# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address Henderickx,Huub ; DSM Research P.O.Box 18 6160 MD Geleen The Netherlands ; 'Kwakkenboes, Gerard' ; DSM Research P.O.Box 18 6160 MD Geleen The Netherlands ; 'Peters, Alexander' ; DSM Research P.O.Box 18 6160 MD Geleen The Netherlands ; 'van der Spoel, Jan' ; DSM Research P.O.Box 18 6160 MD Geleen The Netherlands ; 'de Vries, Koen' ; DSM Research P.O.Box 18 6160 MD Geleen The Netherlands ; _publ_contact_author_name 'Dr Alexander Peters' _publ_contact_author_address ; Industrial Chemicals dsm research P.O. Box 18 Geleen 6160MD NETHERLANDS ; _publ_contact_author_email alexander.peters@dsm.com _publ_contact_author_fax '031 46 47 605089' _publ_contact_author_phone ? _publ_requested_coeditor_name ? _publ_requested_journal 'Chemical Communications' _publ_section_title ; Direct acid amide formation from a molybdenum nitrido species ; data_dsm01 _database_code_CSD 207154 #============================================================================ _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H27 F9 Mo N2 O6' _chemical_formula_sum 'C26 H27 F9 Mo N2 O6' _chemical_formula_weight 730.44 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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 10.0930(5) _cell_length_b 19.1220(10) _cell_length_c 15.8531(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.2300(10) _cell_angle_gamma 90.00 _cell_volume 3011.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.611 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 0.533 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8948 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 190(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28341 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 32.02 _reflns_number_total 10079 _reflns_number_gt 8103 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^ > 2sigma(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^)+(0.0333P)^2^+1.5815P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10079 _refine_ls_number_parameters 533 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0802 _refine_ls_wR_factor_gt 0.0713 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.016 _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 0.256238(12) 0.265046(6) -0.000357(8) 0.01781(4) Uani 1 1 