# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1405 data_feph2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C11 H13 Fe P' _chemical_formula_sum 'C11 H13 Fe P' _chemical_formula_weight 232.03 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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.7111(9) _cell_length_b 7.5225(5) _cell_length_c 10.5662(7) _cell_angle_alpha 90.00 _cell_angle_beta 107.448(5) _cell_angle_gamma 90.00 _cell_volume 1039.67(12) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 3032 _cell_measurement_theta_min 3.11 _cell_measurement_theta_max 30.00 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 1.552 _exptl_absorpt_correction_type 'psi scans' _exptl_absorpt_correction_T_min 0.408 _exptl_absorpt_correction_T_max 0.560 _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 'Nicolet R3' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3190 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0325 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 30.00 _reflns_number_total 3032 _reflns_number_gt 2407 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+0.8063P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3032 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0594 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1187 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_restrained_S_all 1.146 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.003 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.18681(3) 0.01592(4) 0.43482(3) 0.02205(12) Uani 1 d . . . P P 0.46109(8) -0.38430(14) 0.64120(11) 0.0534(3) Uani 1 d . . . H2A H 0.4000 -0.5000 0.6486 0.050 Uiso 1 d . . . H2B H 0.5400 -0.3990 0.6310 0.050 Uiso 1 d . . . C1 C 0.3897(3) -0.2160(5) 0.5209(4) 0.0426(7) Uani 1 d . . . H1A H 0.4303 -0.1050 0.5336 0.051 Uiso 1 calc R . . H1B H 0.3816 -0.2594 0.4299 0.051 Uiso 1 calc R . . C11 C 0.2865(2) -0.1750(3) 0.5337(3) 0.0265(5) Uani 1 d . . . C12 C 0.2652(2) -0.0523(4) 0.6250(2) 0.0287(5) Uani 1 d . . . H12 H 0.3142 0.0181 0.6876 0.034 Uiso 1 calc R . . C13 C 0.1577(2) -0.0537(4) 0.6063(3) 0.0299(6) Uani 1 d . . . H13 H 0.1225 0.0159 0.6536 0.036 Uiso 1 calc R . . C14 C 0.1127(2) -0.1782(4) 0.5039(3) 0.0298(6) Uani 1 d . . . H14 H 0.0421 -0.2065 0.4709 0.036 Uiso 1 calc R . . C15 C 0.1919(2) -0.2525(3) 0.4597(3) 0.0284(5) Uani 1 d . . . H15 H 0.1831 -0.3394 0.3920 0.034 Uiso 1 calc R . . C21 C 0.2530(3) 0.1434(5) 0.3123(4) 0.0565(11) Uani 1 d . . . H21 H 0.3183 0.1174 0.3028 0.068 Uiso 1 calc R . . C22 C 0.2333(3) 0.2637(4) 0.4007(4) 0.0472(8) Uani 1 d . . . H22 H 0.2829 0.3340 0.4625 0.057 Uiso 1 calc R . . C23 C 0.1289(3) 0.2646(4) 0.3839(4) 0.0476(9) Uani 1 d . . . H23 H 0.0949 0.3358 0.4319 0.057 Uiso 1 calc R . . C24 C 0.0826(3) 0.1439(6) 0.2852(4) 0.0584(12) Uani 1 d . . . H24 H 0.0116 0.1178 0.2540 0.070 Uiso 1 calc R . . C25 C 0.1597(5) 0.0662(5) 0.2389(3) 0.0678(15) Uani 1 d . . . H25 H 0.1502 -0.0212 0.1714 0.081 Uiso 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 Fe 0.02559(19) 0.01945(17) 0.02059(18) 0.00120(13) 0.00617(13) -0.00063(14) P 0.0450(5) 0.0555(6) 0.0536(6) 0.0091(5) 0.0055(4) 0.0204(4) C1 0.0368(16) 0.0459(17) 0.0492(19) 0.0131(15) 0.0191(14) 0.0107(14) C11 0.0289(13) 0.0253(11) 0.0254(12) 0.0054(10) 0.0084(10) 0.0044(10) C12 0.0310(13) 0.0319(13) 0.0184(11) 0.0001(10) 0.0001(10) 0.0002(10) C13 0.0339(14) 0.0324(13) 0.0248(12) 0.0071(10) 0.0112(11) 0.0076(11) C14 0.0270(13) 0.0284(12) 0.0315(14) 0.0118(11) 0.0051(11) -0.0025(10) C15 0.0369(14) 0.0200(11) 0.0267(13) 0.0033(9) 0.0071(11) 0.0006(10) C21 0.062(2) 0.048(2) 0.078(3) 0.037(2) 0.048(2) 0.0184(18) C22 0.055(2) 0.0292(15) 0.052(2) 0.0103(14) 0.0070(16) -0.0108(14) C23 0.065(2) 0.0333(15) 0.054(2) 0.0189(15) 0.0309(19) 0.0184(16) C24 0.0431(19) 0.065(2) 0.053(2) 0.040(2) -0.0065(17) -0.0092(18) C25 0.148(5) 0.0325(16) 0.0261(16) 0.0080(13) 0.031(2) -0.006(2) _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 Fe C25 2.026(3) . ? Fe C24 2.028(3) . ? Fe C21 2.031(3) . ? Fe C22 2.037(3) . ? Fe C15 2.034(3) . ? Fe C14 2.035(3) . ? Fe C12 2.040(3) . ? Fe C23 2.040(3) . ? Fe C11 2.042(3) . ? Fe C13 2.037(3) . ? P C1 1.852(3) . ? C1 C11 1.493(4) . ? C11 C15 1.424(4) . ? C11 C12 1.427(4) . ? C12 C13 1.427(4) . ? C13 C14 1.423(4) . ? C14 C15 1.418(4) . ? C21 C22 1.384(5) . ? C21 C25 1.408(7) . ? C22 C23 1.389(5) . ? C23 C24 1.384(6) . ? C24 C25 1.417(6) . ? 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 C25 Fe C24 40.92(19) . . ? C25 Fe C21 40.61(19) . . ? C24 Fe C21 67.92(16) . . ? C25 Fe C22 67.63(16) . . ? C24 Fe C22 67.17(15) . . ? C21 Fe C22 39.78(16) . . ? C25 Fe C15 107.82(13) . . ? C24 Fe C15 124.10(15) . . ? C21 Fe C15 123.13(14) . . ? C22 Fe C15 158.54(14) . . ? C25 Fe C14 122.81(16) . . ? C24 Fe C14 108.03(13) . . ? C21 Fe C14 159.08(16) . . ? C22 Fe C14 159.48(15) . . ? C15 Fe C14 40.80(11) . . ? C25 Fe C12 159.2(2) . . ? C24 Fe C12 158.00(17) . . ? C21 Fe C12 122.86(16) . . ? C22 Fe C12 107.73(13) . . ? C15 Fe C12 68.62(11) . . ? C14 Fe C12 68.79(11) . . ? C25 Fe C23 67.76(16) . . ? C24 Fe C23 39.77(17) . . ? C21 Fe C23 67.18(14) . . ? C22 Fe C23 39.84(15) . . ? C15 Fe C23 159.93(14) . . ? C14 Fe C23 123.75(13) . . ? C12 Fe C23 122.63(14) . . ? C25 Fe C11 122.95(16) . . ? C24 Fe C11 160.09(16) . . ? C21 Fe C11 107.44(13) . . ? C22 Fe C11 122.51(13) . . ? C15 Fe C11 40.89(11) . . ? C14 Fe C11 68.98(11) . . ? C12 Fe C11 40.94(11) . . ? C23 Fe C11 158.15(15) . . ? C25 Fe C13 158.71(19) . . ? C24 Fe C13 122.36(15) . . ? C21 Fe C13 158.85(17) . . ? C22 Fe C13 123.24(14) . . ? C15 Fe C13 68.78(11) . . ? C14 Fe C13 40.93(12) . . ? C12 Fe C13 40.98(11) . . ? C23 Fe C13 107.81(13) . . ? C11 Fe C13 69.12(11) . . ? C11 C1 P 113.5(2) . . ? C15 C11 C12 107.3(2) . . ? C15 C11 C1 126.7(3) . . ? C12 C11 C1 125.9(3) . . ? C15 C11 Fe 69.29(15) . . ? C12 C11 Fe 69.48(15) . . ? C1 C11 Fe 127.3(2) . . ? C13 C12 C11 108.3(2) . . ? C13 C12 Fe 69.39(15) . . ? C11 C12 Fe 69.58(14) . . ? C14 C13 C12 107.7(2) . . ? C14 C13 Fe 69.46(15) . . ? C12 C13 Fe 69.64(15) . . ? C15 C14 C13 108.0(2) . . ? C15 C14 Fe 69.59(15) . . ? C13 C14 Fe 69.61(15) . . ? C14 C15 C11 108.6(2) . . ? C14 C15 Fe 69.61(15) . . ? C11 C15 Fe 69.82(15) . . ? C22 C21 C25 108.2(3) . . ? C22 C21 Fe 70.35(19) . . ? C25 C21 Fe 69.51(19) . . ? C21 C22 C23 108.6(3) . . ? C21 C22 Fe 69.87(19) . . ? C23 C22 Fe 70.22(18) . . ? C24 C23 C22 108.4(3) . . ? C24 C23 Fe 69.62(19) . . ? C22 C23 Fe 69.94(18) . . ? C23 C24 C25 108.1(3) . . ? C23 C24 Fe 70.60(19) . . ? C25 C24 Fe 69.5(2) . . ? C21 C25 C24 106.8(3) . . ? C21 C25 Fe 69.9(2) . . ? C24 C25 Fe 69.62(19) . