# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Morales, Dolores' _publ_contact_author_email moralesdolores.uo@uniovi.es _publ_section_title ; Hydrogen-bonded adducts between neutral molecules and [Mo(h3-methallyl)(CO)2(HOC(py)3)]+: snapshots of a deprotonation ; loop_ _publ_author_name D.Morales J.Perez H.Martinez-Garcia M.Puerto 'I.del Rio' # Attachment 'CIFS.cif' data_1H_(mp121) _database_code_depnum_ccdc_archive 'CCDC 786107' #TrackingRef 'CIFS.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H12 B F24, C22 H20 Mo N3 O3' _chemical_formula_sum 'C54 H32 B F24 Mo N3 O3' _chemical_formula_weight 1333.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2834(2) _cell_length_b 13.4971(2) _cell_length_c 19.7289(2) _cell_angle_alpha 87.6610(10) _cell_angle_beta 79.1610(10) _cell_angle_gamma 89.2440(10) _cell_volume 2687.16(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9781 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 25.350 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.648 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.375 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.938 _exptl_absorpt_correction_T_max 0.956 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46149 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 25.36_reflns_number_total _reflns_number_gt 8367 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'DIRDIF-2008 (Beurskens et al., 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [1.00000+-1.00000exp(-110.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+1.4511*P+(0.1269P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9879 _refine_ls_number_parameters 884 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0654 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1695 _refine_ls_wR_factor_gt 0.1551 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3386(4) -0.1205(3) 0.2171(2) 0.0311(9) Uani 1 1 d . . . H1A H 0.3140 -0.1247 0.2670 0.037 Uiso 1 1 calc R . . H1B H 0.3491 -0.1845 0.1960 0.037 Uiso 1 1 calc R . . C2 C 0.4311(4) -0.0468(3) 0.1884(2) 0.0299(8) Uani 1 1 d . . . C3 C 0.4581(4) -0.0390(4) 0.1159(2) 0.0370(9) Uani 1 1 d . . . C4 C 0.4937(5) 0.0205(3) 0.2325(2) 0.0348(9) Uani 1 1 d . . . C5 C 0.1300(3) 0.1560(2) 0.26011(17) 0.0201(7) Uani 1 1 d . . . C10 C 0.1319(4) -0.1185(3) 0.17032(18) 0.0263(8) Uiso 1 1 d . . . C20 C 0.2576(4) -0.0286(3) 0.0641(2) 0.0295(8) Uiso 1 1 d . . . C31 C 0.0168(3) 0.1480(2) 0.21984(17) 0.0219(7) Uani 1 1 d . . . C32 C -0.1019(4) 0.1969(3) 0.2336(2) 0.0316(9) Uani 1 1 d . . . C33 C -0.1924(4) 0.1848(3) 0.1893(2) 0.0389(10) Uani 1 1 d . . . C34 C -0.1586(4) 0.1243(3) 0.1344(2) 0.0376(10) Uani 1 1 d . . . C35 C -0.0392(4) 0.0757(3) 0.1249(2) 0.0295(8) Uani 1 1 d . . . C41 C 0.0900(3) 0.1900(3) 0.33418(18) 0.0228(7) Uani 1 1 d . . . C42 C 0.0375(4) 0.2820(3) 0.3540(2) 0.0286(8) Uani 1 1 d . . . C43 C 0.0105(4) 0.3008(3) 0.4241(2) 0.0359(9) Uani 1 1 d . . . C44 C 0.0357(5) 0.2277(4) 0.4714(2) 0.0425(11) Uani 1 1 d . . . C45 C 0.0864(5) 0.1380(3) 0.4472(2) 0.0381(10) Uani 1 1 d . . . C51 C 0.2410(3) 0.2152(2) 0.21325(17) 0.0204(7) Uani 1 1 d . . . C52 C 0.2721(4) 0.3127(3) 0.22243(19) 0.0248(8) Uani 1 1 d . . . C53 C 0.3683(4) 0.3591(3) 0.1732(2) 0.0309(9) Uani 1 1 d . . . C54 C 0.4295(4) 0.3087(3) 0.1167(2) 0.0364(10) Uani 1 1 d . . . C55 C 0.3938(4) 0.2106(3) 0.11140(19) 0.0312(9) Uani 1 1 d . . . C61 C 0.7175(3) 0.6270(2) 0.20894(17) 0.0181(7) Uani 1 1 d . . . C62 C 0.7431(3) 0.7090(3) 0.16288(17) 0.0209(7) Uani 1 1 d . . . C63 C 0.8385(3) 0.7073(3) 0.10274(18) 0.0240(8) Uani 1 1 d . . . C64 C 0.9150(4) 0.6231(3) 0.08613(18) 0.0256(8) Uani 1 1 d . . . C65 C 0.8930(3) 0.5409(3) 0.13193(18) 0.0237(7) Uani 1 1 d . . . C66 C 0.7955(3) 0.5435(3) 0.19164(17) 0.0199(7) Uani 1 1 d . . . C67 C 0.8567(4) 0.7956(3) 0.0537(2) 0.0350(9) Uani 1 1 d . . . C68 C 0.9713(4) 0.4484(3) 0.1161(2) 0.0345(9) Uani 1 1 d . . . C71 C 0.6055(3) 0.5374(2) 0.33022(17) 0.0192(7) Uani 1 1 d . . . C72 C 0.6642(3) 0.5489(3) 0.38812(17) 0.0208(7) Uani 1 1 d . . . C73 C 0.6790(3) 0.4717(3) 0.43437(17) 0.0229(7) Uani 1 1 d . . . C74 C 0.6338(4) 0.3769(3) 0.42558(19) 0.0272(8) Uani 1 1 d . . . C75 C 0.5765(4) 0.3622(3) 0.36879(19) 0.0264(8) Uani 1 1 d . . . C76 C 0.5627(4) 0.4408(3) 0.32246(19) 0.0239(8) Uani 1 1 d . . . C77 C 0.5246(5) 0.2620(3) 0.3602(2) 0.0500(11) Uani 1 1 d . . . C78 C 0.7415(4) 0.4914(3) 0.49510(18) 0.0298(8) Uani 1 1 d . . . C81 C 0.5916(3) 0.7338(2) 0.31435(16) 0.0185(7) Uani 1 1 d . . . C82 C 0.7084(4) 0.7858(3) 0.31529(17) 0.0230(7) Uani 1 1 d . . . C83 C 0.7104(4) 0.8709(3) 0.35263(17) 0.0245(8) Uani 1 1 d . . . C84 C 0.5958(4) 0.9088(3) 0.39121(18) 0.0262(8) Uani 1 1 d . . . C85 C 0.4778(4) 0.8588(3) 0.39184(17) 0.0232(7) Uani 1 1 d . . . C86 C 0.4769(4) 0.7739(3) 0.35414(17) 0.0211(7) Uani 1 1 d . . . C87 C 0.8385(4) 0.9237(3) 0.34938(19) 0.0301(8) Uani 1 1 d . . . C88 C 0.3515(4) 0.8964(3) 0.43271(18) 0.0297(8) Uani 1 1 d . . . C91 C 0.4560(3) 0.6175(2) 0.24343(17) 0.0184(7) Uani 1 1 d . . . C92 C 0.4503(3) 0.6300(2) 0.17341(17) 0.0181(7) Uani 1 1 d . . . C93 C 0.3323(3) 0.6286(2) 0.14888(16) 0.0199(7) Uani 1 1 d . . . C94 C 0.2115(3) 0.6150(2) 0.19346(17) 0.0207(7) Uani 1 1 d . . . C95 C 0.2149(3) 0.5999(2) 0.26309(17) 0.0206(7) Uani 1 1 d . . . C96 C 0.3340(3) 0.5987(2) 0.28698(17) 0.0202(7) Uani 1 1 d . . . C97 C 0.3374(4) 0.6437(3) 0.07254(17) 0.0247(8) Uani 1 1 d . . . C98 C 0.0883(4) 0.5875(3) 0.31456(19) 0.0308(9) Uani 1 1 d . . . N1 N 0.0489(3) 0.0865(2) 0.16623(14) 0.0226(6) Uani 1 1 d . . . N2 N 0.1137(3) 0.1197(2) 0.38006(15) 0.0281(7) Uani 1 1 d . . . N3 N 0.3023(3) 0.1641(2) 0.15890(14) 0.0230(6) Uani 1 1 d . . . O1 O 0.1812(2) 0.05746(16) 0.26560(13) 0.0214(5) Uani 1 1 d . . . O10 O 0.0645(3) -0.1876(2) 0.17477(17) 0.0418(7) Uani 1 1 d . . . O20 O 0.2678(3) -0.0516(2) 0.00734(13) 0.0455(8) Uani 1 1 d . . . F1 F 0.7923(5) 0.7901(3) 0.00367(19) 0.1005(15) Uani 1 1 d . . . F2 F 0.8191(4) 0.8803(2) 0.08409(16) 0.0741(10) Uani 1 1 d . . . F3 F 0.9825(3) 0.8131(3) 0.02571(19) 0.0854(12) Uani 1 1 d . . . F4 F 1.0829(3) 0.4619(2) 0.06951(14) 0.0521(7) Uani 1 1 d . . . F5 F 0.9030(3) 0.37920(18) 0.09119(14) 0.0520(7) Uani 1 1 d . . . F6 F 1.0078(3) 0.40570(19) 0.17261(13) 0.0498(7) Uani 1 1 d . . . F7 F 0.8633(2) 0.5281(2) 0.47594(12) 0.0409(6) Uani 1 1 d . . . F8 F 0.6733(3) 0.5559(2) 0.53684(13) 0.0578(8) Uani 1 1 d . . . F9 F 0.7557(3) 0.4089(2) 0.53355(13) 0.0539(7) Uani 1 1 d . . . F10 F 0.6100(5) 0.1901(2) 0.3659(3) 0.1234(19) Uani 1 1 d . . . F11 F 0.4188(7) 0.2423(4) 0.3962(4) 0.107(5) Uani 1 1 d . . . F12 F 0.5115(5) 0.2470(2) 0.2952(2) 0.1079(16) Uani 1 1 d . . . F13 F 0.8301(3) 1.0005(3) 0.3886(2) 0.0999(15) Uani 1 1 d . . . F14 F 0.8882(3) 0.9573(3) 0.28640(15) 0.0740(10) Uani 1 1 d . . . F15 F 0.9328(3) 0.8657(2) 0.3661(2) 0.0869(13) Uani 1 1 d . . . F16 F 0.3565(3) 0.9898(3) 0.4506(2) 0.0944(14) Uani 1 1 d . . . F17 F 0.2516(3) 0.8986(3) 0.39901(16) 0.0727(10) Uani 1 1 d . . . F18 F 0.3091(4) 0.8456(3) 0.48943(18) 0.1143(19) Uani 1 1 d . . . F19 F 0.4178(3) 0.7188(2) 0.04532(12) 0.0497(7) Uani 1 1 d . . . F20 F 0.3841(3) 0.5654(2) 0.03765(12) 0.0559(8) Uani 1 1 d . . . F21 F 0.2211(2) 0.6655(3) 0.05599(12) 0.0569(8) Uani 1 1 d . . . F22 F 0.0667(3) 0.6605(2) 0.35759(17) 0.0749(10) Uani 1 1 d . . . F23 F -0.0139(3) 0.5759(5) 0.28766(15) 0.143(3) Uani 1 1 d . . . F24 F 0.0939(3) 0.5093(2) 0.35749(18) 0.0742(10) Uani 1 1 d . . . Mo1 Mo 0.23807(3) 0.00230(2) 0.160917(14) 0.02044(13) Uani 1 1 d . . . B1 B 0.5927(4) 0.6288(3) 0.27395(19) 0.0184(8) Uani 1 1 d . . . H1 H 0.170(4) 0.046(3) 0.311(2) 0.022 Uiso 1 1 d . . . H3A H 0.461(5) -0.096(4) 0.093(3) 0.047(13) Uiso 1 1 d . . . H3B H 0.516(4) 0.015(3) 0.095(2) 0.029(10) Uiso 1 1 d . . . H4A H 0.569(5) -0.012(3) 0.240(2) 0.041(12) Uiso 1 1 d . . . H4B H 0.515(5) 0.073(4) 0.208(2) 0.039(13) Uiso 1 1 d . . . H4C H 0.426(4) 0.035(3) 0.281(2) 0.027(10) Uiso 1 1 d . . . H32 H -0.119(5) 0.239(4) 0.280(2) 0.048(13) Uiso 1 1 d . . . H33 H -0.269(5) 0.211(3) 0.203(2) 0.035(12) Uiso 1 1 d . . . H34 H -0.217(4) 0.119(3) 0.107(2) 0.028(10) Uiso 1 1 d . . . H35 H -0.018(4) 0.032(3) 0.090(2) 0.027(10) Uiso 1 1 d . . . H42 H 0.028(4) 0.327(3) 0.321(2) 0.031(11) Uiso 1 1 d . . . H43 H -0.024(5) 0.359(4) 0.444(2) 0.041(12) Uiso 1 1 d . . . H44 H 0.009(5) 0.240(4) 0.523(3) 0.063(15) Uiso 1 1 d . . . H45 H 0.090(5) 0.087(4) 0.477(3) 0.061(16) Uiso 1 1 d . . . H52 H 0.231(4) 0.347(3) 0.260(2) 0.019(9) Uiso 1 1 d . . . H53 H 0.400(5) 0.427(4) 0.174(2) 0.048(13) Uiso 1 1 d . . . H54 H 0.489(5) 0.338(4) 0.080(3) 0.054(14) Uiso 1 1 d . . . H55 H 0.436(4) 0.170(3) 0.076(2) 0.030(10) Uiso 1 1 d . . . H62 H 0.690(4) 0.762(3) 0.1699(19) 0.022(10) Uiso 1 1 d . . . H64 H 0.983(5) 0.622(4) 0.044(3) 0.059(15) Uiso 1 1 d . . . H66 H 0.789(3) 0.481(3) 0.2247(18) 0.016(8) Uiso 1 1 d . . . H72 H 0.697(4) 0.609(3) 0.3969(19) 0.021(9) Uiso 1 1 d . . . H74 H 0.652(5) 0.322(4) 0.456(2) 0.047(13) Uiso 1 1 d . . . H76 H 0.525(4) 0.434(3) 0.286(2) 0.020(9) Uiso 1 1 d . . . H82 H 0.789(4) 0.765(3) 0.290(2) 0.028(10) Uiso 1 1 d . . . H84 H 0.600(4) 0.965(3) 0.414(2) 0.031(11) Uiso 1 1 d . . . H86 H 0.394(4) 0.739(3) 0.3575(17) 0.014(8) Uiso 1 1 d . . . H92 H 0.523(3) 0.641(2) 0.1403(17) 0.006(7) Uiso 1 1 d . . . H94 H 0.135(4) 0.620(3) 0.1748(18) 0.019(9) Uiso 1 1 d . . . H96 H 0.323(3) 0.582(3) 0.3369(19) 0.018(9) Uiso 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 C1 0.040(2) 0.0201(18) 0.037(2) -0.0037(15) -0.0166(18) 0.0058(16) C2 0.027(2) 0.029(2) 0.036(2) -0.0098(16) -0.0102(16) 0.0082(16) C3 0.033(2) 0.039(2) 0.038(2) -0.013(2) -0.0015(18) 0.0045(19) C4 0.035(2) 0.029(2) 0.044(3) -0.0067(19) -0.016(2) 0.0006(19) C5 0.0244(18) 0.0160(16) 0.0200(17) 0.0001(13) -0.0041(14) -0.0008(13) C31 0.0266(19) 0.0168(16) 0.0231(17) 0.0021(13) -0.0069(14) -0.0082(14) C32 0.028(2) 0.030(2) 0.038(2) -0.0021(17) -0.0080(17) -0.0040(16) C33 0.024(2) 0.047(3) 0.049(3) -0.001(2) -0.0127(19) 0.0020(19) C34 0.032(2) 0.049(3) 0.036(2) 0.0007(19) -0.0163(19) -0.0062(19) C35 0.034(2) 0.030(2) 0.0258(19) 0.0021(16) -0.0107(16) -0.0091(17) C41 0.0203(18) 0.0238(18) 0.0240(18) -0.0029(14) -0.0033(14) 0.0000(14) C42 0.027(2) 0.027(2) 0.031(2) -0.0076(17) -0.0025(16) 0.0009(16) C43 0.036(2) 0.031(2) 0.038(2) -0.0141(18) 0.0022(18) 0.0032(18) C44 0.047(3) 0.052(3) 0.026(2) -0.0126(19) -0.0002(19) 0.004(2) C45 0.052(3) 0.038(2) 0.022(2) -0.0028(18) -0.0024(18) 0.006(2) C51 0.0236(18) 0.0193(17) 0.0198(16) -0.0002(13) -0.0083(14) 0.0006(14) C52 0.032(2) 0.0183(17) 0.0262(19) -0.0004(15) -0.0111(16) -0.0025(15) C53 0.040(2) 0.0201(19) 0.034(2) 0.0035(16) -0.0102(18) -0.0112(16) C54 0.044(2) 0.034(2) 0.028(2) 0.0069(17) -0.0010(18) -0.0163(19) C55 0.040(2) 0.030(2) 0.0217(19) 0.0014(16) -0.0015(17) -0.0126(17) C61 0.0173(17) 0.0194(16) 0.0202(16) -0.0013(13) -0.0094(13) -0.0024(13) C62 0.0200(18) 0.0207(17) 0.0228(17) 0.0003(14) -0.0059(14) 0.0001(14) C63 0.0235(18) 0.0262(18) 0.0235(18) 0.0010(14) -0.0077(14) -0.0059(15) C64 0.0209(18) 0.036(2) 0.0195(17) -0.0028(15) -0.0020(15) -0.0055(15) C65 0.0220(18) 0.0259(18) 0.0234(17) -0.0053(14) -0.0036(14) -0.0018(14) C66 0.0209(18) 0.0226(17) 0.0173(16) -0.0009(13) -0.0059(13) -0.0050(14) C67 0.036(2) 0.037(2) 0.030(2) 0.0081(17) -0.0024(17) -0.0060(18) C68 0.036(2) 0.031(2) 0.034(2) -0.0080(17) 0.0028(18) 0.0026(17) C71 0.0177(17) 0.0207(17) 0.0184(16) 0.0000(13) -0.0015(13) 0.0009(13) C72 0.0169(17) 0.0239(18) 0.0201(17) -0.0026(14) 0.0003(13) -0.0009(14) C73 0.0186(17) 0.0316(19) 0.0173(16) -0.0006(14) -0.0007(13) 0.0040(14) C74 0.026(2) 0.0275(19) 0.0267(18) 0.0068(16) -0.0047(15) 0.0044(15) C75 0.0255(19) 0.0201(18) 0.033(2) 0.0011(15) -0.0039(15) 0.0006(14) C76 0.0260(19) 0.0240(18) 0.0237(18) -0.0019(14) -0.0098(15) 0.0028(15) C77 0.066(3) 0.036(2) 0.048(3) 0.0079(18) -0.022(2) -0.004(2) C78 0.028(2) 0.041(2) 0.0191(18) 0.0001(16) -0.0043(15) 0.0083(17) C81 0.0221(17) 0.0177(16) 0.0162(15) 0.0020(12) -0.0054(13) 0.0003(13) C82 0.0250(19) 0.0239(18) 0.0198(17) -0.0024(14) -0.0030(15) 0.0011(15) C83 0.031(2) 0.0241(18) 0.0195(17) 0.0007(14) -0.0063(15) -0.0068(15) C84 0.037(2) 0.0210(18) 0.0218(18) -0.0053(15) -0.0081(16) -0.0007(16) C85 0.029(2) 0.0214(17) 0.0189(17) -0.0002(13) -0.0052(14) 0.0030(14) C86 0.0218(18) 0.0232(17) 0.0188(17) -0.0006(13) -0.0051(14) -0.0024(15) C87 0.033(2) 0.0270(19) 0.030(2) -0.0045(16) -0.0058(17) -0.0054(16) C88 0.039(2) 0.030(2) 0.0220(18) -0.0078(15) -0.0082(16) 0.0057(17) C91 0.0211(17) 0.0119(15) 0.0216(16) -0.0005(12) -0.0023(13) -0.0007(13) C92 0.0186(17) 0.0164(16) 0.0177(16) -0.0005(13) 0.0005(14) -0.0012(13) C93 0.0276(19) 0.0158(16) 0.0172(16) -0.0022(13) -0.0060(14) -0.0012(13) C94 0.0195(18) 0.0195(17) 0.0249(18) -0.0045(14) -0.0082(15) -0.0002(13) C95 0.0207(18) 0.0198(17) 0.0220(17) -0.0035(13) -0.0048(14) -0.0019(13) C96 0.0249(18) 0.0202(17) 0.0159(17) -0.0021(13) -0.0040(14) -0.0019(14) C97 0.0262(19) 0.0296(19) 0.0189(17) -0.0012(14) -0.0051(14) -0.0059(15) C98 0.026(2) 0.044(2) 0.0229(18) -0.0073(17) -0.0032(15) -0.0032(17) N1 0.0268(16) 0.0198(14) 0.0215(14) 0.0022(12) -0.0058(12) -0.0081(12) N2 0.0339(18) 0.0275(16) 0.0220(15) -0.0020(12) -0.0029(13) 0.0029(13) N3 0.0266(16) 0.0219(15) 0.0207(15) -0.0005(12) -0.0050(12) -0.0049(12) O1 0.0310(14) 0.0150(12) 0.0185(12) -0.0011(9) -0.0054(10) 0.0036(10) O10 0.0461(18) 0.0225(14) 0.0607(19) 0.0004(13) -0.0201(15) -0.0096(13) O20 0.075(2) 0.0435(17) 0.0182(14) -0.0068(12) -0.0081(14) -0.0089(16) F1 0.165(4) 0.080(2) 0.082(2) 0.052(2) -0.095(3) -0.062(2) F2 0.123(3) 0.0317(15) 0.0590(18) 0.0154(13) 0.0013(18) -0.0067(16) F3 0.054(2) 0.099(3) 0.089(2) 0.061(2) 0.0095(17) -0.0146(18) F4 0.0398(15) 0.0473(15) 0.0587(16) -0.0087(13) 0.0183(13) 0.0074(12) F5 0.0548(17) 0.0360(14) 0.0637(17) -0.0215(12) -0.0031(13) -0.0026(12) F6 0.0534(16) 0.0432(15) 0.0512(15) -0.0020(12) -0.0074(12) 0.0252(12) F7 0.0290(13) 0.0633(16) 0.0329(12) -0.0059(11) -0.0109(10) -0.0036(11) F8 0.0499(16) 0.094(2) 0.0343(13) -0.0363(14) -0.0165(12) 0.0362(15) F9 0.075(2) 0.0574(17) 0.0340(13) 0.0169(12) -0.0272(13) -0.0044(14) F10 0.170(4) 0.0304(17) 0.203(5) -0.008(2) -0.122(4) 0.009(2) F11 0.188(6) 0.041(4) 0.122(9) -0.002(5) -0.102(6) -0.033(4) F12 0.191(5) 0.0450(19) 0.109(3) -0.0010(19) -0.080(3) -0.033(2) F13 0.056(2) 0.103(3) 0.134(3) -0.090(3) 0.022(2) -0.0420(19) F14 0.072(2) 0.096(2) 0.0517(17) 0.0171(16) -0.0063(15) -0.0558(19) F15 0.0489(19) 0.066(2) 0.159(4) 0.032(2) -0.060(2) -0.0217(16) F16 0.053(2) 0.063(2) 0.159(4) -0.067(2) 0.013(2) 0.0051(16) F17 0.0412(16) 0.121(3) 0.0604(18) -0.0388(18) -0.0159(14) 0.0322(17) F18 0.101(3) 0.138(4) 0.070(2) 0.061(2) 0.054(2) 0.084(3) F19 0.0687(18) 0.0570(16) 0.0247(12) 0.0118(11) -0.0130(12) -0.0309(14) F20 0.096(2) 0.0484(16) 0.0227(12) -0.0148(11) -0.0079(13) 0.0124(15) F21 0.0352(14) 0.111(2) 0.0269(12) 0.0105(14) -0.0143(11) 0.0005(15) F22 0.069(2) 0.0570(19) 0.079(2) -0.0231(16) 0.0401(17) 0.0019(15) F23 0.0221(15) 0.376(8) 0.0300(16) -0.017(3) -0.0003(12) -0.050(3) F24 0.0569(19) 0.0619(19) 0.084(2) 0.0278(17) 0.0320(16) -0.0016(15) Mo1 0.0280(2) 0.01641(18) 0.01727(19) -0.00311(12) -0.00465(13) -0.00225(12) B1 0.0198(19) 0.0193(18) 0.0171(18) -0.0005(14) -0.0060(15) -0.0014(15) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; 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 C1 C2 1.411(6) . ? C1 Mo1 2.297(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.405(6) . ? C2 C4 1.512(5) . ? C2 Mo1 2.240(4) . ? C3 Mo1 2.339(4) . ? C3 H3A 0.90(5) . ? C3 H3B 0.98(4) . ? C4 H4A 0.92(5) . ? C4 H4B 0.85(5) . ? C4 H4C 1.09(4) . ? C5 O1 1.431(4) . ? C5 C41 1.529(5) . ? C5 C31 1.536(5) . ? C5 C51 1.537(5) . ? C10 O10 1.159(5) . ? C10 Mo1 1.958(4) . ? C20 O20 1.159(5) . ? C20 Mo1 1.945(4) . ? C31 N1 1.360(5) . ? C31 C32 1.366(5) . ? C32 C33 1.407(6) . ? C32 H32 1.08(5) . ? C33 C34 1.373(7) . ? C33 H33 0.86(5) . ? C34 C35 1.369(6) . ? C34 H34 0.89(4) . ? C35 N1 1.341(5) . ? C35 H35 0.92(4) . ? C41 N2 1.337(5) . ? C41 C42 1.388(5) . ? C42 C43 1.391(6) . ? C42 H42 0.89(4) . ? C43 C44 1.386(7) . ? C43 H43 0.93(5) . ? C44 C45 1.379(6) . ? C44 H44 1.03(6) . ? C45 N2 1.333(5) . ? C45 H45 0.89(5) . ? C51 N3 1.348(5) . ? C51 C52 1.385(5) . ? C52 C53 1.386(5) . ? C52 H52 0.93(4) . ? C53 C54 1.373(6) . ? C53 H53 0.98(5) . ? C54 C55 1.392(6) . ? C54 H54 0.93(5) . ? C55 N3 1.339(5) . ? C55 H55 0.95(4) . ? C61 C66 1.392(5) . ? C61 C62 1.399(5) . ? C61 B1 1.636(5) . ? C62 C63 1.391(5) . ? C62 H62 0.89(4) . ? C63 C64 1.387(5) . ? C63 C67 1.496(5) . ? C64 C65 1.396(5) . ? C64 H64 0.98(5) . ? C65 C66 1.397(5) . ? C65 C68 1.489(5) . ? C66 H66 1.04(4) . ? C67 F1 1.292(5) . ? C67 F3 1.328(5) . ? C67 F2 1.331(5) . ? C68 F5 1.338(5) . ? C68 F4 1.338(5) . ? C68 F6 1.348(5) . ? C71 C72 1.404(5) . ? C71 C76 1.405(5) . ? C71 B1 1.647(5) . ? C72 C73 1.383(5) . ? C72 H72 0.92(4) . ? C73 C74 1.396(5) . ? C73 C78 1.497(5) . ? C74 C75 1.382(5) . ? C74 H74 0.98(5) . ? C75 C76 1.395(5) . ? C75 C77 1.488(6) . ? C76 H76 0.89(4) . ? C77 F10 1.316(6) . ? C77 F12 1.339(6) . ? C78 F8 1.325(5) . ? C78 F7 1.335(4) . ? C78 F9 1.343(5) . ? C81 C82 1.403(5) . ? C81 C86 1.403(5) . ? C81 B1 1.652(5) . ? C82 C83 1.392(5) . ? C82 H82 0.93(4) . ? C83 C84 1.381(5) . ? C83 C87 1.496(5) . ? C84 C85 1.394(5) . ? C84 H84 0.90(4) . ? C85 C86 1.392(5) . ? C85 C88 1.489(5) . ? C86 H86 0.97(4) . ? C87 F13 1.311(5) . ? C87 F14 1.316(5) . ? C87 F15 1.319(5) . ? C88 F18 1.294(5) . ? C88 F17 1.324(5) . ? C88 F16 1.327(5) . ? C91 C92 1.397(5) . ? C91 C96 1.400(5) . ? C91 B1 1.642(5) . ? C92 C93 1.389(5) . ? C92 H92 0.90(3) . ? C93 C94 1.390(5) . ? C93 C97 1.503(5) . ? C94 C95 1.387(5) . ? C94 H94 0.93(4) . ? C95 C96 1.393(5) . ? C95 C98 1.499(5) . ? C96 H96 0.99(4) . ? C97 F20 1.320(4) . ? C97 F21 1.324(4) . ? C97 F19 1.346(4) . ? C98 F23 1.277(5) . ? C98 F22 1.316(5) . ? C98 F24 1.334(5) . ? N1 Mo1 2.227(3) . ? N3 Mo1 2.286(3) . ? O1 Mo1 2.196(2) . ? O1 H1 0.88(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 C2 C1 Mo1 69.7(2) . . ? C2 C1 H1A 116.7 . . ? Mo1 C1 H1A 116.7 . . ? C2 C1 H1B 116.7 . . ? Mo1 C1 H1B 116.7 . . ? H1A C1 H1B 113.7 . . ? C3 C2 C1 114.9(4) . . ? C3 C2 C4 122.6(4) . . ? C1 C2 C4 122.5(4) . . ? C3 C2 Mo1 76.0(2) . . ? C1 C2 Mo1 74.1(2) . . ? C4 C2 Mo1 117.3(3) . . ? C2 C3 Mo1 68.3(2) . . ? C2 C3 H3A 117(3) . . ? Mo1 C3 H3A 110(3) . . ? C2 C3 H3B 117(2) . . ? Mo1 C3 H3B 117(2) . . ? H3A C3 H3B 117(4) . . ? C2 C4 H4A 106(3) . . ? C2 C4 H4B 106(3) . . ? H4A C4 H4B 110(4) . . ? C2 C4 H4C 111(2) . . ? H4A C4 H4C 111(3) . . ? H4B C4 H4C 113(4) . . ? O1 C5 C41 105.9(3) . . ? O1 C5 C31 105.7(3) . . ? C41 C5 C31 115.7(3) . . ? O1 C5 C51 105.6(3) . . ? C41 C5 C51 116.1(3) . . ? C31 C5 C51 106.9(3) . . ? O10 C10 Mo1 176.8(3) . . ? O20 C20 Mo1 176.8(3) . . ? N1 C31 C32 122.6(3) . . ? N1 C31 C5 111.7(3) . . ? C32 C31 C5 125.7(3) . . ? C31 C32 C33 118.3(4) . . ? C31 C32 H32 116(3) . . ? C33 C32 H32 126(3) . . ? C34 C33 C32 119.0(4) . . ? C34 C33 H33 127(3) . . ? C32 C33 H33 114(3) . . ? C35 C34 C33 119.3(4) . . ? C35 C34 H34 124(3) . . ? C33 C34 H34 117(3) . . ? N1 C35 C34 122.8(4) . . ? N1 C35 H35 117(3) . . ? C34 C35 H35 120(3) . . ? N2 C41 C42 122.2(3) . . ? N2 C41 C5 111.5(3) . . ? C42 C41 C5 126.3(3) . . ? C41 C42 C43 118.2(4) . . ? C41 C42 H42 118(3) . . ? C43 C42 H42 124(3) . . ? C44 C43 C42 119.3(4) . . ? C44 C43 H43 114(3) . . ? C42 C43 H43 127(3) . . ? C45 C44 C43 118.5(4) . . ? C45 C44 H44 122(3) . . ? C43 C44 H44 119(3) . . ? N2 C45 C44 122.5(4) . . ? N2 C45 H45 118(4) . . ? C44 C45 H45 119(4) . . ? N3 C51 C52 122.3(3) . . ? N3 C51 C5 112.9(3) . . ? C52 C51 C5 124.7(3) . . ? C51 C52 C53 118.3(4) . . ? C51 C52 H52 122(2) . . ? C53 C52 H52 119(2) . . ? C54 C53 C52 120.0(4) . . ? C54 C53 H53 113(3) . . ? C52 C53 H53 127(3) . . ? C53 C54 C55 118.3(4) . . ? C53 C54 H54 123(3) . . ? C55 C54 H54 118(3) . . ? N3 C55 C54 122.6(4) . . ? N3 C55 H55 114(2) . . ? C54 C55 H55 123(3) . . ? C66 C61 C62 115.8(3) . . ? C66 C61 B1 123.6(3) . . ? C62 C61 B1 120.3(3) . . ? C63 C62 C61 122.5(3) . . ? C63 C62 H62 119(2) . . ? C61 C62 H62 118(2) . . ? C64 C63 C62 120.9(3) . . ? C64 C63 C67 119.0(3) . . ? C62 C63 C67 120.0(3) . . ? C63 C64 C65 117.7(3) . . ? C63 C64 H64 121(3) . . ? C65 C64 H64 121(3) . . ? C64 C65 C66 120.7(3) . . ? C64 C65 C68 119.8(3) . . ? C66 C65 C68 119.5(3) . . ? C61 C66 C65 122.4(3) . . ? C61 C66 H66 121.2(19) . . ? C65 C66 H66 116(2) . . ? F1 C67 F3 107.4(4) . . ? F1 C67 F2 106.3(4) . . ? F3 C67 F2 102.3(4) . . ? F1 C67 C63 113.5(3) . . ? F3 C67 C63 113.3(3) . . ? F2 C67 C63 113.1(3) . . ? F5 C68 F4 106.0(3) . . ? F5 C68 F6 105.6(3) . . ? F4 C68 F6 106.1(3) . . ? F5 C68 C65 112.4(3) . . ? F4 C68 C65 113.9(3) . . ? F6 C68 C65 112.2(3) . . ? C72 C71 C76 114.8(3) . . ? C72 C71 B1 122.8(3) . . ? C76 C71 B1 122.4(3) . . ? C73 C72 C71 123.1(3) . . ? C73 C72 H72 116(2) . . ? C71 C72 H72 121(2) . . ? C72 C73 C74 120.6(3) . . ? C72 C73 C78 119.2(3) . . ? C74 C73 C78 120.1(3) . . ? C75 C74 C73 118.1(3) . . ? C75 C74 H74 122(3) . . ? C73 C74 H74 120(3) . . ? C74 C75 C76 120.6(3) . . ? C74 C75 C77 118.4(3) . . ? C76 C75 C77 121.0(3) . . ? C75 C76 C71 122.8(3) . . ? C75 C76 H76 123(2) . . ? C71 C76 H76 114(2) . . ? F11 C77 F10 109.9(6) . . ? F11 C77 F12 106.3(6) . . ? F10 C77 F12 97.5(4) . . ? F11 C77 C75 115.3(4) . . ? F10 C77 C75 113.4(4) . . ? F12 C77 C75 112.8(4) . . ? F8 C78 F7 106.4(3) . . ? F8 C78 F9 107.1(3) . . ? F7 C78 F9 105.3(3) . . ? F8 C78 C73 112.7(3) . . ? F7 C78 C73 112.0(3) . . ? F9 C78 C73 112.7(3) . . ? C82 C81 C86 114.9(3) . . ? C82 C81 B1 121.8(3) . . ? C86 C81 B1 123.2(3) . . ? C83 C82 C81 122.6(3) . . ? C83 C82 H82 117(2) . . ? C81 C82 H82 121(2) . . ? C84 C83 C82 121.2(3) . . ? C84 C83 C87 119.4(3) . . ? C82 C83 C87 119.3(3) . . ? C83 C84 C85 117.9(3) . . ? C86 C85 C84 120.4(3) . . ? C86 C85 C88 119.6(3) . . ? C84 C85 C88 120.0(3) . . ? C85 C86 C81 123.0(3) . . ? C85 C86 H86 118(2) . . ? C81 C86 H86 119(2) . . ? F13 C87 F14 105.9(4) . . ? F13 C87 F15 106.8(4) . . ? F14 C87 F15 104.0(4) . . ? F13 C87 C83 114.2(3) . . ? F14 C87 C83 112.0(3) . . ? F15 C87 C83 113.1(3) . . ? F18 C88 F17 105.2(4) . . ? F18 C88 F16 105.9(4) . . ? F17 C88 F16 102.3(4) . . ? F18 C88 C85 114.2(3) . . ? F17 C88 C85 113.9(3) . . ? F16 C88 C85 114.1(3) . . ? C92 C91 C96 114.9(3) . . ? C92 C91 B1 123.4(3) . . ? C96 C91 B1 121.7(3) . . ? C93 C92 C91 122.8(3) . . ? C93 C92 H92 114(2) . . ? C91 C92 H92 123(2) . . ? C92 C93 C94 121.3(3) . . ? C92 C93 C97 118.4(3) . . ? C94 C93 C97 120.3(3) . . ? C95 C94 C93 116.9(3) . . ? C95 C94 H94 125(2) . . ? C93 C94 H94 118(2) . . ? C94 C95 C96 121.3(3) . . ? C94 C95 C98 120.0(3) . . ? C96 C95 C98 118.6(3) . . ? C95 C96 C91 122.6(3) . . ? C95 C96 H96 113(2) . . ? C91 C96 H96 125(2) . . ? F20 C97 F21 107.0(3) . . ? F20 C97 F19 105.4(3) . . ? F21 C97 F19 105.6(3) . . ? F20 C97 C93 112.6(3) . . ? F21 C97 C93 113.7(3) . . ? F19 C97 C93 112.0(3) . . ? F23 C98 F22 109.4(4) . . ? F23 C98 F24 106.6(4) . . ? F22 C98 F24 101.8(3) . . ? F23 C98 C95 114.2(3) . . ? F22 C98 C95 112.5(3) . . ? F24 C98 C95 111.5(3) . . ? C35 N1 C31 118.0(3) . . ? C35 N1 Mo1 125.8(3) . . ? C31 N1 Mo1 116.1(2) . . ? C45 N2 C41 119.2(3) . . ? C55 N3 C51 118.4(3) . . ? C55 N3 Mo1 127.3(3) . . ? C51 N3 Mo1 114.3(2) . . ? C5 O1 Mo1 108.08(18) . . ? C5 O1 H1 103(2) . . ? Mo1 O1 H1 149(2) . . ? C20 Mo1 C10 80.45(15) . . ? C20 Mo1 O1 167.74(13) . . ? C10 Mo1 O1 100.28(12) . . ? C20 Mo1 N1 95.80(13) . . ? C10 Mo1 N1 87.01(13) . . ? O1 Mo1 N1 72.08(9) . . ? C20 Mo1 C2 103.63(15) . . ? C10 Mo1 C2 104.56(15) . . ? O1 Mo1 C2 88.10(11) . . ? N1 Mo1 C2 158.71(12) . . ? C20 Mo1 N3 104.43(13) . . ? C10 Mo1 N3 163.23(13) . . ? O1 Mo1 N3 71.53(9) . . ? N1 Mo1 N3 76.60(10) . . ? C2 Mo1 N3 90.03(12) . . ? C20 Mo1 C1 108.91(15) . . ? C10 Mo1 C1 70.46(14) . . ? O1 Mo1 C1 82.64(12) . . ? N1 Mo1 C1 142.51(13) . . ? C2 Mo1 C1 36.21(14) . . ? N3 Mo1 C1 121.36(12) . . ? C20 Mo1 C3 69.68(16) . . ? C10 Mo1 C3 108.46(16) . . ? O1 Mo1 C3 120.98(12) . . ? N1 Mo1 C3 155.87(14) . . ? C2 Mo1 C3 35.66(15) . . ? N3 Mo1 C3 88.19(14) . . ? C1 Mo1 C3 61.60(16) . . ? C61 B1 C91 108.0(3) . . ? C61 B1 C71 110.6(3) . . ? C91 B1 C71 110.0(3) . . ? C61 B1 C81 110.1(3) . . ? C91 B1 C81 110.7(3) . . ? C71 B1 C81 107.5(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.433 _refine_diff_density_min -1.036 _refine_diff_density_rms 0.191 #===END data_1_(mp145) _database_code_depnum_ccdc_archive 'CCDC 786108' #TrackingRef 'CIFS.