# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'ProfD Christian Limberg' _publ_contact_author_address ; Institut für Chemie Humboldt Universität zu Berlin Brook-Taylor-Strasse 2 D-12489 Berlin GERMANY ; _publ_contact_author_email CHRISTIAN.LIMBERG@CHEMIE.HU-BERLIN.DE _publ_section_title ; A (H2O)4/crown ether network spanned between organometallic complex metal fragments ; loop_ _publ_author_name 'Christian Limberg' 'Hans Pritzkow' 'C. Rodrigues' data_2 _database_code_depnum_ccdc_archive 'CCDC 239590' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H29 Mo N2 O2, C12 H24 O6, C F3 O3 S, 2( H2 O)' _chemical_formula_sum 'C36 H57 F3 Mo N2 O13 S' _chemical_formula_weight 910.84 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' S S 0.1246 0.1234 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.3645(5) _cell_length_b 13.1170(6) _cell_length_c 17.6983(9) _cell_angle_alpha 104.8170(10) _cell_angle_beta 100.7200(10) _cell_angle_gamma 106.7510(10) _cell_volume 2137.93(18) _cell_formula_units_Z 2 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 0.430 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.855 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(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 \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47879 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0266 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 32.01 _reflns_number_total 14659 _reflns_number_gt 12737 _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^)+(0.0420P)^2^+2.2103P] 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 14659 _refine_ls_number_parameters 733 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.1018 _refine_ls_wR_factor_gt 0.0939 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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 Mo1 Mo 0.501607(14) 0.650749(12) 0.718003(8) 0.01772(4) Uani 1 1 d . . . S1 S 0.61751(4) 0.20191(3) 0.84064(3) 0.01974(8) Uani 1 1 d . . . F1 F 0.67806(14) 0.39326(10) 0.80879(8) 0.0352(3) Uani 1 1 d . . . F2 F 0.82712(15) 0.31047(14) 0.79418(11) 0.0486(4) Uani 1 1 d . . . F3 F 0.6275(2) 0.24669(14) 0.70462(8) 0.0570(5) Uani 1 1 d . . . O1 O 0.78765(16) 0.68462(17) 0.83439(10) 0.0414(4) Uani 1 1 d . . . O2 O 0.5758(2) 0.44917(16) 0.62345(11) 0.0446(4) Uani 1 1 d . . . O3 O 0.28065(13) 0.59594(12) 0.64414(8) 0.0227(2) Uani 1 1 d . . . O4 O 0.64317(17) 0.10022(12) 0.80604(10) 0.0348(3) Uani 1 1 d . . . O5 O 0.47137(15) 0.19061(13) 0.82122(11) 0.0357(3) Uani 1 1 d . . . O6 O 0.69766(18) 0.26606(12) 0.92366(9) 0.0346(3) Uani 1 1 d . . . O7 O 0.06354(13) 0.35848(10) 0.37444(7) 0.0208(2) Uani 1 1 d . . . O8 O 0.03068(13) 0.31839(10) 0.52788(7) 0.0198(2) Uani 1 1 d . . . O9 