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.935 _refine_diff_density_max 0.714 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.097 data_hunos #(Space group C2/c) _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C13 H13 Fe Mo0.5 O2 P' _chemical_formula_structural 'C26 H13 Fe2 Mo O4 P2' _chemical_formula_analytical 'as above' _chemical_formula_sum 'C26 H26 Fe2 Mo O4 P2' _chemical_formula_weight 672.05 _chemical_melting_point '141-145 deg. C' _chemical_compound_source 'inorganic synthesis' 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' 'Fe' 'Fe' 0.3463 0.8444 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.626(3) _cell_length_b 10.426(2) _cell_length_c 12.3240(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.950(10) _cell_angle_gamma 90.00 _cell_volume 2649.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 2899 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 26.99 _exptl_crystal_description 'rounded prisms' _exptl_crystal_colour orange _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.685 _exptl_crystal_density_method ? _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 1.697 _exptl_absorpt_correction_type 'psi scans' _exptl_absorpt_correction_T_min 0.525 _exptl_absorpt_correction_T_max 0.612 _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 'Seimens P4' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2978 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0922 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 26.99 _reflns_number_total 2899 _reflns_number_observed 1701 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 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 'calc w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+1.3103P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2898 _refine_ls_number_parameters 159 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1255 _refine_ls_R_factor_obs 0.0621 _refine_ls_wR_factor_all 0.1495 _refine_ls_wR_factor_obs 0.1237 _refine_ls_goodness_of_fit_all 1.067 _refine_ls_goodness_of_fit_obs 1.173 _refine_ls_restrained_S_all 1.069 _refine_ls_restrained_S_obs 1.173 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo Mo 0.5000 0.02618(8) 0.7500 0.0308(3) Uani 1 d S . Fe Fe 0.33399(5) 0.51001(10) 0.65556(9) 0.0413(3) Uani 1 d . . P P 0.44985(10) 0.1979(2) 0.8653(2) 0.0386(5) Uani 1 d . . H0A H 0.43596(10) 0.1432(2) 0.9614(2) 0.046 Uiso 1 calc R . H0B H 0.49648(10) 0.2860(2) 0.8854(2) 0.046 Uiso 1 calc R . C1 C 0.4204(4) 0.0204(7) 0.6488(6) 0.041(2) Uani 1 d . . O1 O 0.3757(3) 0.0081(5) 0.5945(5) 0.057(2) Uani 1 d . . C2 C 0.5409(4) -0.1086(7) 0.6603(6) 0.047(2) Uani 1 d . . O2 O 0.5657(3) -0.1884(6) 0.6109(5) 0.078(2) Uani 1 d . . C3 C 0.3768(3) 0.2866(7) 0.8206(6) 0.040(2) Uani 1 d . . H3A H 0.3416(3) 0.2251(7) 0.8035(6) 0.049 Uiso 1 calc R . H3B H 0.3622(3) 0.3426(7) 0.8803(6) 0.049 Uiso 1 calc R . C11 C 0.3900(4) 0.3674(7) 0.7219(6) 0.041(2) Uani 1 d . . C12 C 0.4237(4) 0.4861(7) 0.7206(7) 0.046(2) Uani 1 d . . H12 H 0.4409(4) 0.5300(7) 0.7822(7) 0.055 Uiso 1 calc R . C13 C 0.4271(4) 0.5274(9) 0.6125(7) 0.057(2) Uani 1 d . . H13 H 0.4469(4) 0.6044(9) 0.5884(7) 0.068 Uiso 1 calc R . C14 C 0.3967(5) 0.4363(9) 0.5464(8) 0.066(3) Uani 1 d . . H14 H 0.3931(5) 0.4404(9) 0.4695(8) 0.080 Uiso 1 calc R . C15 C 0.3718(5) 0.3357(8) 0.6124(7) 0.060(2) Uani 1 d . . H15 H 0.3480(5) 0.2626(8) 0.5887(7) 0.072 Uiso 1 calc R . C21 C 0.2538(5) 0.5278(11) 0.7451(10) 0.078(3) Uani 1 d . . H21 H 0.2440(5) 0.4766(11) 0.8065(10) 0.094 Uiso 1 calc R . C22 C 0.2892(5) 0.6423(11) 0.7480(9) 0.073(3) Uani 1 d . . H22 H 0.3069(5) 0.6834(11) 0.8105(9) 0.088 Uiso 1 calc R . C23 C 0.2932(4) 0.6845(8) 0.6399(9) 0.064(3) Uani 1 d . . H23 H 0.3151(4) 0.7590(8) 0.6155(9) 0.077 Uiso 1 calc R . C24 C 0.2593(5) 0.5972(10) 0.5753(8) 0.065(3) Uani 1 d . . H24 H 0.2533(5) 0.6028(10) 0.4989(8) 0.077 Uiso 1 calc R . C25 C 0.2357(4) 0.5010(9) 0.6410(11) 0.080(3) Uani 1 d . . H25 H 0.2112(4) 0.4288(9) 0.6174(11) 0.096 Uiso 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 0.0328(5) 0.0220(4) 0.0379(5) 0.000 0.0043(4) 0.000 Fe 0.0406(7) 0.0352(6) 0.0481(7) 0.0045(5) 0.0002(5) 0.0087(5) P 0.0404(11) 0.0360(10) 0.0394(11) 0.0068(8) 0.0015(9) 0.0018(8) C1 0.043(4) 0.034(4) 0.046(4) -0.003(4) 0.002(4) -0.001(4) O1 0.051(4) 0.059(4) 0.061(4) -0.010(3) -0.007(3) -0.008(3) C2 0.052(5) 0.039(4) 0.049(5) -0.005(4) 0.001(4) 0.000(4) O2 0.101(6) 0.050(4) 0.082(5) -0.026(3) 0.011(4) 0.019(4) C3 0.032(4) 0.036(4) 0.053(5) 0.003(3) 0.005(4) 0.004(3) C11 0.036(4) 0.037(4) 0.051(5) 0.006(3) 0.000(4) 0.009(3) C12 0.034(4) 0.045(4) 0.059(5) 0.012(4) -0.001(4) -0.001(3) C13 0.046(5) 0.057(5) 0.068(6) 0.030(5) 0.012(4) 0.014(4) C14 0.082(7) 0.076(7) 0.041(5) 0.008(5) 0.011(5) 0.038(6) C15 0.082(7) 0.043(5) 0.054(6) -0.001(4) -0.008(5) 0.030(5) C21 0.052(6) 0.097(8) 0.086(7) 0.039(7) 0.020(5) 0.039(6) C22 0.057(6) 0.085(8) 0.076(7) -0.028(6) -0.013(5) 0.034(6) C23 0.052(6) 0.035(4) 0.105(8) 0.015(5) 0.010(6) 0.017(4) C24 0.059(6) 0.074(7) 0.061(6) 0.006(5) -0.016(5) 0.024(5) C25 0.042(5) 0.062(7) 0.136(11) 0.015(7) -0.009(6) 0.007(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo C2 1.984(8) . ? Mo C2 1.984(8) 2_656 ? Mo C1 2.047(8) 2_656 ? Mo C1 2.047(8) . ? Mo P 2.518(2) 2_656 ? Mo P 2.518(2) . ? Fe C13 2.010(8) . ? Fe C21 2.012(9) . ? Fe C23 2.012(8) . ? Fe C12 2.020(8) . ? Fe C22 2.022(9) . ? Fe C24 2.032(8) . ? Fe C14 2.033(8) . ? Fe C25 2.034(9) . ? Fe C11 2.046(7) . ? Fe C15 2.052(8) . ? P C3 1.843(7) . ? C1 O1 1.138(9) . ? C2 O2 1.156(9) . ? C3 C11 1.508(10) . ? C11 C12 1.419(10) . ? C11 C15 1.433(11) . ? C12 C13 1.403(11) . ? C13 C14 1.394(13) . ? C14 C15 1.428(12) . ? C21 C25 1.36(2) . ? C21 C22 1.399(14) . ? C22 C23 1.406(14) . ? C23 C24 1.391(13) . ? C24 C25 1.381(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 C2 Mo C2 89.8(5) . 