#------------------------------------------------------------------------------ #$Date: 2026-05-22 23:10:54 +0100 (Fri, 22 May 2026) $ #$Revision: 306070 $ #$URL: svn://www.crystallography.net/cod/cif/1/57/72/1577290.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_1577290 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 O6 W2' _chemical_formula_sum 'C24 H22 B2 O6 W2' _chemical_formula_weight 795.73 _chemical_name_common {eta6,eta'6-[2,3,6,7,9,10-Me6-9,10-DHDBA]}{W(CO)3}2 _chemical_name_systematic 2-W2 _chemical_properties_physical Air-sensitive,Moisture-sensitive _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_date 2025-01-30 _audit_creation_method 'CIF-fill 1.5p (K.Radacki, 2005-25)' _audit_update_record ; 2026-03-18 deposited with the CCDC. 2026-05-13 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 93.3110(10) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 7.10870(10) _cell_length_b 10.15770(10) _cell_length_c 16.8094(2) _cell_measurement_reflns_used 16149 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 74.7700 _cell_measurement_theta_min 4.3260 _cell_volume 1211.75(3) _computing_cell_refinement 'CrysAlisPro 1.171.43.142a (Rigaku OD, 2024)' _computing_data_collection ; CrysAlisPro system (CCD 43.128a 64-bit (release 20-06-2024)) ; _computing_data_reduction 'CrysAlisPro 1.171.43.142a (Rigaku OD, 2024)' _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 0.999 _diffrn_measured_fraction_theta_max 0.974 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): -------------------------------------------------------------------------- 1 \w 42.00 92.00 0.50 0.05 -- 84.76 -95.00-180.00 100 2 \w -111.00 -76.00 0.50 0.05 -- -62.00 -48.00 146.86 70 3 \w 16.00 66.00 0.50 0.05 -- 58.85 -95.00 30.00 100 4 \w -129.00 -93.00 0.50 0.05 -- -79.50 -48.00 -84.43 72 5 \w 4.00 30.00 0.50 0.05 -- -6.00 69.00 84.20 52 6 \w -128.00 -93.00 0.50 0.05 -- -79.50 -50.00 61.88 70 7 \w 16.00 66.00 0.50 0.05 -- 58.85 -95.00-150.00 100 8 \w -121.00 -86.00 0.50 0.05 -- -74.00 -57.00-101.13 70 9 \w -128.00 -93.00 0.50 0.05 -- -79.50 -49.00 81.78 70 10 \w -120.00 -83.00 0.50 0.05 -- -70.00 -46.00 100.78 74 11 \w -116.00 -79.00 0.50 0.05 -- -66.00 -46.00 71.96 74 12 \w -130.00 -92.00 0.50 0.05 -- -79.50 -42.00 -19.90 76 13 \w -129.00 -93.00 0.50 0.05 -- -79.50 -47.00 -41.99 72 14 \w -117.00 -85.00 0.50 0.05 -- -70.00 -58.00 -87.87 64 15 \w 34.00 85.00 0.50 0.05 -- 77.01 -95.00 90.00 102 16 \w -122.00 -64.00 0.50 0.05 -- -69.92 -22.00 -3.00 116 17 \w -96.00 -58.00 0.50 0.05 -- -46.00 -42.00 -96.52 76 18 \w -128.00 -70.00 0.50 0.05 -- -76.45 -22.00 -3.00 116 19 \w 66.00 129.00 0.50 0.05 -- 77.01 22.00 162.00 126 20 \w 74.00 137.00 0.50 0.05 -- 84.76 22.00 162.00 126 21 \w -120.00 -83.00 0.50 0.05 -- -70.00 -45.00 -23.11 74 22 \w 34.00 60.00 0.50 0.05 -- 22.00 58.00 -22.85 52 23 \w 34.00 60.00 0.50 0.05 -- 22.00 59.00-141.25 52 24 \w 34.00 60.00 0.50 0.05 -- 22.00 57.00 27.86 52 25 \w 48.00 111.00 0.50 0.05 -- 58.85 22.00 162.00 126 26 \w 61.00 124.00 0.50 0.05 -- 71.50 22.00 162.00 126 27 \w -120.00 -83.00 0.50 0.05 -- -70.00 -44.00-139.18 74 28 \w 42.00 92.00 0.50 0.05 -- 84.76 -95.00 90.00 100 29 \w 42.00 92.00 0.50 0.05 -- 84.76 -95.00-120.00 100 30 \w -128.00 -93.00 0.50 0.05 -- -79.50 -51.00-162.00 70 31 \w 42.00 92.00 0.50 0.05 -- 84.76 -95.00 -90.00 100 32 \w -112.00 -54.00 0.50 0.05 -- -60.43 -22.00 -3.00 116 33 \w -39.00 -4.00 0.50 0.05 -- -22.00 110.00 -97.87 70 34 \w -128.00 -93.00 0.50 0.05 -- -79.50 -50.00-116.80 70 35 \w -125.00 -91.00 0.50 0.05 -- -79.50 -60.00-173.22 68 36 \w -93.00 -31.00 0.50 0.05 -- -76.45 112.00 120.00 124 37 \w 42.00 92.00 0.50 0.05 -- 84.76 -95.00 30.00 100 38 \w 34.00 85.00 0.50 0.05 -- 77.01 -95.00 0.00 102 39 \w -93.00 -31.00 0.50 0.05 -- -76.45 112.00-180.00 124 40 \w -128.00 -93.00 0.50 0.05 -- -79.50 -50.00-138.50 70 41 \w -93.00 -31.00 0.50 0.05 -- -76.45 112.00 -90.00 124 42 \w 42.00 92.00 0.50 0.05 -- 84.76 -95.00 120.00 100 43 \w 42.00 92.00 0.50 0.05 -- 84.76 -95.00 0.00 100 44 \w 34.00 85.00 0.50 0.05 -- 77.01 -95.00 30.00 102 45 \w -98.00 -22.00 0.50 0.05 -- -69.92 126.00 60.00 152 46 \w 26.00 60.00 0.50 0.05 -- 14.00 57.00-174.56 68 47 \w 42.00 92.00 0.50 0.05 -- 84.76 -95.00 -30.00 100 48 \w -98.00 -33.00 0.50 0.05 -- -79.50 119.00-173.39 130 49 \w 34.00 60.00 0.50 0.05 -- 22.00 57.00 -78.88 52 50 \w 30.00 56.00 0.50 0.05 -- 18.00 60.00 126.50 52 51 \w 39.00 93.00 0.50 0.05 -- 84.76-112.00 90.00 108 52 \w 42.00 92.00 0.50 0.05 -- 84.76 -95.00 60.00 100 ; _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 0.1675947000 _diffrn_orient_matrix_UB_12 0.0964032000 _diffrn_orient_matrix_UB_13 0.0044175000 _diffrn_orient_matrix_UB_21 0.1335271000 _diffrn_orient_matrix_UB_22 -0.1136103000 _diffrn_orient_matrix_UB_23 0.0258283000 _diffrn_orient_matrix_UB_31 0.0344503000 _diffrn_orient_matrix_UB_32 -0.0285812000 _diffrn_orient_matrix_UB_33 -0.0879723000 _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 