#------------------------------------------------------------------------------ #$Date: 2026-05-22 23:10:54 +0100 (Fri, 22 May 2026) $ #$Revision: 306070 $ #$URL: svn://www.crystallography.net/cod/cif/1/57/72/1577291.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_1577291 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 Mo2 O6' _chemical_formula_sum 'C24 H22 B2 Mo2 O6' _chemical_formula_weight 619.91 _chemical_name_common {eta6,eta'6-[2,3,6,7,9,10-Me6-9,10-DHDBA]}{Mo(CO)3}2 _chemical_name_systematic 2-Mo2 _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 2025-01-24 _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 101.946(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.49810(10) _cell_length_b 10.5870(2) _cell_length_c 13.5435(2) _cell_measurement_reflns_used 13325 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 72.2310 _cell_measurement_theta_min 5.3000 _cell_volume 1192.11(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 0.988 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): -------------------------------------------------------------------------- 1 \w 50.00 81.00 0.50 0.84 -- 34.00 49.00 101.00 62 2 \w -91.00 -56.00 0.50 0.84 -- -42.00 -40.00 143.04 70 3 \w -92.00 -61.00 0.50 0.84 -- -46.00 -52.00 -41.02 62 4 \w -99.00 -64.00 0.50 0.84 -- -50.00 -38.00 -31.47 70 5 \w -97.00 -66.00 0.50 0.84 -- -50.00 -50.00 -65.62 62 6 \w -100.00 -70.00 0.50 0.84 -- -54.00 -51.00 -85.24 60 7 \w -100.00 -69.00 0.50 0.84 -- -54.00 -52.00 127.54 62 8 \w -105.00 -74.00 0.50 0.84 -- -58.00 -48.00-159.09 62 9 \w 19.00 65.00 0.50 0.84 -- 60.01 -95.00 -90.00 92 10 \w -110.00 -77.00 0.50 0.84 -- -62.00 -45.00 80.20 66 11 \w -119.00 -84.00 0.50 0.84 -- -70.00 -36.00 117.72 70 12 \w -119.00 -84.00 0.50 0.84 -- -70.00 -39.00 14.90 70 13 \w -122.00 -89.00 0.50 0.84 -- -74.00 -42.00 -18.61 66 14 \w -122.00 -89.00 0.50 0.84 -- -74.00 -43.00 -50.30 66 15 \w -123.00 -88.00 0.50 0.84 -- -74.00 -37.00 0.25 70 16 \w -124.00 -56.00 0.50 0.84 -- -76.37 -15.00-150.00 136 17 \w -92.00 -33.00 0.50 0.84 -- -76.37 112.00-180.00 118 18 \w -92.00 -33.00 0.50 0.84 -- -76.37 112.00 120.00 118 19 \w -92.00 -33.00 0.50 0.84 -- -76.37 112.00 30.00 118 20 \w -124.00 -56.00 0.50 0.84 -- -76.37 -15.00 90.00 136 21 \w -92.00 -33.00 0.50 0.84 -- -76.37 112.00 0.00 118 22 \w -124.00 -56.00 0.50 0.84 -- -76.37 -15.00 90.00 136 23 \w -128.00 -94.00 0.50 0.84 -- -79.50 -42.00 72.32 68 24 \w -128.00 -94.00 0.50 0.84 -- -79.50 -40.00 172.85 68 25 \w -97.00 -36.00 0.50 0.84 -- -79.50 114.00 82.13 122 26 \w -125.00 -95.00 0.50 0.84 -- -79.50 -54.00-136.47 60 27 \w -97.00 -36.00 0.50 0.84 -- -79.50 115.00 -2.12 122 28 \w -97.00 -36.00 0.50 0.84 -- -79.50 115.00-167.09 122 29 \w -97.00 -36.00 0.50 0.84 -- -79.50 115.00 -76.00 122 30 \w -99.00 -34.00 0.50 0.84 -- -79.50 122.00 -0.31 130 31 \w -97.00 -36.00 0.50 0.84 -- -79.50 115.00 133.10 122 32 \w -97.00 -36.00 0.50 0.84 -- -79.50 114.00-114.47 122 33 \w -126.00 -96.00 0.50 0.84 -- -79.50 -49.00 -71.44 60 34 \w -97.00 -36.00 0.50 0.84 -- -79.50 115.00 -35.08 122 35 \w -97.00 -35.00 0.50 0.84 -- -79.50 116.00-155.09 124 36 \w 54.00 128.00 0.50 0.84 -- 80.30 15.00 60.00 148 37 \w 54.00 128.00 0.50 0.84 -- 80.30 15.00 -60.00 148 38 \w 54.00 128.00 0.50 0.84 -- 80.30 15.00 -60.00 148 39 \w 37.00 92.00 0.50 0.84 -- 80.30-112.00 90.00 110 40 \w 40.00 86.00 0.50 0.84 -- 80.30 -95.00 90.00 92 41 \w 37.00 92.00 0.50 0.84 -- 80.30-112.00 0.00 110 42 \w 37.00 92.00 0.50 0.84 -- 80.30-112.00-150.00 110 43 \w 20.00 49.00 0.50 0.84 -- 6.00 62.00-178.72 58 44 \w 20.00 50.00 0.50 0.84 -- 6.00 60.00 41.76 60 45 \w -26.00 0.00 0.50 0.84 -- -14.00 105.00 -81.48 52 46 \w -38.00 -9.00 0.50 0.84 -- -18.00 119.00 121.43 58 47 \w 32.00 60.00 0.50 0.84 -- 18.00 58.00 78.36 56 48 \w -77.00 -46.00 0.50 0.84 -- -30.00 -50.00-146.62 62 49 \w -85.00 -17.00 0.50 0.84 -- -61.71 125.00 -30.00 136 50 \w -118.00 -85.00 0.50 0.84 -- -70.00 -45.00 48.77 66 51 \w -119.00 -89.00 0.50 0.84 -- -74.00 -55.00 161.00 60 52 \w -118.00 -88.00 0.50 0.84 -- -74.00 -59.00 -90.40 60 53 \w -120.00 -89.00 0.50 0.84 -- -74.00 -54.00-161.03 62 54 \w -124.00 -56.00 0.50 0.84 -- -76.37 -15.00 30.00 136 55 \w -124.00 -94.00 0.50 0.84 -- -79.50 -57.00-108.49 60 56 \w -126.00 -95.00 0.50 0.84 -- -79.50 -51.00 -48.21 62 57 \w -102.00 -34.00 0.50 0.84 -- -79.50 130.00 88.41 136 58 \w -101.00 -34.00 0.50 0.84 -- -79.50 128.00 149.25 134 59 \w -127.00 -95.00 0.50 0.84 -- -79.50 -48.00 -29.79 64 60 \w -125.00 -94.00 0.50 0.84 -- -79.50 -53.00 123.98 62 ; _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 0.1304308000 _diffrn_orient_matrix_UB_12 0.0330991000 _diffrn_orient_matrix_UB_13 0.0935285000 _diffrn_orient_matrix_UB_21 0.1235383000 _diffrn_orient_matrix_UB_22 -0.0785497000 _diffrn_orient_matrix_UB_23 -0.0424076000 _diffrn_orient_matrix_UB_31 0.0457154000 _diffrn_orient_matrix_UB_32 0.1178428000 _diffrn_orient_matrix_UB_33 -0.0545504000 _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 0.0351 _diffrn_reflns_av_unetI/netI 0.0153 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 27163 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.771 _diffrn_reflns_theta_min 5.348 _diffrn_source 'rotating-anode X-ray tube' _diffrn_source_type 'PhotonJet-R X-ray Source' _exptl_absorpt_coefficient_mu 8.939 _exptl_absorpt_correction_T_max 0.890 _exptl_absorpt_correction_T_min 0.535 _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 1.727 _exptl_crystal_description block _exptl_crystal_F_000 616 _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 0.090 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.020 _refine_diff_density_max 0.500 _refine_diff_density_min -0.765 _refine_diff_density_rms 0.083 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 157 _refine_ls_number_reflns 2381 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.089 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0276 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+2.8540P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0707 _refine_ls_wR_factor_ref 0.0724 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2171 _reflns_number_total 2381 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6sc02501c2.cif _cod_data_source_block AlGe034_AlGe_a _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1577291 _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 0.500 _shelx_estimated_absorpt_t_max 0.841 _shelx_res_file ; TITL AlGe034_AlGe_a.res in P2(1)/n AlGe034_AlGe_a.res created by SHELXL-2019/2 at 11:56:53 on 24-Jan-2025 REM Old TITL AlGe034_AlGe in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.057, Rweak 0.019, Alpha 0.035, Orientation as input REM Formula found by SHELXT: C13 O3 Mo CELL 1.54184 8.4981 10.5870 13.5435 90.000 101.946 90.000 ZERR 2.000 0.0001 0.0002 0.0002 0.000 0.002 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H B O MO UNIT 48 44 4 12 4 TEMP -173 SIZE 0.02 0.05 0.09 L.S. 10 BOND $H LIST 4 CONF ACTA FMAP 2 PLAN 20 OMIT -2 4 13 OMIT -2 6 13 OMIT -2 2 13 WGHT 0.028900 2.854000 FVAR 0.40634 RESI 1 DBA B1 3 0.512288 0.004709 0.613923 11.00000 0.02339 0.01456 = 0.01813 0.00064 0.00078 -0.00258 C2 1 0.521703 0.012771 0.730976 11.00000 0.02400 0.03256 = 0.01631 0.00076 0.00279 -0.00823 AFIX 137 H2A 2 0.412691 0.012805 0.744341 11.00000 -1.50000 H2B 2 0.577073 0.090721 0.757342 11.00000 -1.50000 H2C 2 0.581213 -0.060190 0.764171 11.00000 -1.50000 AFIX 0 C3 1 0.658509 0.040208 0.567998 11.00000 0.02220 0.01394 = 0.01664 0.00192 0.00153 -0.00082 C4 1 0.800527 0.094036 0.629168 11.00000 0.02191 0.01807 = 0.01660 0.00137 0.00003 0.00004 AFIX 13 H4 2 0.802638 0.105812 0.702691 11.00000 -1.20000 AFIX 0 C5 1 0.923602 0.150476 0.589782 11.00000 0.01964 0.01797 = 0.02192 -0.00094 -0.00012 0.00004 C6 1 0.906869 0.154783 0.482290 11.00000 0.02180 0.01737 = 0.02170 -0.00110 0.00635 0.00122 C7 1 0.774257 0.095603 0.420963 11.00000 0.02622 0.01747 = 0.01818 -0.00219 0.00683 -0.00007 AFIX 13 H7 2 0.757241 0.108895 0.346402 11.00000 -1.20000 AFIX 0 C8 1 0.645606 0.042386 0.459629 11.00000 0.02318 0.01420 = 0.01775 -0.00067 0.00364 -0.00133 C9 1 1.072964 0.201669 0.659256 11.00000 0.01975 0.02781 = 0.02502 -0.00552 0.00165 -0.00345 AFIX 137 H9A 2 1.164568 0.146497 0.656540 11.00000 -1.50000 H9B 2 1.055605 0.204658 0.728534 11.00000 -1.50000 H9C 2 1.095323 0.286965 0.637628 11.00000 -1.50000 AFIX 0 C10 1 1.035679 0.213988 0.436140 11.00000 0.02466 0.02647 = 0.02890 -0.00264 0.01100 -0.00316 AFIX 137 H10A 2 1.132236 0.160926 0.450066 11.00000 -1.50000 H10B 2 1.061637 0.298046 0.465288 11.00000 -1.50000 H10C 2 0.997041 0.221546 0.363016 11.00000 -1.50000 AFIX 0 RESI 0 RESI 2 MOCO MO1 5 0.668590 0.248623 0.516870 11.00000 0.01933 0.01813 = 0.01624 0.00024 0.00285 -0.00144 C2 1 0.462663 0.294477 0.427595 11.00000 0.02528 0.02723 = 0.02001 0.00339 0.00705 -0.00212 C3 1 0.590545 0.338510 0.627084 11.00000 0.03285 0.02475 = 0.02192 0.00306 0.00268 0.00187 C4 1 0.747745 0.412547 0.475173 11.00000 0.02073 0.02984 = 0.02989 -0.00180 0.00413 0.00073 O5 4 0.343592 0.320744 0.373960 11.00000 0.02186 0.04904 = 0.02926 0.01108 0.00025 0.00044 O6 4 0.544537 0.388214 0.690397 11.00000 0.05408 0.03756 = 0.02480 -0.00319 0.01379 0.00900 O7 4 0.795694 0.504861 0.448227 11.00000 0.03920 0.02380 = 0.05374 0.00626 0.01398 -0.00601 RESI 0 REM REM AlGe034_AlGe_a.hkl REM HKLF 4 REM AlGe034_AlGe_a.res in P2(1)/n REM wR2 = 0.0724, GooF = S = 1.089, Restrained GooF = 1.089 for all data REM R1 = 0.0276 for 2171 Fo > 4sig(Fo) and 0.0305 for all 2381 data REM 157 parameters refined using 0 restraints END WGHT 0.0288 2.8585 REM Highest difference peak 