2_656 ? C2 Mo C1 88.5(3) . 2_656 ? C2 Mo C1 89.1(3) 2_656 2_656 ? C2 Mo C1 89.1(3) . . ? C2 Mo C1 88.6(3) 2_656 . ? C1 Mo C1 176.6(4) 2_656 . ? C2 Mo P 90.4(2) . 2_656 ? C2 Mo P 179.1(2) 2_656 2_656 ? C1 Mo P 91.8(2) 2_656 2_656 ? C1 Mo P 90.6(2) . 2_656 ? C2 Mo P 179.1(2) . . ? C2 Mo P 90.4(2) 2_656 . ? C1 Mo P 90.6(2) 2_656 . ? C1 Mo P 91.8(2) . . ? P Mo P 89.37(9) 2_656 . ? C13 Fe C21 159.1(5) . . ? C13 Fe C23 107.0(4) . . ? C21 Fe C23 67.9(4) . . ? C13 Fe C12 40.7(3) . . ? C21 Fe C12 123.3(4) . . ? C23 Fe C12 121.9(4) . . ? C13 Fe C22 122.3(4) . . ? C21 Fe C22 40.6(4) . . ? C23 Fe C22 40.8(4) . . ? C12 Fe C22 106.6(4) . . ? C13 Fe C24 123.5(4) . . ? C21 Fe C24 66.6(4) . . ? C23 Fe C24 40.2(4) . . ? C12 Fe C24 158.6(4) . . ? C22 Fe C24 67.6(4) . . ? C13 Fe C14 40.3(4) . . ? C21 Fe C14 159.4(5) . . ? C23 Fe C14 123.2(4) . . ? C12 Fe C14 68.1(4) . . ? C22 Fe C14 158.8(5) . . ? C24 Fe C14 109.4(4) . . ? C13 Fe C25 159.4(5) . . ? C21 Fe C25 39.3(4) . . ? C23 Fe C25 67.6(4) . . ? C12 Fe C25 159.1(4) . . ? C22 Fe C25 67.5(4) . . ? C24 Fe C25 39.7(4) . . ? C14 Fe C25 124.6(5) . . ? C13 Fe C11 68.6(3) . . ? C21 Fe C11 108.2(4) . . ? C23 Fe C11 158.1(4) . . ? C12 Fe C11 40.9(3) . . ? C22 Fe C11 122.1(4) . . ? C24 Fe C11 159.8(4) . . ? C14 Fe C11 68.2(3) . . ? C25 Fe C11 123.9(4) . . ? C13 Fe C15 69.0(4) . . ? C21 Fe C15 122.9(4) . . ? C23 Fe C15 159.5(4) . . ? C12 Fe C15 69.1(4) . . ? C22 Fe C15 158.4(4) . . ? C24 Fe C15 124.0(4) . . ? C14 Fe C15 40.9(3) . . ? C25 Fe C15 108.6(4) . . ? C11 Fe C15 40.9(3) . . ? C3 P Mo 122.0(3) . . ? O1 C1 Mo 175.0(7) . . ? O2 C2 Mo 177.9(7) . . ? C11 C3 P 111.3(5) . . ? C12 C11 C15 108.1(7) . . ? C12 C11 C3 126.2(7) . . ? C15 C11 C3 125.6(7) . . ? C12 C11 Fe 68.6(4) . . ? C15 C11 Fe 69.8(4) . . ? C3 C11 Fe 128.3(5) . . ? C13 C12 C11 108.1(8) . . ? C13 C12 Fe 69.3(5) . . ? C11 C12 Fe 70.5(4) . . ? C14 C13 C12 108.4(8) . . ? C14 C13 Fe 70.7(5) . . ? C12 C13 Fe 70.0(4) . . ? C13 C14 C15 109.3(8) . . ? C13 C14 Fe 68.9(5) . . ? C15 C14 Fe 70.2(5) . . ? C14 C15 C11 106.0(8) . . ? C14 C15 Fe 68.8(5) . . ? C11 C15 Fe 69.3(4) . . ? C25 C21 C22 109.5(10) . . ? C25 C21 Fe 71.2(6) . . ? C22 C21 Fe 70.1(6) . . ? C21 C22 C23 106.4(9) . . ? C21 C22 Fe 69.3(6) . . ? C23 C22 Fe 69.2(5) . . ? C24 C23 C22 107.5(9) . . ? C24 C23 Fe 70.7(5) . . ? C22 C23 Fe 70.0(5) . . ? C25 C24 C23 108.5(9) . . ? C25 C24 Fe 70.2(5) . . ? C23 C24 Fe 69.1(5) . . ? C21 C25 C24 108.1(10) . . ? C21 C25 Fe 69.5(6) . . ? C24 C25 Fe 70.1(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Mo P C3 C11 -65.2(6) . . . . ? _refine_diff_density_max 1.025 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.145 data_96113 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety C20H13O9PFeRu3 _chemical_formula_structural Ru3(H)2(CO)9PCH2(cp)Fe(cp) _chemical_formula_analytical ? _chemical_formula_sum 'C20 H13 Fe O9 P Ru3' _chemical_formula_weight 787.33 _chemical_melting_point ? _chemical_compound_source ? 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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ru' 'Ru' -1.2594 0.8363 '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 9.961(1) _cell_length_b 15.506(3) _cell_length_c 16.496(2) _cell_angle_alpha 83.96(1) _cell_angle_beta 88.72(1) _cell_angle_gamma 80.79(1) _cell_volume 2501.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 38 _cell_measurement_theta_min 4.8 _cell_measurement_theta_max 12.5 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.62 _exptl_crystal_size_min 0.56 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.091 _exptl_crystal_density_method ? _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 2.455 _exptl_absorpt_correction_type 'semi-empirical based on psi scan data' _exptl_absorpt_correction_T_min 0.842 _exptl_absorpt_correction_T_max 0.728 _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 'Siemens P4 Diffractometer' _diffrn_measurement_method omega _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1% _diffrn_reflns_number 9576 _diffrn_reflns_av_R_equivalents 0.0072 _diffrn_reflns_av_sigmaI/netI 0.0159 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8809 _reflns_number_observed 8012 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'XSCANS (Fait, 1991)' _computing_cell_refinement 'XSCANS (Fait, 1991)' _computing_data_reduction 'XSCANS (Fait, 1991)' _computing_structure_solution 'SHELXS-96 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-96 (Sheldrick, 1996)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1990)' _computing_publication_material 'CIFTAB (Sheldrick, 1996)' _refine_special_details ; Refinement of F^2^ against ALL reflections. 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 'calc w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+3.5167P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'hydride H atoms from difmap others calc.' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8809 _refine_ls_number_parameters 617 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0263 _refine_ls_R_factor_obs 0.0220 _refine_ls_wR_factor_all 0.0493 _refine_ls_wR_factor_obs 0.0480 _refine_ls_goodness_of_fit_all 1.079 _refine_ls_goodness_of_fit_obs 1.106 _refine_ls_restrained_S_all 1.079 _refine_ls_restrained_S_obs 1.106 _refine_ls_shift/esd_max 0.006 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ru1 Ru 0.13248(3) 0.216846(16) 0.291530(15) 0.02328(6) Uani 1 d . . Ru2 Ru 0.23977(3) 0.196374(17) 0.451570(14) 0.02427(6) Uani 1 d . . Ru3 Ru 0.36036(3) 0.075994(16) 0.334909(16) 0.02569(6) Uani 1 d . . H1 H 0.1941 0.0982 0.2965 0.039(10) Uiso 1 d R . H2 H 0.3029 0.0899 0.4367 0.071(14) Uiso 1 d R . Fe1 Fe 0.61066(5) 0.34954(3) 0.12003(3) 0.02602(10) Uani 1 d . . P1 P 0.34764(8) 0.22685(5) 0.33013(5) 0.02205(16) Uani 1 d . . C1 C 0.1385(4) 0.2198(2) 0.1745(2) 0.0330(8) Uani 1 d . . O1 O 0.1436(3) 0.2213(2) 0.10624(15) 0.0544(8) Uani 1 d . . C2 C 0.0663(3) 0.3384(2) 0.2913(2) 0.0309(7) Uani 1 d . . O2 O 0.0287(3) 0.41138(16) 0.29129(17) 0.0480(7) Uani 1 d . . C3 C -0.0413(4) 0.1765(2) 0.3184(2) 0.0387(8) Uani 1 d . . O3 O -0.1423(3) 0.1552(2) 0.3354(2) 0.0635(9) Uani 1 d . . C4 C 0.1722(4) 0.3126(2) 0.4730(2) 0.0342(8) Uani 1 d . . O4 O 0.1336(3) 0.38242(18) 0.48693(18) 0.0535(7) Uani 1 d . . C5 C 0.0951(4) 0.1370(2) 0.5009(2) 0.0421(9) Uani 1 d . . O5 O 0.0125(4) 0.0999(2) 0.5271(2) 0.0707(10) Uani 1 d . . C6 C 0.3701(4) 0.1798(3) 0.5367(2) 0.0418(9) Uani 1 d . . O6 O 0.4464(4) 0.1707(2) 0.5882(2) 0.0737(10) Uani 1 d . . C7 C 0.2988(4) -0.0394(2) 0.3554(2) 0.0412(9) Uani 1 d . . O7 O 0.2564(3) -0.10241(18) 0.3672(2) 0.0608(8) Uani 1 d . . C8 C 0.5373(4) 0.0490(2) 0.3818(2) 0.0375(8) Uani 1 d . . O8 O 0.6411(3) 0.0362(2) 0.4113(2) 0.0613(8) Uani 1 d . . C9 C 0.4267(4) 0.0590(2) 0.2262(2) 0.0346(8) Uani 1 d . . O9 O 0.4649(3) 0.04701(19) 0.16273(17) 0.0526(7) Uani 1 d . . C10 C 0.4717(3) 0.2958(2) 0.28789(18) 0.0283(7) Uani 1 d . . H10A H 0.5562 0.2788 0.3166 0.034 Uiso 1 d R . H10B H 0.4388 0.3563 0.2944 0.034 Uiso 1 d R . C11 C 0.4944(3) 0.2844(2) 0.19955(18) 0.0245(7) Uani 1 d . . C12 C 0.4140(3) 0.3301(2) 0.1338(2) 0.0311(7) Uani 1 d . . H12 H 0.3368 0.3751 0.1387 0.037 Uiso 1 d R . C13 C 0.4684(4) 0.2987(3) 0.0599(2) 0.0371(8) Uani 1 d . . H13 H 0.4347 0.3188 0.0060 0.044 Uiso 1 d R . C14 C 0.5812(4) 0.2332(2) 0.0804(2) 0.0385(9) Uani 1 d . . H14 H 0.6385 0.2014 0.0423 0.046 Uiso 1 d R . C15 C 0.5988(3) 0.2244(2) 0.1662(2) 0.0317(7) Uani 1 d . . H15 H 0.6681 0.1846 0.1965 0.038 Uiso 1 d R . C16 C 0.6993(5) 0.4277(3) 0.1855(3) 0.0572(12) Uani 1 d . . H16 H 0.6903 0.4307 0.2432 0.069 Uiso 1 d R . C17 C 0.6178(5) 0.4792(3) 0.1255(3) 0.0601(13) Uani 1 d . . H17 H 0.5413 0.5233 0.1347 0.072 Uiso 1 d R . C18 C 0.6654(5) 0.4552(3) 0.0498(3) 0.0574(12) Uani 1 d . . H18 H 0.6278 0.4798 -0.0023 0.069 Uiso 1 d R . C19 C 0.7766(4) 0.3893(3) 0.0628(3) 0.0572(12) Uani 1 d . . H19 H 0.8291 0.3601 0.0212 0.069 Uiso 1 d R . C20 C 0.7987(4) 0.3718(3) 0.1466(3) 0.0572(12) Uani 1 d . . H20 H 0.8698 0.3294 0.1724 0.069 Uiso 1 d R . Ru1' Ru 1.06156(3) 0.334503(16) 0.858917(15) 0.02383(6) Uani 1 d . . H3 H 1.1887 0.2458 0.8927 0.045(10) Uiso 1 d R . H4 H 0.9591 0.2736 0.9268 0.043(10) Uiso 1 d R . Ru2' Ru 1.19169(3) 0.152618(17) 0.842619(15) 0.02626(6) Uani 1 d . . Ru3' Ru 0.91185(3) 0.185289(17) 0.885284(15) 0.02533(6) Uani 1 d . . Fe1' Fe 0.71831(5) 0.37588(3) 0.55692(3) 0.02510(10) Uani 1 d . . P1' P 1.01637(8) 0.23666(5) 0.77008(5) 0.02182(16) Uani 1 d . . C1' C 0.9046(4) 0.4219(2) 0.8366(2) 0.0335(8) Uani 1 d . . O1' O 0.8079(3) 0.47095(18) 0.82733(16) 0.0541(8) Uani 1 d . . C2' C 1.1728(4) 0.3868(2) 0.7780(2) 0.0381(8) Uani 1 d . . O2' O 1.2373(3) 0.4121(2) 0.72612(18) 0.0601(8) Uani 1 d . . C3' C 1.1099(3) 0.3834(2) 0.9588(2) 0.0312(7) Uani 1 d . . O3' O 1.1324(3) 0.41177(17) 1.01590(15) 0.0451(6) Uani 1 d . . C4' C 1.3652(4) 0.1667(3) 0.7946(2) 0.0430(9) Uani 1 d . . O4' O 1.4693(3) 0.1728(2) 0.7684(2) 0.0714(10) Uani 1 d . . C5' C 1.2469(4) 0.0923(3) 0.9498(2) 0.0442(9) Uani 1 d . . O5' O 1.2756(4) 0.0542(2) 1.01033(18) 0.0745(10) Uani 1 d . . C6' C 1.1844(4) 0.0484(3) 0.7949(2) 0.0427(9) Uani 1 d . . O6' O 1.1813(4) -0.0143(2) 0.7655(2) 0.0733(10) Uani 1 d . . C7' C 0.9280(4) 0.1312(2) 0.9981(2) 0.0379(8) Uani 1 d . . O7' O 0.9355(3) 0.0984(2) 1.06230(16) 0.0621(9) Uani 1 d . . C8' C 0.8679(4) 0.0843(3) 0.8434(2) 0.0411(9) Uani 1 d . . O8' O 0.8421(4) 0.0244(2) 0.81745(19) 0.0661(9) Uani 1 d . . C9' C 0.7289(4) 0.2477(3) 0.8799(2) 0.0384(9) Uani 1 d . . O9' O 0.6224(3) 0.2864(2) 0.87526(17) 0.0605(8) Uani 1 d . . C10' C 0.9621(3) 0.2623(2) 0.66322(18) 0.0271(7) Uani 1 d . . H10C H 0.9414 0.2102 0.6427 0.033 Uiso 1 d R . H10D H 1.0349 0.2819 0.6309 0.033 Uiso 1 d R . C11' C 0.8400(3) 0.3321(2) 0.65578(17) 0.0260(7) Uani 1 d . . C12' C 0.8403(4) 0.4236(2) 0.63350(19) 0.0335(8) Uani 1 d . . H12' H 0.9188 0.4503 0.6177 0.040 Uiso 1 d R . C13' C 0.7054(4) 0.4675(2) 0.6382(2) 0.0434(10) Uani 1 d . . H13' H 0.6757 0.5295 0.6259 0.052 Uiso 1 d R . C14' C 0.6210(4) 0.4045(3) 0.6638(2) 0.0437(10) Uani 1 d . . H14' H 0.5242 0.4161 0.6716 0.052 Uiso 1 d R . C15' C 0.7040(3) 0.3204(2) 0.67448(19) 0.0332(8) Uani 1 d . . H15' H 0.6737 0.2654 0.6910 0.040 Uiso 1 d R . C16' C 0.8052(4) 0.3186(3) 0.4591(2) 0.0399(9) Uani 1 d . . H16' H 0.8931 0.2828 0.4582 0.048 Uiso 1 d R . C17' C 0.7785(4) 0.4102(3) 0.4404(2) 0.0402(9) Uani 1 d . . H17' H 0.8441 0.4480 0.4247 0.048 Uiso 1 d R . C18' C 0.6378(4) 0.4369(2) 0.4493(2) 0.0411(9) Uani 1 d . . H18' H 0.5905 0.4961 0.4409 0.049 Uiso 1 d R . C19' C 0.5779(4) 0.3619(3) 0.4737(2) 0.0412(9) Uani 1 d . . H19' H 0.4829 0.3610 0.4844 0.049 Uiso 1 d R . C20' C 0.6812(4) 0.2886(2) 0.4790(2) 0.0399(9) Uani 1 d . . H20' H 0.6697 0.2288 0.4942 0.048 Uiso 1 d 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 Ru1 0.02444(13) 0.02311(13) 0.02255(13) -0.00260(10) -0.00177(10) -0.00415(10) Ru2 0.02598(13) 0.02776(14) 0.01850(12) 0.00001(10) 0.00252(10) -0.00450(11) Ru3 0.02660(14) 0.02256(13) 0.02696(13) 0.00026(10) 0.00051(10) -0.00291(10) Fe1 0.0235(2) 0.0301(2) 0.0246(2) -0.00009(19) 0.00256(18) -0.00683(19) P1 