Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Mays, M.J.' 'Raithby, Paul R.' 'Sarveswaran, Koshala' 'Solan, Gregory A.' _publ_contact_author_name 'Dr M.J Mays' _publ_contact_author_address ; Deparment of Chemistry Lensfield Road, Cambridge. CB2 1EW ; _publ_contact_author_email 'MJM14@CAM.AC.UK' _publ_section_title ; Perpendicular to Parallel Reorientation of a Terminal Alkyne on a Mixed-Metal Triangle; Synthesis and Structural Characterisation ; data_mm9605 _database_code_CSD 175751 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C31 H21 Fe2 Mo O6 P' _chemical_formula_weight 728.09 _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' 'Mo' 'Mo' -1.6832 0.6857 '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 ? _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.108(2) _cell_length_b 13.177(3) _cell_length_c 10.810(2) _cell_angle_alpha 100.85(2) _cell_angle_beta 111.250(10) _cell_angle_gamma 74.77(2) _cell_volume 1415.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 1 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.709 _exptl_crystal_density_method ? _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 1.548 _exptl_absorpt_correction_type 'empirical (10 psi scans)' _exptl_absorpt_correction_T_min 0.863 _exptl_absorpt_correction_T_max 0.999 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Rigaku AFC5-R _diffrn_measurement_method 'omega-2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4 _diffrn_reflns_number 5255 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0707 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4973 _reflns_number_observed 3610 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'standard MSC/Rigaku supplied software' _computing_cell_refinement 'standard MSC/Rigaku supplied software' _computing_data_reduction 'MSC teXsan' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XP' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 9 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^)+(0.1000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4964 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0798 _refine_ls_R_factor_obs 0.0380 _refine_ls_wR_factor_all 0.1566 _refine_ls_wR_factor_obs 0.1076 _refine_ls_goodness_of_fit_all 0.884 _refine_ls_goodness_of_fit_obs 0.829 _refine_ls_restrained_S_all 1.015 _refine_ls_restrained_S_obs 0.829 _refine_ls_shift/esd_max 0.121 _refine_ls_shift/esd_mean 0.010 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 Mo1 Mo 0.20793(4) 0.82648(3) 0.27619(4) 0.0313(2) Uani 1 d . . Fe1 Fe 0.15893(7) 0.63371(6) 0.13661(7) 0.0339(2) Uani 1 d . . Fe2 Fe 0.31061(7) 0.72871(6) 0.09082(7) 0.0325(2) Uani 1 d . . P1 P 0.39662(13) 0.85264(11) 0.23278(14) 0.0330(3) Uani 1 d . . C1 C -0.0061(6) 0.6532(4) 0.1351(5) 0.0404(13) Uani 1 d . . O1 O -0.1117(5) 0.6672(4) 0.1377(5) 0.0659(13) Uani 1 d . . C2 C 0.2566(6) 0.7816(5) -0.0649(6) 0.0422(13) Uani 1 d . . O2 O 0.2186(5) 0.8167(4) -0.1641(4) 0.0621(12) Uani 1 d . . C3 C 0.1985(6) 0.4952(5) 0.1529(6) 0.0461(14) Uani 1 d . . O3 O 0.2263(6) 0.4078(4) 0.1684(6) 0.080(2) Uani 1 d . . C4 C 0.4509(6) 0.6475(4) 0.0546(5) 0.0375(12) Uani 1 d . . O4 O 0.5451(4) 0.6026(4) 0.0328(5) 0.0583(11) Uani 1 d . . C5 C 0.0967(5) 0.8302(5) 0.0882(6) 0.0417(13) Uani 1 d . . O5 O 0.0114(4) 0.8602(4) -0.0085(4) 0.0540(11) Uani 1 d . . C6 C 0.1312(6) 0.6186(5) -0.0400(6) 0.0487(15) Uani 1 d . . O6 O 0.0955(6) 0.5990(5) -0.1537(5) 0.081(2) Uani 1 d . . C7 C 0.2045(7) 0.8997(5) 0.4929(6) 0.052(2) Uani 1 d . . H7 H 0.2664 0.8738 0.5773 0.062 Uiso 1 calc R . C8 C 0.0833(7) 0.8734(5) 0.4220(7) 0.059(2) Uani 1 d . . H8 H 0.0457 0.8247 0.4480 0.071 Uiso 1 calc R . C9 C 0.0181(6) 0.9345(6) 0.3158(7) 0.066(2) Uani 1 d . . H9 H -0.0732 0.9371 0.2561 0.079 Uiso 1 calc R . C10 C 0.1013(7) 1.0007(5) 0.3179(7) 0.057(2) Uani 1 d . . H10 H 0.0777 1.0581 0.2618 0.068 Uiso 1 calc R . C11 C 0.2154(6) 0.9791(5) 0.4296(7) 0.052(2) Uani 1 d . . H11 H 0.2871 1.0178 0.4627 0.062 Uiso 1 calc R . C12 C 0.5588(5) 0.8115(4) 0.3571(6) 0.0385(12) Uani 1 d . . C13 C 0.5713(6) 0.8169(5) 0.4905(6) 0.0454(14) Uani 1 d . . H13 H 0.4977 0.8464 0.5172 0.055 Uiso 1 calc R . C14 C 0.6924(7) 0.7789(6) 0.5853(6) 0.058(2) Uani 1 d . . H14 H 0.6991 0.7827 0.6743 0.070 Uiso 1 calc R . C15 C 0.8017(6) 0.7357(5) 0.5461(7) 0.058(2) Uani 1 d . . H15 H 0.8823 0.7090 0.6083 0.069 Uiso 1 calc R . C16 C 0.7912(6) 0.7321(6) 0.4146(7) 0.061(2) Uani 1 d . . H16 H 0.8655 0.7045 0.3886 0.073 Uiso 1 calc R . C17 C 0.6711(6) 0.7692(5) 0.3208(6) 0.0495(15) Uani 1 d . . H17 H 0.6654 0.7658 0.2322 0.059 Uiso 1 calc R . C18 C 0.4025(5) 0.9722(4) 0.1762(5) 0.0375(12) Uani 1 d . . C19 C 0.2880(6) 1.0273(5) 0.0906(6) 0.0476(15) Uani 1 d . . H19 H 0.2100 1.0029 0.0635 0.057 Uiso 1 calc R . C20 C 0.2888(7) 1.1188(5) 0.0449(7) 0.059(2) Uani 1 d . . H20 H 0.2110 1.1559 -0.0114 0.070 Uiso 1 calc R . C21 C 0.4029(7) 1.1550(5) 0.0819(7) 0.056(2) Uani 1 d . . H21 H 0.4031 1.2157 0.0498 0.068 Uiso 1 calc R . C22 C 0.5178(7) 1.1007(5) 0.1674(7) 0.058(2) Uani 1 d . . H22 H 0.5953 1.1256 0.1936 0.070 Uiso 1 calc R . C23 C 0.5188(6) 1.0104(5) 0.2140(6) 0.0463(14) Uani 1 d . . H23 H 0.5970 0.9743 0.2709 0.056 Uiso 1 calc R . C24 C 0.3378(6) 0.6612(4) 0.2571(5) 0.0347(12) Uani 1 d . . H24 H 0.4176(54) 0.6265(43) 0.2845(53) 0.034(15) Uiso 1 d . . C25 C 0.2490(5) 0.6732(4) 0.3278(5) 0.0325(11) Uani 1 d . . C26 C 0.2716(5) 0.6313(4) 0.4536(5) 0.0372(12) Uani 1 d . . C27 C 0.3897(6) 0.6297(5) 0.5573(6) 0.0473(14) Uani 1 d . . H27 H 0.4566 0.6539 0.5470 0.057 Uiso 1 calc R . C28 C 0.4098(6) 0.5925(5) 0.6758(6) 0.054(2) Uani 1 d . . H28 H 0.4890 0.5945 0.7455 0.065 Uiso 1 calc R . C29 C 0.3155(7) 0.5529(5) 0.6927(6) 0.060(2) Uani 1 d . . H29 H 0.3307 0.5266 0.7724 0.072 Uiso 1 calc R . C30 C 0.1963(7) 0.5523(6) 0.5892(7) 0.060(2) Uani 1 d . . H30 H 0.1306 0.5264 0.5992 0.072 Uiso 1 calc R . C31 C 0.1763(6) 0.5909(5) 0.4705(6) 0.0491(15) Uani 1 d . . H31 H 0.0970 0.5896 0.4010 0.059 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 Mo1 0.0284(3) 0.0308(3) 0.0357(3) 0.0009(2) 0.0114(2) -0.0088(2) Fe1 0.0359(4) 0.0364(4) 0.0327(4) 0.0010(3) 0.0115(3) -0.0149(3) Fe2 0.0333(4) 0.0348(4) 0.0322(4) 0.0028(3) 0.0114(3) -0.0117(3) P1 0.0279(7) 0.0338(7) 0.0384(7) 0.0030(6) 0.0101(6) -0.0104(5) C1 0.050(4) 0.041(3) 0.033(3) 0.004(2) 0.012(3) -0.017(3) O1 0.046(3) 0.087(4) 0.074(3) 0.012(3) 0.025(2) -0.018(2) C2 0.040(3) 0.048(3) 0.048(3) 0.008(3) 0.018(3) -0.016(3) O2 0.066(3) 0.083(3) 0.047(3) 0.026(2) 0.017(2) -0.021(3) C3 0.045(3) 0.045(4) 0.046(3) -0.003(3) 0.010(3) -0.017(3) O3 0.098(4) 0.039(3) 0.092(4) 0.012(3) 0.014(3) -0.017(3) C4 0.043(3) 0.037(3) 0.037(3) 0.004(2) 0.016(3) -0.013(2) O4 0.054(3) 0.060(3) 0.064(3) 0.009(2) 0.031(2) 0.000(2) C5 0.034(3) 0.045(3) 0.048(3) 0.011(3) 0.013(3) -0.007(2) O5 0.038(2) 0.067(3) 0.049(3) 0.019(2) 0.005(2) -0.002(2) C6 0.060(4) 0.056(4) 0.041(4) -0.003(3) 0.024(3) -0.026(3) O6 0.099(4) 0.124(5) 0.040(3) -0.013(3) 0.027(3) -0.067(4) C7 0.062(4) 0.051(4) 0.045(3) -0.003(3) 0.023(3) -0.014(3) C8 0.064(4) 0.054(4) 0.080(5) -0.013(4) 0.053(4) -0.019(3) C9 0.035(3) 0.075(5) 0.068(5) -0.024(4) 0.020(3) 0.004(3) C10 0.073(5) 0.038(3) 0.055(4) -0.001(3) 0.025(4) -0.001(3) C11 0.053(4) 0.037(3) 0.068(4) -0.014(3) 0.031(3) -0.014(3) C12 0.033(3) 0.035(3) 0.049(3) 0.003(2) 0.012(2) -0.011(2) C13 0.039(3) 0.052(3) 0.046(3) 0.004(3) 0.012(3) -0.012(3) C14 0.054(4) 0.070(4) 0.042(4) 0.008(3) 0.000(3) -0.021(3) C15 0.038(4) 0.055(4) 0.063(4) 0.017(3) -0.007(3) -0.007(3) C16 0.032(3) 0.067(5) 0.071(5) 0.007(4) 0.012(3) 0.004(3) C17 0.035(3) 0.060(4) 0.046(3) -0.002(3) 0.011(3) -0.007(3) C18 0.037(3) 0.041(3) 0.039(3) -0.003(2) 0.018(2) -0.013(2) C19 0.034(3) 0.042(3) 0.067(4) 0.017(3) 0.010(3) -0.013(3) C20 0.058(4) 0.049(4) 0.067(4) 0.019(3) 0.015(3) -0.005(3) C21 0.075(5) 0.047(4) 0.060(4) 0.012(3) 0.024(4) -0.028(3) C22 0.064(4) 0.061(4) 0.063(4) 0.008(3) 0.019(4) -0.039(4) C23 0.047(3) 0.060(4) 0.042(3) 0.008(3) 0.012(3) -0.028(3) C24 0.033(3) 0.030(3) 0.039(3) 0.001(2) 0.009(2) -0.010(2) C25 0.031(3) 0.031(3) 0.033(3) 0.003(2) 0.007(2) -0.009(2) C26 0.045(3) 0.036(3) 0.032(3) 0.004(2) 0.012(2) -0.010(2) C27 0.042(3) 0.059(4) 0.044(3) 0.007(3) 0.012(3) -0.017(3) C28 0.047(4) 0.066(4) 0.035(3) 0.010(3) 0.005(3) 0.003(3) C29 0.068(5) 0.064(4) 0.046(4) 0.024(3) 0.018(3) 0.002(4) C30 0.066(4) 0.074(5) 0.052(4) 0.019(3) 0.025(3) -0.019(4) C31 0.046(3) 0.062(4) 0.044(3) 0.013(3) 0.016(3) -0.014(3) _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 C5 1.960(6) . ? Mo1 C25 2.087(5) . ? Mo1 C24 2.294(6) . ? Mo1 C10 2.334(6) . ? Mo1 C9 2.346(6) . ? Mo1 C11 2.352(6) . ? Mo1 C8 2.355(6) . ? Mo1 C7 2.370(6) . ? Mo1 P1 2.4260(14) . ? Mo1 Fe2 2.6246(10) . ? Mo1 Fe1 2.7773(11) . ? Fe1 C1 1.778(6) . ? Fe1 C3 1.789(6) . ? Fe1 C6 1.800(6) . ? Fe1 C25 1.978(5) . ? Fe1 C24 2.025(6) . ? Fe1 Fe2 2.5684(11) . ? Fe2 C4 1.771(6) . ? Fe2 C2 1.780(6) . ? Fe2 C24 2.045(5) . ? Fe2 P1 2.179(2) . ? Fe2 C5 2.394(6) . ? P1 C18 1.818(5) . ? P1 C12 1.831(6) . ? C1 O1 1.149(7) . ? C2 O2 1.139(7) . ? C3 O3 1.139(7) . ? C4 O4 1.141(7) . ? C5 O5 1.178(7) . ? C6 O6 1.147(7) . ? C7 C8 1.384(9) . ? C7 C11 1.406(9) . ? C8 C9 1.389(10) . ? C9 C10 1.422(10) . ? C10 C11 1.406(9) . ? C12 C13 1.386(8) . ? C12 C17 1.389(8) . ? C13 C14 1.396(8) . ? C14 C15 1.377(9) . ? C15 C16 1.377(9) . ? C16 C17 1.382(8) . ? C18 C19 1.384(8) . ? C18 C23 1.404(7) . ? C19 C20 1.391(8) . ? C20 C21 1.368(9) . ? C21 C22 1.382(9) . ? C22 C23 1.373(8) . ? C24 C25 1.414(7) . ? C25 C26 1.476(7) . ? C26 C27 1.380(8) . ? C26 C31 1.382(8) . ? C27 C28 1.380(8) . ? C28 C29 1.366(9) . ? C29 C30 1.390(9) . ? C30 C31 1.390(8) . ? 