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H19 Mo N3 O3, C4 H8 O' _chemical_formula_sum 'C26 H27 Mo N3 O4' _chemical_formula_weight 541.45 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' 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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.02250(10) _cell_length_b 15.13590(10) _cell_length_c 17.68920(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2415.70(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9196 _cell_measurement_theta_min 2.9151 _cell_measurement_theta_max 73.6879 _exptl_crystal_description prism _exptl_crystal_colour red_exptl_crystal_size_max _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 4.751 _exptl_absorpt_correction_T_min 0.745 _exptl_absorpt_correction_T_max 0.790 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54180 _diffrn_measurement_device_type ? _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_detector_area_resol_mean 8.2640 _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10845 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.84 _diffrn_reflns_theta_max 73.90 _reflns_number_total 4436 _reflns_number_gt 4215 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [1.00000+-1.00000exp(-15.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+5.3341*P+(0.0278P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.016(14) _refine_ls_number_reflns 4436 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0353 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0903 _refine_ls_wR_factor_gt 0.0805 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8485(6) 0.5096(4) 0.2253(3) 0.0380(11) Uani 1 1 d . . . C2 C 0.8355(5) 0.5627(3) 0.2903(3) 0.0375(10) Uani 1 1 d . . . C3 C 0.9009(6) 0.6468(4) 0.2838(3) 0.0414(11) Uani 1 1 d . . . C4 C 0.7544(7) 0.5354(5) 0.3607(3) 0.0462(14) Uani 1 1 d . . . C5 C 0.4431(5) 0.6940(3) 0.2828(2) 0.0255(9) Uani 1 1 d . . . C10 C 0.7535(5) 0.5783(3) 0.1074(3) 0.0339(10) Uani 1 1 d . . . C20 C 0.8362(5) 0.7225(4) 0.1645(3) 0.0354(11) Uani 1 1 d . . . C21 C 0.2178(11) 0.4177(5) 0.0049(5) 0.076(2) Uani 1 1 d . . . H21A H 0.1549 0.4038 -0.0379 0.091 Uiso 1 1 calc R . . H21B H 0.2385 0.3633 0.0318 0.091 Uiso 1 1 calc R . . C22 C 0.3502(5) 0.4552(3) -0.0205(3) 0.0354(10) Uani 1 1 d . . . H22A H 0.4330 0.4178 -0.0063 0.042 Uiso 1 1 calc R . . H22B H 0.3486 0.4601 -0.0751 0.042 Uiso 1 1 calc R . . C23 C 0.3671(9) 0.5384(6) 0.0117(5) 0.0666(19) Uani 1 1 d . . . H23A H 0.3844 0.5822 -0.0274 0.080 Uiso 1 1 calc R . . H23B H 0.4508 0.5387 0.0460 0.080 Uiso 1 1 calc R . . C31 C 0.4017(5) 0.5940(3) 0.2776(2) 0.0262(9) Uani 1 1 d . . . C32 C 0.2765(5) 0.5540(3) 0.3058(3) 0.0348(10) Uani 1 1 d . . . H32 H 0.2062 0.5865 0.3324 0.042 Uiso 1 1 calc R . . C33 C 0.2569(5) 0.4640(3) 0.2939(3) 0.0364(10) Uani 1 1 d . . . H33 H 0.1757 0.4350 0.3147 0.044 Uiso 1 1 calc R . . C34 C 0.3587(6) 0.4178(3) 0.2509(3) 0.0375(11) Uani 1 1 d . . . H34 H 0.3453 0.3581 0.2406 0.045 Uiso 1 1 calc R . . C35 C 0.4813(6) 0.4627(3) 0.2237(3) 0.0327(10) Uani 1 1 d . . . H35 H 0.5504 0.4319 0.1949 0.039 Uiso 1 1 calc R . . C24 C 0.1466(13) 0.4755(8) 0.0517(11) 0.168(9) Uani 1 1 d . . . H24A H 0.1409 0.4507 0.1022 0.202 Uiso 1 1 calc R . . H24B H 0.0463 0.4851 0.0337 0.202 Uiso 1 1 calc R . . C41 C 0.3612(5) 0.7433(3) 0.3455(3) 0.0275(9) Uani 1 1 d . . . C42 C 0.4424(6) 0.7827(3) 0.4038(3) 0.0321(10) Uani 1 1 d . . . H42 H 0.5453 0.7792 0.4046 0.039 Uiso 1 1 calc R . . C43 C 0.3671(6) 0.8267(3) 0.4600(3) 0.0379(11) Uani 1 1 d . . . H43 H 0.4192 0.8537 0.4991 0.046 Uiso 1 1 calc R . . C44 C 0.2140(7) 0.8308(3) 0.4584(3) 0.0381(11) Uani 1 1 d . . . H44 H 0.1609 0.8606 0.4956 0.046 Uiso 1 1 calc R . . C45 C 0.1423(6) 0.7885(3) 0.3984(3) 0.0374(11) Uani 1 1 d . . . H45 H 0.0393 0.7900 0.3970 0.045 Uiso 1 1 calc R . . C51 C 0.4054(4) 0.7293(2) 0.2029(3) 0.0247(7) Uani 1 1 d . . . C52 C 0.2799(5) 0.7754(3) 0.1799(2) 0.0292(9) Uani 1 1 d . . . H52 H 0.2036 0.7873 0.2138 0.035 Uiso 1 1 calc R . . C53 C 0.2711(5) 0.8033(3) 0.1048(3) 0.0344(10) Uani 1 1 d . . . H53 H 0.1885 0.8345 0.0882 0.041 Uiso 1 1 calc R . . C54 C 0.3844(6) 0.7847(4) 0.0554(3) 0.0392(11) Uani 1 1 d . . . H54 H 0.3809 0.8044 0.0056 0.047 Uiso 1 1 calc R . . C55 C 0.5035(6) 0.7362(3) 0.0814(3) 0.0314(9) Uani 1 1 d . . . H55 H 0.5788 0.7217 0.0478 0.038 Uiso 1 1 calc R . . O1 O 0.5946(3) 0.70128(18) 0.29244(19) 0.0272(6) Uani 1 1 d . . . O10 O 0.7827(5) 0.5473(2) 0.04882(19) 0.0462(9) Uani 1 1 d . . . O20 O 0.9165(4) 0.7745(3) 0.1381(2) 0.0455(9) Uani 1 1 d . . . O24 O 0.2259(13) 0.5592(6) 0.0539(9) 0.177(5) Uani 1 1 d . . . Mo01 Mo 0.70158(4) 0.63408(2) 0.203710(18) 0.02549(10) Uani 1 1 d . . . N1 N 0.5148(4) 0.7092(2) 0.1536(2) 0.0263(7) Uani 1 1 d . . . N2 N 0.2133(5) 0.7461(2) 0.3432(2) 0.0325(8) Uani 1 1 d . . . N3 N 0.5046(5) 0.5494(2) 0.2372(2) 0.0273(8) Uani 1 1 d . . . H1A H 0.807(7) 0.455(4) 0.220(3) 0.038(14) Uiso 1 1 d . . . H1B H 0.931(8) 0.511(4) 0.197(4) 0.055(18) Uiso 1 1 d . . . H3A H 0.985(9) 0.654(5) 0.260(4) 0.06(2) Uiso 1 1 d . . . H3B H 0.878(9) 0.694(5) 0.314(5) 0.07(2) Uiso 1 1 d . . . H4A H 0.690(6) 0.499(3) 0.349(3) 0.018(11) Uiso 1 1 d . . . H4B H 0.829(7) 0.520(4) 0.399(3) 0.035(14) Uiso 1 1 d . . . H4C H 0.692(10) 0.588(5) 0.381(4) 0.066(19) Uiso 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 C1 0.041(3) 0.030(3) 0.043(3) 0.002(2) 0.003(2) 0.012(2) C2 0.035(2) 0.037(2) 0.041(2) 0.002(2) -0.008(2) 0.0129(17) C3 0.035(2) 0.035(3) 0.053(3) 0.006(2) -0.015(2) 0.002(2) C4 0.051(3) 0.057(4) 0.031(3) 0.001(2) -0.010(2) 0.008(3) C5 0.033(2) 0.0159(18) 0.027(2) 0.0002(16) -0.0036(17) -0.0002(15) C10 0.038(2) 0.026(2) 0.038(2) 0.0050(19) 0.0045(19) -0.0040(16) C20 0.026(2) 0.040(3) 0.040(2) -0.004(2) 0.0015(18) 0.0034(18) C21 0.085(5) 0.052(4) 0.091(5) -0.016(4) 0.015(5) -0.010(4) C22 0.035(2) 0.028(2) 0.043(3) -0.011(2) 0.0031(19) 0.0030(18) C23 0.057(4) 0.077(5) 0.066(4) -0.006(4) -0.005(3) -0.018(4) C31 0.029(2) 0.024(2) 0.026(2) 0.0010(15) 0.0006(16) 0.0023(17) C32 0.032(2) 0.036(2) 0.037(2) -0.005(2) 0.001(2) 0.0017(18) C33 0.039(2) 0.021(2) 0.048(2) 0.003(2) 0.004(2) -0.0049(15) C34 0.039(3) 0.028(3) 0.045(3) -0.001(2) 0.001(2) -0.0046(19) C35 0.044(3) 0.018(2) 0.036(2) -0.0044(16) 0.0035(19) 0.0029(18) C24 0.094(8) 0.117(9) 0.29(2) -0.129(11) 0.109(11) -0.055(7) C41 0.037(2) 0.014(2) 0.031(2) 0.0035(17) -0.0007(18) -0.0012(16) C42 0.037(3) 0.027(2) 0.032(2) -0.0029(18) 0.0002(19) -0.0026(18) C43 0.049(3) 0.032(2) 0.032(2) -0.0076(19) 0.000(2) -0.005(2) C44 0.052(3) 0.025(2) 0.037(2) -0.0045(17) 0.006(3) 0.000(2) C45 0.037(3) 0.033(3) 0.042(3) -0.001(2) 0.003(2) 0.0011(19) C51 0.0277(18) 0.0193(17) 0.0272(18) -0.0006(18) -0.0012(19) -0.0013(15) C52 0.030(2) 0.0224(19) 0.035(2) -0.0034(15) -0.0032(18) -0.0008(17) C53 0.034(3) 0.034(2) 0.035(2) 0.0036(19) -0.0094(19) 0.0021(19) C54 0.044(3) 0.044(3) 0.030(2) 0.009(2) -0.008(2) 0.003(2) C55 0.038(2) 0.029(2) 0.028(2) -0.0026(17) 0.0021(19) -0.0017(19) O1 0.0279(14) 0.0230(13) 0.0307(14) -0.0029(13) -0.0006(14) 0.0013(11) O10 0.064(3) 0.0409(19) 0.0340(17) -0.0011(14) 0.0139(19) 0.003(2) O20 0.0348(19) 0.044(2) 0.058(2) 0.0048(17) 0.0103(17) -0.0105(16) O24 0.132(8) 0.092(5) 0.306(15) -0.079(8) 0.009(10) -0.010(6) Mo01 0.02572(15) 0.02240(15) 0.02835(15) 0.00057(14) 0.00052(14) 0.00085(14) N1 0.0296(19) 0.0216(18) 0.0276(17) 0.0021(14) 0.0011(15) 0.0030(14) N2 0.032(2) 0.0299(19) 0.0360(19) -0.0025(15) 0.0043(18) 0.0022(18) N3 0.035(2) 0.0186(18) 0.0288(17) 0.0018(14) 0.0011(16) 0.0000(15) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; 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 C1 C2 1.408(8) . ? C1 Mo01 2.335(5) . ? C1 H1A 0.92(6) . ? C1 H1B 0.90(8) . ? C2 C3 1.408(8) . ? C2 C4 1.502(8) . ? C2 Mo01 2.230(5) . ? C3 Mo01 2.298(5) . ? C3 H3A 0.88(8) . ? C3 H3B 0.92(8) . ? C4 H4A 0.82(6) . ? C4 H4B 0.98(6) . ? C4 H4C 1.04(8) . ? C5 O1 1.382(5) . ? C5 C41 1.529(6) . ? C5 C51 1.549(6) . ? C5 C31 1.561(6) . ? C10 O10 1.168(6) . ? C10 Mo01 1.958(5) . ? C20 O20 1.167(6) . ? C20 Mo01 1.936(5) . ? C21 C24 1.364(12) . ? C21 C22 1.396(10) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.391(9) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 O24 1.510(13) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C31 N3 1.352(6) . ? C31 C32 1.376(7) . ? C32 C33 1.390(6) . ? C32 H32 0.9300 . ? C33 C34 1.382(7) . ? C33 H33 0.9300 . ? C34 C35 1.384(7) . ? C34 H34 0.9300 . ? C35 N3 1.351(6) . ? C35 H35 0.9300 . ? C24 O24 1.455(13) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C41 N2 1.336(6) . ? C41 C42 1.398(7) . ? C42 C43 1.376(7) . ? C42 H42 0.9300 . ? C43 C44 1.383(8) . ? C43 H43 0.9300 . ? C44 C45 1.398(8) . ? C44 H44 0.9300 . ? C45 N2 1.333(7) . ? C45 H45 0.9300 . ? C51 N1 1.352(6) . ? C51 C52 1.390(6) . ? C52 C53 1.397(6) . ? C52 H52 0.9300 . ? C53 C54 1.374(8) . ? C53 H53 0.9300 . ? C54 C55 1.381(7) . ? C54 H54 0.9300 . ? C55 N1 1.345(6) . ? C55 H55 0.9300 . ? O1 Mo01 2.105(3) . ? Mo01 N1 2.218(4) . ? Mo01 N3 2.269(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 C2 C1 Mo01 68.0(3) . . ? C2 C1 H1A 125(4) . . ? Mo01 C1 H1A 119(4) . . ? C2 C1 H1B 121(5) . . ? Mo01 C1 H1B 111(4) . . ? H1A C1 H1B 108(6) . . ? C1 C2 C3 114.4(5) . . ? C1 C2 C4 124.1(5) . . ? C3 C2 C4 121.4(5) . . ? C1 C2 Mo01 76.1(3) . . ? C3 C2 Mo01 74.5(3) . . ? C4 C2 Mo01 116.0(3) . . ? C2 C3 Mo01 69.3(3) . . ? C2 C3 H3A 121(5) . . ? Mo01 C3 H3A 113(5) . . ? C2 C3 H3B 124(5) . . ? Mo01 C3 H3B 105(5) . . ? H3A C3 H3B 112(7) . . ? C2 C4 H4A 109(3) . . ? C2 C4 H4B 107(3) . . ? H4A C4 H4B 120(5) . . ? C2 C4 H4C 110(4) . . ? H4A C4 H4C 102(6) . . ? H4B C4 H4C 109(5) . . ? O1 C5 C41 110.5(4) . . ? O1 C5 C51 107.6(3) . . ? C41 C5 C51 112.8(3) . . ? O1 C5 C31 108.8(3) . . ? C41 C5 C31 113.6(4) . . ? C51 C5 C31 103.2(3) . . ? O10 C10 Mo01 177.9(4) . . ? O20 C20 Mo01 177.3(5) . . ? C24 C21 C22 109.8(7) . . ? C24 C21 H21A 109.7 . . ? C22 C21 H21A 109.7 . . ? C24 C21 H21B 109.7 . . ? C22 C21 H21B 109.7 . . ? H21A C21 H21B 108.2 . . ? C23 C22 C21 109.3(5) . . ? C23 C22 H22A 109.8 . . ? C21 C22 H22A 109.8 . . ? C23 C22 H22B 109.8 . . ? C21 C22 H22B 109.8 . . ? H22A C22 H22B 108.3 . . ? C22 C23 O24 107.4(6) . . ? C22 C23 H23A 110.2 . . ? O24 C23 H23A 110.2 . . ? C22 C23 H23B 110.2 . . ? O24 C23 H23B 110.2 . . ? H23A C23 H23B 108.5 . . ? N3 C31 C32 122.4(4) . . ? N3 C31 C5 110.5(4) . . ? C32 C31 C5 127.0(4) . . ? C31 C32 C33 118.7(4) . . ? C31 C32 H32 120.6 . . ? C33 C32 H32 120.6 . . ? C34 C33 C32 119.6(4) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C33 C34 C35 118.3(4) . . ? C33 C34 H34 120.8 . . ? C35 C34 H34 120.8 . . ? N3 C35 C34 122.7(5) . . ? N3 C35 H35 118.7 . . ? C34 C35 H35 118.7 . . ? C21 C24 O24 110.0(9) . . ? C21 C24 H24A 109.7 . . ? O24 C24 H24A 109.7 . . ? C21 C24 H24B 109.7 . . ? O24 C24 H24B 109.7 . . ? H24A C24 H24B 108.2 . . ? N2 C41 C42 122.2(5) . . ? N2 C41 C5 118.4(4) . . ? C42 C41 C5 119.3(4) . . ? C43 C42 C41 118.7(5) . . ? C43 C42 H42 120.6 . . ? C41 C42 H42 120.6 . . ? C42 C43 C44 120.0(5) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C43 C44 C45 117.2(5) . . ? C43 C44 H44 121.4 . . ? C45 C44 H44 121.4 . . ? N2 C45 C44 123.7(5) . . ? N2 C45 H45 118.2 . . ? C44 C45 H45 118.2 . . ? N1 C51 C52 121.3(4) . . ? N1 C51 C5 110.5(4) . . ? C52 C51 C5 128.2(4) . . ? C51 C52 C53 118.4(4) . . ? C51 C52 H52 120.8 . . ? C53 C52 H52 120.8 . . ? C54 C53 C52 120.1(4) . . ? C54 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? C53 C54 C55 118.4(4) . . ? C53 C54 H54 120.8 . . ? C55 C54 H54 120.8 . . ? N1 C55 C54 122.5(4) . . ? N1 C55 H55 118.7 . . ? C54 C55 H55 118.7 . . ? C5 O1 Mo01 108.8(3) . . ? C24 O24 C23 102.7(7) . . ? C20 Mo01 C10 80.6(2) . . ? C20 Mo01 O1 102.76(17) . . ? C10 Mo01 O1 165.19(16) . . ? C20 Mo01 N1 88.84(17) . . ? C10 Mo01 N1 93.15(17) . . ? O1 Mo01 N1 72.64(13) . . ? C20 Mo01 C2 103.9(2) . . ? C10 Mo01 C2 105.0(2) . . ? O1 Mo01 C2 88.30(16) . . ? N1 Mo01 C2 159.14(16) . . ? C20 Mo01 N3 167.21(17) . . ? C10 Mo01 N3 99.84(16) . . ? O1 Mo01 N3 73.69(13) . . ? N1 Mo01 N3 78.38(14) . . ? C2 Mo01 N3 88.36(17) . . ? C20 Mo01 C3 70.8(2) . . ? C10 Mo01 C3 112.7(2) . . ? O1 Mo01 C3 81.87(18) . . ? N1 Mo01 C3 142.97(17) . . ? C2 Mo01 C3 36.20(19) . . ? N3 Mo01 C3 119.95(18) . . ? C20 Mo01 C1 105.1(2) . . ? C10 Mo01 C1 70.04(19) . . ? O1 Mo01 C1 121.90(16) . . ? N1 Mo01 C1 155.55(18) . . ? C2 Mo01 C1 35.84(19) . . ? N3 Mo01 C1 86.93(19) . . ? C3 Mo01 C1 61.5(2) . . ? C55 N1 C51 119.2(4) . . ? C55 N1 Mo01 126.4(3) . . ? C51 N1 Mo01 114.4(3) . . ? C45 N2 C41 118.2(5) . . ? C35 N3 C31 118.1(4) . . ? C35 N3 Mo01 128.7(3) . . ? C31 N3 Mo01 113.2(3) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 73.90 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.514 _refine_diff_density_min -0.595 _refine_diff_density_rms 0.088 #===END data_1H_THF_(hm667) _database_code_depnum_ccdc_archive 'CCDC 786109' #TrackingRef 'CIFS.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H12 B F24, C22 H20 Mo N3 O3, C4 H8 O' _chemical_formula_sum 'C58 H40 B F24 Mo N3 O4' _chemical_formula_weight 1405.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0010 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0170 0.0100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6830 0.6860 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.4276(2) _cell_length_b 18.3539(3) _cell_length_c 25.8077(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.5260(10) _cell_angle_gamma 90.00 _cell_volume 5868.25(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10165 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 25.350 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2816 _exptl_absorpt_coefficient_mu 0.349 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.894 _exptl_absorpt_correction_T_max 0.966 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39251 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 25.37 _reflns_number_total 10718 _reflns_number_gt 8016 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'DIRDIF-2008 (Beurskens et al., 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+3.1760P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10718 _refine_ls_number_parameters 839 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.0644 _refine_ls_wR_factor_ref 0.2204 _refine_ls_wR_factor_gt 0.1916 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8060(5) 0.8214(3) 0.7112(2) 0.0553(13) Uani 1 1 d . . . C2 C 0.7044(4) 0.8014(3) 0.72669(18) 0.0493(12) Uani 1 1 d . . . C3 C 0.6868(5) 0.7256(3) 0.7271(2) 0.0504(12) Uani 1 1 d . . . C4 C 0.6225(5) 0.8561(3) 0.7424(2) 0.0608(14) Uani 1 1 d . . . H4A H 0.6591 0.8981 0.7573 0.091 Uiso 1 1 calc R . . H4B H 0.5793 0.8346 0.7675 0.091 Uiso 1 1 calc R . . H4C H 0.5770 0.8704 0.7123 0.091 Uiso 1 1 calc R . . C6 C 0.7115(5) 0.5787(3) 0.8911(3) 0.0724(17) Uani 1 1 d . . . H6A H 0.7289 0.5937 0.9269 0.087 Uiso 1 1 calc R . . H6B H 0.7781 0.5752 0.8740 0.087 Uiso 1 1 calc R . . C7 C 0.6563(5) 0.5087(3) 0.8895(3) 0.088(2) Uani 1 1 d . . . H7A H 0.6218 0.5006 0.9215 0.105 Uiso 1 1 calc R . . H7B H 0.7069 0.4694 0.8851 0.105 Uiso 1 1 calc R . . C8 C 0.5743(6) 0.5122(3) 0.8444(3) 0.086(2) Uani 1 1 d . . . H8A H 0.5070 0.4902 0.8530 0.103 Uiso 1 1 calc R . . H8B H 0.5997 0.4872 0.8146 0.103 Uiso 1 1 calc R . . C9 C 0.5592(6) 0.5921(3) 0.8333(3) 0.093(2) Uani 1 1 d . . . H9A H 0.5665 0.6019 0.7968 0.111 Uiso 1 1 calc R . . H9B H 0.4879 0.6076 0.8416 0.111 Uiso 1 1 calc R . . C31 C 0.8177(3) 0.7550(2) 0.91113(18) 0.0348(9) Uani 1 1 d . . . C32 C 0.8402(4) 0.7380(2) 0.96223(19) 0.0412(10) Uani 1 1 d . . . H32 H 0.7966 0.7548 0.9874 0.049 Uiso 1 1 calc R . . C33 C 0.9307(4) 0.6945(3) 0.9759(2) 0.0535(12) Uani 1 1 d . . . H33 H 0.9472 0.6809 1.0104 0.064 Uiso 1 1 calc R . . C34 C 0.9945(4) 0.6721(3) 0.9380(2) 0.0535(13) Uani 1 1 d . . . H34 H 1.0559 0.6442 0.9465 0.064 Uiso 1 1 calc R . . C35 C 0.9668(3) 0.6911(2) 0.8878(2) 0.0457(11) Uani 1 1 d . . . H35 H 1.0101 0.6748 0.8623 0.055 Uiso 1 1 calc R . . C41 C 0.6269(3) 0.8109(2) 0.92180(16) 0.0359(9) Uani 1 1 d . . . C42 C 0.5217(3) 0.8019(3) 0.90146(19) 0.0440(11) Uani 1 1 d . . . H42 H 0.5065 0.7856 0.8675 0.053 Uiso 1 1 calc R . . C43 C 0.4398(4) 0.8177(3) 0.9327(2) 0.0602(14) Uani 1 1 d . . . H43 H 0.3682 0.8111 0.9202 0.072 Uiso 1 1 calc R . . C44 C 0.4644(4) 0.8431(3) 0.9820(2) 0.0616(14) Uani 1 1 d . . . H44 H 0.4101 0.8556 1.0032 0.074 Uiso 1 1 calc R . . C45 C 0.5709(4) 0.8495(3) 0.9994(2) 0.0600(14) Uani 1 1 d . . . H45 H 0.5876 0.8656 1.0333 0.072 Uiso 1 1 calc R . . C51 C 0.7682(3) 0.8736(2) 0.87134(16) 0.0319(9) Uani 1 1 d . . . C52 C 0.7622(3) 0.9376(2) 0.89961(18) 0.0388(10) Uani 1 1 d . . . H52 H 0.7224 0.9396 0.9287 0.047 Uiso 1 1 calc R . . C53 C 0.8166(3) 0.9984(2) 0.8836(2) 0.0451(11) Uani 1 1 d . . . H53 H 0.8129 1.0422 0.9015 0.054 Uiso 1 1 calc R . . C54 C 0.8764(4) 0.9938(2) 0.8408(2) 0.0460(11) Uani 1 1 d . . . H54 H 0.9146 1.0340 0.8300 0.055 Uiso 1 1 calc R . . C55 C 0.8785(4) 0.9287(2) 0.81436(19) 0.0436(11) Uani 1 1 d . . . H55 H 0.9185 0.9256 0.7855 0.052 Uiso 1 1 calc R . . C87 C 0.4921(4) 0.0350(3) 0.8648(2) 0.0533(13) Uani 1 1 d . . . F13 F 0.5165(3) 0.02410(18) 0.91629(14) 0.0763(10) Uani 1 1 d . . . F14 F 0.3952(2) 0.06311(18) 0.86069(16) 0.0808(11) Uani 1 1 d . . . F15 F 0.4879(3) -0.03178(15) 0.84449(14) 0.0708(9) Uani 1 1 d . . . N1 N 0.8800(3) 0.73225(17) 0.87280(15) 0.0358(8) Uani 1 1 d . . . N2 N 0.6525(3) 0.8336(2) 0.97017(14) 0.0472(9) Uani 1 1 d . . . N3 N 0.8243(3) 0.86875(17) 0.82900(14) 0.0361(8) Uani 1 1 d . . . O1 O 0.6824(2) 0.76367(14) 0.84021(11) 0.0315(6) Uani 1 1 d . . . O100 O 0.6399(3) 0.63041(16) 0.86475(13) 0.0506(8) Uani 1 1 d . . . H1A H 0.839(4) 0.789(2) 0.6859(19) 0.063(12) Uiso 1 1 d . . . H1B H 0.814(4) 0.869(3) 0.710(2) 0.061(15) Uiso 1 1 d . . . H3A H 0.730(5) 0.693(4) 0.705(3) 0.09(2) Uiso 1 1 d . . . H3B H 0.621(4) 0.706(3) 0.7389(19) 0.050(14) Uiso 1 1 d . . . H1 H 0.652(5) 0.721(3) 0.848(2) 0.060 Uiso 1 1 d . . . C5 C 0.7206(3) 0.8004(2) 0.88767(15) 0.0312(9) Uani 1 1 d . . . C10 C 0.9569(5) 0.7557(2) 0.7593(2) 0.0580(15) Uani 1 1 d . . . C20 C 0.8336(4) 0.6563(3) 0.7749(2) 0.0526(12) Uani 1 1 d . . . Mo1 Mo 0.81989(3) 0.758823(19) 0.790666(15) 0.03744(17) Uani 1 1 d . . . O10 O 1.0382(4) 0.7497(2) 0.7409(2) 0.0830(15) Uani 1 1 d . . . O20 O 0.8477(4) 0.59552(19) 0.76503(17) 0.0842(14) Uani 1 1 d . . . C61 C 0.8474(3) 0.20756(19) 0.92276(15) 0.0273(8) Uani 1 1 d . . . C62 C 0.8351(3) 0.17921(19) 0.97210(15) 0.0311(8) Uani 1 1 d . . . H62 H 0.7725 0.1899 0.9881 0.037 Uiso 1 1 calc R . . C63 C 0.9127(3) 0.1357(2) 0.99805(16) 0.0327(9) Uani 1 1 d . . . C64 C 1.0072(3) 0.1192(2) 0.97627(18) 0.0373(10) Uani 1 1 d . . . H64 H 1.0599 0.0907 0.9940 0.045 Uiso 1 1 calc R . . C65 C 1.0219(3) 0.1460(2) 0.92737(16) 0.0324(9) Uani 1 1 d . . . C66 C 0.9433(3) 0.18941(19) 0.90112(16) 0.0314(9) Uani 1 1 d . . . H66 H 0.9552 0.2068 0.8682 0.038 Uiso 1 1 calc R . . C67 C 0.8946(4) 0.1085(2) 1.05157(18) 0.0657(11) Uani 1 1 d . . . C68 C 1.1232(3) 0.1296(2) 0.9012(2) 0.0430(11) Uani 1 1 d . . . C71 C 0.6686(3) 0.29346(19) 0.92481(15) 0.0276(8) Uani 1 1 d . . . C72 C 0.7069(3) 0.3292(2) 0.97039(16) 0.0337(9) Uani 1 1 d . . . H72 H 0.7799 0.3254 0.9812 0.040 Uiso 1 1 calc R . . C73 C 0.6416(3) 0.3700(2) 1.00016(18) 0.0417(10) Uani 1 1 d . . . C74 C 0.5314(3) 0.3760(2) 0.98593(18) 0.0428(10) Uani 1 1 d . . . H74 H 0.4868 0.4027 1.0062 0.051 Uiso 1 1 calc R . . C75 C 0.4904(3) 0.3421(2) 0.94170(16) 0.0349(9) Uani 1 1 d . . . C76 C 0.5576(3) 0.3020(2) 0.91100(15) 0.0323(9) Uani 1 1 d . . . H76 H 0.5278 0.2804 0.8806 0.039 Uiso 1 1 calc R . . C77 C 0.6901(5) 0.4077(4) 1.0478(2) 0.0682(17) Uani 1 1 d . . . C78 C 0.3734(3) 0.3489(3) 0.92476(19) 0.0453(11) Uani 1 1 d . . . C81 C 0.6932(3) 0.1883(2) 0.85129(15) 0.0287(8) Uani 1 1 d . . . C82 C 0.6139(3) 0.1430(2) 0.86901(16) 0.0331(9) Uani 1 1 d . . . H82 H 0.5865 0.1535 0.9007 0.040 Uiso 1 1 calc R . . C83 C 0.5743(3) 0.0826(2) 0.84104(18) 0.0387(10) Uani 1 1 d . . . C84 C 0.6113(3) 0.0659(2) 0.79294(18) 0.0417(10) Uani 1 1 d . . . H84 H 0.5833 0.0266 0.7735 0.050 Uiso 1 1 calc R . . C85 C 0.6916(4) 0.1098(2) 0.77501(17) 0.0420(10) Uani 1 1 d . . . C86 C 0.7317(3) 0.1689(2) 0.80365(15) 0.0351(9) Uani 1 1 d . . . H86 H 0.7861 0.1967 0.7908 0.042 Uiso 1 1 calc R . . C88 C 0.7384(5) 0.0936(3) 0.7243(2) 0.0595(14) Uani 1 1 d . . . C91 C 0.8040(3) 0.3173(2) 0.85495(15) 0.0287(8) Uani 1 1 d . . . C92 C 0.7634(3) 0.3388(2) 0.80530(17) 0.0380(9) Uani 1 1 d . . . H92 H 0.7031 0.3152 0.7896 0.046 Uiso 1 1 calc R . . C93 C 0.8112(4) 0.3949(3) 0.77865(19) 0.0489(12) Uani 1 1 d . . . C94 C 0.8981(4) 0.4331(2) 0.80117(19) 0.0429(11) Uani 1 1 d . . . H94 H 0.9302 0.4699 0.7830 0.052 Uiso 1 1 calc R . . C95 C 0.9362(3) 0.4156(2) 0.85084(18) 0.0367(9) Uani 1 1 d . . . C96 C 0.8915(3) 0.3577(2) 0.87699(16) 0.0305(8) Uani 1 1 d . . . H96 H 0.9209 0.3456 0.9101 0.037 Uiso 1 1 calc R . . C97 C 0.7661(7) 0.4134(4) 0.7253(3) 0.085(2) Uani 1 1 d . . . C98 C 1.0266(4) 0.4574(2) 0.8784(2) 0.0753(12) Uani 1 1 d . . . B1 B 0.7511(3) 0.2520(2) 0.88825(17) 0.0265(9) Uani 1 1 d . . . F1 F 0.7981(3) 0.0887(3) 1.05685(17) 0.133(2) Uani 1 1 d . . . F2 F 0.9164(8) 0.1551(3) 1.08655(16) 0.056(5) Uani 1 1 d . . . F3 F 0.9525(3) 0.0516(3) 1.06614(16) 0.1103(16) Uani 1 1 d . . . F4 F 1.1943(3) 0.0924(2) 0.93154(16) 0.0972(13) Uani 1 1 d . . . F5 F 1.1741(3) 0.18797(19) 0.8897(2) 0.127(2) Uani 1 1 d . . . F6 F 1.1071(3) 0.0922(3) 0.86019(17) 0.1166(18) Uani 1 1 d . . . F7 F 0.7740(3) 0.4507(2) 1.03719(17) 0.1025(14) Uani 1 1 d . . . F8 F 0.7387(4) 0.3617(3) 1.08133(14) 0.1087(15) Uani 1 1 d . . . F9 F 0.6227(3) 0.4482(3) 1.07131(18) 0.139(2) Uani 1 1 d . . . F10 F 0.3317(2) 0.28678(19) 0.90592(17) 0.0890(12) Uani 1 1 d . . . F11 F 0.3145(2) 0.3686(2) 0.96295(12) 0.0803(11) Uani 1 1 d . . . F12 F 0.3539(2) 0.39672(18) 0.88683(12) 0.0640(8) Uani 1 1 d . . . F16 F 0.6968(3) 0.0347(2) 0.70091(13) 0.0818(11) Uani 1 1 d . . . F17 F 0.7192(5) 0.1474(2) 0.69069(13) 0.1108(16) Uani 1 1 d . . . F18 F 0.8445(3) 0.0859(3) 0.72978(15) 0.0998(14) Uani 1 1 d . . . F19 F 0.7088(6) 0.3651(3) 0.70159(16) 0.124(3) Uani 1 1 d . . . F20 F 0.8324(5) 0.4448(3) 0.69673(15) 0.1312(19) Uani 1 1 d . . . F21 F 0.6956(5) 0.4696(3) 0.7263(2) 0.157(2) Uani 1 1 d . . . F22 F 0.9954(3) 0.4948(3) 0.9167(2) 0.150(3) Uani 1 1 d . . . F23 F 1.0717(5) 0.5027(3) 0.85038(19) 0.172(3) Uani 1 1 d . . . F24 F 1.1017(3) 0.4167(2) 0.8998(2) 0.1045(15) 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 C1 0.083(4) 0.044(3) 0.040(3) 0.007(2) 0.014(3) 0.006(3) C2 0.068(3) 0.052(3) 0.027(2) 0.006(2) 0.000(2) 0.010(2) C3 0.064(4) 0.051(3) 0.036(3) 0.002(2) -0.001(2) 0.003(2) C4 0.076(4) 0.066(3) 0.038(3) 0.006(2) -0.011(3) 0.021(3) C6 0.072(4) 0.058(3) 0.083(4) 0.020(3) -0.022(3) -0.008(3) C7 0.076(4) 0.045(3) 0.140(7) 0.020(4) -0.009(4) -0.003(3) C8 0.082(5) 0.057(3) 0.117(6) -0.018(4) 0.000(4) -0.012(3) C9 0.083(5) 0.070(4) 0.117(6) 0.014(4) -0.045(4) -0.032(3) C31 0.030(2) 0.036(2) 0.037(2) 0.0041(17) -0.0027(19) -0.0043(16) C32 0.034(2) 0.049(2) 0.039(3) 0.0028(19) -0.011(2) -0.0028(18) C33 0.050(3) 0.054(3) 0.052(3) 0.007(2) -0.025(2) 0.000(2) C34 0.032(2) 0.048(2) 0.076(4) 0.000(3) -0.021(3) 0.0085(19) C35 0.026(2) 0.041(2) 0.069(3) -0.006(2) -0.004(2) 0.0054(17) C41 0.031(2) 0.044(2) 0.033(2) 0.0014(18) 0.0017(18) 0.0028(17) C42 0.027(2) 0.062(3) 0.042(3) 0.000(2) -0.0041(19) 0.0014(19) C43 0.031(3) 0.090(4) 0.059(3) 0.002(3) 0.004(2) -0.007(2) C44 0.040(3) 0.096(4) 0.050(3) 0.002(3) 0.012(2) 0.003(3) C45 0.051(3) 0.092(4) 0.038(3) -0.006(3) 0.008(2) 0.008(3) C51 0.024(2) 0.036(2) 0.034(2) -0.0008(17) -0.0053(17) 0.0041(15) C52 0.028(2) 0.042(2) 0.044(3) -0.0062(19) -0.0112(19) 0.0066(17) C53 0.034(2) 0.036(2) 0.061(3) -0.008(2) -0.016(2) 0.0022(18) C54 0.036(2) 0.040(2) 0.060(3) 0.004(2) -0.011(2) -0.0028(18) C55 0.042(2) 