0.500, deepest hole -0.765, 1-sigma level 0.083 Q1 1 0.5402 0.2541 0.4402 11.00000 0.05 0.50 Q2 1 0.6524 0.3569 0.5763 11.00000 0.05 0.42 Q3 1 0.5777 0.0091 0.4254 11.00000 0.05 0.41 Q4 1 0.9915 0.1688 0.6196 11.00000 0.05 0.36 Q5 1 0.8600 0.1256 0.6053 11.00000 0.05 0.34 Q6 1 0.7234 0.0652 0.5886 11.00000 0.05 0.34 Q7 1 0.5985 0.0423 0.5975 11.00000 0.05 0.33 Q8 1 0.7105 0.0661 0.4378 11.00000 0.05 0.33 Q9 1 0.6792 0.3666 0.4546 11.00000 0.05 0.31 Q10 1 0.9013 0.1556 0.5367 11.00000 0.05 0.31 Q11 1 0.7929 0.2350 0.5967 11.00000 0.05 0.30 Q12 1 0.6513 0.0372 0.5088 11.00000 0.05 0.30 Q13 1 0.5680 0.1883 0.5203 11.00000 0.05 0.29 Q14 1 0.8218 0.0754 0.6779 11.00000 0.05 0.29 Q15 1 0.4892 0.2488 0.5594 11.00000 0.05 0.28 Q16 1 0.6933 0.1186 0.4603 11.00000 0.05 0.28 Q17 1 0.6551 0.1119 0.5591 11.00000 0.05 0.27 Q18 1 0.6108 0.3512 0.4766 11.00000 0.05 0.27 Q19 1 0.3856 0.2536 0.5719 11.00000 0.05 0.27 Q20 1 0.6644 0.1632 0.5976 11.00000 0.05 0.27 ; _shelx_res_checksum 13068 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 0.5123(4) 0.0047(3) 0.6139(2) 0.0192(6) Uani 1 1 d . . . . . C2_1 C 0.5217(4) 0.0128(3) 0.7310(2) 0.0245(6) Uani 1 1 d . . . . . H2A_1 H 0.412691 0.012805 0.744341 0.037 Uiso 1 1 calc R U . . . H2B_1 H 0.577073 0.090721 0.757342 0.037 Uiso 1 1 calc R U . . . H2C_1 H 0.581213 -0.060190 0.764171 0.037 Uiso 1 1 calc R U . . . C3_1 C 0.6585(3) 0.0402(3) 0.5680(2) 0.0180(6) Uani 1 1 d . . . . . C4_1 C 0.8005(3) 0.0940(3) 0.6292(2) 0.0194(6) Uani 1 1 d . . . . . H4_1 H 0.802638 0.105812 0.702691 0.023 Uiso 1 1 calc R U . . . C5_1 C 0.9236(3) 0.1505(3) 0.5898(2) 0.0205(6) Uani 1 1 d . . . . . C6_1 C 0.9069(3) 0.1548(3) 0.4823(2) 0.0200(6) Uani 1 1 d . . . . . C7_1 C 0.7743(4) 0.0956(3) 0.4210(2) 0.0203(6) Uani 1 1 d . . . . . H7_1 H 0.757241 0.108895 0.346402 0.024 Uiso 1 1 calc R U . . . C8_1 C 0.6456(3) 0.0424(3) 0.4596(2) 0.0185(6) Uani 1 1 d . . . . . C9_1 C 1.0730(4) 0.2017(3) 0.6593(2) 0.0246(6) Uani 1 1 d . . . . . H9A_1 H 1.164568 0.146497 0.656540 0.037 Uiso 1 1 calc R U . . . H9B_1 H 1.055605 0.204658 0.728534 0.037 Uiso 1 1 calc R U . . . H9C_1 H 1.095323 0.286965 0.637628 0.037 Uiso 1 1 calc R U . . . C10_1 C 1.0357(4) 0.2140(3) 0.4361(2) 0.0259(6) Uani 1 1 d . . . . . H10A_1 H 1.132236 0.160926 0.450066 0.039 Uiso 1 1 calc R U . . . H10B_1 H 1.061637 0.298046 0.465288 0.039 Uiso 1 1 calc R U . . . H10C_1 H 0.997041 0.221546 