#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2001 data_p25 _database_code_CSD 159215 _journal_coden_Cambridge 186 # 1. SUBMISSION DETAILS _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'le Grognec, Erwan' 'Rinaldo Poli' 'Philippe Richard' _publ_contact_author_name 'Prof Rinaldo Poli' _publ_contact_author_address ; Prof Rinaldo Poli Laboratoire de Syntheses et d'Electrosynthese Organometalliques Universite de Bourgogne Faculte des Sciences "Gabriel" 6 Boulevard Gabriel 21000 Dijon FRANCE ; _publ_contact_author_email 'poli@satie.u-bourgogne.fr' _publ_contact_author_fax '+33-0380396098' _publ_contact_author_phone '+33-0380396881' _publ_section_title ; A reinvestigation of compound CpMo(PMe3)2(CH3)2: An alkylation by single electron transfer and radical addition? ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H29 Mo P2' _chemical_formula_weight 343.24 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' 'P' 'P' 0.1023 0.0942 '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 P21/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 13.0760(4) _cell_length_b 10.0550(5) _cell_length_c 12.7220(4) _cell_angle_alpha 90.00 _cell_angle_beta 86.809(2) _cell_angle_gamma 90.00 _cell_volume 1670.08(11) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 6715 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 0.955 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_method 'KappaCCD' _diffrn_reflns_number 13262 _diffrn_reflns_av_R_equivalents 0.0025 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 27.48 _reflns_number_total 3761 _reflns_number_gt 3475 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_cell_refinement 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP3 _computing_publication_material ? _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^)+(0.0190P)^2^+1.6638P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _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 3761 _refine_ls_number_parameters 261 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0271 _refine_ls_R_factor_gt 0.0239 _refine_ls_wR_factor_ref 0.0583 _refine_ls_wR_factor_gt 0.0563 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.006 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo Mo -0.287041(11) 0.037637(15) 0.316241(11) 0.01182(6) Uani 1 1 d . . . P1 P -0.28163(4) -0.20007(5) 0.35659(4) 0.01586(11) Uani 1 1 d . . . P2 P -0.15769(4) 0.21006(5) 0.33587(4) 0.01723(11) Uani 1 1 d . . . C1 C -0.38761(17) 0.0842(3) 0.17077(17) 0.0294(5) Uani 1 1 d . . . C2 C -0.43722(17) -0.0113(3) 0.2360(2) 0.0313(5) Uani 1 1 d . . . C3 C -0.45817(16) 0.0465(2) 0.33705(19) 0.0295(5) Uani 1 1 d . . . C4 C -0.42022(16) 0.1795(2) 0.33259(18) 0.0279(5) Uani 1 1 d . . . C5 C -0.37620(16) 0.2010(2) 0.22907(18) 0.0264(5) Uani 1 1 d . . . C6 C -0.16568(17) -0.0314(2) 0.19363(16) 0.0212(4) Uani 1 1 d . . . C7 C -0.27828(19) 0.0427(2) 0.49376(16) 0.0228(4) Uani 1 1 d . . . C8 C -0.2829(2) -0.3208(2) 0.24946(18) 0.0304(5) Uani 1 1 d . . . C9 C -0.16709(18) -0.2501(2) 0.42260(18) 0.0273(5) Uani 1 1 d . . . C10 C -0.38389(18) -0.2691(2) 0.44402(18) 0.0285(5) Uani 1 1 d . . . C11 C -0.11496(18) 0.3094(3) 0.22097(18) 0.0291(5) Uani 1 1 d . . . C12 C -0.03539(18) 0.1510(3) 0.3807(2) 0.0330(5) Uani 1 1 d . . . C13 C -0.1874(2) 0.3442(2) 0.4295(2) 0.0354(5) Uani 1 1 d . . . H1 H -0.364(2) 0.071(3) 0.099(2) 0.050(8) Uiso 1 1 d . . . H2 H -0.455(2) -0.095(3) 0.213(2) 0.046(8) Uiso 1 1 d . . . H3 H -0.493(2) 0.009(3) 0.389(2) 0.046(8) Uiso 1 1 d . . . H4 H -0.4252(19) 0.240(3) 0.383(2) 0.035(7) Uiso 1 1 d . . . H5 H -0.350(2) 0.273(3) 0.203(2) 0.033(7) Uiso 1 1 d . . . H6A H -0.197(2) -0.074(3) 0.139(2) 0.039(7) Uiso 1 1 d . . . H6B H -0.118(2) -0.086(3) 0.221(2) 0.039(7) Uiso 1 1 d . . . H6C H -0.128(3) 0.031(3) 0.156(3) 0.058(10) Uiso 1 1 d . . . H7A H -0.215(2) 0.048(3) 0.518(2) 0.035(7) Uiso 1 1 d . . . H7B H -0.308(2) -0.029(3) 0.531(2) 0.040(8) Uiso 1 1 d . . . H7C H -0.316(2) 0.115(3) 0.522(2) 0.053(9) Uiso 1 1 d . . . H8A H -0.228(2) -0.305(3) 0.199(2) 0.040(8) Uiso 1 1 d . . . H8B H -0.347(2) -0.318(3) 0.216(2) 0.043(8) Uiso 1 1 d . . . H8C H -0.277(2) -0.408(3) 0.275(2) 0.041(7) Uiso 1 1 d . . . H9A H -0.110(2) -0.232(3) 0.374(2) 0.043(8) Uiso 1 1 d . . . H9B H -0.1691(19) -0.337(3) 0.441(2) 0.035(7) Uiso 1 1 d . . . H9C H -0.165(2) -0.202(3) 0.490(2) 0.043(8) Uiso 1 1 d . . . H10A H -0.447(2) -0.261(3) 0.411(2) 0.052(9) Uiso 1 1 d . . . H10B H -0.3893(19) -0.219(3) 0.510(2) 0.034(7) Uiso 1 1 d . . . H10C H -0.372(2) -0.359(3) 0.457(2) 0.042(8) Uiso 1 1 d . . . H11A H -0.089(2) 0.250(3) 0.169(2) 0.046(8) Uiso 1 1 d . . . H11B H -0.060(2) 0.366(3) 0.235(2) 0.037(7) Uiso 1 1 d . . . H11C H -0.174(2) 0.364(3) 0.198(2) 0.042(7) Uiso 1 1 d . . . H12A H -0.006(2) 0.091(3) 0.330(2) 0.051(9) Uiso 1 1 d . . . H12B H -0.046(2) 0.103(3) 0.446(2) 0.046(8) Uiso 1 1 d . . . H12C H 0.010(2) 0.223(3) 0.392(2) 0.042(8) Uiso 1 1 d . . . H13A H -0.248(2) 0.396(3) 0.407(2) 0.038(7) Uiso 1 1 d . . . H13B H -0.132(2) 0.405(3) 0.432(2) 0.042(8) Uiso 1 1 d . . . H13C H -0.204(2) 0.306(3) 0.500(2) 0.048(8) 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 Mo 0.01135(9) 0.01300(9) 0.01109(9) 0.00036(5) -0.00052(6) 0.00081(5) P1 0.0184(2) 0.0144(2) 0.0151(2) 0.00077(17) -0.00352(17) -0.00092(18) P2 0.0193(2) 0.0147(2) 0.0182(2) 0.00157(18) -0.00534(18) -0.00192(18) C1 0.0234(11) 0.0436(14) 0.0222(10) 0.0023(9) -0.0104(8) 0.0082(10) C2 0.0233(11) 0.0259(12) 0.0468(14) 0.0029(10) -0.0216(10) 0.0007(9) C3 0.0112(10) 0.0390(13) 0.0379(12) 0.0161(10) 0.0027(9) 0.0012(9) C4 0.0227(11) 0.0286(12) 0.0322(11) -0.0008(9) -0.0003(9) 