#------------------------------------------------------------------------------ #$Date: 2026-05-04 14:12:18 +0100 (Mon, 04 May 2026) $ #$Revision: 305707 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/09/7720981.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_7720981 loop_ _publ_author_name 'Li, Wenjuan' 'Li, Yuanping' 'Shi, Yanting' 'Xu, Hui' 'Zhu, Linyun' 'Chen, Xinyu' 'Li, Xiaopei' 'Yan, Jianfeng' 'Liu, Lantao' 'Li, Yuanming' _publ_section_title ; One-step synthesis of 1,3- and 1,1'-diarylated ferrocenes toward main-chain metallomacrocycles. ; _journal_issue 14 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 5443 _journal_page_last 5447 _journal_paper_doi 10.1039/d6dt00371k _journal_volume 55 _journal_year 2026 _chemical_formula_moiety 'C22 H16 Br2 Fe' _chemical_formula_sum 'C22 H16 Br2 Fe' _chemical_formula_weight 496.02 _space_group_crystal_system orthorhombic _space_group_IT_number 29 _space_group_name_Hall 'P 2c -2ac' _space_group_name_H-M_alt 'P c a 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2026-01-04 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) ; _audit_update_record ; 2026-01-04 deposited with the CCDC. 2026-03-18 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.7343(6) _cell_length_b 11.0932(8) _cell_length_c 21.7094(14) _cell_measurement_reflns_used 3521 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 24.3650 _cell_measurement_theta_min 2.7360 _cell_volume 1862.6(2) _computing_cell_refinement 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _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 -95.00 -64.00 0.50 4.55 -- -9.80 20.00 22.00 62 2 \w 69.00 94.00 0.50 4.55 -- 5.00 55.00 -60.00 50 3 \w -26.00 80.00 0.50 4.55 -- -9.80 55.00-180.00 212 4 \w -99.00 -41.00 0.50 4.55 -- -9.80 55.00-180.00 116 5 \w 49.00 74.00 0.50 4.55 -- -9.80 20.00 22.00 50 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB AFC11 (RCD3): quarter-chi single' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0819855000 _diffrn_orient_matrix_UB_12 -0.0271602000 _diffrn_orient_matrix_UB_13 0.0045955000 _diffrn_orient_matrix_UB_21 -0.0410565000 _diffrn_orient_matrix_UB_22 0.0534755000 _diffrn_orient_matrix_UB_23 -0.0103460000 _diffrn_orient_matrix_UB_31 0.0015291000 _diffrn_orient_matrix_UB_32 -0.0221169000 _diffrn_orient_matrix_UB_33 -0.0306587000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_unetI/netI 0.0359 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 9495 _diffrn_reflns_point_group_measured_fraction_full 0.962 _diffrn_reflns_point_group_measured_fraction_max 0.962 _diffrn_reflns_theta_full 25.027 _diffrn_reflns_theta_max 25.027 _diffrn_reflns_theta_min 3.211 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 5.101 