d . A . F1 F -0.20863(12) 0.26230(8) -0.09070(11) 0.0531(4) Uani 1 1 d . . . F2 F -0.15608(12) 0.33903(7) -0.17820(8) 0.0420(3) Uani 1 1 d . . . F3 F -0.14503(13) 0.22986(7) -0.20696(10) 0.0554(4) Uani 1 1 d . . . F4 F 0.3248(9) 0.4572(2) -0.1626(4) 0.076(2) Uani 0.559(11) 1 d PD A 1 F5 F 0.5238(5) 0.4340(4) -0.1802(4) 0.078(2) Uani 0.559(11) 1 d PD A 1 F6 F 0.3554(7) 0.3820(3) -0.2511(3) 0.0671(17) Uani 0.559(11) 1 d PD A 1 F4A F 0.3271(9) 0.3986(6) -0.2370(6) 0.109(4) Uani 0.441(11) 1 d PD A 2 F5A F 0.4288(13) 0.46156(19) -0.1327(4) 0.086(3) Uani 0.441(11) 1 d PD A 2 F6A F 0.5347(6) 0.3972(5) -0.2032(4) 0.0716(18) Uani 0.441(11) 1 d PD A 2 F7 F -0.09107(13) 0.16621(8) 0.12573(10) 0.0535(3) Uani 1 1 d . . . F8 F 0.07453(14) 0.18532(9) 0.22852(8) 0.0555(4) Uani 1 1 d . . . F9 F 0.02573(17) 0.08075(8) 0.18627(12) 0.0679(5) Uani 1 1 d . . . C1 C 0.02085(15) 0.27421(9) -0.09477(11) 0.0239(3) Uani 1 1 d . . . C2 C -0.12432(17) 0.27639(10) -0.14416(13) 0.0327(4) Uani 1 1 d . . . C3 C 0.41821(17) 0.34622(9) -0.10533(11) 0.0276(3) Uani 1 1 d D A . C4 C 0.4142(2) 0.40378(12) -0.17350(14) 0.0428(5) Uani 1 1 d D . . C5 C 0.1285(2) 0.15291(9) 0.09438(12) 0.0310(4) Uani 1 1 d . A . C6 C 0.0327(2) 0.14564(11) 0.15958(13) 0.0383(4) Uani 1 1 d . . . C7 C 0.48017(17) 0.30557(9) 0.16046(11) 0.0267(3) Uani 1 1 d . A . C8 C 0.5621(2) 0.24469(14) 0.13565(15) 0.0445(6) Uani 1 1 d . . . C9 C 0.4378(2) 0.29126(14) 0.24673(13) 0.0402(4) Uani 1 1 d . . . C10 C 0.5621(2) 0.37308(12) 0.16569(16) 0.0425(5) Uani 1 1 d . . . C11 C 0.26862(15) 0.37447(8) 0.10559(10) 0.0213(3) Uani 1 1 d . A . C12 C 0.28118(16) 0.43524(8) 0.05945(10) 0.0228(3) Uani 1 1 d . . . C13 C 0.19627(16) 0.49193(8) 0.06506(11) 0.0248(3) Uani 1 1 d . . . C14 C 0.10026(17) 0.48594(9) 0.11793(12) 0.0281(3) Uani 1 1 d . . . C15 C 0.08663(17) 0.42517(9) 0.16454(12) 0.0275(3) Uani 1 1 d . . . C16 C 0.17144(17) 0.36878(9) 0.15754(11) 0.0255(3) Uani 1 1 d . . . C17 C 0.2084(2) 0.55735(10) 0.01453(14) 0.0326(4) Uani 1 1 d . . . C18 C -0.0198(2) 0.41934(13) 0.21973(18) 0.0415(5) Uani 1 1 d . . . C19 C 0.42014(15) 0.13954(8) -0.04656(10) 0.0212(3) Uani 1 1 d . A . C20 C 0.33702(17) 0.08495(9) -0.08240(11) 0.0247(3) Uani 1 1 d . . . C21 C 0.39366(18) 0.02712(9) -0.11598(11) 0.0263(3) Uani 1 1 d . . . C22 C 0.53283(18) 0.02558(9) -0.11224(11) 0.0283(3) Uani 1 