#------------------------------------------------------------------------------ #$Date: 2026-05-22 23:10:54 +0100 (Fri, 22 May 2026) $ #$Revision: 306070 $ #$URL: svn://www.crystallography.net/cod/cif/1/57/72/1577289.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_1577289 loop_ _publ_author_name 'Gerstner, Alexander' 'Arrowsmith, Merle' 'Dietz, Maximilian' 'Mihm, Cornelius' 'Braunschweig, Holger' _publ_section_title ; Zerovalent transition-metal inverse-sandwich complexes of a diborataanthracene dianion ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D6SC02501C _journal_year 2026 _chemical_formula_moiety 'C24 H22 B2 Cr2 O6' _chemical_formula_sum 'C24 H22 B2 Cr2 O6' _chemical_formula_weight 532.03 _chemical_name_common {eta6,eta'6-[2,3,6,7,9,10-Me6-9,10-DHDBA]}{Cr(CO)3}2 _chemical_name_systematic 2-Cr2 _chemical_properties_physical Air-sensitive,Moisture-sensitive _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-I 2ya' _space_group_name_H-M_alt 'I 1 2/a 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_date 2026-01-16 _audit_creation_method 'CIF-fill 1.6l (K.Radacki, 2005-26)' _audit_update_record ; 2026-03-18 deposited with the CCDC. 2026-05-13 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 114.150(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.6159(2) _cell_length_b 13.9295(2) _cell_length_c 14.9564(3) _cell_measurement_reflns_used 20764 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 75.3770 _cell_measurement_theta_min 4.4980 _cell_volume 2398.30(8) _computing_cell_refinement 'CrysAlisPro 1.171.44.108a (Rigaku OD, 2025)' _computing_data_collection ; CrysAlisPro system (CCD 44.111a 64-bit (release 13-05-2025)) ; _computing_data_reduction 'CrysAlisPro 1.171.44.108a (Rigaku OD, 2025)' _computing_molecular_graphics 'ShelXLe (Huebschle et all, 2011)' _computing_publication_material 'SHELXL-2019/2 (Sheldrick, 2019)' _computing_structure_refinement 'SHELXL-2019/2 (Sheldrick, 2019)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)'' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100(2) _diffrn_detector HPA _diffrn_detector_area_resol_mean 10.0 _diffrn_detector_type 'HyPix Arc150' _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): -------------------------------------------------------------------------- 1 \w 16.00 85.00 0.50 1.20 -- 61.40-120.00-176.00 138 2 \w -86.00 -16.00 0.50 1.20 -- -62.85 120.00 -92.00 140 3 \w -96.00 -26.00 0.50 1.20 -- -72.99 120.00 -92.00 140 4 \w 27.00 98.00 0.50 1.20 -- 74.55-120.00-176.00 142 5 \w -98.00 -29.00 0.50 1.20 -- -75.50 120.00 -92.00 138 6 \w 36.00 98.00 0.50 1.20 -- 82.97-120.00-176.00 124 7 \w 50.00 81.00 0.50 1.20 -- 34.00 49.00 78.95 62 8 \w 58.00 