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.80912 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015) 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 1.769 _exptl_crystal_description block _exptl_crystal_F_000 976 _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.308 _refine_diff_density_min -0.277 _refine_diff_density_rms 0.051 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.076(14) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 227 _refine_ls_number_reflns 3162 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.024 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0294 _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^)+(0.0235P)^2^+0.4933P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.0565 _reflns_Friedel_coverage 0.871 _reflns_Friedel_fraction_full 0.924 _reflns_Friedel_fraction_max 0.924 _reflns_number_gt 2718 _reflns_number_total 3162 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00371k2.cif _cod_data_source_block xjd-tong _cod_database_code 7720981 _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_estimated_absorpt_t_max 0.905 _shelx_estimated_absorpt_t_min 0.785 _reflns_odcompleteness_completeness 99.77 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.924(14) 0.076(14) 2. Fixed Uiso At 1.2 times of: All C(H) groups 3.a Aromatic/amide H refined with riding coordinates: C006(H006), C008(H008), C00A(H00A), C00C(H00C), C00D(H00D), C00E(H00E), C00G(H00G), C00H(H00H), C00I(H00I), C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M), C00N(H00N), C00O(H00O), C00P(H00P) ; _shelx_res_file ; TITL xjd-tong_a.res in Pca2(1) xjd-tong.res created by SHELXL-2018/3 at 16:59:05 on 04-Jan-2026 REM Old TITL xjd-tong_a.res in Pca2(1) REM SHELXT solution in Pca2(1) REM R1 0.111, Rweak 0.024, Alpha 0.007, Orientation as input REM Flack x = 0.213 ( 0.058 ) from Parsons' quotients REM Formula found by SHELXT: C22 Fe Br2 CELL 0.71073 7.7343 11.0932 21.7094 90 90 90 ZERR 4 0.0006 0.0008 0.0014 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM 0.5+X,-Y,+Z SYMM 0.5-X,+Y,0.5+Z SFAC C H Br Fe UNIT 88 64 8 4 L.S. 20 0 0 PLAN 2 SIZE 0.02 0.03 0.05 CONF list 4 MORE -1 BOND $H fmap 2 53 acta SHEL 999 0.84 TWIN -1 0 0 0 -1 0 0 0 -1 2 OMIT 0 1 2 OMIT 0 1 -2 REM REM REM WGHT 0.023500 0.493300 BASF 0.07629 FVAR 0.39813 BR01 3 -0.573697 -0.473776 -0.809509 11.00000 0.05998 0.07638 = 0.05864 -0.02041 -0.00116 -0.00388 BR02 3 -0.590396 -0.119566 -0.190442 11.00000 0.07008 0.09343 = 0.04465 -0.00017 0.00786 0.00639 FE03 4 -0.235282 -0.236716 -0.509939 11.00000 0.03517 0.03999 = 0.03848 -0.00016 -0.00274 0.00307 C004 1 -0.461577 -0.256760 -0.628733 11.00000 0.03612 0.04466 = 0.04083 0.00651 -0.00595 0.00029 C005 1 -0.534642 -0.124952 -0.276006 11.00000 0.03903 