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 Mo1 C25 108.9(2) . . ? C5 Mo1 C24 97.8(2) . . ? C25 Mo1 C24 37.3(2) . . ? C5 Mo1 C10 88.7(2) . . ? C25 Mo1 C10 143.8(2) . . ? C24 Mo1 C10 172.2(2) . . ? C5 Mo1 C9 83.8(2) . . ? C25 Mo1 C9 113.3(3) . . ? C24 Mo1 C9 149.4(2) . . ? C10 Mo1 C9 35.4(2) . . ? C5 Mo1 C11 122.3(2) . . ? C25 Mo1 C11 124.4(2) . . ? C24 Mo1 C11 137.7(2) . . ? C10 Mo1 C11 34.9(2) . . ? C9 Mo1 C11 57.6(2) . . ? C5 Mo1 C8 112.6(3) . . ? C25 Mo1 C8 85.8(2) . . ? C24 Mo1 C8 122.4(2) . . ? C10 Mo1 C8 58.0(2) . . ? C9 Mo1 C8 34.4(3) . . ? C11 Mo1 C8 57.0(2) . . ? C5 Mo1 C7 141.0(2) . . ? C25 Mo1 C7 91.3(2) . . ? C24 Mo1 C7 117.2(2) . . ? C10 Mo1 C7 58.3(2) . . ? C9 Mo1 C7 57.4(2) . . ? C11 Mo1 C7 34.6(2) . . ? C8 Mo1 C7 34.1(2) . . ? C5 Mo1 P1 92.8(2) . . ? C25 Mo1 P1 108.83(15) . . ? C24 Mo1 P1 74.12(14) . . ? C10 Mo1 P1 101.4(2) . . ? C9 Mo1 P1 136.4(2) . . ? C11 Mo1 P1 89.7(2) . . ? C8 Mo1 P1 145.2(2) . . ? C7 Mo1 P1 112.2(2) . . ? C5 Mo1 Fe2 60.9(2) . . ? C25 Mo1 Fe2 82.46(14) . . ? C24 Mo1 Fe2 48.57(14) . . ? C10 Mo1 Fe2 133.2(2) . . ? C9 Mo1 Fe2 144.7(2) . . ? C11 Mo1 Fe2 139.7(2) . . ? C8 Mo1 Fe2 163.3(2) . . ? C7 Mo1 Fe2 157.4(2) . . ? P1 Mo1 Fe2 50.93(4) . . ? C5 Mo1 Fe1 63.9(2) . . ? C25 Mo1 Fe1 45.29(14) . . ? C24 Mo1 Fe1 45.84(14) . . ? C10 Mo1 Fe1 141.9(2) . . ? C9 Mo1 Fe1 111.3(2) . . ? C11 Mo1 Fe1 163.4(2) . . ? C8 Mo1 Fe1 106.7(2) . . ? C7 Mo1 Fe1 130.1(2) . . ? P1 Mo1 Fe1 105.75(4) . . ? Fe2 Mo1 Fe1 56.69(3) . . ? C1 Fe1 C3 94.8(3) . . ? C1 Fe1 C6 100.0(3) . . ? C3 Fe1 C6 95.5(3) . . ? C1 Fe1 C25 100.4(2) . . ? C3 Fe1 C25 94.3(2) . . ? C6 Fe1 C25 156.4(2) . . ? C1 Fe1 C24 141.0(2) . . ? C3 Fe1 C24 95.8(2) . . ? C6 Fe1 C24 116.1(2) . . ? C25 Fe1 C24 41.4(2) . . ? C1 Fe1 Fe2 140.8(2) . . ? C3 Fe1 Fe2 123.5(2) . . ? C6 Fe1 Fe2 70.7(2) . . ? C25 Fe1 Fe2 86.03(15) . . ? C24 Fe1 Fe2 51.2(2) . . ? C1 Fe1 Mo1 97.2(2) . . ? C3 Fe1 Mo1 142.5(2) . . ? C6 Fe1 Mo1 117.0(2) . . ? C25 Fe1 Mo1 48.56(15) . . ? C24 Fe1 Mo1 54.4(2) . . ? Fe2 Fe1 Mo1 58.65(3) . . ? C4 Fe2 C2 89.8(3) . . ? C4 Fe2 C24 96.5(2) . . ? C2 Fe2 C24 169.1(2) . . ? C4 Fe2 P1 101.4(2) . . ? C2 Fe2 P1 102.9(2) . . ? C24 Fe2 P1 84.67(15) . . ? C4 Fe2 C5 167.3(2) . . ? C2 Fe2 C5 80.1(2) . . ? C24 Fe2 C5 92.4(2) . . ? P1 Fe2 C5 88.44(15) . . ? C4 Fe2 Fe1 116.5(2) . . ? C2 Fe2 Fe1 118.6(2) . . ? C24 Fe2 Fe1 50.5(2) . . ? P1 Fe2 Fe1 121.89(5) . . ? C5 Fe2 Fe1 63.11(14) . . ? C4 Fe2 Mo1 146.8(2) . . ? C2 Fe2 Mo1 119.7(2) . . ? C24 Fe2 Mo1 57.2(2) . . ? P1 Fe2 Mo1 59.81(4) . . ? C5 Fe2 Mo1 45.70(14) . . ? Fe1 Fe2 Mo1 64.65(3) . . ? C18 P1 C12 106.0(2) . . ? C18 P1 Fe2 120.8(2) . . ? C12 P1 Fe2 117.0(2) . . ? C18 P1 Mo1 124.5(2) . . ? C12 P1 Mo1 116.4(2) . . ? Fe2 P1 Mo1 69.25(4) . . ? O1 C1 Fe1 178.0(5) . . ? O2 C2 Fe2 178.0(5) . . ? O3 C3 Fe1 177.3(5) . . ? O4 C4 Fe2 174.4(5) . . ? O5 C5 Mo1 159.9(5) . . ? O5 C5 Fe2 124.2(4) . . ? Mo1 C5 Fe2 73.4(2) . . ? O6 C6 Fe1 166.9(5) . . ? C8 C7 C11 107.2(6) . . ? C8 C7 Mo1 72.4(4) . . ? C11 C7 Mo1 72.0(4) . . ? C7 C8 C9 109.4(6) . . ? C7 C8 Mo1 73.5(4) . . ? C9 C8 Mo1 72.5(4) . . ? C8 C9 C10 108.0(6) . . ? C8 C9 Mo1 73.2(4) . . ? C10 C9 Mo1 71.8(4) . . ? C11 C10 C9 106.3(6) . . ? C11 C10 Mo1 73.3(4) . . ? C9 C10 Mo1 72.8(4) . . ? C7 C11 C10 109.0(6) . . ? C7 C11 Mo1 73.4(3) . . ? C10 C11 Mo1 71.8(4) . . ? C13 C12 C17 118.0(5) . . ? C13 C12 P1 120.4(4) . . ? C17 C12 P1 121.5(5) . . ? C12 C13 C14 121.2(6) . . ? C15 C14 C13 119.5(6) . . ? C16 C15 C14 119.8(6) . . ? C15 C16 C17 120.6(6) . . ? C16 C17 C12 120.9(6) . . ? C19 C18 C23 118.4(5) . . ? C19 C18 P1 118.7(4) . . ? C23 C18 P1 122.9(4) . . ? C18 C19 C20 120.3(6) . . ? C21 C20 C19 120.7(6) . . ? C20 C21 C22 119.4(6) . . ? C23 C22 C21 120.7(6) . . ? C22 C23 C18 120.4(6) . . ? C25 C24 Fe1 67.6(3) . . ? C25 C24 Fe2 128.8(4) . . ? Fe1 C24 Fe2 78.3(2) . . ? C25 C24 Mo1 63.4(3) . . ? Fe1 C24 Mo1 79.8(2) . . ? Fe2 C24 Mo1 74.2(2) . . ? C24 C25 C26 128.9(5) . . ? C24 C25 Fe1 71.1(3) . . ? C26 C25 Fe1 135.0(4) . . ? C24 C25 Mo1 79.3(3) . . ? C26 C25 Mo1 132.7(4) . . ? Fe1 C25 Mo1 86.2(2) . . ? C27 C26 C31 117.9(5) . . ? C27 C26 C25 120.9(5) . . ? C31 C26 C25 121.1(5) . . ? C28 C27 C26 120.9(6) . . ? C29 C28 C27 121.1(6) . . ? C28 C29 C30 119.0(6) . . ? C29 C30 C31 119.5(6) . . ? C26 C31 C30 121.5(6) . . ? _refine_diff_density_max 0.624 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.089 data_mm9611 _database_code_CSD 175752 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H25 Fe Mo2 O5 P' _chemical_formula_sum 'C35 H25 Fe Mo2 O5 P' _chemical_formula_weight 804.25 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' 'Mo' 'Mo' -1.6832 0.6857 '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' '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.505(4) _cell_length_b 19.905(5) _cell_length_c 9.282(2) _cell_angle_alpha 97.65(2) _cell_angle_beta 112.72(2) _cell_angle_gamma 85.76(3) _cell_volume 1773.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 25.0 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 1.182 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.839 _exptl_absorpt_correction_T_max 0.998 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method 'omega-2theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6762 _diffrn_reflns_av_R_equivalents 0.0875 _diffrn_reflns_av_sigmaI/netI 0.0871 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.70 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4605 _reflns_number_gt 3231 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'standard MSC/Rigaku supplied software' _computing_cell_refinement 'standard MSC/Rigaku supplied software' _computing_data_reduction 'standard MSC/Rigaku supplied software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP' _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^)+(0.0661P)^2^+24.4670P] 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 4605 _refine_ls_number_parameters 409 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1076 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.1991 _refine_ls_wR_factor_gt 0.1695 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.908 _refine_ls_shift/su_mean 0.007 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 0.76663(11) 0.23050(6) 0.80937(13) 0.0379(4) Uani 1 1 d . . . Mo2 Mo 0.49396(10) 0.27624(6) 0.82308(12) 0.0324(3) Uani 1 1 d . . . Fe1 Fe 0.52206(18) 0.24723(9) 0.5400(2) 0.0373(5) Uani 1 1 d . . . P1 P 0.7050(3) 0.34082(17) 0.9054(4) 0.0338(8) Uani 1 1 d . . . O1 O 0.7988(13) 0.1737(7) 1.1192(15) 0.089(4) Uani 1 1 d . . . C1 C 0.7824(14) 0.1981(8) 1.0080(18) 0.053(4) Uani 1 1 d . . . O2 O 0.6541(12) 0.3588(6) 0.4752(12) 0.066(3) Uani 1 1 d . . . C2 C 0.6063(15) 0.3162(8) 0.5089(15) 0.050(4) Uani 1 1 d . . . O3 O 0.6143(13) 0.1426(6) 0.3442(13) 0.081(4) Uani 1 1 d . . . C3 C 0.5777(16) 0.1848(8) 0.4201(17) 0.055(4) Uani 1 1 d . . . O4 O 0.2516(13) 0.2635(7) 0.2832(14) 0.087(4) Uani 1 1 d . . . C4 C 0.3563(16) 0.2574(8) 0.3852(17) 0.051(4) Uani 1 1 d . . . O5 O 0.3055(11) 0.3735(6) 0.5921(12) 0.069(3) Uani 1 1 d . . . C5 C 0.3858(14) 0.3351(7) 0.6656(17) 0.046(3) Uani 1 1 d . . . C6 C 0.5850(13) 0.1854(6) 0.7181(14) 0.038(3) Uani 1 1 d . . . C7 C 0.4485(12) 0.1830(6) 0.6490(14) 0.034(3) Uani 1 1 d . . . C8 C 0.3376(13) 0.1336(7) 0.5776(14) 0.042(3) Uani 1 1 d . . . C9 C 0.3685(16) 0.0659(8) 0.560(2) 0.072(5) Uani 1 1 d . . . H9A H 0.4602 0.0509 0.5969 0.087 Uiso 1 1 calc R . . C10 C 0.266(2) 0.0202(10) 0.489(3) 0.120(9) Uani 1 1 d . . . H10A H 0.2901 -0.0256 0.4773 0.143 Uiso 1 1 calc R . . C11 C 0.129(2) 0.0396(10) 0.433(3) 0.101(7) Uani 1 1 d . . . H11A H 0.0607 0.0076 0.3906 0.121 Uiso 1 1 calc R . . C12 C 0.0974(15) 0.1062(10) 0.4423(19) 0.070(5) Uani 1 1 d . . . H12A H 0.0055 0.1207 0.3996 0.084 Uiso 1 1 calc R . . C13 C 0.1987(15) 0.1533(7) 0.5138(17) 0.054(4) Uani 1 1 d . . . H13A H 0.1742 0.1991 0.5198 0.065 Uiso 1 1 calc R . . C14 C 0.4660(18) 0.2226(9) 1.0171(19) 0.062(4) Uani 1 1 d . . . H14A H 0.5041 0.1778 1.0473 0.075 Uiso 1 1 calc R . . C15 C 0.3350(19) 0.2358(9) 0.9059(18) 0.065(5) Uani 1 1 d . . . H15A H 0.2661 0.2015 0.8454 0.078 Uiso 1 1 calc R . . C16 C 0.3139(18) 0.3025(10) 0.906(2) 0.077(5) Uani 1 1 d . . . H16A H 0.2268 0.3253 0.8472 0.092 Uiso 1 1 calc R . . C17 C 0.437(2) 0.3358(10) 1.025(2) 0.085(7) Uani 1 1 d . . . H17A H 0.4482 0.3842 1.0622 0.102 Uiso 1 1 calc R . . C18 C 0.528(2) 0.2830(10) 1.0847(18) 0.068(5) Uani 1 1 d . . . H18A H 0.6177 0.2883 1.1723 0.082 Uiso 1 1 calc R . . C19 C 0.988(3) 0.185(2) 0.889(5) 0.160(18) Uani 1 1 d . . . H19A H 1.0330 0.1576 0.9758 0.192 Uiso 1 1 calc R . . C20 C 0.914(4) 0.1610(12) 0.724(7) 0.17(2) Uani 1 1 d . . . H20A H 0.8988 0.1135 0.6792 0.204 Uiso 1 1 calc R . . C21 C 