0.363016 0.039 Uiso 1 1 calc R U . . . Mo1_2 Mo 0.66859(3) 0.24862(2) 0.51687(2) 0.01802(10) Uani 1 1 d . . . . . C2_2 C 0.4627(4) 0.2945(3) 0.4276(2) 0.0238(6) Uani 1 1 d . . . . . C3_2 C 0.5905(4) 0.3385(3) 0.6271(2) 0.0269(7) Uani 1 1 d . . . . . C4_2 C 0.7477(4) 0.4125(3) 0.4752(2) 0.0270(7) Uani 1 1 d . . . . . O5_2 O 0.3436(3) 0.3207(3) 0.37396(17) 0.0341(6) Uani 1 1 d . . . . . O6_2 O 0.5445(3) 0.3882(2) 0.69040(17) 0.0380(6) Uani 1 1 d . . . . . O7_2 O 0.7957(3) 0.5049(2) 0.4482(2) 0.0383(6) 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 0.0234(16) 0.0146(15) 0.0181(15) 0.0006(12) 0.0008(13) -0.0026(12) C2_1 0.0240(15) 0.0326(17) 0.0163(14) 0.0008(12) 0.0028(11) -0.0082(13) C3_1 0.0222(14) 0.0139(13) 0.0166(13) 0.0019(10) 0.0015(11) -0.0008(11) C4_1 0.0219(14) 0.0181(14) 0.0166(13) 0.0014(11) 0.0000(11) 0.0000(11) C5_1 0.0196(14) 0.0180(14) 0.0219(14) -0.0009(11) -0.0001(11) 0.0000(11) C6_1 0.0218(14) 0.0174(14) 0.0217(14) -0.0011(11) 0.0064(11) 0.0012(11) C7_1 0.0262(15) 0.0175(14) 0.0182(13) -0.0022(11) 0.0068(11) -0.0001(12) C8_1 0.0232(14) 0.0142(13) 0.0178(13) -0.0007(11) 0.0036(11) -0.0013(11) C9_1 0.0198(14) 0.0278(16) 0.0250(15) -0.0055(13) 0.0016(12) -0.0035(12) C10_1 0.0247(15) 0.0265(16) 0.0289(16) -0.0026(13) 0.0110(13) -0.0032(13) Mo1_2 0.01933(14) 0.01813(15) 0.01624(14) 0.00024(8) 0.00285(10) -0.00144(9) C2_2 0.0253(15) 0.0272(16) 0.0200(14) 0.0034(12) 0.0071(12) -0.0021(13) C3_2 0.0328(17) 0.0248(16) 0.0219(15) 0.0031(13) 0.0027(13) 0.0019(13) C4_2 0.0207(14) 0.0298(17) 0.0299(16) -0.0018(13) 0.0041(12) 0.0007(13) O5_2 0.0219(11) 0.0490(15) 0.0293(12) 0.0111(11) 0.0002(10) 0.0004(11) O6_2 0.0541(16) 0.0376(14) 0.0248(12) -0.0032(11) 0.0138(11) 0.0090(12) O7_2 0.0392(14) 0.0238(13) 0.0537(16) 0.0063(11) 0.0140(12) -0.0060(11) 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' Mo Mo -0.0483 2.7339 '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 0 1 0.0469 -1 1 1 0.0377 0 1 0 0.0046 0 -1 0 0.0204 0 -1 -1 0.0194 0 1 1 0.0116 -1 0 -1 0.0431 0 1 -1 0.0107 0 -1 1 0.0148 -1 1 -1 0.0361 -1 0 0 0.0483 1 -1 1 0.0320 1 1 -1 0.0279 -1 -1 1 0.0402 1 -1 0 0.0328 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_1 121.0(3) . . ? C3_1 B1_1 C8_1 118.2(2) . 3_656 ? C2_1 B1_1 C8_1 120.8(3) . 3_656 ? 