1 d . . . C23 C 0.61658(17) 0.08013(9) -0.07736(11) 0.0270(3) Uani 1 1 d . . . C24 C 0.55963(16) 0.13798(9) -0.04425(11) 0.0246(3) Uani 1 1 d . . . C25 C 0.3059(2) -0.03190(11) -0.15555(16) 0.0382(4) Uani 1 1 d . . . C26 C 0.7660(2) 0.07656(13) -0.07620(17) 0.0408(5) Uani 1 1 d . . . O1 O 0.05810(11) 0.32191(6) -0.04214(8) 0.0250(2) Uani 1 1 d . . . O2 O 0.09521(11) 0.22366(6) -0.10534(8) 0.0257(2) Uani 1 1 d . . . O3 O 0.29845(11) 0.32824(6) -0.09580(7) 0.0240(2) Uani 1 1 d . . . O4 O 0.52460(14) 0.32563(9) -0.06751(11) 0.0460(4) Uani 1 1 d . . . O5 O 0.13868(12) 0.21740(6) 0.07385(8) 0.0281(2) Uani 1 1 d . . . O6 O 0.1804(3) 0.10298(8) 0.06995(14) 0.0743(7) Uani 1 1 d . . . N1 N 0.35382(13) 0.31477(7) 0.09422(8) 0.0209(2) Uani 1 1 d . . . N2 N 0.36148(13) 0.19750(7) -0.01450(8) 0.0207(2) Uani 1 1 d . . . H8A H 0.592(3) 0.2551(14) 0.0817(19) 0.049(7) Uiso 1 1 d . . . H8B H 0.505(3) 0.2025(14) 0.1278(17) 0.049(7) Uiso 1 1 d . . . H8C H 0.645(3) 0.2408(14) 0.1778(19) 0.055(8) Uiso 1 1 d . . . H9A H 0.510(3) 0.2799(14) 0.2858(17) 0.047(7) Uiso 1 1 d . . . H9C H 0.379(3) 0.2553(15) 0.2462(18) 0.053(8) Uiso 1 1 d . . . H9B H 0.396(2) 0.3284(14) 0.2703(16) 0.041(6) Uiso 1 1 d . . . H10A H 0.645(2) 0.3666(12) 0.2061(15) 0.039(6) Uiso 1 1 d . . . H10B H 0.511(3) 0.4122(14) 0.1831(17) 0.052(7) Uiso 1 1 d . . . H10C H 0.586(3) 0.3836(16) 0.109(2) 0.070(9) Uiso 1 1 d . . . H12 H 0.347(2) 0.4393(10) 0.0233(13) 0.024(5) Uiso 1 1 d . . . H14 H 0.042(2) 0.5243(12) 0.1207(15) 0.037(6) Uiso 1 1 d . . . H16 H 0.164(2) 0.3289(12) 0.1872(14) 0.034(6) Uiso 1 1 d . . . H17A H 0.228(3) 0.5474(14) -0.0450(18) 0.053(7) Uiso 1 1 d . . . H17B H 0.125(3) 0.5826(13) 0.0025(16) 0.047(7) Uiso 1 1 d . . . H17C H 0.275(3) 0.5858(14) 0.0442(17) 0.046(7) Uiso 1 1 d . . . H18A H -0.064(3) 0.458(2) 0.224(2) 0.086(11) Uiso 1 1 d . . . H18B H 0.010(3) 0.4033(18) 0.271(2) 0.078(11) Uiso 1 1 d . . . H18C H -0.088(3) 0.3937(18) 0.194(2) 0.075(10) Uiso 1 1 d . . . H20 H 0.245(2) 0.0878(11) -0.0822(13) 0.026(5) Uiso 1 1 d . . . H22 H 0.572(2) -0.0127(12) -0.1308(14) 0.033(6) Uiso 1 1 d . . . H24 H 0.612(2) 0.1759(11) -0.0232(13) 0.025(5) Uiso 1 1 d . . . H25A H 0.342(3) -0.0752(18) -0.140(2) 0.071(9) Uiso 1 1 d . . . H25B H 0.286(3) -0.0275(16) -0.212(2) 0.068(9) Uiso 1 1 d . . . H25C H 0.221(4) -0.030(2) -0.141(3) 0.106(13) Uiso 1 