0.040(2) 0.049(3) 0.005(2) 0.003(2) -0.0021(18) C87 0.034(3) 0.054(3) 0.070(4) -0.020(3) -0.006(2) -0.010(2) F13 0.083(2) 0.079(2) 0.068(2) 0.0032(17) 0.0110(19) -0.0366(17) F14 0.0352(16) 0.0730(19) 0.135(3) -0.001(2) 0.0119(19) -0.0021(14) F15 0.0644(19) 0.0500(15) 0.098(3) -0.0202(16) 0.0091(18) -0.0184(14) N1 0.0275(18) 0.0354(17) 0.044(2) 0.0020(15) 0.0018(16) 0.0003(14) N2 0.036(2) 0.073(3) 0.032(2) -0.0048(19) -0.0022(17) 0.0053(18) N3 0.0303(18) 0.0342(17) 0.043(2) 0.0025(15) 0.0004(16) 0.0001(13) O1 0.0308(15) 0.0337(14) 0.0292(16) 0.0004(12) -0.0034(12) -0.0014(11) O100 0.0490(19) 0.0406(16) 0.059(2) 0.0064(15) -0.0132(16) -0.0045(14) C5 0.025(2) 0.039(2) 0.028(2) -0.0032(17) -0.0040(17) -0.0009(15) C10 0.065(4) 0.041(2) 0.071(4) 0.003(2) 0.023(3) 0.009(2) C20 0.067(3) 0.043(3) 0.047(3) 0.003(2) 0.000(2) 0.008(2) Mo1 0.0422(3) 0.0336(2) 0.0372(3) 0.00096(14) 0.00794(19) 0.00400(14) O10 0.070(3) 0.081(3) 0.106(4) 0.001(2) 0.054(3) 0.015(2) O20 0.136(4) 0.043(2) 0.071(3) -0.0102(19) -0.010(3) 0.021(2) C61 0.0239(19) 0.0280(17) 0.029(2) -0.0034(15) -0.0042(16) -0.0029(14) C62 0.026(2) 0.0335(19) 0.033(2) -0.0034(17) -0.0027(17) -0.0031(15) C63 0.032(2) 0.0341(19) 0.030(2) 0.0034(16) -0.0081(17) -0.0042(16) C64 0.028(2) 0.0338(19) 0.049(3) 0.0067(19) -0.0076(19) 0.0030(16) C65 0.025(2) 0.0325(19) 0.039(2) -0.0019(17) -0.0040(17) -0.0022(15) C66 0.029(2) 0.0306(18) 0.034(2) -0.0008(16) -0.0018(17) -0.0018(15) C67 0.090(3) 0.058(2) 0.048(3) 0.006(2) -0.003(2) 0.001(2) C68 0.027(2) 0.042(2) 0.060(3) 0.002(2) 0.003(2) 0.0040(17) C71 0.0231(19) 0.0297(18) 0.029(2) -0.0004(15) -0.0083(16) 0.0004(14) C72 0.0238(19) 0.044(2) 0.032(2) -0.0054(18) -0.0065(17) 0.0028(16) C73 0.032(2) 0.054(2) 0.038(2) -0.015(2) -0.0082(19) 0.0049(18) C74 0.033(2) 0.054(2) 0.041(3) -0.012(2) -0.001(2) 0.0089(19) C75 0.024(2) 0.042(2) 0.037(2) 0.0000(18) -0.0043(18) 0.0026(16) C76 0.029(2) 0.039(2) 0.027(2) -0.0034(17) -0.0081(17) -0.0010(16) C77 0.049(3) 0.099(4) 0.054(4) -0.038(3) -0.012(3) 0.018(3) C78 0.028(2) 0.058(3) 0.048(3) -0.004(2) -0.008(2) 0.005(2) C81 0.0212(18) 0.0360(19) 0.027(2) -0.0045(16) -0.0084(16) 0.0036(15) C82 0.0238(19) 0.039(2) 0.035(2) -0.0076(17) -0.0061(17) 0.0010(16) C83 0.027(2) 0.041(2) 0.046(3) -0.0088(19) -0.0091(19) 0.0004(17) C84 0.040(2) 0.041(2) 0.042(3) -0.0143(19) -0.014(2) -0.0003(18) C85 0.048(3) 0.049(2) 0.027(2) -0.0079(19) -0.007(2) 0.005(2) C86 0.034(2) 0.044(2) 0.026(2) 0.0002(17) -0.0054(17) -0.0045(17) C88 0.078(4) 0.067(3) 0.033(3) -0.013(3) -0.002(3) -0.001(3) C91 0.0228(19) 0.0339(19) 0.028(2) 0.0001(16) -0.0047(16) 0.0052(15) C92 0.035(2) 0.041(2) 0.035(2) 0.0028(18) -0.0120(19) 0.0021(17) C93 0.055(3) 0.046(3) 0.044(3) 0.013(2) -0.007(2) 0.012(2) C94 0.046(3) 0.033(2) 0.050(3) 0.012(2) 0.007(2) 0.0020(18) C95 0.029(2) 0.035(2) 0.046(3) 0.0059(19) 0.0010(19) 0.0030(16) C96 0.026(2) 0.0343(19) 0.030(2) 0.0031(16) -0.0043(17) 0.0021(15) C97 0.124(6) 0.072(4) 0.054(4) 0.038(3) -0.035(4) -0.020(4) C98 0.079(3) 0.046(2) 0.100(4) -0.002(2) 0.004(2) -0.0056(19) B1 0.021(2) 0.035(2) 0.022(2) -0.0001(17) -0.0042(18) 0.0003(16) F1 0.052(2) 0.251(6) 0.099(3) 0.119(4) 0.011(2) 0.015(3) F2 0.048(15) 0.074(3) 0.039(2) -0.020(2) -0.035(2) -0.0022(15) F3 0.096(3) 0.146(4) 0.091(3) 0.080(3) 0.021(2) 0.058(3) F4 0.0470(19) 0.150(4) 0.096(3) 0.031(3) 0.0142(19) 0.047(2) F5 0.076(2) 0.063(2) 0.257(6) 0.034(3) 0.100(3) 0.0028(17) F6 0.0389(18) 0.203(5) 0.110(3) -0.097(3) 0.0212(19) -0.009(2) F7 0.075(2) 0.118(3) 0.110(3) -0.063(3) -0.020(2) -0.023(2) F8 0.115(3) 0.163(4) 0.042(2) -0.031(2) -0.034(2) 0.014(3) F9 0.061(2) 0.224(5) 0.128(4) -0.143(4) -0.024(2) 0.035(3) F10 0.0349(16) 0.074(2) 0.151(4) -0.020(2) -0.035(2) -0.0022(15) F11 0.0326(16) 0.151(3) 0.057(2) -0.005(2) 0.0048(14) 0.0209(17) F12 0.0399(16) 0.089(2) 0.0598(19) 0.0104(17) -0.0162(14) 0.0155(14) F16 0.105(3) 0.087(2) 0.055(2) -0.0436(18) 0.0097(19) -0.0143(19) F17 0.209(5) 0.092(3) 0.0341(19) -0.0038(18) 0.028(2) -0.006(3) F18 0.078(3) 0.156(4) 0.069(2) -0.049(2) 0.029(2) -0.015(2) F19 0.196(7) 0.114(4) 0.055(2) -0.019(2) -0.036(2) -0.002(15) F20 0.187(5) 0.158(4) 0.046(2) 0.038(3) -0.004(3) -0.043(4) F21 0.189(6) 0.144(5) 0.124(4) 0.034(4) -0.071(4) 0.052(4) F22 0.073(3) 0.157(4) 0.223(6) -0.141(4) 0.025(3) -0.038(3) F23 0.176(5) 0.207(5) 0.122(4) 0.086(4) -0.056(4) -0.160(5) F24 0.058(2) 0.073(2) 0.172(4) -0.012(2) -0.058(2) -0.0032(17) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; 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 C1 C2 1.403(8) . ? C1 Mo1 2.346(5) . ? C1 H1A 1.00(5) . ? C1 H1B 0.87(5) . ? C2 C3 1.409(7) . ? C2 C4 1.508(7) . ? C2 Mo1 2.241(5) . ? C3 Mo1 2.318(6) . ? C3 H3A 1.01(7) . ? C3 H3B 0.96(5) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C6 O100 1.435(6) . ? C6 C7 1.455(8) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.487(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.503(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 O100 1.425(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C31 C32 1.363(6) . ? C31 N1 1.368(5) . ? C31 C5 1.550(6) . ? C32 C33 1.402(7) . ? C32 H32 0.9300 . ? C33 C34 1.370(7) . ? C33 H33 0.9300 . ? C34 C35 1.361(7) . ? C34 H34 0.9300 . ? C35 N1 1.348(5) . ? C35 H35 0.9300 . ? C41 N2 1.331(6) . ? C41 C42 1.379(6) . ? C41 C5 1.527(5) . ? C42 C43 1.377(6) . ? C42 H42 0.9300 . ? C43 C44 1.369(8) . ? C43 H43 0.9300 . ? C44 C45 1.368(7) . ? C44 H44 0.9300 . ? C45 N2 1.343(6) . ? C45 H45 0.9300 . ? C51 N3 1.344(5) . ? C51 C52 1.388(6) . ? C51 C5 1.540(5) . ? C52 C53 1.386(6) . ? C52 H52 0.9300 . ? C53 C54 1.381(7) . ? C53 H53 0.9300 . ? C54 C55 1.377(6) . ? C54 H54 0.9300 . ? C55 N3 1.360(5) . ? C55 H55 0.9300 . ? C87 F14 1.307(6) . ? C87 F15 1.332(5) . ? C87 F13 1.355(6) . ? C87 C83 1.511(6) . ? N1 Mo1 2.245(4) . ? N3 Mo1 2.246(3) . ? O1 C5 1.445(5) . ? O1 Mo1 2.215(3) . ? O1 H1 0.90(6) . ? C10 O10 1.155(6) . ? C10 Mo1 1.943(5) . ? C20 O20 1.161(6) . ? C20 Mo1 1.935(5) . ? C61 C66 1.396(5) . ? C61 C62 1.395(5) . ? C61 B1 1.651(6) . ? C62 C63 1.384(6) . ? C62 H62 0.9300 . ? C63 C64 1.375(6) . ? C63 C67 1.503(6) . ? C64 C65 1.380(6) . ? C64 H64 0.9300 . ? C65 C66 1.394(6) . ? C65 C68 1.504(6) . ? C66 H66 0.9300 . ? C67 F2 1.258(6) . ? C67 F1 1.270(6) . ? C67 F3 1.306(6) . ? C68 F6 1.264(6) . ? C68 F5 1.291(5) . ? C68 F4 1.323(6) . ? C71 C72 1.398(5) . ? C71 C76 1.405(5) . ? C71 B1 1.635(5) . ? C72 C73 1.381(5) . ? C72 H72 0.9300 . ? C73 C74 1.393(6) . ? C73 C77 1.495(7) . ? C74 C75 1.364(6) . ? C74 H74 0.9300 . ? C75 C76 1.404(5) . ? C75 C78 1.490(6) . ? C76 H76 0.9300 . ? C77 F9 1.306(6) . ? C77 F8 1.320(7) . ? C77 F7 1.354(7) . ? C78 F12 1.322(6) . ? C78 F11 1.323(5) . ? C78 F10 1.329(6) . ? C81 C82 1.394(5) . ? C81 C86 1.400(5) . ? C81 B1 1.639(6) . ? C82 C83 1.391(6) . ? C82 H82 0.9300 . ? C83 C84 1.392(6) . ? C84 C85 1.390(6) . ? C84 H84 0.9300 . ? C85 C86 1.383(6) . ? C85 C88 1.503(6) . ? C86 H86 0.9300 . ? C88 F18 1.322(7) . ? C88 F16 1.323(6) . ? C88 F17 1.324(7) . ? C91 C92 1.396(6) . ? C91 C96 1.400(5) . ? C91 B1 1.642(5) . ? C92 C93 1.397(6) . ? C92 H92 0.9300 . ? C93 C94 1.377(7) . ? C93 C97 1.484(7) . ? C94 C95 1.369(6) . ? C94 H94 0.9300 . ? C95 C96 1.397(5) . ? C95 C98 1.494(6) . ? C96 H96 0.9300 . ? C97 F19 1.265(8) . ? C97 F20 1.284(8) . ? C97 F21 1.355(9) . ? C98 F23 1.261(6) . ? C98 F24 1.285(6) . ? C98 F22 1.290(6) . ? 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 C1 Mo1 68.1(3) . . ? C2 C1 H1A 117(3) . . ? Mo1 C1 H1A 106(3) . . ? C2 C1 H1B 112(4) . . ? Mo1 C1 H1B 121(4) . . ? H1A C1 H1B 121(4) . . ? C1 C2 C3 113.9(5) . . ? C1 C2 C4 123.0(5) . . ? C3 C2 C4 123.2(5) . . ? C1 C2 Mo1 76.3(3) . . ? C3 C2 Mo1 75.0(3) . . ? C4 C2 Mo1 116.2(3) . . ? C2 C3 Mo1 69.0(3) . . ? C2 C3 H3A 119(4) . . ? Mo1 C3 H3A 100(4) . . ? C2 C3 H3B 120(3) . . ? Mo1 C3 H3B 117(3) . . ? H3A C3 H3B 118(5) . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O100 C6 C7 107.3(5) . . ? O100 C6 H6A 110.3 . . ? C7 C6 H6A 110.3 . . ? O100 C6 H6B 110.3 . . ? C7 C6 H6B 110.3 . . ? H6A C6 H6B 108.5 . . ? C6 C7 C8 106.1(5) . . ? C6 C7 H7A 110.5 . . ? C8 C7 H7A 110.5 . . ? C6 C7 H7B 110.5 . . ? C8 C7 H7B 110.5 . . ? H7A C7 H7B 108.7 . . ? C7 C8 C9 105.0(5) . . ? C7 C8 H8A 110.7 . . ? C9 C8 H8A 110.7 . . ? C7 C8 H8B 110.7 . . ? C9 C8 H8B 110.7 . . ? H8A C8 H8B 108.8 . . ? O100 C9 C8 107.5(5) . . ? O100 C9 H9A 110.2 . . ? C8 C9 H9A 110.2 . . ? O100 C9 H9B 110.2 . . ? C8 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? C32 C31 N1 123.1(4) . . ? C32 C31 C5 126.5(4) . . ? N1 C31 C5 110.4(4) . . ? C31 C32 C33 118.3(5) . . ? C31 C32 H32 120.9 . . ? C33 C32 H32 120.9 . . ? C34 C33 C32 119.3(5) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C35 C34 C33 119.1(4) . . ? C35 C34 H34 120.4 . . ? C33 C34 H34 120.4 . . ? N1 C35 C34 123.6(4) . . ? N1 C35 H35 118.2 . . ? C34 C35 H35 118.2 . . ? N2 C41 C42 122.9(4) . . ? N2 C41 C5 116.3(4) . . ? C42 C41 C5 120.6(4) . . ? C43 C42 C41 118.3(5) . . ? C43 C42 H42 120.9 . . ? C41 C42 H42 120.9 . . ? C44 C43 C42 119.7(5) . . ? C44 C43 H43 120.2 . . ? C42 C43 H43 120.2 . . ? C45 C44 C43 118.3(5) . . ? C45 C44 H44 120.9 . . ? C43 C44 H44 120.9 . . ? N2 C45 C44 123.4(5) . . ? N2 C45 H45 118.3 . . ? C44 C45 H45 118.3 . . ? N3 C51 C52 122.4(4) . . ? N3 C51 C5 113.6(3) . . ? C52 C51 C5 123.8(4) . . ? C53 C52 C51 118.5(4) . . ? C53 C52 H52 120.8 . . ? C51 C52 H52 120.8 . . ? C54 C53 C52 119.7(4) . . ? C54 C53 H53 120.1 . . ? C52 C53 H53 120.1 . . ? C55 C54 C53 118.8(4) . . ? C55 C54 H54 120.6 . . ? C53 C54 H54 120.6 . . ? N3 C55 C54 122.4(4) . . ? N3 C55 H55 118.8 . . ? C54 C55 H55 118.8 . . ? F14 C87 F15 108.9(4) . . ? F14 C87 F13 105.7(4) . . ? F15 C87 F13 104.4(4) . . ? F14 C87 C83 112.8(4) . . ? F15 C87 C83 112.3(4) . . ? F13 C87 C83 112.1(4) . . ? C35 N1 C31 116.7(4) . . ? C35 N1 Mo1 126.3(3) . . ? C31 N1 Mo1 116.8(3) . . ? C41 N2 C45 117.4(4) . . ? C51 N3 C55 118.2(4) . . ? C51 N3 Mo1 114.9(2) . . ? C55 N3 Mo1 126.9(3) . . ? C5 O1 Mo1 106.9(2) . . ? C5 O1 H1 106(5) . . ? Mo1 O1 H1 117(5) . . ? C9 O100 C6 109.0(4) . . ? O1 C5 C41 109.4(3) . . ? O1 C5 C51 106.4(3) . . ? C41 C5 C51 112.0(3) . . ? O1 C5 C31 105.9(3) . . ? C41 C5 C31 116.6(3) . . ? C51 C5 C31 105.8(3) . . ? O10 C10 Mo1 176.3(4) . . ? O20 C20 Mo1 176.3(5) . . ? C20 Mo1 C10 77.8(2) . . ? C20 Mo1 O1 104.22(17) . . ? C10 Mo1 O1 169.4(2) . . ? C20 Mo1 C2 104.2(2) . . ? C10 Mo1 C2 103.6(2) . . ? O1 Mo1 C2 86.16(15) . . ? C20 Mo1 N1 87.68(18) . . ? C10 Mo1 N1 98.6(2) . . ? O1 Mo1 N1 71.23(11) . . ? C2 Mo1 N1 156.58(15) . . ? C20 Mo1 N3 165.15(18) . . ? C10 Mo1 N3 102.63(17) . . ? O1 Mo1 N3 72.71(11) . . ? C2 Mo1 N3 90.19(15) . . ? N1 Mo1 N3 77.55(12) . . ? C20 Mo1 C3 70.4(2) . . ? C10 Mo1 C3 107.3(2) . . ? O1 Mo1 C3 83.06(16) . . ? C2 Mo1 C3 35.97(18) . . ? N1 Mo1 C3 140.99(16) . . ? N3 Mo1 C3 122.67(16) . . ? C20 Mo1 C1 107.1(2) . . ? C10 Mo1 C1 69.9(2) . . ? O1 Mo1 C1 118.57(16) . . ? C2 Mo1 C1 35.52(19) . . ? N1 Mo1 C1 158.16(18) . . ? N3 Mo1 C1 86.73(17) . . ? C3 Mo1 C1 60.7(2) . . ? C66 C61 C62 115.8(3) . . ? C66 C61 B1 120.5(3) . . ? C62 C61 B1 123.3(3) . . ? C63 C62 C61 122.3(4) . . ? C63 C62 H62 118.9 . . ? C61 C62 H62 118.9 . . ? C64 C63 C62 121.0(4) . . ? C64 C63 C67 119.8(4) . . ? C62 C63 C67 119.2(4) . . ? C63 C64 C65 118.3(4) . . ? C63 C64 H64 120.9 . . ? C65 C64 H64 120.9 . . ? C64 C65 C66 120.7(4) . . ? C64 C65 C68 121.0(4) . . ? C66 C65 C68 118.4(4) . . ? C65 C66 C61 122.0(4) . . ? C65 C66 H66 119.0 . . ? C61 C66 H66 119.0 . . ? F2 C67 F1 105.6(6) . . ? F2 C67 F3 104.7(6) . . ? F1 C67 F3 104.2(4) . . ? F2 C67 C63 113.2(4) . . ? F1 C67 C63 113.9(4) . . ? F3 C67 C63 114.3(4) . . ? F6 C68 F5 107.8(5) . . ? F6 C68 F4 105.6(4) . . ? F5 C68 F4 104.3(4) . . ? F6 C68 C65 113.7(4) . . ? F5 C68 C65 112.3(4) . . ? F4 C68 C65 112.4(4) . . ? C72 C71 C76 115.1(3) . . ? C72 C71 B1 121.1(3) . . ? C76 C71 B1 123.6(3) . . ? C73 C72 C71 123.1(4) . . ? C73 C72 H72 118.5 . . ? C71 C72 H72 118.5 . . ? C72 C73 C74 120.3(4) . . ? C72 C73 C77 119.4(4) . . ? C74 C73 C77 120.3(4) . . ? C75 C74 C73 118.6(4) . . ? C75 C74 H74 120.7 . . ? C73 C74 H74 120.7 . . ? C74 C75 C76 120.8(4) . . ? C74 C75 C78 119.9(4) . . ? C76 C75 C78 119.3(4) . . ? C75 C76 C71 122.1(4) . . ? C75 C76 H76 119.0 . . ? C71 C76 H76 119.0 . . ? F9 C77 F8 109.6(6) . . ? F9 C77 F7 107.1(5) . . ? F8 C77 F7 100.7(5) . . ? F9 C77 C73 114.4(4) . . ? F8 C77 C73 112.2(5) . . ? F7 C77 C73 111.8(5) . . ? F12 C78 F11 106.9(4) . . ? F12 C78 F10 104.8(4) . . ? F11 C78 F10 106.5(4) . . ? F12 C78 C75 113.0(4) . . ? F11 C78 C75 112.9(4) . . ? F10 C78 C75 112.2(4) . . ? C82 C81 C86 115.8(3) . . ? C82 C81 B1 121.6(3) . . ? C86 C81 B1 121.9(3) . . ? C83 C82 C81 122.3(4) . . ? C83 C82 H82 118.8 . . ? C81 C82 H82 118.8 . . ? C82 C83 C84 120.7(4) . . ? C82 C83 C87 118.3(4) . . ? C84 C83 C87 121.0(4) . . ? C85 C84 C83 117.7(4) . . ? C85 C84 H84 121.1 . . ? C83 C84 H84 121.1 . . ? C86 C85 C84 121.0(4) . . ? C86 C85 C88 118.2(4) . . ? C84 C85 C88 120.8(4) . . ? C85 C86 C81 122.4(4) . . ? C85 C86 H86 118.8 . . ? C81 C86 H86 118.8 . . ? F18 C88 F16 108.2(5) . . ? F18 C88 F17 106.0(5) . . ? F16 C88 F17 105.4(5) . . ? F18 C88 C85 112.3(4) . . ? F16 C88 C85 113.2(5) . . ? F17 C88 C85 111.2(5) . . ? C92 C91 C96 115.9(4) . . ? C92 C91 B1 123.7(3) . . ? C96 C91 B1 120.3(3) . . ? C91 C92 C93 121.5(4) . . ? C91 C92 H92 119.2 . . ? C93 C92 H92 119.2 . . ? C94 C93 C92 121.1(4) . . ? C94 C93 C97 120.1(5) . . ? C92 C93 C97 118.8(5) . . ? C95 C94 C93 118.5(4) . . ? C95 C94 H94 120.7 . . ? C93 C94 H94 120.7 . . ? C94 C95 C96 120.6(4) . . ? C94 C95 C98 121.1(4) . . ? C96 C95 C98 118.3(4) . . ? C95 C96 C91 122.1(4) . . ? C95 C96 H96 118.9 . . ? C91 C96 H96 118.9 . . ? F19 C97 F20 113.4(7) . . ? F19 C97 F21 101.7(7) . . ? F20 C97 F21 96.6(5) . . ? F19 C97 C93 116.4(5) . . ? F20 C97 C93 115.0(6) . . ? F21 C97 C93 110.7(6) . . ? F23 C98 F24 106.8(5) . . ? F23 C98 F22 105.3(5) . . ? F24 C98 F22 103.4(5) . . ? F23 C98 C95 114.7(5) . . ? F24 C98 C95 113.5(4) . . ? F22 C98 C95 112.2(4) . . ? C71 B1 C81 113.7(3) . . ? C71 B1 C91 104.9(3) . . ? C81 B1 C91 113.1(3) . . ? C71 B1 C61 112.3(3) . . ? C81 B1 C61 103.2(3) . . ? C91 B1 C61 109.9(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.304 _refine_diff_density_min -0.993 _refine_diff_density_rms 0.134 #===END data_1H_DBU_(mp169) _database_code_depnum_ccdc_archive 'CCDC 786110' #TrackingRef 'CIFS.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H12 B F24, C22 H19 Mo N3 O3, C9 H17 N2' _chemical_formula_sum 'C63 H48 B F24 Mo N5 O3' _chemical_formula_weight 1485.81 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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 12.7311(3) _cell_length_b 14.0298(4) _cell_length_c 35.9014(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6412.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6360 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 25.350 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2992 _exptl_absorpt_coefficient_mu 0.324 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.937 _exptl_absorpt_correction_T_max 1.046 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47737 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1164 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.13 _diffrn_reflns_theta_max 25.34 _reflns_number_total 11495 _reflns_number_gt 7758 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'DIRDIF-2008 (Beurskens et al., 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0924P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(4) _refine_ls_number_reflns 11495 _refine_ls_number_parameters 877 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0970 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1792 _refine_ls_wR_factor_gt 0.1362 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.047 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.18936(5) 0.77667(4) 0.871877(17) 0.03544(19) Uani 1 1 d . . . C1 C 0.1085(6) 0.8420(6) 0.8197(2) 0.053(2) Uani 1 1 d . . . H1A H 0.0368 0.8639 0.8227 0.063 Uiso 1 1 calc R . . H1B H 0.1512 0.8829 0.8040 0.063 Uiso 1 1 calc R . . C2 C 0.1238(6) 0.7418(6) 0.8159(2) 0.054(2) Uani 1 1 d . . . C3 C 0.0616(7) 0.6875(6) 0.8414(2) 0.065(3) Uani 1 1 d . . . H3A H 0.0711 0.6189 0.8411 0.078 Uiso 1 1 calc R . . H3B H -0.0108 0.7073 0.8447 0.078 Uiso 1 1 calc R . . C4 C 0.2001(6) 0.6961(6) 0.7876(2) 0.058(2) Uani 1 1 d . . . H4A H 0.1983 0.6280 0.7902 0.086 Uiso 1 1 calc R . . H4B H 0.2701 0.7187 0.7922 0.086 Uiso 1 1 calc R . . H4C H 0.1793 0.7132 0.7628 0.086 Uiso 1 1 calc R . . C5 C 0.3779(5) 0.6629(4) 0.87787(16) 0.0279(15) Uani 1 1 d . . . C10 C 0.0772(7) 0.7450(5) 0.9068(2) 0.054(2) Uani 1 1 d . . . C11 C 0.1642(6) 0.4210(5) 0.86142(18) 0.0423(19) Uani 1 1 d . . . H11A H 0.1442 0.4596 0.8402 0.051 Uiso 1 1 calc R . . H11B H 0.2226 0.3806 0.8543 0.051 Uiso 1 1 calc R . . C12 C 0.0763(7) 0.3635(6) 0.8737(2) 0.066(2) Uani 1 1 d . . . H12A H 0.0535 0.3217 0.8537 0.079 Uiso 1 1 calc R . . H12B H 0.0178 0.4041 0.8806 0.079 Uiso 1 1 calc R . . C13 C 0.1136(8) 0.3023(5) 0.9085(2) 0.063(3) Uani 1 1 d . . . H13A H 0.0537 0.2707 0.9197 0.075 Uiso 1 1 calc R . . H13B H 0.1631 0.2539 0.9005 0.075 Uiso 1 1 calc R . . C14 C 0.1740(7) 0.3244(6) 0.9734(2) 0.061(2) Uani 1 1 d . . . H14A H 0.2442 0.3372 0.9825 0.073 Uiso 1 1 calc R . . H14B H 0.1650 0.2558 0.9722 0.073 Uiso 1 1 calc R . . C15 C 0.0940(7) 0.3661(6) 1.0005(2) 0.061(2) Uani 1 1 d . . . H15A H 0.0258 0.3671 0.9885 0.073 Uiso 1 1 calc R . . H15B H 0.0889 0.3241 1.0220 0.073 Uiso 1 1 calc R . . C16 C 0.1192(6) 0.4656(6) 1.01410(19) 0.052(2) Uani 1 1 d . . . H16A H 0.0628 0.4864 1.0304 0.063 Uiso 1 1 calc R . . H16B H 0.1828 0.4627 1.0289 0.063 Uiso 1 1 calc R . . C17 C 0.1340(6) 0.5388(6) 0.98461(19) 0.050(2) Uani 1 1 d . . . H17A H 0.1471 0.5997 0.9965 0.060 Uiso 1 1 calc R . . H17B H 0.0690 0.5446 0.9707 0.060 Uiso 1 1 calc R . . C18 C 0.2214(5) 0.5192(5) 0.95773(19) 0.0411(19) Uani 1 1 d . . . H18A H 0.2441 0.5792 0.9469 0.049 Uiso 1 1 calc R . . H18B H 0.2804 0.4929 0.9714 0.049 Uiso 1 1 calc R . . C19 C 0.1931(6) 0.4522(5) 0.92693(18) 0.0361(16) Uani 1 1 d . . . C20 C 0.1369(6) 0.9080(6) 0.8833(2) 0.053(2) Uani 1 1 d . . . C31 C 0.3814(5) 0.7123(5) 0.91632(17) 0.0298(15) Uani 1 1 d . . . C32 C 0.4574(6) 0.7016(5) 0.94417(17) 0.0406(19) Uani 1 1 d . . . H32 H 0.5117 0.6578 0.9414 0.049 Uiso 1 1 calc R . . C33 C 0.4502(7) 0.7575(5) 0.97598(18) 0.054(2) Uani 1 1 d . . . H33 H 0.4999 0.7517 0.9948 0.065 Uiso 1 1 calc R . . C34 C 0.3688(7) 0.8219(6) 0.97939(19) 0.052(2) Uani 1 1 d . . . H34 H 0.3640 0.8607 1.0003 0.062 Uiso 1 1 calc R . . C35 C 0.2950(6) 0.8282(5) 0.95177(19) 0.044(2) Uani 1 1 d . . . H35 H 0.2390 0.8701 0.9547 0.053 Uiso 1 1 calc R . . C41 C 0.4372(5) 0.5674(4) 0.87391(19) 0.0305(15) Uani 1 1 d . . . C42 C 0.4600(6) 0.5314(5) 0.83927(17) 0.0352(17) Uani 1 1 d . . . H42 H 0.4485 0.5683 0.8182 0.042 Uiso 1 1 calc R . . C43 C 0.4991(6) 0.4425(5) 0.8358(2) 0.048(2) Uani 1 1 d . . . H43 H 0.5150 0.4177 0.8125 0.057 Uiso 1 1 calc R . . C44 C 0.5149(6) 0.3899(5) 0.8671(2) 0.0461(19) Uani 1 1 d . . . H44 H 0.5434 0.3290 0.8655 0.055 Uiso 1 1 calc R . . C45 C 0.4884(6) 0.4273(5) 0.9011(2) 0.047(2) Uani 1 1 d . . . H45 H 0.4982 0.3905 0.9224 0.057 Uiso 1 1 calc R . . C51 C 0.4210(5) 0.7411(4) 0.85202(15) 0.0240(15) Uani 1 1 d . . . C52 C 0.5242(5) 0.7491(4) 0.84096(16) 0.0308(16) Uani 1 1 d . . . H52 H 0.5725 0.7014 0.8466 0.037 Uiso 1 1 calc R . . C53 C 0.5557(6) 0.8310(5) 0.82087(17) 0.0350(17) Uani 1 1 d . . . H53 H 0.6251 0.8383 0.8134 0.042 Uiso 1 1 calc R . . C54 C 0.4826(6) 0.8994(5) 0.81262(18) 0.0370(18) Uani 1 1 d . . . H54 H 0.5014 0.9529 0.7989 0.044 Uiso 1 1 calc R . . C55 C 0.3800(6) 0.8878(5) 0.82507(18) 0.0370(18) Uani 1 1 d . . . H55 H 0.3310 0.9351 0.8199 0.044 Uiso 1 1 calc R . . C61 C -0.2004(5) 0.0672(4) 0.89548(14) 0.0203(13) Uani 1 1 d . . . C62 C -0.2409(5) -0.0264(4) 0.89576(15) 0.0218(14) Uani 1 1 d . . . H62 H -0.2930 -0.0426 0.8787 0.026 Uiso 1 1 calc R . . C63 C -0.2059(5) -0.0944(4) 0.92042(16) 0.0253(14) Uani 1 1 d . . . C64 C -0.1283(5) -0.0757(5) 0.94596(17) 0.0295(16) Uani 1 1 d . . . H64 H -0.1057 -0.1220 0.9627 0.035 Uiso 1 1 calc R . . C65 C -0.0850(5) 0.0142(4) 0.94593(16) 0.0245(15) Uani 1 1 d . . . C66 C -0.1200(5) 0.0844(4) 0.92101(15) 0.0222(14) Uani 1 1 d . . . H66 H -0.0886 0.1442 0.9215 0.027 Uiso 1 1 calc R . . C67 C 0.0002(5) 0.0389(5) 0.97327(17) 0.0298(16) Uani 1 1 d . . . C68 C -0.2546(6) -0.1931(5) 0.91859(19) 0.0408(19) Uani 1 1 d . . . C71 C -0.2146(4) 0.2550(4) 0.87161(16) 0.0244(14) Uani 1 1 d . . . C72 C -0.2024(5) 0.3213(4) 0.84328(16) 0.0257(14) Uani 1 1 d . . . H72 H -0.1937 0.2992 0.8191 0.031 Uiso 1 1 calc R . . C73 C -0.2027(5) 0.4191(4) 0.84934(17) 0.0274(15) Uani 1 1 d . . . C74 C -0.2119(5) 0.4539(5) 0.88483(18) 0.0309(16) Uani 1 1 d . . . H74 H -0.2110 0.5192 0.8892 0.037 Uiso 1 1 calc R . . C074 C -0.1889(7) 0.4873(5) 0.81781(19) 0.0414(18) Uani 1 1 d . . . C75 C -0.2225(5) 0.3906(5) 0.91412(17) 0.0295(16) Uani 1 1 d . . . C76 C -0.2263(4) 0.2930(4) 0.90736(16) 0.0230(14) Uani 1 1 d . . . H76 H -0.2371 0.2517 0.9273 0.028 Uiso 1 1 calc R . . C077 C -0.2338(7) 0.4277(5) 0.9531(2) 0.048(2) Uani 1 1 d . . . C81 C -0.3602(5) 0.1366(4) 0.85292(15) 0.0192(14) Uani 1 1 d . . . C82 C -0.3983(5) 0.1588(4) 0.81763(16) 0.0252(15) Uani 1 1 d . . . H82 H -0.3507 0.1695 0.7984 0.030 Uiso 1 1 calc R . . C83 C -0.5048(5) 0.1654(5) 0.81028(16) 0.0279(15) Uani 1 1 d . . . C84 C -0.5778(5) 0.1491(5) 0.83807(18) 0.0316(16) Uani 1 1 d . . . H84 H -0.6493 0.1539 0.8331 0.038 Uiso 1 1 calc R . . C85 C -0.5427(5) 0.1255(4) 0.87360(18) 0.0295(15) Uani 1 1 d . . . C86 C -0.4353(5) 0.1191(4) 0.88041(16) 0.0258(15) Uani 1 1 d . . . H86 H -0.4128 0.1026 0.9042 0.031 Uiso 1 1 calc R . . C87 C -0.6174(6) 0.1075(7) 0.9042(2) 0.050(2) Uani 1 1 d . . . C88 C -0.5427(6) 0.1897(7) 0.77248(19) 0.048(2) Uani 1 1 d . . . C91 C -0.1628(4) 0.1035(4) 0.82730(14) 0.0189(14) Uani 1 1 d . . . C92 C -0.1979(5) 0.0309(4) 0.80312(14) 0.0239(14) Uani 1 1 d . . . H92 H -0.2660 0.0080 0.8057 0.029 Uiso 1 1 calc R . . C93 C -0.1346(5) -0.0068(4) 0.77601(16) 0.0259(15) Uani 1 1 d . . . C94 C -0.0328(5) 0.0244(4) 0.77164(16) 0.0297(16) Uani 1 1 d . . . H94 H 0.0092 -0.0011 0.7529 0.036 Uiso 1 1 calc R . . C95 C 0.0070(5) 0.0937(4) 0.79516(16) 0.0235(14) Uani 1 1 d . . . C96 C -0.0589(5) 0.1335(4) 0.82232(16) 0.0222(14) Uani 1 1 d . . . H96 H -0.0326 0.1814 0.8376 0.027 Uiso 1 1 calc R . . C97 C -0.1768(7) -0.0842(5) 0.75189(18) 0.0439(19) Uani 1 1 d . . . C98 C 0.1162(5) 0.1285(5) 0.7902(2) 0.0355(17) Uani 1 1 d . . . N1 N 0.3013(5) 0.7749(4) 0.92017(13) 0.0366(13) Uani 1 1 d . . . N2 N 0.4485(5) 0.5160(4) 0.90474(15) 0.0367(14) Uani 1 1 d . . . N3 N 0.3489(4) 0.8090(4) 0.84467(14) 0.0290(13) Uani 1 1 d . . . N4 N 0.1935(5) 0.4814(4) 0.89264(14) 0.0374(14) Uani 1 1 d D . . N5 N 0.1629(5) 0.3647(4) 0.93534(15) 0.0456(16) Uani 1 1 d . . . O1 O 0.2725(3) 0.6452(3) 0.86943(11) 0.0281(10) Uani 1 1 d . . . O10 O 0.0134(4) 0.7274(5) 0.92882(17) 0.0726(18) Uani 1 1 d . . . O20 O 0.1034(5) 0.9824(4) 0.88964(17) 0.0666(17) Uani 1 1 d . . . F1 F -0.3591(4) -0.1867(3) 0.91520(14) 0.0676(14) Uani 1 1 d . . . F2 F -0.2368(4) -0.2457(3) 0.94814(14) 0.0804(18) Uani 1 1 d . . . F3 F -0.2244(4) -0.2417(3) 0.88912(14) 0.0799(16) Uani 1 1 d . . . F4 F -0.0360(4) 0.0879(5) 1.00172(14) 0.112(2) Uani 1 1 d . . . F5 F 0.0463(4) -0.0341(3) 0.98743(17) 0.105(2) Uani 1 1 d . . . F6 F 0.0732(4) 0.0921(4) 0.95972(12) 0.0706(15) Uani 1 1 d . . . F7 F -0.2789(8) 0.3722(4) 0.97547(14) 0.174(5) Uani 1 1 d . . . F8 F -0.1473(5) 0.4547(7) 0.96732(16) 0.146(4) Uani 1 1 d . . . F9 F -0.2873(5) 0.5067(4) 0.95550(14) 0.103(2) Uani 1 1 d . . . F10 F -0.0896(4) 0.5087(4) 0.81278(14) 0.0889(18) Uani 1 1 d . . . F11 F -0.2361(6) 0.5667(4) 0.82285(15) 0.129(3) Uani 1 1 d . . . F12 F -0.2216(5) 0.4539(4) 0.78648(13) 0.097(2) Uani 1 1 d . . . F13 F -0.6090(5) 0.1662(6) 0.93167(15) 0.116(3) Uani 1 1 d . . . F14 F -0.6049(5) 0.0253(5) 0.92054(18) 0.115(2) Uani 1 1 d . . . F15 F -0.7171(3) 0.1096(5) 0.89444(14) 0.097(2) Uani 1 1 d . . . F16 F -0.4792(6) 0.2396(9) 0.75422(19) 0.215(6) Uani 