0.06258 = 0.03802 -0.00267 0.00141 0.00735 C006 1 -0.496311 -0.215442 -0.512087 11.00000 0.02968 0.03985 = 0.04874 0.00220 -0.00129 -0.00024 AFIX 43 H006 2 -0.578015 -0.274844 -0.503932 11.00000 -1.20000 AFIX 0 C007 1 -0.424044 -0.189449 -0.571245 11.00000 0.03199 0.04384 = 0.04299 0.00717 -0.00409 0.00799 C008 1 -0.600422 -0.216267 -0.311388 11.00000 0.06142 0.04749 = 0.05632 0.00339 0.01622 -0.00348 AFIX 43 H008 2 -0.671007 -0.275013 -0.294019 11.00000 -1.20000 AFIX 0 C009 1 -0.530173 -0.384998 -0.736642 11.00000 0.04343 0.05292 = 0.04482 -0.00422 -0.00633 0.00529 C00A 1 -0.579882 -0.348952 -0.630450 11.00000 0.06198 0.06539 = 0.04049 0.00720 0.00024 -0.01850 AFIX 43 H00A 2 -0.637974 -0.369214 -0.594400 11.00000 -1.20000 AFIX 0 C00B 1 -0.423266 -0.135885 -0.467626 11.00000 0.03505 0.03606 = 0.04470 -0.00146 -0.00212 0.00622 C00C 1 -0.434761 -0.037130 -0.301350 11.00000 0.05879 0.07030 = 0.05276 -0.01058 0.00124 -0.01681 AFIX 43 H00C 2 -0.392530 0.025220 -0.276984 11.00000 -1.20000 AFIX 0 C00D 1 -0.396179 -0.040953 -0.363649 11.00000 0.05060 0.06191 = 0.05275 -0.00533 0.00631 -0.01627 AFIX 43 H00D 2 -0.326894 0.018672 -0.380900 11.00000 -1.20000 AFIX 0 C00E 1 -0.412313 -0.291832 -0.737297 11.00000 0.05954 0.06985 = 0.04179 -0.00143 0.00573 -0.01608 AFIX 43 H00E 2 -0.354966 -0.271411 -0.773475 11.00000 -1.20000 AFIX 0 C00F 1 -0.460153 -0.133195 -0.400644 11.00000 0.02813 0.04028 = 0.04979 -0.00242 0.00269 0.00875 C00G 1 -0.306778 -0.094036 -0.563199 11.00000 0.05302 0.04044 = 0.04437 0.00842 -0.00174 -0.00005 AFIX 43 H00G 2 -0.241564 -0.058666 -0.594323 11.00000 -1.20000 AFIX 0 C00H 1 -0.616165 -0.412771 -0.683415 11.00000 0.06856 0.06156 = 0.05419 0.00766 -0.00200 -0.02715 AFIX 43 H00H 2 -0.698221 -0.474045 -0.682960 11.00000 -1.20000 AFIX 0 C00I 1 -0.303291 -0.060031 -0.500246 11.00000 0.04538 0.03612 = 0.05103 -0.00126 0.00088 -0.00014 AFIX 43 H00I 2 -0.235511 0.000532 -0.483090 11.00000 -1.20000 AFIX 0 C00J 1 -0.068409 -0.352563 -0.550611 11.00000 0.07513 0.07679 = 0.06353 -0.00989 0.00561 0.03615 AFIX 43 H00J 2 -0.060937 -0.367965 -0.592637 11.00000 -1.20000 AFIX 0 C00K 1 -0.560023 -0.219554 -0.373382 11.00000 0.06279 0.04348 = 0.05745 -0.00703 0.01348 -0.01022 AFIX 43 H00K 2 -0.602201 -0.282594 -0.397292 11.00000 -1.20000 AFIX 0 C00L 1 -0.380522 -0.229194 -0.683482 11.00000 0.04965 0.06276 = 0.04967 -0.00364 0.00450 -0.02029 AFIX 43 H00L 2 -0.301452 -0.166051 -0.684226 11.00000 -1.20000 AFIX 0 C00M 1 -0.020795 -0.273952 -0.458816 11.00000 0.07238 0.10514 = 0.07662 -0.01510 -0.04065 0.03094 AFIX 43 H00M 2 0.025663 -0.226815 -0.427494 11.00000 -1.20000 AFIX 0 C00N 1 0.022540 -0.266597 -0.520080 11.00000 0.03588 0.09005 = 0.10904 0.00269 -0.00281 0.01293 AFIX 43 H00N 2 0.100225 -0.212453 -0.537507 11.00000 -1.20000 AFIX 0 C00O 1 -0.146020 -0.363723 -0.451103 11.00000 0.09100 0.09659 = 0.06908 0.04068 0.01403 0.04980 AFIX 43 H00O 2 -0.199643 -0.385504 -0.414411 11.00000 -1.20000 AFIX 0 C00P 1 -0.175090 -0.414479 -0.509265 11.00000 0.07175 0.03912 = 0.14287 -0.01154 -0.02239 0.01387 AFIX 43 H00P 2 -0.250587 -0.477127 -0.518589 11.00000 -1.20000 AFIX 0 HKLF 4 REM xjd-tong_a.res in Pca2(1) REM wR2 = 0.0565, GooF = S = 1.024, Restrained GooF = 1.024 for all data REM R1 = 0.0294 for 2718 Fo > 4sig(Fo) and 0.0392 for all 3162 data REM 227 parameters refined using 1 restraints END WGHT 0.0218 0.5495 REM Highest difference peak 0.308, deepest hole -0.277, 1-sigma level 0.051 Q1 1 -0.5134 -0.4037 -0.8021 11.00000 0.05 0.31 Q2 1 -0.5860 -0.5274 -0.7794 11.00000 0.05 0.29 ; _shelx_res_checksum 18421 _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 1.194 _oxdiff_exptl_absorpt_empirical_full_min 0.818 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, 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 Br01 Br -0.57370(9) -0.47378(6) -0.80951(3) 0.0650(2) Uani 1 1 d . . . . . Br02 Br -0.59040(9) -0.11957(7) -0.19044(3) 0.0694(2) Uani 1 1 d . . . . . Fe03 Fe -0.23528(9) -0.23672(6) -0.50994(4) 0.03788(19) Uani 1 1 d . . . . . C004 C -0.4616(7) -0.2568(5) -0.6287(3) 0.0405(13) Uani 1 1 d . . . . . C005 C -0.5346(7) -0.1250(6) -0.2760(3) 0.0465(14) Uani 1 1 d . . . . . C006 C -0.4963(6) -0.2154(4) -0.5121(3) 0.0394(12) Uani 1 1 d . . . . . H006 H -0.578015 -0.274844 -0.503932 0.047 Uiso 1 1 calc R U . . . C007 C -0.4240(7) -0.1894(5) -0.5712(2) 0.0396(13) Uani 1 1 d . . . . . C008 C -0.6004(8) -0.2163(5) -0.3114(3) 0.0551(16) Uani 1 1 d . . . . . H008 H -0.671007 -0.275013 -0.294019 0.066 Uiso 1 1 calc R U . . . C009 C -0.5302(8) -0.3850(5) -0.7366(3) 0.0471(15) Uani 1 1 d . . . . . C00A C -0.5799(8) -0.3490(5) -0.6305(3) 0.0560(17) Uani 1 1 d . . . . . H00A H -0.637974 -0.369214 -0.594400 0.067 Uiso 1 1 calc R U . . . C00B C -0.4233(6) -0.1359(5) -0.4676(2) 0.0386(13) Uani 1 1 d . . . . . C00C C -0.4348(8) -0.0371(6) -0.3013(3) 0.0606(17) Uani 1 1 d . . . . . H00C H -0.392530 0.025220 -0.276984 0.073 Uiso 1 1 calc R U . . . C00D C -0.3962(8) -0.0410(6) -0.3636(3) 0.0551(16) Uani 1 1 d . . . . . H00D H -0.326894 0.018672 -0.380900 0.066 Uiso 1 1 calc R U . . . C00E C -0.4123(9) -0.2918(6) -0.7373(3) 0.0571(17) Uani 1 1 d . . . . . H00E H -0.354966 -0.271411 -0.773475 0.068 Uiso 1 1 calc R U . . . C00F C -0.4602(7) -0.1332(5) -0.4006(3) 0.0394(13) Uani 1 1 d . . . . . C00G C -0.3068(7) -0.0940(5) -0.5632(3) 0.0459(15) Uani 1 1 d . . . . . H00G H -0.241564 -0.058666 -0.594323 0.055 Uiso 1 1 calc R U . . . C00H C -0.6162(9) -0.4128(6) -0.6834(3) 0.0614(17) Uani 1 1 d . . . . . H00H