# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Kevin John' _publ_contact_author_email KJOHN@LANL.GOV _publ_section_title ; Interplay of Metal-Allyl and Metal-Metal Bonding in Dimolybdenum Allyl Complexes ; loop_ _publ_author_name 'Kevin John' 'R Baker' 'Kevin D John' 'Richard L Martin' 'Stephen J Obrey' 'Alfred P. Sattelberger' ; B.L.Scott ; 'Ryan J Trovitch' # Attachment 'ccd439.cif' data_ccd439 _database_code_depnum_ccdc_archive 'CCDC 729110' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H38 Mo2 P2' _chemical_formula_weight 508.30 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 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.7554(7) _cell_length_b 8.8269(6) _cell_length_c 11.9842(8) _cell_angle_alpha 90.00 _cell_angle_beta 108.5150(10) _cell_angle_gamma 90.00 _cell_volume 1078.85(12) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 1.307 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6649 _exptl_absorpt_correction_T_max 0.7359 _exptl_absorpt_process_details 'SADABS 2.03 (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 141(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 'Bruker SMART 1k CCD' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5780 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.99 _reflns_number_total 2318 _reflns_number_gt 1921 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 4.210 (Bruker, 1996)' _computing_cell_refinement 'SAINT 4.05 (Bruker, 1996)' _computing_data_reduction 'SAINT 4.05 (Bruker, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 6.10 (Bruker, 2001)' _computing_publication_material 'SHELXTL 6.10 (Bruker, 2001)' _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^)+(0.0617P)^2^+5.7269P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2318 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1403 _refine_ls_wR_factor_gt 0.1323 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo Mo 0.44914(5) 0.06798(6) 0.06609(4) 0.02505(19) Uani 1 1 d . . . P P 0.27354(17) -0.1132(2) 0.04378(16) 0.0330(4) Uani 1 1 d . . . C1 C 0.5331(9) 0.3045(11) 0.1507(10) 0.075(3) Uani 1 1 d . . . H1A H 0.5319 0.3236 0.2301 0.090 Uiso 1 1 calc R . . H1B H 0.6114 0.3413 0.1359 0.090 Uiso 1 1 calc R . . C2 C 0.4010(11) 0.3244(11) 0.0496(12) 0.083(3) Uani 1 1 d . . . H2A H 0.4031 0.3764 -0.0220 0.100 Uiso 1 1 calc R . . C3 C 0.2839(9) 0.2455(10) 0.0456(11) 0.075(3) Uani 1 1 d . . . H3A H 0.2140 0.2463 -0.0292 0.090 Uiso 1 1 calc R . . H3B H 0.2531 0.2587 0.1128 0.090 Uiso 1 1 calc R . . C4 C 0.6095(8) -0.1132(9) 0.1412(6) 