# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global #=================================================================== _journal_coden_Cambridge 440 loop_ _publ_author_name 'Carlos Romao' 'Maria Calhorda' 'Isabel Gonçalves' 'Brian J. Goodfellow' 'Eberhardt Herdtweck' 'Beatriz Royo' 'Luis Veiros' _publ_contact_author_name 'Prof Carlos Romao' _publ_contact_author_address ; ITQB Quinta do Marques, EAN Apt 127 Oeiras 2781-901 PORTUGAL ; _publ_contact_author_email 'CCR@ITQB.UNL.PT' _publ_requested_journal 'New Journal of Chemistry' _publ_requested_coeditor_name ? _publ_contact_letter # Include date of submission ; February 2002 ; _publ_section_title ; Exocyclic Coordination of the \h3-Fluorenyl, \h3-Cyclopenta(def)phenanthrenyl and \h3-8,9-Dihydro-Cyclopenta(def)phenanthrenyl Anion: X-ray Crystal Structures, NMR Fluxionality and Theortical Study ; _publ_section_abstract ; The novel complexes IndMo(\h3-Flu)(CO)2, (Flu=fluorenyl) (\h5-Ind)Mo(\h3-Cpp)(CO)2 ... ; # Insert blank lines between paragraphs _publ_section_comment ; none ; _publ_section_experimental ; none ; # Insert blank lines between references _publ_section_references ; Allen, F.H., Kennard, O. & Taylor, R. (1983). Acc. Chem. Res. 16, 146-153. Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). SIR92, J. Appl. Cryst. 27, 435-436. Sheldrick, G. M. (1998). SHELXL97, University of Gottingen, Gottingen, Germany. Spek, A. L. (1999). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. STOE (1997), IPDS Operating System, Version 2.8., Stoe&Cie. GmbH: Darmstadt, Germany. Wilson, A.J.C. (1992) Ed. International Tables for Crystallography, Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands. ; _publ_section_figure_captions ; none ; _publ_section_acknowledgements ; none ; _publ_section_table_legends ; none ; data_ROMU-3071-173 _database_code_CSD 189189 _audit_creation_date 16-Apr-99 _audit_creation_method 'PLATON option' _audit_update_record ; 5-Sept-00 Updated by the Author E.H. 6-Oct-00 Updated by the Author E.H. X-ray textwriting by E.H. Checkcif OK 5-Feb-02 Updated by the Author E.H. 3-Jul-02 Updated by the Author E.H. ; #=================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C26 H18 Mo O2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H18 Mo O2' _chemical_formula_weight 458.37 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 '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' 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' #=================================================================== # 6. CRYSTAL DATA #=================================================================== _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 9.1945(11) _cell_length_b 9.7882(12) _cell_length_c 10.9604(12) _cell_angle_alpha 91.929(14) _cell_angle_beta 106.072(13) _cell_angle_gamma 99.804(15) _cell_volume 930.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used 4881 _cell_measurement_theta_min 8.95 _cell_measurement_theta_max 25.85 _exptl_crystal_description 'fragment' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_method none _exptl_crystal_F_000 464 _exptl_absorpt_coefficient_mu 0.725 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min 0.516 _exptl_absorpt_correction_T_max 0.949 _exptl_absorpt_process_details ; Neither decay correction nor absorption correction ; _exptl_special_details ; Diffractometer operator E. Herdtweck exposure_time 150 s per image exposure_phi_range 0-360 exposure_delta_phi 2.0 exposure_sum_images 180 exposure_sum_images_used 1-180 ; _publ_section_exptl_prep ; the crystal was fixed in a capillary with perfluorinated ether and transfered to the diffractometer ; _publ_section_exptl_refinement ; straight forward after integration with the program INTEGRATE; source: 'IPDS (STOE, 1997)' ; #=================================================================== # 7. EXPERIMENTAL DATA #=================================================================== _diffrn_ambient_temperature 173(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'one-circle diffractometer' _diffrn_measurement_device_type 'IPDS (STOE&CIE)' _diffrn_measurement_method 'phi-rotation ' _diffrn_detector 'imaging plate' _diffrn_detector_area_resol_mean 6.7 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% 0 # number of measured reflections (redundant set) _diffrn_reflns_number 12871 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0252 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.69 _reflns_number_total 3291 _reflns_number_gt 2956 # number of observed reflections (> n sig(I)) _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (STOE, 1997)' _computing_cell_refinement 'IPDS (STOE, 1997)' _computing_data_reduction 'IPDS (STOE, 1997)' _computing_structure_solution 'SIR-92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 1999)' _computing_publication_material 'PLATON (Spek, 1999)' #=================================================================== # 8. REFINEMENT DATA #=================================================================== _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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 sigma _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+0.0000P] 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_number_reflns 3291 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0244 _refine_ls_R_factor_gt 0.0205 _refine_ls_wR_factor_ref 0.0523 _refine_ls_wR_factor_gt 0.0515 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max -0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 25.69 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 0.395 _refine_diff_density_min -0.337 _refine_diff_density_rms 0.056 #=================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=================================================================== loop_ _atom_site_label _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv Mo Uani 0.77625(2) 0.25071(2) 0.20849(2) 1.000 0.0161(1) O1 Uani 0.4543(2) 0.0598(2) 0.1375(2) 1.000 0.0309(5) O2 Uani 0.6278(2) 0.3845(2) 0.3932(2) 1.000 0.0363(5) C1 Uani 0.5764(2) 0.1285(2) 0.1670(2) 1.000 0.0218(6) C2 Uani 0.6847(2) 0.3348(2) 0.3259(2) 1.000 0.0232(6) C3 Uani 0.8538(2) 0.0380(2) 0.2512(2) 1.000 0.0214(6) C4 Uani 0.9061(2) 0.1239(2) 0.3713(2) 1.000 0.0206(6) C5 Uani 0.9951(2) 0.2578(2) 0.4106(2) 1.000 0.0273(7) C6 Uani 1.0026(3) 0.3159(2) 0.5340(2) 1.000 0.0330(7) C7 Uani 0.9243(3) 0.2502(2) 0.6107(2) 1.000 0.0294(7) C8 Uani 0.8287(2) 0.1169(2) 0.5709(2) 1.000 0.0224(6) C9 Uani 0.8229(2) 0.0623(2) 0.4548(2) 1.000 0.0204(6) C10 Uani 0.7333(2) -0.0675(2) 0.3938(2) 1.000 0.0191(6) C11 Uani 0.6451(2) -0.1588(2) 0.4514(2) 1.000 0.0217(6) C12 Uani 0.5704(3) -0.2841(2) 0.3804(2) 1.000 0.0268(7) C13 Uani 0.5856(3) -0.3092(2) 0.2583(2) 1.000 0.0275(7) C14 Uani 0.6723(3) -0.2135(2) 0.2025(2) 1.000 0.0249(6) C15 Uani 0.7498(2) -0.0878(2) 0.2720(2) 1.000 0.0200(6) C16 Uani 0.7325(3) 0.0319(3) 0.6426(3) 1.000 0.0339(8) C17 Uani 0.6451(4) -0.1135(3) 0.5846(3) 1.000 0.0373(10) C21 Uani 0.7339(2) 0.2733(2) -0.0056(2) 1.000 0.0220(6) C22 Uani 0.7031(2) 0.3933(2) 0.0508(2) 1.000 0.0224(6) C23 Uani 0.8409(2) 0.4673(2) 0.1358(2) 1.000 0.0227(6) C23A Uani 0.9646(2) 0.4004(2) 0.1237(2) 1.000 0.0219(6) C24 Uani 1.1258(3) 0.4299(2) 0.1806(2) 1.000 0.0307(7) C25 Uani 1.2129(3) 0.3405(3) 0.1510(3) 1.000 0.0377(10) C26 Uani 1.1460(3) 0.2203(3) 0.0665(3) 1.000 0.0374(9) C27 Uani 0.9919(3) 0.1891(2) 0.0089(2) 1.000 0.0297(7) C27A Uani 0.8972(2) 0.2793(2) 0.0359(2) 1.000 0.0217(6) H31 Uiso 0.913(3) 0.031(3) 0.193(2) 1.000 0.033(6) H51 Uiso 1.068(3) 0.298(2) 0.367(2) 1.000 0.026(6) H61 Uiso 1.065(3) 0.400(3) 0.560(3) 1.000 0.054(8) H71 Uiso 0.928(3) 0.282(3) 0.689(3) 1.000 0.040(7) H121 Uiso 0.514(3) -0.352(3) 0.416(3) 1.000 0.036(7) H131 Uiso 