H -0.698221 -0.474045 -0.682960 0.074 Uiso 1 1 calc R U . . . C00I C -0.3033(7) -0.0600(4) -0.5002(3) 0.0442(14) Uani 1 1 d . . . . . H00I H -0.235511 0.000532 -0.483090 0.053 Uiso 1 1 calc R U . . . C00J C -0.0684(11) -0.3526(7) -0.5506(3) 0.072(2) Uani 1 1 d . . . . . H00J H -0.060937 -0.367965 -0.592637 0.086 Uiso 1 1 calc R U . . . C00K C -0.5600(9) -0.2196(5) -0.3734(3) 0.0546(16) Uani 1 1 d . . . . . H00K H -0.602201 -0.282594 -0.397292 0.065 Uiso 1 1 calc R U . . . C00L C -0.3805(8) -0.2292(5) -0.6835(3) 0.0540(15) Uani 1 1 d . . . . . H00L H -0.301452 -0.166051 -0.684226 0.065 Uiso 1 1 calc R U . . . C00M C -0.0208(12) -0.2740(9) -0.4588(4) 0.085(3) Uani 1 1 d . . . . . H00M H 0.025663 -0.226815 -0.427494 0.102 Uiso 1 1 calc R U . . . C00N C 0.0225(9) -0.2666(7) -0.5201(5) 0.078(2) Uani 1 1 d . . . . . H00N H 0.100225 -0.212453 -0.537507 0.094 Uiso 1 1 calc R U . . . C00O C -0.1460(12) -0.3637(9) -0.4511(4) 0.086(3) Uani 1 1 d . . . . . H00O H -0.199643 -0.385504 -0.414411 0.103 Uiso 1 1 calc R U . . . C00P C -0.1751(10) -0.4145(6) -0.5093(5) 0.085(2) Uani 1 1 d . . . . . H00P H -0.250587 -0.477127 -0.518589 0.101 Uiso 1 1 calc R 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 Br01 0.0600(4) 0.0764(4) 0.0586(4) -0.0204(4) -0.0012(4) -0.0039(3) Br02 0.0701(5) 0.0934(5) 0.0446(3) -0.0002(3) 0.0079(4) 0.0064(4) Fe03 0.0352(4) 0.0400(4) 0.0385(4) -0.0002(4) -0.0027(4) 0.0031(3) C004 0.036(3) 0.045(3) 0.041(3) 0.007(3) -0.006(3) 0.000(3) C005 0.039(3) 0.063(4) 0.038(3) -0.003(3) 0.001(3) 0.007(3) C006 0.030(3) 0.040(3) 0.049(3) 0.002(3) -0.001(3) 0.000(2) C007 0.032(3) 0.044(3) 0.043(3) 0.007(3) -0.004(3) 0.008(2) C008 0.061(4) 0.047(3) 0.056(4) 0.003(3) 0.016(4) -0.003(3) C009 0.043(4) 0.053(4) 0.045(3) -0.004(3) -0.006(3) 0.005(3) C00A 0.062(4) 0.065(4) 0.040(3) 0.007(3) 0.000(3) -0.019(3) C00B 0.035(3) 0.036(3) 0.045(3) -0.001(2) -0.002(3) 0.006(3) C00C 0.059(4) 0.070(4) 0.053(4) -0.011(3) 0.001(4) -0.017(3) C00D 0.051(4) 0.062(4) 0.053(4) -0.005(3) 0.006(3) -0.016(3) C00E 0.060(4) 0.070(4) 0.042(3) -0.001(3) 0.006(3) -0.016(3) C00F 0.028(3) 0.040(3) 0.050(3) -0.002(3) 0.003(2) 0.009(2) C00G 0.053(4) 0.040(3) 0.044(3) 0.008(3) -0.002(3) 0.000(3) C00H 0.069(4) 0.062(4) 0.054(4) 0.008(4) -0.002(3) -0.027(3) C00I 0.045(3) 0.036(3) 0.051(4) -0.001(3) 0.001(3) 0.000(2) C00J 0.075(5) 0.077(5) 0.064(5) -0.010(4) 0.006(4) 0.036(5) C00K 0.063(4) 0.043(3) 0.057(4) -0.007(3) 0.013(3) -0.010(3) C00L 0.050(4) 0.063(4) 0.050(4) -0.004(3) 0.004(3) -0.020(3) C00M 0.072(6) 0.105(7) 0.077(6) -0.015(5) -0.041(5) 0.031(5) C00N 0.036(4) 0.090(5) 0.109(8) 0.003(5) -0.003(4) 0.013(4) C00O 0.091(7) 0.097(6) 0.069(6) 0.041(5) 0.014(5) 0.050(6) C00P 0.072(5) 0.039(3) 0.143(8) -0.012(5) -0.022(6) 0.014(3) 