O 0.04406(12) 0.48007(10) 0.67327(7) 0.0197(2) Uani 1 1 d . . . O10 O 0.04220(14) 0.02847(12) 0.63541(8) 0.0260(3) Uani 1 1 d . . . O11 O -0.18789(14) 0.09267(11) 0.58669(8) 0.0251(3) Uani 1 1 d . . . O12 O -0.22921(14) 0.07722(11) 0.41917(8) 0.0266(3) Uani 1 1 d . . . O13 O 0.17319(14) 0.57787(12) 0.49350(8) 0.0223(2) Uani 1 1 d . . . N1 N 0.42006(14) 0.76440(11) 0.80078(8) 0.0173(2) Uani 1 1 d . . . N2 N 0.39981(13) 0.55559(11) 0.79052(8) 0.0153(2) Uani 1 1 d . . . C1 C 0.42400(19) 0.86793(14) 0.80029(11) 0.0227(3) Uani 1 1 d . . . C2 C 0.35783(18) 0.92866(14) 0.84440(11) 0.0213(3) Uani 1 1 d . . . C3 C 0.28336(17) 0.88412(13) 0.89368(9) 0.0171(3) Uani 1 1 d . . . C4 C 0.28262(17) 0.77838(13) 0.89611(9) 0.0168(3) Uani 1 1 d . . . C5 C 0.34914(15) 0.72067(12) 0.84867(9) 0.0147(2) Uani 1 1 d . . . C6 C 0.34265(15) 0.60531(12) 0.84542(9) 0.0145(2) Uani 1 1 d . . . C7 C 0.28174(17) 0.55101(13) 0.89515(9) 0.0161(3) Uani 1 1 d . . . C8 C 0.27753(16) 0.44195(12) 0.88982(9) 0.0157(3) Uani 1 1 d . . . C9 C 0.33704(17) 0.39180(13) 0.83264(10) 0.0178(3) Uani 1 1 d . . . C10 C 0.39612(17) 0.44991(14) 0.78533(9) 0.0177(3) Uani 1 1 d . . . C11 C 0.20542(19) 0.94855(14) 0.93980(10) 0.0214(3) Uani 1 1 d . . . C12 C 0.0967(2) 0.96533(18) 0.87671(13) 0.0287(4) Uani 1 1 d . . . C13 C 0.3097(3) 1.0641(2) 0.99693(16) 0.0444(6) Uani 1 1 d . . . C14 C 0.1258(3) 0.8832(2) 0.98736(18) 0.0436(6) Uani 1 1 d . . . C15 C 0.21985(18) 0.38146(13) 0.94597(10) 0.0192(3) Uani 1 1 d . . . C16 C 0.3465(3) 0.3815(2) 1.00710(14) 0.0395(5) Uani 1 1 d . . . C17 C 0.1261(2) 0.25875(16) 0.89695(13) 0.0301(4) Uani 1 1 d . . . C18 C 0.1316(3) 0.43725(16) 0.99009(14) 0.0316(4) Uani 1 1 d . . . C19 C 0.5463(2) 0.52347(19) 0.65676(12) 0.0300(4) Uani 1 1 d . . . C20 C 0.6809(2) 0.67452(19) 0.79241(12) 0.0292(4) Uani 1 1 d . . . C21 C 0.5454(2) 0.6729(2) 0.59779(13) 0.0345(4) Uani 1 1 d . . . C22 C 0.5575(2) 0.7730(2) 0.65452(13) 0.0318(4) Uani 1 1 d . . . C23 C 0.6721(2) 0.81547(18) 0.72828(14) 0.0309(4) Uani 1 1 d . . . C24 C 0.6908(2) 0.29236(16) 0.78427(11) 0.0262(3) Uani 1 1 d . . . C25 C -0.0360(2) 0.06119(17) 0.68871(11) 0.0267(3) Uani 1 1 d . . . C26 C -0.1857(2) 0.02882(16) 0.64051(12) 0.0261(3) Uani 1 1 d . . . C27 C -0.32436(19) 0.06253(17) 0.53550(12) 0.0262(3) Uani 1 1 d . . . C28 C -0.31595(19) 0.10994(17) 0.46659(13) 0.0274(4) Uani 1 1 d . . . C29 C -0.2673(2) -0.04164(17) 0.38438(13) 0.0304(4) Uani 1 1 d . . . C30 C -0.1870(2) -0.06478(19) 0.32328(12) 0.0313(4) Uani 1 1 d . . . C31 C 0.0154(2) 0.25098(14) 0.38557(11) 0.0227(3) Uani 1 1 d . . . C32 C 0.0841(2) 0.25721(15) 0.47004(11) 0.0229(3) Uani 1 1 d . . . C33 C 0.07926(18) 0.31140(15) 0.60667(10) 0.0210(3) Uani 1 1 d . . . C34 C 0.00508(19) 0.36221(14) 