0.0450(18) Uani 1 1 d . . . H4A H 0.5807 -0.2139 0.1540 0.054 Uiso 1 1 calc R . . H4B H 0.6851 -0.1115 0.1136 0.054 Uiso 1 1 calc R . . C5 C 0.6003(10) 0.0137(14) 0.2290(8) 0.073(3) Uani 1 1 d . . . H5A H 0.6737 0.0831 0.2626 0.087 Uiso 1 1 calc R . . C6 C 0.4798(9) 0.0240(14) 0.2635(7) 0.073(3) Uani 1 1 d . . . H6A H 0.4720 0.1102 0.3111 0.087 Uiso 1 1 calc R . . H6B H 0.4450 -0.0698 0.2838 0.087 Uiso 1 1 calc R . . C7 C 0.1564(7) -0.1429(10) -0.1023(7) 0.0484(18) Uani 1 1 d . . . H7A H 0.0929 -0.2172 -0.0980 0.073 Uiso 1 1 calc R . . H7B H 0.2018 -0.1779 -0.1546 0.073 Uiso 1 1 calc R . . H7C H 0.1127 -0.0492 -0.1313 0.073 Uiso 1 1 calc R . . C8 C 0.3134(8) -0.3097(9) 0.0925(8) 0.054(2) Uani 1 1 d . . . H8A H 0.2338 -0.3669 0.0776 0.082 Uiso 1 1 calc R . . H8B H 0.3606 -0.3110 0.1753 0.082 Uiso 1 1 calc R . . H8C H 0.3665 -0.3539 0.0501 0.082 Uiso 1 1 calc R . . C9 C 0.1604(7) -0.0653(9) 0.1252(7) 0.0477(18) Uani 1 1 d . . . H9A H 0.0940 -0.1421 0.1120 0.071 Uiso 1 1 calc R . . H9B H 0.1199 0.0307 0.0986 0.071 Uiso 1 1 calc R . . H9C H 0.2080 -0.0596 0.2078 0.071 Uiso 1 1 calc R . . 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 0.0296(3) 0.0239(3) 0.0216(3) -0.0013(2) 0.0081(2) 0.0024(2) P 0.0358(9) 0.0325(9) 0.0337(9) -0.0013(7) 0.0153(7) -0.0026(7) C1 0.062(5) 0.066(6) 0.109(8) -0.055(6) 0.046(6) -0.021(5) C2 0.096(8) 0.042(5) 0.123(10) 0.006(6) 0.051(7) 0.013(5) C3 0.054(5) 0.051(5) 0.130(9) 0.036(6) 0.044(6) 0.017(4) C4 0.050(4) 0.042(4) 0.037(4) 0.012(3) 0.006(3) 0.005(3) C5 0.068(6) 0.096(8) 0.051(5) 0.008(5) 0.015(5) -0.006(6) C6 0.062(5) 0.125(9) 0.029(4) 0.010(5) 0.012(4) -0.027(6) C7 0.043(4) 0.058(5) 0.043(4) -0.012(4) 0.013(3) -0.010(4) C8 0.065(5) 0.034(4) 0.074(6) 0.014(4) 0.036(5) 0.002(4) C9 0.046(4) 0.058(5) 0.047(4) -0.004(4) 0.027(3) -0.003(4) _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 C5 2.161(10) . ? Mo C4 2.314(7) . ? Mo C6 2.316(8) . ? Mo C2 2.317(9) . ? Mo C3 2.323(8) . ? Mo C1 2.371(8) . ? Mo C4 2.394(7) 3_655 ? Mo P 2.4240(18) . ? Mo Mo 2.4994(10) 3_655 ? P C7 1.822(7) . ? P C9 1.835(7) . ? P C8 1.837(8) . ? C1 C2 1.557(15) . ? C2 C3 1.426(14) . ? C4 C5 1.562(14) . ? C5 C6 1.483(13) . ? 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 C5 Mo C4 40.7(4) . . ? C5 Mo C6 38.5(3) . . ? C4 Mo C6 68.9(3) . . ? C5 Mo C2 112.2(5) . . ? C4 Mo C2 145.8(4) . . ? C6 Mo C2 101.9(5) . . ? C5 Mo C3 125.1(4) . . ? C4 Mo C3 163.3(3) . . ? C6 Mo C3 94.4(4) . . ? C2 Mo C3 35.8(3) . . ? C5 Mo C1 74.6(4) . . ? C4 Mo C1 107.8(3) . . ? C6 Mo C1 78.4(4) . . ? C2 Mo C1 38.8(4) . . ? C3 Mo C1 68.0(3) . . ? C5 Mo C4 148.1(3) . 