1 d . . . H26A H 0.814(3) 0.1149(17) -0.044(2) 0.072(9) Uiso 1 1 d . . . H26B H 0.799(4) 0.036(2) -0.060(2) 0.093(12) Uiso 1 1 d . . . H26C H 0.784(3) 0.0782(19) -0.131(2) 0.085(11) 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 Mo1 0.01725(6) 0.01536(6) 0.02082(6) -0.00084(4) 0.00334(4) 0.00065(4) F1 0.0227(5) 0.0623(9) 0.0762(10) 0.0056(7) 0.0136(6) -0.0056(5) F2 0.0338(6) 0.0387(6) 0.0489(7) 0.0012(5) -0.0058(5) 0.0108(5) F3 0.0354(6) 0.0522(8) 0.0680(10) -0.0300(7) -0.0199(6) 0.0084(6) F4 0.120(5) 0.0394(17) 0.084(3) 0.0293(18) 0.057(3) 0.032(2) F5 0.056(2) 0.094(4) 0.080(3) 0.046(3) -0.0030(19) -0.042(3) F6 0.117(5) 0.0472(19) 0.0317(17) 0.0049(15) -0.001(2) -0.003(2) F4A 0.061(3) 0.138(8) 0.105(6) 0.094(5) -0.044(4) -0.053(5) F5A 0.151(8) 0.0187(15) 0.099(4) 0.0125(18) 0.053(5) -0.004(3) F6A 0.075(3) 0.078(4) 0.074(3) 0.026(3) 0.049(3) -0.011(3) F7 0.0346(6) 0.0673(9) 0.0586(8) 0.0087(7) 0.0083(6) -0.0101(6) F8 0.0535(8) 0.0833(11) 0.0336(6) -0.0093(7) 0.0185(6) -0.0179(7) F9 0.0737(10) 0.0514(9) 0.0847(12) 0.0300(8) 0.0305(9) -0.0142(8) C1 0.0180(6) 0.0241(7) 0.0292(8) -0.0011(6) 0.0030(6) -0.0013(5) C2 0.0207(7) 0.0319(9) 0.0429(10) -0.0067(8) -0.0016(7) 0.0021(6) C3 0.0290(8) 0.0278(8) 0.0272(8) -0.0037(6) 0.0084(6) -0.0075(6) C4 0.0517(12) 0.0419(11) 0.0380(11) 0.0055(9) 0.0168(9) -0.0142(10) C5 0.0431(10) 0.0233(8) 0.0283(8) 0.0001(6) 0.0107(7) -0.0062(7) C6 0.0373(10) 0.0408(11) 0.0380(10) 0.0075(8) 0.0095(8) -0.0115(8) C7 0.0266(7) 0.0276(8) 0.0232(7) -0.0036(6) -0.0032(6) 0.0031(6) C8 0.0379(11) 0.0510(13) 0.0375(11) -0.0152(10) -0.0130(9) 0.0211(10) C9 0.0454(11) 0.0474(12) 0.0254(9) 0.0051(9) -0.0005(8) 0.0074(10) C10 0.0329(10) 0.0407(11) 0.0481(12) 0.0005(10) -0.0086(9) -0.0071(9) C11 0.0235(7) 0.0179(6) 0.0221(7) -0.0038(5) 0.0030(5) 0.0002(5) C12 0.0244(7) 0.0199(7) 0.0243(7) -0.0028(6) 0.0052(6) -0.0016(5) C13 0.0260(7) 0.0182(7) 0.0291(8) -0.0023(6) 0.0018(6) -0.0009(6) C14 0.0257(7) 0.0205(7) 0.0381(9) -0.0055(7) 0.0060(7) 0.0016(6) C15 0.0262(7) 0.0245(8) 0.0334(8) -0.0061(7) 0.0093(6) -0.0009(6) C16 0.0297(8) 0.0208(7) 0.0270(8) -0.0018(6) 0.0074(6) -0.0014(6) C17 0.0335(9) 0.0213(8) 0.0426(10) 0.0037(7) 0.0053(8) 0.0004(7) C18 0.0401(11) 0.0380(11) 0.0530(13) -0.0018(10) 0.0260(10) 0.0029(9) C19 0.0243(7) 0.0189(6) 0.0204(7) -0.0005(5) 0.0039(5) 0.0032(5) C20 