0.0242(4) 0.0238(4) 0.0181(4) -0.0010(3) 0.0015(3) -0.0049(3) C1 0.037(2) 0.0299(18) 0.034(2) -0.0038(15) -0.0058(15) -0.0070(15) O1 0.077(2) 0.0655(19) 0.0243(14) -0.0061(13) -0.0061(13) -0.0211(16) C2 0.0299(18) 0.033(2) 0.0311(18) -0.0057(14) -0.0056(14) -0.0055(15) O2 0.0576(18) 0.0277(15) 0.0575(17) -0.0051(12) -0.0090(14) -0.0015(13) C3 0.040(2) 0.035(2) 0.045(2) -0.0157(16) 0.0046(17) -0.0097(17) O3 0.0451(18) 0.070(2) 0.087(2) -0.0362(18) 0.0215(16) -0.0310(16) C4 0.038(2) 0.037(2) 0.0282(18) 0.0000(15) 0.0055(15) -0.0095(16) O4 0.066(2) 0.0338(16) 0.0603(18) -0.0101(13) 0.0095(15) -0.0054(14) C5 0.054(2) 0.038(2) 0.037(2) -0.0125(16) 0.0181(18) -0.0130(19) O5 0.079(2) 0.060(2) 0.082(2) -0.0189(17) 0.0478(19) -0.0380(18) C6 0.045(2) 0.044(2) 0.034(2) 0.0003(17) -0.0043(18) -0.0037(18) O6 0.073(2) 0.088(3) 0.058(2) 0.0023(18) -0.0353(18) -0.0071(19) C7 0.038(2) 0.034(2) 0.050(2) 0.0047(17) -0.0026(17) -0.0035(17) O7 0.0573(19) 0.0345(16) 0.090(2) 0.0083(15) -0.0007(17) -0.0146(14) C8 0.035(2) 0.034(2) 0.041(2) 0.0042(16) -0.0001(17) -0.0059(16) O8 0.0383(17) 0.066(2) 0.074(2) 0.0166(16) -0.0168(15) -0.0076(15) C9 0.0343(19) 0.0267(18) 0.042(2) -0.0056(15) -0.0017(16) -0.0020(15) O9 0.0604(19) 0.0602(19) 0.0407(16) -0.0226(14) 0.0146(14) -0.0114(15) C10 0.0334(18) 0.0320(18) 0.0222(16) -0.0045(13) 0.0033(13) -0.0126(14) C11 0.0254(16) 0.0254(16) 0.0245(16) -0.0029(13) 0.0052(13) -0.0100(13) C12 0.0233(17) 0.041(2) 0.0304(18) -0.0021(15) 0.0019(14) -0.0101(15) C13 0.038(2) 0.054(2) 0.0235(17) -0.0024(16) -0.0005(15) -0.0205(18) C14 0.047(2) 0.039(2) 0.0334(19) -0.0142(16) 0.0156(16) -0.0138(17) C15 0.0339(19) 0.0263(17) 0.0340(18) -0.0021(14) 0.0067(15) -0.0037(14) C16 0.080(3) 0.061(3) 0.043(2) -0.012(2) 0.004(2) -0.047(3) C17 0.048(3) 0.029(2) 0.105(4) -0.010(2) 0.011(3) -0.0133(19) C18 0.060(3) 0.062(3) 0.052(3) 0.021(2) -0.009(2) -0.036(2) C19 0.047(3) 0.075(3) 0.059(3) -0.019(2) 0.023(2) -0.034(2) C20 0.036(2) 0.052(3) 0.086(4) 0.004(2) -0.018(2) -0.017(2) Ru1' 0.02913(14) 0.02180(13) 0.02103(13) -0.00278(10) -0.00047(10) -0.00502(10) Ru2' 0.02923(14) 0.02527(13) 0.02236(13) -0.00201(10) -0.00425(10) 0.00177(11) Ru3' 0.03012(14) 0.02912(14) 0.01790(12) 0.00053(10) -0.00149(10) -0.00997(11) Fe1' 0.0270(2) 0.0276(2) 0.0184(2) -0.00163(18) -0.00304(18) 0.00221(19) P1' 0.0257(4) 0.0219(4) 0.0171(4) -0.0004(3) -0.0019(3) -0.0024(3) C1' 0.046(2) 0.0282(18) 0.0254(17) -0.0065(14) 0.0008(15) -0.0020(17) O1' 0.0630(19) 0.0462(17) 0.0444(16) -0.0102(13) -0.0039(14) 0.0218(15) C2' 0.050(2) 0.0293(18) 0.039(2) -0.0092(16) 0.0023(18) -0.0169(17) O2' 0.081(2) 0.0563(18) 0.0520(18) -0.0085(14) 0.0269(16) -0.0400(17) C3' 0.0327(19) 0.0302(18) 0.0314(19) -0.0013(15) 0.0007(15) -0.0086(15) O3' 0.0568(17) 0.0501(16) 0.0336(14) -0.0115(12) -0.0075(12) -0.0187(13) C4' 0.046(2) 0.047(2) 0.036(2) -0.0100(17) 0.0000(18) -0.0038(18) O4' 0.0447(19) 0.104(3) 0.070(2) -0.0209(19) 0.0209(16) -0.0204(18) C5' 0.048(2) 0.044(2) 0.036(2) -0.0013(18) -0.0065(18) 0.0041(18) O5' 0.090(3) 0.081(2) 0.0404(17) 0.0179(17) -0.0208(17) 0.012(2) C6' 0.051(2) 0.039(2) 0.036(2) -0.0067(17) -0.0008(17) 0.0029(18) O6' 0.109(3) 0.0410(18) 0.072(2) -0.0275(16) -0.001(2) -0.0060(18) C7' 0.043(2) 0.044(2) 0.0293(19) 0.0002(16) -0.0055(16) -0.0167(17) O7' 0.082(2) 0.076(2) 0.0283(15) 0.0217(14) -0.0074(14) -0.0279(18) C8' 0.053(2) 0.045(2) 0.0281(18) 0.0029(16) -0.0062(17) -0.0209(19) O8' 0.101(3) 0.0518(18) 0.0566(19) -0.0082(15) -0.0179(18) -0.0425(18) C9' 0.036(2) 0.059(2) 0.0216(17) -0.0031(16) 0.0018(15) -0.0123(19) O9' 0.0342(17) 0.101(3) 0.0401(16) -0.0042(16) 0.0023(13) 0.0045(16) C10' 0.0324(18) 0.0309(17) 0.0168(15) -0.0015(13) -0.0021(13) -0.0016(14) C11' 0.0317(18) 0.0310(17) 0.0144(14) -0.0010(12) -0.0029(13) -0.0028(14) C12' 0.046(2) 0.0293(18) 0.0252(17) -0.0022(14) -0.0114(15) -0.0036(16) C13' 0.065(3) 0.033(2) 0.0277(18) -0.0110(15) -0.0112(18) 0.0124(19) C14' 0.038(2) 0.065(3) 0.0202(17) -0.0065(17) 0.0005(15) 0.0186(19) C15' 0.0327(19) 0.046(2) 0.0185(16) 0.0029(14) 0.0005(14) -0.0024(16) C16' 0.040(2) 0.050(2) 0.0262(18) -0.0123(16) -0.0035(15) 0.0106(18) C17' 0.046(2) 0.049(2) 0.0226(17) 0.0012(16) 0.0039(16) -0.0037(18) C18' 0.053(2) 0.041(2) 0.0217(17) -0.0008(15) -0.0096(16) 0.0142(18) C19' 0.036(2) 0.056(2) 0.0304(19) -0.0115(17) -0.0106(16) 0.0013(18) C20' 0.056(2) 0.035(2) 0.0301(19) -0.0099(15) -0.0097(17) -0.0046(18) _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 Ru1 C2 1.894(3) . ? Ru1 C1 1.926(4) . ? Ru1 C3 1.959(4) . ? Ru1 P1 2.2828(9) . ? Ru1 Ru2 2.8379(5) . ? Ru1 Ru3 2.9311(5) . ? Ru2 C4 1.888(4) . ? Ru2 C6 1.904(4) . ? Ru2 C5 1.950(4) . ? Ru2 P1 2.2930(8) . ? Ru2 Ru3 2.9267(5) . ? Ru3 C8 1.907(4) . ? Ru3 C9 1.926(4) . ? Ru3 C7 1.976(4) . ? Ru3 P1 2.3153(9) . ? Fe1 C16 2.019(4) . ? Fe1 C20 2.024(4) . ? Fe1 C11 2.027(3) . ? Fe1 C15 2.030(3) . ? Fe1 C19 2.034(4) . ? Fe1 C17 2.035(4) . ? Fe1 C12 2.034(3) . ? Fe1 C18 2.045(4) . ? Fe1 C14 2.048(4) . ? Fe1 C13 2.049(3) . ? P1 C10 1.839(3) . ? C1 O1 1.124(4) . ? C2 O2 1.133(4) . ? C3 O3 1.129(4) . ? C4 O4 1.134(4) . ? C5 O5 1.130(4) . ? C6 O6 1.134(5) . ? C7 O7 1.122(4) . ? C8 O8 1.132(4) . ? C9 O9 1.130(4) . ? C10 C11 1.494(4) . ? C11 C12 1.419(4) . ? C11 C15 1.422(4) . ? C12 C13 1.425(5) . ? C13 C14 1.410(5) . ? C14 C15 1.420(5) . ? C16 C17 1.393(7) . ? C16 C20 1.399(6) . ? C17 C18 1.393(7) . ? C18 C19 1.386(7) . ? C19 C20 1.396(6) . ? Ru1' C2' 1.914(4) . ? Ru1' C1' 1.913(4) . ? Ru1' C3' 1.984(3) . ? Ru1' P1' 2.3168(8) . ? Ru1' Ru3' 2.9377(5) . ? Ru1' Ru2' 2.9463(6) . ? Ru2' C6' 1.883(4) . ? Ru2' C4' 1.920(4) . ? Ru2' C5' 1.958(4) . ? Ru2' P1' 2.2840(8) . ? Ru2' Ru3' 2.8386(5) . ? Ru3' C8' 1.892(4) . ? Ru3' C9' 1.922(4) . ? Ru3' C7' 1.958(4) . ? Ru3' P1' 2.2778(8) . ? Fe1' C19' 2.033(3) . ? Fe1' C16' 2.034(3) . ? Fe1' C18' 2.039(3) . ? Fe1' C20' 2.041(3) . ? Fe1' C13' 2.042(3) . ? Fe1' C17' 2.043(3) . ? Fe1' C12' 2.043(3) . ? Fe1' C11' 2.045(3) . ? Fe1' C15' 2.049(3) . ? Fe1' C14' 2.048(3) . ? P1' C10' 1.839(3) . ? C1' O1' 1.130(4) . ? C2' O2' 1.133(4) . ? C3' O3' 1.122(4) . ? C4' O4' 1.128(5) . ? C5' O5' 1.124(4) . ? C6' O6' 1.136(5) . ? C7' O7' 1.124(4) . ? C8' O8' 1.131(4) . ? C9' O9' 1.132(4) . ? C10' C11' 1.491(4) . ? C11' C15' 1.418(5) . ? C11' C12' 1.429(5) . ? C12' C13' 1.411(5) . ? C13' C14' 1.415(6) . ? C14' C15' 1.425(5) . ? C16' C17' 1.404(5) . ? C16' C20' 1.408(5) . ? C17' C18' 1.406(5) . ? C18' C19' 1.409(6) . ? C19' C20' 1.402(5) . ? 