0.66270(10) 0.0211(3) Uani 1 1 d . . . C35 C -0.03757(19) 0.53342(15) 0.71415(11) 0.0225(3) Uani 1 1 d . . . C36 C 0.00478(19) 0.35015(15) 0.29268(10) 0.0224(3) Uani 1 1 d . . . H1 H 0.475(3) 0.899(2) 0.7690(15) 0.025(6) Uiso 1 1 d . . . H2 H 0.366(3) 1.000(2) 0.8413(17) 0.037(7) Uiso 1 1 d . . . H4 H 0.237(2) 0.7440(19) 0.9290(14) 0.018(5) Uiso 1 1 d . . . H7 H 0.249(2) 0.590(2) 0.9345(14) 0.020(5) Uiso 1 1 d . . . H9 H 0.347(3) 0.322(2) 0.8301(15) 0.028(6) Uiso 1 1 d . . . H10 H 0.437(2) 0.4177(19) 0.7496(14) 0.018(5) Uiso 1 1 d . . . H12A H 0.048(3) 1.004(2) 0.9042(17) 0.035(7) Uiso 1 1 d . . . H12B H 0.140(3) 1.010(2) 0.8439(18) 0.040(7) Uiso 1 1 d . . . H12C H 0.030(3) 0.890(3) 0.8369(19) 0.050(8) Uiso 1 1 d . . . H13A H 0.374(3) 1.054(3) 1.036(2) 0.050(9) Uiso 1 1 d . . . H13B H 0.359(3) 1.109(3) 0.966(2) 0.051(9) Uiso 1 1 d . . . H13C H 0.263(3) 1.108(3) 1.0260(19) 0.047(8) Uiso 1 1 d . . . H14A H 0.191(3) 0.877(3) 1.028(2) 0.049(9) Uiso 1 1 d . . . H14B H 0.057(4) 0.805(3) 0.950(2) 0.058(10) Uiso 1 1 d . . . H14C H 0.077(3) 0.927(3) 1.018(2) 0.055(9) Uiso 1 1 d . . . H16A H 0.394(3) 0.459(2) 1.0400(17) 0.033(7) Uiso 1 1 d . . . H16B H 0.313(4) 0.345(3) 1.046(2) 0.059(10) Uiso 1 1 d . . . H16C H 0.403(4) 0.342(3) 0.978(2) 0.059(10) Uiso 1 1 d . . . H17A H 0.176(3) 0.216(2) 0.8689(17) 0.038(7) Uiso 1 1 d . . . H17B H 0.048(3) 0.254(2) 0.8550(18) 0.038(7) Uiso 1 1 d . . . H17C H 0.092(3) 0.223(2) 0.9357(18) 0.041(7) Uiso 1 1 d . . . H18A H 0.051(3) 0.435(2) 0.9514(18) 0.043(8) Uiso 1 1 d . . . H18B H 0.095(3) 0.394(3) 1.0240(18) 0.043(8) Uiso 1 1 d . . . H18C H 0.190(3) 0.515(3) 1.0256(19) 0.048(8) Uiso 1 1 d . . . H21A H 0.635(3) 0.662(2) 0.5922(16) 0.033(7) Uiso 1 1 d . . . H21B H 0.462(3) 0.631(2) 0.5500(17) 0.040(7) Uiso 1 1 d . . . H22 H 0.485(3) 0.804(2) 0.6482(16) 0.034(7) Uiso 1 1 d . . . H23A H 0.683(3) 0.880(2) 0.7764(16) 0.032(7) Uiso 1 1 d . . . H23B H 0.758(3) 0.806(2) 0.7267(17) 0.040(7) Uiso 1 1 d . . . H25A H -0.037(3) 0.024(2) 0.7305(16) 0.030(6) Uiso 1 1 d . . . H25B H 0.005(3) 0.143(2) 0.7159(16) 0.038(7) Uiso 1 1 d . . . H26A H -0.226(3) -0.052(2) 0.6092(16) 0.029(6) Uiso 1 1 d . . . H26B H -0.244(3) 0.043(2) 0.6758(16) 0.031(6) Uiso 1 1 d . . . H27A H -0.367(3) -0.019(2) 0.5135(15) 0.025(6) Uiso 1 1 d . . . H27B H -0.384(3) 0.094(2) 0.5662(17) 0.039(7) Uiso 1 1 d . . . H28A H -0.278(3) 0.195(2) 0.4876(16) 0.031(6) Uiso 1 1 d . . . H28B H -0.416(3) 0.084(2) 0.4308(16) 0.033(7) Uiso 1 1 d . . . H29A H -0.245(2) -0.075(2) 0.4271(15) 0.023(6) Uiso 1 1 d . . . H29B H -0.375(3) -0.077(3) 0.3564(19) 0.046(8) Uiso 1 1 d . . . H30A H -0.200(3) -0.025(2) 0.2826(16) 0.029(6) Uiso 1 1 d . . . H30B H -0.221(3) -0.150(3) 0.2937(18) 0.045(8) Uiso 1 1 d . . . H31A