0.0880 _diffrn_reflns_av_unetI/netI 0.0298 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.974 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 22436 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.974 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.972 _diffrn_reflns_theta_min 5.090 _diffrn_source 'rotating-anode X-ray tube' _diffrn_source_type 'PhotonJet-R X-ray Source' _exptl_absorpt_coefficient_mu 17.607 _exptl_absorpt_correction_T_max 0.677 _exptl_absorpt_correction_T_min 0.138 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.43.142a (Rigaku Oxford Diffraction, 2024) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 2.181 _exptl_crystal_description block _exptl_crystal_F_000 744 _exptl_crystal_preparation ; Crystals were grown at 25 \%C from saturated solution in THF. 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 0.070 _exptl_crystal_size_min 0.040 _refine_diff_density_max 0.679 _refine_diff_density_min -1.519 _refine_diff_density_rms 0.185 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 157 _refine_ls_number_reflns 2426 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.109 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0312 _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^)+(0.0512P)^2^+1.9567P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0841 _refine_ls_wR_factor_ref 0.0850 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2312 _reflns_number_total 2426 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6sc02501c2.cif _cod_data_source_block AlGe037_AlGe_a _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1577290 _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 0.165 _shelx_estimated_absorpt_t_max 0.539 _shelx_res_file ; TITL AlGe037_AlGe_a.res in P2(1)/n AlGe037_AlGe_a.res created by SHELXL-2019/2 at 16:25:08 on 30-Jan-2025 REM Old TITL AlGe037_AlGe in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.051, Rweak 0.003, Alpha 0.026, Orientation as input REM Formula found by SHELXT: C13 O3 W CELL 1.54184 7.1087 10.1577 16.8094 90.000 93.311 90.000 ZERR 2.000 0.0001 0.0001 0.0002 0.000 0.001 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H B O W UNIT 48 44 4 12 4 TEMP -173 SIZE 0.04 0.07 0.16 L.S. 10 BOND $H LIST 4 CONF ACTA FMAP 2 PLAN 20 WGHT 0.051200 1.956700 FVAR 0.35944 RESI 1 DBA B1 3 0.440941 0.584208 0.428002 11.00000 0.02752 0.02900 = 0.02823 0.00213 0.00199 -0.00442 C2 1 0.369516 0.672162 0.355529 