3_655 ? C4 Mo C4 115.91(18) . 3_655 ? C6 Mo C4 173.3(3) . 3_655 ? C2 Mo C4 76.8(4) . 3_655 ? C3 Mo C4 80.6(4) . 3_655 ? C1 Mo C4 103.7(4) . 3_655 ? C5 Mo P 106.8(3) . . ? C4 Mo P 92.6(2) . . ? C6 Mo P 81.7(2) . . ? C2 Mo P 119.3(3) . . ? C3 Mo P 83.7(2) . . ? C1 Mo P 143.7(2) . . ? C4 Mo P 93.2(2) 3_655 . ? C5 Mo Mo 96.4(3) . 3_655 ? C4 Mo Mo 59.51(19) . 3_655 ? C6 Mo Mo 128.2(3) . 3_655 ? C2 Mo Mo 123.1(3) . 3_655 ? C3 Mo Mo 137.0(3) . 3_655 ? C1 Mo Mo 120.7(2) . 3_655 ? C4 Mo Mo 56.40(19) 3_655 3_655 ? P Mo Mo 95.50(5) . 3_655 ? C7 P C9 99.8(4) . . ? C7 P C8 101.0(4) . . ? C9 P C8 100.1(4) . . ? C7 P Mo 118.5(3) . . ? C9 P Mo 114.5(3) . . ? C8 P Mo 119.5(3) . . ? C2 C1 Mo 68.7(5) . . ? C3 C2 C1 123.3(10) . . ? C3 C2 Mo 72.4(5) . . ? C1 C2 Mo 72.5(5) . . ? C2 C3 Mo 71.8(5) . . ? C5 C4 Mo 64.4(5) . . ? C6 C5 C4 118.7(9) . . ? C6 C5 Mo 76.4(5) . . ? C4 C5 Mo 75.0(5) . . ? C5 C6 Mo 65.1(5) . . ? _diffrn_measured_fraction_theta_max 0.889 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.097 _refine_diff_density_min -0.968 _refine_diff_density_rms 0.151 # Attachment 'ccd7411.cif' data_ccd741 _database_code_depnum_ccdc_archive 'CCDC 729811' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H50 Mo2 O2 P2' _chemical_formula_weight 600.44 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' O O 0.0106 0.0060 '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 'P 2/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 11.935(3) _cell_length_b 8.710(2) _cell_length_c 14.177(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.592(5) _cell_angle_gamma 90.00 _cell_volume 1460.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 141(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description slab _exptl_crystal_colour green _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 0.982 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7189 _exptl_absorpt_correction_T_max 0.9256 _exptl_absorpt_process_details 'SADABS 2.03 (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 141(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 'Bruker SMART 1k CCD' _diffrn_measurement_method '\f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8736 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.37 _reflns_number_total 2666 _reflns_number_gt 2125 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 4.210 (Bruker, 1996)' _computing_cell_refinement 'SAINT 4.05 (Bruker, 1996)' _computing_data_reduction 'SAINT 4.05 (Bruker, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 6.10 (Bruker, 2001)' _computing_publication_material 'SHELXTL 6.10 (Bruker, 2001)' _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^)+(0.0421P)^2^+4.8153P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2666 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0936 _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.1395 _refine_ls_wR_factor_gt 0.1318 _refine_ls_goodness_of_fit_ref 1.194 _refine_ls_restrained_S_all 1.194 _refine_ls_shift/su_max 0.000 _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 0.70033(5) 0.95323(7) 0.17849(4) 0.0407(2) Uani 0.881(2) 1 d P . . P1 P 0.53548(15) 0.7630(2) 0.17085(14) 0.0495(5) Uani 1 1 d . . . O1 O 0.7402(5) 0.8072(7) 0.0802(4) 0.0766(17) Uani 1 1 d . . . C1A C 0.7962(7) 1.1409(11) 0.1243(7) 0.088(3) Uani 1 1 d . . . H1AA H 0.7726 1.2417 0.1408 0.106 Uiso 1 1 d R . . H1AB H 0.8068 1.1332 0.0585 0.106 Uiso 1 1 d R . . C1P C 0.4621(7) 0.7713(11) 0.0519(6) 0.081(3) Uani 1 1 d . . . H1PA H 0.3994 0.7014 0.0460 0.122 Uiso 1 1 calc R . . H1PB H 0.5129 0.7433 0.0075 0.122 Uiso 1 1 calc R . . H1PC H 0.4349 0.8738 0.0385 0.122 Uiso 1 1 calc R . . Mo1' Mo 0.8233(5) 0.9534(7) 0.2128(5) 0.068(2) Uani 0.119(2) 1 d P . . C2A C 0.8824(8) 1.0805(10) 0.1932(7) 0.085(3) Uani 1 1 d . . . H2AA H 0.9401 1.0258 0.1660 0.102 Uiso 1 1 d R . . C2 C 0.8349(7) 0.7540(11) 0.0453(5) 0.074(2) Uani 1 1 d . . . H2A H 0.8547 0.6570 0.0767 0.088 Uiso 1 1 d R . . H2B H 0.8971 0.8247 0.0622 0.088 Uiso 1 1 d R . . C2P C 0.4189(6) 0.7736(9) 0.2423(6) 0.064(2) Uani 1 1 d . . . H2PA H 0.3683 0.6891 0.2264 0.096 Uiso 1 1 calc R . . H2PB H 0.3790 0.8685 0.2294 0.096 Uiso 1 1 calc R . . H2PC H 0.4484 0.7686 0.3086 0.096 Uiso 1 1 calc R . . C3P C 0.5812(7) 0.5663(8) 0.1868(6) 0.071(2) Uani 1 1 d . . . H3PA H 0.5163 0.5004 0.1835 0.107 Uiso 1 1 calc R . . H3PB H 0.6260 0.5551 0.2478 0.107 Uiso 1 1 calc R . . H3PC H 0.6255 0.5388 0.1376 0.107 Uiso 1 1 calc R . . C3 C 0.8195(6) 0.7238(10) -0.0589(5) 0.062(2) Uani 1 1 d . . . C3A C 0.9170(7) 1.1305(9) 0.2886(6) 0.074(2) Uani 1 1 d . . . H3AD H 0.8926 1.2350 0.2980 0.088 Uiso 1 1 d R . . H3AE H 0.9952 1.1145 0.3154 0.088 Uiso 1 1 d R . . C31 C 0.7296(10) 0.6162(19) -0.0891(10) 0.175(8) Uani 1 1 d . . . H31A H 0.7216 0.6052 -0.1571 0.263 Uiso 1 1 calc R . . H31B H 0.6601 0.6536 -0.0706 0.263 Uiso 1 1 calc R . . H31C H 0.7475 0.5183 -0.0598 0.263 Uiso 1 1 calc R . . C32 C 0.7932(13) 0.8796(15) -0.1062(7) 0.148(6) Uani 1 1 d . . . H32A H 0.7826 0.8674 -0.1741 0.222 Uiso 1 1 calc R . . H32B H 0.8550 0.9487 -0.0880 0.222 Uiso 1 1 calc R . . H32C H 0.7256 0.9207 -0.0861 0.222 Uiso 1 1 calc R . . C33 C 0.9246(8) 0.6643(15) -0.0900(8) 0.107(4) Uani 1 1 d . . . H33A H 0.9138 0.6510 -0.1578 0.161 Uiso 1 1 calc R . . H33B H 0.9434 0.5673 -0.0598 0.161 Uiso 1 1 calc R . . H33C H 0.9850 0.7358 -0.0726 0.161 Uiso 1 1 calc R . . 