H -0.081(3) 0.228(2) 0.3779(15) 0.025(6) Uiso 1 1 d . . . H31B H 0.040(3) 0.197(2) 0.3479(15) 0.026(6) Uiso 1 1 d . . . H32A H 0.182(3) 0.292(2) 0.4834(15) 0.026(6) Uiso 1 1 d . . . H32B H 0.065(3) 0.182(2) 0.4716(16) 0.031(6) Uiso 1 1 d . . . H33A H 0.060(2) 0.236(2) 0.6038(14) 0.023(6) Uiso 1 1 d . . . H33B H 0.179(3) 0.350(2) 0.6278(14) 0.022(6) Uiso 1 1 d . . . H34A H -0.092(2) 0.3272(19) 0.6407(14) 0.020(5) Uiso 1 1 d . . . H34B H 0.033(3) 0.351(2) 0.7149(16) 0.031(6) Uiso 1 1 d . . . H35A H -0.132(3) 0.489(2) 0.6913(15) 0.025(6) Uiso 1 1 d . . . H35B H -0.013(3) 0.537(2) 0.7699(17) 0.037(7) Uiso 1 1 d . . . H36A H -0.100(2) 0.3102(19) 0.2760(14) 0.020(5) Uiso 1 1 d . . . H36B H 0.040(3) 0.307(2) 0.2551(16) 0.031(6) Uiso 1 1 d . . . H3O H 0.217(3) 0.564(2) 0.6567(17) 0.031(7) Uiso 1 1 d . . . H3P H 0.251(3) 0.590(2) 0.6002(17) 0.027(6) Uiso 1 1 d . . . H13O H 0.144(3) 0.518(3) 0.4630(19) 0.041(8) Uiso 1 1 d . . . H13P H 0.112(3) 0.601(2) 0.4894(17) 0.035(7) 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 0.01488(6) 0.02094(7) 0.01749(6) 0.00606(5) 0.00815(5) 0.00451(5) S1 0.02174(18) 0.01614(17) 0.02269(18) 0.00739(14) 0.00810(14) 0.00658(14) F1 0.0412(7) 0.0255(6) 0.0437(7) 0.0198(5) 0.0111(6) 0.0119(5) F2 0.0346(7) 0.0554(9) 0.0762(11) 0.0404(8) 0.0327(7) 0.0180(7) F3 0.0818(12) 0.0485(9) 0.0216(6) 0.0124(6) 0.0066(7) -0.0001(8) O1 0.0230(7) 0.0716(12) 0.0342(8) 0.0263(8) 0.0080(6) 0.0157(7) O2 0.0554(11) 0.0480(10) 0.0421(9) 0.0115(8) 0.0283(8) 0.0287(9) O3 0.0167(5) 0.0336(7) 0.0166(5) 0.0120(5) 0.0043(4) 0.0039(5) O4 0.0418(8) 0.0196(6) 0.0474(9) 0.0090(6) 0.0216(7) 0.0134(6) O5 0.0222(6) 0.0320(7) 0.0584(10) 0.0216(7) 0.0140(6) 0.0100(6) O6 0.0515(9) 0.0260(7) 0.0213(6) 0.0099(5) 0.0041(6) 0.0085(6) O7 0.0230(6) 0.0188(5) 0.0183(5) 0.0061(4) 0.0060(4) 0.0038(4) O8 0.0237(6) 0.0206(5) 0.0170(5) 0.0071(4) 0.0066(4) 0.0094(4) O9 0.0191(5) 0.0180(5) 0.0209(5) 0.0068(4) 0.0083(4) 0.0029(4) O10 0.0266(6) 0.0263(6) 0.0202(6) 0.0040(5) 0.0031(5) 0.0075(5) O11 0.0220(6) 0.0249(6) 0.0270(6) 0.0134(5) 0.0041(5) 0.0036(5) O12 0.0242(6) 0.0251(6) 0.0289(6) 0.0122(5) 0.0071(5) 0.0036(5) O13 0.0221(6) 0.0233(6) 0.0180(5) 0.0049(5) 0.0018(4) 0.0070(5) N1 0.0176(6) 0.0165(6) 0.0189(6) 0.0070(5) 0.0081(5) 0.0047(5) N2 0.0146(5) 0.0166(6) 0.0147(5) 0.0042(4) 0.0042(4) 0.0064(4) C1 0.0247(8) 0.0182(7) 0.0287(8) 0.0114(6) 0.0137(7) 0.0056(6) C2 0.0238(7) 0.0157(7) 0.0273(8) 0.0101(6) 0.0098(6) 0.0070(6) C3 0.0193(7) 0.0157(6) 0.0172(6) 0.0058(5) 0.0048(5) 0.0074(5) C4 0.0209(7) 0.0166(6) 0.0166(6) 0.0078(5) 0.0073(5) 0.0087(5) C5 0.0155(6) 0.0141(6) 0.0147(6) 0.0051(5) 0.0048(5) 0.0049(5) C6 0.0154(6) 0.0151(6) 0.0134(6) 0.0047(5) 0.0040(5) 0.0059(5) C7 0.0201(7) 0.0149(6) 