89.00 0.50 1.20 -- 42.00 50.00-151.07 62 9 \w -100.00 -69.00 0.50 1.20 -- -54.00 -52.00-140.91 62 10 \w -104.00 -73.00 0.50 1.20 -- -58.00 -52.00 -0.69 62 11 \w -113.00 -81.00 0.50 1.20 -- -66.00 -51.00 -81.21 64 12 \w -115.00 -85.00 0.50 1.20 -- -70.00 -58.00 -11.65 60 13 \w -115.00 -84.00 0.50 1.20 -- -70.00 -57.00 -99.01 62 14 \w -115.00 -85.00 0.50 1.20 -- -70.00 -58.00 167.80 60 15 \w -118.00 -90.00 0.50 1.20 -- -74.00 -62.00 -79.47 56 16 \w -123.00 -88.00 0.50 1.20 -- -74.00 -41.00 101.11 70 17 \w -123.00 -88.00 0.50 1.20 -- -74.00 -42.00-160.06 70 18 \w -123.00 -88.00 0.50 1.20 -- -74.00 -39.00-143.26 70 19 \w 34.00 80.00 0.50 1.20 -- 74.45 -95.00 -30.00 92 20 \w 27.00 100.00 0.50 1.20 -- 74.45-125.00 -30.00 146 21 \w 28.00 100.00 0.50 1.20 -- 74.55-125.00 90.00 144 22 \w 34.00 80.00 0.50 1.20 -- 74.55 -95.00-150.00 92 23 \w -100.00 -29.00 0.50 1.20 -- -75.50 125.00-180.00 142 24 \w -100.00 -29.00 0.50 1.20 -- -75.50 125.00 0.00 142 25 \w -127.00 -92.00 0.50 1.20 -- -78.00 -40.00 136.85 70 26 \w -126.00 -95.00 0.50 1.20 -- -78.76 -49.00-166.95 62 27 \w -122.00 -92.00 0.50 1.20 -- -78.76 -63.00 84.99 60 28 \w -97.00 -32.00 0.50 1.20 -- -78.76 114.00 63.81 130 29 \w -127.00 -93.00 0.50 1.20 -- -78.76 -42.00-179.98 68 30 \w -125.00 -94.00 0.50 1.20 -- -78.76 -51.00 12.99 62 31 \w -122.00 -92.00 0.50 1.20 -- -78.76 -63.00-126.45 60 32 \w -125.00 -94.00 0.50 1.20 -- -78.76 -52.00 105.56 62 33 \w -121.00 -95.00 0.50 1.20 -- -78.76 -65.00 -26.26 52 34 \w 56.00 131.00 0.50 1.20 -- 82.97 15.00 120.00 150 35 \w 36.00 101.00 0.50 1.20 -- 82.97-125.00 -60.00 130 36 \w 36.00 101.00 0.50 1.20 -- 82.97-125.00-150.00 130 37 \w 42.00 89.00 0.50 1.20 -- 82.97 -95.00 0.00 94 38 \w 36.00 101.00 0.50 1.20 -- 82.97-125.00 90.00 130 39 \w 42.00 89.00 0.50 1.20 -- 82.97 -95.00-150.00 94 40 \w 42.00 89.00 0.50 1.20 -- 82.97 -95.00 90.00 94 41 \w 36.00 101.00 0.50 1.20 -- 82.97-125.00 60.00 130 42 \w 36.00 101.00 0.50 1.20 -- 82.97-125.00 -30.00 130 43 \w 42.00 89.00 0.50 1.20 -- 82.97 -95.00 -30.00 94 44 \w 56.00 131.00 0.50 1.20 -- 82.97 15.00 30.00 150 45 \w -39.00 -13.00 0.50 1.20 -- -14.00 125.00 53.87 52 46 \w 32.00 60.00 0.50 1.20 -- 18.00 57.00 -27.97 56 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku XtaLAB Synergy-R' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type ; CrysAlisPro convention (1999,Acta A55,543-557) ; _diffrn_orient_matrix_UB_11 -0.0159043000 _diffrn_orient_matrix_UB_12 0.0758737000 _diffrn_orient_matrix_UB_13 -0.0794995000 _diffrn_orient_matrix_UB_21 -0.0078383000 _diffrn_orient_matrix_UB_22 0.0794026000 _diffrn_orient_matrix_UB_23 0.0688429000 _diffrn_orient_matrix_UB_31 0.1325690000 _diffrn_orient_matrix_UB_32 0.0137853000 _diffrn_orient_matrix_UB_33 0.0411478000 _diffrn_radiation_monochromator 'multi-layer mirror' _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_xray_symbol K-L~2,3~ _diffrn_reflns_av_R_equivalents 0.1544 _diffrn_reflns_av_unetI/netI 0.0606 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 21911 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 70.074 _diffrn_reflns_theta_min 4.536 _diffrn_source 'rotating-anode X-ray tube' _diffrn_source_type 'PhotonJet-R X-ray Source' _exptl_absorpt_coefficient_mu 7.785 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.64930 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.44.108a (Rigaku Oxford Diffraction, 2025) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.473 _exptl_crystal_description block _exptl_crystal_F_000 1088 _exptl_crystal_preparation ; For data collection the crystal was immersed in a film of perfluoropolyether oil, mounted on a polyimide loop and transferred to stream of cold nitrogen (Oxford Cryostream 800). ; _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent' _exptl_crystal_size_max 0.160 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.060 _refine_diff_density_max 1.248 _refine_diff_density_min -0.902 _refine_diff_density_rms 0.138 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 157 _refine_ls_number_reflns 2271 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.080 _refine_ls_R_factor_all 0.0641 _refine_ls_R_factor_gt 0.0638 _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^)+(0.1018P)^2^+1.9553P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1389 _refine_ls_wR_factor_ref 0.1396 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2234 _reflns_number_total 2271 _reflns_threshold_expression 'I > 2\s(I)' _twin_dimensionality triperiodic _twin_formation_mechanism gt _twin_morphology polysynthetic _twin_special_details ; Component 2 rotated by 179.9657\% around [0.90 -0.00 -0.44] (reciprocal) or [1.00 -0.00 0.00] (direct) ; _cod_data_source_file d6sc02501c2.cif _cod_data_source_block AlGe061_AlGe_twin1_hklf4_a _cod_original_sg_symbol_H-M 'I 2/a' _cod_database_code 1577289 _shelx_shelxl_version_number 2019/2 _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_min 0.369 _shelx_estimated_absorpt_t_max 0.652 _shelx_res_file ; TITL AlGe061_AlGe_twin1_hklf4_a.res in I2/a AlGe061_AlGe_twin1_hklf4_a.res created by SHELXL-2019/2 at 09:15:11 on 16-Jan-2026 REM Old TITL AlGe061_AlGe_twin1_hklf4 in I2/a REM SHELXT solution in I2/a REM R1 0.095, Rweak 0.007, Alpha 0.060, Orientation as input REM Formula found by SHELXT: C13 Cr O3 CELL 1.54184 12.6159 13.9295 14.9564 90.000 114.150 90.000 ZERR 4.000 0.0002 0.0002 0.0003 0.000 0.002 0.000 