1 1 d . . . F17 F -0.5533(9) 0.1152(5) 0.75198(17) 0.171(5) Uani 1 1 d . . . F18 F -0.6285(5) 0.2316(6) 0.77004(14) 0.138(3) Uani 1 1 d . . . F19 F 0.1441(3) 0.2004(3) 0.81156(14) 0.0693(15) Uani 1 1 d . . . F20 F 0.1873(4) 0.0605(3) 0.79637(18) 0.0864(18) Uani 1 1 d . . . F21 F 0.1379(4) 0.1561(4) 0.75534(13) 0.0737(15) Uani 1 1 d . . . F22 F -0.2050(4) -0.1598(3) 0.77180(12) 0.0644(14) Uani 1 1 d . . . F23 F -0.2620(4) -0.0573(4) 0.73310(15) 0.0882(18) Uani 1 1 d . . . F24 F -0.1091(4) -0.1149(3) 0.72663(11) 0.0711(16) Uani 1 1 d . . . B1 B -0.2325(5) 0.1395(5) 0.86240(17) 0.0217(16) Uani 1 1 d . . . H1 H 0.222(4) 0.529(3) 0.8831(15) 0.036 Uiso 1 1 d 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 Mo1 0.0304(3) 0.0247(3) 0.0512(4) 0.0044(3) 0.0063(3) 0.0017(3) C1 0.043(5) 0.043(5) 0.072(5) 0.005(4) -0.004(4) 0.001(4) C2 0.043(5) 0.047(5) 0.074(5) 0.004(4) -0.031(4) -0.003(4) C3 0.041(5) 0.046(5) 0.107(7) 0.005(5) -0.020(5) -0.014(4) C4 0.048(5) 0.065(6) 0.060(5) -0.014(4) -0.015(4) -0.020(5) C5 0.029(4) 0.025(4) 0.030(4) 0.005(3) 0.002(3) -0.004(3) C10 0.047(5) 0.046(5) 0.070(5) 0.011(4) 0.007(4) 0.013(4) C11 0.053(5) 0.029(4) 0.045(4) -0.010(3) -0.008(4) -0.014(4) C12 0.063(6) 0.067(6) 0.067(5) -0.028(5) -0.008(5) -0.014(5) C13 0.088(7) 0.033(5) 0.067(5) 0.001(4) 0.001(5) -0.033(5) C14 0.069(6) 0.052(5) 0.062(5) 0.028(4) 0.003(5) 0.004(5) C15 0.061(6) 0.068(6) 0.053(5) 0.021(5) 0.004(5) -0.023(5) C16 0.053(5) 0.068(6) 0.035(4) 0.007(4) 0.007(4) -0.004(5) C17 0.066(6) 0.046(5) 0.038(4) -0.004(4) -0.001(4) -0.006(4) C18 0.039(5) 0.043(4) 0.041(4) 0.004(3) -0.006(3) -0.014(4) C19 0.029(4) 0.032(4) 0.047(4) 0.008(3) 0.000(4) -0.017(4) C20 0.051(5) 0.046(5) 0.061(5) 0.000(4) 0.009(4) -0.009(4) C31 0.038(4) 0.021(4) 0.030(3) 0.004(3) 0.012(3) -0.009(3) C32 0.055(5) 0.035(4) 0.032(4) 0.007(3) -0.003(4) -0.021(4) C33 0.089(7) 0.046(5) 0.026(4) 0.001(4) -0.003(4) -0.038(5) C34 0.096(7) 0.038(5) 0.023(4) -0.009(3) 0.020(4) -0.022(5) C35 0.062(6) 0.030(4) 0.040(4) -0.006(3) 0.024(4) -0.004(4) C41 0.028(4) 0.023(3) 0.041(4) 0.003(3) -0.004(3) 0.001(3) C42 0.048(5) 0.032(4) 0.025(4) -0.007(3) -0.003(3) 0.001(4) C43 0.060(6) 0.034(5) 0.048(5) -0.003(4) 0.011(4) 0.000(4) C44 0.046(5) 0.030(4) 0.062(5) -0.011(4) 0.002(4) 0.017(4) C45 0.048(5) 0.037(5) 0.057(5) 0.015(4) -0.005(4) 0.006(4) C51 0.026(4) 0.024(4) 0.023(3) -0.007(3) 0.005(3) -0.001(3) C52 0.028(4) 0.030(4) 0.035(4) -0.003(3) 0.006(3) -0.003(3) C53 0.039(4) 0.032(4) 0.034(4) 0.002(3) 0.007(3) -0.016(4) C54 0.048(5) 0.029(4) 0.034(4) 0.002(3) 0.012(4) -0.017(4) C55 0.054(5) 0.017(4) 0.040(4) 0.003(3) 0.000(4) 0.001(3) C61 0.016(3) 0.025(3) 0.020(3) 0.000(2) 0.006(3) 0.000(3) C62 0.016(3) 0.032(4) 0.018(3) 0.000(3) -0.002(2) -0.003(3) C63 0.022(4) 0.026(3) 0.028(3) 0.002(3) 0.002(3) -0.005(3) C64 0.028(4) 0.032(4) 0.029(3) 0.007(3) -0.001(3) 0.001(3) C65 0.021(4) 0.028(4) 0.024(3) 0.000(3) -0.002(3) -0.004(3) C66 0.019(4) 0.025(4) 0.022(3) -0.001(3) -0.001(3) -0.010(3) C67 0.024(4) 0.041(4) 0.025(3) 0.008(3) -0.007(3) -0.004(4) C68 0.035(5) 0.051(5) 0.037(4) -0.003(4) -0.011(3) -0.009(4) C71 0.021(3) 0.027(3) 0.026(3) -0.007(3) 0.006(3) 0.000(3) C72 0.027(4) 0.028(3) 0.022(3) -0.001(3) 0.010(3) 0.001(3) C73 0.026(4) 0.025(4) 0.031(3) 0.001(3) 0.003(3) 0.007(3) C74 0.023(4) 0.020(3) 0.050(4) -0.003(3) 0.012(3) 0.000(3) C074 0.052(5) 0.028(4) 0.045(4) 0.003(3) 0.021(4) 0.003(4) C75 0.027(4) 0.032(4) 0.030(3) -0.006(3) 0.007(3) -0.001(3) C76 0.019(3) 0.026(4) 0.024(3) -0.003(3) 0.005(3) -0.005(3) C077 0.070(6) 0.033(5) 0.040(4) -0.012(4) 0.011(4) -0.004(4) C81 0.020(3) 0.019(3) 0.019(3) 0.003(3) -0.002(3) 0.004(3) C82 0.027(4) 0.025(4) 0.023(3) 0.001(3) 0.003(3) -0.002(3) C83 0.030(4) 0.031(4) 0.023(3) 0.007(3) -0.001(3) 0.004(3) C84 0.010(3) 0.032(4) 0.053(4) 0.004(3) -0.006(3) 0.002(3) C85 0.022(4) 0.035(4) 0.031(4) 0.000(3) 0.004(3) 0.002(3) C86 0.024(4) 0.034(4) 0.019(3) 0.001(3) 0.000(3) 0.002(3) C87 0.030(5) 0.066(6) 0.055(5) 0.014(5) 0.006(4) 0.010(4) C88 0.035(5) 0.082(6) 0.028(4) 0.008(4) -0.011(4) 0.009(4) C91 0.020(4) 0.021(3) 0.015(3) 0.005(2) -0.003(2) -0.001(3) C92 0.028(4) 0.021(3) 0.022(3) -0.002(3) -0.005(3) -0.001(3) C93 0.032(4) 0.019(3) 0.026(3) -0.002(3) 0.005(3) -0.005(3) C94 0.044(5) 0.025(4) 0.020(3) -0.002(3) 0.005(3) 0.003(3) C95 0.026(4) 0.016(3) 0.028(3) 0.002(3) 0.002(3) 0.000(3) C96 0.024(4) 0.018(3) 0.025(3) -0.001(3) -0.002(3) -0.001(3) C97 0.062(5) 0.036(4) 0.034(4) -0.015(3) 0.016(4) -0.004(4) C98 0.025(4) 0.034(4) 0.047(4) 0.003(4) 0.008(3) 0.006(4) N1 0.047(4) 0.031(3) 0.032(3) -0.003(3) 0.011(3) -0.011(4) N2 0.040(4) 0.030(3) 0.040(3) 0.009(3) -0.003(3) 0.004(3) N3 0.029(3) 0.025(3) 0.033(3) -0.005(2) 0.005(2) -0.001(3) N4 0.049(4) 0.029(3) 0.034(3) 0.003(3) 0.004(3) -0.021(3) N5 0.065(5) 0.025(3) 0.047(4) 0.003(3) 0.008(3) -0.015(3) O1 0.023(2) 0.027(2) 0.035(2) 0.000(2) -0.006(2) -0.0013(19) O10 0.052(4) 0.069(4) 0.097(5) 0.016(4) 0.039(3) 0.007(4) O20 0.064(4) 0.029(3) 0.106(5) -0.001(3) 0.027(3) 0.018(3) F1 0.045(3) 0.053(3) 0.104(4) 0.024(3) -0.019(3) -0.024(2) F2 0.108(4) 0.042(3) 0.091(4) 0.045(3) -0.056(3) -0.041(3) F3 0.108(4) 0.045(3) 0.086(3) -0.022(3) 0.009(3) -0.028(3) F4 0.052(3) 0.223(8) 0.060(3) -0.064(4) -0.018(3) -0.012(4) F5 0.110(5) 0.056(3) 0.150(5) 0.046(3) -0.111(4) -0.038(3) F6 0.062(3) 0.099(4) 0.051(3) 0.018(3) -0.028(2) -0.054(3) F7 0.401(13) 0.072(4) 0.049(3) -0.034(3) 0.104(6) -0.094(6) F8 0.067(4) 0.289(11) 0.081(4) -0.116(6) -0.018(3) 0.011(5) F9 0.150(6) 0.090(4) 0.070(3) -0.042(3) 0.011(4) 0.040(4) F10 0.085(4) 0.113(5) 0.069(3) 0.039(3) 0.014(3) -0.043(4) F11 0.234(9) 0.051(3) 0.101(4) 0.044(3) 0.096(5) 0.065(4) F12 0.179(7) 0.065(3) 0.048(3) 0.028(3) -0.033(3) -0.036(4) F13 0.100(5) 0.185(7) 0.062(3) -0.034(4) 0.043(3) -0.044(5) F14 0.092(4) 0.121(5) 0.133(5) 0.081(5) 0.058(4) 0.022(4) F15 0.025(3) 0.187(6) 0.078(3) 0.035(4) 0.016(2) -0.003(3) F16 0.102(5) 0.443(16) 0.102(5) 0.188(8) -0.068(4) -0.129(8) F17 0.340(14) 0.117(6) 0.056(4) -0.016(4) -0.099(6) 0.053(7) F18 0.100(5) 0.246(9) 0.069(4) 0.055(5) -0.022(3) 0.089(6) F19 0.034(3) 0.068(3) 0.106(4) -0.045(3) 0.016(2) -0.019(2) F20 0.025(2) 0.039(3) 0.195(6) 0.017(3) 0.007(3) 0.002(2) F21 0.058(3) 0.096(4) 0.066(3) 0.009(3) 0.016(2) -0.030(3) F22 0.090(4) 0.043(3) 0.061(3) -0.024(2) 0.026(3) -0.028(3) F23 0.092(4) 0.084(4) 0.089(4) -0.042(3) -0.058(3) 0.003(3) F24 0.097(4) 0.068(3) 0.048(3) -0.042(2) 0.032(3) -0.035(3) B1 0.021(4) 0.028(4) 0.016(4) -0.001(3) 0.001(3) -0.006(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; 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 Mo1 C10 1.951(9) . ? Mo1 C20 2.001(9) . ? Mo1 O1 2.129(4) . ? Mo1 C2 2.230(8) . ? Mo1 N1 2.245(6) . ? Mo1 N3 2.299(5) . ? Mo1 C3 2.326(8) . ? Mo1 C1 2.327(8) . ? C1 C2 1.425(11) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.430(11) . ? C2 C4 1.545(11) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 O1 1.397(7) . ? C5 C51 1.538(8) . ? C5 C41 1.545(9) . ? C5 C31 1.545(9) . ? C10 O10 1.160(9) . ? C11 C12 1.448(10) . ? C11 N4 1.454(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.589(12) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N5 1.446(9) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N5 1.485(9) . ? C14 C15 1.526(11) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.513(11) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.487(10) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.499(10) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.496(9) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 N4 1.298(8) . ? C19 N5 1.320(8) . ? C20 O20 1.152(9) . ? C31 N1 1.353(8) . ? C31 C32 1.399(9) . ? C32 C33 1.388(9) . ? C32 H32 0.9300 . ? C33 C34 1.381(11) . ? C33 H33 0.9300 . ? C34 C35 1.368(11) . ? C34 H34 0.9300 . ? C35 N1 1.361(8) . ? C35 H35 0.9300 . ? C41 N2 1.328(8) . ? C41 C42 1.374(9) . ? C42 C43 1.348(10) . ? C42 H42 0.9300 . ? C43 C44 1.359(10) . ? C43 H43 0.9300 . ? C44 C45 1.372(10) . ? C44 H44 0.9300 . ? C45 N2 1.350(9) . ? C45 H45 0.9300 . ? C51 N3 1.350(8) . ? C51 C52 1.377(9) . ? C52 C53 1.415(9) . ? C52 H52 0.9300 . ? C53 C54 1.369(10) . ? C53 H53 0.9300 . ? C54 C55 1.390(10) . ? C54 H54 0.9300 . ? C55 N3 1.369(8) . ? C55 H55 0.9300 . ? C61 C66 1.395(8) . ? C61 C62 1.411(8) . ? C61 B1 1.614(9) . ? C62 C63 1.376(8) . ? C62 H62 0.9300 . ? C63 C64 1.374(9) . ? C63 C68 1.518(9) . ? C64 C65 1.376(9) . ? C64 H64 0.9300 . ? C65 C66 1.403(8) . ? C65 C67 1.504(8) . ? C66 H66 0.9300 . ? C67 F5 1.285(8) . ? C67 F6 1.286(7) . ? C67 F4 1.315(8) . ? C68 F2 1.312(8) . ? C68 F3 1.316(8) . ? C68 F1 1.339(8) . ? C71 C72 1.386(8) . ? C71 C76 1.398(8) . ? C71 B1 1.670(9) . ? C72 C73 1.390(8) . ? C72 H72 0.9300 . ? C73 C74 1.370(8) . ? C73 C074 1.493(9) . ? C74 C75 1.383(9) . ? C74 H74 0.9300 . ? C074 F11 1.278(8) . ? C074 F12 1.287(8) . ? C074 F10 1.311(9) . ? C75 C76 1.392(8) . ? C75 C077 1.500(9) . ? C76 H76 0.9300 . ? C077 F7 1.257(9) . ? C077 F8 1.271(9) . ? C077 F9 1.305(9) . ? C81 C82 1.392(8) . ? C81 C86 1.397(8) . ? C81 B1 1.661(9) . ? C82 C83 1.385(9) . ? C82 H82 0.9300 . ? C83 C84 1.383(9) . ? C83 C88 1.480(9) . ? C84 C85 1.392(9) . ? C84 H84 0.9300 . ? C85 C86 1.391(8) . ? C85 C87 1.474(10) . ? C86 H86 0.9300 . ? C87 F13 1.291(10) . ? C87 F14 1.304(9) . ? C87 F15 1.317(9) . ? C88 F18 1.244(9) . ? C88 F16 1.254(9) . ? C88 F17 1.285(10) . ? C91 C96 1.400(8) . ? C91 C92 1.410(8) . ? C91 B1 1.622(8) . ? C92 C93 1.370(8) . ? C92 H92 0.9300 . ? C93 C94 1.377(9) . ? C93 C97 1.489(9) . ? C94 C95 1.384(8) . ? C94 H94 0.9300 . ? C95 C96 1.402(8) . ? C95 C98 1.484(9) . ? C96 H96 0.9300 . ? C97 F24 1.323(8) . ? C97 F22 1.330(8) . ? C97 F23 1.332(9) . ? C98 F19 1.316(8) . ? C98 F20 1.334(8) . ? C98 F21 1.338(8) . ? N4 H1 0.83(3) . ? 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 C10 Mo1 C20 80.5(3) . . ? C10 Mo1 O1 101.1(2) . . ? C20 Mo1 O1 166.4(3) . . ? C10 Mo1 C2 104.8(3) . . ? C20 Mo1 C2 105.1(3) . . ? O1 Mo1 C2 87.6(2) . . ? C10 Mo1 N1 88.0(3) . . ? C20 Mo1 N1 93.7(3) . . ? O1 Mo1 N1 72.93(18) . . ? C2 Mo1 N1 158.6(3) . . ? C10 Mo1 N3 164.6(3) . . ? C20 Mo1 N3 101.5(3) . . ? O1 Mo1 N3 73.39(17) . . ? C2 Mo1 N3 89.5(3) . . ? N1 Mo1 N3 76.66(18) . . ? C10 Mo1 C3 70.6(3) . . ? C20 Mo1 C3 111.0(3) . . ? O1 Mo1 C3 82.1(2) . . ? C2 Mo1 C3 36.5(3) . . ? N1 Mo1 C3 143.3(3) . . ? N3 Mo1 C3 121.6(3) . . ? C10 Mo1 C1 106.5(3) . . ? C20 Mo1 C1 69.8(3) . . ? O1 Mo1 C1 121.9(2) . . ? C2 Mo1 C1 36.4(3) . . ? N1 Mo1 C1 155.2(2) . . ? N3 Mo1 C1 88.3(3) . . ? C3 Mo1 C1 61.5(3) . . ? C2 C1 Mo1 68.1(4) . . ? C2 C1 H1A 116.9 . . ? Mo1 C1 H1A 116.9 . . ? C2 C1 H1B 116.9 . . ? Mo1 C1 H1B 116.9 . . ? H1A C1 H1B 113.9 . . ? C1 C2 C3 112.9(8) . . ? C1 C2 C4 123.9(8) . . ? C3 C2 C4 123.2(7) . . ? C1 C2 Mo1 75.5(5) . . ? C3 C2 Mo1 75.4(5) . . ? C4 C2 Mo1 116.7(5) . . ? C2 C3 Mo1 68.1(4) . . ? C2 C3 H3A 116.9 . . ? Mo1 C3 H3A 116.9 . . ? C2 C3 H3B 116.9 . . ? Mo1 C3 H3B 116.9 . . ? H3A C3 H3B 113.9 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O1 C5 C51 109.8(5) . . ? O1 C5 C41 107.2(5) . . ? C51 C5 C41 112.8(5) . . ? O1 C5 C31 107.6(5) . . ? C51 C5 C31 102.0(5) . . ? C41 C5 C31 117.2(5) . . ? O10 C10 Mo1 177.0(8) . . ? C12 C11 N4 106.8(6) . . ? C12 C11 H11A 110.4 . . ? N4 C11 H11A 110.4 . . ? C12 C11 H11B 110.4 . . ? N4 C11 H11B 110.4 . . ? H11A C11 H11B 108.6 . . ? C11 C12 C13 108.0(7) . . ? C11 C12 H12A 110.1 . . ? C13 C12 H12A 110.1 . . ? C11 C12 H12B 110.1 . . ? C13 C12 H12B 110.1 . . ? H12A C12 H12B 108.4 . . ? N5 C13 C12 109.1(6) . . ? N5 C13 H13A 109.9 . . ? C12 C13 H13A 109.9 . . ? N5 C13 H13B 109.9 . . ? C12 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? N5 C14 C15 112.3(7) . . ? N5 C14 H14A 109.1 . . ? C15 C14 H14A 109.1 . . ? N5 C14 H14B 109.1 . . ? C15 C14 H14B 109.1 . . ? H14A C14 H14B 107.9 . . ? C16 C15 C14 114.7(7) . . ? C16 C15 H15A 108.6 . . ? C14 C15 H15A 108.6 . . ? C16 C15 H15B 108.6 . . ? C14 C15 H15B 108.6 . . ? H15A C15 H15B 107.6 . . ? C17 C16 C15 115.8(6) . . ? C17 C16 H16A 108.3 . . ? C15 C16 H16A 108.3 . . ? C17 C16 H16B 108.3 . . ? C15 C16 H16B 108.3 . . ? H16A C16 H16B 107.4 . . ? C16 C17 C18 115.2(7) . . ? C16 C17 H17A 108.5 . . ? C18 C17 H17A 108.5 . . ? C16 C17 H17B 108.5 . . ? C18 C17 H17B 108.5 . . ? H17A C17 H17B 107.5 . . ? C19 C18 C17 114.3(6) . . ? C19 C18 H18A 108.7 . . ? C17 C18 H18A 108.7 . . ? C19 C18 H18B 108.7 . . ? C17 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? N4 C19 N5 120.8(6) . . ? N4 C19 C18 120.1(6) . . ? N5 C19 C18 119.0(6) . . ? O20 C20 Mo1 177.7(7) . . ? N1 C31 C32 121.2(6) . . ? N1 C31 C5 111.1(5) . . ? C32 C31 C5 127.6(6) . . ? C33 C32 C31 118.8(7) . . ? C33 C32 H32 120.6 . . ? C31 C32 H32 120.6 . . ? C34 C33 C32 119.5(7) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C35 C34 C33 119.6(7) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? N1 C35 C34 121.9(7) . . ? N1 C35 H35 119.1 . . ? C34 C35 H35 119.1 . . ? N2 C41 C42 122.2(6) . . ? N2 C41 C5 116.5(6) . . ? C42 C41 C5 120.4(6) . . ? C43 C42 C41 120.1(7) . . ? C43 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? C42 C43 C44 118.8(7) . . ? C42 C43 H43 120.6 . . ? C44 C43 H43 120.6 . . ? C43 C44 C45 119.4(7) . . ? C43 C44 H44 120.3 . . ? C45 C44 H44 120.3 . . ? N2 C45 C44 122.1(7) . . ? N2 C45 H45 119.0 . . ? C44 C45 H45 119.0 . . ? N3 C51 C52 122.4(6) . . ? N3 C51 C5 112.2(5) . . ? C52 C51 C5 124.9(6) . . ? C51 C52 C53 118.9(6) . . ? C51 C52 H52 120.6 . . ? C53 C52 H52 120.6 . . ? C54 C53 C52 119.2(6) . . ? C54 C53 H53 120.4 . . ? C52 C53 H53 120.4 . . ? C53 C54 C55 119.2(6) . . ? C53 C54 H54 120.4 . . ? C55 C54 H54 120.4 . . ? N3 C55 C54 122.1(7) . . ? N3 C55 H55 118.9 . . ? C54 C55 H55 118.9 . . ? C66 C61 C62 115.1(5) . . ? C66 C61 B1 124.1(5) . . ? C62 C61 B1 119.8(5) . . ? C63 C62 C61 122.1(5) . . ? C63 C62 H62 118.9 . . ? C61 C62 H62 118.9 . . ? C64 C63 C62 122.0(6) . . ? C64 C63 C68 119.8(6) . . ? C62 C63 C68 118.2(5) . . ? C63 C64 C65 117.6(6) . . ? C63 C64 H64 121.2 . . ? C65 C64 H64 121.2 . . ? C64 C65 C66 121.1(5) . . ? C64 C65 C67 120.0(6) . . ? C66 C65 C67 118.9(5) . . ? C61 C66 C65 122.0(6) . . ? C61 C66 H66 119.0 . . ? C65 C66 H66 119.0 . . ? F5 C67 F6 106.3(6) . . ? F5 C67 F4 105.6(6) . . ? F6 C67 F4 104.2(6) . . ? F5 C67 C65 113.8(6) . . ? F6 C67 C65 114.1(5) . . ? F4 C67 C65 112.0(5) . . ? F2 C68 F3 108.0(6) . . ? F2 C68 F1 106.4(6) . . ? F3 C68 F1 104.5(6) . . ? F2 C68 C63 114.1(5) . . ? F3 C68 C63 112.9(6) . . ? F1 C68 C63 110.4(6) . . ? C72 C71 C76 115.5(5) . . ? C72 C71 B1 121.4(5) . . ? C76 C71 B1 122.5(5) . . ? C71 C72 C73 123.2(5) . . ? C71 C72 H72 118.4 . . ? C73 C72 H72 118.4 . . ? C74 C73 C72 119.9(6) . . ? C74 C73 C074 119.2(6) . . ? C72 C73 C074 120.9(5) . . ? C73 C74 C75 119.1(6) . . ? C73 C74 H74 120.4 . . ? C75 C74 H74 120.4 . . ? F11 C074 F12 106.8(7) . . ? F11 C074 F10 105.9(7) . . ? F12 C074 F10 105.9(6) . . ? F11 C074 C73 113.3(6) . . ? F12 C074 C73 113.0(6) . . ? F10 C074 C73 111.4(7) . . ? C74 C75 C76 120.2(6) . . ? C74 C75 C077 119.8(6) . . ? C76 C75 C077 120.0(6) . . ? C75 C76 C71 122.1(6) . . ? C75 C76 H76 119.0 . . ? C71 C76 H76 119.0 . . ? F7 C077 F8 108.9(8) . . ? F7 C077 F9 104.2(8) . . ? F8 C077 F9 99.9(7) . . ? F7 C077 C75 115.2(6) . . ? F8 C077 C75 113.3(7) . . ? F9 C077 C75 114.0(7) . . ? C82 C81 C86 116.4(5) . . ? C82 C81 B1 121.5(5) . . ? C86 C81 B1 122.0(5) . . ? C83 C82 C81 122.0(5) . . ? C83 C82 H82 119.0 . . ? C81 C82 H82 119.0 . . ? C84 C83 C82 120.7(6) . . ? C84 C83 C88 118.7(6) . . ? C82 C83 C88 120.6(6) . . ? C83 C84 C85 119.0(6) . . ? C83 C84 H84 120.5 . . ? C85 C84 H84 120.5 . . ? C86 C85 C84 119.5(6) . . ? C86 C85 C87 119.5(6) . . ? C84 C85 C87 121.0(6) . . ? C85 C86 C81 122.5(6) . . ? C85 C86 H86 118.7 . . ? C81 C86 H86 118.7 . . ? F13 C87 F14 102.1(7) . . ? F13 C87 F15 105.5(7) . . ? F14 C87 F15 104.9(8) . . ? F13 C87 C85 114.0(7) . . ? F14 C87 C85 114.1(7) . . ? F15 C87 C85 114.9(7) . . ? F18 C88 F16 105.4(9) . . ? F18 C88 F17 104.6(8) . . ? F16 C88 F17 102.9(9) . . ? F18 C88 C83 117.3(7) . . ? F16 C88 C83 113.4(7) . . ? F17 C88 C83 111.9(7) . . ? C96 C91 C92 115.9(5) . . ? C96 C91 B1 121.5(5) . . ? C92 C91 B1 122.0(5) . . ? C93 C92 C91 122.0(6) . . ? C93 C92 H92 119.0 . . ? C91 C92 H92 119.0 . . ? C92 C93 C94 120.8(6) . . ? C92 C93 C97 118.9(6) . . ? C94 C93 C97 120.3(6) . . ? C93 C94 C95 119.9(6) . . ? C93 C94 H94 120.1 . . ? C95 C94 H94 120.1 . . ? C94 C95 C96 119.0(6) . . ? C94 C95 C98 120.1(6) . . ? C96 C95 C98 120.9(6) . . ? C91 C96 C95 122.4(6) . . ? C91 C96 H96 118.8 . . ? C95 C96 H96 118.8 . . ? F24 C97 F22 106.5(6) . . ? F24 C97 F23 106.0(6) . . ? F22 C97 F23 106.2(7) . . ? F24 C97 C93 113.7(6) . . ? F22 C97 C93 111.5(5) . . ? F23 C97 C93 112.4(6) . . ? F19 C98 F20 105.6(6) . . ? F19 C98 F21 105.6(6) . . ? F20 C98 F21 102.8(6) . . ? F19 C98 C95 115.8(6) . . ? F20 C98 C95 112.3(6) . . ? F21 C98 C95 113.6(6) . . ? C31 N1 C35 119.1(6) . . ? C31 N1 Mo1 114.0(4) . . ? C35 N1 Mo1 126.9(5) . . ? C41 N2 C45 117.4(6) . . ? C51 N3 C55 118.3(5) . . ? C51 N3 Mo1 112.3(4) . . ? C55 N3 Mo1 129.3(5) . . ? C19 N4 C11 123.1(6) . . ? C19 N4 H1 131(4) . . ? C11 N4 H1 105(4) . . ? C19 N5 C13 122.4(6) . . ? C19 N5 C14 122.5(6) . . ? C13 N5 C14 115.1(6) . . ? C5 O1 Mo1 108.3(3) . . ? C61 B1 C91 103.7(5) . . ? C61 B1 C81 112.5(5) . . ? C91 B1 C81 111.6(5) . . ? C61 B1 C71 115.4(5) . . ? C91 B1 C71 112.4(5) . . ? C81 B1 C71 101.4(5) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.769 _refine_diff_density_min -0.930 _refine_diff_density_rms 0.183 #===END data_1H_DMPU_(mp175) _database_code_depnum_ccdc_archive 'CCDC 786111' #TrackingRef 'CIFS.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H12 B F24, C22 H20 Mo N3 O3, C6 H12 N2 O, 2(C H2 Cl2)' _chemical_formula_sum 'C62 H48 B Cl4 F24 Mo N5 O4' _chemical_formula_weight 1631.60 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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.3433(4) _cell_length_b 21.3842(4) _cell_length_c 16.9253(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.6440(10) _cell_angle_gamma 90.00 _cell_volume 6938.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12607 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 25.350 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3272 _exptl_absorpt_coefficient_mu 0.457 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.890 _exptl_absorpt_correction_T_max 0.915 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43998 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 25.36 _reflns_number_total 12703 _reflns_number_gt 9998 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'DIRDIF-2008 (Beurskens et al., 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [1.00000+-1.00000exp(-60.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+19.2780*P+(0.1362P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12703 _refine_ls_number_parameters 903 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0944 _refine_ls_R_factor_gt 0.0731 _refine_ls_wR_factor_ref 0.2256 _refine_ls_wR_factor_gt 0.2106 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7040(3) 0.3092(2) 0.2055(4) 0.0426(13) Uani 1 1 d . . . H1A H 0.7363 0.3362 0.1823 0.051 Uiso 1 1 calc R . . H1B H 0.6553 0.3183 0.1875 0.051 Uiso 1 1 calc R . . C2 C 0.7215(3) 0.2935(2) 0.2857(4) 0.0429(13) Uani 1 1 d . . . C3 C 0.7921(3) 0.2761(3) 0.3068(4) 0.0529(16) Uani 1 1 d . . . H3A H 0.8058 0.2629 0.3615 0.063 Uiso 1 1 calc R . . H3B H 0.8268 0.3018 0.2858 0.063 Uiso 1 1 calc R . . C4 C 0.6697(4) 0.2929(3) 0.3445(4) 0.0534(16) Uani 1 1 d . . . H4A H 0.6926 0.2806 0.3959 0.080 Uiso 1 1 calc R . . H4B H 0.6330 0.2638 0.3271 0.080 Uiso 1 1 calc R . . H4C H 0.6503 0.3340 0.3480 0.080 Uiso 1 1 calc R . . C5 C 0.6717(2) 0.1044(2) 0.3118(3) 0.0241(9) Uani 1 1 d . . . C6 C 0.8928(2) 0.1147(2) 0.3920(3) 0.0318(11) Uani 1 1 d . . . C7 C 0.9922(3) 0.1817(4) 0.4446(5) 0.0643(19) Uani 1 1 d . . . H7A H 0.9959 0.2269 0.4469 0.077 Uiso 1 1 calc R . . H7B H 1.0158 0.1650 0.4943 0.077 Uiso 1 1 calc R . . C8 C 1.0261(3) 0.1591(4) 0.3801(5) 0.076(2) Uani 1 1 d . . . H8A H 1.0162 0.1880 0.3359 0.091 Uiso 1 1 calc R . . H8B H 1.0760 0.1601 0.3967 0.091 Uiso 1 1 calc R . . C9 C 1.0079(3) 0.0978(4) 0.3514(5) 0.072(2) Uani 1 1 d . . . H9A H 1.0348 0.0676 0.3855 0.086 Uiso 1 1 calc R . . H9B H 1.0209 0.0934 0.2982 0.086 Uiso 1 1 calc R . . C10 C 0.8349(3) 0.1988(3) 0.2180(4) 0.0444(14) Uani 1 1 d . . . C11 C 0.1222(17) -0.0540(13) 0.1027(15) 0.33(2) Uani 1 1 d . . . H11A H 0.0775 -0.0338 0.0875 0.396 Uiso 1 1 calc R . . H11B H 0.1209 -0.0729 0.1546 0.396 Uiso 1 1 calc R . . C12 C 0.5335(4) 0.0958(3) 0.0216(4) 0.0534(15) Uani 1 1 d . . . H12A H 0.4976 0.1218 0.0397 0.064 Uiso 1 1 calc R . . H12B H 0.5148 0.0780 -0.0294 0.064 Uiso 1 1 calc R . . C15 C 0.8777(3) 0.1934(3) 0.4922(4) 0.0458(14) Uani 1 1 d . . . H15A H 0.9038 0.2274 0.5184 0.069 Uiso 1 1 calc R . . H15B H 0.8676 0.1633 0.5312 0.069 Uiso 1 1 calc R . . H15C H 0.8348 0.2091 0.4641 0.069 Uiso 1 1 calc R . . C16 C 0.9082(3) 0.0313(3) 0.2984(5) 0.0596(17) Uani 1 1 d . . . H16A H 0.9451 0.0145 0.2721 0.089 Uiso 1 1 calc R . . H16B H 0.8711 0.0457 0.2593 0.089 Uiso 1 1 calc R . . H16C H 0.8909 -0.0006 0.3305 0.089 Uiso 1 1 calc R . . C20 C 0.7375(3) 0.2302(3) 0.1121(3) 0.0392(12) Uani 1 1 d . . . C31 C 0.7011(2) 0.0655(2) 0.2465(3) 0.0269(10) Uani 1 1 d . . . C32 C 0.6991(3) 0.0011(2) 0.2392(3) 0.0345(11) Uani 1 1 d . . . H32 H 0.6789 -0.0234 0.2753 0.041 Uiso 1 1 calc R . . C33 C 0.7277(3) -0.0259(3) 0.1770(4) 0.0452(14) Uani 1 1 d . . . H33 H 0.7277 -0.0691 0.1715 0.054 Uiso 1 1 calc R . . C34 C 0.7561(3) 0.0106(3) 0.1238(4) 0.0472(14) Uani 1 1 d . . . H34 H 0.7750 -0.0073 0.0814 0.057 Uiso 1 1 calc R . . C35 C 0.7566(3) 0.0750(3) 0.1338(3) 0.0405(13) Uani 1 1 d . . . H35 H 0.7759 0.1001 0.0976 0.049 Uiso 1 1 calc R . . C41 C 0.6568(2) 0.0686(2) 0.3858(3) 0.0263(10) Uani 1 1 d . . . C42 C 0.6785(2) 0.0911(2) 0.4621(3) 0.0306(10) Uani 1 1 d . . . H42 H 0.7050 0.1274 0.4702 0.037 Uiso 1 1 calc R . . C43 C 0.6593(3) 0.0577(3) 0.5258(3) 0.0382(12) Uani 1 1 d . . . H43 H 0.6730 0.0715 0.5777 0.046 Uiso 1 1 calc R . . C44 C 0.6201(3) 0.0045(3) 0.5126(3) 0.0403(13) Uani 1 1 d . . . H44 H 0.6072 -0.0185 0.5549 0.048 Uiso 1 1 calc R . . C45 C 0.6004(3) -0.0143(2) 0.4346(3) 0.0430(13) Uani 1 1 d . . . H45 H 0.5736 -0.0503 0.4254 0.052 Uiso 1 1 calc R . . C51 C 0.6066(2) 0.1381(2) 0.2706(3) 0.0228(9) Uani 1 1 d . . . C52 C 0.5385(2) 0.1219(2) 0.2797(3) 0.0267(10) Uani 1 1 d . . . H52 H 0.5296 0.0901 0.3144 0.032 Uiso 1 1 calc R . . C53 C 0.4840(2) 0.1540(2) 0.2361(3) 0.0291(10) Uani 1 1 d . . . H53 H 0.4380 0.1445 0.2420 0.035 Uiso 1 1 calc R . . C54 C 0.4984(2) 0.2000(2) 0.1840(3) 0.0293(10) Uani 1 1 d . . . H54 H 0.4625 0.2215 0.1535 0.035 Uiso 1 1 calc R . . C55 C 0.5671(3) 0.2137(2) 0.1777(3) 0.0314(11) Uani 1 1 d . . . H55 H 0.5768 0.2447 0.1422 0.038 Uiso 1 1 calc R . . C61 C 0.3264(2) 0.2037(2) 0.3389(3) 0.0225(9) Uani 1 1 d . . . C62 C 0.3772(2) 0.1803(2) 0.3982(3) 0.0236(9) Uani 1 1 d . . . H62 H 0.3677 0.1436 0.4242 0.028 Uiso 1 1 calc R . . C63 C 0.4407(2) 0.2092(2) 0.4197(3) 0.0247(9) Uani 1 1 d . . . C64 C 0.4577(2) 0.2639(2) 0.3824(3) 0.0268(10) Uani 1 1 d . . . H64 H 0.5005 0.2834 0.3964 0.032 Uiso 1 1 calc R . . C65 C 0.4081(2) 0.2887(2) 0.3232(3) 0.0259(10) Uani 1 1 d . . . C66 C 0.3441(2) 0.2594(2) 0.3022(3) 0.0239(9) Uani 1 1 d . . . H66 H 0.3120 0.2772 0.2628 0.029 Uiso 1 1 calc R . . C67 C 0.4921(2) 0.1791(2) 0.4828(3) 0.0310(10) Uani 1 1 d . . . C68 C 0.4266(3) 0.3472(2) 0.2817(3) 0.0323(11) Uani 1 1 d . . . C71 C 0.2312(2) 0.1167(2) 0.3711(3) 0.0212(9) Uani 1 1 d . . . C72 C 0.2309(2) 0.1370(2) 0.4495(3) 0.0258(10) Uani 1 1 d . . . H72 H 0.2504 0.1757 0.4645 0.031 Uiso 1 1 calc R . . C73 C 0.2025(2) 0.1013(2) 0.5059(3) 0.0292(10) Uani 1 1 d . . . C74 C 0.1738(2) 0.0432(2) 0.4867(3) 0.0317(11) Uani 1 1 d . . . H74 H 0.1565 0.0187 0.5250 0.038 Uiso 1 1 calc R . . C75 C 0.1715(2) 0.0224(2) 0.4086(3) 0.0282(10) Uani 1 1 d . . . C76 C 0.1994(2) 0.0588(2) 0.3519(3) 0.0236(9) Uani 1 1 d . . . H76 H 0.1967 0.0442 0.2998 0.028 Uiso 1 1 calc R . . C77 C 0.2013(3) 0.1265(3) 0.5874(3) 0.0401(12) Uani 1 1 d . . . C78 C 0.1380(3) -0.0384(2) 