0.8929(19) 0.213(2) 0.645(3) 0.129(12) Uani 1 1 d . . . H21A H 0.8525 0.2109 0.5305 0.154 Uiso 1 1 calc R . . C22 C 0.9388(19) 0.2678(10) 0.741(3) 0.074(5) Uani 1 1 d . . . H22A H 0.9388 0.3126 0.7083 0.089 Uiso 1 1 calc R . . C23 C 1.0007(17) 0.2527(12) 0.891(3) 0.078(5) Uani 1 1 d . . . H23A H 1.0542 0.2838 0.9821 0.093 Uiso 1 1 calc R . . C24 C 0.7908(12) 0.3723(6) 1.1169(14) 0.036(3) Uani 1 1 d . . . C25 C 0.7417(14) 0.4322(7) 1.1743(15) 0.044(3) Uani 1 1 d . . . H25A H 0.6686 0.4567 1.1080 0.053 Uiso 1 1 calc R . . C26 C 0.8065(17) 0.4554(8) 1.3380(17) 0.058(4) Uani 1 1 d . . . H26A H 0.7731 0.4947 1.3792 0.070 Uiso 1 1 calc R . . C27 C 0.9155(17) 0.4212(9) 1.4337(18) 0.063(4) Uani 1 1 d . . . H27A H 0.9572 0.4374 1.5395 0.076 Uiso 1 1 calc R . . C28 C 0.9650(15) 0.3624(8) 1.3749(16) 0.056(4) Uani 1 1 d . . . H28A H 1.0398 0.3386 1.4406 0.067 Uiso 1 1 calc R . . C29 C 0.9026(13) 0.3391(8) 1.2177(15) 0.050(4) Uani 1 1 d . . . H29A H 0.9372 0.2997 1.1784 0.060 Uiso 1 1 calc R . . C30 C 0.7164(12) 0.4194(6) 0.8261(14) 0.045(3) Uani 1 1 d G . . C31 C 0.6024(13) 0.4610(6) 0.7569(17) 0.052(4) Uani 1 1 d G . . H31A H 0.5149 0.4490 0.7455 0.062 Uiso 1 1 calc R . . C32 C 0.620(2) 0.5203(8) 0.705(2) 0.080(6) Uani 1 1 d G . . H32A H 0.5437 0.5475 0.6549 0.096 Uiso 1 1 calc R . . C33 C 0.753(3) 0.5394(9) 0.729(2) 0.086(7) Uani 1 1 d G . . H33A H 0.7641 0.5796 0.6948 0.103 Uiso 1 1 calc R . . C34 C 0.865(2) 0.5011(9) 0.800(2) 0.070(5) Uani 1 1 d G . . H34A H 0.9522 0.5145 0.8146 0.084 Uiso 1 1 calc R . . C35 C 0.8477(16) 0.4423(8) 0.8496(17) 0.060(4) Uani 1 1 d G . . H35A H 0.9254 0.4163 0.9008 0.072 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 0.0251(6) 0.0445(7) 0.0409(7) -0.0015(5) 0.0118(5) 0.0031(5) Mo2 0.0254(6) 0.0411(7) 0.0314(6) -0.0005(5) 0.0127(5) -0.0026(5) Fe1 0.0367(11) 0.0458(11) 0.0282(10) 0.0031(8) 0.0110(8) -0.0038(8) P1 0.0269(17) 0.043(2) 0.0295(17) 0.0017(14) 0.0092(14) -0.0030(14) O1 0.083(9) 0.106(10) 0.069(8) 0.049(8) 0.010(7) 0.011(7) C1 0.039(8) 0.062(10) 0.049(9) 0.011(8) 0.003(7) -0.006(7) O2 0.087(8) 0.065(7) 0.056(7) 0.008(5) 0.036(6) -0.023(6) C2 0.052(9) 0.065(10) 0.035(8) 0.004(7) 0.019(7) -0.005(8) O3 0.115(10) 0.066(8) 0.064(7) -0.007(6) 0.043(7) 0.023(7) C3 0.065(10) 0.049(9) 0.049(9) 0.011(7) 0.021(8) 0.004(8) O4 0.065(8) 0.109(10) 0.059(7) 0.012(7) -0.006(7) 0.007(7) C4 0.049(9) 0.061(10) 0.039(8) 0.007(7) 0.010(8) -0.003(7) O5 0.053(6) 0.071(7) 0.062(7) 0.016(6) -0.001(5) 0.020(6) C5 0.038(8) 0.037(8) 0.053(9) -0.003(7) 0.008(7) -0.003(7) C6 0.040(8) 0.042(8) 0.032(7) 0.008(6) 0.012(6) -0.002(6) C7 0.035(8) 0.035(7) 0.032(7) 0.008(6) 0.011(6) -0.003(6) C8 0.041(8) 0.054(9) 0.032(7) -0.004(6) 0.016(6) -0.014(7) C9 0.051(10) 0.038(9) 0.102(14) -0.009(9) 0.005(9) -0.005(8) C10 0.081(16) 0.062(13) 0.18(2) 0.004(14) 0.011(16) -0.018(12) C11 0.082(15) 0.065(14) 0.137(19) -0.012(13) 0.023(14) -0.039(12) C12 0.036(9) 0.101(15) 0.068(11) -0.005(10) 0.017(8) -0.018(9) C13 0.050(9) 0.042(8) 0.061(10) -0.009(7) 0.015(8) -0.003(7) C14 0.077(12) 0.070(12) 0.059(10) 0.021(9) 0.043(10) -0.001(9) C15 0.083(13) 0.071(12) 0.051(10) -0.022(8) 0.039(10) -0.044(10) C16 0.060(11) 0.084(14) 0.114(16) 0.019(12) 0.064(12) 0.018(10) C17 0.110(16) 0.080(13) 0.108(15) -0.040(12) 0.097(14) -0.038(13) C18 0.087(13) 0.087(14) 0.040(9) -0.020(9) 0.039(9) -0.031(12) C19 0.078(18) 0.25(4) 0.22(3) 0.18(3) 0.11(2) 0.12(2) C20 0.15(3) 0.042(13) 0.40(7) 0.01(2) 0.21(4) 0.022(16) C21 0.044(11) 0.24(3) 0.088(15) -0.09(2) 0.043(11) -0.012(17) C22 0.069(12) 0.089(14) 0.095(15) 0.009(12) 0.065(12) 0.005(10) C23 0.041(10) 0.090(15) 0.090(15) -0.014(12) 0.018(10) -0.008(10) C24 0.031(7) 0.040(8) 0.037(7) 0.001(6) 0.012(6) -0.011(6) C25 0.044(8) 0.054(9) 0.033(7) -0.006(6) 0.016(6) -0.004(7) C26 0.076(11) 0.055(10) 0.051(10) -0.016(8) 0.037(9) -0.022(9) C27 0.060(11) 0.087(13) 0.036(9) 0.002(9) 0.008(8) -0.034(10) C28 0.043(9) 0.069(11) 0.041(9) 0.008(8) -0.003(7) -0.016(8) C29 0.040(8) 0.066(10) 0.035(8) 0.001(7) 0.005(7) -0.004(7) C30 0.058(9) 0.044(8) 0.028(7) -0.004(6) 0.012(7) -0.012(7) C31 0.053(9) 0.024(7) 0.060(9) -0.002(7) 0.003(8) 0.001(6) C32 0.120(17) 0.034(9) 0.062(11) 0.003(8) 0.011(11) 0.011(10) C33 0.17(2) 0.046(11) 0.055(11) -0.005(9) 0.048(13) -0.045(13) C34 0.089(13) 0.062(11) 0.070(11) 0.018(9) 0.037(10) -0.018(10) C35 0.062(10) 0.072(11) 0.054(9) 0.003(8) 0.029(8) -0.013(8) _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 C1 1.977(16) . ? Mo1 C6 1.992(13) . ? Mo1 C20 2.30(2) . ? Mo1 C19 2.300(19) . ? Mo1 C22 2.329(15) . ? Mo1 C23 2.335(16) . ? Mo1 C21 2.355(18) . ? Mo1 P1 2.398(4) . ? Mo1 Fe1 2.846(2) . ? Mo1 Mo2 2.9858(18) . ? Mo2 C5 1.943(15) . ? Mo2 C7 2.240(12) . ? Mo2 C6 2.265(13) . ? Mo2 C18 2.300(15) . ? Mo2 C16 2.304(14) . ? Mo2 C15 2.321(14) . ? Mo2 C17 2.332(15) . ? Mo2 C14 2.332(14) . ? Mo2 P1 2.450(3) . ? Mo2 Fe1 2.738(2) . ? Fe1 C3 1.775(16) . ? Fe1 C4 1.797(15) . ? Fe1 C2 1.798(16) . ? Fe1 C6 2.065(12) . ? Fe1 C7 2.086(12) . ? P1 C30 1.846(13) . ? P1 C24 1.857(12) . ? O1 C1 1.146(17) . ? O2 C2 1.151(16) . ? O3 C3 1.164(17) . ? O4 C4 1.152(16) . ? O5 C5 1.167(15) . ? C6 C7 1.327(17) . ? C7 C8 1.471(17) . ? C8 C9 1.365(19) . ? C8 C13 1.393(19) . ? C9 C10 1.36(2) . ? C10 C11 1.37(3) . ? C11 C12 1.34(2) . ? C12 C13 1.37(2) . ? C14 C18 1.37(2) . ? C14 C15 1.40(2) . ? C15 C16 1.33(2) . ? C16 C17 1.47(3) . ? C17 C18 1.39(3) . ? C19 C23 1.36(4) . ? C19 C20 1.45(4) . ? C20 C21 1.30(4) . ? C21 C22 1.31(3) . ? C22 C23 1.35(3) . ? C24 C29 1.375(18) . ? C24 C25 1.387(18) . ? C25 C26 1.430(19) . ? C26 C27 1.35(2) . ? C27 C28 1.38(2) . ? C28 C29 1.378(19) . ? C30 C31 1.3900 . ? C30 C35 1.411(19) . ? C31 C32 1.38(2) . ? C32 C33 1.40(3) . ? C33 C34 1.34(3) . ? C34 C35 1.36(2) . ? 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 C1 Mo1 C6 85.0(5) . . ? C1 Mo1 C20 105.1(13) . . ? C6 Mo1 C20 106.2(10) . . ? C1 Mo1 C19 80.0(8) . . ? C6 Mo1 C19 130.6(14) . . ? C20 Mo1 C19 36.9(11) . . ? C1 Mo1 C22 129.1(7) . . ? C6 Mo1 C22 142.3(7) . . ? C20 Mo1 C22 55.1(8) . . ? C19 Mo1 C22 56.4(9) . . ? C1 Mo1 C23 95.5(7) . . ? C6 Mo1 C23 163.3(6) . . ? C20 Mo1 C23 57.5(10) . . ? C19 Mo1 C23 34.1(10) . . ? C22 Mo1 C23 33.6(7) . . ? C1 Mo1 C21 135.5(10) . . ? C6 Mo1 C21 113.6(7) . . ? C20 Mo1 C21 32.5(10) . . ? C19 Mo1 C21 56.9(10) . . ? C22 Mo1 C21 32.4(8) . . ? C23 Mo1 C21 55.4(7) . . ? C1 Mo1 P1 88.6(5) . . ? C6 Mo1 P1 101.6(4) . . ? C20 Mo1 P1 149.8(7) . . ? C19 Mo1 P1 124.6(14) . . ? C22 Mo1 P1 95.4(5) . . ? C23 Mo1 P1 95.1(5) . . ? C21 Mo1 P1 123.3(10) . . ? C1 Mo1 Fe1 127.6(4) . . ? C6 Mo1 Fe1 46.5(3) . . ? C20 Mo1 Fe1 106.7(14) . . ? C19 Mo1 Fe1 143.2(11) . . ? C22 Mo1 Fe1 103.3(6) . . ? C23 Mo1 Fe1 136.8(6) . . ? C21 Mo1 Fe1 89.1(6) . . ? P1 Mo1 Fe1 84.25(9) . . ? C1 Mo1 Mo2 78.9(4) . . ? C6 Mo1 Mo2 49.3(4) . . ? C20 Mo1 Mo2 155.3(10) . . ? C19 Mo1 Mo2 158.7(7) . . ? C22 Mo1 Mo2 140.2(5) . . ? C23 Mo1 Mo2 147.2(5) . . ? C21 Mo1 Mo2 144.2(7) . . ? P1 Mo1 Mo2 52.77(8) . . ? Fe1 Mo1 Mo2 55.94(5) . . ? C5 Mo2 C7 93.2(5) . . ? C5 Mo2 C6 111.8(5) . . ? C7 Mo2 C6 34.3(4) . . ? C5 Mo2 C18 129.8(7) . . ? C7 Mo2 C18 126.9(6) . . ? C6 Mo2 C18 118.2(6) . . ? C5 Mo2 C16 81.2(6) . . ? C7 Mo2 C16 110.4(6) . . ? C6 Mo2 C16 139.3(6) . . ? C18 Mo2 C16 58.9(7) . . ? C5 Mo2 C15 104.5(7) . . ? C7 Mo2 C15 85.3(5) . . ? C6 Mo2 C15 107.2(5) . . ? C18 Mo2 C15 58.0(6) . . ? C16 Mo2 C15 33.4(6) . . ? C5 Mo2 C17 95.0(8) . . ? C7 Mo2 C17 143.7(5) . . ? C6 Mo2 C17 152.6(7) . . ? C18 Mo2 C17 34.8(6) . . ? C16 Mo2 C17 37.0(6) . . ? C15 Mo2 C17 58.4(6) . . ? C5 Mo2 C14 137.7(6) . . ? C7 Mo2 C14 93.8(5) . . ? C6 Mo2 C14 96.8(5) . . ? C18 Mo2 C14 34.3(6) . . ? C16 Mo2 C14 57.3(6) . . ? C15 Mo2 C14 34.9(6) . . ? C17 Mo2 C14 57.6(7) . . ? C5 Mo2 P1 93.9(4) . . ? C7 Mo2 P1 123.6(3) . . ? C6 Mo2 P1 92.6(3) . . ? C18 Mo2 P1 87.3(4) . . ? C16 Mo2 P1 126.0(5) . . ? C15 Mo2 P1 145.0(4) . . ? C17 Mo2 P1 91.0(4) . . ? C14 Mo2 P1 116.0(5) . . ? C5 Mo2 Fe1 65.4(4) . . ? C7 Mo2 Fe1 48.3(3) . . ? C6 Mo2 Fe1 47.6(3) . . ? C18 Mo2 Fe1 163.7(5) . . ? C16 Mo2 Fe1 136.2(5) . . ? C15 Mo2 Fe1 129.0(4) . . ? C17 Mo2 Fe1 159.8(6) . . ? C14 Mo2 Fe1 140.9(4) . . ? P1 Mo2 Fe1 85.65(9) . . ? C5 Mo2 Mo1 114.5(4) . . ? C7 Mo2 Mo1 75.3(3) . . ? C6 Mo2 Mo1 41.8(3) . . ? C18 Mo2 Mo1 105.0(5) . . ? C16 Mo2 Mo1 163.4(5) . . ? C15 Mo2 Mo1 136.9(5) . . ? C17 Mo2 Mo1 131.3(6) . . ? C14 Mo2 Mo1 107.6(4) . . ? P1 Mo2 Mo1 51.20(8) . . ? Fe1 Mo2 Mo1 59.44(5) . . ? C3 Fe1 C4 92.4(7) . . ? C3 Fe1 C2 95.1(7) . . ? C4 Fe1 C2 97.9(6) . . ? C3 Fe1 C6 90.6(6) . . ? C4 Fe1 C6 130.5(6) . . ? C2 Fe1 C6 131.0(6) . . ? C3 Fe1 C7 98.7(6) . . ? C4 Fe1 C7 93.6(6) . . ? C2 Fe1 C7 161.6(5) . . ? C6 Fe1 C7 37.3(5) . . ? C3 Fe1 Mo2 144.6(5) . . ? C4 Fe1 Mo2 108.7(5) . . ? C2 Fe1 Mo2 109.1(4) . . ? C6 Fe1 Mo2 54.1(4) . . ? C7 Fe1 Mo2 53.3(3) . . ? C3 Fe1 Mo1 92.4(5) . . ? C4 Fe1 Mo1 173.0(5) . . ? C2 Fe1 Mo1 86.7(4) . . ? C6 Fe1 Mo1 44.4(4) . . ? C7 Fe1 Mo1 80.7(3) . . ? Mo2 Fe1 Mo1 64.62(5) . . ? C30 P1 C24 97.2(6) . . ? C30 P1 Mo1 123.6(4) . . ? C24 P1 Mo1 119.5(4) . . ? C30 P1 Mo2 124.2(4) . . ? C24 P1 Mo2 118.1(4) . . ? Mo1 P1 Mo2 76.03(11) . . ? O1 C1 Mo1 173.0(14) . . ? O2 C2 Fe1 174.0(12) . . ? O3 C3 Fe1 178.1(13) . . ? O4 C4 