LATT 2 SYMM 1/2-X, Y, -Z SFAC C H B CR O UNIT 96 88 8 8 24 TEMP -173 SIZE 0.06 0.09 0.16 L.S. 10 BOND $H LIST 4 CONF ACTA shel 999 0.82 OMIT 1 16 5 FMAP 2 PLAN 20 WGHT 0.101800 1.955300 FVAR 0.19837 RESI NA1 1 CR1 4 0.377951 0.576027 0.249419 11.00000 0.02216 0.01599 = 0.01833 0.00087 0.00568 0.00052 C2 1 0.511521 0.521520 0.341130 11.00000 0.03024 0.02865 = 0.02385 0.00112 0.01271 0.00083 C3 1 0.412295 0.521809 0.151266 11.00000 0.02425 0.02456 = 0.02288 0.00256 0.00420 0.00117 C4 1 0.462195 0.684940 0.247079 11.00000 0.02906 0.02490 = 0.02779 -0.00128 0.01008 0.00153 O5 5 0.592710 0.486384 0.399742 11.00000 0.03103 0.04966 = 0.02702 0.01209 0.00886 0.01254 O6 5 0.432070 0.486817 0.090315 11.00000 0.03777 0.04290 = 0.02610 -0.00519 0.01261 0.00415 O7 5 0.517109 0.751003 0.246526 11.00000 0.03943 0.02837 = 0.05307 -0.00155 0.02246 -0.00953 RESI BC 2 B1 3 0.313217 0.752502 0.362148 11.00000 0.02347 0.01940 = 0.02236 0.00017 0.00604 0.00255 C2 1 0.384594 0.756372 0.476242 11.00000 0.04588 0.02116 = 0.02264 -0.00118 0.00378 0.00286 AFIX 137 H2A 2 0.354408 0.807992 0.503802 11.00000 -1.50000 H2B 2 0.466551 0.768636 0.490974 11.00000 -1.50000 H2C 2 0.377346 0.694900 0.505119 11.00000 -1.50000 AFIX 0 RESI XYL 3 C1 1 0.279247 0.477094 0.308412 11.00000 0.02653 0.01590 = 0.02771 0.00303 0.01216 0.00058 C2 1 0.224935 0.474629 0.205594 11.00000 0.02409 0.01683 = 0.02990 -0.00191 0.01049 -0.00268 C3 1 0.190757 0.562652 0.153969 11.00000 0.02195 0.01825 = 0.02350 0.00010 0.00483 0.00029 AFIX 43 H3 2 0.151978 0.560396 0.084557 11.00000 -1.20000 AFIX 0 C4 1 0.211223 0.653686 0.200136 11.00000 0.02121 0.01630 = 0.02199 -0.00209 0.00561 -0.00066 C5 1 0.268907 0.656210 0.306265 11.00000 0.02207 0.01836 = 0.01986 0.00177 0.00656 0.00197 C6 1 0.299285 0.567659 0.356436 11.00000 0.02607 0.01794 = 0.02463 0.00110 0.01167 0.00102 AFIX 43 H6 2 0.335030 0.568666 0.426014 11.00000 -1.20000 AFIX 0 C7 1 0.315822 0.386572 0.368454 11.00000 0.04107 0.01862 = 0.03094 0.00535 0.01440 0.00441 AFIX 137 H7A 2 0.246810 0.352649 0.366403 11.00000 -1.50000 H7B 2 0.365984 0.403000 0.436447 11.00000 -1.50000 H7C 2 0.358461 0.345190 0.341565 11.00000 -1.50000 AFIX 0 C8 1 0.201315 0.381529 0.149828 11.00000 0.03402 0.01822 = 0.03184 -0.00279 0.00808 -0.00104 AFIX 137 H8A 2 0.139279 0.346760 0.159482 11.00000 -1.50000 H8B 2 0.272019 0.342347 0.173767 11.00000 -1.50000 H8C 2 0.177259 0.394827 0.079906 11.00000 -1.50000 REM REM AlGe061_AlGe_twin1_hklf4_a.hkl REM AFIX 0 HKLF 4 REM AlGe061_AlGe_twin1_hklf4_a.res in I2/a REM wR2 = 0.1396, GooF = S = 1.080, Restrained GooF = 1.080 for all data REM R1 = 0.0638 for 2234 Fo > 4sig(Fo) and 0.0641 for all 2271 data REM 157 parameters refined