0.763818 0.094 Uiso 1 1 calc R U . . . H00D H 0.781063 0.701187 0.824482 0.094 Uiso 1 1 calc R U . . . C00F C 0.506(2) 0.8028(11) 0.8940(7) 0.083(3) Uani 1 1 d . . . . . H00E H 0.313920 0.804111 0.886061 0.100 Uiso 1 1 calc R U . . . H00F H 0.572036 0.781258 0.958994 0.100 Uiso 1 1 calc R U . . . C00G C 0.615(3) 0.4272(11) 0.7938(7) 0.102(4) Uani 1 1 d . . . . . H00G H 0.785923 0.451327 0.775343 0.122 Uiso 1 1 calc R U . A 2 C00H C 0.8958(19) 0.3089(13) 0.9227(6) 0.081(3) Uani 1 1 d . . . . . H00K H 1.052940 0.323941 0.895449 0.121 Uiso 0.69(3) 1 calc R U P B 2 H00L H 0.913074 0.223816 0.956716 0.121 Uiso 0.69(3) 1 calc R U P B 2 H00M H 0.871818 0.386974 0.965246 0.121 Uiso 0.69(3) 1 calc R U P B 2 H00H H 1.083241 0.294774 0.927546 0.121 Uiso 0.31(3) 1 calc R U P B 1 H00I H 0.808575 0.219882 0.924998 0.121 Uiso 0.31(3) 1 calc R U P B 1 H00J H 0.860658 0.370111 0.974283 0.121 Uiso 0.31(3) 1 calc R U P B 1 C00I C 0.550(3) 0.5510(11) 0.8572(7) 0.096(4) Uani 1 1 d . . . . . H00N H 0.364600 0.543013 0.864004 0.115 Uiso 1 1 calc R U . . . H00O H 0.653268 0.541980 0.919529 0.115 Uiso 1 1 calc R U . . . C00J C 0.608(3) 0.9461(13) 0.8740(10) 0.108(4) Uani 1 1 d . . . . . H00P H 0.557691 0.963330 0.808034 0.161 Uiso 1 1 calc R U . . . H00Q H 0.798043 0.948541 0.889696 0.161 Uiso 1 1 calc R U . . . H00R H 0.534504 1.017300 0.911423 0.161 Uiso 1 1 calc R U . . . C0 C 0.662(2) 0.2964(13) 0.8460(8) 0.059(4) Uani 0.69(3) 1 d . . P B 2 H0A H 0.690198 0.219412 0.801978 0.071 Uiso 1 1 calc R U . B 2 H0B H 0.506253 0.274174 0.873322 0.071 Uiso 1 1 calc R U . B 2 C1 C 0.782(7) 0.382(3) 0.8197(17) 0.063(10) Uani 0.31(3) 1 d . . P B 1 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 Br01 0.0775(7) 0.0575(6) 0.0584(6) -0.0003(4) 0.0071(4) -0.0065(4) Br02 0.0856(9) 0.1023(10) 0.0725(8) 0.0002(6) 0.0105(6) 0.0003(6) N003 0.061(3) 0.050(3) 0.047(3) -0.020(2) 0.002(3) 0.008(3) O004 0.072(4) 0.104(5) 0.106(5) -0.067(4) 0.034(4) -0.022(4) C005 0.047(3) 0.039(3) 0.036(3) -0.010(2) -0.001(2) 0.003(2) O006 0.198(9) 0.057(4) 0.109(5) -0.042(4) 0.088(6) -0.053(5) C007 0.045(3) 0.047(3) 0.036(3) -0.011(2) 0.000(2) 0.000(3) C008 0.052(4) 0.037(3) 0.044(3) -0.001(2) -0.006(3) -0.008(3) C009 0.052(3) 0.037(3) 0.039(3) -0.008(2) 0.001(3) -0.002(3) C00A 0.044(3) 0.051(3) 0.041(3) -0.001(3) 0.003(2) 0.000(3) C00B 0.076(5) 0.042(4) 0.056(4) -0.015(3) 0.011(4) -0.006(3) C00C 0.055(4) 0.055(4) 0.055(4) -0.022(3) 0.000(3) -0.004(3) C00D 0.067(4) 0.050(4) 0.062(4) -0.032(3) 0.004(3) 0.000(3) C00E 0.081(6) 0.063(5) 0.085(6) -0.032(5) 0.002(5) 0.004(4) C00F 0.108(8) 0.068(6) 0.067(5) -0.024(4) 0.003(5) 0.015(5) C00G 0.168(12) 0.059(5) 0.064(5) -0.037(4) -0.018(7) 0.036(7) C00H 0.063(5) 0.118(8) 0.057(4) -0.008(5) -0.003(4) 0.002(5) C00I 0.159(11) 0.062(5) 0.058(5) -0.030(4) 0.002(6) 0.014(6) C00J 0.135(10) 0.070(6) 0.112(9) -0.045(6) 