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 0.0465(4) 0.0345(3) 0.0388(3) 0.0042(3) -0.0034(2) -0.0082(3) P1 0.0435(10) 0.0426(10) 0.0610(11) -0.0012(8) 0.0016(8) -0.0050(8) O1 0.085(4) 0.091(4) 0.058(3) -0.021(3) 0.025(3) -0.026(3) C1A 0.091(6) 0.073(6) 0.093(6) 0.035(5) -0.020(5) -0.027(5) C1P 0.073(6) 0.093(7) 0.074(6) -0.002(5) -0.003(4) -0.019(5) Mo1' 0.066(4) 0.039(3) 0.097(5) 0.014(3) 0.006(3) -0.003(3) C2A 0.074(6) 0.079(6) 0.097(7) 0.031(5) -0.005(5) -0.035(5) C2 0.079(6) 0.087(6) 0.053(5) -0.002(4) 0.005(4) 0.004(5) C2P 0.050(4) 0.069(5) 0.074(5) -0.004(4) 0.011(4) -0.003(4) C3P 0.068(5) 0.044(4) 0.102(6) 0.000(4) 0.014(4) -0.007(4) C3 0.053(4) 0.089(6) 0.045(4) 0.000(4) 0.005(3) 0.001(4) C3A 0.070(5) 0.044(4) 0.097(6) -0.011(4) -0.024(5) -0.012(4) C31 0.107(9) 0.265(19) 0.163(12) -0.150(13) 0.051(9) -0.071(11) C32 0.256(17) 0.133(11) 0.060(6) 0.031(7) 0.040(8) 0.065(11) C33 0.078(7) 0.138(10) 0.110(8) 0.000(8) 0.027(6) 0.008(7) _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 Mo1' 1.484(6) . ? Mo1 Mo1' 1.603(7) 2_655 ? Mo1 O1 1.990(5) . ? Mo1 C3A 2.176(8) 2_655 ? Mo1 C1A 2.192(8) . ? Mo1 Mo1 2.2094(13) 2_655 ? Mo1 C2A 2.424(8) . ? Mo1 C2A 2.446(9) 2_655 ? Mo1 P1 2.5638(19) . ? P1 C1P 1.796(8) . ? P1 C3P 1.802(7) . ? P1 C2P 1.828(7) . ? P1 Mo1' 2.753(6) 2_655 ? O1 C2 1.372(9) . ? O1 Mo1' 2.376(8) . ? C1A C2A 1.423(11) . ? C1A Mo1' 2.059(10) . ? Mo1' C2A 1.361(9) . ? Mo1' Mo1 1.603(7) 2_655 ? Mo1' C3A 2.114(9) . ? Mo1' Mo1' 2.159(13) 2_655 ? Mo1' P1 2.753(6) 2_655 ? C2A C3A 1.429(11) . ? C2A Mo1 2.446(9) 2_655 ? C2 C3 1.489(10) . ? C3 C31 1.446(13) . ? C3 C33 1.478(11) . ? C3 C32 1.527(13) . ? C3A Mo1 2.176(8) 2_655 ? 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 Mo1' Mo1 Mo1' 88.7(3) . 2_655 ? Mo1' Mo1 O1 85.0(3) . . ? Mo1' Mo1 O1 139.7(3) 2_655 . ? Mo1' Mo1 C3A 124.5(3) . 2_655 ? Mo1' Mo1 C3A 66.0(3) 2_655 2_655 ? O1 Mo1 C3A 145.4(3) . 2_655 ? Mo1' Mo1 C1A 64.8(3) . . ? Mo1' Mo1 C1A 120.2(4) 2_655 . ? O1 Mo1 C1A 92.7(3) . . ? C3A Mo1 C1A 85.8(4) 2_655 . ? Mo1' Mo1 Mo1 46.5(3) . 2_655 ? Mo1' Mo1 Mo1 42.2(2) 2_655 2_655 ? O1 Mo1 Mo1 119.59(18) . 2_655 ? C3A Mo1 Mo1 94.9(2) 2_655 2_655 ? C1A Mo1 Mo1 94.6(2) . 