0.533(3) -0.394(2) 0.211(2) 1.000 0.021(5) H141 Uiso 0.680(3) -0.233(2) 0.120(3) 1.000 0.030(6) H161 Uiso 0.796(5) 0.035(4) 0.727(4) 1.000 0.096(14) H162 Uiso 0.660(5) 0.082(4) 0.657(4) 1.000 0.094(13) H171 Uiso 0.548(4) -0.127(3) 0.593(3) 1.000 0.066(10) H172 Uiso 0.688(4) -0.172(4) 0.638(4) 1.000 0.078(12) H211 Uiso 0.662(3) 0.207(3) -0.067(3) 1.000 0.032(6) H221 Uiso 0.613(3) 0.417(3) 0.034(2) 1.000 0.030(6) H231 Uiso 0.848(3) 0.554(3) 0.182(3) 1.000 0.033(6) H241 Uiso 1.167(3) 0.503(3) 0.239(3) 1.000 0.029(6) H251 Uiso 1.316(3) 0.362(3) 0.192(3) 1.000 0.043(7) H261 Uiso 1.208(3) 0.159(3) 0.052(3) 1.000 0.047(8) H271 Uiso 0.947(3) 0.110(3) -0.045(3) 1.000 0.035(7) 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 Mo 0.0151(1) 0.0156(1) 0.0174(1) 0.0053(1) 0.0037(1) 0.0031(1) O1 0.0185(7) 0.0291(8) 0.0409(10) 0.0024(7) 0.0059(7) -0.0025(6) O2 0.0436(9) 0.0309(8) 0.0435(11) 0.0015(7) 0.0279(9) 0.0066(7) C1 0.0262(11) 0.0191(9) 0.0225(12) 0.0049(8) 0.0074(9) 0.0098(8) C2 0.0225(10) 0.0176(10) 0.0269(12) 0.0086(8) 0.0042(9) 0.0002(8) C3 0.0217(10) 0.0216(10) 0.0249(12) 0.0093(8) 0.0088(9) 0.0103(8) C4 0.0169(9) 0.0225(10) 0.0226(12) 0.0098(8) 0.0027(8) 0.0080(8) C5 0.0190(10) 0.0285(11) 0.0307(14) 0.0138(9) 0.0016(9) 0.0016(8) C6 0.0310(12) 0.0229(11) 0.0323(15) 0.0036(10) -0.0068(10) -0.0033(9) C7 0.0323(12) 0.0284(11) 0.0201(13) -0.0019(10) -0.0026(10) 0.0034(9) C8 0.0220(10) 0.0230(10) 0.0207(12) 0.0044(8) 0.0014(9) 0.0078(8) C9 0.0186(9) 0.0186(9) 0.0229(12) 0.0055(8) 0.0024(8) 0.0060(7) C10 0.0224(9) 0.0177(9) 0.0190(11) 0.0047(8) 0.0059(8) 0.0084(8) C11 0.0239(10) 0.0222(10) 0.0205(12) 0.0072(8) 0.0065(9) 0.0074(8) C12 0.0308(11) 0.0200(10) 0.0300(14) 0.0082(9) 0.0104(10) 0.0016(9) C13 0.0342(11) 0.0180(10) 0.0273(13) 0.0009(9) 0.0051(10) 0.0029(9) C14 0.0343(11) 0.0220(10) 0.0197(12) 0.0021(9) 0.0066(9) 0.0110(9) C15 0.0228(10) 0.0194(10) 0.0213(12) 0.0066(8) 0.0078(9) 0.0099(8) C16 0.0322(12) 0.0422(14) 0.0260(14) -0.0039(11) 0.0125(11) -0.0025(10) C17 0.062(2) 0.0267(12) 0.028(2) 0.0067(10) 0.0251(13) 0.0000(11) C21 0.0251(10) 0.0220(10) 0.0169(12) 0.0057(8) 0.0036(9) 0.0020(8) C22 0.0224(10) 0.0234(10) 0.0219(12) 0.0106(9) 0.0035(9) 0.0089(8) C23 0.0300(11) 0.0153(9) 0.0229(12) 0.0081(8) 0.0073(9) 0.0036(8) C23A 0.0237(10) 0.0199(10) 0.0226(12) 0.0099(8) 0.0083(9) 0.0008(8) C24 0.0258(11) 0.0317(12) 0.0303(14) 0.0129(10) 0.0055(10) -0.0040(9) C25 0.0210(11) 0.054(2) 0.042(2) 0.0292(13) 0.0124(11) 0.0073(11) C26 0.0379(13) 0.0457(14) 0.045(2) 0.0252(12) 0.0284(13) 0.0208(12) C27 0.0411(13) 0.0286(11) 0.0283(14) 0.0120(10) 0.0198(11) 0.0125(10) C27A 0.0267(10) 0.0216(10) 0.0194(12) 0.0107(8) 0.0095(9) 0.0050(8) #================================================================== # 10. MOLECULAR GEOMETRY #=================================================================== _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo C1 1.941(2) . . yes Mo C2 1.951(2) . . yes Mo C3 2.334(2) . . yes Mo C4 2.372(2) . . yes Mo C5 2.537(2) . . yes Mo C21 2.295(2) . . yes Mo C22 2.286(2) . . yes Mo C23 2.330(2) . . yes Mo C23A 2.476(2) . . yes Mo C27A 2.447(2) . . yes O1 C1 1.159(3) . . yes O2 C2 1.154(3) . . yes C3 C4 1.452(3) . . no C3 C15 1.490(3) . . no C4 C5 1.405(3) . . no C4 C9 1.433(3) . . no C5 C6 1.429(3) . . no C6 C7 1.361(3) . . no C7 C8 1.423(3) . . no C8 C9 1.347(3) . . no C8 C16 1.507(4) . . no C9 C10 1.422(3) . . no C10 C11 1.389(3) . . no C10 C15 1.396(3) . . no C11 C12 1.391(3) . . no C11 C17 1.511(4) . . no C12 C13 1.401(3) . . no C13 C14 1.393(3) . . no C14 C15 1.393(3) . . no C16 C17 1.530(4) . . no C21 C22 1.415(3) . . no C21 C27A 1.433(3) . . no C22 C23 1.409(3) . . no C23 C23A 1.439(3) . . no C23A C24 1.414(3) . . no C23A C27A 1.435(3) . . no C24 C25 1.370(4) . . no C25 C26 1.409(4) . . no C26 C27 1.358(4) . . no C27 C27A 1.418(3) . . no C3 H31 0.95(3) . . no C5 H51 0.97(3) . . no C6 H61 