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' Fe Fe 0.3463 0.8444 '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 C006 Fe03 C007 41.1(2) . . ? C006 Fe03 C00B 40.8(2) . . ? C006 Fe03 C00G 68.1(2) . . ? C006 Fe03 C00I 68.6(2) . . ? C006 Fe03 C00M 147.6(4) . . ? C006 Fe03 C00N 172.0(3) . . ? C007 Fe03 C00B 69.2(2) . . ? C00G Fe03 C007 40.3(2) . . ? C00G Fe03 C00B 68.8(2) . . ? C00G Fe03 C00I 40.7(2) . . ? C00G Fe03 C00M 133.4(4) . . ? C00I Fe03 C007 68.7(2) . . ? C00I Fe03 C00B 41.2(2) . . ? C00J Fe03 C006 134.2(3) . . ? C00J Fe03 C007 109.5(3) . . ? C00J Fe03 C00B 173.4(3) . . ? C00J Fe03 C00G 114.8(3) . . ? C00J Fe03 C00I 145.0(3) . . ? C00J Fe03 C00M 65.8(3) . . ? C00J Fe03 C00N 39.1(3) . . ? C00J Fe03 C00P 40.4(3) . . ? C00M Fe03 C007 171.1(4) . . ? C00M Fe03 C00B 116.3(3) . . ? C00M Fe03 C00I 110.4(3) . . ? C00N Fe03 C007 132.2(3) . . ? C00N Fe03 C00B 146.3(3) . . ? C00N Fe03 C00G 109.4(3) . . ? C00N Fe03 C00I 114.9(3) . . ? C00N Fe03 C00M 39.4(4) . . ? C00O Fe03 C006 115.7(3) . . ? C00O Fe03 C007 146.5(4) . . ? C00O Fe03 C00B 109.8(3) . . ? C00O Fe03 C00G 172.9(4) . . ? C00O Fe03 C00I 133.8(3) . . ? C00O Fe03 C00J 67.4(3) . . ? C00O Fe03 C00M 40.3(4) . . ? C00O Fe03 C00N 67.7(3) . . ? C00O Fe03 C00P 40.5(3) . . ? C00P Fe03 C006 110.0(3) . . ? C00P Fe03 C007 114.7(3) . . ? C00P Fe03 C00B 133.6(3) . . ? C00P Fe03 C00G 145.4(4) . . ? C00P Fe03 C00I 173.4(4) . . ? C00P Fe03 C00M 67.2(3) . . ? C00P Fe03 C00N 67.5(3) . . ? C00A C004 C007 121.9(5) . . ? C00A C004 C00L 116.4(5) . . ? C00L C004 C007 121.7(5) . . ? C008 C005 Br02 119.0(5) . . ? C00C C005 Br02 120.0(5) . . ? C00C C005 C008 120.9(6) . . ? Fe03 C006 H006 126.0 . . ? C007 C006 Fe03 69.9(3) . . ? C007 C006 H006 125.4 . . ? C00B C006 Fe03 70.3(3) . . ? C00B C006 H006 125.4 . . ? C00B C006 C007 109.2(5) . . ? C004 C007 Fe03 124.0(4) . . ? C006 C007 Fe03 69.1(3) . . ? C006 C007 C004 125.3(5) . . ? C00G C007 Fe03 69.6(3) . . ? C00G C007 C004 127.6(5) . . ? C00G C007 C006 107.0(5) . . ? C005 C008 H008 120.6 . . ? C005 C008 C00K 118.8(6) . . ? C00K C008 H008 120.6 . . ? C00E C009 Br01 119.9(5) . . ? C00H C009 Br01 120.1(5) . . ? C00H C009 C00E 119.9(6) . . ? C004 C00A H00A 118.6 . . ? C004 C00A C00H 122.7(6) . . ? C00H C00A H00A 118.6 . . ? C006 C00B Fe03 68.9(3) . . ? C006 C00B C00F 126.9(5) . . ? C006 C00B C00I 106.5(4) . . ? C00F C00B Fe03 125.9(4) . . ? C00I C00B Fe03 69.0(3) . . ? C00I C00B C00F 126.5(5) . . ? C005 C00C H00C 120.2 . . ? C005 C00C C00D 119.7(6) . . ? C00D C00C H00C 120.2 . . ? C00C C00D H00D 119.7 . . ? C00C C00D C00F 120.6(6) . . ? C00F C00D H00D 119.7 . . ? C009 C00E H00E 120.5 . . ? C009 C00E C00L 119.1(6) . . ? C00L C00E H00E 120.5 . . ? C00D C00F C00B 120.8(5) . . ? C00K C00F C00B 121.3(5) . . ? C00K