using 0 restraints END WGHT 0.1017 1.9551 REM Highest difference peak 1.248, deepest hole -0.902, 1-sigma level 0.138 Q1 1 0.1261 0.5777 0.2555 11.00000 0.05 1.25 Q2 1 0.3605 0.4270 0.2427 11.00000 0.05 0.83 Q3 1 0.2966 0.5776 0.2515 11.00000 0.05 0.83 Q4 1 0.4626 0.5771 0.2467 11.00000 0.05 0.82 Q5 1 0.5145 0.4198 0.2722 11.00000 0.05 0.57 Q6 1 0.2468 0.4198 0.2211 11.00000 0.05 0.54 Q7 1 0.3397 0.5308 0.3234 11.00000 0.05 0.43 Q8 1 0.4336 0.5279 0.3334 11.00000 0.05 0.42 Q9 1 0.2991 0.5291 0.3295 11.00000 0.05 0.41 Q10 1 0.2049 0.4306 0.1652 11.00000 0.05 0.41 Q11 1 0.6215 0.7465 0.2776 11.00000 0.05 0.39 Q12 1 0.4217 0.5176 0.3822 11.00000 0.05 0.38 Q13 1 0.5203 0.5125 0.1415 11.00000 0.05 0.38 Q14 1 0.0935 0.4211 0.2382 11.00000 0.05 0.37 Q15 1 0.2588 0.6347 0.2000 11.00000 0.05 0.35 Q16 1 0.2397 0.3378 0.2116 11.00000 0.05 0.33 Q17 1 0.2023 0.5179 0.1938 11.00000 0.05 0.33 Q18 1 0.3181 0.4876 0.0880 11.00000 0.05 0.32 Q19 1 0.2630 0.4747 0.2654 11.00000 0.05 0.32 Q20 1 0.5357 0.4173 0.3372 11.00000 0.05 0.30 ; _shelx_res_checksum 76205 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -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 Cr1_1 Cr 0.37795(3) 0.57603(2) 0.24942(2) 0.0197(2) Uani 1 1 d . . . . . C2_1 C 0.51152(19) 0.52152(17) 0.34113(17) 0.0270(5) Uani 1 1 d . . . . . C3_1 C 0.41229(19) 0.52181(16) 0.15127(17) 0.0257(5) Uani 1 1 d . . . . . C4_1 C 0.4622(2) 0.68494(17) 0.24708(17) 0.0278(5) Uani 1 1 d . . . . . O5_1 O 0.59271(14) 0.48638(15) 0.39974(13) 0.0369(4) Uani 1 1 d . . . . . O6_1 O 0.43207(15) 0.48682(14) 0.09032(13) 0.0357(4) Uani 1 1 d . . . . . O7_1 O 0.51711(17) 0.75100(13) 0.24653(16) 0.0391(5) Uani 1 1 d . . . . . B1_2 B 0.3132(2) 0.75250(17) 0.3621(2) 0.0228(5) Uani 1 1 d . . . . . C2_2 C 0.3846(2) 0.75637(16) 0.47624(19) 0.0332(5) Uani 1 1 d . . . . . H2A_2 H 0.354408 0.807992 0.503802 0.050 Uiso 1 1 calc R U . . . H2B_2 H 0.466551 0.768636 0.490974 0.050 Uiso 1 1 calc R U . . . H2C_2 H 0.377346 0.694900 0.505119 0.050 Uiso 1 1 calc R U . . . C1_3 C 0.27925(19) 0.47709(14) 0.30841(18) 0.0230(5) Uani 1 1 d . . . . . C2_3 C 0.22493(19) 0.47463(15) 0.20559(18) 0.0238(5) Uani 1 1 d . . . . . C3_3 C 0.1908(2) 0.56265(16) 0.15397(18) 0.0227(5) Uani 1 1 d . . . . . H3_3 H 0.151978 0.560396 0.084557 0.027 Uiso 1 1 calc R U . . . C4_3 C 0.21122(18) 0.65369(15) 0.20014(16) 0.0209(4) Uani 1 1 d . . . . . C5_3 C 0.26891(18) 0.65621(15) 0.30627(16) 0.0208(4) Uani 1 1 d . . . . . C6_3 C 0.2993(2) 0.56766(15) 0.35644(19) 0.0225(5) Uani 1 1 d . . . . . H6_3 H 0.335030 0.568666 0.426014 0.027 Uiso 1 1 calc R U . . . C7_3 C 0.3158(2) 0.38657(17) 0.36845(19) 0.0303(5) Uani 1 1 d . . . . . H7A_3 H 0.246810 0.352649 