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(3) . . ? C4_1 C3_1 B1_1 121.0(2) . . ? C8_1 C3_1 B1_1 120.8(2) . . ? C4_1 C3_1 Mo1_2 73.48(16) . . ? C8_1 C3_1 Mo1_2 71.47(15) . . ? B1_1 C3_1 Mo1_2 115.70(19) . . ? C5_1 C4_1 C3_1 123.7(3) . . ? C5_1 C4_1 Mo1_2 75.58(17) . . ? C3_1 C4_1 Mo1_2 70.82(15) . . ? C5_1 C4_1 H4_1 117.7 . . ? C3_1 C4_1 H4_1 117.7 . . ? Mo1_2 C4_1 H4_1 117.7 . . ? C4_1 C5_1 C6_1 118.3(3) . . ? C4_1 C5_1 C9_1 120.7(3) . . ? C6_1 C5_1 C9_1 120.9(3) . . ? C4_1 C5_1 Mo1_2 70.31(16) . . ? C6_1 C5_1 Mo1_2 71.34(16) . . ? C9_1 C5_1 Mo1_2 131.6(2) . . ? C7_1 C6_1 C5_1 119.1(3) . . ? C7_1 C6_1 C10_1 120.3(3) . . ? C5_1 C6_1 C10_1 120.5(3) . . ? C7_1 C6_1 Mo1_2 72.04(16) . . ? C5_1 C6_1 Mo1_2 73.98(16) . . ? C10_1 C6_1 Mo1_2 128.9(2) . . ? C6_1 C7_1 C8_1 122.9(3) . . ? C6_1 C7_1 Mo1_2 73.66(16) . . ? C8_1 C7_1 Mo1_2 70.20(16) . . ? C6_1 C7_1 H7_1 117.8 . . ? C8_1 C7_1 H7_1 117.8 . . ? Mo1_2 C7_1 H7_1 117.8 . . ? C7_1 C8_1 C3_1 118.4(3) . . ? C7_1 C8_1 B1_1 120.7(2) . 3_656 ? C3_1 C8_1 B1_1 120.7(2) . 3_656 ? C7_1 C8_1 Mo1_2 74.42(16) . . ? C3_1 C8_1 Mo1_2 72.06(15) . . ? B1_1 C8_1 Mo1_2 120.81(19) 3_656 . ? 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 Mo1_2 C4_2 85.43(13) . . ? C2_2 Mo1_2 C3_2 87.19(13) . . ? C4_2 Mo1_2 C3_2 88.89(13) . . ? C2_2 Mo1_2 C8_1 91.39(12) . . ? C4_2 Mo1_2 C8_1 137.77(12) . . ? C3_2 Mo1_2 C8_1 133.08(12) . . ? C2_2 Mo1_2 C3_1 109.54(12) . . ? C4_2 Mo1_2 C3_1 162.22(12) . . ? C3_2 Mo1_2 C3_1 101.06(11) . . ? C8_1 Mo1_2 C3_1 36.47(10) . . ? C2_2 Mo1_2 C4_1 144.22(11) . . ? C4_2 Mo1_2 C4_1 130.35(11) . . ? C3_2 Mo1_2 C4_1 92.05(11) . . ? C8_1 Mo1_2 C4_1 63.64(10) . . ? C3_1 Mo1_2 C4_1 35.70(9) . . ? C2_2 Mo1_2 C7_1 102.80(12) . . ? C4_2 Mo1_2 C7_1 104.65(11) . . ? C3_2 Mo1_2 C7_1 163.63(12) . . ? C8_1 Mo1_2 C7_1 35.38(10) . . ? C3_1 Mo1_2 C7_1 63.53(10) . . ? C4_1 Mo1_2 C7_1 72.22(10) . . ? C2_2 Mo1_2 C6_1 131.58(11) . . ? C4_2 Mo1_2 C6_1 87.53(11) . . ? C3_2 Mo1_2 C6_1 140.52(12) . . ? C8_1 Mo1_2 C6_1 63.73(10) . . ? C3_1 Mo1_2 C6_1 75.40(10) . . ? C4_1 Mo1_2 C6_1 61.81(10) . . ? C7_1 Mo1_2 C6_1 34.30(10) . . ? C2_2 Mo1_2 C5_1 164.12(12) . . ? C4_2 Mo1_2 C5_1 99.43(11) . . ? C3_2 Mo1_2 C5_1 107.91(11) . . ? C8_1 Mo1_2 C5_1 74.80(10) . . ? C3_1 Mo1_2 C5_1 63.60(10) . . ? C4_1 Mo1_2 C5_1 34.11(10) . . ? C7_1 Mo1_2 C5_1 61.38(10) . . ? C6_1 Mo1_2 C5_1 34.68(9) . . ? O5_2 C2_2 Mo1_2 178.8(3) . . ? O6_2 C3_2 Mo1_2 178.9(3) . . ? O7_2 C4_2 Mo1_2 177.4(3) . . ? 