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 C2 Ru1 C1 94.52(14) . . ? C2 Ru1 C3 96.43(15) . . ? C1 Ru1 C3 102.26(15) . . ? C2 Ru1 P1 95.00(10) . . ? C1 Ru1 P1 105.78(11) . . ? C3 Ru1 P1 148.68(12) . . ? C2 Ru1 Ru2 95.05(10) . . ? C1 Ru1 Ru2 156.36(11) . . ? C3 Ru1 Ru2 98.09(11) . . ? P1 Ru1 Ru2 51.83(2) . . ? C2 Ru1 Ru3 145.38(10) . . ? C1 Ru1 Ru3 100.18(10) . . ? C3 Ru1 Ru3 110.60(11) . . ? P1 Ru1 Ru3 50.89(2) . . ? Ru2 Ru1 Ru3 60.944(9) . . ? C4 Ru2 C6 93.06(16) . . ? C4 Ru2 C5 99.73(15) . . ? C6 Ru2 C5 102.48(17) . . ? C4 Ru2 P1 98.58(10) . . ? C6 Ru2 P1 108.54(12) . . ? C5 Ru2 P1 142.82(11) . . ? C4 Ru2 Ru1 94.74(11) . . ? C6 Ru2 Ru1 159.50(12) . . ? C5 Ru2 Ru1 94.85(12) . . ? P1 Ru2 Ru1 51.51(2) . . ? C4 Ru2 Ru3 148.36(10) . . ? C6 Ru2 Ru3 103.96(12) . . ? C5 Ru2 Ru3 102.28(10) . . ? P1 Ru2 Ru3 50.91(2) . . ? Ru1 Ru2 Ru3 61.100(11) . . ? C8 Ru3 C9 93.61(15) . . ? C8 Ru3 C7 100.59(15) . . ? C9 Ru3 C7 95.21(15) . . ? C8 Ru3 P1 95.29(11) . . ? C9 Ru3 P1 99.56(10) . . ? C7 Ru3 P1 157.54(11) . . ? C8 Ru3 Ru2 97.01(11) . . ? C9 Ru3 Ru2 148.68(10) . . ? C7 Ru3 Ru2 111.53(12) . . ? P1 Ru3 Ru2 50.24(2) . . ? C8 Ru3 Ru1 144.64(11) . . ? C9 Ru3 Ru1 97.91(10) . . ? C7 Ru3 Ru1 111.42(11) . . ? P1 Ru3 Ru1 49.91(2) . . ? Ru2 Ru3 Ru1 57.956(11) . . ? C16 Fe1 C20 40.49(19) . . ? C16 Fe1 C11 106.28(15) . . ? C20 Fe1 C11 123.53(17) . . ? C16 Fe1 C15 119.91(17) . . ? C20 Fe1 C15 106.68(16) . . ? C11 Fe1 C15 41.05(12) . . ? C16 Fe1 C19 67.61(18) . . ? C20 Fe1 C19 40.25(18) . . ? C11 Fe1 C19 161.00(18) . . ? C15 Fe1 C19 124.92(18) . . ? C16 Fe1 C17 40.19(19) . . ? C20 Fe1 C17 67.52(18) . . ? C11 Fe1 C17 120.78(17) . . ? C15 Fe1 C17 155.53(18) . . ? C19 Fe1 C17 66.99(19) . . ? C16 Fe1 C12 124.42(17) . . ? C20 Fe1 C12 160.87(18) . . ? C11 Fe1 C12 40.91(13) . . ? C15 Fe1 C12 68.68(14) . . ? C19 Fe1 C12 157.34(17) . . ? C17 Fe1 C12 108.56(16) . . ? C16 Fe1 C18 67.49(18) . . ? C20 Fe1 C18 67.40(18) . . ? C11 Fe1 C18 156.52(17) . . ? C15 Fe1 C18 161.97(18) . . ? C19 Fe1 C18 39.72(19) . . ? C17 Fe1 C18 39.91(19) . . ? C12 Fe1 C18 122.52(17) . . ? C16 Fe1 C14 155.81(19) . . ? C20 Fe1 C14 121.29(18) . . ? C11 Fe1 C14 68.62(13) . . ? C15 Fe1 C14 40.74(14) . . ? C19 Fe1 C14 109.12(16) . . ? C17 Fe1 C14 162.72(19) . . ? C12 Fe1 C14 68.10(14) . . ? C18 Fe1 C14 126.38(17) . . ? C16 Fe1 C13 162.03(19) . . ? C20 Fe1 C13 156.50(18) . . ? C11 Fe1 C13 68.97(13) . . ? C15 Fe1 C13 68.62(15) . . ? C19 Fe1 C13 122.35(16) . . ? C17 Fe1 C13 126.20(18) . . ? C12 Fe1 C13 40.87(13) . . ? C18 Fe1 C13 109.57(16) . . ? C14 Fe1 C13 40.26(15) . . ? C10 P1 Ru1 132.06(11) . . ? C10 P1 Ru2 138.82(10) . . ? Ru1 P1 Ru2 76.66(3) . . ? C10 P1 Ru3 128.64(11) . . ? Ru1 P1 Ru3 79.20(3) . . ? Ru2 P1 Ru3 78.85(3) . . ? O1 C1 Ru1 179.2(3) . . ? O2 C2 Ru1 178.9(3) . . ? O3 C3 Ru1 177.9(3) . . ? O4 C4 Ru2 178.6(3) . . ? O5 C5 Ru2 177.0(3) . . ? O6 C6 Ru2 179.0(4) . . ? O7 C7 Ru3 176.0(3) . . ? O8 C8 Ru3 177.0(3) . . ? O9 C9 Ru3 178.3(3) . . ? C11 C10 P1 109.5(2) . . ? C12 C11 C15 107.6(3) . . ? C12 C11 C10 126.3(3) . . ? C15 C11 C10 126.2(3) . . ? C12 C11 Fe1 69.80(17) . . ? C15 C11 Fe1 69.58(18) . . ? C10 C11 Fe1 127.0(2) . . ? C11 C12 C13 108.5(3) . . ? C11 C12 Fe1 69.30(18) . . ? C13 C12 Fe1 70.15(19) . . ? C14 C13 C12 107.4(3) . . ? C14 C13 Fe1 69.8(2) . . ? C12 C13 Fe1 68.99(19) . . ? C13 C14 C15 108.7(3) . . ? C13 C14 Fe1 69.9(2) . . ? C15 C14 Fe1 68.93(19) . . ? C14 C15 C11 107.9(3) . . ? C14 C15 Fe1 70.3(2) . . ? C11 C15 Fe1 69.37(18) . . ? C17 C16 C20 107.8(4) . . ? C17 C16 Fe1 70.5(2) . . ? C20 C16 Fe1 70.0(2) . . ? C18 C17 C16 108.3(4) . . ? C18 C17 Fe1 70.4(2) . . ? C16 C17 Fe1 69.3(2) . . ? C19 C18 C17 107.9(4) . . ? C19 C18 Fe1 69.7(2) . . ? C17 C18 Fe1 69.7(2) . . ? C18 C19 C20 108.5(4) . . ? C18 C19 Fe1 70.6(2) . . ? C20 C19 Fe1 69.5(2) . . ? C19 C20 C16 107.5(4) . . ? C19 C20 Fe1 70.3(2) . . ? C16 C20 Fe1 69.6(2) . . ? C2' Ru1' C1' 94.51(16) . . ? C2' Ru1' C3' 102.07(14) . . ? C1' Ru1' C3' 94.17(14) . . ? C2' Ru1' P1' 90.46(10) . . ? C1' Ru1' P1' 98.09(10) . . ? C3' Ru1' P1' 161.73(10) . . ? C2' Ru1' Ru3' 139.85(10) . . ? C1' Ru1' Ru3' 95.69(11) . . ? C3' Ru1' Ru3' 115.73(9) . . ? P1' Ru1' Ru3' 49.67(2) . . ? C2' Ru1' Ru2' 95.06(11) . . ? C1' Ru1' Ru2' 146.35(10) . . ? C3' Ru1' Ru2' 115.12(10) . . ? P1' Ru1' Ru2' 49.69(2) . . ? Ru3' Ru1' Ru2' 57.688(14) . . ? C6' Ru2' C4' 93.41(17) . . ? C6' Ru2' C5' 94.49(16) . . ? C4' Ru2' C5' 101.01(17) . . ? C6' Ru2' P1' 96.30(12) . . ? C4' Ru2' P1' 111.92(12) . . ? C5' Ru2' P1' 144.52(12) . . ? C6' Ru2' Ru3' 96.12(12) . . ? C4' Ru2' Ru3' 161.62(12) . . ? C5' Ru2' Ru3' 93.88(12) . . ? P1' Ru2' Ru3' 51.42(2) . . ? C6' Ru2' Ru1' 146.58(12) . . ? C4' Ru2' Ru1' 103.28(12) . . ? C5' Ru2' Ru1' 110.09(11) . . ? P1' Ru2' Ru1' 50.67(2) . . ? Ru3' Ru2' Ru1' 61.004(9) . . ? C8' Ru3' C9' 94.65(17) . . ? C8' Ru3' C7' 94.50(15) . . ? C9' Ru3' C7' 103.51(15) . . ? C8' Ru3' P1' 95.97(11) . . ? C9' Ru3' P1' 105.30(10) . . ? C7' Ru3' P1' 148.34(11) . . ? C8' Ru3' Ru2' 95.20(12) . . ? C9' Ru3' Ru2' 155.76(11) . . ? C7' Ru3' Ru2' 97.73(11) . . ? P1' Ru3' Ru2' 51.62(2) . . ? C8' Ru3' Ru1' 146.31(11) . . ? C9' Ru3' Ru1' 99.53(12) . . ? C7' Ru3' Ru1' 111.40(10) . . ? P1' Ru3' Ru1' 50.84(2) . . ? Ru2' Ru3' Ru1' 61.308(12) . . ? C19' Fe1' C16' 67.91(15) . . ? C19' Fe1' C18' 40.49(16) . . ? C16' Fe1' C18' 