0.366403 0.045 Uiso 1 1 calc R U . . . H7B_3 H 0.365984 0.403000 0.436447 0.045 Uiso 1 1 calc R U . . . H7C_3 H 0.358461 0.345190 0.341565 0.045 Uiso 1 1 calc R U . . . C8_3 C 0.2013(2) 0.38153(16) 0.14983(19) 0.0298(5) Uani 1 1 d . . . . . H8A_3 H 0.139279 0.346760 0.159482 0.045 Uiso 1 1 calc R U . . . H8B_3 H 0.272019 0.342347 0.173767 0.045 Uiso 1 1 calc R U . . . H8C_3 H 0.177259 0.394827 0.079906 0.045 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 Cr1_1 0.0222(3) 0.0160(3) 0.0183(3) 0.00087(10) 0.0057(2) 0.00052(10) C2_1 0.0302(11) 0.0287(12) 0.0239(11) 0.0011(9) 0.0127(9) 0.0008(8) C3_1 0.0242(10) 0.0246(12) 0.0229(11) 0.0026(8) 0.0042(9) 0.0012(8) C4_1 0.0291(11) 0.0249(12) 0.0278(12) -0.0013(9) 0.0101(9) 0.0015(9) O5_1 0.0310(9) 0.0497(11) 0.0270(9) 0.0121(8) 0.0089(7) 0.0125(8) O6_1 0.0378(9) 0.0429(11) 0.0261(9) -0.0052(7) 0.0126(7) 0.0042(7) O7_1 0.0394(10) 0.0284(10) 0.0531(12) -0.0016(7) 0.0225(9) -0.0095(7) B1_2 0.0235(12) 0.0194(12) 0.0224(13) 0.0002(9) 0.0060(10) 0.0025(8) C2_2 0.0459(14) 0.0212(12) 0.0226(11) -0.0012(8) 0.0038(10) 0.0029(9) C1_3 0.0265(10) 0.0159(11) 0.0277(12) 0.0030(8) 0.0122(9) 0.0006(7) C2_3 0.0241(10) 0.0168(11) 0.0299(12) -0.0019(8) 0.0105(9) -0.0027(7) C3_3 0.0219(11) 0.0183(11) 0.0235(12) 0.0001(8) 0.0048(9) 0.0003(7) C4_3 0.0212(10) 0.0163(10) 0.0220(11) -0.0021(8) 0.0056(8) -0.0007(7) C5_3 0.0221(10) 0.0184(10) 0.0199(10) 0.0018(8) 0.0066(8) 0.0020(7) C6_3 0.0261(12) 0.0179(11) 0.0246(12) 0.0011(8) 0.0117(10) 0.0010(7) C7_3 0.0411(13) 0.0186(12) 0.0309(13) 0.0053(10) 0.0144(10) 0.0044(9) C8_3 0.0340(12) 0.0182(12) 0.0318(12) -0.0028(9) 0.0081(10) -0.0010(8) 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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr -0.1635 2.4439 '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 1 1 0 0.0247 1 0 0 0.0536 -1 -1 0 0.0333 -1 0 0 0.0471 0 1 0 0.0658 -1 1 0 0.0753 0 -1 0 0.0584 1 1 -1 0.0413 0 1 -1 0.0698 -1 1 -1 0.0688 0 -1 1 0.0754 -1 -1 1 0.0334 0 0 1 0.0502 0 0 -1 0.0627 1 0 -1 0.0170 -1 0 1 0.0480 -1 -1 -1 0.0347 1 1 1 0.0281 0 -1 -1 0.0479 0 1 1 0.0421 -1 1 1 0.0660 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 C2_1 Cr1_1 C3_1 89.01(10) . . ? C2_1 Cr1_1 C4_1 89.69(10) . . ? C3_1 Cr1_1 C4_1 89.82(10) . . ? C2_1 Cr1_1 C5_3 116.60(9) . . ? C3_1 Cr1_1 C5_3 154.27(9) . . ? C4_1 Cr1_1 C5_3 92.62(9) . . ? C2_1 Cr1_1 C6_3 89.08(9) . . ? C3_1 Cr1_1 C6_3 150.96(9) . . ? C4_1 Cr1_1 C6_3 119.14(9) . . ? C5_3 Cr1_1 C6_3 37.46(8) . . ? C2_1 Cr1_1 C4_3 154.91(9) . . ? C3_1 Cr1_1 C4_3 115.79(9) . . ? C4_1 Cr1_1 C4_3 93.89(9) . . ? C5_3 Cr1_1 C4_3 38.49(8) . . ? C6_3 Cr1_1 C4_3 67.52(8) . . ? C2_1 Cr1_1 C3_3 148.68(9) . . ? C3_1 Cr1_1 C3_3 