11.00000 0.04985 0.03983 = 0.03076 0.00404 0.00273 0.00729 AFIX 137 H2A 2 0.240725 0.701847 0.363363 11.00000 -1.50000 H2B 2 0.370986 0.620705 0.306252 11.00000 -1.50000 H2C 2 0.452287 0.748793 0.351767 11.00000 -1.50000 AFIX 0 C3 1 0.546329 0.452926 0.417087 11.00000 0.02577 0.03156 = 0.02623 -0.00266 0.00169 -0.00890 C4 1 0.562647 0.397455 0.339340 11.00000 0.03071 0.03355 = 0.02625 0.00087 0.00344 -0.00628 AFIX 13 H4 2 0.514574 0.450459 0.292325 11.00000 -1.20000 AFIX 0 C5 1 0.615440 0.266659 0.326056 11.00000 0.02806 0.03749 = 0.03288 -0.00723 0.00673 -0.00477 C6 1 0.649237 0.182020 0.392839 11.00000 0.02515 0.03367 = 0.03741 -0.00561 0.00165 0.00139 C7 1 0.645423 0.236773 0.470868 11.00000 0.02217 0.03431 = 0.03658 -0.00460 -0.00149 0.00077 AFIX 13 H7 2 0.653355 0.174961 0.517243 11.00000 -1.20000 AFIX 0 C8 1 0.590273 0.368167 0.484633 11.00000 0.02286 0.02938 = 0.03017 -0.00465 -0.00314 -0.00148 C9 1 0.635296 0.218471 0.241426 11.00000 0.04626 0.04534 = 0.03125 -0.01211 0.00946 -0.00868 AFIX 137 H9A 2 0.769136 0.213497 0.230660 11.00000 -1.50000 H9B 2 0.571313 0.279835 0.203888 11.00000 -1.50000 H9C 2 0.578253 0.130986 0.235118 11.00000 -1.50000 AFIX 0 C10 1 0.701156 0.039395 0.383070 11.00000 0.04518 0.03628 = 0.05431 -0.00937 0.00019 0.00718 AFIX 137 H10A 2 0.829739 0.033242 0.365280 11.00000 -1.50000 H10B 2 0.613401 -0.001678 0.343373 11.00000 -1.50000 H10C 2 0.694107 -0.006168 0.434201 11.00000 -1.50000 AFIX 0 RESI 0 RESI 2 WCO W1 5 0.346162 0.274717 0.406377 11.00000 0.02317 0.02811 = 0.02460 0.00090 0.00056 -0.00070 O1 4 0.023459 0.395605 0.294981 11.00000 0.03942 0.05119 = 0.05746 0.00958 -0.01768 0.00714 C1 1 0.139904 0.349440 0.336913 11.00000 0.03493 0.03155 = 0.03740 -0.00341 0.00270 -0.00159 O2 4 0.186963 -0.005252 0.365421 11.00000 0.05306 0.03066 = 0.12254 -0.00127 -0.00783 -0.00925 C2 1 0.242733 0.099816 0.381424 11.00000 0.03051 0.03609 = 0.06094 0.00438 -0.00409 -0.00044 O3 4 0.077765 0.287258 0.546162 11.00000 0.04391 0.17271 = 0.03621 -0.00020 0.01366 -0.00459 C3 1 0.176739 0.282473 0.494154 11.00000 0.03124 0.08572 = 0.03068 -0.00125 0.00450 -0.01150 RESI 0 REM REM AlGe037_AlGe_a.hkl REM HKLF 4 REM AlGe037_AlGe_a.res in P2(1)/n REM wR2 = 0.0850, GooF = S = 1.109, Restrained GooF = 1.109 for all data REM R1 = 0.0312 for 2312 Fo > 4sig(Fo) and 0.0322 for all 2426 data REM 157 parameters refined using 0 restraints END WGHT 0.0511 1.9564 REM Highest difference peak 0.679, deepest hole -1.519, 