0.91(3) . . no C7 H71 0.89(3) . . no C12 H121 0.94(3) . . no C13 H131 0.94(2) . . no C14 H141 0.94(3) . . no C16 H161 0.94(4) . . no C16 H162 0.93(5) . . no C17 H171 0.91(4) . . no C17 H172 0.89(4) . . no C21 H211 0.94(3) . . no C22 H221 0.87(3) . . no C23 H231 0.96(3) . . no C24 H241 0.90(3) . . no C25 H251 0.91(3) . . no C26 H261 0.93(3) . . no C27 H271 0.92(3) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Mo C2 79.71(8) . . . yes C1 Mo C3 80.13(8) . . . yes C1 Mo C4 96.92(8) . . . yes C1 Mo C5 125.89(8) . . . yes C1 Mo C21 87.76(8) . . . yes C1 Mo C22 94.66(8) . . . yes C1 Mo C23 128.45(8) . . . yes C1 Mo C23A 145.74(8) . . . yes C1 Mo C27A 116.22(8) . . . yes C2 Mo C3 118.56(8) . . . yes C2 Mo C4 91.00(8) . . . yes C2 Mo C5 82.14(8) . . . yes C2 Mo C21 128.33(8) . . . yes C2 Mo C22 95.02(8) . . . yes C2 Mo C23 90.34(8) . . . yes C2 Mo C23A 119.14(8) . . . yes C2 Mo C27A 148.09(8) . . . yes C3 Mo C4 35.93(7) . . . yes C3 Mo C5 65.15(7) . . . yes C3 Mo C21 108.01(7) . . . yes C3 Mo C22 144.00(7) . . . yes C3 Mo C23 144.33(7) . . . yes C3 Mo C23A 109.66(7) . . . yes C3 Mo C27A 92.23(7) . . . yes C4 Mo C5 33.05(7) . . . yes C4 Mo C21 140.47(7) . . . yes C4 Mo C22 167.74(7) . . . yes C4 Mo C23 134.01(7) . . . yes C4 Mo C23A 110.09(7) . . . yes C4 Mo C27A 112.67(7) . . . yes C5 Mo C21 140.67(7) . . . yes C5 Mo C22 137.57(7) . . . yes C5 Mo C23 102.03(7) . . . yes C5 Mo C23A 86.77(7) . . . yes C5 Mo C27A 105.77(7) . . . yes C21 Mo C22 36.00(7) . . . yes C21 Mo C23 59.69(7) . . . yes C21 Mo C23A 58.00(7) . . . yes C21 Mo C27A 35.01(7) . . . yes C22 Mo C23 35.54(7) . . . yes C22 Mo C23A 57.66(7) . . . yes C22 Mo C27A 57.99(7) . . . yes C23 Mo C23A 34.69(7) . . . yes C23 Mo C27A 57.89(7) . . . yes C23A Mo C27A 33.88(7) . . . yes Mo C1 O1 176.55(19) . . . yes Mo C2 O2 178.54(19) . . . yes Mo C3 C4 73.44(11) . . . yes Mo C3 C15 123.37(13) . . . yes C4 C3 C15 105.85(17) . . . no Mo C4 C3 70.63(11) . . . yes Mo C4 C5 79.94(12) . . . yes Mo C4 C9 117.68(14) . . . yes C3 C4 C5 133.80(19) . . . no C3 C4 C9 108.10(17) . . . no C5 C4 C9 117.02(18) . . . no Mo C5 C4 67.01(12) . . . yes Mo C5 C6 126.14(16) . . . yes C4 C5 C6 116.87(19) . . . no C5 C6 C7 123.24(19) . . . no C6 C7 C8 120.89(19) . . . no C7 C8 C9 115.58(19) . . . no C7 C8 C16 127.5(2) . . . no C9 C8 C16 116.9(2) . . . no C4 C9 C8 126.26(19) . . . no C4 C9 C10 107.92(18) . . . no C8 C9 C10 125.81(19) . . . no C9 C10 C11 123.20(19) . . . no C9 C10 C15 110.25(18) . . . no C11 C10 C15 126.54(19) . . . no C10 C11 C12 115.64(19) . . . no C10 C11 C17 116.9(2) . . . no C12 C11 C17 127.5(2) . . . no C11 C12 C13 119.5(2) . . . no C12 C13 C14 123.12(19) . . . no C13 C14 C15 118.6(2) . . . no C3 C15 C10 107.40(17) . . . no C3 C15 C14 136.0(2) . . . no C10 C15 C14 116.55(19) . . . no C8 C16 C17 118.7(3) . . . no C11 C17 C16 118.2(3) . . . no Mo C21 C22 71.67(12) . . . yes Mo C21 C27A 78.32(12) . . . yes C22 C21 C27A 107.59(17) . . . no Mo C22 C21 72.33(12) . . . yes Mo C22 C23 73.94(12) . . . yes C21 C22 C23 109.13(17) . . . no Mo C23 C22 70.52(11) . . . yes Mo C23 C23A 78.19(11) . . . yes C22 C23 C23A 107.83(17) . . . no Mo C23A C23 67.12(11) . . . yes Mo C23A C24 125.16(15) . . . yes Mo C23A C27A 71.97(11) . . . yes C23 C23A C24 133.33(19) . . . no C23 C23A C27A 107.28(17) . . . no C24 C23A C27A 119.38(18) . . . no C23A C24 C25 118.7(2) . . . no C24 C25 C26 121.8(3) . . . no C25 C26 C27 121.3(3) . . . no C26 C27 C27A 118.9(2) . . . no Mo C27A C21 66.68(11) . . . yes Mo C27A C23A 74.15(12) . . . yes Mo C27A C27 123.20(14) . . . yes C21 C27A C23A 107.85(17) . . . no C21 C27A C27 132.18(19) . . . no C23A C27A C27 119.92(19) . . . no Mo C3 H31 101.5(17) . . . no C4 C3 H31 125.3(16) . . . no C15 C3 H31 119.9(17) . . . no Mo C5 H51 90.0(14) . . . no C4 C5 H51 120.9(12) . . . no C6 C5 H51 120.3(12) . . . no C5 C6 H61 116(2) . . . no C7 C6 H61 121(2) . . . no C6 C7 H71 