0.3837(3) 0.0348(11) Uani 1 1 d . . . C81 C 0.2896(2) 0.12114(19) 0.2330(3) 0.0216(9) Uani 1 1 d . . . C82 C 0.3246(2) 0.0644(2) 0.2490(3) 0.0244(9) Uani 1 1 d . . . H82 H 0.3263 0.0468 0.2994 0.029 Uiso 1 1 calc R . . C83 C 0.3571(2) 0.0335(2) 0.1915(3) 0.0300(10) Uani 1 1 d . . . C84 C 0.3561(3) 0.0581(2) 0.1158(3) 0.0309(10) Uani 1 1 d . . . H84 H 0.3776 0.0374 0.0773 0.037 Uiso 1 1 calc R . . C85 C 0.3221(2) 0.1146(2) 0.0992(3) 0.0293(10) Uani 1 1 d . . . C86 C 0.2901(2) 0.1452(2) 0.1566(3) 0.0249(9) Uani 1 1 d . . . H86 H 0.2681 0.1832 0.1437 0.030 Uiso 1 1 calc R . . C87 C 0.3202(3) 0.1438(3) 0.0188(3) 0.0393(12) Uani 1 1 d . . . C88 C 0.3962(3) -0.0258(2) 0.2147(3) 0.0384(12) Uani 1 1 d . . . C91 C 0.1898(2) 0.2014(2) 0.2665(3) 0.0250(9) Uani 1 1 d . . . C92 C 0.1697(2) 0.2583(2) 0.2978(3) 0.0314(11) Uani 1 1 d . . . H92 H 0.1992 0.2774 0.3386 0.038 Uiso 1 1 calc R . . C93 C 0.1067(3) 0.2869(2) 0.2695(4) 0.0378(12) Uani 1 1 d . . . C94 C 0.0618(3) 0.2607(3) 0.2090(3) 0.0422(14) Uani 1 1 d . . . H94 H 0.0201 0.2804 0.1898 0.051 Uiso 1 1 calc R . . C95 C 0.0797(3) 0.2044(3) 0.1770(3) 0.0392(13) Uani 1 1 d . . . C96 C 0.1425(2) 0.1757(2) 0.2061(3) 0.0317(11) Uani 1 1 d . . . H96 H 0.1534 0.1376 0.1841 0.038 Uiso 1 1 calc R . . C97 C 0.0871(3) 0.3467(3) 0.3071(5) 0.0557(18) Uani 1 1 d . . . C98 C 0.0335(3) 0.1711(4) 0.1115(4) 0.0619(19) Uani 1 1 d . . . N1 N 0.7296(2) 0.10186(19) 0.1946(2) 0.0309(9) Uani 1 1 d . . . N2 N 0.62054(19) 0.18416(18) 0.2206(2) 0.0252(8) Uani 1 1 d . . . N3 N 0.6179(2) 0.0169(2) 0.3719(3) 0.0370(10) Uani 1 1 d . . . N4 N 0.9181(2) 0.1639(2) 0.4363(3) 0.0391(10) Uani 1 1 d . . . N5 N 0.9345(2) 0.0830(2) 0.3485(3) 0.0408(11) Uani 1 1 d . . . O1 O 0.72198(15) 0.15328(14) 0.33365(19) 0.0245(7) Uani 1 1 d D . . O2 O 0.82983(16) 0.09769(15) 0.3909(2) 0.0355(8) Uani 1 1 d . . . O10 O 0.8942(3) 0.1965(2) 0.2135(3) 0.0689(13) Uiso 1 1 d . . . O20 O 0.7407(2) 0.2448(2) 0.0469(3) 0.0553(11) Uiso 1 1 d . . . F1 F 0.55586(17) 0.20391(16) 0.4883(2) 0.0567(10) Uani 1 1 d . . . F2 F 0.49932(15) 0.11801(13) 0.47061(18) 0.0383(7) Uani 1 1 d . . . F3 F 0.47229(19) 0.18366(18) 0.55549(18) 0.0543(9) Uani 1 1 d . . . F4 F 0.48900(19) 0.34363(15) 0.2565(3) 0.0616(10) Uani 1 1 d . . . F5 F 0.4305(2) 0.39693(14) 0.3289(2) 0.0604(10) Uani 1 1 d . . . F6 F 0.3825(2) 0.36088(19) 0.2177(3) 0.0791(14) Uani 1 1 d . . . F7 F 0.2106(6) 0.0880(3) 0.6429(3) 0.179(4) Uani 1 1 d . . . F8 F 0.2440(6) 0.1673(5) 0.6089(4) 0.222(6) Uani 1 1 d . . . F9 F 0.1457(4) 0.1502(6) 0.5970(4) 0.240(7) Uani 1 1 d . . . F10 F 0.08942(17) -0.05584(15) 0.4287(2) 0.0515(9) Uani 1 1 d . . . F11 F 0.1059(2) -0.03787(16) 0.3095(2) 0.0600(10) Uani 1 1 d . . . F12 F 0.18369(17) -0.08585(14) 0.3882(3) 0.0595(10) Uani 1 1 d . . . F13 F 0.3405(4) 0.2023(2) 0.0219(2) 0.110(2) Uani 1 1 d . . . F14 F 0.3591(3) 0.1151(2) -0.0283(2) 0.0812(14) Uani 1 1 d . . . F15 F 0.2577(2) 0.1429(3) -0.0223(3) 0.0944(17) Uani 1 1 d . . . F16 F 0.4111(2) -0.05869(17) 0.1532(2) 0.0688(11) Uani 1 1 d . . . F17 F 0.3602(2) -0.06382(16) 0.2550(3) 0.0829(15) Uani 1 1 d . . . F18 F 0.4561(2) -0.01531(18) 0.2603(3) 0.0881(16) Uani 1 1 d . . . F19 F 0.0093(2) 0.1173(2) 0.1352(3) 0.0853(14) Uani 1 1 d . . . F20 F -0.0224(2) 0.2054(2) 0.0836(3) 0.0800(14) Uani 1 1 d . . . F21 F 0.0666(2) 0.1599(4) 0.0494(3) 0.118(2) Uani 1 1 d . . . F22 F 0.0603(5) 0.3383(2) 0.3697(4) 0.175(4) Uani 1 1 d . . . F23 F 0.1351(3) 0.3861(2) 0.3172(6) 0.148(3) Uani 1 1 d . . . F24 F 0.0384(4) 0.3779(3) 0.2606(5) 0.146(3) Uani 1 1 d . . . Mo1 Mo 0.73504(2) 0.203758(19) 0.22152(3) 0.02791(16) Uani 1 1 d . . . B1 B 0.2588(2) 0.1618(2) 0.3031(3) 0.0221(10) Uani 1 1 d . . . Cl1 Cl 0.1302(5) -0.1125(3) 0.0362(3) 0.257(4) Uani 1 1 d . . . Cl2 Cl 0.1787(4) -0.0028(4) 0.1119(4) 0.277(4) Uani 1 1 d . . . Cl3 Cl 0.55447(10) 0.03538(8) 0.09011(10) 0.0656(5) Uani 1 1 d . . . Cl4 Cl 0.60559(9) 0.14254(8) 0.00919(10) 0.0593(4) Uani 1 1 d . . . H1 H 0.761(2) 0.135(3) 0.349(4) 0.071 Uiso 1 1 d 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 C1 0.053(3) 0.023(2) 0.053(4) 0.009(2) 0.012(3) -0.005(2) C2 0.057(4) 0.022(2) 0.050(3) 0.004(2) 0.005(3) -0.007(2) C3 0.056(4) 0.038(3) 0.060(4) 0.005(3) -0.008(3) -0.016(3) C4 0.085(5) 0.029(3) 0.049(4) -0.004(2) 0.019(3) 0.006(3) C5 0.022(2) 0.021(2) 0.029(2) 0.0017(18) 0.0022(18) -0.0036(17) C6 0.029(2) 0.025(2) 0.041(3) 0.010(2) 0.003(2) 0.0024(19) C7 0.031(3) 0.075(5) 0.089(5) -0.015(4) 0.016(3) -0.020(3) C8 0.032(3) 0.102(6) 0.097(6) -0.023(5) 0.025(4) -0.020(4) C9 0.032(3) 0.091(6) 0.095(6) -0.033(5) 0.022(3) 0.000(3) C10 0.018(2) 0.058(4) 0.060(4) 0.017(3) 0.013(2) -0.004(2) C11 0.47(5) 0.32(3) 0.22(2) -0.17(2) 0.14(3) -0.25(3) C12 0.061(4) 0.054(4) 0.043(3) -0.003(3) 0.001(3) 0.003(3) C15 0.040(3) 0.035(3) 0.065(4) -0.005(3) 0.018(3) -0.003(2) C16 0.048(4) 0.051(4) 0.079(5) -0.020(3) 0.010(3) 0.002(3) C20 0.040(3) 0.047(3) 0.033(3) 0.014(2) 0.014(2) -0.005(2) C31 0.023(2) 0.028(2) 0.029(2) 0.0016(19) 0.0008(19) 0.0040(18) C32 0.035(3) 0.028(3) 0.039(3) -0.004(2) 0.001(2) 0.001(2) C33 0.048(3) 0.036(3) 0.051(4) -0.012(3) 0.004(3) 0.007(2) C34 0.050(3) 0.049(3) 0.045(3) -0.012(3) 0.015(3) 0.012(3) C35 0.036(3) 0.049(3) 0.039(3) 0.000(2) 0.014(2) 0.011(2) C41 0.024(2) 0.023(2) 0.032(2) 0.0052(19) 0.0030(19) -0.0010(18) C42 0.026(2) 0.038(3) 0.028(2) 0.005(2) 0.0037(19) -0.002(2) C43 0.031(3) 0.054(3) 0.030(3) 0.006(2) 0.004(2) 0.003(2) C44 0.041(3) 0.041(3) 0.040(3) 0.015(2) 0.009(2) 0.001(2) C45 0.053(3) 0.030(3) 0.048(3) 0.010(2) 0.011(3) -0.009(2) C51 0.024(2) 0.025(2) 0.020(2) -0.0018(17) 0.0046(17) -0.0033(17) C52 0.029(2) 0.027(2) 0.025(2) -0.0021(18) 0.0062(19) -0.0046(19) C53 0.023(2) 0.034(3) 0.032(3) -0.008(2) 0.0099(19) -0.0030(19) C54 0.025(2) 0.031(3) 0.031(3) -0.002(2) 0.001(2) 0.0050(19) C55 0.032(3) 0.031(3) 0.031(3) 0.006(2) 0.006(2) 0.002(2) C61 0.023(2) 0.022(2) 0.023(2) -0.0015(17) 0.0054(18) 0.0014(17) C62 0.027(2) 0.021(2) 0.023(2) -0.0006(17) 0.0055(18) 0.0005(17) C63 0.027(2) 0.022(2) 0.026(2) -0.0064(18) 0.0048(19) 0.0010(17) C64 0.025(2) 0.025(2) 0.031(3) -0.0062(19) 0.0051(19) -0.0023(18) C65 0.030(2) 0.021(2) 0.028(2) -0.0023(18) 0.0088(19) -0.0024(18) C66 0.025(2) 0.021(2) 0.026(2) -0.0001(17) 0.0040(18) 0.0010(17) C67 0.027(2) 0.033(3) 0.031(3) -0.001(2) -0.003(2) -0.003(2) C68 0.035(3) 0.022(2) 0.040(3) 0.000(2) 0.004(2) -0.0056(19) C71 0.019(2) 0.023(2) 0.021(2) 0.0027(17) 0.0027(17) 0.0032(16) C72 0.022(2) 0.025(2) 0.031(2) 0.0031(19) 0.0038(19) 0.0003(17) C73 0.025(2) 0.037(3) 0.026(2) 0.005(2) 0.0057(19) 0.003(2) C74 0.026(2) 0.040(3) 0.031(3) 0.013(2) 0.010(2) 0.003(2) C75 0.019(2) 0.027(2) 0.038(3) 0.008(2) 0.0043(19) 0.0022(18) C76 0.018(2) 0.029(2) 0.025(2) -0.0004(18) 0.0042(17) 0.0006(17) C77 0.044(3) 0.051(3) 0.028(3) -0.001(2) 0.016(2) -0.007(3) C78 0.030(3) 0.034(3) 0.041(3) 0.008(2) 0.009(2) -0.003(2) C81 0.018(2) 0.020(2) 0.026(2) -0.0007(17) 0.0028(17) -0.0031(16) C82 0.026(2) 0.022(2) 0.026(2) 0.0008(18) 0.0060(18) -0.0055(17) C83 0.031(2) 0.023(2) 0.037(3) -0.004(2) 0.012(2) -0.0036(19) C84 0.034(2) 0.027(2) 0.034(3) -0.008(2) 0.011(2) -0.001(2) C85 0.029(2) 0.034(3) 0.025(2) -0.001(2) 0.0059(19) -0.005(2) C86 0.024(2) 0.025(2) 0.026(2) 0.0024(18) 0.0049(18) -0.0016(17) C87 0.041(3) 0.049(3) 0.029(3) 0.000(2) 0.010(2) -0.001(2) C88 0.047(3) 0.025(3) 0.046(3) -0.004(2) 0.017(3) 0.003(2) C91 0.025(2) 0.025(2) 0.026(2) 0.0059(18) 0.0073(19) -0.0012(17) C92 0.023(2) 0.031(3) 0.042(3) 0.005(2) 0.011(2) 0.0010(19) C93 0.030(3) 0.032(3) 0.055(3) 0.016(2) 0.019(2) 0.007(2) C94 0.025(2) 0.051(3) 0.052(3) 0.026(3) 0.008(2) 0.010(2) C95 0.024(2) 0.062(4) 0.032(3) 0.018(2) 0.004(2) 0.000(2) C96 0.028(2) 0.040(3) 0.027(2) 0.008(2) 0.005(2) -0.001(2) C97 0.044(3) 0.035(3) 0.094(5) 0.015(3) 0.029(3) 0.016(3) C98 0.042(3) 0.108(6) 0.032(3) 0.006(3) -0.010(3) 0.010(4) N1 0.028(2) 0.034(2) 0.032(2) -0.0008(17) 0.0070(17) 0.0053(16) N2 0.0229(18) 0.0263(19) 0.027(2) 0.0036(16) 0.0049(16) -0.0024(15) N3 0.044(2) 0.032(2) 0.036(2) 0.0035(18) 0.008(2) -0.0083(19) N4 0.026(2) 0.039(2) 0.054(3) -0.003(2) 0.013(2) -0.0057(18) N5 0.028(2) 0.044(3) 0.052(3) -0.004(2) 0.007(2) 0.0054(19) O1 0.0217(15) 0.0220(16) 0.0290(17) 0.0029(13) 0.0008(13) -0.0041(12) O2 0.0219(16) 0.0308(18) 0.054(2) 0.0092(16) 0.0039(15) -0.0014(14) F1 0.0318(16) 0.053(2) 0.079(3) 0.0180(18) -0.0178(17) -0.0115(14) F2 0.0379(16) 0.0309(15) 0.0431(17) 0.0014(13) -0.0059(13) 0.0058(12) F3 0.066(2) 0.069(2) 0.0256(16) -0.0029(15) -0.0027(15) 0.0166(18) F4 0.064(2) 0.0383(18) 0.093(3) 0.0126(18) 0.048(2) 0.0001(16) F5 0.097(3) 0.0237(16) 0.067(2) -0.0078(15) 0.037(2) -0.0124(17) F6 0.083(3) 0.067(2) 0.077(3) 0.044(2) -0.028(2) -0.039(2) F7 0.412(14) 0.099(4) 0.029(2) 0.006(3) 0.033(4) 0.051(6) F8 0.321(12) 0.297(11) 0.069(4) -0.108(6) 0.108(6) -0.230(10) F9 0.170(7) 0.461(17) 0.073(4) -0.137(7) -0.037(4) 0.196(10) F10 0.0444(18) 0.0397(17) 0.075(2) 0.0055(16) 0.0235(17) -0.0155(14) F11 0.072(2) 0.048(2) 0.056(2) 0.0013(16) -0.0073(18) -0.0296(18) F12 0.0410(18) 0.0296(16) 0.109(3) -0.0079(18) 0.0156(19) 0.0018(14) F13 0.232(7) 0.062(3) 0.039(2) 0.0085(19) 0.033(3) -0.055(3) F14 0.109(3) 0.104(3) 0.038(2) 0.015(2) 0.041(2) 0.037(3) F15 0.064(3) 0.169(5) 0.049(2) 0.046(3) 0.003(2) 0.013(3) F16 0.100(3) 0.045(2) 0.064(2) -0.0105(18) 0.023(2) 0.030(2) F17 0.106(3) 0.0319(19) 0.125(4) 0.028(2) 0.069(3) 0.021(2) F18 0.078(3) 0.041(2) 0.130(4) -0.012(2) -0.043(3) 0.0210(19) F19 0.077(3) 0.081(3) 0.085(3) -0.007(3) -0.036(2) -0.013(2) F20 0.043(2) 0.131(4) 0.058(2) 0.026(2) -0.0200(19) 0.009(2) F21 0.058(3) 0.246(8) 0.046(3) -0.045(3) -0.004(2) 0.013(4) F22 0.346(11) 0.052(3) 0.169(6) -0.005(3) 0.191(8) 0.026(4) F23 0.080(3) 0.066(3) 0.307(10) -0.087(5) 0.054(5) -0.008(3) F24 0.147(5) 0.085(4) 0.191(7) -0.018(4) -0.028(5) 0.081(4) Mo1 0.0236(2) 0.0282(2) 0.0329(3) 0.00701(17) 0.00720(17) -0.00317(15) B1 0.020(2) 0.024(2) 0.021(2) 0.001(2) 0.0020(19) -0.0009(19) Cl1 0.448(11) 0.176(5) 0.154(4) -0.033(4) 0.064(5) -0.086(6) Cl2 0.266(7) 0.322(8) 0.261(7) -0.167(7) 0.101(6) -0.170(7) Cl3 0.0768(11) 0.0617(10) 0.0546(10) 0.0104(8) -0.0050(8) -0.0116(8) Cl4 0.0661(10) 0.0622(10) 0.0498(9) 0.0026(7) 0.0084(8) -0.0058(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; 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 C1 C2 1.395(8) . ? C1 Mo1 2.340(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.416(9) . ? C2 C4 1.504(9) . ? C2 Mo1 2.238(5) . ? C3 Mo1 2.297(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 O1 1.442(5) . ? C5 C41 1.527(6) . ? C5 C51 1.536(6) . ? C5 C31 1.552(6) . ? C6 O2 1.268(6) . ? C6 N5 1.345(7) . ? C6 N4 1.346(7) . ? C7 C8 1.430(10) . ? C7 N4 1.471(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.426(11) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N5 1.449(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 O10 1.161(7) . ? C10 Mo1 1.943(5) . ? C11 Cl2 1.54(2) . ? C11 Cl1 1.70(2) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 Cl3 1.747(7) . ? C12 Cl4 1.750(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C15 N4 1.451(7) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 N5 1.444(8) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C20 O20 1.158(6) . ? C20 Mo1 1.943(5) . ? C31 N1 1.345(6) . ? C31 C32 1.381(7) . ? C32 C33 1.379(8) . ? C32 H32 0.9300 . ? C33 C34 1.362(9) . ? C33 H33 0.9300 . ? C34 C35 1.387(8) . ? C34 H34 0.9300 . ? C35 N1 1.343(6) . ? C35 H35 0.9300 . ? C41 N3 1.342(6) . ? C41 C42 1.390(7) . ? C42 C43 1.384(7) . ? C42 H42 0.9300 . ? C43 C44 1.370(8) . ? C43 H43 0.9300 . ? C44 C45 1.384(8) . ? C44 H44 0.9300 . ? C45 N3 1.334(7) . ? C45 H45 0.9300 . ? C51 N2 1.349(6) . ? C51 C52 1.391(6) . ? C52 C53 1.385(7) . ? C52 H52 0.9300 . ? C53 C54 1.375(7) . ? C53 H53 0.9300 . ? C54 C55 1.378(7) . ? C54 H54 0.9300 . ? C55 N2 1.340(6) . ? C55 H55 0.9300 . ? C61 C62 1.400(6) . ? C61 C66 1.406(6) . ? C61 B1 1.634(6) . ? C62 C63 1.380(6) . ? C62 H62 0.9300 . ? C63 C64 1.390(7) . ? C63 C67 1.503(7) . ? C64 C65 1.395(7) . ? C64 H64 0.9300 . ? C65 C66 1.391(6) . ? C65 C68 1.501(6) . ? C66 H66 0.9300 . ? C67 F2 1.333(6) . ? C67 F1 1.334(6) . ? C67 F3 1.341(6) . ? C68 F6 1.319(6) . ? C68 F5 1.327(6) . ? C68 F4 1.336(6) . ? C71 C72 1.397(6) . ? C71 C76 1.402(6) . ? C71 B1 1.644(6) . ? C72 C73 1.392(6) . ? C72 H72 0.9300 . ? C73 C74 1.380(7) . ? C73 C77 1.484(7) . ? C74 C75 1.390(7) . ? C74 H74 0.9300 . ? C75 C76 1.399(6) . ? C75 C78 1.489(7) . ? C76 H76 0.9300 . ? C77 F9 1.219(8) . ? C77 F8 1.223(8) . ? C77 F7 1.242(7) . ? C78 F11 1.325(6) . ? C78 F10 1.339(6) . ? C78 F12 1.341(6) . ? C81 C86 1.392(6) . ? C81 C82 1.398(6) . ? C81 B1 1.645(6) . ? C82 C83 1.393(6) . ? C82 H82 0.9300 . ? C83 C84 1.383(7) . ? C83 C88 1.502(7) . ? C84 C85 1.387(7) . ? C84 H84 0.9300 . ? C85 C86 1.384(6) . ? C85 C87 1.493(7) . ? C86 H86 0.9300 . ? C87 F13 1.311(7) . ? C87 F15 1.313(7) . ? C87 F14 1.317(6) . ? C88 F17 1.318(6) . ? C88 F16 1.319(6) . ? C88 F18 1.324(7) . ? C91 C96 1.392(7) . ? C91 C92 1.403(7) . ? C91 B1 1.632(6) . ? C92 C93 1.389(7) . ? C92 H92 0.9300 . ? C93 C94 1.372(8) . ? C93 C97 1.500(8) . ? C94 C95 1.383(8) . ? C94 H94 0.9300 . ? C95 C96 1.390(7) . ? C95 C98 1.507(9) . ? C96 H96 0.9300 . ? C97 F23 1.247(8) . ? C97 F22 1.252(8) . ? C97 F24 1.325(8) . ? C98 F19 1.323(9) . ? C98 F21 1.323(8) . ? C98 F20 1.340(8) . ? N1 Mo1 2.226(4) . ? N2 Mo1 2.252(4) . ? O1 Mo1 2.227(3) . ? O1 H1 0.86(3) . ? 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 C1 Mo1 68.3(3) . . ? C2 C1 H1A 116.8 . . ? Mo1 C1 H1A 116.8 . . ? C2 C1 H1B 116.8 . . ? Mo1 C1 H1B 116.8 . . ? H1A C1 H1B 113.9 . . ? C1 C2 C3 114.2(6) . . ? C1 C2 C4 123.4(6) . . ? C3 C2 C4 122.4(6) . . ? C1 C2 Mo1 76.3(3) . . ? C3 C2 Mo1 74.1(3) . . ? C4 C2 Mo1 116.4(4) . . ? C2 C3 Mo1 69.6(3) . . ? C2 C3 H3A 116.7 . . ? Mo1 C3 H3A 116.7 . . ? C2 C3 H3B 116.7 . . ? Mo1 C3 H3B 116.7 . . ? H3A C3 H3B 113.7 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O1 C5 C41 110.3(4) . . ? O1 C5 C51 105.1(3) . . ? C41 C5 C51 112.0(3) . . ? O1 C5 C31 105.9(3) . . ? C41 C5 C31 116.3(4) . . ? C51 C5 C31 106.5(3) . . ? O2 C6 N5 119.5(5) . . ? O2 C6 N4 120.6(4) . . ? N5 C6 N4 119.9(4) . . ? C8 C7 N4 112.3(6) . . ? C8 C7 H7A 109.1 . . ? N4 C7 H7A 109.1 . . ? C8 C7 H7B 109.1 . . ? N4 C7 H7B 109.1 . . ? H7A C7 H7B 107.9 . . ? C9 C8 C7 116.9(6) . . ? C9 C8 H8A 108.1 . . ? C7 C8 H8A 108.1 . . ? C9 C8 H8B 108.1 . . ? C7 C8 H8B 108.1 . . ? H8A C8 H8B 107.3 . . ? C8 C9 N5 114.1(5) . . ? C8 C9 H9A 108.7 . . ? N5 C9 H9A 108.7 . . ? C8 C9 H9B 108.7 . . ? N5 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? O10 C10 Mo1 177.8(6) . . ? Cl2 C11 Cl1 117.6(17) . . ? Cl2 C11 H11A 107.9 . . ? Cl1 C11 H11A 107.9 . . ? Cl2 C11 H11B 107.9 . . ? Cl1 C11 H11B 107.9 . . ? H11A C11 H11B 107.2 . . ? Cl3 C12 Cl4 112.6(4) . . ? Cl3 C12 H12A 109.1 . . ? Cl4 C12 H12A 109.1 . . ? Cl3 C12 H12B 109.1 . . ? Cl4 C12 H12B 109.1 . . ? H12A C12 H12B 107.8 . . ? N4 C15 H15A 109.5 . . ? N4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N5 C16 H16A 109.5 . . ? N5 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N5 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O20 C20 Mo1 177.9(5) . . ? N1 C31 C32 121.8(4) . . ? N1 C31 C5 112.1(4) . . ? C32 C31 C5 126.1(4) . . ? C33 C32 C31 118.4(5) . . ? C33 C32 H32 120.8 . . ? C31 C32 H32 120.8 . . ? C34 C33 C32 120.2(5) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C35 119.0(5) . . ? C33 C34 H34 120.5 . . ? C35 C34 H34 120.5 . . ? N1 C35 C34 121.4(5) . . ? N1 C35 H35 119.3 . . ? C34 C35 H35 119.3 . . ? N3 C41 C42 122.7(4) . . ? N3 C41 C5 115.6(4) . . ? C42 C41 C5 121.5(4) . . ? C43 C42 C41 117.8(5) . . ? C43 C42 H42 121.1 . . ? C41 C42 H42 121.1 . . ? C44 C43 C42 120.1(5) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 118.3(5) . . ? C43 C44 H44 120.9 . . ? C45 C44 H44 120.9 . . ? N3 C45 C44 123.1(5) . . ? N3 C45 H45 118.4 . . ? C44 C45 H45 118.4 . . ? N2 C51 C52 121.5(4) . . ? N2 C51 C5 114.1(4) . . ? C52 C51 C5 124.4(4) . . ? C53 C52 C51 118.9(4) . . ? C53 C52 H52 120.5 . . ? C51 C52 H52 120.5 . . ? C54 C53 C52 119.4(4) . . ? C54 C53 H53 120.3 . . ? C52 C53 H53 120.3 . . ? C53 C54 C55 118.8(4) . . ? C53 C54 H54 120.6 . . ? C55 C54 H54 120.6 . . ? N2 C55 C54 122.6(4) . . ? N2 C55 H55 118.7 . . ? C54 C55 H55 118.7 . . ? C62 C61 C66 115.5(4) . . ? C62 C61 B1 121.3(4) . . ? C66 C61 B1 122.0(4) . . ? C63 C62 C61 123.0(4) . . ? C63 C62 H62 118.5 . . ? C61 C62 H62 118.5 . . ? C62 C63 C64 120.8(4) . . ? C62 C63 C67 118.5(4) . . ? C64 C63 C67 120.6(4) . . ? C63 C64 C65 117.7(4) . . ? C63 C64 H64 121.1 . . ? C65 C64 H64 121.1 . . ? C66 C65 C64 121.0(4) . . ? C66 C65 C68 121.0(4) . . ? C64 C65 C68 118.0(4) . . ? C65 C66 C61 121.9(4) . . ? C65 C66 H66 119.0 . . ? C61 C66 H66 119.0 . . ? F2 C67 F1 106.6(4) . . ? F2 C67 F3 105.1(4) . . ? F1 C67 F3 106.3(4) . . ? F2 C67 C63 112.5(4) . . ? F1 C67 C63 113.4(4) . . ? F3 C67 C63 112.2(4) . . ? F6 C68 F5 107.2(4) . . ? F6 C68 F4 105.3(5) . . ? F5 C68 F4 104.9(4) . . ? F6 C68 C65 113.6(4) . . ? F5 C68 C65 112.6(4) . . ? F4 C68 C65 112.5(4) . . ? C72 C71 C76 115.9(4) . . ? C72 C71 B1 121.8(4) . . ? C76 C71 B1 121.9(4) . . ? C73 C72 C71 122.2(4) . . ? C73 C72 H72 118.9 . . ? C71 C72 H72 118.9 . . ? C74 C73 C72 121.0(4) . . ? C74 C73 C77 119.4(4) . . ? C72 C73 C77 119.7(4) . . ? C73 C74 C75 118.3(4) . . ? C73 C74 H74 120.9 . . ? C75 C74 H74 120.9 . . ? C74 C75 C76 120.5(4) . . ? C74 C75 C78 120.5(4) . . ? C76 C75 C78 119.0(4) . . ? C75 C76 C71 122.0(4) . . ? C75 C76 H76 119.0 . . ? C71 C76 H76 119.0 . . ? F9 C77 F8 103.7(9) . . ? F9 C77 F7 102.5(8) . . ? F8 C77 F7 103.0(8) . . ? F9 C77 C73 113.4(5) . . ? F8 C77 C73 116.2(5) . . ? F7 C77 C73 116.3(5) . . ? F11 C78 F10 105.5(4) . . ? F11 C78 F12 106.4(5) . . ? F10 C78 F12 105.3(4) . . ? F11 C78 C75 113.1(4) . . ? F10 C78 C75 113.2(4) . . ? F12 C78 C75 112.6(4) . . ? C86 C81 C82 115.9(4) . . ? C86 C81 B1 121.5(4) . . ? C82 C81 B1 122.1(4) . . ? C83 C82 C81 121.9(4) . . ? C83 C82 H82 119.0 . . ? C81 C82 H82 119.0 . . ? C84 C83 C82 121.0(4) . . ? C84 C83 C88 120.5(4) . . ? C82 C83 C88 118.5(4) . . ? C83 C84 C85 117.8(4) . . ? C83 C84 H84 121.1 . . ? C85 C84 H84 121.1 . . ? C86 C85 C84 120.9(4) . . ? C86 C85 C87 119.0(4) . . ? C84 C85 C87 120.1(4) . . ? C85 C86 C81 122.5(4) . . ? C85 C86 H86 118.8 . . ? C81 C86 H86 118.8 . . ? F13 C87 F15 106.5(6) . . ? F13 C87 F14 106.1(5) . . ? F15 C87 F14 103.4(5) . . ? F13 C87 C85 113.0(5) . . ? F15 C87 C85 112.8(4) . . ? F14 C87 C85 114.3(5) . . ? F17 C88 F16 105.5(4) . . ? F17 C88 F18 106.5(5) . . ? F16 C88 F18 106.5(5) . . ? F17 C88 C83 112.0(4) . . ? F16 C88 C83 113.5(5) . . ? F18 C88 C83 112.3(4) . . ? C96 C91 C92 115.6(4) . . ? C96 C91 B1 119.9(4) . . ? C92 C91 B1 124.1(4) . . ? C93 C92 C91 121.7(5) . . ? C93 C92 H92 119.2 . . ? C91 C92 H92 119.2 . . ? C94 C93 C92 121.1(5) . . ? C94 C93 C97 119.7(5) . . ? C92 C93 C97 119.2(6) . . ? C93 C94 C95 118.7(5) . . ? C93 C94 H94 120.6 . . ? C95 C94 H94 120.6 . . ? C94 C95 C96 119.9(5) . . ? C94 C95 C98 122.9(5) . . ? C96 C95 C98 117.2(6) . . ? C95 C96 C91 122.9(5) . . ? C95 C96 H96 118.5 . . ? C91 C96 H96 118.5 . . ? F23 C97 F22 111.5(8) . . ? F23 C97 F24 101.4(7) . . ? F22 C97 F24 103.5(7) . . ? F23 C97 C93 114.1(5) . . ? F22 C97 C93 113.1(5) . . ? F24 C97 C93 112.1(7) . . ? F19 C98 F21 108.1(7) . . ? F19 C98 F20 106.4(6) . . ? F21 C98 F20 105.8(5) . . ? F19 C98 C95 112.8(5) . . ? F21 C98 C95 111.6(6) . . ? F20 C98 C95 111.9(7) . . ? C35 N1 C31 119.2(4) . . ? C35 N1 Mo1 124.3(4) . . ? C31 N1 Mo1 116.4(3) . . ? C55 N2 C51 118.7(4) . . ? C55 N2 Mo1 127.1(3) . . ? C51 N2 Mo1 114.2(3) . . ? C45 N3 C41 118.0(5) . . ? C6 N4 C15 121.1(4) . . ? C6 N4 C7 122.2(5) . . ? C15 N4 C7 115.4(5) . . ? C6 N5 C16 121.1(5) . . ? C6 N5 C9 121.9(5) . . ? C16 N5 C9 117.0(5) . . ? C5 O1 Mo1 106.4(2) . . ? C5 O1 H1 106(5) . . ? Mo1 O1 H1 107(5) . . ? C20 Mo1 C10 80.6(2) . . ? C20 Mo1 N1 95.5(2) . . ? C10 Mo1 N1 87.7(2) . . ? C20 Mo1 O1 166.74(19) . . ? C10 Mo1 O1 103.04(19) . . ? N1 Mo1 O1 72.09(13) . . ? C20 Mo1 C2 103.4(2) . . ? C10 Mo1 C2 104.0(2) . . ? N1 Mo1 C2 159.03(18) . . ? O1 Mo1 C2 88.20(16) . . ? C20 Mo1 N2 101.29(19) . . ? C10 Mo1 N2 166.0(2) . . ? N1 Mo1 N2 78.28(14) . . ? O1 Mo1 N2 72.11(12) . . ? C2 Mo1 N2 89.10(18) . . ? C20 Mo1 C3 109.4(2) . . ? C10 Mo1 C3 70.1(3) . . ? N1 Mo1 C3 142.57(19) . . ? O1 Mo1 C3 83.72(18) . . ? C2 Mo1 C3 36.4(2) . . ? N2 Mo1 C3 121.3(2) . . ? C20 Mo1 C1 69.3(2) . . ? C10 Mo1 C1 106.8(2) . . ? N1 Mo1 C1 156.25(19) . . ? O1 Mo1 C1 120.65(17) . . ? C2 Mo1 C1 35.4(2) . . ? N2 Mo1 C1 86.67(18) . . ? C3 Mo1 C1 61.2(2) . . ? C91 B1 C61 115.5(4) . . ? C91 B1 C71 104.1(3) . . ? C61 B1 C71 112.3(4) . . ? C91 B1 C81 111.0(4) . . ? C61 B1 C81 102.1(3) . . ? C71 B1 C81 112.2(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.635 _refine_diff_density_min -1.019 _refine_diff_density_rms 0.194 #===END data_1H_py_(mp181) _database_code_depnum_ccdc_archive 'CCDC 786112' #TrackingRef 'CIFS.