Fe1 178.2(14) . . ? O5 C5 Mo2 165.4(12) . . ? C7 C6 Mo1 155.2(10) . . ? C7 C6 Fe1 72.2(7) . . ? Mo1 C6 Fe1 89.1(5) . . ? C7 C6 Mo2 71.9(8) . . ? Mo1 C6 Mo2 88.9(5) . . ? Fe1 C6 Mo2 78.3(4) . . ? C6 C7 C8 140.6(12) . . ? C6 C7 Fe1 70.5(7) . . ? C8 C7 Fe1 129.0(8) . . ? C6 C7 Mo2 73.9(8) . . ? C8 C7 Mo2 137.3(9) . . ? Fe1 C7 Mo2 78.4(4) . . ? C9 C8 C13 117.0(13) . . ? C9 C8 C7 120.4(12) . . ? C13 C8 C7 122.4(12) . . ? C10 C9 C8 120.7(16) . . ? C9 C10 C11 122.0(19) . . ? C12 C11 C10 118.1(17) . . ? C11 C12 C13 120.8(16) . . ? C12 C13 C8 121.3(14) . . ? C18 C14 C15 108.4(16) . . ? C18 C14 Mo2 71.6(9) . . ? C15 C14 Mo2 72.1(8) . . ? C16 C15 C14 109.1(15) . . ? C16 C15 Mo2 72.6(9) . . ? C14 C15 Mo2 73.0(8) . . ? C15 C16 C17 108.1(17) . . ? C15 C16 Mo2 74.0(9) . . ? C17 C16 Mo2 72.5(8) . . ? C18 C17 C16 104.8(16) . . ? C18 C17 Mo2 71.3(9) . . ? C16 C17 Mo2 70.5(9) . . ? C14 C18 C17 109.5(17) . . ? C14 C18 Mo2 74.2(9) . . ? C17 C18 Mo2 73.8(10) . . ? C23 C19 C20 105(2) . . ? C23 C19 Mo1 74.3(11) . . ? C20 C19 Mo1 71.4(13) . . ? C21 C20 C19 107(3) . . ? C21 C20 Mo1 76.2(13) . . ? C19 C20 Mo1 71.7(14) . . ? C20 C21 C22 110(3) . . ? C20 C21 Mo1 71.3(15) . . ? C22 C21 Mo1 72.7(10) . . ? C21 C22 C23 110(2) . . ? C21 C22 Mo1 74.9(12) . . ? C23 C22 Mo1 73.4(10) . . ? C22 C23 C19 108(2) . . ? C22 C23 Mo1 73.0(10) . . ? C19 C23 Mo1 71.6(12) . . ? C29 C24 C25 119.0(12) . . ? C29 C24 P1 122.4(10) . . ? C25 C24 P1 118.6(10) . . ? C24 C25 C26 118.2(13) . . ? C27 C26 C25 121.1(15) . . ? C26 C27 C28 120.1(14) . . ? C27 C28 C29 119.3(14) . . ? C24 C29 C28 122.2(14) . . ? C31 C30 C35 117.7(13) . . ? C31 C30 P1 123.0(10) . . ? C35 C30 P1 119.0(9) . . ? C30 C31 C32 119.6(15) . . ? C33 C32 C31 119.7(16) . . ? C32 C33 C34 121.6(16) . . ? C35 C34 C33 118.9(17) . . ? C34 C35 C30 122.3(16) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.282 _refine_diff_density_min -1.063 _refine_diff_density_rms 0.164 data_mm9614 _database_code_CSD 175753 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H21 Fe2 O6 P W' _chemical_formula_weight 816.00 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' 'Fe' 'Fe' 0.3463 0.8444 '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' 'W' 'W' -0.8490 6.8722 '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' _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 11.122(3) _cell_length_b 13.160(4) _cell_length_c 10.756(2) _cell_angle_alpha 100.34(3) _cell_angle_beta 111.19(2) _cell_angle_gamma 75.27(3) _cell_volume 1412.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 30 _cell_measurement_theta_max 40 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.918 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 5.174 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.740 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'empirical, from psi scans' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method 'omega/2theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.4% _diffrn_reflns_number 5672 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0735 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5341 _reflns_number_gt 4300 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'standard MSC/Rigaku supplied software' _computing_cell_refinement 'standard MSC/Rigaku supplied software' _computing_data_reduction 'standard MSC/Rigaku supplied software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP' _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^)+(0.0701P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5341 _refine_ls_number_parameters 374 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1205 _refine_ls_wR_factor_gt 0.1097 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.127 _refine_ls_shift/su_mean 0.002 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 W1 W 0.29305(3) 0.17243(2) 0.22458(3) 0.02892(12) Uani 1 1 d . . . Fe1 Fe 0.34290(11) 0.36568(8) 0.36342(10) 0.0308(2) Uani 1 1 d . . . Fe2 Fe 0.19159(10) 0.27021(8) 0.41062(10) 0.0305(2) Uani 1 1 d . . . P1 P 0.10536(19) 0.14643(15) 0.26893(19) 0.0318(4) Uani 1 1 d . . . C1 C 0.5080(8) 0.3475(6) 0.3656(8) 0.0370(17) Uani 1 1 d . . . O1 O 0.6124(6) 0.3351(6) 0.3623(7) 0.0614(18) Uani 1 1 d . . . C2 C 0.2452(8) 0.2172(7) 0.5677(9) 0.0412(18) Uani 1 1 d . . . O2 O 0.2854(7) 0.1828(6) 0.6684(6) 0.0605(18) Uani 1 1 d . . . C3 C 0.3029(9) 0.5045(7) 0.3465(9) 0.045(2) Uani 1 1 d . . . O3 O 0.2730(9) 0.5915(5) 0.3284(8) 0.078(2) Uani 1 1 d . . . C4 C 0.0527(9) 0.3519(6) 0.4465(7) 0.0382(18) Uani 1 1 d . . . O4 O -0.0413(6) 0.3961(5) 0.4680(7) 0.0532(16) Uani 1 1 d . . . C5 C 0.4062(8) 0.1682(6) 0.4140(8) 0.0383(18) Uani 1 1 d . . . O5 O 0.4903(6) 0.1393(5) 0.5116(6) 0.0534(16) Uani 1 1 d . . . C6 C 0.3710(9) 0.3790(8) 0.5409(9) 0.050(2) Uani 1 1 d . . . O6 O 0.4100(8) 0.3976(7) 0.6563(6) 0.078(2) Uani 1 1 d . . . C7 C 0.2944(11) 0.1007(8) 0.0073(9) 0.057(3) Uani 1 1 d . . . H7 H 0.2317 0.1311 -0.0677 0.058(6) Uiso 1 1 calc R . . C8 C 0.2820(10) 0.0203(7) 0.0690(10) 0.053(2) Uani 1 1 d . . . H8 H 0.2111 -0.0131 0.0413 0.058(6) Uiso 1 1 calc R . . C9 C 0.3983(10) -0.0004(7) 0.1817(10) 0.053(2) Uani 1 1 d . . . H9 H 0.4163 -0.0488 0.2425 0.058(6) Uiso 1 1 calc R . . C10 C 0.4794(11) 0.0639(9) 0.1846(11) 0.065(3) Uani 1 1 d . . . H10 H 0.5627 0.0653 0.2473 0.058(6) Uiso 1 1 calc R . . C11 C 0.4163(11) 0.1271(8) 0.0776(11) 0.061(3) Uani 1 1 d . . . H11 H 0.4500 0.1776 0.0574 0.058(6) Uiso 1 1 calc R . . C12 C -0.0571(7) 0.1883(6) 0.1456(8) 0.0334(16) Uani 1 1 d . . . C13 C -0.0705(8) 0.1840(7) 0.0098(8) 0.0417(19) Uani 1 1 d . . . H13 H 0.0026 0.1547 -0.0172 0.058(6) Uiso 1 1 calc R . . C14 C -0.1891(10) 0.2221(8) -0.0842(9) 0.054(2) Uani 1 1 d . . . H14 H -0.1947 0.2199 -0.1730 0.058(6) Uiso 1 1 calc R . . C15 C -0.3013(10) 0.2641(8) -0.0464(10) 0.058(3) Uani 1 1 d . . . H15 H -0.3818 0.2905 -0.1090 0.058(6) Uiso 1 1 calc R . . C16 C -0.2897(9) 0.2652(8) 0.0847(10) 0.056(2) Uani 1 1 d . . . H16 H -0.3643 0.2903 0.1100 0.058(6) Uiso 1 1 calc R . . C17 C -0.1696(9) 0.2301(7) 0.1814(9) 0.048(2) Uani 1 1 d . . . H17 H -0.1644 0.2345 0.2704 0.058(6) Uiso 1 1 calc R . . C18 C 0.0982(8) 0.0265(6) 0.3249(8) 0.0351(17) Uani 1 1 d . . . C19 C -0.0166(9) -0.0119(7) 0.2868(9) 0.047(2) Uani 1 1 d . . . H19 H -0.0944 0.0238 0.2291 0.058(6) Uiso 1 1 calc R . . C20 C -0.0155(10) -0.1032(8) 0.3346(10) 0.057(3) Uani 1 1 d . . . H20 H -0.0932 -0.1278 0.3089 0.058(6) Uiso 1 1 calc R . . C21 C 0.0986(11) -0.1584(8) 0.4194(10) 0.058(3) Uani 1 1 d . . . H21 H 0.0976 -0.2195 0.4508 0.058(6) Uiso 1 1 calc R . . C22 C 0.2139(10) -0.1228(8) 0.4575(10) 0.055(2) Uani 1 1 d . . . H22 H 0.2915 -0.1606 0.5130 0.058(6) Uiso 1 1 calc R . . C23 C 0.2143(9) -0.0289(7) 0.4123(10) 0.047(2) Uani 1 1 d . . . H23 H 0.2916 -0.0035 0.4404 0.058(6) Uiso 1 1 calc R . . C24 C 0.1655(8) 0.3389(6) 0.2433(7) 0.0315(15) Uani 1 1 d D . . H24 H 0.075(4) 0.386(6) 0.213(9) 0.058(6) Uiso 1 1 d D . . C25 C 0.2542(7) 0.3232(6) 0.1720(7) 0.0303(15) Uani 1 1 d . . . C26 C 0.2298(7) 0.3693(6) 0.0450(7) 0.0318(16) Uani 1 1 d . . . C27 C 0.3286(9) 0.4069(7) 0.0282(8) 0.045(2) Uani 1 1 d . . . H27 H 0.4094 0.4045 0.0965 0.058(6) Uiso 1 1 calc R . . C28 C 0.3075(10) 0.4480(8) -0.0896(9) 0.057(2) Uani 1 1 d . . . H28 H 0.3733 0.4748 -0.0989 0.058(6) Uiso 1 1 calc R . . C29 C 0.1895(10) 0.4495(7) -0.1931(9) 0.056(2) Uani 1 1 d . . . H29 H 0.1761 0.4759 -0.2728 0.058(6) Uiso 1 1 calc R . . C30 C 0.0916(9) 0.4116(8) -0.1775(8) 0.053(2) Uani 1 1 d . . . H30 H 0.0118 0.4125 -0.2471 0.058(6) Uiso 1 1 calc R . . C31 C 0.1111(9) 0.3719(7) -0.0589(8) 0.045(2) Uani 1 1 d . . . H31 H 0.0442 0.3470 -0.0492 0.058(6) 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 W1 0.02674(18) 0.02844(16) 0.03196(17) 0.00227(11) 0.00889(12) -0.00805(11) Fe1 0.0333(6) 0.0319(5) 0.0291(5) 0.0017(4) 0.0086(4) -0.0137(4) Fe2 0.0317(6) 0.0325(5) 0.0295(5) 0.0041(4) 0.0098(4) -0.0102(4) P1 0.0294(10) 0.0320(9) 0.0336(9) 0.0056(8) 0.0074(8) -0.0085(8) C1 0.038(5) 0.041(4) 0.034(4) 0.002(3) 0.009(3) -0.016(4) O1 0.039(4) 0.081(5) 0.071(5) 0.011(4) 0.021(3) -0.016(3) C2 0.039(5) 0.042(4) 0.048(5) 0.008(4) 0.018(4) -0.010(4) O2 0.059(4) 0.083(5) 0.044(4) 0.031(3) 0.011(3) -0.014(4) C3 0.047(5) 0.040(5) 0.043(5) 0.002(4) 0.004(4) -0.018(4) O3 0.099(6) 0.038(4) 0.087(6) 0.014(4) 0.013(5) -0.017(4) C4 0.046(5) 0.038(4) 0.031(4) 0.009(3) 0.009(4) -0.012(4) O4 0.050(4) 0.052(4) 0.061(4) 0.006(3) 0.028(3) -0.001(3) C5 0.034(4) 0.035(4) 0.048(5) 0.013(3) 0.013(4) -0.005(3) O5 0.039(3) 0.064(4) 0.045(3) 0.019(3) -0.001(3) -0.003(3) C6 0.054(6) 0.055(5) 0.049(5) 0.004(4) 0.021(4) -0.022(4) O6 0.095(6) 0.128(7) 0.031(3) -0.012(4) 0.025(4) -0.066(5) C7 0.081(7) 0.051(5) 0.035(4) -0.002(4) 0.024(5) -0.005(5) C8 0.067(6) 0.038(5) 0.061(6) -0.010(4) 0.030(5) -0.020(4) C9 0.058(6) 0.039(5) 0.053(5) 0.003(4) 0.019(5) 0.003(4) C10 0.049(6) 0.069(7) 0.065(6) -0.015(5) 0.024(5) 0.000(5) C11 0.070(7) 0.059(6) 0.080(7) -0.024(5) 0.055(6) -0.033(5) C12 0.034(4) 0.029(4) 0.041(4) -0.002(3) 0.015(3) -0.014(3) C13 0.040(5) 0.044(4) 0.043(4) 0.002(4) 0.013(4) -0.015(4) C14 0.052(6) 0.064(6) 0.039(5) 0.018(4) 0.002(4) -0.010(5) C15 0.045(5) 0.049(5) 0.060(6) 