0.0257(7) 0.0239(7) 0.0247(7) -0.0023(6) 0.0051(6) 0.0006(6) C21 0.0351(8) 0.0206(7) 0.0237(7) -0.0025(6) 0.0069(6) -0.0007(6) C22 0.0362(9) 0.0222(7) 0.0280(8) -0.0023(6) 0.0099(7) 0.0065(7) C23 0.0277(8) 0.0255(8) 0.0291(8) 0.0003(6) 0.0081(6) 0.0065(6) C24 0.0254(7) 0.0213(7) 0.0273(8) -0.0020(6) 0.0050(6) 0.0018(6) C25 0.0441(11) 0.0286(9) 0.0420(11) -0.0119(8) 0.0082(9) -0.0062(8) C26 0.0301(9) 0.0389(11) 0.0561(13) -0.0062(10) 0.0147(9) 0.0077(8) O1 0.0206(5) 0.0221(5) 0.0317(6) -0.0043(5) 0.0029(4) 0.0016(4) O2 0.0212(5) 0.0234(5) 0.0312(6) -0.0058(5) 0.0012(4) 0.0017(4) O3 0.0231(5) 0.0242(5) 0.0249(5) 0.0029(4) 0.0051(4) -0.0011(4) O4 0.0249(6) 0.0592(10) 0.0539(9) 0.0104(8) 0.0068(6) -0.0048(6) O5 0.0302(6) 0.0223(5) 0.0348(7) 0.0022(5) 0.0141(5) -0.0004(5) O6 0.137(2) 0.0249(7) 0.0802(14) 0.0048(8) 0.0704(14) 0.0083(10) N1 0.0223(6) 0.0183(6) 0.0219(6) 0.0004(5) 0.0035(5) 0.0011(5) N2 0.0203(6) 0.0195(6) 0.0222(6) -0.0013(5) 0.0035(5) 0.0009(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 N2 1.7122(13) . ? Mo1 N1 1.8967(13) . ? Mo1 O5 2.0292(12) . ? Mo1 O3 2.0395(11) . ? Mo1 O2 2.2532(12) . ? Mo1 O1 2.2693(11) . ? Mo1 C1 2.5791(16) . ? F1 C2 1.331(2) . ? F2 C2 1.329(2) . ? F3 C2 1.324(2) . ? F4 C4 1.394(4) . ? F5 C4 1.269(4) . ? F6 C4 1.334(5) . ? F4A C4 1.218(6) . ? F5A C4 1.275(5) . ? F6A C4 1.385(5) . ? F7 C6 1.328(2) . ? F8 C6 1.336(3) . ? F9 C6 1.317(2) . ? C1 O1 1.248(2) . ? C1 O2 1.2532(19) . ? C1 C2 1.534(2) . ? C3 O4 1.200(2) . ? C3 O3 1.2911(19) . ? C3 C4 1.538(3) . ? C5 O6 1.186(2) . ? C5 O5 1.284(2) . ? C5 C6 1.542(3) . ? C7 N1 1.511(2) . ? C7 C8 1.520(3) . ? C7 C10 1.528(3) . ? C7 C9 1.528(3) . ? C8 H8A 0.98(3) . ? C8 H8B 0.99(3) . ? C8 H8C 0.98(3) . ? C9 H9A 0.89(3) . ? C9 H9C 0.91(3) . ? C9 H9B 0.94(3) . ? C10 H10A 0.96(2) . ? C10 H10B 0.98(3) . ? C10 H10C 0.99(3) . ? C11 C12 1.391(2) . ? C11 C16 1.393(2) . ? C11 N1 1.4595(19) . ? C12 C13 1.394(2) . ? C12 H12 0.95(2) . ? C13 C14 1.394(2) . ? C13 C17 1.502(2) . ? C14 C15 1.397(3) . ? C14 H14 0.95(2) . ? C15 C16 1.393(2) . ? C15 C18 1.505(3) . ? C16 H16 0.91(2) . ? C17 H17A 1.01(3) . ? C17 H17B 0.96(3) . ? C17 H17C 0.93(3) . ? C18 H18A 0.88(4) . ? C18 H18B 0.87(4) . ? C18 H18C 0.88(3) . ? C19 N2 1.3943(19) . ? C19 C20 1.395(2) . ? C19 C24 1.402(2) . ? C20 C21 1.393(2) . ? C20 H20 0.93(2) . ? C21 C22 