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H12 B F24, C22 H19 Mo N3 O3, C5 H6 N' _chemical_formula_sum 'C59 H37 B F24 Mo N4 O3' _chemical_formula_weight 1412.68 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' C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 '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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8482(3) _cell_length_b 12.9690(3) _cell_length_c 18.5662(5) _cell_angle_alpha 98.097(2) _cell_angle_beta 108.331(2) _cell_angle_gamma 90.332(2) _cell_volume 2903.26(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14334 _cell_measurement_theta_min 3.4443 _cell_measurement_theta_max 73.9580 _exptl_crystal_description blocks _exptl_crystal_colour orange _exptl_crystal_size_max 0.0637 _exptl_crystal_size_mid 0.0524 _exptl_crystal_size_min 0.0154 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1412 _exptl_absorpt_coefficient_mu 2.998 _exptl_absorpt_correction_T_min 0.830 _exptl_absorpt_correction_T_max 0.950 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Onyx, Nova' _diffrn_detector_area_resol_mean 8.2640 _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27147 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0288 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 74.12 _reflns_number_total 11177 _reflns_number_gt 9766 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [1.00000+-1.00000exp(-22.20(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+3.6498*P+(0.1033P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11177 _refine_ls_number_parameters 832 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1606 _refine_ls_wR_factor_gt 0.1556 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.16109(2) 0.96781(2) 0.864127(15) 0.02937(11) Uani 1 1 d . . . F17 F 0.8500(2) 1.4788(2) 0.65118(17) 0.0556(7) Uani 1 1 d . . . F5 F 0.05648(17) 1.62661(19) 0.72916(13) 0.0423(5) Uani 1 1 d . . . F4 F 0.0698(2) 1.4972(2) 0.79157(15) 0.0511(6) Uani 1 1 d . . . F20 F 0.50682(18) 1.21177(14) 0.94951(13) 0.0366(5) Uani 1 1 d . . . F6 F 0.18758(17) 1.62747(19) 0.83460(12) 0.0406(5) Uani 1 1 d . . . F23 F 0.8274(2) 1.6047(2) 1.0698(2) 0.0773(10) Uani 1 1 d . . . F19 F 0.40602(19) 1.33245(18) 0.97539(16) 0.0480(6) Uani 1 1 d . . . O1 O 0.05450(18) 1.02231(17) 0.76308(13) 0.0283(5) Uani 1 1 d . . . F21 F 0.5612(2) 1.31012(19) 1.05901(12) 0.0470(6) Uani 1 1 d . . . F12 F 0.71312(19) 1.90362(19) 0.86432(16) 0.0508(6) Uani 1 1 d . . . F11 F 0.5824(2) 1.85807(16) 0.90418(13) 0.0467(6) Uani 1 1 d . . . F7 F 0.4942(3) 1.65731(18) 0.51325(12) 0.0534(7) Uani 1 1 d . . . F16 F 0.7921(3) 1.3648(3) 0.55193(17) 0.0802(11) Uani 1 1 d . . . F10 F 0.5547(2) 1.96484(15) 0.82329(13) 0.0414(5) Uani 1 1 d . . . F22 F 0.90218(19) 1.4738(2) 1.03330(17) 0.0580(7) Uani 1 1 d . . . N2 N 0.1857(2) 0.8677(2) 0.76073(16) 0.0265(5) Uani 1 1 d . . . F14 F 0.4855(3) 1.0766(2) 0.57431(17) 0.0819(12) Uani 1 1 d . . . F13 F 0.5128(4) 1.07736(19) 0.6930(2) 0.0805(12) Uani 1 1 d . . . F1 F 0.2156(3) 1.3420(3) 0.48977(18) 0.0868(12) Uani 1 1 d . . . N4 N -0.0791(3) 1.1402(2) 0.80309(18) 0.0329(6) Uani 1 1 d D . . C51 C 0.1022(3) 0.8707(2) 0.69547(18) 0.0247(6) Uani 1 1 d . . . F9 F 0.6034(2) 1.7928(3) 0.55897(15) 0.0617(8) Uani 1 1 d . . . N1 N 0.0098(2) 0.8628(2) 0.82029(16) 0.0282(5) Uani 1 1 d . . . F24 F 0.8758(3) 1.5942(5) 0.9668(2) 0.142(3) Uani 1 1 d . . . C80 C 0.5733(3) 1.3967(2) 0.70491(17) 0.0227(6) Uani 1 1 d . . . C71 C 0.5216(2) 1.6218(2) 0.66054(17) 0.0219(6) Uani 1 1 d . . . H71 H 0.5044 1.5665 0.6202 0.026 Uiso 1 1 calc R . . F15 F 0.6373(3) 1.03780(19) 0.6460(3) 0.0832(11) Uani 1 1 d . . . C85 C 0.6644(3) 1.4223(2) 0.68394(18) 0.0254(6) Uani 1 1 d . . . H85 H 0.6891 1.4919 0.6924 0.030 Uiso 1 1 calc R . . C81 C 0.5418(3) 1.2897(2) 0.69152(17) 0.0256(6) Uani 1 1 d . . . H81 H 0.4822 1.2685 0.7051 0.031 Uiso 1 1 calc R . . F8 F 0.4331(2) 1.8045(2) 0.54186(14) 0.0591(7) Uani 1 1 d . . . C60 C 0.3784(3) 1.4659(2) 0.71616(18) 0.0239(6) Uani 1 1 d . . . O10 O 0.2630(3) 0.8389(3) 0.99665(18) 0.0591(8) Uani 1 1 d . . . C90 C 0.5641(2) 1.4675(2) 0.83986(17) 0.0201(5) Uani 1 1 d . . . C73 C 0.5589(3) 1.8071(2) 0.70366(18) 0.0256(6) Uani 1 1 d . . . H73 H 0.5674 1.8743 0.6935 0.031 Uiso 1 1 calc R . . C61 C 0.3231(3) 1.4196(2) 0.64072(19) 0.0281(6) Uani 1 1 d . . . H61 H 0.3632 1.3876 0.6108 0.034 Uiso 1 1 calc R . . C95 C 0.6691(3) 1.5112(2) 0.88431(18) 0.0236(6) Uani 1 1 d . . . H95 H 0.7064 1.5529 0.8625 0.028 Uiso 1 1 calc R . . C72 C 0.5325(3) 1.7221(2) 0.64495(18) 0.0249(6) Uani 1 1 d . . . C92 C 0.5660(3) 1.3842(2) 0.95044(18) 0.0231(6) Uani 1 1 d . . . C82 C 0.5969(3) 1.2151(2) 0.65865(18) 0.0292(7) Uani 1 1 d . . . C64 C 0.1982(3) 1.5134(3) 0.72611(19) 0.0280(6) Uani 1 1 d . . . F18 F 0.9048(3) 1.3253(3) 0.6553(3) 0.0800(10) Uani 1 1 d . . . C63 C 0.1455(3) 1.4670(3) 0.6514(2) 0.0337(7) Uani 1 1 d . . . H63 H 0.0697 1.4673 0.6301 0.040 Uiso 1 1 calc R . . C31 C -0.0487(3) 0.8612(2) 0.74559(19) 0.0268(6) Uani 1 1 d . . . C91 C 0.5145(2) 1.4034(2) 0.87577(17) 0.0215(6) Uani 1 1 d . . . H91 H 0.4450 1.3726 0.8490 0.026 Uiso 1 1 calc R . . C2 C 0.2988(3) 1.0730(3) 0.8633(2) 0.0387(8) Uani 1 1 d . . . C84 C 0.7196(3) 1.3474(3) 0.65087(19) 0.0294(6) Uani 1 1 d . . . O20 O 0.0755(3) 1.0867(3) 0.98954(18) 0.0570(8) Uani 1 1 d . . . C32 C -0.1416(3) 0.7956(3) 0.7104(2) 0.0329(7) Uani 1 1 d . . . H32 H -0.1816 0.7954 0.6591 0.039 Uiso 1 1 calc R . . C1 C 0.3503(3) 0.9991(3) 0.9101(2) 0.0414(9) Uani 1 1 d . . . H1A H 0.3826 1.0239 0.9645 0.050 Uiso 1 1 calc R . . H1B H 0.3937 0.9493 0.8896 0.050 Uiso 1 1 calc R . . C70 C 0.5358(2) 1.6008(2) 0.73517(17) 0.0200(5) Uani 1 1 d . . . C55 C 0.2691(3) 0.8071(3) 0.7574(2) 0.0298(7) Uani 1 1 d . . . H55 H 0.3264 0.8033 0.8022 0.036 Uiso 1 1 calc R . . C65 C 0.3124(3) 1.5121(2) 0.75799(18) 0.0241(6) Uani 1 1 d . . . H65 H 0.3457 1.5429 0.8086 0.029 Uiso 1 1 calc R . . C41 C -0.0647(3) 0.9707(3) 0.6341(2) 0.0325(7) Uani 1 1 d . . . C93 C 0.6684(3) 1.4301(2) 0.99333(18) 0.0264(6) Uani 1 1 d . . . H93 H 0.7021 1.4181 1.0434 0.032 Uiso 1 1 calc R . . C5 C 0.0062(3) 0.9338(2) 0.70748(19) 0.0272(6) Uani 1 1 d . . . C67 C 0.1295(3) 1.5654(3) 0.7709(2) 0.0339(7) Uani 1 1 d . . . C77 C 0.6053(3) 1.8777(2) 0.84214(19) 0.0292(7) Uani 1 1 d . . . C96 C 0.5107(3) 1.3105(3) 0.98373(19) 0.0291(7) Uani 1 1 d . . . C35 C -0.0231(3) 0.8003(3) 0.8613(2) 0.0347(7) Uani 1 1 d . . . H35 H 0.0168 0.8025 0.9129 0.042 Uiso 1 1 calc R . . C75 C 0.5601(2) 1.6877(2) 0.79287(17) 0.0209(5) Uani 1 1 d . . . H75 H 0.5686 1.6779 0.8430 0.025 Uiso 1 1 calc R . . C33 C -0.1736(3) 0.7300(3) 0.7537(3) 0.0400(8) Uani 1 1 d . . . H33 H -0.2351 0.6846 0.7311 0.048 Uiso 1 1 calc R . . C20 C 0.1062(3) 1.0434(3) 0.9432(2) 0.0424(9) Uani 1 1 d . . . C100 C -0.1636(3) 1.0972(3) 0.8164(2) 0.0389(8) Uani 1 1 d . . . H100 H -0.1743 1.0249 0.8071 0.047 Uiso 1 1 calc R . . C101 C -0.2361(3) 1.1554(3) 0.8435(2) 0.0401(8) Uani 1 1 d . . . H101 H -0.2952 1.1238 0.8524 0.048 Uiso 1 1 calc R . . C10 C 0.2280(3) 0.8881(3) 0.9473(2) 0.0412(9) Uani 1 1 d . . . C74 C 0.5720(3) 1.7885(2) 0.77745(18) 0.0238(6) Uani 1 1 d . . . C86 C 0.5569(4) 1.1030(3) 0.6431(2) 0.0373(8) Uani 1 1 d . . . C104 C -0.0619(3) 1.2443(3) 0.8161(2) 0.0391(8) Uani 1 1 d . . . H104 H -0.0025 1.2740 0.8064 0.047 Uiso 1 1 calc R . . C76 C 0.5160(3) 1.7428(3) 0.56488(19) 0.0316(7) Uani 1 1 d . . . C83 C 0.6865(3) 1.2426(3) 0.63784(19) 0.0310(7) Uani 1 1 d . . . H83 H 0.7234 1.1924 0.6158 0.037 Uiso 1 1 calc R . . C52 C 0.0995(3) 0.8140(3) 0.62600(19) 0.0289(6) Uani 1 1 d . . . H52 H 0.0402 0.8164 0.5820 0.035 Uiso 1 1 calc R . . C62 C 0.2086(3) 1.4202(3) 0.6093(2) 0.0347(7) Uani 1 1 d . . . C3 C 0.2309(3) 1.1380(3) 0.8953(3) 0.0466(10) Uani 1 1 d . . . H3A H 0.1900 1.1876 0.8643 0.056 Uiso 1 1 calc R . . H3B H 0.2606 1.1653 0.9495 0.056 Uiso 1 1 calc R . . C97 C 0.8298(3) 1.5446(3) 1.0056(2) 0.0403(8) Uani 1 1 d . . . C103 C -0.1300(4) 1.3074(3) 0.8433(3) 0.0425(9) Uani 1 1 d . . . H103 H -0.1173 1.3794 0.8523 0.051 Uiso 1 1 calc R . . C102 C -0.2184(3) 1.2623(3) 0.8572(2) 0.0389(8) Uani 1 1 d . . . H102 H -0.2656 1.3041 0.8758 0.047 Uiso 1 1 calc R . . F2 F 0.0979(5) 1.2810(5) 0.5309(3) 0.146(3) Uani 1 1 d . . . C34 C -0.1147(3) 0.7324(3) 0.8292(2) 0.0396(8) Uani 1 1 d . . . H34 H -0.1358 0.6891 0.8586 0.047 Uiso 1 1 calc R . . C53 C 0.1878(3) 0.7531(3) 0.6232(2) 0.0328(7) Uani 1 1 d . . . H53 H 0.1889 0.7151 0.5771 0.039 Uiso 1 1 calc R . . B1 B 0.5125(3) 1.4821(2) 0.74956(19) 0.0206(6) Uani 1 1 d . . . C87 C 0.8145(3) 1.3793(3) 0.6268(2) 0.0416(9) Uani 1 1 d . . . C54 C 0.2726(3) 0.7501(3) 0.6892(2) 0.0303(7) Uani 1 1 d . . . H54 H 0.3322 0.7102 0.6885 0.036 Uiso 1 1 calc R . . C94 C 0.7191(3) 1.4945(2) 0.95950(19) 0.0273(6) Uani 1 1 d . . . C66 C 0.1523(3) 1.3675(4) 0.5294(3) 0.0509(10) Uani 1 1 d . . . C44 C -0.1859(4) 1.0375(4) 0.5030(3) 0.0535(11) Uani 1 1 d . . . H44 H -0.2318 1.0595 0.4589 0.064 Uiso 1 1 calc R . . F3 F 0.0750(4) 1.4202(5) 0.4893(2) 0.124(2) Uani 1 1 d . . . C42 C -0.1420(4) 0.9081(4) 0.5864(3) 0.0581(13) Uani 1 1 d . . . H42 H -0.1549 0.8421 0.5969 0.070 Uiso 1 1 calc R . . C4 C 0.3123(4) 1.0830(3) 0.7872(3) 0.0465(9) Uani 1 1 d . . . H4A H 0.2694 1.1383 0.7660 0.070 Uiso 1 1 calc R . . H4B H 0.2878 1.0187 0.7529 0.070 Uiso 1 1 calc R . . H4C H 0.3883 1.0983 0.7940 0.070 Uiso 1 1 calc R . . C45 C -0.1024(5) 1.0981(4) 0.5498(3) 0.0599(12) Uani 1 1 d . . . H45 H -0.0863 1.1619 0.5372 0.072 Uiso 1 1 calc R . . N3 N -0.0384(5) 1.0671(4) 0.6179(3) 0.0731(13) Uani 1 1 d . . . C43 C -0.2039(6) 0.9406(6) 0.5209(4) 0.088(2) Uani 1 1 d . . . H43 H -0.2605 0.8961 0.4868 0.106 Uiso 1 1 calc R . . H1 H -0.034(6) 1.108(6) 0.781(5) 0.106 Uiso 1 1 d 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 Mo1 0.02317(15) 0.03443(17) 0.02887(16) -0.00554(10) 0.01039(10) 0.00146(11) F17 0.0482(14) 0.0501(14) 0.0763(18) -0.0120(12) 0.0405(13) -0.0131(11) F5 0.0282(10) 0.0595(14) 0.0417(12) 0.0151(10) 0.0109(9) 0.0184(10) F4 0.0436(13) 0.0650(15) 0.0570(14) 0.0197(12) 0.0289(11) -0.0008(12) F20 0.0420(11) 0.0211(9) 0.0504(12) 0.0085(8) 0.0189(9) -0.0001(8) F6 0.0286(10) 0.0563(13) 0.0345(11) 0.0021(9) 0.0084(8) 0.0128(9) F23 0.0420(14) 0.0644(17) 0.089(2) -0.0342(16) -0.0110(14) 0.0026(13) F19 0.0366(12) 0.0432(12) 0.0846(18) 0.0279(12) 0.0399(12) 0.0099(10) O1 0.0258(11) 0.0249(10) 0.0336(12) -0.0038(9) 0.0123(9) 0.0008(9) F21 0.0602(14) 0.0527(13) 0.0315(11) 0.0117(9) 0.0173(10) -0.0154(11) F12 0.0317(11) 0.0423(12) 0.0661(16) -0.0173(11) 0.0093(11) -0.0063(10) F11 0.0816(17) 0.0269(10) 0.0344(11) -0.0031(8) 0.0257(11) -0.0076(11) F7 0.092(2) 0.0414(12) 0.0265(10) 0.0056(9) 0.0182(12) 0.0034(12) F16 0.087(2) 0.109(3) 0.0513(16) -0.0189(16) 0.0456(16) -0.043(2) F10 0.0574(14) 0.0203(9) 0.0463(12) 0.0025(8) 0.0173(10) 0.0097(9) F22 0.0258(11) 0.0755(17) 0.0644(16) 0.0098(13) 0.0027(11) 0.0094(11) N2 0.0243(13) 0.0268(13) 0.0297(13) -0.0006(10) 0.0124(11) 0.0022(11) F14 0.127(3) 0.0370(13) 0.0529(16) 0.0087(11) -0.0122(17) -0.0348(16) F13 0.160(4) 0.0250(11) 0.085(2) 0.0035(12) 0.083(2) -0.0122(16) F1 0.0517(16) 0.137(3) 0.0467(16) -0.0395(18) 0.0031(13) 0.0074(18) N4 0.0322(15) 0.0288(14) 0.0378(15) -0.0002(11) 0.0134(12) 0.0075(12) C51 0.0226(14) 0.0245(14) 0.0281(15) 0.0016(11) 0.0107(12) 0.0010(12) F9 0.0596(16) 0.092(2) 0.0405(13) 0.0254(13) 0.0191(12) -0.0212(15) N1 0.0237(13) 0.0308(13) 0.0316(14) 0.0006(10) 0.0129(11) 0.0039(11) F24 0.076(2) 0.229(5) 0.092(3) 0.110(3) -0.049(2) -0.109(3) C80 0.0259(14) 0.0181(13) 0.0236(14) 0.0023(10) 0.0075(11) 0.0017(11) C71 0.0198(13) 0.0210(13) 0.0251(14) 0.0030(10) 0.0076(11) 0.0016(11) F15 0.087(2) 0.0236(12) 0.144(3) 0.0098(15) 0.045(2) 0.0142(13) C85 0.0255(15) 0.0220(14) 0.0283(15) 0.0011(11) 0.0094(12) 0.0022(12) C81 0.0332(16) 0.0181(13) 0.0260(14) 0.0035(11) 0.0102(12) -0.0002(12) F8 0.0719(17) 0.0726(17) 0.0371(12) 0.0268(12) 0.0151(12) 0.0394(14) C60 0.0229(14) 0.0202(13) 0.0285(15) 0.0077(11) 0.0062(12) 0.0003(11) O10 0.0481(17) 0.089(2) 0.0413(16) 0.0198(16) 0.0113(14) 0.0176(17) C90 0.0197(13) 0.0154(12) 0.0274(14) 0.0021(10) 0.0109(11) 0.0038(10) C73 0.0271(15) 0.0200(13) 0.0316(16) 0.0084(11) 0.0102(12) 0.0010(12) C61 0.0252(15) 0.0269(15) 0.0298(16) 0.0019(12) 0.0066(12) -0.0014(12) C95 0.0225(14) 0.0210(13) 0.0292(15) 0.0055(11) 0.0104(12) 0.0004(11) C72 0.0245(14) 0.0254(14) 0.0266(15) 0.0073(11) 0.0093(12) 0.0034(12) C92 0.0252(14) 0.0175(13) 0.0311(15) 0.0036(11) 0.0155(12) 0.0039(11) C82 0.0452(19) 0.0192(14) 0.0236(14) 0.0043(11) 0.0109(13) 0.0055(13) C64 0.0224(15) 0.0295(15) 0.0332(16) 0.0088(12) 0.0087(12) 0.0023(12) F18 0.0528(17) 0.075(2) 0.136(3) 0.030(2) 0.057(2) 0.0246(15) C63 0.0218(15) 0.0344(17) 0.0409(19) 0.0069(14) 0.0039(13) -0.0018(13) C31 0.0230(14) 0.0249(14) 0.0347(16) -0.0001(12) 0.0141(13) 0.0050(12) C91 0.0196(13) 0.0165(12) 0.0298(15) 0.0023(10) 0.0102(11) 0.0021(11) C2 0.0279(17) 0.0387(19) 0.046(2) -0.0105(15) 0.0151(15) -0.0102(15) C84 0.0311(16) 0.0280(15) 0.0308(16) 0.0004(12) 0.0140(13) 0.0051(13) O20 0.0505(17) 0.073(2) 0.0462(17) -0.0200(15) 0.0265(14) 0.0041(15) C32 0.0249(16) 0.0339(17) 0.0392(18) 0.0049(14) 0.0095(14) 0.0012(14) C1 0.0251(17) 0.054(2) 0.0391(19) -0.0095(16) 0.0083(14) -0.0027(16) C70 0.0176(13) 0.0183(13) 0.0249(14) 0.0026(10) 0.0084(11) 0.0015(10) C55 0.0233(15) 0.0322(16) 0.0345(17) 0.0019(13) 0.0113(13) 0.0033(13) C65 0.0211(14) 0.0242(14) 0.0262(14) 0.0051(11) 0.0061(11) 0.0008(11) C41 0.0321(17) 0.0314(16) 0.0354(17) 0.0031(13) 0.0135(14) 0.0079(14) C93 0.0268(15) 0.0262(14) 0.0269(15) 0.0068(11) 0.0084(12) 0.0049(12) C5 0.0260(15) 0.0239(14) 0.0314(16) -0.0015(12) 0.0110(12) 0.0030(12) C67 0.0223(15) 0.0446(19) 0.0389(18) 0.0163(15) 0.0113(14) 0.0064(14) C77 0.0343(17) 0.0195(14) 0.0341(17) 0.0043(12) 0.0114(13) 0.0000(13) C96 0.0312(16) 0.0264(15) 0.0339(17) 0.0074(12) 0.0153(13) 0.0023(13) C35 0.0304(17) 0.0427(19) 0.0374(18) 0.0074(14) 0.0191(14) 0.0061(15) C75 0.0200(13) 0.0191(13) 0.0252(14) 0.0043(10) 0.0090(11) 0.0014(11) C33 0.0271(17) 0.0359(18) 0.060(2) 0.0088(16) 0.0171(16) -0.0010(15) C20 0.0315(18) 0.055(2) 0.0379(19) -0.0054(17) 0.0130(15) 0.0014(17) C100 0.040(2) 0.0286(16) 0.051(2) 0.0043(15) 0.0188(17) 0.0026(15) C101 0.0366(19) 0.0383(19) 0.050(2) 0.0051(16) 0.0210(17) 0.0069(16) C10 0.0309(18) 0.058(2) 0.0344(19) 0.0008(17) 0.0124(15) 0.0087(17) C74 0.0233(14) 0.0178(13) 0.0316(15) 0.0030(11) 0.0111(12) 0.0008(11) C86 0.061(2) 0.0186(14) 0.0335(17) 0.0042(12) 0.0169(16) 0.0059(15) C104 0.0375(19) 0.0292(17) 0.052(2) 0.0021(15) 0.0181(17) 0.0019(15) C76 0.0370(18) 0.0298(16) 0.0300(16) 0.0094(13) 0.0116(14) 0.0027(14) C83 0.0431(19) 0.0258(15) 0.0257(15) 0.0012(12) 0.0141(14) 0.0103(14) C52 0.0312(16) 0.0289(15) 0.0268(15) 0.0019(12) 0.0105(13) -0.0001(13) C62 0.0267(16) 0.0360(17) 0.0354(18) 0.0020(14) 0.0028(14) -0.0023(14) C3 0.0355(19) 0.042(2) 0.054(2) -0.0161(17) 0.0131(17) -0.0078(17) C97 0.0306(18) 0.046(2) 0.0398(19) 0.0128(16) 0.0023(15) -0.0071(16) C103 0.046(2) 0.0244(16) 0.056(2) -0.0004(15) 0.0167(18) 0.0083(15) C102 0.040(2) 0.0352(18) 0.043(2) 0.0028(15) 0.0173(16) 0.0133(16) F2 0.171(5) 0.164(5) 0.072(3) -0.045(3) 0.023(3) -0.123(4) C34 0.0363(19) 0.0416(19) 0.053(2) 0.0169(16) 0.0266(17) 0.0066(16) C53 0.0409(19) 0.0287(16) 0.0327(17) -0.0008(13) 0.0194(14) 0.0014(14) B1 0.0195(15) 0.0166(14) 0.0263(16) 0.0020(11) 0.0087(12) 0.0006(12) C87 0.042(2) 0.0396(19) 0.051(2) -0.0010(16) 0.0292(18) 0.0051(17) C54 0.0299(16) 0.0257(15) 0.0412(18) 0.0027(13) 0.0206(14) 0.0060(13) C94 0.0235(15) 0.0275(15) 0.0299(16) 0.0067(12) 0.0060(12) 0.0021(12) C66 0.033(2) 0.062(3) 0.046(2) -0.0082(19) 0.0016(17) -0.0047(19) C44 0.054(3) 0.064(3) 0.050(2) 0.026(2) 0.019(2) 0.019(2) F3 0.092(3) 0.192(5) 0.0449(17) -0.023(2) -0.0230(18) 0.083(3) C42 0.051(3) 0.060(3) 0.051(2) 0.030(2) -0.011(2) -0.019(2) C4 0.038(2) 0.046(2) 0.055(2) 0.0002(18) 0.0182(18) -0.0089(18) C45 0.085(4) 0.048(2) 0.052(3) 0.020(2) 0.025(3) 0.010(2) N3 0.078(3) 0.073(3) 0.070(3) 0.029(2) 0.017(2) -0.006(3) C43 0.069(4) 0.106(5) 0.070(4) 0.045(3) -0.018(3) -0.035(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; 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 Mo1 C10 1.954(4) . ? Mo1 C20 1.967(4) . ? Mo1 O1 2.159(2) . ? Mo1 N1 2.227(3) . ? Mo1 C2 2.232(4) . ? Mo1 N2 2.271(3) . ? Mo1 C3 2.302(4) . ? Mo1 C1 2.321(4) . ? F17 C87 1.332(5) . ? F5 C67 1.355(4) . ? F4 C67 1.338(4) . ? F20 C96 1.340(4) . ? F6 C67 1.331(4) . ? F23 C97 1.338(5) . ? F19 C96 1.341(4) . ? O1 C5 1.422(4) . ? F21 C96 1.344(4) . ? F12 C77 1.341(4) . ? F11 C77 1.331(4) . ? F7 C76 1.324(4) . ? F16 C87 1.313(5) . ? F10 C77 1.342(4) . ? F22 C97 1.346(5) . ? N2 C55 1.344(4) . ? N2 C51 1.348(4) . ? F14 C86 1.313(5) . ? F13 C86 1.307(5) . ? F1 C66 1.274(6) . ? N4 C100 1.324(5) . ? N4 C104 1.342(5) . ? N4 H1 0.89(8) . ? C51 C52 1.382(4) . ? C51 C5 1.541(4) . ? F9 C76 1.335(5) . ? N1 C35 1.337(5) . ? N1 C31 1.351(4) . ? F24 C97 1.295(5) . ? C80 C85 1.397(4) . ? C80 C81 1.409(4) . ? C80 B1 1.637(4) . ? C71 C72 1.388(4) . ? C71 C70 1.406(4) . ? C71 H71 0.9300 . ? F15 C86 1.331(5) . ? C85 C84 1.393(4) . ? C85 H85 0.9300 . ? C81 C82 1.387(5) . ? C81 H81 0.9300 . ? F8 C76 1.333(4) . ? C60 C61 1.400(4) . ? C60 C65 1.403(4) . ? C60 B1 1.639(4) . ? O10 C10 1.165(5) . ? C90 C91 1.399(4) . ? C90 C95 1.408(4) . ? C90 B1 1.636(4) . ? C73 C74 1.383(4) . ? C73 C72 1.394(4) . ? C73 H73 0.9300 . ? C61 C62 1.402(5) . ? C61 H61 0.9300 . ? C95 C94 1.390(4) . ? C95 H95 0.9300 . ? C72 C76 1.497(4) . ? C92 C93 1.385(5) . ? C92 C91 1.394(4) . ? C92 C96 1.495(4) . ? C82 C83 1.384(5) . ? C82 C86 1.498(4) . ? C64 C63 1.384(5) . ? C64 C65 1.401(4) . ? C64 C67 1.496(5) . ? F18 C87 1.359(5) . ? C63 C62 1.381(5) . ? C63 H63 0.9300 . ? C31 C32 1.385(5) . ? C31 C5 1.542(5) . ? C91 H91 0.9300 . ? C2 C1 1.411(6) . ? C2 C3 1.420(6) . ? C2 C4 1.500(6) . ? C84 C83 1.385(5) . ? C84 C87 1.499(5) . ? O20 C20 1.136(5) . ? C32 C33 1.390(5) . ? C32 H32 0.9300 . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C70 C75 1.401(4) . ? C70 B1 1.641(4) . ? C55 C54 1.386(5) . ? C55 H55 0.9300 . ? C65 H65 0.9300 . ? C41 C42 1.291(6) . ? C41 N3 1.390(6) . ? C41 C5 1.524(5) . ? C93 C94 1.384(5) . ? C93 H93 0.9300 . ? C77 C74 1.497(4) . ? C35 C34 1.384(6) . ? C35 H35 0.9300 . ? C75 C74 1.395(4) . ? C75 H75 0.9300 . ? C33 C34 1.364(6) . ? C33 H33 0.9300 . ? C100 C101 1.374(5) . ? C100 H100 0.9300 . ? C101 C102 1.378(6) . ? C101 H101 0.9300 . ? C104 C103 1.363(6) . ? C104 H104 0.9300 . ? C83 H83 0.9300 . ? C52 C53 1.397(5) . ? C52 H52 0.9300 . ? C62 C66 1.491(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C97 C94 1.498(5) . ? C103 C102 1.385(6) . ? C103 H103 0.9300 . ? C102 H102 0.9300 . ? F2 C66 1.327(7) . ? C34 H34 0.9300 . ? C53 C54 1.365(5) . ? C53 H53 0.9300 . ? C54 H54 0.9300 . ? C66 F3 1.301(6) . ? C44 C45 1.318(8) . ? C44 C43 1.381(8) . ? C44 H44 0.9300 . ? C42 C43 1.352(7) . ? C42 H42 0.9300 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C45 N3 1.388(7) . ? C45 H45 0.9300 . ? C43 H43 0.9300 . ? 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 C10 Mo1 C20 81.25(17) . . ? C10 Mo1 O1 164.79(14) . . ? C20 Mo1 O1 100.25(14) . . ? C10 Mo1 N1 92.42(15) . . ? C20 Mo1 N1 90.54(14) . . ? O1 Mo1 N1 72.47(10) . . ? C10 Mo1 C2 104.09(17) . . ? C20 Mo1 C2 103.67(16) . . ? O1 Mo1 C2 90.34(13) . . ? N1 Mo1 C2 159.55(13) . . ? C10 Mo1 N2 102.68(13) . . ? C20 Mo1 N2 167.49(14) . . ? O1 Mo1 N2 72.84(9) . . ? N1 Mo1 N2 77.51(10) . . ? C2 Mo1 N2 87.02(12) . . ? C10 Mo1 C3 110.96(18) . . ? C20 Mo1 C3 69.83(17) . . ? O1 Mo1 C3 83.50(14) . . ? N1 Mo1 C3 145.81(13) . . ? C2 Mo1 C3 36.46(14) . . ? N2 Mo1 C3 118.62(13) . . ? C10 Mo1 C1 68.99(16) . . ? C20 Mo1 C1 105.40(15) . . ? O1 Mo1 C1 124.32(13) . . ? N1 Mo1 C1 152.74(13) . . ? C2 Mo1 C1 36.03(16) . . ? N2 Mo1 C1 87.06(12) . . ? C3 Mo1 C1 61.44(16) . . ? C5 O1 Mo1 108.16(18) . . ? C55 N2 C51 118.2(3) . . ? C55 N2 Mo1 128.9(2) . . ? C51 N2 Mo1 112.9(2) . . ? C100 N4 C104 120.0(3) . . ? C100 N4 H1 127(6) . . ? C104 N4 H1 113(6) . . ? N2 C51 C52 122.5(3) . . ? N2 C51 C5 113.7(3) . . ? C52 C51 C5 123.6(3) . . ? C35 N1 C31 119.4(3) . . ? C35 N1 Mo1 124.9(2) . . ? C31 N1 Mo1 115.6(2) . . ? C85 C80 C81 115.6(3) . . ? C85 C80 B1 123.3(3) . . ? C81 C80 B1 120.9(3) . . ? C72 C71 C70 122.2(3) . . ? C72 C71 H71 118.9 . . ? C70 C71 H71 118.9 . . ? C84 C85 C80 122.3(3) . . ? C84 C85 H85 118.8 . . ? C80 C85 H85 118.8 . . ? C82 C81 C80 122.0(3) . . ? C82 C81 H81 119.0 . . ? C80 C81 H81 119.0 . . ? C61 C60 C65 116.0(3) . . ? C61 C60 B1 122.1(3) . . ? C65 C60 B1 121.1(3) . . ? C91 C90 C95 115.5(3) . . ? C91 C90 B1 123.6(3) . . ? C95 C90 B1 120.6(2) . . ? C74 C73 C72 118.0(3) . . ? C74 C73 H73 121.0 . . ? C72 C73 H73 121.0 . . ? C60 C61 C62 121.5(3) . . ? C60 C61 H61 119.2 . . ? C62 C61 H61 119.2 . . ? C94 C95 C90 122.4(3) . . ? C94 C95 H95 118.8 . . ? C90 C95 H95 118.8 . . ? C71 C72 C73 120.8(3) . . ? C71 C72 C76 121.3(3) . . ? C73 C72 C76 117.9(3) . . ? C93 C92 C91 121.1(3) . . ? C93 C92 C96 119.7(3) . . ? C91 C92 C96 119.2(3) . . ? C83 C82 C81 121.3(3) . . ? C83 C82 C86 119.2(3) . . ? C81 C82 C86 119.5(3) . . ? C63 C64 C65 120.6(3) . . ? C63 C64 C67 118.0(3) . . ? C65 C64 C67 121.5(3) . . ? C62 C63 C64 118.3(3) . . ? C62 C63 H63 120.9 . . ? C64 C63 H63 120.9 . . ? N1 C31 C32 121.3(3) . . ? N1 C31 C5 111.4(3) . . ? C32 C31 C5 127.2(3) . . ? C92 C91 C90 122.1(3) . . ? C92 C91 H91 118.9 . . ? C90 C91 H91 118.9 . . ? C1 C2 C3 113.1(4) . . ? C1 C2 C4 124.4(4) . . ? C3 C2 C4 122.5(4) . . ? C1 C2 Mo1 75.4(2) . . ? C3 C2 Mo1 74.5(2) . . ? C4 C2 Mo1 117.8(3) . . ? C83 C84 C85 120.9(3) . . ? C83 C84 C87 118.8(3) . . ? C85 C84 C87 120.2(3) . . ? C31 C32 C33 118.5(3) . . ? C31 C32 H32 120.8 . . ? C33 C32 H32 120.8 . . ? C2 C1 Mo1 68.5(2) . . ? C2 C1 H1A 116.8 . . ? Mo1 C1 H1A 116.8 . . ? C2 C1 H1B 116.8 . . ? Mo1 C1 H1B 116.8 . . ? H1A C1 H1B 113.8 . . ? C75 C70 C71 115.8(3) . . ? C75 C70 B1 123.7(3) . . ? C71 C70 B1 120.3(3) . . ? N2 C55 C54 122.2(3) . . ? N2 C55 H55 118.9 . . ? C54 C55 H55 118.9 . . ? C64 C65 C60 122.2(3) . . ? C64 C65 H65 118.9 . . ? C60 C65 H65 118.9 . . ? C42 C41 N3 122.1(4) . . ? C42 C41 C5 118.7(3) . . ? N3 C41 C5 119.0(3) . . ? C94 C93 C92 118.1(3) . . ? C94 C93 H93 121.0 . . ? C92 C93 H93 121.0 . . ? O1 C5 C41 109.0(3) . . ? O1 C5 C51 106.2(2) . . ? C41 C5 C51 112.4(3) . . ? O1 C5 C31 107.7(3) . . ? C41 C5 C31 118.0(3) . . ? C51 C5 C31 102.8(2) . . ? F6 C67 F4 107.1(3) . . ? F6 C67 F5 105.8(3) . . ? F4 C67 F5 105.8(3) . . ? F6 C67 C64 113.6(3) . . ? F4 C67 C64 112.7(3) . . ? F5 C67 C64 111.3(3) . . ? F11 C77 F12 106.9(3) . . ? F11 C77 F10 106.0(3) . . ? F12 C77 F10 105.6(3) . . ? F11 C77 C74 113.0(3) . . ? F12 C77 C74 112.4(3) . . ? F10 C77 C74 112.5(3) . . ? F20 C96 F19 105.6(3) . . ? F20 C96 F21 106.3(3) . . ? F19 C96 F21 106.9(3) . . ? F20 C96 C92 112.1(3) . . ? F19 C96 C92 112.4(3) . . ? F21 C96 C92 113.1(3) . . ? N1 C35 C34 121.9(3) . . ? N1 C35 H35 119.0 . . ? C34 C35 H35 119.0 . . ? C74 C75 C70 122.0(3) . . ? C74 C75 H75 119.0 . . ? C70 C75 H75 119.0 . . ? C34 C33 C32 120.0(3) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? O20 C20 Mo1 179.2(4) . . ? N4 C100 C101 122.3(3) . . ? N4 C100 H100 118.8 . . ? C101 C100 H100 118.8 . . ? C100 C101 C102 117.8(4) . . ? C100 C101 H101 121.1 . . ? C102 C101 H101 121.1 . . ? O10 C10 Mo1 176.8(4) . . ? C73 C74 C75 121.1(3) . . ? C73 C74 C77 119.1(3) . . ? C75 C74 C77 119.7(3) . . ? F13 C86 F14 107.9(4) . . ? F13 C86 F15 104.4(3) . . ? F14 C86 F15 104.9(4) . . ? F13 C86 C82 113.3(3) . . ? F14 C86 C82 112.8(3) . . ? F15 C86 C82 112.7(4) . . ? N4 C104 C103 121.1(4) . . ? N4 C104 H104 119.5 . . ? C103 C104 H104 119.5 . . ? F7 C76 F8 106.5(3) . . ? F7 C76 F9 107.1(3) . . ? F8 C76 F9 105.2(3) . . ? F7 C76 C72 113.7(3) . . ? F8 C76 C72 111.6(3) . . ? F9 C76 C72 112.2(3) . . ? C82 C83 C84 117.9(3) . . ? C82 C83 H83 121.1 . . ? C84 C83 H83 121.1 . . ? C51 C52 C53 118.6(3) . . ? C51 C52 H52 120.7 . . ? C53 C52 H52 120.7 . . ? C63 C62 C61 121.4(3) . . ? C63 C62 C66 118.6(3) . . ? C61 C62 C66 120.0(3) . . ? C2 C3 Mo1 69.1(2) . . ? C2 C3 H3A 116.7 . . ? Mo1 C3 H3A 116.7 . . ? C2 C3 H3B 116.7 . . ? Mo1 C3 H3B 116.7 . . ? H3A C3 H3B 113.8 . . ? F24 C97 F23 111.5(4) . . ? F24 C97 F22 104.5(4) . . ? F23 C97 F22 102.3(3) . . ? F24 C97 C94 113.9(3) . . ? F23 C97 C94 111.9(3) . . ? F22 C97 C94 112.0(3) . . ? C104 C103 C102 118.9(3) . . ? C104 C103 H103 120.6 . . ? C102 C103 H103 120.6 . . ? C101 C102 C103 119.9(3) . . ? C101 C102 H102 120.1 . . ? C103 C102 H102 120.1 . . ? C33 C34 C35 118.9(3) . . ? C33 C34 H34 120.6 . . ? C35 C34 H34 120.6 . . ? C54 C53 C52 119.0(3) . . ? C54 C53 H53 120.5 . . ? C52 C53 H53 120.5 . . ? C90 B1 C80 104.2(2) . . ? C90 B1 C60 113.5(2) . . ? C80 B1 C60 112.5(2) . . ? C90 B1 C70 112.3(2) . . ? C80 B1 C70 111.2(2) . . ? C60 B1 C70 103.3(2) . . ? F16 C87 F17 106.5(4) . . ? F16 C87 F18 106.5(4) . . ? F17 C87 F18 103.9(4) . . ? F16 C87 C84 112.6(3) . . ? F17 C87 C84 114.3(3) . . ? F18 C87 C84 112.3(3) . . ? C53 C54 C55 119.5(3) . . ? C53 C54 H54 120.2 . . ? C55 C54 H54 120.2 . . ? C93 C94 C95 120.8(3) . . ? C93 C94 C97 118.3(3) . . ? C95 C94 C97 120.9(3) . . ? F1 C66 F3 107.3(5) . . ? F1 C66 F2 107.1(5) . . ? F3 C66 F2 102.4(5) . . ? F1 C66 C62 115.0(4) . . ? F3 C66 C62 114.1(4) . . ? F2 C66 C62 109.9(4) . . ? C45 C44 C43 118.6(5) . . ? C45 C44 H44 120.7 . . ? C43 C44 H44 120.7 . . ? C41 C42 C43 118.6(4) . . ? C41 C42 H42 120.7 . . ? C43 C42 H42 120.7 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C44 C45 N3 120.2(4) . . ? C44 C45 H45 119.9 . . ? N3 C45 H45 119.9 . . ? C45 N3 C41 118.0(5) . . ? C42 C43 C44 122.2(5) . . ? C42 C43 H43 118.9 . . ? C44 C43 H43 118.9 . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 74.12 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 1.338 _refine_diff_density_min -1.371 _refine_diff_density_rms 0.099 #===END data_1H_TEA_(mp283b) _database_code_depnum_ccdc_archive 'CCDC 786113' #TrackingRef 'CIFS.