0.009(4) -0.004(5) -0.006(4) C16 0.037(5) 0.060(6) 0.058(6) 0.002(5) 0.009(4) -0.002(4) C17 0.044(5) 0.051(5) 0.041(4) 0.006(4) 0.011(4) 0.004(4) C18 0.046(5) 0.029(4) 0.038(4) 0.000(3) 0.024(4) -0.009(3) C19 0.044(5) 0.054(5) 0.047(5) 0.007(4) 0.012(4) -0.018(4) C20 0.057(6) 0.068(6) 0.060(6) 0.008(5) 0.017(5) -0.038(5) C21 0.083(8) 0.046(5) 0.057(6) 0.008(4) 0.029(5) -0.025(5) C22 0.053(6) 0.050(5) 0.066(6) 0.016(5) 0.021(5) -0.011(4) C23 0.041(5) 0.039(4) 0.064(6) 0.015(4) 0.014(4) -0.012(4) C24 0.029(4) 0.031(4) 0.034(4) 0.006(3) 0.005(3) -0.011(3) C25 0.031(4) 0.030(4) 0.030(3) 0.004(3) 0.008(3) -0.010(3) C26 0.037(4) 0.034(4) 0.028(3) 0.007(3) 0.010(3) -0.011(3) C27 0.047(5) 0.060(5) 0.029(4) 0.014(4) 0.008(4) -0.012(4) C28 0.065(6) 0.069(6) 0.048(5) 0.017(5) 0.023(5) -0.019(5) C29 0.076(7) 0.057(6) 0.041(5) 0.024(4) 0.025(5) -0.004(5) C30 0.045(5) 0.066(6) 0.033(4) 0.009(4) 0.002(4) 0.003(4) C31 0.043(5) 0.054(5) 0.039(4) 0.006(4) 0.010(4) -0.015(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 W1 C5 1.972(8) . ? W1 C25 2.058(7) . ? W1 C24 2.307(8) . ? W1 C9 2.327(9) . ? W1 C10 2.332(10) . ? W1 C11 2.355(9) . ? W1 C7 2.362(8) . ? W1 C8 2.366(9) . ? W1 P1 2.417(2) . ? W1 Fe2 2.6273(13) . ? W1 Fe1 2.7858(14) . ? Fe1 C1 1.782(8) . ? Fe1 C3 1.793(9) . ? Fe1 C6 1.803(9) . ? Fe1 C25 1.981(7) . ? Fe1 C24 2.008(7) . ? Fe1 Fe2 2.5671(16) . ? Fe2 C4 1.769(9) . ? Fe2 C2 1.783(9) . ? Fe2 C24 2.053(7) . ? Fe2 P1 2.178(2) . ? Fe2 C5 2.413(8) . ? P1 C18 1.816(8) . ? P1 C12 1.830(8) . ? C1 O1 1.143(10) . ? C2 O2 1.141(10) . ? C3 O3 1.140(10) . ? C4 O4 1.141(10) . ? C5 O5 1.172(9) . ? C6 O6 1.159(11) . ? C7 C11 1.392(14) . ? C7 C8 1.403(13) . ? C8 C9 1.422(14) . ? C9 C10 1.374(15) . ? C10 C11 1.404(16) . ? C12 C17 1.392(11) . ? C12 C13 1.406(11) . ? C13 C14 1.376(12) . ? C14 C15 1.402(14) . ? C15 C16 1.366(14) . ? C16 C17 1.391(12) . ? C18 C19 1.389(11) . ? C18 C23 1.404(12) . ? C19 C20 1.384(13) . ? C20 C21 1.380(14) . ? C21 C22 1.374(13) . ? C22 C23 1.408(12) . ? C24 C25 1.410(10) . ? C25 C26 1.501(10) . ? C26 C31 1.385(11) . ? C26 C27 1.393(11) . ? C27 C28 1.385(12) . ? C28 C29 1.379(13) . ? C29 C30 1.380(14) . ? C30 C31 1.388(12) . ? 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 W1 C25 109.0(3) . . ? C5 W1 C24 97.9(3) . . ? C25 W1 C24 37.2(3) . . ? C5 W1 C9 88.9(3) . . ? C25 W1 C9 142.8(3) . . ? C24 W1 C9 172.5(3) . . ? C5 W1 C10 83.6(4) . . ? C25 W1 C10 113.6(4) . . ? C24 W1 C10 149.5(4) . . ? C9 W1 C10 34.3(4) . . ? C5 W1 C11 112.3(4) . . ? C25 W1 C11 85.1(3) . . ? C24 W1 C11 121.7(3) . . ? C9 W1 C11 57.8(4) . . ? C10 W1 C11 34.9(4) . . ? C5 W1 C7 141.0(4) . . ? C25 W1 C7 90.9(3) . . ? C24 W1 C7 116.8(3) . . ? C9 W1 C7 58.0(3) . . ? C10 W1 C7 57.5(4) . . ? C11 W1 C7 34.3(4) . . ? C5 W1 C8 122.7(3) . . ? C25 W1 C8 123.8(3) . . ? C24 W1 C8 137.4(3) . . ? C9 W1 C8 35.3(3) . . ? C10 W1 C8 57.5(4) . . ? C11 W1 C8 57.4(3) . . ? C7 W1 C8 34.5(3) . . ? C5 W1 P1 93.2(2) . . ? C25 W1 P1 109.0(2) . . ? C24 W1 P1 74.52(19) . . ? C9 W1 P1 101.9(3) . . ? C10 W1 P1 135.9(3) . . ? C11 W1 P1 145.5(2) . . ? C7 W1 P1 112.1(3) . . ? C8 W1 P1 89.6(3) . . ? C5 W1 Fe2 61.4(2) . . ? C25 W1 Fe2 82.6(2) . . ? C24 W1 Fe2 48.65(19) . . ? C9 W1 Fe2 134.0(3) . . ? C10 W1 Fe2 144.9(3) . . ? C11 W1 Fe2 162.9(2) . . ? C7 W1 Fe2 157.1(3) . . ? C8 W1 Fe2 139.7(2) . . ? P1 W1 Fe2 50.94(6) . . ? C5 W1 Fe1 64.1(2) . . ? C25 W1 Fe1 45.3(2) . . ? C24 W1 Fe1 45.25(18) . . ? C9 W1 Fe1 142.0(3) . . ? C10 W1 Fe1 112.1(3) . . ? C11 W1 Fe1 106.4(2) . . ? C7 W1 Fe1 130.0(2) . . ? C8 W1 Fe1 163.4(2) . . ? P1 W1 Fe1 105.57(6) . . ? Fe2 W1 Fe1 56.53(4) . . ? C1 Fe1 C3 94.8(4) . . ? C1 Fe1 C6 99.8(4) . . ? C3 Fe1 C6 95.9(4) . . ? C1 Fe1 C25 100.4(3) . . ? C3 Fe1 C25 95.5(3) . . ? C6 Fe1 C25 155.7(4) . . ? C1 Fe1 C24 141.3(3) . . ? C3 Fe1 C24 95.3(3) . . ? C6 Fe1 C24 116.1(4) . . ? C25 Fe1 C24 41.4(3) . . ? C1 Fe1 Fe2 141.0(3) . . ? C3 Fe1 Fe2 123.1(3) . . ? C6 Fe1 Fe2 70.2(3) . . ? C25 Fe1 Fe2 85.6(2) . . ? C24 Fe1 Fe2 51.6(2) . . ? C1 Fe1 W1 97.6(3) . . ? C3 Fe1 W1 142.6(3) . . ? C6 Fe1 W1 116.3(3) . . ? C25 Fe1 W1 47.5(2) . . ? C24 Fe1 W1 54.7(2) . . ? Fe2 Fe1 W1 58.62(4) . . ? C4 Fe2 C2 90.0(4) . . ? C4 Fe2 C24 96.1(3) . . ? C2 Fe2 C24 168.8(3) . . ? C4 Fe2 P1 101.8(3) . . ? C2 Fe2 P1 102.9(3) . . ? C24 Fe2 P1 85.1(2) . . ? C4 Fe2 C5 167.2(3) . . ? C2 Fe2 C5 80.1(3) . . ? C24 Fe2 C5 92.4(3) . . ? P1 Fe2 C5 88.3(2) . . ? C4 Fe2 Fe1 115.9(3) . . ? C2 Fe2 Fe1 118.8(3) . . ? C24 Fe2 Fe1 50.0(2) . . ? P1 Fe2 Fe1 121.78(7) . . ? C5 Fe2 Fe1 63.31(18) . . ? C4 Fe2 W1 146.7(2) . . ? C2 Fe2 W1 119.7(3) . . ? C24 Fe2 W1 57.5(2) . . ? P1 Fe2 W1 59.54(6) . . ? C5 Fe2 W1 45.8(2) . . ? Fe1 Fe2 W1 64.85(4) . . ? C18 P1 C12 105.6(4) . . ? C18 P1 Fe2 121.3(3) . . ? C12 P1 Fe2 116.5(2) . . ? C18 P1 W1 124.3(3) . . ? C12 P1 W1 116.8(2) . . ? Fe2 P1 W1 69.52(7) . . ? O1 C1 Fe1 177.7(7) . . ? O2 C2 Fe2 176.8(8) . . ? O3 C3 Fe1 176.1(8) . . ? O4 C4 Fe2 173.5(7) . . ? O5 C5 W1 161.0(7) . . ? O5 C5 Fe2 123.7(6) . . ? W1 C5 Fe2 72.8(3) . . ? O6 C6 Fe1 165.6(8) . . ? C11 C7 C8 108.4(9) . . ? C11 C7 W1 72.6(5) . . ? C8 C7 W1 72.9(5) . . ? C7 C8 C9 107.2(9) . . ? C7 C8 W1 72.6(5) . . ? C9 C8 W1 70.9(5) . . ? C10 C9 C8 107.8(9) . . ? C10 C9 W1 73.1(5) . . ? C8 C9 W1 73.8(5) . . ? C9 C10 C11 109.0(9) . . ? C9 C10 W1 72.6(5) . . ? C11 C10 W1 73.5(6) . . ? C7 C11 C10 107.6(9) . . ? C7 C11 W1 73.1(5) . . ? C10 C11 W1 71.7(6) . . ? C17 C12 C13 117.4(7) . . ? C17 C12 P1 122.5(6) . . ? C13 C12 P1 120.0(6) . . ? C14 C13 C12 121.6(8) . . ? C13 C14 C15 120.2(9) . . ? C16 C15 C14 118.3(9) . . ? C15 C16 C17 122.0(9) . . ? C12 C17 C16 120.3(9) . . ? C19 C18 C23 118.7(7) . . ? C19 C18 P1 123.1(7) . . ? C23 C18 P1 118.1(6) . . ? C20 C19 C18 120.2(9) . . ? C21 C20 C19 121.3(9) . . ? C22 C21 C20 119.7(9) . . ? C21 C22 C23 119.9(9) . . ? C18 C23 C22 120.2(8) . . ? C25 C24 Fe1 68.3(4) . . ? C25 C24 Fe2 127.6(6) . . ? Fe1 C24 Fe2 78.4(3) . . ? C25 C24 W1 61.8(4) . . ? Fe1 C24 W1 80.1(3) . . ? Fe2 C24 W1 73.8(2) . . ? C24 C25 C26 126.7(7) . . ? C24 C25 Fe1 70.3(4) . . ? C26 C25 Fe1 132.9(5) . . ? C24 C25 W1 81.1(4) . . ? C26 C25 W1 134.6(5) . . ? Fe1 C25 W1 87.2(3) . . ? C31 C26 C27 118.8(7) . . ? C31 C26 C25 120.9(7) . . ? C27 C26 C25 120.2(7) . . ? C28 C27 C26 120.5(8) . . ? C29 C28 C27 120.3(9) . . ? C28 C29 C30 119.5(8) . . ? C29 C30 C31 120.5(8) . . ? C30 C31 C26 120.3(8) . . ? _diffrn_measured_fraction_theta_max 0.824 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.824 _refine_diff_density_max 2.970 _refine_diff_density_min -1.520 _refine_diff_density_rms 0.186 data_mm9633 _database_code_CSD 175754 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C31 H20 Co Fe Mo O6 P' _chemical_formula_weight 730.16 _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' 'Co' 'Co' 0.3494 0.9721 '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' '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 10.557(4) _cell_length_b 20.399(4) _cell_length_c 13.625(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.51(2) _cell_angle_gamma 90.00 _cell_volume 2928.7(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 17 _cell_measurement_theta_max 25 _exptl_crystal_description prism _exptl_crystal_colour dark _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_method ? _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 1.567 _exptl_absorpt_correction_type 'empirical (4 psi scans)' _exptl_absorpt_correction_T_min 0.871 _exptl_absorpt_correction_T_max 0.997 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device AFC5r _diffrn_measurement_method 'omega 2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0% _diffrn_reflns_number 5453 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0991 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5152 _reflns_number_observed 3252 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'standard MSC/Rigaku supplied software' _computing_cell_refinement 'standard MSC/Rigaku supplied software' _computing_data_reduction 'standard MSC/Rigaku supplied software' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XP' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 16 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^)+(0.0513P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5136 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1227 _refine_ls_R_factor_obs 0.0466 _refine_ls_wR_factor_all 0.2186 _refine_ls_wR_factor_obs 0.1075 _refine_ls_goodness_of_fit_all 1.048 _refine_ls_goodness_of_fit_obs 1.110 _refine_ls_restrained_S_all 1.756 _refine_ls_restrained_S_obs 1.110 _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 Mo1 Mo 0.77443(5) -0.22256(3) 0.18675(4) 0.0325(2) Uani 1 d . . Co1 Co 0.73159(8) -0.09331(4) 0.13810(6) 0.0314(2) Uani 1 d . . Fe1 Fe 0.80974(9) -0.11347(4) 0.31248(7) 0.0358(3) Uani 1 d . . P1 P 0.8778(2) -0.15483(8) 0.07454(12) 0.0312(4) Uani 1 d . . O1 O 0.5520(5) -0.2491(3) 0.0304(4) 0.071(2) Uani 1 d . . C1 C 0.6357(7) -0.2376(3) 0.0847(5) 0.045(2) Uani 1 d . . O2 O 0.5617(6) -0.0821(4) -0.0404(5) 0.089(2) Uani 1 d . . C2 C 0.6237(7) -0.0883(4) 0.0303(6) 0.050(2) Uani 1 d . . O3 O 0.8205(6) 0.0416(3) 0.1380(5) 0.076(2) Uani 1 d . . C3 C 0.7882(7) -0.0120(4) 0.1391(6) 