0.0154(6) 0.0056(5) 0.0067(5) 0.0078(5) C8 0.0184(6) 0.0136(6) 0.0140(6) 0.0043(5) 0.0032(5) 0.0050(5) C9 0.0218(7) 0.0148(6) 0.0176(6) 0.0051(5) 0.0049(5) 0.0081(5) C10 0.0200(7) 0.0187(7) 0.0157(6) 0.0047(5) 0.0060(5) 0.0090(5) C11 0.0297(8) 0.0206(7) 0.0210(7) 0.0086(6) 0.0101(6) 0.0155(6) C12 0.0339(9) 0.0296(9) 0.0304(9) 0.0112(7) 0.0096(8) 0.0211(8) C13 0.0428(13) 0.0366(12) 0.0370(11) -0.0120(9) -0.0007(10) 0.0185(10) C14 0.0708(17) 0.0502(14) 0.0529(14) 0.0373(12) 0.0467(14) 0.0472(14) C15 0.0246(7) 0.0158(7) 0.0166(6) 0.0063(5) 0.0058(6) 0.0054(6) C16 0.0346(11) 0.0550(14) 0.0304(10) 0.0284(10) 0.0031(8) 0.0093(10) C17 0.0402(11) 0.0163(7) 0.0311(9) 0.0062(7) 0.0158(8) 0.0040(7) C18 0.0489(12) 0.0198(8) 0.0346(10) 0.0116(7) 0.0276(9) 0.0121(8) C19 0.0285(9) 0.0385(10) 0.0270(9) 0.0115(8) 0.0139(7) 0.0134(8) C20 0.0216(8) 0.0451(11) 0.0236(8) 0.0159(8) 0.0100(6) 0.0094(7) C21 0.0299(9) 0.0540(13) 0.0238(8) 0.0206(9) 0.0134(7) 0.0104(9) C22 0.0277(9) 0.0453(11) 0.0378(10) 0.0311(9) 0.0186(8) 0.0140(8) C23 0.0214(8) 0.0312(9) 0.0405(11) 0.0146(8) 0.0150(8) 0.0032(7) C24 0.0286(8) 0.0253(8) 0.0232(8) 0.0101(6) 0.0077(7) 0.0056(7) C25 0.0344(9) 0.0257(8) 0.0193(7) 0.0079(6) 0.0067(7) 0.0098(7) C26 0.0307(9) 0.0249(8) 0.0251(8) 0.0120(7) 0.0106(7) 0.0082(7) C27 0.0189(7) 0.0286(9) 0.0301(9) 0.0116(7) 0.0075(6) 0.0050(6) C28 0.0206(8) 0.0297(9) 0.0336(9) 0.0154(7) 0.0060(7) 0.0079(7) C29 0.0270(9) 0.0268(9) 0.0289(9) 0.0071(7) 0.0061(7) 0.0001(7) C30 0.0265(9) 0.0342(10) 0.0228(8) 0.0040(7) 0.0023(7) 0.0035(7) C31 0.0285(8) 0.0178(7) 0.0210(7) 0.0056(6) 0.0095(6) 0.0059(6) C32 0.0257(8) 0.0234(8) 0.0230(7) 0.0082(6) 0.0093(6) 0.0114(6) C33 0.0232(7) 0.0211(7) 0.0193(7) 0.0097(6) 0.0040(6) 0.0070(6) C34 0.0235(7) 0.0202(7) 0.0182(7) 0.0085(6) 0.0059(6) 0.0035(6) C35 0.0247(8) 0.0259(8) 0.0191(7) 0.0093(6) 0.0114(6) 0.0072(6) C36 0.0276(8) 0.0228(8) 0.0159(7) 0.0044(6) 0.0089(6) 0.0073(6) _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 C20 1.9571(19) . ? Mo1 C19 1.971(2) . ? Mo1 C22 2.1900(19) . ? Mo1 N2 2.2096(13) . ? Mo1 O3 2.2196(13) . ? Mo1 N1 2.2700(14) . ? Mo1 C23 2.3028(19) . ? Mo1 C21 2.3275(19) . ? S1 O6 1.4380(15) . ? S1 O4 1.4395(15) . ? S1 O5 1.4440(15) . ? S1 C24 1.8296(19) . ? F1 C24 1.336(2) . ? F2 C24 1.333(2) . ? F3 C24 1.332(2) . ? O1 C20 1.163(2) . ? O2 C19 1.156(3) . ? O3 H3O 0.78(3) . ? O3 H3P 0.76(3) . ? O7 C36 1.425(2) . ? O7 C31 1.432(2) . ? O8 C33 1.427(2) . ? O8 C32 1.430(2) . ? O9 C35 1.428(2) . ? O9 C34 1.433(2) . ? O10 C25 1.418(2) . ? O10 C30 1.420(2) 2_556 ? O11 C27 1.413(2) . ? O11 C26 1.421(2) . ? O12 C28 1.420(2) . ? O12 C29 1.425(2) . ? O13 H13O 0.77(3) . ? O13 H13P 0.77(3) . ? N1 C1 1.349(2) . ? N1 C5 1.3510(19) . ? N2 C6 1.3540(19) . ? N2 