C00F C00D 117.8(5) . . ? Fe03 C00G H00G 126.4 . . ? C007 C00G Fe03 70.1(3) . . ? C007 C00G H00G 125.3 . . ? C007 C00G C00I 109.4(5) . . ? C00I C00G Fe03 69.8(3) . . ? C00I C00G H00G 125.3 . . ? C009 C00H C00A 119.3(6) . . ? C009 C00H H00H 120.3 . . ? C00A C00H H00H 120.3 . . ? Fe03 C00I H00I 126.2 . . ? C00B C00I Fe03 69.8(3) . . ? C00B C00I H00I 126.1 . . ? C00G C00I Fe03 69.5(3) . . ? C00G C00I C00B 107.8(5) . . ? C00G C00I H00I 126.1 . . ? Fe03 C00J H00J 125.7 . . ? C00N C00J Fe03 70.8(4) . . ? C00N C00J H00J 125.2 . . ? C00N C00J C00P 109.7(7) . . ? C00P C00J Fe03 69.9(4) . . ? C00P C00J H00J 125.2 . . ? C008 C00K H00K 118.9 . . ? C00F C00K C008 122.1(6) . . ? C00F C00K H00K 118.9 . . ? C004 C00L C00E 122.5(5) . . ? C004 C00L H00L 118.8 . . ? C00E C00L H00L 118.8 . . ? Fe03 C00M H00M 126.8 . . ? C00N C00M Fe03 70.1(4) . . ? C00N C00M H00M 125.5 . . ? C00N C00M C00O 109.1(7) . . ? C00O C00M Fe03 69.3(4) . . ? C00O C00M H00M 125.5 . . ? Fe03 C00N H00N 124.9 . . ? C00J C00N Fe03 70.1(4) . . ? C00J C00N C00M 107.7(8) . . ? C00J C00N H00N 126.1 . . ? C00M C00N Fe03 70.5(4) . . ? C00M C00N H00N 126.1 . . ? Fe03 C00O H00O 124.7 . . ? C00M C00O Fe03 70.4(4) . . ? C00M C00O H00O 126.6 . . ? C00M C00O C00P 106.8(7) . . ? C00P C00O Fe03 69.9(4) . . ? C00P C00O H00O 126.6 . . ? Fe03 C00P H00P 125.6 . . ? C00J C00P Fe03 69.7(4) . . ? C00J C00P C00O 106.6(7) . . ? C00J C00P H00P 126.7 . . ? C00O C00P Fe03 69.6(4) . . ? C00O C00P H00P 126.7 . . ? 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 C009 1.894(6) . ? Br02 C005 1.908(6) . ? Fe03 C006 2.033(5) . ? Fe03 C007 2.044(5) . ? Fe03 C00B 2.052(5) . ? Fe03 C00G 2.037(5) . ? Fe03 C00I 2.040(5) . ? Fe03 C00J 2.024(6) . ? Fe03 C00M 2.038(7) . ? Fe03 C00N 2.033(7) . ? Fe03 C00O 2.023(6) . ? Fe03 C00P 2.026(6) . ? C004 C007 1.483(8) . ? C004 C00A 1.373(8) . ? C004 C00L 1.378(9) . ? C005 C008 1.369(8) . ? C005 C00C 1.360(8) . ? C006 H006 0.9300 . ? C006 C007 1.430(8) . ? C006 C00B 1.425(7) . ? C007 C00G 1.405(8) . ? C008 H008 0.9300 . ? C008 C00K 1.382(9) . ? C009 C00E 1.378(8) . ? C009 C00H 1.368(9) . ? C00A H00A 0.9300 . ? C00A C00H 1.379(9) . ? C00B C00F 1.482(8) . ? C00B C00I 1.439(7) . ? C00C H00C 0.9300 . ? C00C C00D 1.386(9) . ? C00D H00D 0.9300 . ? C00D C00F 1.392(8) . ? C00E H00E 0.9300 . ? C00E C00L 1.381(9) . ? C00F C00K 1.366(8) . ? C00G H00G 0.9300 . ? C00G C00I 1.418(8) . ? C00H H00H 0.9300 . ? C00I H00I 0.9300 . ? C00J H00J 0.9300 . ? C00J C00N 1.358(10) . ? C00J C00P 1.399(12) . ? C00K H00K 0.9300 . ? C00L H00L 0.9300 . ? C00M H00M 0.9300 . ? C00M C00N 1.374(12) . ? C00M C00O 1.399(12) . ? C00N H00N 0.9300 . ? C00O H00O 0.9300 . ? C00O C00P 1.401(11) . ? C00P H00P 0.9300 . ? 