2_655 ? Mo1' Mo1 C2A 30.1(3) . . ? Mo1' Mo1 C2A 100.7(3) 2_655 . ? O1 Mo1 C2A 93.3(3) . . ? C3A Mo1 C2A 104.6(3) 2_655 . ? C1A Mo1 C2A 35.5(3) . . ? Mo1 Mo1 C2A 63.5(2) 2_655 . ? Mo1' Mo1 C2A 103.6(3) . 2_655 ? Mo1' Mo1 C2A 31.3(3) 2_655 2_655 ? O1 Mo1 C2A 165.3(3) . 2_655 ? C3A Mo1 C2A 35.4(3) 2_655 2_655 ? C1A Mo1 C2A 101.7(4) . 2_655 ? Mo1 Mo1 C2A 62.5(2) 2_655 2_655 ? C2A Mo1 C2A 100.0(4) . 2_655 ? Mo1' Mo1 P1 137.3(2) . . ? Mo1' Mo1 P1 79.0(2) 2_655 . ? O1 Mo1 P1 79.07(16) . . ? C3A Mo1 P1 87.4(2) 2_655 . ? C1A Mo1 P1 154.2(2) . . ? Mo1 Mo1 P1 110.77(5) 2_655 . ? C2A Mo1 P1 166.8(2) . . ? C2A Mo1 P1 86.6(2) 2_655 . ? C1P P1 C3P 105.0(4) . . ? C1P P1 C2P 101.9(4) . . ? C3P P1 C2P 102.6(4) . . ? C1P P1 Mo1 106.8(3) . . ? C3P P1 Mo1 113.0(3) . . ? C2P P1 Mo1 125.4(3) . . ? C1P P1 Mo1' 136.2(3) . 2_655 ? C3P P1 Mo1' 110.2(3) . 2_655 ? C2P P1 Mo1' 95.1(3) . 2_655 ? Mo1 P1 Mo1' 34.86(14) . 2_655 ? C2 O1 Mo1 138.8(5) . . ? C2 O1 Mo1' 100.8(5) . . ? Mo1 O1 Mo1' 38.47(18) . . ? C2A C1A Mo1' 41.1(4) . . ? C2A C1A Mo1 81.2(5) . . ? Mo1' C1A Mo1 40.7(2) . . ? C2A Mo1' Mo1 116.8(6) . . ? C2A Mo1' Mo1 111.0(6) . 2_655 ? Mo1 Mo1' Mo1 91.3(3) . 2_655 ? C2A Mo1' C1A 43.5(4) . . ? Mo1 Mo1' C1A 74.4(3) . . ? Mo1 Mo1' C1A 123.6(5) 2_655 . ? C2A Mo1' C3A 41.9(5) . . ? Mo1 Mo1' C3A 127.0(4) . . ? Mo1 Mo1' C3A 70.1(4) 2_655 . ? C1A Mo1' C3A 76.2(4) . . ? C2A Mo1' Mo1' 125.1(6) . 2_655 ? Mo1 Mo1' Mo1' 47.9(2) . 2_655 ? Mo1 Mo1' Mo1' 43.4(3) 2_655 2_655 ? C1A Mo1' Mo1' 103.0(4) . 2_655 ? C3A Mo1' Mo1' 99.2(4) . 2_655 ? C2A Mo1' O1 116.6(6) . . ? Mo1 Mo1' O1 56.5(3) . . ? Mo1 Mo1' O1 130.7(3) 2_655 . ? C1A Mo1' O1 85.8(4) . . ? C3A Mo1' O1 158.6(4) . . ? Mo1' Mo1' O1 96.1(3) 2_655 . ? C2A Mo1' P1 108.6(5) . 2_655 ? Mo1 Mo1' P1 134.2(3) . 2_655 ? Mo1 Mo1' P1 66.1(2) 2_655 2_655 ? C1A Mo1' P1 151.4(4) . 2_655 ? C3A Mo1' P1 83.9(3) . 2_655 ? Mo1' Mo1' P1 100.3(3) 2_655 2_655 ? O1 Mo1' P1 108.1(3) . 2_655 ? Mo1' C2A C1A 95.4(6) . . ? Mo1' C2A C3A 98.5(7) . . ? C1A C2A C3A 129.0(10) . . ? Mo1' C2A Mo1 33.1(3) . . ? C1A C2A Mo1 63.3(4) . . ? C3A C2A Mo1 111.4(6) . . ? Mo1' C2A Mo1 37.7(4) . 2_655 ? C1A C2A Mo1 110.6(6) . 2_655 ? C3A C2A Mo1 61.9(5) . 2_655 ? Mo1 C2A Mo1 53.95(18) . 2_655 ? O1 C2 C3 114.7(7) . . ? C31 C3 C33 108.1(9) . . ? C31 C3 C2 113.4(8) . . ? C33 C3 C2 111.1(7) . . ? C31 C3 C32 110.2(10) . . ? C33 C3 C32 108.3(9) . . ? C2 C3 C32 105.6(8) . . ? C2A C3A Mo1' 39.6(4) . . ? C2A C3A Mo1 82.7(4) . 2_655 ? Mo1' C3A Mo1 43.8(2) . 2_655 ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.807 _refine_diff_density_min -0.699 _refine_diff_density_rms 0.093