125.9(19) . . . no C8 C7 H71 113.2(19) . . . no C11 C12 H121 119.6(19) . . . no C13 C12 H121 120.8(19) . . . no C12 C13 H131 118.5(14) . . . no C14 C13 H131 118.4(14) . . . no C13 C14 H141 121.3(13) . . . no C15 C14 H141 120.2(14) . . . no C8 C16 H161 106(3) . . . no C8 C16 H162 109(3) . . . no C17 C16 H161 115(2) . . . no C17 C16 H162 107(3) . . . no H161 C16 H162 99(4) . . . no C11 C17 H171 112(2) . . . no C11 C17 H172 109(3) . . . no C16 C17 H171 110.0(19) . . . no C16 C17 H172 105(3) . . . no H171 C17 H172 101(3) . . . no Mo C21 H211 121.4(19) . . . no C22 C21 H211 126.3(18) . . . no C27A C21 H211 125.8(18) . . . no Mo C22 H221 120.6(17) . . . no C21 C22 H221 124.6(17) . . . no C23 C22 H221 126.3(17) . . . no Mo C23 H231 123.9(18) . . . no C22 C23 H231 123.5(18) . . . no C23A C23 H231 128.0(18) . . . no C23A C24 H241 119.1(19) . . . no C25 C24 H241 122.0(19) . . . no C24 C25 H251 115.7(19) . . . no C26 C25 H251 122.5(19) . . . no C25 C26 H261 119.5(19) . . . no C27 C26 H261 119.1(19) . . . no C26 C27 H271 121.9(19) . . . no C27A C27 H271 119.2(19) . . . no # End of Crystallographic Information File #=================================================================== data_ROMX-3077-123 _database_code_CSD 189190 #=================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C26 H16 Mo O2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H16 Mo O2' _chemical_formula_weight 456.33 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 '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' 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' #=================================================================== # 6. CRYSTAL DATA #=================================================================== _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 9.7600(8) _cell_length_b 10.8026(10) _cell_length_c 17.744(2) _cell_angle_alpha 90 _cell_angle_beta 95.899(10) _cell_angle_gamma 90 _cell_volume 1860.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 4934 _cell_measurement_theta_min 11.3 _cell_measurement_theta_max 25.85 _exptl_crystal_description 'fragment' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method none _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 0.725 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min 0.801 _exptl_absorpt_correction_T_max 0.823 _exptl_absorpt_process_details ; Neither decay correction nor absorption correction ; _exptl_special_details ; Diffractometer operator E. Herdtweck exposure_time 120 s per image exposure_phi_range 0-360 exposure_delta_phi 1.5 exposure_sum_images 240 exposure_sum_images_used 1-240 ; _publ_section_exptl_prep ; the crystal was fixed in a capillary with perfluorinated ether and transfered to the diffractometer ; _publ_section_exptl_refinement ; straight forward after integration with the program INTEGRATE; source: 'IPDS (STOE, 1997)' ; #=================================================================== # 7. EXPERIMENTAL DATA #=================================================================== _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'one-circle diffractometer' _diffrn_measurement_device_type 'IPDS (STOE&CIE)' _diffrn_measurement_method 'phi-rotation ' _diffrn_detector 'imaging plate' _diffrn_detector_area_resol_mean 67 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% 0 # number of measured reflections (redundant set) _diffrn_reflns_number 25644 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0141 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.65 _reflns_number_total 3481 _reflns_number_gt 3175 # number of observed reflections (> n sig(I)) _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (STOE, 1997)' _computing_cell_refinement 'IPDS (STOE, 1997)' _computing_data_reduction 'IPDS (STOE, 1997)' _computing_structure_solution 'SIR-92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 