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 1.547(4) . ? B1_1 C2_1 1.573(4) . ? B1_1 C8_1 1.577(4) 3_656 ? C2_1 H2A_1 0.9800 . ? C2_1 H2B_1 0.9800 . ? C2_1 H2C_1 0.9800 . ? C3_1 C4_1 1.433(4) . ? C3_1 C8_1 1.449(4) . ? C3_1 Mo1_2 2.319(3) . ? C4_1 C5_1 1.402(4) . ? C4_1 Mo1_2 2.354(3) . ? C4_1 H4_1 1.0000 . ? C5_1 C6_1 1.434(4) . ? C5_1 C9_1 1.515(4) . ? C5_1 Mo1_2 2.422(3) . ? C6_1 C7_1 1.402(4) . ? C6_1 C10_1 1.505(4) . ? C6_1 Mo1_2 2.387(3) . ? C7_1 C8_1 1.423(4) . ? C7_1 Mo1_2 2.367(3) . ? C7_1 H7_1 1.0000 . ? C8_1 Mo1_2 2.312(3) . ? 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 . ? Mo1_2 C2_2 1.971(3) . ? Mo1_2 C4_2 1.985(3) . ? Mo1_2 C3_2 1.996(3) . ? C2_2 O5_2 1.151(4) . ? C3_2 O6_2 1.142(4) . ? C4_2 O7_2 1.147(4) . ? 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 -6.7(4) . . . . ? C8_1 B1_1 C3_1 C4_1 174.5(3) 3_656 . . . ? C2_1 B1_1 C3_1 C8_1 -175.0(3) . . . . ? C8_1 B1_1 C3_1 C8_1 6.1(4) 3_656 . . . ? C2_1 B1_1 C3_1 Mo1_2 -92.1(3) . . . . ? C8_1 B1_1 C3_1 Mo1_2 89.0(3) 3_656 . . . ? C8_1 C3_1 C4_1 C5_1 1.6(4) . . . . ? B1_1 C3_1 C4_1 C5_1 -167.2(3) . . . . ? Mo1_2 C3_1 C4_1 C5_1 -56.7(3) . . . . ? C8_1 C3_1 C4_1 Mo1_2 58.3(2) . . . . ? B1_1 C3_1 C4_1 Mo1_2 -110.5(3) . . . . ? C3_1 C4_1 C5_1 C6_1 0.0(4) . . . . ? Mo1_2 C4_1 C5_1 C6_1 -54.6(2) . . . . ? C3_1 C4_1 C5_1 C9_1 -178.0(3) . . . . ? Mo1_2 C4_1 C5_1 C9_1 127.4(3) . . . . ? C3_1 C4_1 C5_1 Mo1_2 54.6(3) . . . . ? C4_1 C5_1 C6_1 C7_1 -4.1(4) . . . . ? C9_1 C5_1 C6_1 C7_1 173.9(3) . . . . ? Mo1_2 C5_1 C6_1 C7_1 -58.2(2) . . . . ? C4_1 C5_1 C6_1 C10_1 -179.8(3) . . . . ? C9_1 C5_1 C6_1 C10_1 -1.8(4) . . . . ? Mo1_2 C5_1 C6_1 C10_1 126.1(3) . . . . ? C4_1 C5_1 C6_1 Mo1_2 54.1(2) . . . . ? C9_1 C5_1 C6_1 Mo1_2 -127.9(3) . . . . ? C5_1 C6_1 C7_1 C8_1 6.8(4) . . . . ? C10_1 C6_1 C7_1 C8_1 -177.4(3) . . . . ? Mo1_2 C6_1 C7_1 C8_1 -52.4(3) . . . . ? C5_1 C6_1 C7_1 Mo1_2 59.2(2) . . . . ? C10_1 C6_1 C7_1 Mo1_2 -125.1(3) . . . . ? C6_1 C7_1 C8_1 C3_1 -5.1(4) . . . . ? Mo1_2 C7_1 C8_1 C3_1 -59.0(2) . . . . ? C6_1 C7_1 C8_1 B1_1 170.8(3) . . . 3_656 ? Mo1_2 C7_1 C8_1 B1_1 116.9(3) . . . 3_656 ? C6_1 C7_1 C8_1 Mo1_2 53.9(3) . . . . ? C4_1 C3_1 C8_1 C7_1 0.9(4) . . . . ? B1_1 C3_1 C8_1 C7_1 169.7(3) . . . . ? Mo1_2 C3_1 C8_1 C7_1 60.2(2) . . . . ? C4_1 C3_1 C8_1 B1_1 -175.1(3) . . . 3_656 ? B1_1 C3_1 C8_1 B1_1 -6.3(4) . . . 3_656 ? Mo1_2 C3_1 C8_1 B1_1 -115.7(3) . . . 3_656 ? C4_1 C3_1 C8_1 Mo1_2 -59.4(2) . . . . ? B1_1 C3_1 C8_1 Mo1_2 109.4(3) . . . . ?