1-sigma level 0.185 Q1 1 0.3136 0.2745 0.4587 11.00000 0.05 0.68 Q2 1 0.3154 0.2769 0.2857 11.00000 0.05 0.66 Q3 1 0.0118 0.3813 0.5221 11.00000 0.05 0.60 Q4 1 0.9229 -0.0799 0.3780 11.00000 0.05 0.57 Q5 1 0.3722 0.2675 0.5186 11.00000 0.05 0.56 Q6 1 0.6227 0.0951 0.1790 11.00000 0.05 0.56 Q7 1 0.2252 0.3815 0.5788 11.00000 0.05 0.51 Q8 1 0.3727 0.2790 0.3550 11.00000 0.05 0.50 Q9 1 0.5555 0.4395 0.3815 11.00000 0.05 0.50 Q10 1 0.7943 0.1670 0.5061 11.00000 0.05 0.47 Q11 1 0.5001 0.8475 0.3214 11.00000 0.05 0.47 Q12 1 0.7876 0.5259 0.4257 11.00000 0.05 0.46 Q13 1 0.4701 0.2278 0.1812 11.00000 0.05 0.46 Q14 1 0.0340 0.1235 0.5766 11.00000 0.05 0.46 Q15 1 0.6872 0.0279 0.2183 11.00000 0.05 0.46 Q16 1 0.7949 -0.0762 0.4279 11.00000 0.05 0.46 Q17 1 0.4870 0.2619 0.4619 11.00000 0.05 0.45 Q18 1 0.3706 0.0391 0.2801 11.00000 0.05 0.45 Q19 1 0.1910 0.2221 0.4204 11.00000 0.05 0.45 Q20 1 0.6118 0.7728 0.4163 11.00000 0.05 0.44 ; _shelx_res_checksum 12691 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group B1_1 B 0.4409(7) 0.5842(5) 0.4280(3) 0.0282(10) Uani 1 1 d . . . . . C2_1 C 0.3695(8) 0.6722(5) 0.3555(3) 0.0401(11) Uani 1 1 d . . . . . H2A_1 H 0.240725 0.701847 0.363363 0.060 Uiso 1 1 calc R U . . . H2B_1 H 0.370986 0.620705 0.306252 0.060 Uiso 1 1 calc R U . . . H2C_1 H 0.452287 0.748793 0.351767 0.060 Uiso 1 1 calc R U . . . C3_1 C 0.5463(6) 0.4529(4) 0.4171(2) 0.0278(9) Uani 1 1 d . . . . . C4_1 C 0.5626(6) 0.3975(5) 0.3393(3) 0.0301(9) Uani 1 1 d . . . . . H4_1 H 0.514574 0.450459 0.292325 0.036 Uiso 1 1 calc R U . . . C5_1 C 0.6154(8) 0.2667(5) 0.3261(3) 0.0326(11) Uani 1 1 d . . . . . C6_1 C 0.6492(6) 0.1820(5) 0.3928(3) 0.0321(10) Uani 1 1 d . . . . . C7_1 C 0.6454(7) 0.2368(5) 0.4709(3) 0.0311(10) Uani 1 1 d . . . . . H7_1 H 0.653355 0.174961 0.517243 0.037 Uiso 1 1 calc R U . . . C8_1 C 0.5903(6) 0.3682(5) 0.4846(3) 0.0277(9) Uani 1 1 d . . . . . C9_1 C 0.6353(9) 0.2185(5) 0.2414(3) 0.0407(13) Uani 1 1 d . . . . . H9A_1 H 0.769136 0.213497 0.230660 0.061 Uiso 1 1 calc R U . . . H9B_1 H 0.571313 0.279835 0.203888 0.061 Uiso 1 1 calc R U . . . H9C_1 H 0.578253 0.130986 0.235118 0.061 Uiso 1 1 calc R U . . . C10_1 C 0.7012(8) 0.0394(5) 0.3831(4) 0.0454(12) Uani 1 1 d . . . . . H10A_1 H 0.829739 0.033242 0.365280 0.068 Uiso 1 1 calc R U . . . H10B_1 H 0.613401 -0.001678 0.343373 0.068 Uiso 1 1 calc R U . . . H10C_1 H 0.694107 -0.006168 0.434201 0.068 Uiso 1 1 calc R U . . . W1_2 W 0.34616(3) 0.27472(2) 0.40638(2) 