1999)' _computing_publication_material 'PLATON (Spek, 1999)' #=================================================================== # 8. REFINEMENT DATA #=================================================================== _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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 sigma _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.9290P] 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_number_reflns 3481 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0249 _refine_ls_R_factor_gt 0.0222 _refine_ls_wR_factor_ref 0.0598 _refine_ls_wR_factor_gt 0.0587 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.65 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.401 _refine_diff_density_min -0.557 _refine_diff_density_rms 0.059 #=================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=================================================================== loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv Mo Mo Uani 0.29348(1) 0.20979(1) 0.095367(8) 1.000 0.0158(1) O1 O Uani 0.54968(16) 0.16353(16) 0.20979(9) 1.000 0.0353(5) O2 O Uani 0.22790(18) 0.34527(15) 0.24117(9) 1.000 0.0381(5) C1 C Uani 0.4560(2) 0.18213(18) 0.16586(11) 1.000 0.0241(6) C2 C Uani 0.2495(2) 0.29538(18) 0.18616(12) 1.000 0.0251(6) C3 C Uani 0.45896(19) 0.30551(17) 0.02767(10) 1.000 0.0185(5) C4 C Uani 0.36581(19) 0.40085(16) 0.04862(10) 1.000 0.0182(5) C5 C Uani 0.2221(2) 0.41626(17) 0.03847(11) 1.000 0.0211(5) C6 C Uani 0.1654(2) 0.51658(19) 0.07970(12) 1.000 0.0250(6) C7 C Uani 0.2418(2) 0.59279(18) 0.12907(12) 1.000 0.0243(6) C8 C Uani 0.38885(19) 0.57621(17) 0.14267(10) 1.000 0.0203(5) C9 C Uani 0.44112(18) 0.48162(17) 0.10274(10) 1.000 0.0175(5) C10 C Uani 0.57884(19) 0.44646(17) 0.11021(10) 1.000 0.0181(5) C11 C Uani 0.67823(19) 0.50808(17) 0.15858(10) 1.000 0.0193(5) C12 C Uani 0.8135(2) 0.46128(19) 0.15865(12) 1.000 0.0243(6) C13 C Uani 0.8368(2) 0.3608(2) 0.11333(13) 1.000 0.0272(6) C14 C Uani 0.7319(2) 0.29906(18) 0.06643(12) 1.000 0.0237(6) C15 C Uani 0.59825(19) 0.34149(17) 0.06488(10) 1.000 0.0194(5) C16 C Uani 0.4897(2) 0.64208(18) 0.19252(11) 1.000 0.0244(6) C17 C Uani 0.6270(2) 0.60965(17) 0.19982(11) 1.000 0.0218(5) C21 C Uani 0.2831(2) -0.00226(18) 0.07722(12) 1.000 0.0253(6) C22 C Uani 0.1764(2) 0.03174(18) 0.12102(12) 1.000 0.0257(6) C23 C Uani 0.0831(2) 0.10879(18) 0.07724(12) 1.000 0.0259(6) C23A C Uani 0.1244(2) 0.11459(17) 0.00194(12) 1.000 0.0245(6) C24 C Uani 0.0678(3) 0.1731(2) -0.06539(15) 1.000 0.0429(8) C25 C Uani 0.1348(4) 0.1586(3) -0.12950(15) 1.000 0.0647(12) C26 C Uani 0.2565(4) 0.0883(3) -0.12895(15) 1.000 0.0576(10) C27 C Uani 0.3150(3) 0.0322(2) -0.06529(14) 1.000 0.0412(8) C27A C Uani 0.2494(2) 0.04432(18) 0.00168(11) 1.000 0.0241(6) H3 H Uiso 0.452(2) 0.265(2) -0.0192(14) 1.000 0.025(6) H5 H Uiso 0.164(2) 0.381(2) -0.0037(12) 1.000 0.022(5) H6 H Uiso 0.067(3) 0.531(2) 0.0700(13) 1.000 0.029(6) H7 H Uiso 0.205(2) 0.661(2) 0.1546(12) 1.000 0.024(6) H12 H Uiso 0.886(2) 0.500(2) 0.1876(13) 1.000 0.028(6) H13 H Uiso 0.933(3) 0.332(2) 0.1136(13) 1.000 0.026(6) H14 H Uiso 0.750(3) 0.228(2) 0.0363(14) 1.000 0.029(6) H16 H Uiso 0.460(2) 0.712(2) 0.2224(14) 1.000 0.027(6) H17 H Uiso 0.688(2) 0.652(2) 0.2341(13) 1.000 0.023(5) H21 H Uiso 0.361(3) -0.058(2) 0.0941(13) 1.000 0.031(6) H22 H Uiso 0.169(3) 0.011(3) 0.1717(15) 1.000 0.040(7) H23 H Uiso 0.002(3) 0.138(2) 0.0945(13) 1.000 0.032(6) H24 H Uiso -0.007(3) 0.213(2) -0.0640(15) 1.000 0.031(7) H25 H Uiso 0.097(4) 0.195(3) -0.169(2) 1.000 0.072(11) H26 H Uiso 0.304(4) 0.078(3) -0.173(2) 1.000 0.074(11) H27 H Uiso 0.401(3) -0.014(3) -0.0645(16) 1.000 0.052(8) 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 Mo 0.0146(1) 0.0148(1) 0.0173(1) 0.0009(1) -0.0016(1) -0.0029(1) O1 0.0314(8) 0.0383(9) 0.0325(8) 0.0078(7) -0.0145(7) -0.0018(7) O2 0.0535(11) 0.0341(9) 0.0293(8) -0.0096(7) 0.0167(7) -0.0147(8) C1 