0.048(2) Uani 1 d . . C4 C 0.9724(8) -0.1376(4) 0.3205(6) 0.050(2) Uani 1 d . . O4 O 1.0765(5) -0.1513(3) 0.3355(5) 0.074(2) Uani 1 d . . O5 O 0.8528(7) 0.0203(3) 0.3849(5) 0.088(2) Uani 1 d . . C5 C 0.8334(8) -0.0313(4) 0.3562(6) 0.053(2) Uani 1 d . . O6 O 0.7487(7) -0.1710(3) 0.5002(4) 0.092(2) Uani 1 d . . C6 C 0.7743(8) -0.1489(4) 0.4283(6) 0.050(2) Uani 1 d . . C7 C 0.6576(6) -0.1559(3) 0.2391(4) 0.0319(15) Uani 1 d . . C8 C 0.6237(6) -0.0955(3) 0.2587(5) 0.036(2) Uani 1 d . . C9 C 0.5251(6) -0.0554(3) 0.3014(5) 0.037(2) Uani 1 d . . C10 C 0.4469(8) -0.0848(4) 0.3670(6) 0.061(2) Uani 1 d . . H10A H 0.4588 -0.1288 0.3833 0.073 Uiso 1 calc R . C11 C 0.3526(9) -0.0499(6) 0.4080(7) 0.084(3) Uani 1 d . . H11A H 0.2998 -0.0705 0.4507 0.101 Uiso 1 calc R . C12 C 0.3360(9) 0.0145(5) 0.3866(7) 0.077(3) Uani 1 d . . H12A H 0.2739 0.0384 0.4164 0.092 Uiso 1 calc R . C13 C 0.4106(8) 0.0445(4) 0.3209(8) 0.073(3) Uani 1 d . . H13A H 0.3969 0.0883 0.3043 0.087 Uiso 1 calc R . C14 C 0.5065(7) 0.0096(4) 0.2792(6) 0.057(2) Uani 1 d . . H14A H 0.5584 0.0303 0.2360 0.069 Uiso 1 calc R . C15 C 0.8902(12) -0.2867(4) 0.3047(8) 0.079(3) Uani 1 d . . H15A H 0.9286 -0.2710 0.3677 0.094 Uiso 1 calc R . C16 C 0.9495(9) -0.2895(4) 0.2169(10) 0.082(3) Uani 1 d . . H16A H 1.0380 -0.2781 0.2070 0.098 Uiso 1 calc R . C17 C 0.8656(14) -0.3218(5) 0.1498(7) 0.088(4) Uani 1 d . . H17A H 0.8849 -0.3368 0.0840 0.106 Uiso 1 calc R . C18 C 0.7570(12) -0.3356(4) 0.1964(11) 0.088(4) Uani 1 d . . H18A H 0.6854 -0.3620 0.1695 0.105 Uiso 1 calc R . C19 C 0.7735(12) -0.3133(5) 0.2899(8) 0.082(3) Uani 1 d . . H19A H 0.7138 -0.3202 0.3413 0.099 Uiso 1 calc R . C20 C 0.8645(6) -0.1701(3) -0.0583(5) 0.038(2) Uani 1 d . . C21 C 0.9019(7) -0.1199(4) -0.1195(5) 0.053(2) Uani 1 d . . H21A H 0.9303 -0.0802 -0.0927 0.064 Uiso 1 calc R . C22 C 0.8967(9) -0.1293(5) -0.2211(6) 0.072(3) Uani 1 d . . H22A H 0.9193 -0.0953 -0.2620 0.087 Uiso 1 calc R . C23 C 0.8588(8) -0.1877(5) -0.2609(6) 0.064(2) Uani 1 d . . H23A H 0.8584 -0.1939 -0.3285 0.077 Uiso 1 calc R . C24 C 0.8211(9) -0.2373(5) -0.2019(6) 0.070(3) Uani 1 d . . H24A H 0.7939 -0.2771 -0.2290 0.084 Uiso 1 calc R . C25 C 0.8241(7) -0.2275(4) -0.1007(5) 0.053(2) Uani 1 d . . H25A H 0.7975 -0.2611 -0.0608 0.063 Uiso 1 calc R . C26 C 1.0451(6) -0.1328(3) 0.0886(5) 0.035(2) Uani 1 d . . C27 C 1.0889(7) -0.0745(4) 0.1289(6) 0.053(2) Uani 1 d . . H27A H 1.0305 -0.0441 0.1497 0.063 Uiso 1 calc R . C28 C 1.2159(8) -0.0598(5) 0.1393(7) 0.070(3) Uani 1 d . . H28A H 1.2431 -0.0201 0.1668 0.084 Uiso 1 calc R . C29 C 1.3030(7) -0.1049(5) 0.1083(6) 0.066(3) Uani 1 d . . H29A H 1.3893 -0.0954 0.1146 0.079 Uiso 1 calc R . C30 C 1.2626(7) -0.1635(5) 0.0683(6) 0.065(3) Uani 1 d . . H30A H 1.3214 -0.1939 0.0482 0.078 Uiso 1 calc R . C31 C 1.1352(7) -0.1773(4) 0.0581(5) 0.049(2) Uani 1 d . . H31A H 1.1085 -0.2170 0.0304 0.058 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 Mo1 0.0408(3) 0.0248(3) 0.0319(3) -0.0001(3) 0.0014(2) -0.0004(3) Co1 0.0333(5) 0.0296(5) 0.0315(5) 0.0028(4) 0.0045(4) 0.0032(4) Fe1 0.0429(6) 0.0309(5) 0.0332(6) -0.0012(4) -0.0019(4) 0.0022(4) P1 0.0306(9) 0.0311(9) 0.0320(9) -0.0029(7) 0.0034(7) 0.0002(8) O1 0.048(3) 0.086(4) 0.076(4) -0.014(3) -0.015(3) -0.014(3) C1 0.048(4) 0.042(4) 0.046(4) 0.000(3) 0.006(4) 0.001(4) O2 0.069(4) 0.138(7) 0.055(4) 0.019(4) -0.022(3) 0.010(4) C2 0.038(4) 0.064(5) 0.049(5) 0.007(4) 0.009(4) 0.006(4) O3 0.101(5) 0.039(3) 0.092(5) 0.002(3) 0.029(4) -0.006(3) C3 0.054(5) 0.041(4) 0.051(5) 0.002(4) 0.012(4) 0.007(4) C4 0.061(5) 0.040(4) 0.049(5) -0.003(4) -0.012(4) -0.001(4) O4 0.046(4) 0.082(5) 0.091(5) 0.003(4) -0.012(3) 0.017(3) O5 0.132(6) 0.038(3) 0.092(5) -0.016(3) -0.011(4) -0.015(4) C5 0.067(5) 0.039(4) 0.050(5) 0.001(4) -0.009(4) 0.006(4) O6 0.153(7) 0.083(5) 0.042(4) 0.020(3) 0.010(4) -0.004(5) C6 0.060(5) 0.046(5) 0.043(5) -0.003(4) -0.009(4) 0.009(4) C7 0.038(4) 0.030(4) 0.028(4) -0.001(3) 0.004(3) -0.005(3) C8 0.035(4) 0.041(4) 0.033(4) 0.002(3) 0.002(3) -0.006(3) C9 0.038(4) 0.039(4) 0.035(4) -0.003(3) 0.009(3) 0.001(3) C10 0.073(6) 0.062(5) 0.051(5) 0.013(4) 0.027(5) 0.022(5) C11 0.077(7) 0.104(9) 0.077(7) 0.010(6) 0.050(6) 0.008(6) C12 0.062(6) 0.083(7) 0.088(7) -0.032(6) 0.026(5) 0.014(6) C13 0.052(5) 0.041(5) 0.126(9) -0.019(5) 0.009(6) 0.003(4) C14 0.042(5) 0.050(5) 0.081(6) 0.000(4) 0.008(4) -0.003(4) C15 0.123(9) 0.042(5) 0.066(7) 0.009(5) -0.040(7) 0.008(6) C16 0.062(6) 0.051(6) 0.132(10) 0.038(6) 0.001(7) 0.023(5) C17 0.154(12) 0.056(6) 0.055(6) -0.018(5) 0.001(7) 0.056(7) C18 0.097(9) 0.032(5) 0.128(11) 0.014(6) -0.038(8) -0.008(5) C19 0.124(10) 0.055(6) 0.070(7) 0.036(5) 0.020(7) 0.015(6) C20 0.033(4) 0.047(4) 0.034(4) 0.000(3) 0.004(3) 0.000(3) C21 0.057(5) 0.060(5) 0.042(5) 0.011(4) -0.003(4) -0.006(4) C22 0.085(7) 0.091(7) 0.041(5) 0.029(5) 0.003(5) -0.008(6) C23 0.069(6) 0.089(7) 0.033(5) -0.008(5) -0.005(4) 0.001(5) C24 0.089(7) 0.081(7) 0.040(5) -0.016(5) 0.002(5) -0.009(5) C25 0.064(5) 0.059(5) 0.035(4) -0.006(4) 0.004(4) -0.007(4) C26 0.028(4) 0.044(4) 0.032(4) 0.003(3) 0.002(3) -0.003(3) C27 0.031(4) 0.055(5) 0.072(6) -0.017(4) 0.009(4) -0.009(4) C28 0.056(6) 0.079(6) 0.073(6) -0.015(5) 0.000(5) -0.019(5) C29 0.032(4) 0.120(8) 0.044(5) -0.007(5) 0.000(4) -0.013(5) C30 0.039(5) 0.106(8) 0.052(5) 0.004(5) 0.007(4) 0.023(5) C31 0.044(4) 0.055(5) 0.047(5) -0.002(4) 0.004(4) 0.009(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 Mo1 C1 1.980(8) . ? Mo1 C7 1.997(6) . ? Mo1 C17 2.310(8) . ? Mo1 C16 2.314(8) . ? Mo1 C18 2.318(8) . ? Mo1 C19 2.325(8) . ? Mo1 C15 2.355(8) . ? Mo1 P1 2.375(2) . ? Mo1 Co1 2.7493(11) . ? Mo1 Fe1 2.8190(11) . ? Co1 C3 1.763(8) . ? Co1 C2 1.806(8) . ? Co1 C8 2.056(7) . ? Co1 C7 2.065(6) . ? Co1 P1 2.207(2) . ? Co1 Fe1 2.5009(13) . ? Fe1 C4 1.783(9) . ? Fe1 C5 1.792(8) . ? Fe1 C6 1.796(9) . ? Fe1 C7 2.032(6) . ? Fe1 C8 2.086(7) . ? P1 C26 1.821(6) . ? P1 C20 1.833(7) . ? O1 C1 1.142(8) . ? O2 C2 1.138(9) . ? O3 C3 1.146(8) . ? C4 O4 1.141(9) . ? O5 C5 1.136(9) . ? O6 C6 1.126(9) . ? C7 C8 1.314(9) . ? C8 C9 1.471(9) . ? C9 C14 1.370(10) . ? C9 C10 1.390(10) . ? C10 C11 1.371(11) . ? C11 C12 1.354(13) . ? C12 C13 1.372(12) . ? C13 C14 1.389(11) . ? C15 C19 1.351(13) . ? C15 C16 1.385(14) . ? C16 C17 1.398(14) . ? C17 C18 1.373(14) . ? C18 C19 1.355(14) . ? C20 C25 1.361(9) . ? C20 C21 1.394(10) . ? C21 C22 1.396(11) . ? C22 C23 1.359(12) . ? C23 C24 1.367(12) . ? C24 C25 1.392(10) . ? C26 C27 1.378(9) . ? C26 C31 1.397(9) . ? C27 C28 1.373(10) . ? C28 C29 1.385(12) . ? C29 C30 1.371(12) . ? C30 C31 1.373(10) . ? 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 C1 Mo1 C7 84.8(3) . . ? C1 Mo1 C17 90.7(4) . . ? C7 Mo1 C17 161.7(4) . . ? C1 Mo1 C16 125.5(4) . . ? C7 Mo1 C16 147.4(4) . . ? C17 Mo1 C16 35.2(4) . . ? C1 Mo1 C18 80.1(3) . . ? C7 Mo1 C18 127.2(4) . . ? C17 Mo1 C18 34.5(4) . . ? C16 Mo1 C18 57.9(4) . . ? C1 Mo1 C19 105.7(4) . . ? C7 Mo1 C19 107.5(3) . . ? C17 Mo1 C19 56.7(4) . . ? C16 Mo1 C19 57.0(4) . . ? C18 Mo1 C19 33.9(4) . . ? C1 Mo1 C15 136.4(3) . . ? C7 Mo1 C15 116.1(3) . . ? C17 Mo1 C15 57.1(3) . . ? C16 Mo1 C15 34.5(3) . . ? C18 Mo1 C15 56.6(3) . . ? C19 Mo1 C15 33.5(3) . . ? C1 Mo1 P1 89.3(2) . . ? C7 Mo1 P1 98.7(2) . . ? C17 Mo1 P1 98.9(3) . . ? C16 Mo1 P1 93.7(3) . . ? C18 Mo1 P1 131.0(4) . . ? C19 Mo1 P1 150.6(3) . . ? C15 Mo1 P1 121.5(3) . . ? C1 Mo1 Co1 82.8(2) . . ? C7 Mo1 Co1 48.5(2) . . ? C17 Mo1 Co1 148.5(3) . . ? C16 Mo1 Co1 136.6(2) . . ? C18 Mo1 Co1 162.8(3) . . ? C19 Mo1 Co1 154.5(3) . . ? C15 Mo1 Co1 140.2(2) . . ? P1 Mo1 Co1 50.37(5) . . ? C1 Mo1 Fe1 127.8(2) . . ? C7 Mo1 Fe1 46.1(2) . . ? C17 Mo1 Fe1 141.5(3) . . ? C16 Mo1 Fe1 106.5(3) . . ? C18 Mo1 Fe1 139.4(4) . . ? C19 Mo1 Fe1 105.4(3) . . ? C15 Mo1 Fe1 88.8(2) . . ? P1 Mo1 Fe1 83.29(5) . . ? Co1 Mo1 Fe1 53.36(3) . . ? C3 Co1 C2 98.6(4) . . ? C3 Co1 C8 102.6(3) . . ? C2 Co1 C8 107.4(3) . . ? C3 Co1 C7 135.9(3) . . ? C2 Co1 C7 109.4(3) . . ? C8 Co1 C7 37.2(2) . . ? C3 Co1 P1 107.0(2) . . ? C2 Co1 P1 97.7(2) . . ? C8 Co1 P1 137.4(2) . . ? C7 Co1 P1 102.3(2) . . ? C3 Co1 Fe1 93.2(3) . . ? C2 Co1 Fe1 159.6(2) . . ? C8 Co1 Fe1 53.4(2) . . ? C7 Co1 Fe1 51.8(2) . . ? P1 Co1 Fe1 94.66(6) . . ? C3 Co1 Mo1 148.2(3) . . ? C2 Co1 Mo1 109.7(3) . . ? C8 Co1 Mo1 83.0(2) . . ? C7 Co1 Mo1 46.4(2) . . ? P1 Co1 Mo1 55.99(5) . . ? Fe1 Co1 Mo1 64.75(3) . . ? C4 Fe1 C5 97.1(4) . . ? C4 Fe1 C6 95.0(4) . . ? C5 Fe1 C6 96.7(3) . . ? C4 Fe1 C7 129.9(3) . . ? C5 Fe1 C7 130.7(3) . . ? C6 Fe1 C7 93.4(3) . . ? C4 Fe1 C8 162.3(3) . . ? C5 Fe1 C8 93.5(3) . . ? C6 Fe1 C8 97.9(3) . . ? C7 Fe1 C8 37.2(2) . . ? C4 Fe1 Co1 111.4(3) . . ? C5 Fe1 Co1 101.1(2) . . ? C6 Fe1 Co1 145.7(3) . . ? C7 Fe1 Co1 53.0(2) . . ? C8 Fe1 Co1 52.3(2) . . ? C4 Fe1 Mo1 84.9(2) . . ? C5 Fe1 Mo1 162.0(2) . . ? C6 Fe1 Mo1 100.9(2) . . ? C7 Fe1 Mo1 45.1(2) . . ? C8 Fe1 Mo1 80.7(2) . . ? Co1 Fe1 Mo1 61.90(3) . . ? C26 P1 C20 99.3(3) . . ? C26 P1 Co1 121.0(2) . . ? C20 P1 Co1 118.1(2) . . ? C26 P1 Mo1 123.8(2) . . ? C20 P1 Mo1 121.7(2) . . ? Co1 P1 Mo1 73.64(6) . . ? O1 C1 Mo1 175.2(7) . . ? O2 C2 Co1 175.1(7) . . ? O3 C3 Co1 177.3(8) . . ? O4 C4 Fe1 173.1(7) . . ? O5 C5 Fe1 177.5(8) . . ? O6 C6 Fe1 178.2(8) . . ? C8 C7 Mo1 