0.015(8) 0.005(7) C0 0.053(6) 0.067(8) 0.054(6) -0.021(5) 0.004(4) -0.004(5) C1 0.10(2) 0.046(15) 0.043(12) -0.018(10) 0.016(13) 0.007(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.0031 0 0 1 0.0411 0 -2 -1 0.0345 0 2 1 0.0345 1 0 0 0.1068 -1 0 -2 0.0612 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 C00B N003 C00D 116.2(7) . . ? C00C N003 C00B 123.8(6) . . ? C00C N003 C00D 119.8(6) . . ? C005 C005 C007 119.2(8) 2_656 2_656 ? C005 C005 C009 121.1(8) 2_656 . ? C009 C005 C007 119.6(6) . 2_656 ? C005 C007 C00C 118.6(6) 2_656 . ? C00A C007 C005 118.4(6) . 2_656 ? C00A C007 C00C 122.9(6) . . ? C009 C008 Br01 122.2(5) . . ? C009 C008 C00A 121.0(6) . . ? C00A C008 Br01 116.8(5) . . ? C005 C009 C00B 119.1(6) . 2_656 ? C008 C009 C005 118.3(6) . . ? C008 C009 C00B 122.6(6) . 2_656 ? C007 C00A Br02 121.3(5) . . ? C007 C00A C008 121.8(6) . . ? C008 C00A Br02 116.9(5) . . ? N003 C00B C009 118.3(7) . 2_656 ? O006 C00B N003 117.0(7) . . ? O006 C00B C009 124.6(8) . 2_656 ? N003 C00C C007 120.0(7) . . ? O004 C00C N003 120.2(7) . . ? O004 C00C C007 119.8(7) . . ? N003 C00D H00A 109.0 . . ? N003 C00D H00B 109.0 . . ? N003 C00D C00G 112.8(7) . . ? H00A C00D H00B 107.8 . . ? C00G C00D H00A 109.0 . . ? C00G C00D H00B 109.0 . . ? H00C C00E H00D 108.0 . . ? C00F C00E H00C 109.3 . . ? C00F C00E H00D 109.3 . . ? C00I C00E H00C 109.3 . . ? C00I C00E H00D 109.3 . . ? C00I C00E C00F 111.6(9) . . ? C00E C00F H00E 109.5 . . ? C00E C00F H00F 109.5 . . ? H00E C00F H00F 108.1 . . ? C00J C00F C00E 110.8(9) . . ? C00J C00F H00E 109.5 . . ? C00J C00F H00F 109.5 . . ? C00D C00G H00G 105.5 . . ? C00D C00G C00I 108.8(10) . . ? C00D C00G C0 118.3(10) . . ? C00I C00G H00G 105.5 . . ? C0 C00G H00G 105.5 . . ? C0 C00G C00I 112.1(9) . . ? C1 C00G C00D 138.6(15) . . ? C1 C00G C00I 112.0(16) . . ? H00K C00H H00L 109.5 . . ? H00K C00H H00M 109.5 . . ? H00L C00H H00M 109.5 . . ? H00H C00H H00I 109.5 . . ? H00H C00H H00J 109.5 . . ? H00I C00H H00J 109.5 . . ? C0 C00H H00K 109.5 . . ? C0 C00H H00L 109.5 . . ? C0 C00H H00M 109.5 . . ? C1 C00H H00H 109.5 . . ? C1 C00H H00I 109.5 . . ? C1 C00H H00J 109.5 . . ? C00E C00I C00G 117.0(10) . . ? C00E C00I H00N 108.1 . . ? C00E C00I H00O 108.1 . . ? C00G C00I H00N 108.1 . . ? C00G C00I H00O 108.1 . . ? H00N C00I H00O 107.3 . . ? C00F C00J H00P 109.5 . . ? C00F C00J H00Q 109.5 . . ? C00F C00J H00R 109.5 . . ? H00P C00J H00Q 109.5 . . ? H00P C00J H00R 109.5 . . ? H00Q C00J H00R 109.5 . . ? C00G C0 C00H 112.3(11) . . ? C00G C0 H0A 109.1 . . ? C00G C0 H0B 109.1 . . ? C00H C0 H0A 109.1 . . ? C00H C0 H0B 109.1 . . ? H0A C0 H0B 107.9 . . ? C00G C1 C00H 134(2) . . ? 