0.0258(11) 0.0210(9) 0.0249(10) 0.0034(8) -0.0008(8) -0.0054(8) C2 0.0268(11) 0.0228(10) 0.0259(10) 0.0037(8) 0.0040(8) -0.0095(8) C3 0.0179(9) 0.0196(9) 0.0182(9) -0.0010(7) 0.0032(7) -0.0030(7) C4 0.0212(9) 0.0138(8) 0.0193(8) 0.0038(7) 0.0008(7) -0.0026(7) C5 0.0202(9) 0.0178(9) 0.0240(9) 0.0031(7) -0.0033(7) -0.0026(7) C6 0.0162(9) 0.0241(10) 0.0342(11) 0.0029(8) -0.0003(8) 0.0022(8) C7 0.0202(10) 0.0199(9) 0.0332(10) -0.0013(8) 0.0047(8) 0.0045(8) C8 0.0175(9) 0.0187(9) 0.0247(9) 0.0001(7) 0.0019(7) -0.0007(7) C9 0.0160(9) 0.0171(9) 0.0193(9) 0.0025(7) 0.0017(7) -0.0040(7) C10 0.0177(9) 0.0172(8) 0.0201(9) 0.0010(7) 0.0051(7) -0.0018(7) C11 0.0188(9) 0.0186(9) 0.0207(9) 0.0003(7) 0.0024(7) -0.0012(7) C12 0.0167(9) 0.0249(10) 0.0309(10) -0.0026(8) 0.0001(8) -0.0027(8) C13 0.0156(9) 0.0247(10) 0.0416(11) -0.0024(9) 0.0049(8) 0.0011(8) C14 0.0195(10) 0.0202(10) 0.0320(11) -0.0044(8) 0.0059(8) 0.0001(7) C15 0.0196(9) 0.0172(9) 0.0217(9) -0.0004(7) 0.0039(7) -0.0031(7) C16 0.0240(10) 0.0210(9) 0.0285(10) -0.0066(8) 0.0042(8) -0.0010(8) C17 0.0192(9) 0.0211(9) 0.0245(9) -0.0057(8) -0.0010(7) -0.0049(8) C21 0.0231(10) 0.0135(9) 0.0373(11) -0.0016(8) -0.0071(8) -0.0005(8) C22 0.0320(11) 0.0175(9) 0.0272(10) 0.0019(8) 0.0006(8) -0.0103(8) C23 0.0173(10) 0.0186(9) 0.0416(12) -0.0041(8) 0.0027(8) -0.0062(8) C23A 0.0238(10) 0.0150(9) 0.0323(10) -0.0012(8) -0.0089(8) -0.0092(8) C24 0.0507(16) 0.0217(11) 0.0488(15) 0.0083(10) -0.0307(12) -0.0147(11) C25 0.115(3) 0.0415(16) 0.0290(14) 0.0148(12) -0.0335(17) -0.0466(19) C26 0.093(2) 0.0504(17) 0.0305(13) -0.0127(12) 0.0119(15) -0.0434(18) C27 0.0506(15) 0.0373(13) 0.0376(13) -0.0180(10) 0.0141(11) -0.0224(12) C27A 0.0242(10) 0.0173(9) 0.0304(10) -0.0055(7) 0.0005(8) -0.0074(8) #================================================================== # 10. MOLECULAR GEOMETRY #=================================================================== _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All esds are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo C1 1.940(2) . . yes Mo C2 1.943(2) . . yes Mo C3 2.3494(19) . . yes Mo C4 2.3594(18) . . yes Mo C5 2.5169(19) . . yes Mo C21 2.314(2) . . yes Mo C22 2.306(2) . . yes Mo C23 2.318(2) . . yes Mo C23A 2.443(2) . . yes Mo C27A 2.449(2) . . yes O1 C1 1.156(3) . . yes O2 C2 1.153(3) . . yes C3 C4 1.447(3) . . no C3 C15 1.500(3) . . no C4 C5 1.406(3) . . no C4 C9 1.442(3) . . no C5 C6 1.449(3) . . no C6 C7 1.366(3) . . no C7 C8 1.442(3) . . no C8 C9 1.371(3) . . no C8 C16 1.442(3) . . no C9 C10 1.390(3) . . no C10 C11 1.396(3) . . no C10 C15 1.414(3) . . no C11 C12 1.414(3) . . no C11 C17 1.437(3) . . no C12 C13 1.384(3) . . no C13 C14 1.418(3) . . no C14 C15 1.380(3) . . no C16 C17 1.378(3) . . no C21 C22 1.411(3) . . no C21 C27A 1.438(3) . . no C22 C23 1.407(3) . . no C23 C23A 1.436(3) . . no C23A C24 1.413(3) . . no C23A C27A 1.437(3) . . no C24 C25 1.378(4) . . no C25 C26 1.409(5) . . no C26 C27 1.355(4) . . no C27 C27A 1.413(3) . . no C3 H3 0.94(2) . . no C5 H5 0.97(2) . . no C6 H6 0.97(3) . . no C7 H7 0.95(2) . . no C12 H12 0.93(2) . . no C13 H13 0.99(3) . . no C14 H14 0.96(2) . . no C16 H16 0.98(2) . . no C17 H17 0.93(2) . . no C21 H21 0.99(3) . . no C22 H22 0.94(3) . . no C23 H23 0.93(3) . . no C24 H24 0.85(3) . . no C25 H25 0.85(4) . . no C26 H26 0.96(4) . . no C27 H27 0.98(3) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Mo C2 76.96(8) . . . yes C1 Mo C3 80.67(7) . . . yes C1 Mo C4 96.15(7) . . . yes C1 Mo C5 124.72(7) . . . yes C1 Mo C21 87.62(8) . . . yes C1 Mo C22 97.65(8) . . . yes C1 Mo C23 132.14(8) . . . yes C1 Mo C23A 145.43(7) . . . yes C1 Mo C27A 113.59(7) . . . yes C2 Mo C3 115.88(7) . . . yes C2 Mo C4 88.56(7) . . . yes C2 Mo C5 80.52(7) . . . yes C2 Mo C21 125.18(8) . . . yes C2 Mo C22 94.42(8) . . . yes C2 Mo C23 94.07(8) . . . yes C2 Mo C23A 124.86(8) . . . yes C2 Mo C27A 150.66(7) . . . yes C3 