89.33(9) . . ? C4_1 Cr1_1 C3_3 121.59(9) . . ? C5_3 Cr1_1 C3_3 67.67(8) . . ? C6_3 Cr1_1 C3_3 77.60(9) . . ? C4_3 Cr1_1 C3_3 37.39(8) . . ? C2_1 Cr1_1 C2_3 111.71(9) . . ? C3_1 Cr1_1 C2_3 87.96(9) . . ? C4_1 Cr1_1 C2_3 158.43(9) . . ? C5_3 Cr1_1 C2_3 80.45(8) . . ? C6_3 Cr1_1 C2_3 65.98(9) . . ? C4_3 Cr1_1 C2_3 68.00(8) . . ? C3_3 Cr1_1 C2_3 36.96(8) . . ? C2_1 Cr1_1 C1_3 86.59(9) . . ? C3_1 Cr1_1 C1_3 113.88(9) . . ? C4_1 Cr1_1 C1_3 155.91(9) . . ? C5_3 Cr1_1 C1_3 68.11(8) . . ? C6_3 Cr1_1 C1_3 37.08(8) . . ? C4_3 Cr1_1 C1_3 80.07(8) . . ? C3_3 Cr1_1 C1_3 65.67(8) . . ? C2_3 Cr1_1 C1_3 36.16(9) . . ? O5_1 C2_1 Cr1_1 177.8(2) . . ? O6_1 C3_1 Cr1_1 178.7(2) . . ? O7_1 C4_1 Cr1_1 178.2(2) . . ? C5_3 B1_2 C4_3 117.4(2) . 7_565 ? C5_3 B1_2 C2_2 122.2(2) . . ? C4_3 B1_2 C2_2 120.3(2) 7_565 . ? B1_2 C2_2 H2A_2 109.5 . . ? B1_2 C2_2 H2B_2 109.5 . . ? H2A_2 C2_2 H2B_2 109.5 . . ? B1_2 C2_2 H2C_2 109.5 . . ? H2A_2 C2_2 H2C_2 109.5 . . ? H2B_2 C2_2 H2C_2 109.5 . . ? C2_3 C1_3 C6_3 118.74(19) . . ? C2_3 C1_3 C7_3 121.7(2) . . ? C6_3 C1_3 C7_3 119.6(2) . . ? C2_3 C1_3 Cr1_1 71.82(12) . . ? C6_3 C1_3 Cr1_1 69.18(12) . . ? C7_3 C1_3 Cr1_1 131.18(16) . . ? C1_3 C2_3 C3_3 118.57(19) . . ? C1_3 C2_3 C8_3 121.7(2) . . ? C3_3 C2_3 C8_3 119.7(2) . . ? C1_3 C2_3 Cr1_1 72.02(12) . . ? C3_3 C2_3 Cr1_1 69.60(12) . . ? C8_3 C2_3 Cr1_1 130.62(16) . . ? C4_3 C3_3 C2_3 123.7(2) . . ? C4_3 C3_3 Cr1_1 71.11(13) . . ? C2_3 C3_3 Cr1_1 73.44(13) . . ? C4_3 C3_3 H3_3 118.2 . . ? C2_3 C3_3 H3_3 118.2 . . ? Cr1_1 C3_3 H3_3 130.1 . . ? C3_3 C4_3 C5_3 117.70(19) . . ? C3_3 C4_3 B1_2 120.4(2) . 7_565 ? C5_3 C4_3 B1_2 121.39(19) . 7_565 ? C3_3 C4_3 Cr1_1 71.50(13) . . ? C5_3 C4_3 Cr1_1 70.34(12) . . ? B1_2 C4_3 Cr1_1 122.58(15) 7_565 . ? C6_3 C5_3 C4_3 117.75(19) . . ? C6_3 C5_3 B1_2 120.5(2) . . ? C4_3 C5_3 B1_2 121.13(19) . . ? C6_3 C5_3 Cr1_1 71.62(13) . . ? C4_3 C5_3 Cr1_1 71.17(12) . . ? B1_2 C5_3 Cr1_1 120.10(15) . . ? C5_3 C6_3 C1_3 123.5(2) . . ? C5_3 C6_3 Cr1_1 70.92(13) . . ? C1_3 C6_3 Cr1_1 73.74(13) . . ? C5_3 C6_3 H6_3 118.2 . . ? C1_3 C6_3 H6_3 118.2 . . ? Cr1_1 C6_3 H6_3 129.9 . . ? C1_3 C7_3 H7A_3 109.5 . . ? C1_3 C7_3 H7B_3 109.5 . . ? H7A_3 C7_3 H7B_3 109.5 . . ? C1_3 C7_3 H7C_3 109.5 . . ? H7A_3 C7_3 H7C_3 109.5 . . ? H7B_3 C7_3 H7C_3 109.5 . . ? C2_3 C8_3 H8A_3 109.5 . . ? C2_3 C8_3 H8B_3 109.5 . . ? H8A_3 C8_3 H8B_3 109.5 . . ? C2_3 C8_3 H8C_3 109.5 . . ? H8A_3 C8_3 H8C_3 109.5 . . ? H8B_3 C8_3 H8C_3 109.5 . . ? 