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 Br01 C008 1.869(6) . ? Br02 C00A 1.880(7) . ? N003 C00B 1.405(10) . ? N003 C00C 1.340(11) . ? N003 C00D 1.497(8) . ? O004 C00C 1.265(10) . ? C005 C005 1.395(12) 2_656 ? C005 C007 1.450(10) 2_656 ? C005 C009 1.424(10) . ? O006 C00B 1.200(12) . ? C007 C00A 1.373(10) . ? C007 C00C 1.463(9) . ? C008 C009 1.386(10) . ? C008 C00A 1.402(10) . ? C009 C00B 1.476(9) 2_656 ? C00D H00A 0.9900 . ? C00D H00B 0.9900 . ? C00D C00G 1.504(14) . ? C00E H00C 0.9900 . ? C00E H00D 0.9900 . ? C00E C00F 1.563(11) . ? C00E C00I 1.455(16) . ? C00F H00E 0.9900 . ? C00F H00F 0.9900 . ? C00F C00J 1.546(18) . ? C00G H00G 1.0000 . ? C00G C00I 1.557(11) . ? C00G C0 1.510(18) . ? C00G C1 1.00(3) . ? C00H H00K 0.9800 . ? C00H H00L 0.9800 . ? C00H H00M 0.9800 . ? C00H H00H 0.9800 . ? C00H H00I 0.9800 . ? C00H H00J 0.9800 . ? C00H C0 1.520(14) . ? C00H C1 1.71(3) . ? C00I H00N 0.9900 . ? C00I H00O 0.9900 . ? C00J H00P 0.9800 . ? C00J H00Q 0.9800 . ? C00J H00R 0.9800 . ? C0 H0A 0.9900 . ? C0 H0B 0.9900 . ? 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 Br01 C008 C009 C005 -178.7(5) . . . . ? Br01 C008 C009 C00B 1.7(10) . . . 2_656 ? Br01 C008 C00A Br02 3.5(7) . . . . ? Br01 C008 C00A C007 -177.8(5) . . . . ? N003 C00D C00G C00I -171.2(10) . . . . ? N003 C00D C00G C0 -41.7(15) . . . . ? N003 C00D C00G C1 18(4) . . . . ? C005 C005 C009 C008 -4.3(11) 2_656 . . . ? C005 C005 C009 C00B 175.3(8) 2_656 . . 2_656 ? C005 C007 C00A Br02 175.8(4) 2_656 . . . ? C005 C007 C00A C008 -2.9(10) 2_656 . . . ? C005 C007 C00C N003 -8.7(10) 2_656 . . . ? C005 C007 C00C O004 171.3(7) 2_656 . . . ? C007 C005 C009 C008 178.5(6) 2_656 . . . ? C007 C005 C009 C00B -1.9(9) 2_656 . . 2_656 ? C009 C008 C00A Br02 -177.4(5) . . . . ? C009 C008 C00A C007 1.3(10) . . . . ? C00A C007 C00C N003 171.7(7) . . . . ? C00A C007 C00C O004 -8.3(11) . . . . ? C00A C008 C009 C005 2.3(10) . . . . ? C00A C008 C009 C00B -177.3(6) . . . 2_656 ? C00B N003 C00C O004 -172.5(8) . . . . ? C00B N003 C00C C007 7.5(11) . . . . ? C00B N003 C00D C00G -88.7(11) . . . . ? C00C N003 C00B O006 179.0(9) . . . . ? C00C N003 C00B C009 -1.4(12) . . . 2_656 ? C00C N003 C00D C00G 96.0(10) . . . . ? C00C C007 C00A Br02 -4.6(9) . . . . ? C00C C007 C00A C008 176.7(6) . . . . ? C00D N003 C00B O006 3.9(13) . . . . ? C00D N003 C00B C009 -176.5(6) . . . 2_656 ? C00D N003 C00C O004 2.5(11) . . . . ? C00D N003 C00C C007 -177.5(6) . . . . ? C00D C00G C00I C00E -69.2(16) . . . . ? C00D C00G C0 C00H 169.0(10) . . . . ? C00D C00G C1 C00H -133(2) . . . . ? C00F C00E C00I C00G 176.8(11) . . . . ? C00I C00E C00F C00J 167.4(11) . . . . ? C00I C00G C0 C00H -63.0(15) . . . . ? C00I C00G C1 C00H 57(4) . . . . ? C0 C00G C00I C00E 158.0(12) . . . . ? C1 C00G C00I C00E 104(2) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -0.0000 0.0004 -1.0002 0.0435 -0.0953 0.0211 0.0000 -0.0004 1.0002 -0.0435 0.0953 -0.0211 -0.0010 -2.0015 -0.9984 0.3374 0.0256 0.0337 0.0010 2.0015 0.9984 -0.3374 -0.0256 -0.0337 1.0006 0.0020 0.0019 0.0121 -0.0071 -0.2988 -1.0006 -0.0011 -2.0023 0.0748 -0.1835 0.3410