C10 1.354(2) . ? C1 C2 1.382(2) . ? C1 H1 0.92(3) . ? C2 C3 1.396(2) . ? C2 H2 0.93(3) . ? C3 C4 1.396(2) . ? C3 C11 1.523(2) . ? C4 C5 1.395(2) . ? C4 H4 0.94(2) . ? C5 C6 1.481(2) . ? C6 C7 1.396(2) . ? C7 C8 1.397(2) . ? C7 H7 0.93(2) . ? C8 C9 1.401(2) . ? C8 C15 1.525(2) . ? C9 C10 1.380(2) . ? C9 H9 0.94(3) . ? C10 H10 0.91(2) . ? C11 C14 1.531(3) . ? C11 C13 1.534(3) . ? C11 C12 1.538(3) . ? C12 H12A 0.93(3) . ? C12 H12B 1.00(3) . ? C12 H12C 1.01(3) . ? C13 H13A 0.94(3) . ? C13 H13B 1.01(3) . ? C13 H13C 0.97(3) . ? C14 H14A 0.92(3) . ? C14 H14B 1.02(4) . ? C14 H14C 1.00(3) . ? C15 C18 1.530(3) . ? C15 C17 1.536(2) . ? C15 C16 1.538(3) . ? C16 H16A 0.96(3) . ? C16 H16B 0.99(4) . ? C16 H16C 1.02(4) . ? C17 H17A 0.97(3) . ? C17 H17B 0.97(3) . ? C17 H17C 0.98(3) . ? C18 H18A 0.96(3) . ? C18 H18B 0.98(3) . ? C18 H18C 0.99(3) . ? C21 C22 1.389(3) . ? C21 H21A 1.00(3) . ? C21 H21B 0.99(3) . ? C22 C23 1.448(3) . ? C22 H22 0.95(3) . ? C23 H23A 1.00(3) . ? C23 H23B 0.93(3) . ? C25 C26 1.502(3) . ? C25 H25A 0.99(3) . ? C25 H25B 0.98(3) . ? C26 H26A 0.99(3) . ? C26 H26B 0.97(3) . ? C27 C28 1.509(3) . ? C27 H27A 0.97(2) . ? C27 H27B 1.00(3) . ? C28 H28A 1.01(3) . ? C28 H28B 1.01(3) . ? C29 C30 1.505(3) . ? C29 H29A 0.99(2) . ? C29 H29B 1.04(3) . ? C30 O10 1.420(2) 2_556 ? C30 H30A 1.00(3) . ? C30 H30B 1.03(3) . ? C31 C32 1.502(3) . ? C31 H31A 0.93(3) . ? C31 H31B 0.97(2) . ? C32 H32A 0.94(3) . ? C32 H32B 0.96(3) . ? C33 C34 1.503(3) . ? C33 H33A 0.93(2) . ? C33 H33B 0.96(2) . ? C34 H34A 0.94(2) . ? C34 H34B 0.97(3) . ? C35 C36 1.508(3) 2_566 ? C35 H35A 0.93(3) . ? C35 H35B 0.96(3) . ? C36 C35 1.508(2) 2_566 ? C36 H36A 1.01(2) . ? C36 H36B 0.95(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 C20 Mo1 C19 79.92(9) . . ? C20 Mo1 C22 103.75(8) . . ? C19 Mo1 C22 102.69(9) . . ? C20 Mo1 N2 86.87(6) . . ? C19 Mo1 N2 93.40(7) . . ? C22 Mo1 N2 161.98(7) . . ? C20 Mo1 O3 168.13(7) . . ? C19 Mo1 O3 97.30(7) . . ? C22 Mo1 O3 88.11(7) . . ? N2 Mo1 O3 81.77(5) . . ? C20 Mo1 N1 100.60(7) . . ? C19 Mo1 N1 165.55(7) . . ? C22 Mo1 N1 91.27(7) . . ? N2 Mo1 N1 72.26(5) . . ? O3 Mo1 N1 79.20(5) . . ? C20 Mo1 C23 68.62(8) . . ? C19 Mo1 C23 108.06(8) . . ? C22 Mo1 C23 37.49(8) . . ? N2 Mo1 C23 143.17(7) . . ? O3 Mo1 C23 122.99(7) . . ? N1 Mo1 C23 85.29(7) . . ? C20 Mo1 C21 107.48(8) . . ? C19 Mo1 C21 68.82(9) . . ? C22 Mo1 C21 35.66(9) . . ? N2 Mo1 C21 153.98(7) . . ? O3 Mo1 C21 81.89(6) . . ? N1 Mo1 C21 123.90(7) . . ? C23 Mo1 C21 62.69(8) . . ? O6 S1 O4 115.51(10) . . ? O6 S1 O5 115.33(11) . . ? O4 S1 O5 114.49(10) . . ? O6 S1 C24 102.94(9) . . ? O4 S1 C24 102.89(9) . . ? O5 S1 C24 103.10(9) . . ? Mo1 O3 H3O 123(2) . . ? Mo1 O3 H3P 130(2) . . ? H3O O3 H3P 105(3) . . ? C36 O7 C31 110.64(13) . . ? C33 O8 C32 110.93(13) . . ? C35 O9 C34 113.82(13) . . ? C25 O10 C30 111.74(14) . 