153.2(5) . . ? C8 C7 Fe1 73.6(4) . . ? Mo1 C7 Fe1 88.8(3) . . ? C8 C7 Co1 71.0(4) . . ? Mo1 C7 Co1 85.2(2) . . ? Fe1 C7 Co1 75.2(2) . . ? C7 C8 C9 144.0(6) . . ? C7 C8 Co1 71.8(4) . . ? C9 C8 Co1 138.0(5) . . ? C7 C8 Fe1 69.2(4) . . ? C9 C8 Fe1 129.2(5) . . ? Co1 C8 Fe1 74.3(2) . . ? C14 C9 C10 118.5(7) . . ? C14 C9 C8 123.1(6) . . ? C10 C9 C8 118.4(6) . . ? C11 C10 C9 120.8(8) . . ? C12 C11 C10 120.3(9) . . ? C11 C12 C13 120.1(8) . . ? C12 C13 C14 120.0(8) . . ? C9 C14 C13 120.3(8) . . ? C19 C15 C16 108.1(9) . . ? C19 C15 Mo1 72.0(5) . . ? C16 C15 Mo1 71.1(5) . . ? C15 C16 C17 106.5(10) . . ? C15 C16 Mo1 74.4(5) . . ? C17 C16 Mo1 72.3(5) . . ? C18 C17 C16 107.9(9) . . ? C18 C17 Mo1 73.0(5) . . ? C16 C17 Mo1 72.6(5) . . ? C19 C18 C17 107.6(10) . . ? C19 C18 Mo1 73.3(5) . . ? C17 C18 Mo1 72.4(5) . . ? C15 C19 C18 109.8(10) . . ? C15 C19 Mo1 74.5(5) . . ? C18 C19 Mo1 72.7(5) . . ? C25 C20 C21 118.1(7) . . ? C25 C20 P1 124.6(5) . . ? C21 C20 P1 117.2(6) . . ? C20 C21 C22 119.8(8) . . ? C23 C22 C21 120.6(8) . . ? C22 C23 C24 120.3(8) . . ? C23 C24 C25 119.0(8) . . ? C20 C25 C24 122.2(8) . . ? C27 C26 C31 117.5(6) . . ? C27 C26 P1 123.7(5) . . ? C31 C26 P1 118.9(5) . . ? C28 C27 C26 122.1(8) . . ? C27 C28 C29 119.1(8) . . ? C30 C29 C28 120.3(7) . . ? C29 C30 C31 119.9(8) . . ? C30 C31 C26 121.2(8) . . ? _refine_diff_density_max 0.547 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.169 data_mm9815 _database_code_CSD 175755 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H23 Cl2 Fe2 Mo O7 P' _chemical_formula_weight 841.02 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' 'Cl' 'Cl' 0.1484 0.1585 '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 9.4030(10) _cell_length_b 12.500(4) _cell_length_c 14.208(2) _cell_angle_alpha 93.070(10) _cell_angle_beta 98.320(10) _cell_angle_gamma 104.59(2) _cell_volume 1592.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 15.0 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.754 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 1.554 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.5898 _exptl_absorpt_correction_T_max 0.8118 _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe' _diffrn_measurement_method \w/2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 90 _diffrn_standards_decay_% 1 _diffrn_reflns_number 6691 _diffrn_reflns_av_R_equivalents 0.1529 _diffrn_reflns_av_sigmaI/netI 0.1781 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5571 _reflns_number_gt 3102 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'standard MSC/Rigaku supplied software' _computing_cell_refinement 'standard MSC/Rigaku supplied software' _computing_data_reduction 'standard MSC/Rigaku supplied software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP' _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^)+(0.1299P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5571 _refine_ls_number_parameters 381 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1760 _refine_ls_R_factor_gt 0.0938 _refine_ls_wR_factor_ref 0.2607 _refine_ls_wR_factor_gt 0.2173 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.001 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 Mo1 Mo 0.24665(12) 0.40137(10) 0.18664(9) 0.0175(3) Uani 1 d . . . Fe1 Fe 0.11749(19) 0.43763(16) 0.33997(15) 0.0187(5) Uani 1 d . . . Fe2 Fe 0.03910(19) 0.23560(16) 0.24399(15) 0.0203(5) Uani 1 d . . . Cl1 Cl 0.3096(8) 0.0331(6) -0.0332(5) 0.092(2) Uani 1 d . . . Cl2 Cl 0.3776(8) 0.1799(6) -0.1776(5) 0.091(2) Uani 1 d . . . P1 P 0.2669(3) 0.5717(3) 0.2732(3) 0.0181(8) Uani 1 d . . . O1 O -0.0545(10) 0.4273(8) 0.0803(7) 0.030(2) Uani 1 d . . . O2 O 0.2328(12) 0.5630(9) 0.5237(8) 0.037(3) Uani 1 d . . . O3 O -0.1622(10) 0.4954(9) 0.2747(8) 0.034(3) Uani 1 d . . . O4 O -0.0292(10) 0.2750(8) 0.4577(8) 0.033(3) Uani 1 d . . . O5 O -0.2666(11) 0.2424(10) 0.1607(9) 0.045(3) Uani 1 d . . . O6 O -0.0391(14) 0.0450(10) 0.3534(10) 0.049(3) Uani 1 d . . . O7 O 0.0565(11) 0.1081(9) 0.0719(8) 0.031(2) Uani 1 d . . . C1 C 0.0521(15) 0.4130(11) 0.1240(10) 0.022(3) Uani 1 d . . . C2 C 0.1861(14) 0.5137(13) 0.4517(11) 0.024(3) Uani 1 d . . . C3 C -0.0549(14) 0.4763(11) 0.3006(11) 0.024(3) Uani 1 d . . . C4 C 0.0216(14) 0.3243(12) 0.3982(12) 0.027(3) Uani 1 d . . . C5 C -0.1482(16) 0.2405(12) 0.1945(11) 0.028(3) Uani 1 d . . . C6 C -0.0085(15) 0.1205(13) 0.3131(11) 0.028(4) Uani 1 d . . . C7 C 0.0516(14) 0.1572(12) 0.1391(11) 0.026(3) Uani 1 d . . . C8 C 0.2932(14) 0.3757(11) 0.3413(11) 0.024(3) Uani 1 d . . . H8 H 0.3229 0.4144 0.4033 0.029 Uiso 1 calc R . . C9 C 0.2540(13) 0.2729(11) 0.2946(10) 0.019(3) Uani 1 d . . . C10 C 0.3587(14) 0.1994(11) 0.3009(10) 0.021(3) Uani 1 d . . . C11 C 0.5069(13) 0.2400(12) 0.3400(11) 0.025(3) Uani 1 d . . . H11 H 0.5455 0.3169 0.3603 0.030 Uiso 1 calc R . . C12 C 0.5998(15) 0.1705(12) 0.3501(12) 0.031(4) Uani 1 d . . . H12 H 0.7019 0.2014 0.3764 0.037 Uiso 1 calc R . . C13 C 0.5512(16) 0.0592(13) 0.3240(12) 0.035(4) Uani 1 d . . . H13 H 0.6174 0.0131 0.3329 0.042 Uiso 1 calc R . . C14 C 0.4033(16) 0.0150(14) 0.2844(12) 0.036(4) Uani 1 d . . . H14 H 0.3665 -0.0623 0.2654 0.043 Uiso 1 calc R . . C15 C 0.3090(15) 0.0839(12) 0.2726(12) 0.030(4) Uani 1 d . . . H15 H 0.2078 0.0529 0.2447 0.037 Uiso 1 calc R . . C16 C 0.3180(15) 0.4606(12) 0.0431(10) 0.0260(14) Uiso 1 d . . . H16 H 0.2695 0.5072 0.0074 0.031 Uiso 1 calc R . . C17 C 0.4454(15) 0.4960(12) 0.1131(10) 0.0260(14) Uiso 1 d . . . H17 H 0.4974 0.5712 0.1330 0.031 Uiso 1 calc R . . C18 C 0.4845(15) 0.4025(11) 0.1495(11) 0.0260(14) Uiso 1 d . . . H18 H 0.5668 0.4030 0.1971 0.031 Uiso 1 calc R . . C19 C 0.3758(15) 0.3071(12) 0.1005(10) 0.0260(14) Uiso 1 d . . . H19 H 0.3719 0.2319 0.1102 0.031 Uiso 1 calc R . . C20 C 0.2750(16) 0.3447(12) 0.0349(11) 0.0260(14) Uiso 1 d . . . H20 H 0.1921 0.2988 -0.0075 0.031 Uiso 1 calc R . . C21 C 0.1819(14) 0.6783(11) 0.2255(10) 0.018(3) Uiso 1 d . . . C22 C 0.0946(15) 0.7256(11) 0.2784(11) 0.024(3) Uani 1 d . . . H22 H 0.0805 0.7040 0.3402 0.029 Uiso 1 calc R . . C23 C 0.0299(14) 0.8033(11) 0.2397(12) 0.030(4) Uani 1 d . . . H23 H -0.0287 0.8360 0.2756 0.036 Uiso 1 calc R . . C24 C 0.0477(17) 0.8346(13) 0.1508(12) 0.035(4) Uani 1 d . . . H24 H 0.0022 0.8889 0.1252 0.042 Uiso 1 calc R . . C25 C 0.1314(17) 0.7878(13) 0.0986(12) 0.034(4) Uani 1 d . . . H25 H 0.1445 0.8088 0.0365 0.041 Uiso 1 calc R . . C26 C 0.1975(16) 0.7083(12) 0.1382(11) 0.028(3) Uani 1 d . . . H26 H 0.2549 0.6749 0.1019 0.034 Uiso 1 calc R . . C27 C 0.4441(15) 0.7522(11) 0.3962(10) 0.025(3) Uani 1 d . . . H27 H 0.3555 0.7756 0.3963 0.030 Uiso 1 calc R . . C28 C 0.5804(17) 0.8194(13) 0.4480(10) 0.030(3) Uani 1 d . . . H28 H 0.5829 0.8868 0.4833 0.036 Uiso 1 calc R . . C29 C 0.7095(15) 0.7863(13) 0.4467(11) 0.033(4) Uani 1 d . . . H29 H 0.8019 0.8310 0.4804 0.039 Uiso 1 calc R . . C30 C 0.7027(14) 0.6897(12) 0.3969(11) 0.026(3) Uani 1 d . . . H30 H 0.7920 0.6678 0.3949 0.031 Uiso 1 calc R . . C31 C 0.5709(15) 0.6223(13) 0.3493(11) 0.029(4) Uani 1 d . . . H31 H 0.5703 0.5529 0.3181 0.035 Uiso 1 calc R . . C32 C 0.4379(14) 0.6526(13) 0.3452(10) 0.027(3) Uani 1 d . . . C33 C 0.431(4) 0.093(3) -0.094(2) 0.120(12) Uani 1 d . . . H33A H 0.4640 0.0346 -0.1280 0.144 Uiso 1 calc R . . H33B H 0.5188 0.1375 -0.0483 0.144 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 Mo1 0.0080(5) 0.0232(7) 0.0212(7) -0.0031(5) -0.0002(4) 0.0067(4) Fe1 0.0079(9) 0.0231(11) 0.0256(12) -0.0036(9) -0.0001(8) 0.0074(8) Fe2 0.0092(9) 0.0234(11) 0.0282(12) -0.0014(9) -0.0003(8) 0.0069(8) Cl1 0.090(5) 0.095(5) 0.094(5) 0.023(4) 0.024(4) 0.021(4) Cl2 0.095(5) 0.110(5) 0.079(5) 0.037(4) 0.013(4) 0.044(4) P1 0.0102(15) 0.0218(19) 0.024(2) -0.0001(15) -0.0012(14) 0.0105(13) O1 0.013(5) 0.041(6) 0.029(6) -0.005(5) -0.010(4) 0.006(4) O2 0.035(6) 0.044(7) 0.030(7) -0.009(6) -0.001(5) 0.011(5) O3 0.015(5) 0.038(6) 0.049(7) -0.001(5) -0.005(5) 0.014(5) O4 0.016(5) 0.029(6) 0.047(7) 0.008(5) 0.001(5) -0.004(4) O5 0.016(5) 0.066(8) 0.050(8) 0.001(6) -0.013(5) 0.014(5) O6 0.055(8) 0.029(7) 0.069(10) 0.015(7) 0.024(7) 0.012(6) O7 0.029(6) 0.039(6) 0.025(6) -0.010(5) -0.001(5) 0.014(5) C1 0.027(8) 0.024(8) 0.022(8) 0.001(6) 0.008(6) 0.017(6) C2 0.012(6) 0.043(9) 0.024(9) 0.007(7) 0.002(6) 0.017(6) C3 0.012(7) 0.016(7) 0.043(10) 0.000(7) 0.006(6) -0.001(5) C4 0.008(6) 0.032(8) 0.042(10) -0.006(7) -0.001(6) 0.011(6) C5 0.033(9) 0.025(8) 0.031(9) 0.010(7) 0.008(7) 0.015(7) C6 0.021(7) 0.032(9) 0.036(9) -0.008(7) -0.002(6) 0.024(7) C7 0.016(7) 0.033(9) 0.029(9) 0.011(7) 0.003(6) 0.001(6) C8 0.019(7) 0.024(8) 0.028(9) -0.016(6) 0.000(6) 0.007(6) C9 0.011(6) 0.024(7) 0.027(8) 0.001(6) 0.007(6) 0.009(5) C10 0.016(6) 0.028(8) 0.016(8) -0.003(6) -0.003(5) 0.004(6) C11 0.004(6) 0.031(8) 0.036(9) 0.003(7) -0.007(6) 0.001(5) C12 0.013(7) 0.033(9) 0.045(10) 0.002(7) -0.005(6) 0.011(6) C13 0.027(8) 0.036(9) 0.056(11) 0.011(8) 0.008(7) 0.031(7) C14 0.028(8) 0.036(9) 0.045(11) -0.007(8) 0.003(7) 0.016(7) C15 0.018(7) 0.026(8) 0.048(10) -0.008(7) -0.006(7) 0.014(6) C22 0.023(7) 0.018(7) 0.027(9) -0.013(6) -0.006(6) 0.007(6) C23 0.008(6) 0.017(7) 0.059(12) -0.005(7) -0.005(6) 0.002(5) C24 0.033(8) 0.027(9) 0.043(11) -0.002(8) -0.012(7) 