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H12 B F24, C22 H19 Mo N3 O3, C6 H16 N, O' _chemical_formula_sum 'C60 H47 B F24 Mo N4 O4' _chemical_formula_weight 1450.77 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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.480(5) _cell_length_b 13.029(5) _cell_length_c 21.067(5) _cell_angle_alpha 83.950(5) _cell_angle_beta 73.541(5) _cell_angle_gamma 86.462(5) _cell_volume 3265(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13972 _cell_measurement_theta_min 3.4103 _cell_measurement_theta_max 74.0696 _exptl_crystal_description blocks _exptl_crystal_colour orange _exptl_crystal_size_max 0.1154 _exptl_crystal_size_mid 0.0883 _exptl_crystal_size_min 0.0486 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1460 _exptl_absorpt_coefficient_mu 2.695 _exptl_absorpt_correction_T_min 0.750 _exptl_absorpt_correction_T_max 0.875 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Onyx, Nova' _diffrn_detector_area_resol_mean 8.2640 _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26741 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.4103 _diffrn_reflns_theta_max 74.0696 _reflns_number_total 12702 _reflns_number_gt 10240 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1546P)^2^+4.8791P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12702 _refine_ls_number_parameters 844 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0942 _refine_ls_R_factor_gt 0.0772 _refine_ls_wR_factor_ref 0.2397 _refine_ls_wR_factor_gt 0.2232 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.29923(3) 0.73828(3) 0.922571(19) 0.02763(15) Uani 1 1 d . . . F2 F 0.9281(3) 0.5560(2) 0.93581(14) 0.0397(7) Uani 1 1 d . . . O1 O 0.4231(3) 0.7563(3) 0.82757(16) 0.0331(7) Uiso 1 1 d . . . F1 F 0.7763(2) 0.6047(3) 0.91193(17) 0.0449(7) Uani 1 1 d . . . F3 F 0.8951(3) 0.7176(2) 0.91164(16) 0.0443(7) Uani 1 1 d . . . F6 F 1.0309(3) 0.7781(3) 0.61281(18) 0.0596(10) Uani 1 1 d . . . F22 F 0.5439(3) 0.3875(3) 0.76647(18) 0.0549(9) Uani 1 1 d . . . F24 F 0.5549(4) 0.2474(3) 0.7188(2) 0.0653(11) Uani 1 1 d . . . F19 F 0.9449(4) 0.3992(4) 0.48068(17) 0.0662(11) Uani 1 1 d . . . O20 O 0.1822(4) 0.7051(4) 1.07495(19) 0.0497(10) Uani 1 1 d . . . F13 F 1.1642(4) 0.3452(3) 0.9291(2) 0.0653(11) Uani 1 1 d . . . F23 F 0.6189(4) 0.2496(3) 0.8038(2) 0.0677(11) Uani 1 1 d . . . N3 N 0.4056(3) 0.5921(3) 0.9152(2) 0.0331(8) Uani 1 1 d . . . O10 O 0.1953(4) 0.9579(3) 0.9496(2) 0.0526(10) Uani 1 1 d . . . F21 F 0.7706(4) 0.3753(5) 0.4977(2) 0.0835(15) Uani 1 1 d . . . N1 N 0.4542(4) 0.7899(3) 0.9404(2) 0.0352(9) Uani 1 1 d . . . F20 F 0.8260(4) 0.5224(4) 0.5103(2) 0.0723(12) Uani 1 1 d . . . C31 C 0.5493(4) 0.7753(3) 0.8909(3) 0.0334(10) Uani 1 1 d . . . C51 C 0.5080(4) 0.6051(4) 0.8725(2) 0.0321(10) Uani 1 1 d . . . F14 F 1.1585(10) 0.1883(4) 0.9658(3) 0.167(5) Uani 1 1 d . . . N4 N 0.4308(4) 0.9369(4) 0.7488(2) 0.0396(9) Uani 1 1 d D . . N2 N 0.6926(4) 0.7816(4) 0.7540(3) 0.0502(12) Uani 1 1 d . . . F4 F 1.0737(7) 0.8529(4) 0.6867(2) 0.109(2) Uani 1 1 d . . . F17 F 0.9348(5) -0.0385(4) 0.9006(3) 0.0945(17) Uani 1 1 d . . . F9 F 1.5307(4) 0.4544(7) 0.5623(3) 0.118(3) Uani 1 1 d . . . C52 C 0.5903(4) 0.5272(4) 0.8655(3) 0.0354(10) Uani 1 1 d . . . H52 H 0.6606 0.5376 0.8358 0.042 Uiso 1 1 calc R . . C55 C 0.3832(4) 0.5003(4) 0.9519(3) 0.0365(10) Uani 1 1 d . . . H55 H 0.3125 0.4916 0.9815 0.044 Uiso 1 1 calc R . . F8 F 1.4073(4) 0.5774(6) 0.5853(3) 0.0945(17) Uani 1 1 d . . . F5 F 1.1872(3) 0.7455(4) 0.6298(2) 0.0765(13) Uani 1 1 d . . . C10 C 0.2332(4) 0.8765(5) 0.9379(3) 0.0402(11) Uani 1 1 d . . . C76 C 1.4319(6) 0.4771(11) 0.6044(4) 0.088(3) Uani 1 1 d . . . C66 C 0.8865(4) 0.6226(4) 0.8954(3) 0.0356(10) Uani 1 1 d . . . C20 C 0.2233(4) 0.7177(4) 1.0180(3) 0.0403(11) Uani 1 1 d . . . C5 C 0.5246(4) 0.7156(4) 0.8374(3) 0.0344(10) Uani 1 1 d . . . C53 C 0.5663(5) 0.4332(4) 0.9037(3) 0.0405(11) Uani 1 1 d . . . H53 H 0.6208 0.3804 0.9000 0.049 Uiso 1 1 calc R . . C65 C 1.0420(5) 0.5778(4) 0.6930(3) 0.0397(11) Uani 1 1 d . . . H65 H 1.0734 0.5687 0.6482 0.048 Uiso 1 1 calc R . . C64 C 1.0301(5) 0.6778(4) 0.7129(3) 0.0417(12) Uani 1 1 d . . . C60 C 1.0085(4) 0.4909(4) 0.7378(2) 0.0358(10) Uani 1 1 d . . . C2 C 0.1877(4) 0.6630(4) 0.8763(3) 0.0372(11) Uani 1 1 d . . . C94 C 0.7218(5) 0.3333(4) 0.7014(3) 0.0447(12) Uani 1 1 d . . . C34 C 0.5596(6) 0.8711(4) 0.9984(3) 0.0498(14) Uani 1 1 d . . . H34 H 0.5612 0.9031 1.0355 0.060 Uiso 1 1 calc R . . F18 F 0.9630(13) -0.0338(5) 0.7981(3) 0.227(7) Uani 1 1 d . . . C63 C 0.9800(4) 0.6950(4) 0.7790(3) 0.0381(11) Uani 1 1 d . . . H63 H 0.9717 0.7612 0.7927 0.046 Uiso 1 1 calc R . . F7 F 1.4502(4) 0.4799(7) 0.6639(2) 0.121(3) Uani 1 1 d . . . C81 C 1.0964(6) 0.3013(5) 0.8164(3) 0.0474(14) Uani 1 1 d . . . H81 H 1.1343 0.3624 0.8102 0.057 Uiso 1 1 calc R . . C32 C 0.6517(5) 0.8073(4) 0.8937(3) 0.0433(12) Uani 1 1 d . . . H32 H 0.7163 0.7966 0.8596 0.052 Uiso 1 1 calc R . . C62 C 0.9425(4) 0.6097(4) 0.8237(2) 0.0342(10) Uani 1 1 d . . . C61 C 0.9569(4) 0.5107(4) 0.8034(2) 0.0339(10) Uani 1 1 d . . . H61 H 0.9312 0.4554 0.8347 0.041 Uiso 1 1 calc R . . F15 F 1.2841(6) 0.2400(10) 0.8802(4) 0.202(6) Uani 1 1 d . . . C54 C 0.4605(5) 0.4187(4) 0.9475(3) 0.0419(12) Uani 1 1 d . . . H54 H 0.4423 0.3562 0.9730 0.050 Uiso 1 1 calc R . . C1 C 0.1759(4) 0.7701(4) 0.8586(3) 0.0389(11) Uani 1 1 d . . . H1A H 0.1047 0.8035 0.8792 0.047 Uiso 1 1 calc R . . H1B H 0.2075 0.7943 0.8123 0.047 Uiso 1 1 calc R . . C4 C 0.2437(5) 0.5902(4) 0.8249(3) 0.0431(12) Uani 1 1 d . . . H4A H 0.2443 0.5212 0.8460 0.065 Uiso 1 1 calc R . . H4B H 0.3191 0.6105 0.8039 0.065 Uiso 1 1 calc R . . H4C H 0.2035 0.5925 0.7921 0.065 Uiso 1 1 calc R . . C41 C 0.6121(4) 0.7145(4) 0.7703(3) 0.0387(11) Uani 1 1 d . . . C93 C 0.7315(6) 0.3571(5) 0.6335(3) 0.0482(13) Uani 1 1 d . . . H93 H 0.6704 0.3531 0.6169 0.058 Uiso 1 1 calc R . . C33 C 0.6555(5) 0.8558(4) 0.9489(3) 0.0480(14) Uani 1 1 d . . . H33 H 0.7232 0.8777 0.9521 0.058 Uiso 1 1 calc R . . C42 C 0.5997(5) 0.6463(5) 0.7268(3) 0.0446(12) Uani 1 1 d . . . H42 H 0.5408 0.6012 0.7394 0.054 Uiso 1 1 calc R . . C92 C 0.8333(6) 0.3864(5) 0.5922(3) 0.0479(13) Uani 1 1 d . . . C70 C 1.1480(6) 0.3620(5) 0.6571(3) 0.0497(14) Uani 1 1 d . . . F10 F 1.3598(7) 0.1962(6) 0.4694(3) 0.124(3) Uani 1 1 d . . . C12 C 0.3206(5) 1.0987(5) 0.7226(3) 0.0508(14) Uani 1 1 d . . . H12A H 0.2469 1.1303 0.7337 0.076 Uiso 1 1 calc R . . H12B H 0.3444 1.0896 0.6759 0.076 Uiso 1 1 calc R . . H12C H 0.3715 1.1421 0.7330 0.076 Uiso 1 1 calc R . . F16 F 0.8191(8) 0.0391(5) 0.8578(6) 0.162(4) Uani 1 1 d . . . C15 C 0.4730(5) 0.9059(5) 0.6794(3) 0.0474(13) Uani 1 1 d . . . H15A H 0.5460 0.8720 0.6737 0.057 Uiso 1 1 calc R . . H15B H 0.4817 0.9675 0.6484 0.057 Uiso 1 1 calc R . . C11 C 0.3189(5) 0.9945(4) 0.7622(3) 0.0416(11) Uani 1 1 d . . . H11A H 0.2928 1.0044 0.8092 0.050 Uiso 1 1 calc R . . H11B H 0.2656 0.9521 0.7522 0.050 Uiso 1 1 calc R . . C85 C 0.9807(6) 0.1926(5) 0.7852(3) 0.0473(13) Uani 1 1 d . . . H85 H 0.9395 0.1770 0.7572 0.057 Uiso 1 1 calc R . . C13 C 0.5191(5) 0.9969(4) 0.7633(3) 0.0437(12) Uani 1 1 d . . . H13A H 0.5361 1.0568 0.7311 0.052 Uiso 1 1 calc R . . H13B H 0.5869 0.9541 0.7581 0.052 Uiso 1 1 calc R . . C14 C 0.4831(6) 1.0327(4) 0.8334(3) 0.0492(14) Uani 1 1 d . . . H14A H 0.5421 1.0704 0.8402 0.074 Uiso 1 1 calc R . . H14B H 0.4676 0.9736 0.8655 0.074 Uiso 1 1 calc R . . H14C H 0.4171 1.0765 0.8384 0.074 Uiso 1 1 calc R . . C97 C 0.6113(6) 0.3050(5) 0.7468(3) 0.0505(14) Uani 1 1 d . . . C95 C 0.8154(5) 0.3379(4) 0.7251(3) 0.0413(12) Uani 1 1 d . . . H95 H 0.8073 0.3234 0.7704 0.050 Uiso 1 1 calc R . . C90 C 0.9196(5) 0.3633(4) 0.6834(3) 0.0404(11) Uani 1 1 d . . . C3 C 0.1459(5) 0.6323(5) 0.9450(3) 0.0452(13) Uani 1 1 d . . . H3A H 0.1575 0.5603 0.9593 0.054 Uiso 1 1 calc R . . H3B H 0.0737 0.6616 0.9678 0.054 Uiso 1 1 calc R . . C80 C 1.0313(5) 0.2871(4) 0.7737(2) 0.0433(12) Uani 1 1 d . . . C91 C 0.9261(5) 0.3885(4) 0.6163(3) 0.0436(12) Uani 1 1 d . . . H91 H 0.9944 0.4072 0.5869 0.052 Uiso 1 1 calc R . . C35 C 0.4594(5) 0.8381(4) 0.9924(3) 0.0402(11) Uani 1 1 d . . . H35 H 0.3939 0.8499 1.0256 0.048 Uiso 1 1 calc R . . C96 C 0.8434(6) 0.4208(6) 0.5205(3) 0.0557(16) Uani 1 1 d . . . C71 C 1.2384(5) 0.4212(6) 0.6524(3) 0.0560(17) Uani 1 1 d . . . H71 H 1.2295 0.4727 0.6811 0.067 Uiso 1 1 calc R . . C83 C 1.0528(7) 0.1376(5) 0.8788(3) 0.064(2) Uani 1 1 d . . . H83 H 1.0589 0.0892 0.9135 0.077 Uiso 1 1 calc R . . C43 C 0.6757(6) 0.6455(6) 0.6643(3) 0.0576(16) Uani 1 1 d . . . H43 H 0.6691 0.6002 0.6344 0.069 Uiso 1 1 calc R . . C67 C 1.0789(6) 0.7651(5) 0.6618(3) 0.0524(14) Uani 1 1 d . . . C86 C 1.1785(9) 0.2504(7) 0.9101(4) 0.079(3) Uani 1 1 d . . . C84 C 0.9893(7) 0.1199(5) 0.8374(3) 0.0571(17) Uani 1 1 d . . . C45 C 0.7662(5) 0.7800(6) 0.6926(4) 0.0616(18) Uani 1 1 d . . . H45 H 0.8232 0.8271 0.6805 0.074 Uiso 1 1 calc R . . F12 F 1.1909(8) 0.1613(7) 0.5081(3) 0.135(3) Uani 1 1 d . . . C72 C 1.3425(6) 0.4073(8) 0.6067(3) 0.070(2) Uani 1 1 d . . . C82 C 1.1065(7) 0.2286(5) 0.8671(3) 0.0574(18) Uani 1 1 d . . . C16 C 0.3960(7) 0.8343(6) 0.6629(3) 0.0611(17) Uani 1 1 d . . . H16A H 0.4268 0.8169 0.6180 0.092 Uiso 1 1 calc R . . H16B H 0.3240 0.8681 0.6674 0.092 Uiso 1 1 calc R . . H16C H 0.3882 0.7726 0.6928 0.092 Uiso 1 1 calc R . . F11 F 1.3005(10) 0.0886(5) 0.5579(3) 0.172(5) Uani 1 1 d . . . C73 C 1.3604(8) 0.3315(8) 0.5649(3) 0.082(3) Uani 1 1 d . . . H73 H 1.4294 0.3224 0.5340 0.098 Uiso 1 1 calc R . . C44 C 0.7614(6) 0.7141(7) 0.6480(4) 0.0652(19) Uani 1 1 d . . . H44 H 0.8151 0.7150 0.6070 0.078 Uiso 1 1 calc R . . B1 B 1.0266(6) 0.3749(5) 0.7128(3) 0.0431(14) Uani 1 1 d . . . C75 C 1.1672(7) 0.2828(6) 0.6150(3) 0.0631(19) Uani 1 1 d . . . H75 H 1.1096 0.2395 0.6170 0.076 Uiso 1 1 calc R . . C87 C 0.9262(11) 0.0213(6) 0.8476(4) 0.084(3) Uani 1 1 d . . . C77 C 1.2867(13) 0.1772(10) 0.5276(4) 0.114(5) Uani 1 1 d . . . C74 C 1.2724(9) 0.2679(7) 0.5697(3) 0.075(2) Uani 1 1 d . . . O555 O 1.6193(8) 0.1402(8) 0.5518(5) 0.060(2) Uiso 0.50 1 d P A 2 O666 O 1.7900(12) 0.0655(11) 0.6130(7) 0.092(4) Uiso 0.50 1 d P B 1 H1 H 0.415(9) 0.877(5) 0.777(4) 0.111 Uiso 1 1 d 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 Mo1 0.0273(2) 0.0240(2) 0.0330(2) 0.00270(15) -0.01309(15) 0.00135(14) F2 0.0452(16) 0.0405(16) 0.0346(14) 0.0021(12) -0.0156(12) 0.0001(13) F1 0.0303(15) 0.0499(19) 0.0534(18) -0.0017(15) -0.0100(13) -0.0059(13) F3 0.0426(17) 0.0405(17) 0.0499(17) -0.0089(14) -0.0110(13) -0.0018(13) F6 0.065(2) 0.063(2) 0.0472(18) 0.0236(17) -0.0180(17) -0.0108(18) F22 0.065(2) 0.049(2) 0.0519(19) -0.0082(16) -0.0154(16) -0.0105(17) F24 0.077(3) 0.056(2) 0.065(2) -0.0169(18) -0.0133(19) -0.030(2) F19 0.078(3) 0.090(3) 0.0345(17) -0.0033(18) -0.0233(17) 0.001(2) O20 0.051(2) 0.057(3) 0.038(2) 0.0025(18) -0.0104(17) 0.0088(19) F13 0.090(3) 0.053(2) 0.062(2) -0.0044(18) -0.040(2) 0.013(2) F23 0.079(3) 0.060(2) 0.058(2) 0.0192(19) -0.014(2) -0.019(2) N3 0.036(2) 0.031(2) 0.037(2) -0.0045(17) -0.0176(17) 0.0005(16) O10 0.061(3) 0.035(2) 0.063(3) -0.0096(19) -0.023(2) 0.0202(19) F21 0.093(3) 0.124(4) 0.047(2) 0.004(2) -0.037(2) -0.041(3) N1 0.042(2) 0.025(2) 0.042(2) -0.0034(17) -0.0176(18) 0.0027(16) F20 0.093(3) 0.071(3) 0.051(2) 0.015(2) -0.028(2) 0.008(2) C31 0.034(2) 0.021(2) 0.049(3) 0.003(2) -0.018(2) -0.0004(17) C51 0.033(2) 0.029(2) 0.040(2) -0.0052(19) -0.0193(19) 0.0028(18) F14 0.408(14) 0.045(3) 0.113(5) -0.003(3) -0.187(7) 0.020(5) N4 0.038(2) 0.035(2) 0.044(2) 0.0025(19) -0.0114(18) -0.0030(18) N2 0.033(2) 0.051(3) 0.064(3) 0.004(2) -0.012(2) -0.003(2) F4 0.207(7) 0.046(2) 0.056(2) 0.002(2) -0.003(3) -0.046(3) F17 0.094(4) 0.072(3) 0.092(3) 0.045(3) -0.006(3) 0.009(3) F9 0.044(2) 0.236(8) 0.065(3) 0.008(4) -0.012(2) 0.014(3) C52 0.043(3) 0.030(2) 0.039(2) -0.006(2) -0.024(2) 0.006(2) C55 0.041(3) 0.030(2) 0.041(3) 0.005(2) -0.018(2) -0.005(2) F8 0.051(3) 0.147(5) 0.085(3) 0.002(3) -0.018(2) -0.027(3) F5 0.049(2) 0.085(3) 0.088(3) 0.028(3) -0.016(2) -0.023(2) C10 0.039(3) 0.046(3) 0.036(2) 0.002(2) -0.014(2) 0.006(2) C76 0.046(4) 0.164(11) 0.050(4) 0.009(5) -0.015(3) 0.007(5) C66 0.032(2) 0.034(3) 0.042(3) -0.001(2) -0.0122(19) -0.0045(19) C20 0.037(3) 0.040(3) 0.046(3) -0.002(2) -0.015(2) 0.006(2) C5 0.035(2) 0.030(2) 0.041(3) 0.001(2) -0.017(2) 0.0006(19) C53 0.054(3) 0.031(3) 0.044(3) -0.004(2) -0.029(2) 0.008(2) C65 0.042(3) 0.048(3) 0.034(2) 0.003(2) -0.019(2) -0.007(2) C64 0.046(3) 0.043(3) 0.042(3) 0.008(2) -0.024(2) -0.006(2) C60 0.041(3) 0.036(3) 0.036(2) 0.004(2) -0.022(2) 0.000(2) C2 0.028(2) 0.039(3) 0.051(3) 0.002(2) -0.022(2) -0.0058(19) C94 0.061(4) 0.033(3) 0.042(3) -0.002(2) -0.017(2) -0.010(2) C34 0.064(4) 0.034(3) 0.063(4) -0.011(3) -0.036(3) 0.004(2) F18 0.474(19) 0.060(4) 0.086(4) -0.020(3) 0.044(7) -0.101(7) C63 0.042(3) 0.033(3) 0.044(3) 0.003(2) -0.022(2) -0.004(2) F7 0.066(3) 0.249(9) 0.054(3) 0.007(4) -0.029(2) -0.027(4) C81 0.069(4) 0.043(3) 0.035(3) -0.009(2) -0.023(3) 0.016(3) C32 0.040(3) 0.031(3) 0.064(3) -0.003(2) -0.024(2) 0.001(2) C62 0.031(2) 0.038(3) 0.037(2) 0.002(2) -0.0170(19) -0.0027(19) C61 0.036(2) 0.035(3) 0.035(2) 0.007(2) -0.0185(19) -0.0041(19) F15 0.124(5) 0.372(14) 0.177(7) -0.198(9) -0.121(6) 0.160(8) C54 0.057(3) 0.031(3) 0.045(3) -0.004(2) -0.025(2) -0.001(2) C1 0.032(2) 0.042(3) 0.046(3) 0.004(2) -0.020(2) 0.001(2) C4 0.042(3) 0.041(3) 0.053(3) -0.004(2) -0.024(2) -0.004(2) C41 0.035(2) 0.031(3) 0.047(3) 0.005(2) -0.012(2) 0.004(2) C93 0.062(4) 0.042(3) 0.048(3) 0.000(2) -0.027(3) -0.011(3) C33 0.052(3) 0.030(3) 0.074(4) -0.007(3) -0.037(3) 0.000(2) C42 0.049(3) 0.040(3) 0.044(3) 0.004(2) -0.015(2) 0.003(2) C92 0.067(4) 0.045(3) 0.037(3) 0.002(2) -0.025(3) -0.011(3) C70 0.065(4) 0.053(4) 0.031(2) 0.007(2) -0.020(2) 0.013(3) F10 0.150(6) 0.156(6) 0.054(3) -0.028(3) -0.009(3) 0.034(5) C12 0.051(3) 0.047(3) 0.052(3) 0.010(3) -0.017(3) 0.001(3) F16 0.157(7) 0.061(3) 0.304(12) 0.074(5) -0.147(8) -0.040(4) C15 0.050(3) 0.049(3) 0.040(3) 0.001(2) -0.010(2) -0.002(3) C11 0.040(3) 0.042(3) 0.043(3) 0.003(2) -0.014(2) 0.002(2) C85 0.068(4) 0.038(3) 0.035(3) -0.002(2) -0.016(2) 0.009(3) C13 0.043(3) 0.036(3) 0.053(3) 0.006(2) -0.016(2) -0.006(2) C14 0.066(4) 0.031(3) 0.056(3) 0.002(2) -0.029(3) -0.001(2) C97 0.075(4) 0.038(3) 0.042(3) 0.001(2) -0.020(3) -0.017(3) C95 0.064(3) 0.029(2) 0.033(2) 0.002(2) -0.019(2) -0.004(2) C90 0.059(3) 0.031(3) 0.036(2) 0.001(2) -0.022(2) -0.002(2) C3 0.040(3) 0.044(3) 0.055(3) 0.008(3) -0.021(2) -0.008(2) C80 0.062(3) 0.037(3) 0.029(2) -0.002(2) -0.013(2) 0.012(2) C91 0.057(3) 0.041(3) 0.037(3) 0.003(2) -0.021(2) -0.007(2) C35 0.050(3) 0.030(2) 0.049(3) -0.008(2) -0.027(2) 0.007(2) C96 0.063(4) 0.070(4) 0.041(3) -0.001(3) -0.025(3) -0.008(3) C71 0.047(3) 0.088(5) 0.034(3) 0.004(3) -0.017(2) 0.013(3) C83 0.109(6) 0.046(4) 0.032(3) -0.003(3) -0.020(3) 0.039(4) C43 0.064(4) 0.055(4) 0.048(3) -0.001(3) -0.010(3) 0.012(3) C67 0.058(4) 0.045(3) 0.055(3) 0.006(3) -0.019(3) -0.012(3) C86 0.127(7) 0.075(5) 0.054(4) -0.026(4) -0.061(5) 0.059(5) C84 0.086(5) 0.033(3) 0.040(3) 0.003(2) -0.003(3) 0.015(3) C45 0.036(3) 0.071(5) 0.066(4) 0.013(4) -0.002(3) -0.001(3) F12 0.182(8) 0.135(6) 0.087(4) -0.055(4) -0.019(5) 0.005(6) C72 0.054(4) 0.116(7) 0.038(3) 0.010(4) -0.019(3) 0.022(4) C82 0.095(5) 0.044(3) 0.038(3) -0.010(3) -0.032(3) 0.037(3) C16 0.069(4) 0.064(4) 0.052(3) -0.011(3) -0.016(3) -0.012(3) F11 0.350(14) 0.083(4) 0.076(4) -0.021(3) -0.064(6) 0.078(6) C73 0.085(6) 0.108(7) 0.035(3) 0.011(4) -0.006(3) 0.041(5) C44 0.049(4) 0.081(5) 0.054(4) 0.011(4) -0.004(3) 0.014(3) B1 0.056(4) 0.046(3) 0.032(3) -0.002(3) -0.022(3) 0.007(3) C75 0.095(5) 0.056(4) 0.032(3) -0.001(3) -0.013(3) 0.021(4) C87 0.138(9) 0.035(4) 0.068(5) 0.013(4) -0.020(5) 0.006(4) C77 0.165(12) 0.114(9) 0.045(4) -0.024(5) -0.009(6) 0.055(8) C74 0.101(7) 0.075(5) 0.036(3) 0.004(3) -0.007(3) 0.028(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; 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 Mo1 C10 1.954(6) . ? Mo1 C20 1.963(6) . ? Mo1 O1 2.155(3) . ? Mo1 N1 2.226(4) . ? Mo1 C2 2.234(5) . ? Mo1 N3 2.247(4) . ? Mo1 C1 2.309(5) . ? Mo1 C3 2.338(5) . ? F2 C66 1.337(6) . ? O1 C5 1.404(6) . ? F1 C66 1.348(6) . ? F3 C66 1.337(6) . ? F6 C67 1.324(7) . ? F22 C97 1.350(8) . ? F24 C97 1.342(7) . ? F19 C96 1.338(8) . ? O20 C20 1.161(7) . ? F13 C86 1.325(9) . ? F23 C97 1.358(7) . ? N3 C51 1.347(7) . ? N3 C55 1.353(7) . ? O10 C10 1.156(7) . ? F21 C96 1.336(8) . ? N1 C35 1.338(7) . ? N1 C31 1.358(7) . ? F20 C96 1.333(9) . ? C31 C32 1.388(7) . ? C31 C5 1.543(7) . ? C51 C52 1.388(7) . ? C51 C5 1.545(7) . ? F14 C86 1.325(11) . ? N4 C15 1.498(7) . ? N4 C13 1.505(7) . ? N4 C11 1.512(7) . ? N4 H1 0.93(8) . ? N2 C41 1.320(7) . ? N2 C45 1.359(9) . ? F4 C67 1.299(8) . ? F17 C87 1.320(10) . ? F9 C76 1.335(10) . ? C52 C53 1.392(8) . ? C52 H52 0.9300 . ? C55 C54 1.382(8) . ? C55 H55 0.9300 . ? F8 C76 1.369(13) . ? F5 C67 1.350(8) . ? C76 F7 1.341(9) . ? C76 C72 1.470(14) . ? C66 C62 1.496(7) . ? C5 C41 1.522(7) . ? C53 C54 1.391(9) . ? C53 H53 0.9300 . ? C65 C64 1.396(8) . ? C65 C60 1.399(8) . ? C65 H65 0.9300 . ? C64 C63 1.390(8) . ? C64 C67 1.511(8) . ? C60 C61 1.394(7) . ? C60 B1 1.635(8) . ? C2 C3 1.415(8) . ? C2 C1 1.416(8) . ? C2 C4 1.505(8) . ? C94 C95 1.402(8) . ? C94 C93 1.404(8) . ? C94 C97 1.481(9) . ? C34 C33 1.366(10) . ? C34 C35 1.389(8) . ? C34 H34 0.9300 . ? F18 C87 1.287(11) . ? C63 C62 1.391(7) . ? C63 H63 0.9300 . ? C81 C82 1.379(8) . ? C81 C80 1.403(8) . ? C81 H81 0.9300 . ? C32 C33 1.395(8) . ? C32 H32 0.9300 . ? C62 C61 1.388(7) . ? C61 H61 0.9300 . ? F15 C86 1.296(13) . ? C54 H54 0.9300 . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C41 C42 1.387(8) . ? C93 C92 1.371(9) . ? C93 H93 0.9300 . ? C33 H33 0.9300 . ? C42 C43 1.388(9) . ? C42 H42 0.9300 . ? C92 C91 1.393(8) . ? C92 C96 1.500(8) . ? C70 C71 1.381(10) . ? C70 C75 1.397(9) . ? C70 B1 1.643(9) . ? F10 C77 1.314(13) . ? C12 C11 1.515(8) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? F16 C87 1.303(14) . ? C15 C16 1.511(9) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C85 C80 1.386(9) . ? C85 C84 1.398(8) . ? C85 H85 0.9300 . ? C13 C14 1.531(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C95 C90 1.385(8) . ? C95 H95 0.9300 . ? C90 C91 1.398(7) . ? C90 B1 1.643(8) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C80 B1 1.637(8) . ? C91 H91 0.9300 . ? C35 H35 0.9300 . ? C71 C72 1.396(9) . ? C71 H71 0.9300 . ? C83 C82 1.363(11) . ? C83 C84 1.377(11) . ? C83 H83 0.9300 . ? C43 C44 1.381(11) . ? C43 H43 0.9300 . ? C86 C82 1.502(10) . ? C84 C87 1.512(12) . ? C45 C44 1.354(12) . ? C45 H45 0.9300 . ? F12 C77 1.403(17) . ? C72 C73 1.359(13) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? F11 C77 1.285(13) . ? C73 C74 1.391(14) . ? C73 H73 0.9300 . ? C44 H44 0.9300 . ? C75 C74 1.403(11) . ? C75 H75 0.9300 . ? C77 C74 1.523(14) . ? 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 C10 Mo1 C20 79.9(2) . . ? C10 Mo1 O1 105.16(18) . . ? C20 Mo1 O1 164.12(18) . . ? C10 Mo1 N1 88.63(19) . . ? C20 Mo1 N1 92.58(19) . . ? O1 Mo1 N1 72.73(15) . . ? C10 Mo1 C2 105.4(2) . . ? C20 Mo1 C2 103.3(2) . . ? O1 Mo1 C2 90.00(17) . . ? N1 Mo1 C2 160.28(18) . . ? C10 Mo1 N3 166.45(19) . . ? C20 Mo1 N3 97.48(19) . . ? O1 Mo1 N3 74.04(14) . . ? N1 Mo1 N3 78.17(15) . . ? C2 Mo1 N3 88.14(17) . . ? C10 Mo1 C1 73.0(2) . . ? C20 Mo1 C1 112.7(2) . . ? O1 Mo1 C1 83.16(17) . . ? N1 Mo1 C1 144.72(18) . . ? C2 Mo1 C1 36.3(2) . . ? N3 Mo1 C1 119.86(17) . . ? C10 Mo1 C3 104.5(2) . . ? C20 Mo1 C3 68.0(2) . . ? O1 Mo1 C3 123.67(18) . . ? N1 Mo1 C3 153.55(18) . . ? C2 Mo1 C3 36.0(2) . . ? N3 Mo1 C3 86.53(19) . . ? C1 Mo1 C3 61.7(2) . . ? C5 O1 Mo1 106.8(3) . . ? C51 N3 C55 118.7(4) . . ? C51 N3 Mo1 112.5(3) . . ? C55 N3 Mo1 128.4(4) . . ? C35 N1 C31 118.9(5) . . ? C35 N1 Mo1 125.9(4) . . ? C31 N1 Mo1 115.0(3) . . ? N1 C31 C32 121.6(5) . . ? N1 C31 C5 110.2(4) . . ? C32 C31 C5 128.1(5) . . ? N3 C51 C52 121.7(5) . . ? N3 C51 C5 113.2(4) . . ? C52 C51 C5 125.0(5) . . ? C15 N4 C13 108.8(4) . . ? C15 N4 C11 113.3(4) . . ? C13 N4 C11 112.5(4) . . ? C15 N4 H1 108(7) . . ? C13 N4 H1 111(7) . . ? C11 N4 H1 103(7) . . ? C41 N2 C45 117.2(6) . . ? C51 C52 C53 119.1(5) . . ? C51 C52 H52 120.5 . . ? C53 C52 H52 120.5 . . ? N3 C55 C54 123.1(5) . . ? N3 C55 H55 118.5 . . ? C54 C55 H55 118.5 . . ? O10 C10 Mo1 177.0(5) . . ? F9 C76 F7 106.4(6) . . ? F9 C76 F8 105.1(8) . . ? F7 C76 F8 104.9(10) . . ? F9 C76 C72 114.6(10) . . ? F7 C76 C72 112.6(8) . . ? F8 C76 C72 112.5(6) . . ? F2 C66 F3 107.4(4) . . ? F2 C66 F1 105.5(4) . . ? F3 C66 F1 106.4(4) . . ? F2 C66 C62 112.1(4) . . ? F3 C66 C62 112.9(4) . . ? F1 C66 C62 112.1(4) . . ? O20 C20 Mo1 177.5(5) . . ? O1 C5 C41 109.0(4) . . ? O1 C5 C31 107.1(4) . . ? C41 C5 C31 118.2(4) . . ? O1 C5 C51 109.6(4) . . ? C41 C5 C51 110.5(4) . . ? C31 C5 C51 102.1(4) . . ? C54 C53 C52 119.7(5) . . ? C54 C53 H53 120.2 . . ? C52 C53 H53 120.2 . . ? C64 C65 C60 122.5(5) . . ? C64 C65 H65 118.7 . . ? C60 C65 H65 118.7 . . ? C63 C64 C65 120.5(5) . . ? C63 C64 C67 121.2(5) . . ? C65 C64 C67 118.2(5) . . ? C61 C60 C65 115.7(5) . . ? C61 C60 B1 123.2(5) . . ? C65 C60 B1 121.1(5) . . ? C3 C2 C1 114.7(5) . . ? C3 C2 C4 124.0(5) . . ? C1 C2 C4 121.3(5) . . ? C3 C2 Mo1 76.0(3) . . ? C1 C2 Mo1 74.8(3) . . ? C4 C2 Mo1 116.4(3) . . ? C95 C94 C93 119.9(6) . . ? C95 C94 C97 121.3(5) . . ? C93 C94 C97 118.8(6) . . ? C33 C34 C35 119.0(5) . . ? C33 C34 H34 120.5 . . ? C35 C34 H34 120.5 . . ? C64 C63 C62 117.7(5) . . ? C64 C63 H63 121.2 . . ? C62 C63 H63 121.2 . . ? C82 C81 C80 122.9(7) . . ? C82 C81 H81 118.6 . . ? C80 C81 H81 118.6 . . ? C31 C32 C33 118.4(6) . . ? C31 C32 H32 120.8 . . ? C33 C32 H32 120.8 . . ? C61 C62 C63 121.2(5) . . ? C61 C62 C66 118.2(5) . . ? C63 C62 C66 120.6(5) . . ? C62 C61 C60 122.4(5) . . ? C62 C61 H61 118.8 . . ? C60 C61 H61 118.8 . . ? C55 C54 C53 117.8(5) . . ? C55 C54 H54 121.1 . . ? C53 C54 H54 121.1 . . ? C2 C1 Mo1 69.0(3) . . ? C2 C1 H1A 116.8 . . ? Mo1 C1 H1A 116.8 . . ? C2 C1 H1B 116.8 . . ? Mo1 C1 H1B 116.8 . . ? H1A C1 H1B 113.8 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C41 C42 122.3(5) . . ? N2 C41 C5 119.5(5) . . ? C42 C41 C5 118.0(5) . . ? C92 C93 C94 118.3(6) . . ? C92 C93 H93 120.8 . . ? C94 C93 H93 120.8 . . ? C34 C33 C32 119.8(5) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C41 C42 C43 119.7(6) . . ? C41 C42 H42 120.2 . . ? C43 C42 H42 120.2 . . ? C93 C92 C91 121.0(5) . . ? C93 C92 C96 119.3(6) . . ? C91 C92 C96 119.6(6) . . ? C71 C70 C75 116.1(7) . . ? C71 C70 B1 123.3(6) . . ? C75 C70 B1 120.4(7) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N4 C15 C16 112.9(5) . . ? N4 C15 H15A 109.0 . . ? C16 C15 H15A 109.0 . . ? N4 C15 H15B 109.0 . . ? C16 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? N4 C11 C12 114.3(5) . . ? N4 C11 H11A 108.7 . . ? C12 C11 H11A 108.7 . . ? N4 C11 H11B 108.7 . . ? C12 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C80 C85 C84 122.4(6) . . ? C80 C85 H85 118.8 . . ? C84 C85 H85 118.8 . . ? N4 C13 C14 112.6(5) . . ? N4 C13 H13A 109.1 . . ? C14 C13 H13A 109.1 . . ? N4 C13 H13B 109.1 . . ? C14 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? F24 C97 F22 106.3(6) . . ? F24 C97 F23 106.3(5) . . ? F22 C97 F23 105.4(5) . . ? F24 C97 C94 112.2(5) . . ? F22 C97 C94 113.2(5) . . ? F23 C97 C94 112.9(6) . . ? C90 C95 C94 122.2(5) . . ? C90 C95 H95 118.9 . . ? C94 C95 H95 118.9 . . ? C95 C90 C91 116.5(5) . . ? C95 C90 B1 121.4(5) . . ? C91 C90 B1 121.8(5) . . ? C2 C3 Mo1 68.0(3) . . ? C2 C3 H3A 116.9 . . ? Mo1 C3 H3A 116.9 . . ? C2 C3 H3B 116.9 . . ? Mo1 C3 H3B 116.9 . . ? H3A C3 H3B 113.9 . . ? C85 C80 C81 114.5(5) . . ? C85 C80 B1 125.0(5) . . ? C81 C80 B1 120.4(6) . . ? C92 C91 C90 122.0(6) . . ? C92 C91 H91 119.0 . . ? C90 C91 H91 119.0 . . ? N1 C35 C34 122.2(6) . . ? N1 C35 H35 118.9 . . ? C34 C35 H35 118.9 . . ? F20 C96 F21 106.9(6) . . ? F20 C96 F19 106.2(6) . . ? F21 C96 F19 106.3(6) . . ? F20 C96 C92 112.3(6) . . ? F21 C96 C92 112.2(6) . . ? F19 C96 C92 112.5(6) . . ? C70 C71 C72 123.0(7) . . ? C70 C71 H71 118.5 . . ? C72 C71 H71 118.5 . . ? C82 C83 C84 117.6(6) . . ? C82 C83 H83 121.2 . . ? C84 C83 H83 121.2 . . ? C44 C43 C42 117.8(7) . . ? C44 C43 H43 121.1 . . ? C42 C43 H43 121.1 . . ? F4 C67 F6 108.2(6) . . ? F4 C67 F5 107.2(6) . . ? F6 C67 F5 102.9(5) . . ? F4 C67 C64 113.3(6) . . ? F6 C67 C64 112.5(5) . . ? F5 C67 C64 112.0(5) . . ? F15 C86 F13 105.5(10) . . ? F15 C86 F14 106.9(8) . . ? F13 C86 F14 105.3(5) . . ? F15 C86 C82 112.3(6) . . ? F13 C86 C82 113.9(5) . . ? F14 C86 C82 112.3(9) . . ? C83 C84 C85 121.1(7) . . ? C83 C84 C87 120.8(6) . . ? C85 C84 C87 118.1(7) . . ? C44 C45 N2 123.9(7) . . ? C44 C45 H45 118.0 . . ? N2 C45 H45 118.0 . . ? C73 C72 C71 120.7(9) . . ? C73 C72 C76 120.8(8) . . ? C71 C72 C76 118.5(8) . . ? C83 C82 C81 121.4(6) . . ? C83 C82 C86 119.5(6) . . ? C81 C82 C86 119.1(7) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C72 C73 C74 118.0(7) . . ? C72 C73 H73 121.0 . . ? C74 C73 H73 121.0 . . ? C45 C44 C43 118.9(6) . . ? C45 C44 H44 120.5 . . ? C43 C44 H44 120.5 . . ? C60 B1 C80 111.4(4) . . ? C60 B1 C90 103.8(4) . . ? C80 B1 C90 112.9(5) . . ? C60 B1 C70 111.0(5) . . ? C80 B1 C70 104.6(5) . . ? C90 B1 C70 113.2(4) . . ? C70 C75 C74 120.8(8) . . ? C70 C75 H75 119.6 . . ? C74 C75 H75 119.6 . . ? F18 C87 F16 109.4(12) . . ? F18 C87 F17 105.9(8) . . ? F16 C87 F17 104.3(9) . . ? F18 C87 C84 111.8(8) . . ? F16 C87 C84 112.1(7) . . ? F17 C87 C84 112.8(9) . . ? F11 C77 F10 114.6(10) . . ? F11 C77 F12 101.1(14) . . ? F10 C77 F12 100.7(9) . . ? F11 C77 C74 114.8(8) . . ? F10 C77 C74 111.5(12) . . ? F12 C77 C74 112.8(9) . . ? C73 C74 C75 121.3(8) . . ? C73 C74 C77 121.6(9) . . ? C75 C74 C77 117.1(10) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 74.0196 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 2.113 _refine_diff_density_min -1.091 _refine_diff_density_rms 0.151 #===END data_1'H_(mp302) _database_code_depnum_ccdc_archive 'CCDC 786114' #TrackingRef 'CIFS.