2_556 ? C27 O11 C26 111.83(14) . . ? C28 O12 C29 114.08(15) . . ? H13O O13 H13P 106(3) . . ? C1 N1 C5 116.92(14) . . ? C1 N1 Mo1 125.37(11) . . ? C5 N1 Mo1 117.35(10) . . ? C6 N2 C10 117.38(13) . . ? C6 N2 Mo1 119.47(10) . . ? C10 N2 Mo1 123.10(10) . . ? N1 C1 C2 123.52(15) . . ? N1 C1 H1 117.2(15) . . ? C2 C1 H1 119.3(15) . . ? C1 C2 C3 120.14(15) . . ? C1 C2 H2 118.4(17) . . ? C3 C2 H2 121.5(17) . . ? C2 C3 C4 116.41(14) . . ? C2 C3 C11 120.38(14) . . ? C4 C3 C11 123.19(14) . . ? C5 C4 C3 120.43(14) . . ? C5 C4 H4 118.4(14) . . ? C3 C4 H4 121.2(14) . . ? N1 C5 C4 122.53(14) . . ? N1 C5 C6 115.44(13) . . ? C4 C5 C6 122.00(13) . . ? N2 C6 C7 122.05(14) . . ? N2 C6 C5 115.31(13) . . ? C7 C6 C5 122.64(13) . . ? C6 C7 C8 120.69(14) . . ? C6 C7 H7 119.3(15) . . ? C8 C7 H7 119.9(15) . . ? C7 C8 C9 116.47(14) . . ? C7 C8 C15 122.77(14) . . ? C9 C8 C15 120.66(14) . . ? C10 C9 C8 120.18(14) . . ? C10 C9 H9 118.6(16) . . ? C8 C9 H9 120.9(16) . . ? N2 C10 C9 123.23(14) . . ? N2 C10 H10 117.2(14) . . ? C9 C10 H10 119.6(14) . . ? C3 C11 C14 112.15(14) . . ? C3 C11 C13 109.39(16) . . ? C14 C11 C13 110.8(2) . . ? C3 C11 C12 107.61(14) . . ? C14 C11 C12 107.60(18) . . ? C13 C11 C12 109.23(17) . . ? C11 C12 H12A 108.3(17) . . ? C11 C12 H12B 113.0(17) . . ? H12A C12 H12B 108(2) . . ? C11 C12 H12C 110.5(18) . . ? H12A C12 H12C 110(3) . . ? H12B C12 H12C 107(2) . . ? C11 C13 H13A 109(2) . . ? C11 C13 H13B 111.2(19) . . ? H13A C13 H13B 111(3) . . ? C11 C13 H13C 111.6(19) . . ? H13A C13 H13C 107(3) . . ? H13B C13 H13C 107(3) . . ? C11 C14 H14A 108(2) . . ? C11 C14 H14B 111.4(19) . . ? H14A C14 H14B 111(3) . . ? C11 C14 H14C 110.7(19) . . ? H14A C14 H14C 104(3) . . ? H14B C14 H14C 111(3) . . ? C8 C15 C18 112.36(14) . . ? C8 C15 C17 110.30(14) . . ? C18 C15 C17 107.57(16) . . ? C8 C15 C16 107.05(15) . . ? C18 C15 C16 110.96(18) . . ? C17 C15 C16 108.57(17) . . ? C15 C16 H16A 104.6(16) . . ? C15 C16 H16B 109(2) . . ? H16A C16 H16B 103(3) . . ? C15 C16 H16C 111(2) . . ? H16A C16 H16C 117(3) . . ? H16B C16 H16C 112(3) . . ? C15 C17 H17A 113.0(17) . . ? C15 C17 H17B 112.1(17) . . ? H17A C17 H17B 106(2) . . ? C15 C17 H17C 107.2(17) . . ? H17A C17 H17C 108(2) . . ? H17B C17 H17C 110(2) . . ? C15 C18 H18A 110.2(18) . . ? C15 C18 H18B 108.9(17) . . ? H18A C18 H18B 106(2) . . ? C15 C18 H18C 110.4(19) . . ? H18A C18 H18C 112(3) . . ? H18B C18 H18C 109(2) . . ? O2 C19 Mo1 177.5(2) . . ? O1 C20 Mo1 177.1(2) . . ? C22 C21 Mo1 66.77(11) . . ? C22 C21 H21A 116.5(16) . . ? Mo1 C21 H21A 111.0(15) . . ? C22 C21 H21B 121.7(17) . . ? Mo1 C21 H21B 112.6(17) . . ? H21A C21 H21B 117(2) . . ? C21 C22 C23 116.2(2) . . ? C21 C22 Mo1 