0.02532(11) Uani 1 1 d . . . . . O1_2 O 0.0235(5) 0.3956(4) 0.2950(2) 0.0501(10) Uani 1 1 d . . . . . C1_2 C 0.1399(7) 0.3494(5) 0.3369(3) 0.0346(10) Uani 1 1 d . . . . . O2_2 O 0.1870(6) -0.0053(4) 0.3654(3) 0.0693(14) Uani 1 1 d . . . . . C2_2 C 0.2427(7) 0.0998(5) 0.3814(4) 0.0428(12) Uani 1 1 d . . . . . O3_2 O 0.0778(8) 0.2873(7) 0.5462(3) 0.084(2) Uani 1 1 d . . . . . C3_2 C 0.1767(9) 0.2825(7) 0.4942(4) 0.0491(16) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1_1 0.028(2) 0.029(2) 0.028(2) 0.002(2) 0.0020(18) -0.004(2) C2_1 0.050(3) 0.040(3) 0.031(2) 0.004(2) 0.003(2) 0.007(2) C3_1 0.026(2) 0.032(2) 0.026(2) -0.0027(17) 0.0017(16) -0.0089(18) C4_1 0.031(2) 0.034(2) 0.026(2) 0.0009(18) 0.0034(17) -0.0063(19) C5_1 0.028(3) 0.037(3) 0.033(3) -0.0072(19) 0.007(2) -0.0048(19) C6_1 0.025(2) 0.034(2) 0.037(3) -0.006(2) 0.0016(18) 0.001(2) C7_1 0.022(2) 0.034(2) 0.037(3) -0.0046(19) -0.0015(19) 0.0008(18) C8_1 0.023(2) 0.029(2) 0.030(2) -0.0047(18) -0.0031(16) -0.0015(18) C9_1 0.046(3) 0.045(3) 0.031(3) -0.012(2) 0.009(2) -0.009(2) C10_1 0.045(3) 0.036(3) 0.054(3) -0.009(2) 0.000(2) 0.007(2) W1_2 0.02317(16) 0.02811(17) 0.02460(16) 0.00090(6) 0.00056(10) -0.00070(7) O1_2 0.039(2) 0.051(2) 0.057(2) 0.0096(19) -0.0177(18) 0.0071(18) C1_2 0.035(3) 0.032(2) 0.037(2) -0.003(2) 0.003(2) -0.002(2) O2_2 0.053(3) 0.031(2) 0.123(4) -0.001(2) -0.008(3) -0.0093(19) C2_2 0.031(3) 0.036(3) 0.061(3) 0.004(2) -0.004(2) 0.000(2) O3_2 0.044(3) 0.173(7) 0.036(3) 0.000(3) 0.014(2) -0.005(3) C3_2 0.031(3) 0.086(5) 0.031(3) -0.001(3) 0.005(2) -0.012(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -5.4734 5.5774 '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 0.0325 0 0 1 0.0038 1 -1 -1 0.0687 1 -1 1 0.0617 -1 1 -1 0.0635 -1 1 0 0.0672 -1 1 1 0.0641 0 1 0 0.0354 0 -1 -1 0.0299 0 1 1 0.0221 1 1 -1 0.0757 1 1 0 0.0752 -1 -1 -1 0.0728 1 0 -1 0.0758 -1 0 -1 0.0772 -1 0 0 0.0789 1 0 1 0.0725 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 C3_1 B1_1 C2_1 122.4(4) . . ? C3_1 B1_1 C8_1 118.1(4) . 3_666 ? C2_1 B1_1 C8_1 119.5(4) . 3_666 ? B1_1 C2_1 H2A_1 109.5 . . ? B1_1 C2_1 H2B_1 109.5 . . ? H2A_1 C2_1 H2B_1 109.5 . . ? B1_1 C2_1 H2C_1 109.5 . . ? H2A_1 C2_1 H2C_1 109.5 . . ? H2B_1 C2_1 H2C_1 109.5 . . ? C4_1 C3_1 C8_1 117.2(4) . . ? C4_1 C3_1 B1_1 120.8(4) . . ? C8_1 C3_1 B1_1 120.3(4) . . ? C4_1 C3_1 W1_2 72.7(2) . . ? C8_1 C3_1 W1_2 72.4(2) . . ? B1_1 C3_1 W1_2 112.7(3) . . ? C5_1 C4_1 C3_1 123.6(5) . . ? C5_1 C4_1 W1_2 