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H12 B F24, C23 H21 Mo N2 O3, H2 O' _chemical_formula_sum 'C55 H35 B F24 Mo N2 O4' _chemical_formula_weight 1350.60 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' C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 '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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4659(10) _cell_length_b 13.5960(10) _cell_length_c 17.4953(13) _cell_angle_alpha 85.431(6) _cell_angle_beta 83.001(6) _cell_angle_gamma 81.125(6) _cell_volume 2902.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5947 _cell_measurement_theta_min 3.2939 _cell_measurement_theta_max 73.7037 _exptl_crystal_description blocks _exptl_crystal_colour orange _exptl_crystal_size_max 0.1053 _exptl_crystal_size_mid 0.0584 _exptl_crystal_size_min 0.0246 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1348 _exptl_absorpt_coefficient_mu 2.972 _exptl_absorpt_correction_T_min 0.810 _exptl_absorpt_correction_T_max 0.930 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Onyx, Nova' _diffrn_detector_area_resol_mean 8.2640 _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21862 _diffrn_reflns_av_R_equivalents 0.0616 _diffrn_reflns_av_sigmaI/netI 0.0714 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 73.94 _reflns_number_total 11256 _reflns_number_gt 7361 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2008)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [1.00000+-1.00000exp(-7.65(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.2000P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11256 _refine_ls_number_parameters 793 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1194 _refine_ls_R_factor_gt 0.0969 _refine_ls_wR_factor_ref 0.2406 _refine_ls_wR_factor_gt 0.2376 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5870(10) 0.8034(7) 0.4766(7) 0.085(3) Uani 1 1 d . . . H1A H 0.6524 0.8346 0.4732 0.101 Uiso 1 1 calc R . . H1B H 0.5399 0.8129 0.5246 0.101 Uiso 1 1 calc R . . C2 C 0.5978(9) 0.7122(8) 0.4471(6) 0.081(3) Uani 1 1 d . . . C3 C 0.6579(10) 0.7021(8) 0.3735(8) 0.087(3) Uani 1 1 d . . . H3A H 0.6621 0.6385 0.3509 0.105 Uiso 1 1 calc R . . H3B H 0.7257 0.7301 0.3650 0.105 Uiso 1 1 calc R . . C4 C 0.5418(11) 0.6282(7) 0.4901(7) 0.092(4) Uani 1 1 d . . . H4A H 0.5583 0.5698 0.4609 0.138 Uiso 1 1 calc R . . H4B H 0.4642 0.6488 0.4965 0.138 Uiso 1 1 calc R . . H4C H 0.5676 0.6134 0.5398 0.138 Uiso 1 1 calc R . . C5 C 0.3225(6) 0.7022(5) 0.3359(3) 0.0481(15) Uani 1 1 d . . . C10 C 0.5285(10) 0.9417(7) 0.3874(5) 0.077(3) Uani 1 1 d . . . C20 C 0.6051(11) 0.8360(8) 0.2761(7) 0.087(3) Uani 1 1 d . . . C31 C 0.2982(7) 0.7975(5) 0.2827(3) 0.0515(16) Uani 1 1 d . . . C32 C 0.2114(7) 0.8212(5) 0.2409(4) 0.0541(17) Uani 1 1 d . . . H32 H 0.1615 0.7771 0.2405 0.065 Uiso 1 1 calc R . . C33 C 0.1991(8) 0.9136(5) 0.1986(4) 0.0591(18) Uani 1 1 d . . . H33 H 0.1406 0.9316 0.1695 0.071 Uiso 1 1 calc R . . C34 C 0.2739(8) 0.9771(6) 0.2006(4) 0.064(2) Uani 1 1 d . . . H34 H 0.2683 1.0378 0.1717 0.076 Uiso 1 1 calc R . . C35 C 0.3575(8) 0.9495(5) 0.2459(4) 0.0599(19) Uani 1 1 d . . . H35 H 0.4060 0.9941 0.2491 0.072 Uiso 1 1 calc R . . C40 C 0.2787(7) 0.6098(5) 0.3161(4) 0.0560(18) Uani 1 1 d . . . C41 C 0.2617(8) 0.5349(5) 0.3737(4) 0.0592(19) Uani 1 1 d . . . H41 H 0.2657 0.5468 0.4248 0.071 Uiso 1 1 calc R . . C42 C 0.2391(9) 0.4433(6) 0.3563(5) 0.070(2) Uani 1 1 d . . . H42 H 0.2288 0.3939 0.3953 0.084 Uiso 1 1 calc R . . C43 C 0.2319(11) 0.4257(6) 0.2798(6) 0.085(3) Uani 1 1 d . . . H43 H 0.2167 0.3643 0.2676 0.101 Uiso 1 1 calc R . . C44 C 0.2476(10) 0.5003(7) 0.2214(5) 0.079(3) Uani 1 1 d . . . H44 H 0.2429 0.4893 0.1702 0.095 Uiso 1 1 calc R . . C45 C 0.2704(9) 0.5916(6) 0.2415(4) 0.066(2) Uani 1 1 d . . . H45 H 0.2802 0.6416 0.2030 0.080 Uiso 1 1 calc R . . C51 C 0.2785(7) 0.7407(5) 0.4157(4) 0.0523(16) Uani 1 1 d . . . C52 C 0.1760(7) 0.7315(5) 0.4519(4) 0.0588(18) Uani 1 1 d . . . H52 H 0.1309 0.6950 0.4308 0.071 Uiso 1 1 calc R . . C53 C 0.1407(9) 0.7781(6) 0.5209(4) 0.067(2) Uani 1 1 d . . . H53 H 0.0714 0.7741 0.5464 0.080 Uiso 1 1 calc R . . C54 C 0.2125(11) 0.8305(6) 0.5502(4) 0.078(3) Uani 1 1 d . . . H54 H 0.1927 0.8607 0.5967 0.093 Uiso 1 1 calc R . . C55 C 0.3101(10) 0.8370(5) 0.5107(4) 0.070(3) Uani 1 1 d . . . H55 H 0.3558 0.8740 0.5307 0.084 Uiso 1 1 calc R . . C60 C 0.9967(7) 0.1582(5) 0.2543(3) 0.0511(16) Uani 1 1 d . . . C61 C 0.9520(7) 0.0693(5) 0.2648(4) 0.0558(17) Uani 1 1 d . . . H61 H 0.9016 0.0589 0.2323 0.067 Uiso 1 1 calc R . . C62 C 0.9799(7) -0.0048(5) 0.3224(4) 0.0530(16) Uani 1 1 d . . . C63 C 1.0564(7) 0.0064(5) 0.3704(4) 0.0549(17) Uani 1 1 d . . . H63 H 1.0758 -0.0425 0.4086 0.066 Uiso 1 1 calc R . . C64 C 1.1040(7) 0.0944(5) 0.3596(4) 0.0555(18) Uani 1 1 d . . . C65 C 1.0764(7) 0.1664(5) 0.3030(4) 0.0557(18) Uani 1 1 d . . . H65 H 1.1116 0.2225 0.2965 0.067 Uiso 1 1 calc R . . C66 C 0.9232(8) -0.0958(5) 0.3310(5) 0.0601(19) Uani 1 1 d . . . C67 C 1.1883(9) 0.1100(6) 0.4105(5) 0.063(2) Uani 1 1 d . . . C70 C 1.0701(7) 0.2208(5) 0.1169(4) 0.0557(17) Uani 1 1 d . . . C71 C 1.0760(8) 0.1426(6) 0.0685(4) 0.063(2) Uani 1 1 d . . . H71 H 1.0186 0.1053 0.0738 0.075 Uiso 1 1 calc R . . C72 C 1.1621(8) 0.1185(6) 0.0137(4) 0.065(2) Uani 1 1 d . . . C73 C 1.2491(9) 0.1722(9) 0.0039(5) 0.077(2) Uani 1 1 d . . . H73 H 1.3082 0.1579 -0.0334 0.092 Uiso 1 1 calc R . . C74 C 1.2429(11) 0.2500(9) 0.0537(6) 0.084(3) Uani 1 1 d . . . C75 C 1.1563(9) 0.2723(7) 0.1085(5) 0.070(2) Uani 1 1 d . . . H75 H 1.1564 0.3236 0.1405 0.084 Uiso 1 1 calc R . . C76 C 1.1621(12) 0.0348(8) -0.0369(5) 0.085(3) Uani 1 1 d . . . C77 C 1.3392(16) 0.3149(17) 0.0468(12) 0.123(5) Uani 1 1 d . . . C80 C 0.9598(8) 0.3576(5) 0.2149(4) 0.060(2) Uani 1 1 d . . . C81 C 0.9412(8) 0.3829(5) 0.2907(4) 0.063(2) Uani 1 1 d . . . H81 H 0.9359 0.3321 0.3292 0.076 Uiso 1 1 calc R . . C82 C 0.9301(9) 0.4802(6) 0.3122(5) 0.066(2) Uani 1 1 d . . . C83 C 0.9358(9) 0.5585(5) 0.2575(5) 0.070(2) Uani 1 1 d . . . H83 H 0.9288 0.6239 0.2716 0.084 Uiso 1 1 calc R . . C84 C 0.9522(10) 0.5362(6) 0.1818(5) 0.078(3) Uani 1 1 d . . . C85 C 0.9651(10) 0.4392(6) 0.1602(4) 0.073(3) Uani 1 1 d . . . H85 H 0.9777 0.4274 0.1080 0.087 Uiso 1 1 calc R . . C86 C 0.9107(11) 0.5002(6) 0.3960(5) 0.074(3) Uani 1 1 d . . . C87 C 0.9532(16) 0.6211(8) 0.1214(6) 0.108(5) Uani 1 1 d . . . C90 C 0.8496(8) 0.2393(5) 0.1566(4) 0.0595(19) Uani 1 1 d . . . C91 C 0.8307(8) 0.2568(6) 0.0786(4) 0.0634(19) Uani 1 1 d . . . H91 H 0.8874 0.2703 0.0415 0.076 Uiso 1 1 calc R . . C92 C 0.7292(10) 0.2541(9) 0.0572(5) 0.080(3) Uani 1 1 d . . . C93 C 0.6418(11) 0.2366(10) 0.1088(7) 0.089(3) Uani 1 1 d . . . H93 H 0.5742 0.2326 0.0929 0.107 Uiso 1 1 calc R . . C94 C 0.6589(11) 0.2249(12) 0.1866(7) 0.101(4) Uani 1 1 d . . . C95 C 0.7605(9) 0.2244(8) 0.2083(5) 0.077(3) Uani 1 1 d . . . H95 H 0.7698 0.2135 0.2604 0.092 Uiso 1 1 calc R . . C96 C 0.7092(11) 0.2699(13) -0.0271(6) 0.099(4) Uani 1 1 d . . . C97 C 0.5618(18) 0.207(3) 0.2460(12) 0.170(12) Uani 1 1 d . . . N1 N 0.3721(6) 0.8607(4) 0.2858(3) 0.0526(14) Uani 1 1 d . . . N3 N 0.3471(6) 0.7938(4) 0.4438(3) 0.0528(14) Uani 1 1 d . . . O1 O 0.4368(5) 0.6787(3) 0.3361(3) 0.0545(12) Uani 1 1 d D . . O10 O 0.5417(10) 1.0206(5) 0.4018(5) 0.104(3) Uani 1 1 d . . . O20 O 0.6680(9) 0.8531(8) 0.2214(6) 0.110(3) Uani 1 1 d . . . O100 O 0.5449(15) 0.584(2) 0.2258(16) 0.225(14) Uani 1 1 d D . . F1 F 0.8191(5) -0.0752(4) 0.3521(3) 0.0776(14) Uani 1 1 d . . . F2 F 0.9339(6) -0.1410(4) 0.2638(3) 0.0817(16) Uani 1 1 d . . . F3 F 0.9659(6) -0.1653(4) 0.3812(4) 0.0874(18) Uani 1 1 d . . . F4 F 1.2822(9) 0.1150(19) 0.3733(8) 0.236(11) Uani 1 1 d . . . F5 F 1.1662(7) 0.1973(5) 0.4407(4) 0.103(2) Uani 1 1 d . . . F6 F 1.2024(13) 0.0453(6) 0.4647(7) 0.195(8) Uani 1 1 d . . . F7 F 1.0928(9) 0.0591(5) -0.0899(3) 0.108(3) Uani 1 1 d . . . F8 F 1.1305(7) -0.0453(4) 0.0038(3) 0.095(2) Uani 1 1 d . . . F9 F 1.2598(10) 0.0042(8) -0.0735(7) 0.134(4) Uani 1 1 d . . . F10 F 1.2953(11) 0.4107(9) 0.0253(9) 0.152(4) Uani 1 1 d . . . F11 F 1.3738(8) 0.3240(10) 0.1049(11) 0.169(6) Uani 1 1 d . . . F12 F 1.4153(10) 0.2819(13) -0.0098(11) 0.180(7) Uani 1 1 d . . . F13 F 0.9255(9) 0.5911(4) 0.4100(4) 0.110(3) Uani 1 1 d . . . F14 F 0.8072(7) 0.4903(5) 0.4259(3) 0.096(2) Uani 1 1 d . . . F15 F 0.9735(6) 0.4349(4) 0.4389(3) 0.0796(16) Uani 1 1 d . . . F16 F 0.997(2) 0.5994(6) 0.0579(4) 0.260(12) Uani 1 1 d . . . F17 F 0.9922(10) 0.6972(5) 0.1394(4) 0.128(4) Uani 1 1 d . . . F18 F 0.8558(16) 0.6627(16) 0.1091(14) 0.281(14) Uani 1 1 d . . . F19 F 0.8002(8) 0.2495(7) -0.0751(4) 0.112(3) Uani 1 1 d . . . F20 F 0.6496(10) 0.2117(13) -0.0491(6) 0.159(5) Uani 1 1 d . . . F21 F 0.6489(13) 0.3624(8) -0.0396(5) 0.156(5) Uani 1 1 d . . . F22 F 0.530(2) 0.125(3) 0.2381(9) 0.32(2) Uani 1 1 d D . . F23 F 0.5868(9) 0.2071(10) 0.3187(5) 0.136(4) Uani 1 1 d . . . F24 F 0.4838(13) 0.275(3) 0.2439(10) 0.32(2) Uani 1 1 d D . . Mo Mo 0.50138(6) 0.81077(4) 0.36446(4) 0.0591(3) Uani 1 1 d . . . B1 B 0.9696(8) 0.2446(6) 0.1852(4) 0.056(2) Uani 1 1 d . . . H1 H 0.466(8) 0.632(6) 0.304(5) 0.068 Uiso 1 1 d D . . H500 H 0.574(7) 0.565(7) 0.172(2) 0.19 Uiso 1 1 d D . . H600 H 0.471(4) 0.569(7) 0.245(5) 0.19 Uiso 1 1 d 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 C1 0.106(7) 0.071(5) 0.096(6) 0.018(5) -0.078(6) -0.032(5) C2 0.095(6) 0.080(6) 0.079(6) 0.023(5) -0.057(5) -0.029(5) C3 0.091(7) 0.064(5) 0.117(9) 0.014(5) -0.053(7) -0.020(5) C4 0.124(8) 0.056(5) 0.105(7) 0.034(5) -0.064(7) -0.025(5) C5 0.074(4) 0.039(3) 0.038(3) 0.006(2) -0.024(3) -0.021(3) C10 0.125(8) 0.055(4) 0.065(5) 0.004(3) -0.047(5) -0.035(5) C20 0.105(8) 0.071(6) 0.096(7) 0.022(5) -0.045(6) -0.037(5) C31 0.084(5) 0.040(3) 0.035(3) 0.009(2) -0.020(3) -0.020(3) C32 0.084(5) 0.045(3) 0.041(3) 0.010(2) -0.026(3) -0.022(3) C33 0.098(6) 0.047(3) 0.036(3) 0.012(2) -0.026(3) -0.015(3) C34 0.105(6) 0.048(3) 0.039(3) 0.017(3) -0.021(3) -0.016(4) C35 0.105(6) 0.040(3) 0.043(3) 0.012(3) -0.026(3) -0.027(3) C40 0.086(5) 0.045(3) 0.045(3) 0.012(3) -0.032(3) -0.024(3) C41 0.098(6) 0.045(3) 0.046(3) 0.005(3) -0.033(3) -0.029(3) C42 0.109(7) 0.050(4) 0.061(4) 0.023(3) -0.036(4) -0.035(4) C43 0.138(9) 0.047(4) 0.087(6) 0.011(4) -0.056(6) -0.044(5) C44 0.138(8) 0.057(4) 0.059(4) 0.008(3) -0.053(5) -0.043(5) C45 0.121(7) 0.048(4) 0.042(3) 0.006(3) -0.036(4) -0.032(4) C51 0.083(5) 0.036(3) 0.042(3) 0.014(2) -0.027(3) -0.015(3) C52 0.085(5) 0.048(3) 0.045(3) 0.014(3) -0.024(3) -0.013(3) C53 0.107(6) 0.050(4) 0.041(3) 0.016(3) -0.018(4) -0.005(4) C54 0.145(9) 0.049(4) 0.037(3) 0.011(3) -0.020(5) -0.006(5) C55 0.135(8) 0.043(3) 0.042(3) 0.010(3) -0.047(5) -0.021(4) C60 0.092(5) 0.037(3) 0.030(2) 0.007(2) -0.025(3) -0.018(3) C61 0.090(5) 0.044(3) 0.039(3) 0.010(3) -0.028(3) -0.017(3) C62 0.085(5) 0.036(3) 0.042(3) 0.013(2) -0.022(3) -0.016(3) C63 0.096(5) 0.037(3) 0.035(3) 0.013(2) -0.023(3) -0.014(3) C64 0.097(5) 0.036(3) 0.037(3) 0.006(2) -0.029(3) -0.010(3) C65 0.105(6) 0.032(3) 0.038(3) 0.002(2) -0.027(3) -0.021(3) C66 0.083(6) 0.043(3) 0.057(4) 0.020(3) -0.023(4) -0.014(3) C67 0.098(6) 0.044(3) 0.055(4) 0.004(3) -0.036(4) -0.011(4) C70 0.092(5) 0.046(3) 0.033(3) 0.013(2) -0.025(3) -0.016(3) C71 0.104(6) 0.046(3) 0.043(3) 0.015(3) -0.016(4) -0.031(4) C72 0.098(6) 0.054(4) 0.044(3) 0.011(3) -0.012(4) -0.021(4) C73 0.089(6) 0.086(6) 0.056(4) 0.015(4) -0.011(4) -0.020(5) C74 0.112(8) 0.079(6) 0.073(6) -0.019(5) -0.034(6) -0.029(5) C75 0.096(6) 0.070(5) 0.053(4) -0.003(3) -0.029(4) -0.026(4) C76 0.139(10) 0.065(5) 0.052(4) 0.005(4) 0.005(5) -0.031(6) C77 0.110(11) 0.135(15) 0.123(12) -0.024(11) 0.011(10) -0.023(10) C80 0.108(6) 0.043(3) 0.036(3) 0.019(3) -0.033(3) -0.024(3) C81 0.109(6) 0.038(3) 0.047(3) 0.021(3) -0.031(4) -0.020(3) C82 0.108(6) 0.043(3) 0.052(4) 0.014(3) -0.034(4) -0.015(4) C83 0.127(7) 0.035(3) 0.057(4) 0.010(3) -0.043(4) -0.022(4) C84 0.148(9) 0.050(4) 0.045(4) 0.022(3) -0.041(5) -0.035(5) C85 0.147(8) 0.041(3) 0.039(3) 0.018(3) -0.038(4) -0.030(4) C86 0.133(9) 0.039(3) 0.054(4) 0.005(3) -0.032(5) -0.009(4) C87 0.222(16) 0.054(5) 0.059(5) 0.024(4) -0.045(7) -0.045(7) C90 0.102(6) 0.046(3) 0.036(3) 0.014(2) -0.028(3) -0.022(3) C91 0.094(6) 0.064(4) 0.036(3) 0.013(3) -0.023(3) -0.021(4) C92 0.096(7) 0.098(7) 0.050(4) 0.006(4) -0.026(4) -0.021(5) C93 0.099(7) 0.100(7) 0.074(6) 0.030(5) -0.034(5) -0.030(6) C94 0.102(8) 0.130(10) 0.064(5) 0.052(6) -0.018(5) -0.018(7) C95 0.096(6) 0.082(6) 0.049(4) 0.031(4) -0.020(4) -0.011(5) C96 0.093(7) 0.146(12) 0.055(5) 0.014(6) -0.019(5) -0.013(7) C97 0.120(13) 0.27(3) 0.103(11) 0.103(17) -0.026(10) -0.006(16) N1 0.089(4) 0.039(3) 0.038(2) 0.012(2) -0.029(3) -0.024(3) N3 0.095(4) 0.033(2) 0.037(2) 0.0074(19) -0.031(3) -0.016(2) O1 0.086(4) 0.037(2) 0.049(2) 0.0026(17) -0.031(2) -0.020(2) O10 0.182(9) 0.054(3) 0.099(5) 0.008(3) -0.070(6) -0.053(4) O20 0.120(7) 0.109(6) 0.106(6) 0.024(5) -0.019(5) -0.046(5) O100 0.125(10) 0.33(3) 0.24(2) -0.19(2) 0.003(12) -0.036(14) F1 0.094(4) 0.059(3) 0.084(3) 0.015(2) -0.021(3) -0.028(2) F2 0.129(5) 0.052(2) 0.074(3) 0.000(2) -0.025(3) -0.037(3) F3 0.114(4) 0.057(3) 0.099(4) 0.045(3) -0.046(3) -0.035(3) F4 0.104(7) 0.49(3) 0.138(9) -0.162(15) -0.057(6) -0.006(11) F5 0.152(6) 0.067(3) 0.108(5) -0.005(3) -0.079(5) -0.027(3) F6 0.361(17) 0.077(4) 0.208(10) 0.078(6) -0.235(13) -0.103(7) F7 0.213(8) 0.078(3) 0.045(2) 0.002(2) -0.034(4) -0.054(4) F8 0.169(6) 0.049(2) 0.069(3) 0.003(2) -0.012(3) -0.025(3) F9 0.154(8) 0.114(6) 0.130(7) -0.038(5) 0.044(7) -0.040(6) F10 0.172(9) 0.109(7) 0.189(11) -0.022(7) 0.003(8) -0.081(7) F11 0.106(6) 0.167(10) 0.264(16) -0.105(11) -0.064(8) -0.030(6) F12 0.118(7) 0.195(13) 0.242(17) -0.085(12) 0.035(9) -0.079(8) F13 0.229(9) 0.046(2) 0.064(3) -0.002(2) -0.045(4) -0.026(4) F14 0.136(6) 0.087(4) 0.056(3) 0.009(3) -0.014(3) 0.005(4) F15 0.147(5) 0.052(2) 0.045(2) 0.0062(18) -0.039(3) -0.010(3) F16 0.67(4) 0.059(4) 0.047(3) 0.010(3) 0.041(8) -0.120(10) F17 0.253(11) 0.052(3) 0.086(4) 0.025(3) -0.022(5) -0.052(5) F18 0.241(16) 0.27(2) 0.31(2) 0.26(2) -0.104(16) -0.052(15) F19 0.167(7) 0.126(6) 0.052(3) 0.002(3) -0.043(4) -0.024(5) F20 0.156(8) 0.248(15) 0.090(5) -0.057(7) -0.050(5) -0.027(9) F21 0.272(14) 0.131(7) 0.068(4) 0.027(4) -0.080(6) -0.012(8) F22 0.40(4) 0.53(5) 0.117(9) -0.011(17) 0.012(14) -0.39(4) F23 0.143(7) 0.183(9) 0.070(4) 0.052(5) -0.003(4) -0.027(6) F24 0.119(9) 0.60(6) 0.153(12) 0.16(2) 0.026(8) 0.061(18) Mo 0.0896(5) 0.0398(3) 0.0584(4) 0.0095(2) -0.0377(3) -0.0257(3) B1 0.095(6) 0.046(4) 0.033(3) 0.013(3) -0.024(3) -0.020(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; 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 C1 C2 1.363(16) . ? C1 Mo 2.333(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.41(2) . ? C2 C4 1.529(14) . ? C2 Mo 2.225(8) . ? C3 Mo 2.272(11) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 O1 1.412(10) . ? C5 C40 1.524(9) . ? C5 C51 1.538(10) . ? C5 C31 1.548(8) . ? C10 O10 1.161(11) . ? C10 Mo 1.943(8) . ? C20 O20 1.193(17) . ? C20 Mo 1.935(14) . ? C31 N1 1.361(9) . ? C31 C32 1.362(10) . ? C32 C33 1.404(9) . ? C32 H32 0.9300 . ? C33 C34 1.370(12) . ? C33 H33 0.9300 . ? C34 C35 1.374(12) . ? C34 H34 0.9300 . ? C35 N1 1.344(8) . ? C35 H35 0.9300 . ? C40 C45 1.366(10) . ? C40 C41 1.396(9) . ? C41 C42 1.382(10) . ? C41 H41 0.9300 . ? C42 C43 1.394(14) . ? C42 H42 0.9300 . ? C43 C44 1.399(13) . ? C43 H43 0.9300 . ? C44 C45 1.396(11) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C51 N3 1.357(9) . ? C51 C52 1.374(13) . ? C52 C53 1.399(12) . ? C52 H52 0.9300 . ? C53 C54 1.393(15) . ? C53 H53 0.9300 . ? C54 C55 1.335(17) . ? C54 H54 0.9300 . ? C55 N3 1.350(11) . ? C55 H55 0.9300 . ? C60 C61 1.397(9) . ? C60 C65 1.408(10) . ? C60 B1 1.644(8) . ? C61 C62 1.402(8) . ? C61 H61 0.9300 . ? C62 C63 1.378(10) . ? C62 C66 1.505(10) . ? C63 C64 1.406(10) . ? C63 H63 0.9300 . ? C64 C65 1.373(8) . ? C64 C67 1.507(10) . ? C65 H65 0.9300 . ? C66 F1 1.299(12) . ? C66 F3 1.331(8) . ? C66 F2 1.353(11) . ? C67 F6 1.250(10) . ? C67 F4 1.276(18) . ? C67 F5 1.313(11) . ? C70 C75 1.357(12) . ? C70 C71 1.399(11) . ? C70 B1 1.636(13) . ? C71 C72 1.368(14) . ? C71 H71 0.9300 . ? C72 C73 1.384(14) . ? C72 C76 1.496(14) . ? C73 C74 1.410(16) . ? C73 H73 0.9300 . ? C74 C75 1.366(17) . ? C74 C77 1.58(2) . ? C75 H75 0.9300 . ? C76 F9 1.328(18) . ? C76 F7 1.333(16) . ? C76 F8 1.338(11) . ? C77 F11 1.18(3) . ? C77 F12 1.34(2) . ? C77 F10 1.37(3) . ? C80 C81 1.380(11) . ? C80 C85 1.410(8) . ? C80 B1 1.643(11) . ? C81 C82 1.386(11) . ? C81 H81 0.9300 . ? C82 C83 1.379(10) . ? C82 C86 1.496(12) . ? C83 C84 1.366(13) . ? C83 H83 0.9300 . ? C84 C85 1.381(12) . ? C84 C87 1.501(10) . ? C85 H85 0.9300 . ? C86 F13 1.323(10) . ? C86 F15 1.337(10) . ? C86 F14 1.354(15) . ? C87 F16 1.214(18) . ? C87 F17 1.285(14) . ? C87 F18 1.29(3) . ? C90 C95 1.374(14) . ? C90 C91 1.408(9) . ? C90 B1 1.648(12) . ? C91 C92 1.369(15) . ? C91 H91 0.9300 . ? C92 C93 1.365(18) . ? C92 C96 1.518(13) . ? C93 C94 1.396(16) . ? C93 H93 0.9300 . ? C94 C95 1.364(18) . ? C94 C97 1.53(2) . ? C95 H95 0.9300 . ? C96 F20 1.28(2) . ? C96 F19 1.332(17) . ? C96 F21 1.38(2) . ? C97 F24 1.24(3) . ? C97 F22 1.27(4) . ? C97 F23 1.35(3) . ? N1 Mo 2.238(5) . ? N3 Mo 2.262(7) . ? O1 Mo 2.192(4) . ? O1 H1 0.89(8) . ? O100 H500 1.01(5) . ? O100 H600 0.99(6) . ? 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 C1 Mo 68.3(4) . . ? C2 C1 H1A 116.8 . . ? Mo C1 H1A 116.8 . . ? C2 C1 H1B 116.8 . . ? Mo C1 H1B 116.8 . . ? H1A C1 H1B 113.9 . . ? C1 C2 C3 116.3(10) . . ? C1 C2 C4 120.9(12) . . ? C3 C2 C4 122.6(11) . . ? C1 C2 Mo 77.0(5) . . ? C3 C2 Mo 73.5(5) . . ? C4 C2 Mo 115.9(6) . . ? C2 C3 Mo 69.9(6) . . ? C2 C3 H3A 116.7 . . ? Mo C3 H3A 116.7 . . ? C2 C3 H3B 116.7 . . ? Mo C3 H3B 116.7 . . ? H3A C3 H3B 113.7 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O1 C5 C40 108.4(6) . . ? O1 C5 C51 105.9(5) . . ? C40 C5 C51 115.4(6) . . ? O1 C5 C31 108.3(5) . . ? C40 C5 C31 116.6(5) . . ? C51 C5 C31 101.5(5) . . ? O10 C10 Mo 178.1(12) . . ? O20 C20 Mo 178.9(11) . . ? N1 C31 C32 122.4(6) . . ? N1 C31 C5 111.3(5) . . ? C32 C31 C5 126.2(6) . . ? C31 C32 C33 118.6(7) . . ? C31 C32 H32 120.7 . . ? C33 C32 H32 120.7 . . ? C34 C33 C32 119.3(7) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C33 C34 C35 118.8(6) . . ? C33 C34 H34 120.6 . . ? C35 C34 H34 120.6 . . ? N1 C35 C34 122.8(7) . . ? N1 C35 H35 118.6 . . ? C34 C35 H35 118.6 . . ? C45 C40 C41 118.5(6) . . ? C45 C40 C5 121.6(6) . . ? C41 C40 C5 119.3(5) . . ? C42 C41 C40 121.3(7) . . ? C42 C41 H41 119.3 . . ? C40 C41 H41 119.3 . . ? C41 C42 C43 119.4(7) . . ? C41 C42 H42 120.3 . . ? C43 C42 H42 120.3 . . ? C42 C43 C44 120.0(7) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C45 C44 C43 118.7(7) . . ? C45 C44 H44 120.7 . . ? C43 C44 H44 120.7 . . ? C40 C45 C44 122.1(7) . . ? C40 C45 H45 119.0 . . ? C44 C45 H45 119.0 . . ? N3 C51 C52 122.8(7) . . ? N3 C51 C5 113.1(7) . . ? C52 C51 C5 123.9(6) . . ? C51 C52 C53 118.9(8) . . ? C51 C52 H52 120.5 . . ? C53 C52 H52 120.5 . . ? C54 C53 C52 117.9(9) . . ? C54 C53 H53 121.0 . . ? C52 C53 H53 121.0 . . ? C55 C54 C53 119.3(8) . . ? C55 C54 H54 120.4 . . ? C53 C54 H54 120.4 . . ? C54 C55 N3 124.7(8) . . ? C54 C55 H55 117.7 . . ? N3 C55 H55 117.7 . . ? C61 C60 C65 115.4(5) . . ? C61 C60 B1 124.0(6) . . ? C65 C60 B1 120.4(6) . . ? C60 C61 C62 122.7(6) . . ? C60 C61 H61 118.6 . . ? C62 C61 H61 118.6 . . ? C63 C62 C61 120.5(6) . . ? C63 C62 C66 121.0(5) . . ? C61 C62 C66 118.4(6) . . ? C62 C63 C64 117.6(5) . . ? C62 C63 H63 121.2 . . ? C64 C63 H63 121.2 . . ? C65 C64 C63 121.5(6) . . ? C65 C64 C67 118.9(6) . . ? C63 C64 C67 119.6(5) . . ? C64 C65 C60 122.2(6) . . ? C64 C65 H65 118.9 . . ? C60 C65 H65 118.9 . . ? F1 C66 F3 108.3(7) . . ? F1 C66 F2 106.6(7) . . ? F3 C66 F2 105.0(7) . . ? F1 C66 C62 112.7(7) . . ? F3 C66 C62 112.4(6) . . ? F2 C66 C62 111.4(6) . . ? F6 C67 F4 106.6(14) . . ? F6 C67 F5 107.4(9) . . ? F4 C67 F5 101.6(12) . . ? F6 C67 C64 115.1(7) . . ? F4 C67 C64 112.9(7) . . ? F5 C67 C64 112.2(7) . . ? C75 C70 C71 116.8(8) . . ? C75 C70 B1 120.8(7) . . ? C71 C70 B1 122.3(7) . . ? C72 C71 C70 123.0(8) . . ? C72 C71 H71 118.5 . . ? C70 C71 H71 118.5 . . ? C71 C72 C73 120.3(9) . . ? C71 C72 C76 120.1(8) . . ? C73 C72 C76 119.6(10) . . ? C72 C73 C74 116.1(10) . . ? C72 C73 H73 122.0 . . ? C74 C73 H73 122.0 . . ? C75 C74 C73 122.6(10) . . ? C75 C74 C77 117.9(10) . . ? C73 C74 C77 119.5(12) . . ? C70 C75 C74 121.2(8) . . ? C70 C75 H75 119.4 . . ? C74 C75 H75 119.4 . . ? F9 C76 F7 107.5(10) . . ? F9 C76 F8 106.1(10) . . ? F7 C76 F8 105.8(10) . . ? F9 C76 C72 113.2(11) . . ? F7 C76 C72 112.1(10) . . ? F8 C76 C72 111.5(7) . . ? F11 C77 F12 114.2(19) . . ? F11 C77 F10 103.1(17) . . ? F12 C77 F10 108.1(18) . . ? F11 C77 C74 115.4(17) . . ? F12 C77 C74 108.8(15) . . ? F10 C77 C74 106.6(15) . . ? C81 C80 C85 114.6(7) . . ? C81 C80 B1 125.8(5) . . ? C85 C80 B1 119.6(6) . . ? C80 C81 C82 123.3(6) . . ? C80 C81 H81 118.4 . . ? C82 C81 H81 118.4 . . ? C83 C82 C81 120.9(8) . . ? C83 C82 C86 119.7(7) . . ? C81 C82 C86 119.4(6) . . ? C84 C83 C82 117.4(7) . . ? C84 C83 H83 121.3 . . ? C82 C83 H83 121.3 . . ? C83 C84 C85 121.9(6) . . ? C83 C84 C87 118.0(8) . . ? C85 C84 C87 120.1(8) . . ? C84 C85 C80 122.0(7) . . ? C84 C85 H85 119.0 . . ? C80 C85 H85 119.0 . . ? F13 C86 F15 108.1(8) . . ? F13 C86 F14 106.4(9) . . ? F15 C86 F14 104.4(7) . . ? F13 C86 C82 113.4(7) . . ? F15 C86 C82 112.4(8) . . ? F14 C86 C82 111.5(8) . . ? F16 C87 F17 107.5(13) . . ? F16 C87 F18 104.0(17) . . ? F17 C87 F18 99.9(16) . . ? F16 C87 C84 115.7(11) . . ? F17 C87 C84 115.7(9) . . ? F18 C87 C84 112.4(14) . . ? C95 C90 C91 116.2(8) . . ? C95 C90 B1 121.6(6) . . ? C91 C90 B1 122.0(8) . . ? C92 C91 C90 120.3(9) . . ? C92 C91 H91 119.8 . . ? C90 C91 H91 119.8 . . ? C93 C92 C91 122.9(8) . . ? C93 C92 C96 116.6(10) . . ? C91 C92 C96 120.5(10) . . ? C92 C93 C94 116.8(11) . . ? C92 C93 H93 121.6 . . ? C94 C93 H93 121.6 . . ? C95 C94 C93 120.6(11) . . ? C95 C94 C97 121.3(11) . . ? C93 C94 C97 118.0(13) . . ? C94 C95 C90 122.9(8) . . ? C94 C95 H95 118.5 . . ? C90 C95 H95 118.5 . . ? F20 C96 F19 101.0(13) . . ? F20 C96 F21 102.3(12) . . ? F19 C96 F21 115.7(11) . . ? F20 C96 C92 115.1(12) . . ? F19 C96 C92 112.8(10) . . ? F21 C96 C92 109.5(12) . . ? F24 C97 F22 110(2) . . ? F24 C97 F23 103(3) . . ? F22 C97 F23 108.3(17) . . ? F24 C97 C94 112.8(18) . . ? F22 C97 C94 112(3) . . ? F23 C97 C94 111.6(18) . . ? C35 N1 C31 117.9(6) . . ? C35 N1 Mo 125.6(5) . . ? C31 N1 Mo 116.3(4) . . ? C55 N3 C51 116.5(8) . . ? C55 N3 Mo 128.7(6) . . ? C51 N3 Mo 114.5(5) . . ? C5 O1 Mo 108.9(4) . . ? C5 O1 H1 112(7) . . ? Mo O1 H1 130(7) . . ? H500 O100 H600 118(8) . . ? C20 Mo C10 81.0(5) . . ? C20 Mo O1 103.8(4) . . ? C10 Mo O1 168.2(4) . . ? C20 Mo C2 105.3(5) . . ? C10 Mo C2 101.4(4) . . ? O1 Mo C2 87.8(3) . . ? C20 Mo N1 86.1(3) . . ? C10 Mo N1 98.0(3) . . ? O1 Mo N1 71.87(18) . . ? C2 Mo N1 158.7(3) . . ? C20 Mo N3 164.3(3) . . ? C10 Mo N3 101.7(4) . . ? O1 Mo N3 70.8(2) . . ? C2 Mo N3 89.4(4) . . ? N1 Mo N3 78.2(2) . . ? C20 Mo C3 71.1(5) . . ? C10 Mo C3 108.1(4) . . ? O1 Mo C3 83.7(3) . . ? C2 Mo C3 36.6(5) . . ? N1 Mo C3 141.5(4) . . ? N3 Mo C3 121.6(4) . . ? C20 Mo C1 109.1(4) . . ? C10 Mo C1 68.4(3) . . ? O1 Mo C1 118.9(2) . . ? C2 Mo C1 34.7(4) . . ? N1 Mo C1 156.8(4) . . ? N3 Mo C1 86.1(4) . . ? C3 Mo C1 61.6(5) . . ? C70 B1 C80 112.5(6) . . ? C70 B1 C60 104.4(6) . . ? C80 B1 C60 112.1(5) . . ? C70 B1 C90 112.4(6) . . ? C80 B1 C90 104.8(7) . . ? C60 B1 C90 110.7(6) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 73.94 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 1.883 _refine_diff_density_min -0.992 _refine_diff_density_rms 0.169 #===END