1.396(2) . ? C21 C25 1.502(3) . ? C22 C23 1.394(3) . ? C22 H22 0.91(2) . ? C23 C24 1.392(2) . ? C23 C26 1.506(3) . ? C24 H24 0.92(2) . ? C25 H25A 0.92(3) . ? C25 H25B 0.89(3) . ? C25 H25C 0.93(4) . ? C26 H26A 0.97(3) . ? C26 H26B 0.86(4) . ? C26 H26C 0.92(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 N2 Mo1 N1 103.57(6) . . ? N2 Mo1 O5 100.22(6) . . ? N1 Mo1 O5 92.40(5) . . ? N2 Mo1 O3 97.68(5) . . ? N1 Mo1 O3 98.15(5) . . ? O5 Mo1 O3 156.46(5) . . ? N2 Mo1 O2 91.21(5) . . ? N1 Mo1 O2 164.82(5) . . ? O5 Mo1 O2 81.44(5) . . ? O3 Mo1 O2 83.02(5) . . ? N2 Mo1 O1 149.12(5) . . ? N1 Mo1 O1 107.31(5) . . ? O5 Mo1 O1 78.97(5) . . ? O3 Mo1 O1 77.82(4) . . ? O2 Mo1 O1 58.00(4) . . ? N2 Mo1 C1 120.28(6) . . ? N1 Mo1 C1 136.06(5) . . ? O5 Mo1 C1 78.10(5) . . ? O3 Mo1 C1 79.72(5) . . ? O2 Mo1 C1 29.07(5) . . ? O1 Mo1 C1 28.94(5) . . ? O1 C1 O2 122.46(15) . . ? O1 C1 C2 117.92(14) . . ? O2 C1 C2 119.54(15) . . ? O1 C1 Mo1 61.62(8) . . ? O2 C1 Mo1 60.88(8) . . ? C2 C1 Mo1 174.71(13) . . ? F3 C2 F2 107.81(17) . . ? F3 C2 F1 108.03(17) . . ? F2 C2 F1 107.79(15) . . ? F3 C2 C1 111.99(15) . . ? F2 C2 C1 111.79(15) . . ? F1 C2 C1 109.27(16) . . ? O4 C3 O3 128.89(17) . . ? O4 C3 C4 119.70(17) . . ? O3 C3 C4 111.37(16) . . ? F4A C4 F5 118.7(4) . . ? F4A C4 F5A 119.5(5) . . ? F5 C4 F5A 67.9(3) . . ? F4A C4 F6 22.2(8) . . ? F5 C4 F6 108.5(4) . . ? F5A C4 F6 137.0(5) . . ? F4A C4 F6A 105.1(6) . . ? F5 C4 F6A 35.2(3) . . ? F5A C4 F6A 102.8(4) . . ? F6 C4 F6A 86.1(4) . . ? F4A C4 F4 77.0(6) . . ? F5 C4 F4 105.6(3) . . ? F5A C4 F4 47.3(3) . . ? F6 C4 F4 98.8(4) . . ? F6A C4 F4 137.4(3) . . ? F4A C4 C3 116.6(4) . . ? F5 C4 C3 118.1(3) . . ? F5A C4 C3 106.1(3) . . ? F6 C4 C3 112.1(3) . . ? F6A C4 C3 105.0(3) . . ? F4 C4 C3 111.9(2) . . ? O6 C5 O5 129.08(18) . . ? O6 C5 C6 120.79(18) . . ? O5 C5 C6 110.13(16) . . ? F9 C6 F7 108.00(17) . . ? F9 C6 F8 107.42(18) . . ? F7 C6 F8 107.47(19) . . ? F9 C6 C5 112.07(19) . . ? F7 C6 C5 111.06(17) . . ? F8 C6 C5 110.62(15) . . ? N1 C7 C8 109.88(14) . . ? N1 C7 C10 108.74(14) . . ? C8 C7 C10 110.31(18) . . ? N1 C7 C9 107.89(14) . . ? C8 C7 C9 110.24(18) . . ? C10 C7 C9 109.73(17) . . ? C7 C8 H8A 109.7(16) . . ? C7 C8 H8B 108.9(15) . . ? H8A C8 H8B 109(2) . . ? C7 C8 H8C 108.7(16) . . ? H8A C8 H8C 105(2) . . ? H8B C8 H8C 116(2) . . ? C7 C9 H9A 110.0(17) . . ? C7 C9 H9C 