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 Cr1_1 C2_1 1.846(2) . ? Cr1_1 C3_1 1.853(2) . ? Cr1_1 C4_1 1.861(2) . ? Cr1_1 C5_3 2.195(2) . ? Cr1_1 C6_3 2.205(2) . ? Cr1_1 C4_3 2.207(2) . ? Cr1_1 C3_3 2.212(2) . ? Cr1_1 C2_3 2.262(2) . ? Cr1_1 C1_3 2.264(2) . ? C2_1 O5_1 1.150(3) . ? C3_1 O6_1 1.148(3) . ? C4_1 O7_1 1.154(3) . ? B1_2 C5_3 1.558(3) . ? B1_2 C4_3 1.561(3) 7_565 ? B1_2 C2_2 1.571(4) . ? C2_2 H2A_2 0.9800 . ? C2_2 H2B_2 0.9800 . ? C2_2 H2C_2 0.9800 . ? C1_3 C2_3 1.405(4) . ? C1_3 C6_3 1.422(3) . ? C1_3 C7_3 1.507(3) . ? C2_3 C3_3 1.419(3) . ? C2_3 C8_3 1.504(3) . ? C3_3 C4_3 1.416(3) . ? C3_3 H3_3 0.9500 . ? C4_3 C5_3 1.451(3) . ? C5_3 C6_3 1.413(3) . ? C6_3 H6_3 0.9500 . ? C7_3 H7A_3 0.9800 . ? C7_3 H7B_3 0.9800 . ? C7_3 H7C_3 0.9800 . ? C8_3 H8A_3 0.9800 . ? C8_3 H8B_3 0.9800 . ? C8_3 H8C_3 0.9800 . ? 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 C6_3 C1_3 C2_3 C3_3 -0.9(3) . . . . ? C7_3 C1_3 C2_3 C3_3 178.7(2) . . . . ? Cr1_1 C1_3 C2_3 C3_3 -53.56(19) . . . . ? C6_3 C1_3 C2_3 C8_3 179.8(2) . . . . ? C7_3 C1_3 C2_3 C8_3 -0.6(3) . . . . ? Cr1_1 C1_3 C2_3 C8_3 127.2(2) . . . . ? C6_3 C1_3 C2_3 Cr1_1 52.64(19) . . . . ? C7_3 C1_3 C2_3 Cr1_1 -127.7(2) . . . . ? C1_3 C2_3 C3_3 C4_3 1.9(4) . . . . ? C8_3 C2_3 C3_3 C4_3 -178.8(2) . . . . ? Cr1_1 C2_3 C3_3 C4_3 -52.9(2) . . . . ? C1_3 C2_3 C3_3 Cr1_1 54.72(19) . . . . ? C8_3 C2_3 C3_3 Cr1_1 -126.0(2) . . . . ? C2_3 C3_3 C4_3 C5_3 -0.9(3) . . . . ? Cr1_1 C3_3 C4_3 C5_3 -54.80(18) . . . . ? C2_3 C3_3 C4_3 B1_2 171.4(2) . . . 7_565 ? Cr1_1 C3_3 C4_3 B1_2 117.5(2) . . . 7_565 ? C2_3 C3_3 C4_3 Cr1_1 53.9(2) . . . . ? C3_3 C4_3 C5_3 C6_3 -0.9(3) . . . . ? B1_2 C4_3 C5_3 C6_3 -173.1(2) 7_565 . . . ? Cr1_1 C4_3 C5_3 C6_3 -56.24(18) . . . . ? C3_3 C4_3 C5_3 B1_2 169.8(2) . . . . ? B1_2 C4_3 C5_3 B1_2 -2.5(4) 7_565 . . . ? Cr1_1 C4_3 C5_3 B1_2 114.4(2) . . . . ? C3_3 C4_3 C5_3 Cr1_1 55.37(18) . . . . ? B1_2 C4_3 C5_3 Cr1_1 -116.9(2) 7_565 . . . ? C4_3 B1_2 C5_3 C6_3 172.8(2) 7_565 . . . ? C2_2 B1_2 C5_3 C6_3 -4.7(3) . . . . ? C4_3 B1_2 C5_3 C4_3 2.4(3) 7_565 . . . ? C2_2 B1_2 C5_3 C4_3 -175.0(2) . . . . ? C4_3 B1_2 C5_3 Cr1_1 87.4(2) 7_565 . . . ? C2_2 B1_2 C5_3 Cr1_1 -90.0(3) . . . . ? C4_3 C5_3 C6_3 C1_3 1.8(3) . . . . ? B1_2 C5_3 C6_3 C1_3 -168.9(2) . . . . ? Cr1_1 C5_3 C6_3 C1_3 -54.2(2) . . . . ? C4_3 C5_3 C6_3 Cr1_1 56.02(18) . . . . ? B1_2 C5_3 C6_3 Cr1_1 -114.7(2) . . . . ? C2_3 C1_3 C6_3 C5_3 -0.9(4) . . . . ? C7_3 C1_3 C6_3 C5_3 179.4(2) . . . . ? Cr1_1 C1_3 C6_3 C5_3 53.0(2) . . . . ? C2_3 C1_3 C6_3 Cr1_1 -53.89(19) . . . . ? C7_3 C1_3 C6_3 Cr1_1 126.4(2) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined _oxdiff_twin_reflns_isolated _oxdiff_twin_reflns_overlapped _twin_individual_twin_lattice_type _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.8225 20758 23665 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 2 0.1775 20772 23665 nmt 1.0001 -0.0009 -0.0003 -0.0003 -0.9999 -0.0005 -0.9713 0.0010 -0.9992