67.66(14) . . ? C19' Fe1' C20' 40.27(15) . . ? C16' Fe1' C20' 40.43(15) . . ? C18' Fe1' C20' 67.72(15) . . ? C19' Fe1' C13' 128.01(15) . . ? C16' Fe1' C13' 151.77(17) . . ? C18' Fe1' C13' 107.98(15) . . ? C20' Fe1' C13' 166.09(17) . . ? C19' Fe1' C17' 68.05(16) . . ? C16' Fe1' C17' 40.29(15) . . ? C18' Fe1' C17' 40.29(15) . . ? C20' Fe1' C17' 67.89(16) . . ? C13' Fe1' C17' 118.07(16) . . ? C19' Fe1' C12' 165.15(15) . . ? C16' Fe1' C12' 118.43(15) . . ? C18' Fe1' C12' 127.07(15) . . ? C20' Fe1' C12' 152.72(15) . . ? C13' Fe1' C12' 40.40(15) . . ? C17' Fe1' C12' 107.37(15) . . ? C19' Fe1' C11' 152.97(15) . . ? C16' Fe1' C11' 108.16(13) . . ? C18' Fe1' C11' 164.99(15) . . ? C20' Fe1' C11' 119.19(14) . . ? C13' Fe1' C11' 68.44(13) . . ? C17' Fe1' C11' 127.33(14) . . ? C12' Fe1' C11' 40.93(13) . . ? C19' Fe1' C15' 119.55(16) . . ? C16' Fe1' C15' 128.28(15) . . ? C18' Fe1' C15' 153.22(15) . . ? C20' Fe1' C15' 109.06(15) . . ? C13' Fe1' C15' 68.40(15) . . ? C17' Fe1' C15' 165.44(14) . . ? C12' Fe1' C15' 68.40(14) . . ? C11' Fe1' C15' 40.53(13) . . ? C19' Fe1' C14' 108.98(16) . . ? C16' Fe1' C14' 166.51(17) . . ? C18' Fe1' C14' 119.17(14) . . ? C20' Fe1' C14' 128.85(17) . . ? C13' Fe1' C14' 40.46(16) . . ? C17' Fe1' C14' 152.16(16) . . ? C12' Fe1' C14' 68.03(16) . . ? C11' Fe1' C14' 68.25(13) . . ? C15' Fe1' C14' 40.70(14) . . ? C10' P1' Ru3' 132.97(11) . . ? C10' P1' Ru2' 138.32(11) . . ? Ru3' P1' Ru2' 76.96(3) . . ? C10' P1' Ru1' 127.30(11) . . ? Ru3' P1' Ru1' 79.48(3) . . ? Ru2' P1' Ru1' 79.64(3) . . ? O1' C1' Ru1' 175.7(3) . . ? O2' C2' Ru1' 174.1(3) . . ? O3' C3' Ru1' 177.5(3) . . ? O4' C4' Ru2' 177.5(4) . . ? O5' C5' Ru2' 176.4(4) . . ? O6' C6' Ru2' 179.2(4) . . ? O7' C7' Ru3' 178.1(3) . . ? O8' C8' Ru3' 179.2(3) . . ? O9' C9' Ru3' 178.0(3) . . ? C11' C10' P1' 110.8(2) . . ? C15' C11' C12' 107.8(3) . . ? C15' C11' C10' 126.1(3) . . ? C12' C11' C10' 126.0(3) . . ? C15' C11' Fe1' 69.88(18) . . ? C12' C11' Fe1' 69.47(18) . . ? C10' C11' Fe1' 129.0(2) . . ? C13' C12' C11' 108.1(3) . . ? C13' C12' Fe1' 69.8(2) . . ? C11' C12' Fe1' 69.60(18) . . ? C12' C13' C14' 108.2(3) . . ? C12' C13' Fe1' 69.84(19) . . ? C14' C13' Fe1' 70.0(2) . . ? C13' C14' C15' 108.2(3) . . ? C13' C14' Fe1' 69.5(2) . . ? C15' C14' Fe1' 69.66(19) . . ? C11' C15' C14' 107.8(3) . . ? C11' C15' Fe1' 69.59(17) . . ? C14' C15' Fe1' 69.64(19) . . ? C17' C16' C20' 108.4(3) . . ? C17' C16' Fe1' 70.2(2) . . ? C20' C16' Fe1' 70.1(2) . . ? C16' C17' C18' 107.6(3) . . ? C16' C17' Fe1' 69.5(2) . . ? C18' C17' Fe1' 69.7(2) . . ? C17' C18' C19' 108.2(3) . . ? C17' C18' Fe1' 70.0(2) . . ? C19' C18' Fe1' 69.5(2) . . ? C20' C19' C18' 107.9(3) . . ? C20' C19' Fe1' 70.2(2) . . ? C18' C19' Fe1' 70.0(2) . . ? C19' C20' C16' 107.9(3) . . ? C19' C20' Fe1' 69.6(2) . . ? C16' C20' Fe1' 69.5(2) . . ? _refine_diff_density_max 0.480 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.073 data_nick _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C16 H13 Fe Mo O5 P' _chemical_formula_sum 'C16 H13 Fe Mo O5 P' _chemical_formula_weight 468.02 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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.48160(10) _cell_length_b 10.44120(10) _cell_length_c 11.53050(10) _cell_angle_alpha 90.00 _cell_angle_beta 96.7800(10) _cell_angle_gamma 90.00 _cell_volume 894.428(17) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 2093 _cell_measurement_theta_min 1.78 _cell_measurement_theta_max 28.27 _exptl_crystal_description flake _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 464 _exptl_absorpt_coefficient_mu 1.622 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.755 _exptl_absorpt_correction_T_max 0.908 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'Siemens SMART CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2087 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 28.27 _reflns_number_total 2087 _reflns_number_gt 2000 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.09(2) _refine_ls_number_reflns 2087 _refine_ls_number_parameters 217 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0230 _refine_ls_R_factor_gt 0.0213 _refine_ls_wR_factor_ref 0.0476 _refine_ls_wR_factor_gt 0.0469 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.008 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo Mo 0.73574(4) 0.71722(3) -0.00178(3) 0.03139(8) Uani 1 d . . . P P 0.60002(12) 0.65700(10) 0.17913(8) 0.0346(2) Uani 1 d . . . H2A H 0.4713 0.5808 0.1800 0.050 Uiso 1 d . . . H2B H 0.5250 0.7359 0.2400 0.050 Uiso 1 d . . . C2 C 0.4884(6) 0.7648(4) -0.0862(4) 0.0434(9) Uani 1 d . . . C3 C 0.6982(5) 0.5372(4) -0.0637(4) 0.0426(9) Uani 1 d . . . C6 C 0.8483(6) 0.7709(5) -0.1438(4) 0.0548(12) Uani 1 d . . . C5 C 0.7685(6) 0.8980(4) 0.0699(4) 0.0457(10) Uani 1 d . . . O5 O 0.7833(5) 0.9964(3) 0.1126(3) 0.0693(10) Uani 1 d . . . O4 O 1.1197(4) 0.6227(4) 0.1140(3) 0.0724(12) Uani 1 d . . . O3 O 0.6813(5) 0.4346(4) -0.0981(3) 0.0676(9) Uani 1 d . . . O2 O 0.3517(4) 0.7893(4) -0.1375(3) 0.0683(10) Uani 1 d . . . O6 O 0.9117(6) 0.8000(5) -0.2257(3) 0.0947(15) Uani 1 d . . . C4 C 0.9830(5) 0.6601(4) 0.0749(4) 0.0435(10) Uani 1 d . . . Fe Fe 0.74088(5) 0.41982(4) 0.53114(4) 0.02259(10) Uani 1 d . . . C11 C 0.6474(4) 0.5459(3) 0.4020(3) 0.0267(7) Uani 1 d . . . C25 C 0.9993(4) 0.4131(4) 0.6114(3) 0.0374(8) Uani 1 d . . . H25 H 1.0681 0.4824 0.6439 0.045 Uiso 1 calc R . . C1 C 0.7416(4) 0.5763(3) 0.2981(3) 0.0295(7) Uani 1 d . . . H1A H 0.7872 0.4964 0.2680 0.035 Uiso 1 calc R . . H1B H 0.8455 0.6310 0.3231 0.035 Uiso 1 calc R . . C14 C 0.5626(4) 0.5487(4) 0.5878(3) 0.0334(8) Uani 1 d . . . H14 H 0.5539 0.5714 0.6659 0.040 Uiso 1 calc R . . C12 C 0.5203(4) 0.4450(3) 0.4114(3) 0.0285(7) Uani 1 d . . . H12 H 0.4777 0.3874 0.3518 0.034 Uiso 1 calc R . . C21 C 0.9905(5) 0.3694(4) 0.4958(4) 0.0384(8) Uani 1 d . . . H21 H 1.0527 0.4046 0.4371 0.046 Uiso 1 calc R . . C13 C 0.4696(4) 