114.4(18) . . ? H9A C9 H9C 106(2) . . ? C7 C9 H9B 116.0(15) . . ? H9A C9 H9B 106(2) . . ? H9C C9 H9B 104(2) . . ? C7 C10 H10A 108.8(14) . . ? C7 C10 H10B 110.8(15) . . ? H10A C10 H10B 110(2) . . ? C7 C10 H10C 109.8(18) . . ? H10A C10 H10C 108(2) . . ? H10B C10 H10C 109(2) . . ? C12 C11 C16 121.06(15) . . ? C12 C11 N1 118.54(14) . . ? C16 C11 N1 120.29(14) . . ? C11 C12 C13 120.10(15) . . ? C11 C12 H12 121.5(12) . . ? C13 C12 H12 118.4(12) . . ? C14 C13 C12 118.38(15) . . ? C14 C13 C17 121.36(16) . . ? C12 C13 C17 120.26(16) . . ? C13 C14 C15 122.05(15) . . ? C13 C14 H14 117.9(14) . . ? C15 C14 H14 120.0(14) . . ? C16 C15 C14 118.82(15) . . ? C16 C15 C18 120.06(17) . . ? C14 C15 C18 121.10(17) . . ? C11 C16 C15 119.60(16) . . ? C11 C16 H16 120.4(14) . . ? C15 C16 H16 120.0(14) . . ? C13 C17 H17A 112.8(15) . . ? C13 C17 H17B 111.9(15) . . ? H17A C17 H17B 102(2) . . ? C13 C17 H17C 109.8(16) . . ? H17A C17 H17C 110(2) . . ? H17B C17 H17C 110(2) . . ? C15 C18 H18A 114(2) . . ? C15 C18 H18B 114(2) . . ? H18A C18 H18B 109(3) . . ? C15 C18 H18C 110(2) . . ? H18A C18 H18C 98(3) . . ? H18B C18 H18C 110(3) . . ? N2 C19 C20 118.65(14) . . ? N2 C19 C24 119.79(14) . . ? C20 C19 C24 121.54(14) . . ? C21 C20 C19 119.44(15) . . ? C21 C20 H20 121.7(13) . . ? C19 C20 H20 118.8(13) . . ? C20 C21 C22 118.59(15) . . ? C20 C21 C25 120.30(17) . . ? C22 C21 C25 121.11(16) . . ? C23 C22 C21 122.42(15) . . ? C23 C22 H22 117.6(14) . . ? C21 C22 H22 119.9(14) . . ? C24 C23 C22 118.86(15) . . ? C24 C23 C26 120.72(17) . . ? C22 C23 C26 120.42(16) . . ? C23 C24 C19 119.14(15) . . ? C23 C24 H24 120.8(12) . . ? C19 C24 H24 120.0(12) . . ? C21 C25 H25A 112.7(19) . . ? C21 C25 H25B 111(2) . . ? H25A C25 H25B 111(3) . . ? C21 C25 H25C 112(2) . . ? H25A C25 H25C 108(3) . . ? H25B C25 H25C 101(3) . . ? C23 C26 H26A 112.0(18) . . ? C23 C26 H26B 113(2) . . ? H26A C26 H26B 113(3) . . ? C23 C26 H26C 111(2) . . ? H26A C26 H26C 108(3) . . ? H26B C26 H26C 100(3) . . ? C1 O1 Mo1 89.44(9) . . ? C1 O2 Mo1 90.04(10) . . ? C3 O3 Mo1 124.60(11) . . ? C5 O5 Mo1 131.25(12) . . ? C11 N1 C7 116.62(12) . . ? C11 N1 Mo1 104.78(9) . . ? C7 N1 Mo1 138.28(10) . . ? C19 N2 Mo1 163.92(12) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.645 _refine_diff_density_min -0.458 _refine_diff_density_rms 0.069 #=====================================================