76.1(3) . . ? C3_1 C4_1 W1_2 71.2(2) . . ? C5_1 C4_1 H4_1 117.8 . . ? C3_1 C4_1 H4_1 117.8 . . ? W1_2 C4_1 H4_1 117.8 . . ? C4_1 C5_1 C6_1 118.8(5) . . ? C4_1 C5_1 C9_1 119.7(5) . . ? C6_1 C5_1 C9_1 121.6(5) . . ? C4_1 C5_1 W1_2 69.5(3) . . ? C6_1 C5_1 W1_2 71.4(3) . . ? C9_1 C5_1 W1_2 131.0(4) . . ? C5_1 C6_1 C7_1 118.6(4) . . ? C5_1 C6_1 C10_1 121.7(5) . . ? C7_1 C6_1 C10_1 119.5(5) . . ? C5_1 C6_1 W1_2 73.9(3) . . ? C7_1 C6_1 W1_2 72.0(3) . . ? C10_1 C6_1 W1_2 128.4(4) . . ? C8_1 C7_1 C6_1 122.6(5) . . ? C8_1 C7_1 W1_2 70.7(3) . . ? C6_1 C7_1 W1_2 72.9(3) . . ? C8_1 C7_1 H7_1 118.0 . . ? C6_1 C7_1 H7_1 118.0 . . ? W1_2 C7_1 H7_1 118.0 . . ? C7_1 C8_1 C3_1 118.9(4) . . ? C7_1 C8_1 B1_1 119.9(4) . 3_666 ? C3_1 C8_1 B1_1 121.0(4) . 3_666 ? C7_1 C8_1 W1_2 74.1(3) . . ? C3_1 C8_1 W1_2 71.2(2) . . ? B1_1 C8_1 W1_2 120.9(3) 3_666 . ? C5_1 C9_1 H9A_1 109.5 . . ? C5_1 C9_1 H9B_1 109.5 . . ? H9A_1 C9_1 H9B_1 109.5 . . ? C5_1 C9_1 H9C_1 109.5 . . ? H9A_1 C9_1 H9C_1 109.5 . . ? H9B_1 C9_1 H9C_1 109.5 . . ? C6_1 C10_1 H10A_1 109.5 . . ? C6_1 C10_1 H10B_1 109.5 . . ? H10A_1 C10_1 H10B_1 109.5 . . ? C6_1 C10_1 H10C_1 109.5 . . ? H10A_1 C10_1 H10C_1 109.5 . . ? H10B_1 C10_1 H10C_1 109.5 . . ? C2_2 W1_2 C3_2 87.6(3) . . ? C2_2 W1_2 C1_2 88.0(2) . . ? C3_2 W1_2 C1_2 87.8(2) . . ? C2_2 W1_2 C3_1 162.2(2) . . ? C3_2 W1_2 C3_1 108.3(2) . . ? C1_2 W1_2 C3_1 100.29(18) . . ? C2_2 W1_2 C8_1 138.8(2) . . ? C3_2 W1_2 C8_1 91.6(2) . . ? C1_2 W1_2 C8_1 133.2(2) . . ? C3_1 W1_2 C8_1 36.42(16) . . ? C2_2 W1_2 C4_1 129.4(2) . . ? C3_2 W1_2 C4_1 142.9(2) . . ? C1_2 W1_2 C4_1 89.82(19) . . ? C3_1 W1_2 C4_1 36.12(15) . . ? C8_1 W1_2 C4_1 63.92(16) . . ? C2_2 W1_2 C7_1 105.50(19) . . ? C3_2 W1_2 C7_1 103.7(2) . . ? C1_2 W1_2 C7_1 162.4(2) . . ? C3_1 W1_2 C7_1 63.67(16) . . ? C8_1 W1_2 C7_1 35.14(16) . . ? C4_1 W1_2 C7_1 72.90(18) . . ? C2_2 W1_2 C6_1 87.21(19) . . ? C3_2 W1_2 C6_1 133.5(2) . . ? C1_2 W1_2 C6_1 138.0(2) . . ? C3_1 W1_2 C6_1 76.07(16) . . ? C8_1 W1_2 C6_1 64.11(16) . . ? C4_1 W1_2 C6_1 62.35(17) . . ? C7_1 W1_2 C6_1 35.05(17) . . ? C2_2 W1_2 C5_1 98.6(2) . . ? C3_2 W1_2 C5_1 165.3(2) . . ? C1_2 W1_2 C5_1 105.6(2) . . ? C3_1 W1_2 C5_1 64.07(16) . . ? C8_1 W1_2 C5_1 74.86(17) . . ? C4_1 W1_2 C5_1 34.43(16) . . ? C7_1 W1_2 C5_1 61.81(19) . . ? C6_1 W1_2 C5_1 34.63(18) . . ? O1_2 C1_2 W1_2 177.7(5) . . ? O2_2 C2_2 W1_2 177.7(5) . . ? O3_2 C3_2 W1_2 179.6(6) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1_1 C3_1 1.546(7) . ? B1_1 C2_1 