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 C009 C00E C00L -179.1(5) . . . . ? Br01 C009 C00H C00A 178.5(5) . . . . ? Br02 C005 C008 C00K 179.8(5) . . . . ? Br02 C005 C00C C00D -179.4(5) . . . . ? Fe03 C006 C007 C004 117.5(5) . . . . ? Fe03 C006 C007 C00G -59.5(4) . . . . ? Fe03 C006 C00B C00F -119.8(5) . . . . ? Fe03 C006 C00B C00I 59.0(3) . . . . ? Fe03 C007 C00G C00I -58.9(4) . . . . ? Fe03 C00B C00F C00D 98.8(6) . . . . ? Fe03 C00B C00F C00K -82.3(6) . . . . ? Fe03 C00B C00I C00G 59.3(4) . . . . ? Fe03 C00G C00I C00B -59.5(4) . . . . ? Fe03 C00J C00N C00M 60.7(5) . . . . ? Fe03 C00J C00P C00O -60.2(5) . . . . ? Fe03 C00M C00N C00J -60.5(5) . . . . ? Fe03 C00M C00O C00P 60.7(5) . . . . ? Fe03 C00O C00P C00J 60.2(5) . . . . ? C004 C007 C00G Fe03 -117.8(5) . . . . ? C004 C007 C00G C00I -176.6(5) . . . . ? C004 C00A C00H C009 0.8(10) . . . . ? C005 C008 C00K C00F -1.6(10) . . . . ? C005 C00C C00D C00F 0.6(10) . . . . ? C006 C007 C00G Fe03 59.2(3) . . . . ? C006 C007 C00G C00I 0.3(6) . . . . ? C006 C00B C00F C00D -171.9(5) . . . . ? C006 C00B C00F C00K 7.0(8) . . . . ? C006 C00B C00I Fe03 -58.9(3) . . . . ? C006 C00B C00I C00G 0.4(6) . . . . ? C007 C004 C00A C00H -179.8(6) . . . . ? C007 C004 C00L C00E 179.2(6) . . . . ? C007 C006 C00B Fe03 -59.2(4) . . . . ? C007 C006 C00B C00F -179.0(5) . . . . ? C007 C006 C00B C00I -0.2(6) . . . . ? C007 C00G C00I Fe03 59.1(4) . . . . ? C007 C00G C00I C00B -0.4(6) . . . . ? C008 C005 C00C C00D -1.2(10) . . . . ? C009 C00E C00L C004 0.4(10) . . . . ? C00A C004 C007 Fe03 90.6(6) . . . . ? C00A C004 C007 C006 3.5(8) . . . . ? C00A C004 C007 C00G 179.9(5) . . . . ? C00A C004 C00L C00E -1.4(9) . . . . ? C00B C006 C007 Fe03 59.5(4) . . . . ? C00B C006 C007 C004 177.0(5) . . . . ? C00B C006 C007 C00G 0.0(6) . . . . ? C00B C00F C00K C008 -177.8(6) . . . . ? C00C C005 C008 C00K 1.6(9) . . . . ? C00C C00D C00F C00B 178.3(5) . . . . ? C00C C00D C00F C00K -0.6(9) . . . . ? C00D C00F C00K C008 1.1(9) . . . . ? C00E C009 C00H C00A -1.8(10) . . . . ? C00F C00B C00I Fe03 119.8(5) . . . . ? C00F C00B C00I C00G 179.2(5) . . . . ? C00H C009 C00E C00L 1.2(10) . . . . ? C00I C00B C00F C00D 9.6(8) . . . . ? C00I C00B C00F C00K -171.5(6) . . . . ? C00L C004 C007 Fe03 -90.0(6) . . . . ? C00L C004 C007 C006 -177.1(5) . . . . ? C00L C004 C007 C00G -0.7(9) . . . . ? C00L C004 C00A C00H 0.8(9) . . . . ? C00M C00O C00P Fe03 -61.1(5) . . . . ? C00M C00O C00P C00J -0.9(8) . . . . ? C00N C00J C00P Fe03 59.8(5) . . . . ? C00N C00J C00P C00O -0.4(8) . . . . ? C00N C00M C00O Fe03 -58.9(5) . . . . ? C00N C00M C00O C00P 1.8(8) . . . . ? C00O C00M C00N Fe03 58.4(5) . . . . ? C00O C00M C00N C00J -2.0(8) . . . . ? C00P C00J C00N Fe03 -59.2(5) . . . . ? C00P C00J C00N C00M 1.5(8) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.924(14) 2 0.076(14)