0.0148(9) C5 0.0164(10) 0.0275(11) 0.0359(11) 0.0156(9) -0.0075(8) 0.0021(8) C6 0.0240(11) 0.0222(11) 0.0167(9) -0.0004(8) 0.0045(8) 0.0009(8) C7 0.0317(12) 0.0212(11) 0.0154(9) -0.0007(8) -0.0003(8) -0.0025(9) C8 0.0477(15) 0.0188(11) 0.0253(10) -0.0034(9) -0.0067(10) 0.0001(10) C9 0.0273(12) 0.0251(11) 0.0301(11) 0.0086(9) -0.0082(9) 0.0036(9) C10 0.0292(12) 0.0261(12) 0.0301(11) 0.0061(9) -0.0007(9) -0.0092(9) C11 0.0276(12) 0.0287(12) 0.0312(11) 0.0101(10) -0.0043(9) -0.0113(10) C12 0.0244(11) 0.0286(12) 0.0477(14) 0.0084(11) -0.0186(10) -0.0065(10) C13 0.0554(16) 0.0176(11) 0.0332(12) -0.0056(9) -0.0038(11) -0.0043(11) _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 Mo C3 2.240(2) . ? Mo C4 2.251(2) . ? Mo C7 2.268(2) . ? Mo C6 2.271(2) . ? Mo C2 2.316(2) . ? Mo C5 2.330(2) . ? Mo C1 2.3759(19) . ? Mo P2 2.4446(5) . ? Mo P1 2.4465(5) . ? P1 C8 1.826(2) . ? P1 C10 1.828(2) . ? P1 C9 1.828(2) . ? P2 C12 1.826(2) . ? P2 C13 1.827(2) . ? P2 C11 1.832(2) . ? C1 C5 1.401(3) . ? C1 C2 1.404(4) . ? C2 C3 1.424(4) . ? C3 C4 1.426(3) . ? C4 C5 1.424(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 C3 Mo C4 37.02(9) . . ? C3 Mo C7 89.25(9) . . ? C4 Mo C7 88.60(8) . . ? C3 Mo C6 138.46(9) . . ? C4 Mo C6 139.85(8) . . ? C7 Mo C6 128.22(8) . . ? C3 Mo C2 36.37(9) . . ? C4 Mo C2 60.32(9) . . ? C7 Mo C2 122.34(9) . . ? C6 Mo C2 102.09(9) . . ? C3 Mo C5 60.35(8) . . ? C4 Mo C5 36.17(8) . . ? C7 Mo C5 120.83(8) . . ? C6 Mo C5 103.74(8) . . ? C2 Mo C5 58.72(8) . . ? C3 Mo C1 59.45(8) . . ? C4 Mo C1 59.22(8) . . ? C7 Mo C1 146.31(8) . . ? C6 Mo C1 85.47(8) . . ? C2 Mo C1 34.79(9) . . ? C5 Mo C1 34.62(8) . . ? C3 Mo P2 130.68(7) . . ? C4 Mo P2 94.44(7) . . ? C7 Mo P2 78.98(6) . . ? C6 Mo P2 79.97(6) . . ? C2 Mo P2 143.52(6) . . ? C5 Mo P2 85.19(6) . . ? C1 Mo P2 110.85(6) . . ? C3 Mo P1 93.12(6) . . ? C4 Mo P1 129.10(6) . . ? C7 Mo P1 79.01(6) . . ? C6 Mo P1 79.53(6) . . ? C2 Mo P1 85.42(6) . . ? C5 Mo P1 144.04(6) . . ? C1 Mo P1 112.32(6) . . ? P2 Mo P1 130.029(17) . . ? C8 P1 C10 99.50(12) . . ? C8 P1 C9 101.63(12) . . ? C10 P1 C9 101.91(11) . . ? C8 P1 Mo 119.43(8) . . ? C10 P1 Mo 118.02(8) . . ? C9 P1 Mo 113.53(8) . . ? C12 P2 C13 101.23(13) . . ? C12 P2 C11 101.11(12) . . ? C13 P2 C11 99.34(12) . . ? C12 P2 Mo 115.10(8) . . ? C13 P2 Mo 117.83(9) . . ? C11 P2 Mo 119.15(8) . . ? C5 C1 C2 108.6(2) . . ? C5 C1 Mo 70.90(11) . . ? C2 C1 Mo 70.28(12) . . ? C1 C2 C3 108.3(2) . . ? C1 C2 Mo 74.94(12) . . ? C3 C2 Mo 68.92(12) . . ? C2 C3 C4 107.3(2) . . ? C2 C3 Mo 74.71(12) . . ? C4 C3 Mo 71.92(12) . . ? C5 C4 C3 107.5(2) . . ? C5 C4 Mo 74.93(12) . . ? C3 C4 Mo 71.07(12) . . ? C1 C5 C4 108.2(2) . . ? C1 C5 Mo 74.47(12) . . ? C4 C5 Mo 68.90(11) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.520 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.072