0.4471(3) 0.5262(3) 0.0319(8) Uani 1 d . . . H13 H 0.3884 0.3908 0.5561 0.038 Uiso 1 calc R . . C15 C 0.6713(4) 0.6105(3) 0.5122(3) 0.0289(7) Uani 1 d . . . H15 H 0.7461 0.6817 0.5311 0.035 Uiso 1 calc R . . C24 C 0.8844(5) 0.3331(4) 0.6704(3) 0.0393(9) Uani 1 d . . . H24 H 0.8639 0.3405 0.7490 0.047 Uiso 1 calc R . . C23 C 0.8072(5) 0.2411(4) 0.5901(4) 0.0417(9) Uani 1 d . . . H23 H 0.7264 0.1762 0.6056 0.050 Uiso 1 calc R . . C22 C 0.8731(5) 0.2642(4) 0.4823(4) 0.0419(9) Uani 1 d . . . H22 H 0.8435 0.2171 0.4133 0.050 Uiso 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 0.03346(15) 0.03690(15) 0.02377(13) 0.00350(12) 0.00326(9) -0.00053(14) P 0.0322(4) 0.0437(5) 0.0281(5) 0.0109(4) 0.0042(4) 0.0106(4) C2 0.052(2) 0.038(2) 0.039(2) 0.0068(17) -0.0017(19) -0.0039(18) C3 0.045(2) 0.052(3) 0.032(2) -0.0028(18) 0.0117(16) -0.0028(19) C6 0.053(2) 0.077(3) 0.034(2) 0.008(2) 0.0061(18) -0.016(2) C5 0.053(2) 0.043(3) 0.041(2) 0.0104(17) 0.0026(18) -0.0014(19) O5 0.101(3) 0.0369(18) 0.066(2) -0.0001(16) -0.0037(19) -0.0027(18) O4 0.0427(16) 0.097(3) 0.072(3) -0.038(2) -0.0135(16) 0.0227(18) O3 0.086(2) 0.059(2) 0.061(2) -0.0230(19) 0.0230(17) -0.0140(19) O2 0.059(2) 0.070(2) 0.069(2) 0.0190(19) -0.0203(17) 0.0087(17) O6 0.090(3) 0.146(4) 0.053(2) 0.020(3) 0.032(2) -0.026(3) C4 0.040(2) 0.053(2) 0.038(2) -0.0139(18) 0.0048(17) 0.0024(18) Fe 0.0214(2) 0.0213(2) 0.0251(2) 0.00301(18) 0.00304(16) 0.00233(17) C11 0.0242(14) 0.0250(16) 0.0302(17) 0.0062(13) -0.0001(12) 0.0028(12) C25 0.0260(15) 0.0345(19) 0.048(2) 0.0064(19) -0.0097(14) 0.0052(15) C1 0.0254(15) 0.0334(17) 0.0291(17) 0.0055(14) 0.0013(13) -0.0001(13) C14 0.0322(17) 0.0346(18) 0.0339(19) 0.0006(15) 0.0062(14) 0.0106(15) C12 0.0217(14) 0.0281(19) 0.0346(18) 0.0016(13) -0.0014(13) -0.0003(13) C21 0.0256(15) 0.051(2) 0.040(2) 0.0114(17) 0.0083(14) 0.0111(16) C13 0.0224(15) 0.031(2) 0.043(2) 0.0093(14) 0.0065(13) 0.0016(13) C15 0.0299(16) 0.0197(15) 0.0361(19) -0.0005(13) -0.0002(13) 0.0035(13) C24 0.0411(19) 0.045(2) 0.0318(19) 0.0158(16) 0.0046(15) 0.0156(17) C23 0.0343(17) 0.026(2) 0.064(3) 0.0135(17) 0.0049(16) 0.0034(15) C22 0.0390(19) 0.039(2) 0.047(2) -0.0097(17) 0.0009(16) 0.0175(16) _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 C6 2.007(4) . ? Mo C3 2.019(4) . ? Mo C4 2.043(4) . ? Mo C2 2.048(4) . ? Mo C5 2.063(5) . ? Mo P 2.5056(10) . ? P C1 1.836(3) . ? C2 O2 1.148(5) . ? C3 O3 1.143(5) . ? C6 O6 1.148(5) . ? C5 O5 1.140(6) . ? O4 C4 1.137(5) . ? Fe C22 2.017(4) . ? Fe C23 2.027(4) . ? Fe C21 2.027(4) . ? Fe C24 2.036(3) . ? Fe C12 2.040(3) . ? Fe C13 2.043(3) . ? Fe C25 2.044(3) . ? Fe C11 2.048(3) . ? Fe C14 2.055(3) . ? Fe C15 2.063(3) . ? C11 C15 1.431(5) . ? C11 C12 1.432(5) . ? C11 C1 1.494(4) . ? C25 C21 1.403(6) . ? C25 C24 1.427(5) . ? C14 C13 1.413(5) . ? C14 C15 1.416(5) . ? C12 C13 1.420(5) . ? C21 C22 1.403(6) . ? C24 C23 1.409(6) . ? C23 C22 1.411(6) . ? 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 C6 Mo C3 91.49(19) . . ? C6 Mo C4 89.38(18) . . ? C3 Mo C4 87.82(17) . . ? C6 Mo C2 89.25(18) . . ? C3 Mo C2 88.73(17) . . ? C4 Mo C2 176.26(18) . . ? C6 Mo C5 91.71(19) . . ? C3 Mo C5 176.80(18) . . ? C4 Mo C5 92.01(17) . . ? C2 Mo C5 91.51(17) . . ? C6 Mo P 177.98(15) . . ? C3 Mo P 90.44(12) . . ? C4 Mo P 90.09(13) . . ? C2 Mo P 91.39(12) . . ? C5 Mo P 86.36(12) . . ? C1 P Mo 118.84(11) . . ? O2 C2 Mo 177.3(4) . . ? O3 C3 Mo 178.4(4) . . ? O6 C6 Mo 179.0(5) . . ? O5 C5 Mo 177.6(4) . . ? O4 C4 Mo 176.4(4) . . ? C22 Fe C23 40.84(18) . . ? C22 Fe C21 40.60(17) . . ? C23 Fe C21 68.51(16) . . ? C22 Fe C24 68.37(17) . . ? C23 Fe C24 40.60(17) . . ? C21 Fe C24 68.32(15) . . ? C22 Fe C12 107.41(15) . . ? C23 Fe C12 119.48(15) . . ? C21 Fe C12 126.01(16) . . ? C24 Fe C12 154.24(15) . . ? C22 Fe C13 128.53(15) . . ? C23 Fe C13 109.92(14) . . ? C21 Fe C13 164.99(15) . . ? C24 Fe C13 120.91(14) . . ? C12 Fe C13 40.70(15) . . ? C22 Fe C25 68.27(16) . . ? C23 Fe C25 68.63(16) . . ? C21 Fe C25 40.33(16) . . ? C24 Fe C25 40.97(15) . . ? C12 Fe C25 163.20(13) . . ? C13 Fe C25 154.25(16) . . ? C22 Fe C11 116.84(16) . . ? C23 Fe C11 152.20(16) . . ? C21 Fe C11 105.31(15) . . ? C24 Fe C11 164.25(15) . . ? C12 Fe C11 41.02(13) . . ? C13 Fe C11 68.75(13) . . ? C25 Fe C11 125.07(15) . . ? C22 Fe C14 167.06(16) . . ? C23 Fe C14 129.66(16) . . ? C21 Fe C14 151.86(16) . . ? C24 Fe C14 110.00(15) . . ? C12 Fe C14 68.13(14) . . ? C13 Fe C14 40.34(14) . . ? C25 Fe C14 119.54(15) . . ? C11 Fe C14 68.39(14) . . ? C22 Fe C15 150.93(16) . . ? C23 Fe C15 166.51(17) . . ? C21 Fe C15 117.15(16) . . ? C24 Fe C15 128.01(16) . . ? C12 Fe C15 68.28(13) . . ? C13 Fe C15 67.97(13) . . ? C25 Fe C15 107.12(15) . . ? C11 Fe C15 40.74(14) . . ? C14 Fe C15 40.22(14) . . ? C15 C11 C12 107.1(3) . . ? C15 C11 C1 126.2(3) . . ? C12 C11 C1 126.7(3) . . ? C15 C11 Fe 70.19(18) . . ? C12 C11 Fe 69.20(18) . . ? C1 C11 Fe 124.5(2) . . ? C21 C25 C24 107.4(4) . . ? C21 C25 Fe 69.22(19) . . ? C24 C25 Fe 69.22(19) . . ? C11 C1 P 114.3(2) . . ? C13 C14 C15 108.5(3) . . ? C13 C14 Fe 69.39(19) . . ? C15 C14 Fe 70.20(19) . . ? C13 C12 C11 108.2(3) . . ? C13 C12 Fe 69.77(18) . . ? C11 C12 Fe 69.79(17) . . ? C22 C21 C25 108.6(4) . . ? C22 C21 Fe 69.3(2) . . ? C25 C21 Fe 70.5(2) . . ? C14 C13 C12 108.1(3) . . ? C14 C13 Fe 70.27(18) . . ? C12 C13 Fe 69.54(17) . . ? C14 C15 C11 108.2(3) . . ? C14 C15 Fe 69.58(19) . . ? C11 C15 Fe 69.07(19) . . ? C23 C24 C25 108.0(3) . . ? C23 C24 Fe 69.4(2) . . ? C25 C24 Fe 69.8(2) . . ? C24 C23 C22 107.7(3) . . ? C24 C23 Fe 70.0(2) . . ? C22 C23 Fe 69.2(2) . . ? C21 C22 C23 108.4(4) . . ? C21 C22 Fe 70.1(2) . . ? C23 C22 Fe 70.0(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 C1 P Mo 179.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.896 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.896 _refine_diff_density_max 0.293 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.062