77.57(12) . . ? C23 C22 Mo1 75.49(11) . . ? C21 C22 H22 120.5(17) . . ? C23 C22 H22 122.5(17) . . ? Mo1 C22 H22 107.8(17) . . ? C22 C23 Mo1 67.03(10) . . ? C22 C23 H23A 123.3(15) . . ? Mo1 C23 H23A 112.9(16) . . ? C22 C23 H23B 120.4(18) . . ? Mo1 C23 H23B 112.3(18) . . ? H23A C23 H23B 112(2) . . ? F3 C24 F2 107.14(18) . . ? F3 C24 F1 107.27(17) . . ? F2 C24 F1 107.02(16) . . ? F3 C24 S1 111.80(14) . . ? F2 C24 S1 111.39(14) . . ? F1 C24 S1 111.93(13) . . ? O10 C25 C26 109.27(15) . . ? O10 C25 H25A 112.4(15) . . ? C26 C25 H25A 107.4(15) . . ? O10 C25 H25B 108.9(16) . . ? C26 C25 H25B 110.2(16) . . ? H25A C25 H25B 109(2) . . ? O11 C26 C25 108.16(15) . . ? O11 C26 H26A 109.9(15) . . ? C25 C26 H26A 110.6(15) . . ? O11 C26 H26B 110.2(15) . . ? C25 C26 H26B 111.4(15) . . ? H26A C26 H26B 106(2) . . ? O11 C27 C28 109.56(15) . . ? O11 C27 H27A 109.3(14) . . ? C28 C27 H27A 109.5(15) . . ? O11 C27 H27B 110.8(16) . . ? C28 C27 H27B 107.8(16) . . ? H27A C27 H27B 110(2) . . ? O12 C28 C27 114.89(16) . . ? O12 C28 H28A 106.0(15) . . ? C27 C28 H28A 111.1(15) . . ? O12 C28 H28B 109.7(15) . . ? C27 C28 H28B 106.4(15) . . ? H28A C28 H28B 109(2) . . ? O12 C29 C30 108.68(16) . . ? O12 C29 H29A 110.7(14) . . ? C30 C29 H29A 109.3(14) . . ? O12 C29 H29B 109.1(17) . . ? C30 C29 H29B 110.6(17) . . ? H29A C29 H29B 108(2) . . ? O10 C30 C29 109.34(16) 2_556 . ? O10 C30 H30A 109.6(15) 2_556 . ? C29 C30 H30A 111.1(15) . . ? O10 C30 H30B 107.6(17) 2_556 . ? C29 C30 H30B 109.4(17) . . ? H30A C30 H30B 110(2) . . ? O7 C31 C32 111.07(14) . . ? O7 C31 H31A 109.0(15) . . ? C32 C31 H31A 108.5(15) . . ? O7 C31 H31B 109.9(15) . . ? C32 C31 H31B 107.2(15) . . ? H31A C31 H31B 111(2) . . ? O8 C32 C31 110.15(14) . . ? O8 C32 H32A 109.6(15) . . ? C31 C32 H32A 110.8(15) . . ? O8 C32 H32B 110.4(16) . . ? C31 C32 H32B 108.5(16) . . ? H32A C32 H32B 107(2) . . ? O8 C33 C34 109.32(14) . . ? O8 C33 H33A 110.4(15) . . ? C34 C33 H33A 108.3(15) . . ? O8 C33 H33B 110.3(14) . . ? C34 C33 H33B 110.4(14) . . ? H33A C33 H33B 108(2) . . ? O9 C34 C33 108.92(13) . . ? O9 C34 H34A 109.5(14) . . ? C33 C34 H34A 110.4(14) . . ? O9 C34 H34B 110.2(16) . . ? C33 C34 H34B 108.6(15) . . ? H34A C34 H34B 109(2) . . ? O9 C35 C36 108.18(13) . 2_566 ? O9 C35 H35A 108.7(15) . . ? C36 C35 H35A 113.0(15) 2_566 . ? O9 C35 H35B 108.4(17) . . ? C36 C35 H35B 111.1(17) 2_566 . ? H35A C35 H35B 107(2) . . ? O7 C36 C35 109.57(14) . 2_566 ? O7 C36 H36A 110.0(13) . . ? C35 C36 H36A 109.7(13) 2_566 . ? O7 C36 H36B 112.2(16) . . ? C35 C36 H36B 109.1(16) 2_566 . ? H36A C36 H36B 106(2) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 32.01 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 3.368 _refine_diff_density_min -1.648 _refine_diff_density_rms 0.086 #===END