Mo C4 35.80(6) . . . yes C3 Mo C5 65.25(6) . . . yes C3 Mo C21 112.77(7) . . . yes C3 Mo C22 148.05(7) . . . yes C3 Mo C23 141.43(7) . . . yes C3 Mo C23A 106.87(7) . . . yes C3 Mo C27A 93.22(6) . . . yes C4 Mo C5 33.31(6) . . . yes C4 Mo C21 145.84(7) . . . yes C4 Mo C22 166.20(7) . . . yes C4 Mo C23 130.97(7) . . . yes C4 Mo C23A 109.60(6) . . . yes C4 Mo C27A 115.97(6) . . . yes C5 Mo C21 144.60(7) . . . yes C5 Mo C22 134.10(7) . . . yes C5 Mo C23 99.02(7) . . . yes C5 Mo C23A 87.77(6) . . . yes C5 Mo C27A 110.64(6) . . . yes C21 Mo C22 35.55(7) . . . yes C21 Mo C23 59.29(7) . . . yes C21 Mo C23A 58.12(7) . . . yes C21 Mo C27A 35.00(7) . . . yes C22 Mo C23 35.43(7) . . . yes C22 Mo C23A 57.93(7) . . . yes C22 Mo C27A 57.94(7) . . . yes C23 Mo C23A 34.99(7) . . . yes C23 Mo C27A 58.06(7) . . . yes C23A Mo C27A 34.17(6) . . . yes Mo C1 O1 177.35(17) . . . yes Mo C2 O2 177.65(18) . . . yes Mo C3 C4 72.47(10) . . . yes Mo C3 C15 121.90(12) . . . yes C4 C3 C15 105.50(15) . . . no Mo C4 C3 71.72(10) . . . yes Mo C4 C5 79.51(11) . . . yes Mo C4 C9 116.47(12) . . . yes C3 C4 C5 134.13(17) . . . no C3 C4 C9 108.12(16) . . . no C5 C4 C9 116.58(16) . . . no Mo C5 C4 67.18(10) . . . yes Mo C5 C6 124.38(14) . . . yes C4 C5 C6 116.86(17) . . . no C5 C6 C7 124.25(18) . . . no C6 C7 C8 120.05(18) . . . no C7 C8 C9 115.01(17) . . . no C7 C8 C16 130.27(17) . . . no C9 C8 C16 114.71(17) . . . no C4 C9 C8 127.14(17) . . . no C4 C9 C10 108.66(16) . . . no C8 C9 C10 124.18(17) . . . no C9 C10 C11 122.16(17) . . . no C9 C10 C15 110.46(16) . . . no C11 C10 C15 127.35(17) . . . no C10 C11 C12 114.82(17) . . . no C10 C11 C17 114.89(17) . . . no C12 C11 C17 130.28(18) . . . no C11 C12 C13 119.30(18) . . . no C12 C13 C14 123.94(18) . . . no C13 C14 C15 118.65(18) . . . no C3 C15 C10 106.84(16) . . . no C3 C15 C14 137.27(17) . . . no C10 C15 C14 115.88(17) . . . no C8 C16 C17 121.88(18) . . . no C11 C17 C16 122.15(18) . . . no Mo C21 C22 71.93(11) . . . yes Mo C21 C27A 77.63(11) . . . yes C22 C21 C27A 108.14(17) . . . no Mo C22 C21 72.52(11) . . . yes Mo C22 C23 72.74(11) . . . yes C21 C22 C23 108.81(18) . . . no Mo C23 C22 71.83(11) . . . yes Mo C23 C23A 77.25(11) . . . yes C22 C23 C23A 108.17(17) . . . no Mo C23A C23 67.76(11) . . . yes Mo C23A C24 124.31(15) . . . yes Mo C23A C27A 73.15(11) . . . yes C23 C23A C24 133.1(2) . . . no C23 C23A C27A 107.42(17) . . . no C24 C23A C27A 119.5(2) . . . no C23A C24 C25 118.0(3) . . . no C24 C25 C26 121.8(3) . . . no C25 C26 C27 122.0(3) . . . no C26 C27 C27A 118.1(3) . . . no Mo C27A C21 67.37(11) . . . yes Mo C27A C23A 72.68(11) . . . yes Mo C27A C27 125.14(15) . . . yes C21 C27A C23A 107.14(17) . . . no C21 C27A C27 132.2(2) . . . no C23A C27A C27 120.66(19) . . . no Mo C3 H3 104.9(13) . . . no C4 C3 H3 124.8(13) . . . no C15 C3 H3 119.5(12) . . . no Mo C5 H5 94.4(13) . . . no C4 C5 H5 123.3(12) . . . no C6 C5 H5 117.4(12) . . . no C5 C6 H6 116.9(13) . . . no C7 C6 H6 118.8(13) . . . no C6 C7 H7 124.2(12) . . . no C8 C7 H7 115.7(12) . . . no C11 C12 H12 119.8(13) . . . no C13 C12 H12 120.8(13) . . . no C12 C13 H13 117.2(13) . . . no C14 C13 H13 118.9(13) . . . no C13 C14 H14 122.6(17) . . . no C15 C14 H14 118.8(17) . . . no C8 C16 H16 119.3(12) . . . no C17 C16 H16 118.8(12) . . . no C11 C17 H17 118.5(13) . . . no C16 C17 H17 119.3(13) . . . no Mo C21 H21 122.5(14) . . . no C22 C21 H21 125.3(14) . . . no C27A C21 H21 126.1(14) . . . no Mo C22 H22 118.5(19) . . . no C21 C22 H22 126.9(19) . . . no C23 C22 H22 124.2(19) . . . no Mo C23 H23 124.4(15) . . . no C22 C23 H23 122.8(14) . . . no C23A C23 H23 128.3(14) . . . no C23A C24 H24 117.7(18) . . . no C25 C24 H24 124.3(18) . . . no C24 C25 H25 115(3) . . . no C26 C25 H25 123(3) . . . no C25 C26 H26 122(2) . . . no C27 C26 H26 116(2) . . . no C26 C27 H27 121.9(17) . . . no C27A C27 H27 119.9(17) . . . no # End of Crystallographic Information File