1.571(7) . ? B1_1 C8_1 1.574(6) 3_666 ? C2_1 H2A_1 0.9800 . ? C2_1 H2B_1 0.9800 . ? C2_1 H2C_1 0.9800 . ? C3_1 C4_1 1.434(6) . ? C3_1 C8_1 1.445(6) . ? C3_1 W1_2 2.303(4) . ? C4_1 C5_1 1.402(7) . ? C4_1 W1_2 2.322(4) . ? C4_1 H4_1 1.0000 . ? C5_1 C6_1 1.423(7) . ? C5_1 C9_1 1.519(7) . ? C5_1 W1_2 2.407(5) . ? C6_1 C7_1 1.426(7) . ? C6_1 C10_1 1.506(7) . ? C6_1 W1_2 2.374(5) . ? C7_1 C8_1 1.414(6) . ? C7_1 W1_2 2.363(5) . ? C7_1 H7_1 1.0000 . ? C8_1 W1_2 2.319(4) . ? C9_1 H9A_1 0.9800 . ? C9_1 H9B_1 0.9800 . ? C9_1 H9C_1 0.9800 . ? C10_1 H10A_1 0.9800 . ? C10_1 H10B_1 0.9800 . ? C10_1 H10C_1 0.9800 . ? W1_2 C2_2 1.959(6) . ? W1_2 C3_2 1.959(6) . ? W1_2 C1_2 1.973(5) . ? O1_2 C1_2 1.155(6) . ? O2_2 C2_2 1.165(7) . ? O3_2 C3_2 1.154(8) . ? 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 C2_1 B1_1 C3_1 C4_1 -7.9(7) . . . . ? C8_1 B1_1 C3_1 C4_1 173.6(4) 3_666 . . . ? C2_1 B1_1 C3_1 C8_1 -172.9(4) . . . . ? C8_1 B1_1 C3_1 C8_1 8.7(7) 3_666 . . . ? C2_1 B1_1 C3_1 W1_2 -90.7(5) . . . . ? C8_1 B1_1 C3_1 W1_2 90.9(4) 3_666 . . . ? C8_1 C3_1 C4_1 C5_1 1.0(7) . . . . ? B1_1 C3_1 C4_1 C5_1 -164.4(5) . . . . ? W1_2 C3_1 C4_1 C5_1 -57.9(4) . . . . ? C8_1 C3_1 C4_1 W1_2 58.9(3) . . . . ? B1_1 C3_1 C4_1 W1_2 -106.5(4) . . . . ? C3_1 C4_1 C5_1 C6_1 2.1(8) . . . . ? W1_2 C4_1 C5_1 C6_1 -53.6(4) . . . . ? C3_1 C4_1 C5_1 C9_1 -177.9(5) . . . . ? W1_2 C4_1 C5_1 C9_1 126.4(5) . . . . ? C3_1 C4_1 C5_1 W1_2 55.7(4) . . . . ? C4_1 C5_1 C6_1 C7_1 -5.8(7) . . . . ? C9_1 C5_1 C6_1 C7_1 174.2(5) . . . . ? W1_2 C5_1 C6_1 C7_1 -58.5(4) . . . . ? C4_1 C5_1 C6_1 C10_1 178.3(5) . . . . ? C9_1 C5_1 C6_1 C10_1 -1.7(8) . . . . ? W1_2 C5_1 C6_1 C10_1 125.6(5) . . . . ? C4_1 C5_1 C6_1 W1_2 52.7(4) . . . . ? C9_1 C5_1 C6_1 W1_2 -127.3(5) . . . . ? C5_1 C6_1 C7_1 C8_1 6.8(7) . . . . ? C10_1 C6_1 C7_1 C8_1 -177.2(5) . . . . ? W1_2 C6_1 C7_1 C8_1 -52.7(4) . . . . ? C5_1 C6_1 C7_1 W1_2 59.5(4) . . . . ? C10_1 C6_1 C7_1 W1_2 -124.5(5) . . . . ? C6_1 C7_1 C8_1 C3_1 -3.7(7) . . . . ? W1_2 C7_1 C8_1 C3_1 -57.3(4) . . . . ? C6_1 C7_1 C8_1 B1_1 170.6(4) . . . 3_666 ? W1_2 C7_1 C8_1 B1_1 116.9(4) . . . 3_666 ? C6_1 C7_1 C8_1 W1_2 53.6(4) . . . . ? C4_1 C3_1 C8_1 C7_1 -0.3(6) . . . . ? B1_1 C3_1 C8_1 C7_1 165.2(4) . . . . ? W1_2 C3_1 C8_1 C7_1 58.8(4) . . . . ? C4_1 C3_1 C8_1 B1_1 -174.4(4) . . . 3_666 ? B1_1 C3_1 C8_1 B1_1 -8.9(7) . . . 3_666 ? W1_2 C3_1 C8_1 B1_1 -115.4(4) . . . 3_666 ? C4_1 C3_1 C8_1 W1_2 -59.0(3) . . . . ? B1_1 C3_1 C8_1 W1_2 106.5(4) . . . . ?