0.014(7) C25 0.034(8) 0.030(9) 0.033(10) -0.001(7) -0.008(7) 0.006(7) C26 0.031(8) 0.023(8) 0.029(9) -0.008(7) -0.007(7) 0.015(6) C27 0.016(7) 0.024(8) 0.030(9) -0.006(7) 0.000(6) 0.000(6) C28 0.044(9) 0.036(9) 0.014(8) 0.005(7) 0.003(7) 0.018(7) C29 0.017(7) 0.039(10) 0.035(10) -0.007(8) -0.006(6) 0.003(6) C30 0.007(6) 0.033(9) 0.037(9) 0.008(7) 0.000(6) 0.006(6) C31 0.019(7) 0.030(8) 0.039(10) 0.000(7) 0.005(7) 0.008(6) C32 0.010(6) 0.042(9) 0.024(8) -0.008(7) 0.002(6) 0.000(6) C33 0.15(3) 0.18(3) 0.07(2) 0.03(2) 0.07(2) 0.08(3) _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 C1 1.958(14) . ? Mo1 C8 2.233(15) . ? Mo1 C9 2.286(14) . ? Mo1 C20 2.306(14) . ? Mo1 C19 2.315(14) . ? Mo1 C16 2.338(14) . ? Mo1 P1 2.351(4) . ? Mo1 C17 2.360(13) . ? Mo1 C18 2.368(13) . ? Mo1 Fe1 2.714(2) . ? Mo1 Fe2 2.715(2) . ? Fe1 C2 1.753(16) . ? Fe1 C4 1.789(16) . ? Fe1 C3 1.826(14) . ? Fe1 P1 2.248(4) . ? Fe1 Fe2 2.680(3) . ? Fe2 C7 1.775(16) . ? Fe2 C6 1.785(17) . ? Fe2 C5 1.816(15) . ? Fe2 C9 1.971(13) . ? Fe2 C4 2.448(15) . ? Cl1 C33 1.59(2) . ? Cl2 C33 1.76(3) . ? P1 C32 1.803(14) . ? P1 C21 1.830(13) . ? O1 C1 1.159(16) . ? O2 C2 1.134(17) . ? O3 C3 1.111(16) . ? O4 C4 1.161(17) . ? O5 C5 1.153(17) . ? O6 C6 1.128(18) . ? O7 C7 1.120(17) . ? C8 C9 1.352(19) . ? C8 H8 0.9500 . ? C9 C10 1.503(17) . ? C10 C11 1.378(18) . ? C10 C15 1.416(19) . ? C11 C12 1.378(19) . ? C11 H11 0.9500 . ? C12 C13 1.36(2) . ? C12 H12 0.9500 . ? C13 C14 1.38(2) . ? C13 H13 0.9500 . ? C14 C15 1.384(19) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C20 1.396(19) . ? C16 C17 1.40(2) . ? C16 H16 0.9500 . ? C17 C18 1.41(2) . ? C17 H17 0.9500 . ? C18 C19 1.43(2) . ? C18 H18 0.9500 . ? C19 C20 1.41(2) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C26 1.332(19) . ? C21 C22 1.402(18) . ? C22 C23 1.37(2) . ? C22 H22 0.9500 . ? C23 C24 1.36(2) . ? C23 H23 0.9500 . ? C24 C25 1.37(2) . ? C24 H24 0.9500 . ? C25 C26 1.40(2) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.39(2) . ? C27 C28 1.42(2) . ? C27 H27 0.9500 . ? C28 C29 1.38(2) . ? C28 H28 0.9500 . ? C29 C30 1.35(2) . ? C29 H29 0.9500 . ? C30 C31 1.37(2) . ? C30 H30 0.9500 . ? C31 C32 1.390(19) . ? C31 H31 0.9500 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? 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 C1 Mo1 C8 122.6(5) . . ? C1 Mo1 C9 118.6(5) . . ? C8 Mo1 C9 34.8(5) . . ? C1 Mo1 C20 84.4(5) . . ? C8 Mo1 C20 144.5(5) . . ? C9 Mo1 C20 114.6(5) . . ? C1 Mo1 C19 117.7(5) . . ? C8 Mo1 C19 109.7(5) . . ? C9 Mo1 C19 86.3(5) . . ? C20 Mo1 C19 35.7(5) . . ? C1 Mo1 C16 82.4(5) . . ? C8 Mo1 C16 153.1(5) . . ? C9 Mo1 C16 145.0(5) . . ? C20 Mo1 C16 35.0(5) . . ? C19 Mo1 C16 58.7(5) . . ? C1 Mo1 P1 86.5(4) . . ? C8 Mo1 P1 73.2(4) . . ? C9 Mo1 P1 107.4(3) . . ? C20 Mo1 P1 136.2(4) . . ? C19 Mo1 P1 142.9(4) . . ? C16 Mo1 P1 101.3(4) . . ? C1 Mo1 C17 113.1(5) . . ? C8 Mo1 C17 118.6(5) . . ? C9 Mo1 C17 126.8(5) . . ? C20 Mo1 C17 57.9(5) . . ? C19 Mo1 C17 58.3(5) . . ? C16 Mo1 C17 34.7(5) . . ? P1 Mo1 C17 87.2(4) . . ? C1 Mo1 C18 139.8(5) . . ? C8 Mo1 C18 97.6(5) . . ? C9 Mo1 C18 93.3(5) . . ? C20 Mo1 C18 58.9(5) . . ? C19 Mo1 C18 35.5(5) . . ? C16 Mo1 C18 58.4(5) . . ? P1 Mo1 C18 108.0(4) . . ? C17 Mo1 C18 34.8(5) . . ? C1 Mo1 Fe1 78.9(4) . . ? C8 Mo1 Fe1 46.2(3) . . ? C9 Mo1 Fe1 67.0(3) . . ? C20 Mo1 Fe1 161.0(4) . . ? C19 Mo1 Fe1 153.2(4) . . ? C16 Mo1 Fe1 148.0(4) . . ? P1 Mo1 Fe1 52.10(10) . . ? C17 Mo1 Fe1 137.8(4) . . ? C18 Mo1 Fe1 139.7(4) . . ? C1 Mo1 Fe2 73.4(4) . . ? C8 Mo1 Fe2 65.7(3) . . ? C9 Mo1 Fe2 45.4(3) . . ? C20 Mo1 Fe2 107.4(4) . . ? C19 Mo1 Fe2 103.3(4) . . ? C16 Mo1 Fe2 137.8(4) . . ? P1 Mo1 Fe2 110.80(10) . . ? C17 Mo1 Fe2 161.5(4) . . ? C18 Mo1 Fe2 129.9(3) . . ? Fe1 Mo1 Fe2 59.17(6) . . ? C2 Fe1 C4 89.3(7) . . ? C2 Fe1 C3 103.6(6) . . ? C4 Fe1 C3 91.7(6) . . ? C2 Fe1 P1 89.2(5) . . ? C4 Fe1 P1 171.9(4) . . ? C3 Fe1 P1 96.4(4) . . ? C2 Fe1 Fe2 145.5(5) . . ? C4 Fe1 Fe2 62.8(5) . . ? C3 Fe1 Fe2 97.3(4) . . ? P1 Fe1 Fe2 115.55(13) . . ? C2 Fe1 Mo1 133.1(4) . . ? C4 Fe1 Mo1 121.0(5) . . ? C3 Fe1 Mo1 109.7(5) . . ? P1 Fe1 Mo1 55.62(10) . . ? Fe2 Fe1 Mo1 60.44(6) . . ? C7 Fe2 C6 96.4(6) . . ? C7 Fe2 C5 91.0(7) . . ? C6 Fe2 C5 98.4(6) . . ? C7 Fe2 C9 95.1(6) . . ? C6 Fe2 C9 94.8(6) . . ? C5 Fe2 C9 164.8(6) . . ? C7 Fe2 C4 173.4(6) . . ? C6 Fe2 C4 77.2(6) . . ? C5 Fe2 C4 91.4(6) . . ? C9 Fe2 C4 84.1(5) . . ? C7 Fe2 Fe1 145.2(4) . . ? C6 Fe2 Fe1 116.2(5) . . ? C5 Fe2 Fe1 95.6(5) . . ? C9 Fe2 Fe1 71.6(4) . . ? C4 Fe2 Fe1 40.5(4) . . ? C7 Fe2 Mo1 85.4(4) . . ? C6 Fe2 Mo1 150.4(4) . . ? C5 Fe2 Mo1 111.1(5) . . ? C9 Fe2 Mo1 55.7(4) . . ? C4 Fe2 Mo1 99.5(4) . . ? Fe1 Fe2 Mo1 60.39(6) . . ? C32 P1 C21 102.7(7) . . ? C32 P1 Fe1 118.3(5) . . ? C21 P1 Fe1 115.6(4) . . ? C32 P1 Mo1 123.0(5) . . ? C21 P1 Mo1 123.4(5) . . ? Fe1 P1 Mo1 72.28(12) . . ? O1 C1 Mo1 172.4(12) . . ? O2 C2 Fe1 178.9(11) . . ? O3 C3 Fe1 177.0(13) . . ? O4 C4 Fe1 160.0(13) . . ? O4 C4 Fe2 123.0(11) . . ? Fe1 C4 Fe2 76.7(6) . . ? O5 C5 Fe2 178.1(14) . . ? O6 C6 Fe2 177.1(14) . . ? O7 C7 Fe2 178.4(13) . . ? C9 C8 Mo1 74.7(9) . . ? C9 C8 H8 142.6 . . ? Mo1 C8 H8 142.6 . . ? C8 C9 C10 121.6(12) . . ? C8 C9 Fe2 108.0(9) . . ? C10 C9 Fe2 129.4(10) . . ? C8 C9 Mo1 70.5(9) . . ? C10 C9 Mo1 124.7(8) . . ? Fe2 C9 Mo1 78.9(5) . . ? C11 C10 C15 116.4(13) . . ? C11 C10 C9 121.4(12) . . ? C15 C10 C9 122.1(12) . . ? C12 C11 C10 120.8(14) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C13 C12 C11 122.6(13) . . ? C13 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? C12 C13 C14 118.5(13) . . ? C12 C13 H13 120.7 . . ? C14 C13 H13 120.7 . . ? C13 C14 C15 119.6(15) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C14 C15 C10 122.1(13) . . ? C14 C15 H15 118.9 . . ? C10 C15 H15 118.9 . . ? C20 C16 C17 107.9(13) . . ? C20 C16 Mo1 71.2(8) . . ? C17 C16 Mo1 73.5(8) . . ? C20 C16 H16 126.1 . . ? C17 C16 H16 126.1 . . ? Mo1 C16 H16 121.0 . . ? C16 C17 C18 109.4(13) . . ? C16 C17 Mo1 71.8(8) . . ? C18 C17 Mo1 72.9(8) . . ? C16 C17 H17 125.3 . . ? C18 C17 H17 125.3 . . ? Mo1 C17 H17 121.6 . . ? C17 C18 C19 106.4(13) . . ? C17 C18 Mo1 72.3(8) . . ? C19 C18 Mo1 70.2(8) . . ? C17 C18 H18 126.8 . . ? C19 C18 H18 126.8 . . ? Mo1 C18 H18 122.5 . . ? C20 C19 C18 107.8(13) . . ? C20 C19 Mo1 71.8(8) . . ? C18 C19 Mo1 74.3(8) . . ? C20 C19 H19 126.1 . . ? C18 C19 H19 126.1 . . ? Mo1 C19 H19 119.6 . . ? C16 C20 C19 108.5(13) . . ? C16 C20 Mo1 73.8(8) . . ? C19 C20 Mo1 72.5(8) . . ? C16 C20 H20 125.7 . . ? C19 C20 H20 125.7 . . ? Mo1 C20 H20 119.8 . . ? C26 C21 C22 119.3(13) . . ? C26 C21 P1 120.1(10) . . ? C22 C21 P1 120.6(11) . . ? C23 C22 C21 119.1(14) . . ? C23 C22 H22 120.5 . . ? C21 C22 H22 120.5 . . ? C24 C23 C22 121.3(14) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C23 C24 C25 119.8(15) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C24 C25 C26 118.9(16) . . ? C24 C25 H25 120.6 . . ? C26 C25 H25 120.6 . . ? C21 C26 C25 121.7(14) . . ? C21 C26 H26 119.2 . . ? C25 C26 H26 119.2 . . ? C32 C27 C28 121.1(13) . . ? C32 C27 H27 119.5 . . ? C28 C27 H27 119.5 . . ? C29 C28 C27 119.5(14) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C30 C29 C28 119.1(14) . . ? C30 C29 H29 120.5 . . ? C28 C29 H29 120.5 . . ? C29 C30 C31 121.9(13) . . ? C29 C30 H30 119.0 . . ? C31 C30 H30 119.0 . . ? C30 C31 C32 121.7(14) . . ? C30 C31 H31 119.1 . . ? C32 C31 H31 119.1 . . ? C27 C32 C31 116.6(13) . . ? C27 C32 P1 121.0(10) . . ? C31 C32 P1 122.3(12) . . ? Cl1 C33 Cl2 117.0(18) . . ? Cl1 C33 H33A 108.0 . . ? Cl2 C33 H33A 108.0 . . ? Cl1 C33 H33B 108.0 . . ? Cl2 C33 H33B 108.0 . . ? H33A C33 H33B 107.3 . . ? 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 C1 Mo1 Fe1 C2 -142.7(8) . . . . ? C8 Mo1 Fe1 C2 55.4(8) . . . . ? C9 Mo1 Fe1 C2 89.4(7) . . . . ? C20 Mo1 Fe1 C2 -171.7(13) . . . . ? C19 Mo1 Fe1 C2 86.0(10) . . . . ? C16 Mo1 Fe1 C2 -87.5(9) . . . . ? P1 Mo1 Fe1 C2 -48.5(7) . . . . ? C17 Mo1 Fe1 C2 -30.5(9) . . . . ? C18 Mo1 Fe1 C2 23.3(9) . . . . ? Fe2 Mo1 Fe1 C2 140.1(7) . . . . ? C1 Mo1 Fe1 C4 94.5(7) . . . . ? C8 Mo1 Fe1 C4 -67.4(7) . . . . ? C9 Mo1 Fe1 C4 -33.3(6) . . . . ? C20 Mo1 Fe1 C4 65.6(12) . . . . ? C19 Mo1 Fe1 C4 -36.7(9) . . . . ? C16 Mo1 Fe1 C4 149.7(8) . . . . ? P1 Mo1 Fe1 C4 -171.3(5) . . . . ? C17 Mo1 Fe1 C4 -153.3(7) . . . . ? C18 Mo1 Fe1 C4 -99.5(8) . . . . ? Fe2 Mo1 Fe1 C4 17.3(5) . . . . ? C1 Mo1 Fe1 C3 -10.1(6) . . . . ? C8 Mo1 Fe1 C3 -172.0(6) . . . . ? C9 Mo1 Fe1 C3 -137.9(6) . . . . ? C20 Mo1 Fe1 C3 -39.0(12) . . . . ? C19 Mo1 Fe1 C3 -141.3(9) . . . . ? C16 Mo1 Fe1 C3 45.1(8) . . . . ? P1 Mo1 Fe1 C3 84.1(5) . . . . ? C17 Mo1 Fe1 C3 102.1(7) . . . . ? C18 Mo1 Fe1 C3 155.9(7) . . . . ? Fe2 Mo1 Fe1 C3 -87.3(4) . . . . ? C1 Mo1 Fe1 P1 -94.3(4) . . . . ? C8 Mo1 Fe1 P1 103.9(5) . . . . ? C9 Mo1 Fe1 P1 137.9(4) . . . . ? C20 Mo1 Fe1 P1 -123.2(11) . . . . ? C19 Mo1 Fe1 P1 134.5(8) . . . . ? C16 Mo1 Fe1 P1 -39.1(7) . . . . ? C17 Mo1 Fe1 P1 17.9(5) . . . . ? C18 Mo1 Fe1 P1 71.8(5) . . . . ? Fe2 Mo1 Fe1 P1 -171.44(13) . . . . ? C1 Mo1 Fe1 Fe2 77.2(4) . . . . ? C8 Mo1 Fe1 Fe2 -84.7(5) . . . . ? C9 Mo1 Fe1 Fe2 -50.6(4) . . . . ? C20 Mo1 Fe1 Fe2 48.3(11) . . . . ? C19 Mo1 Fe1 Fe2 -54.0(8) . . . . ? C16 Mo1 Fe1 Fe2 132.4(7) . . . . ? P1 Mo1 Fe1 Fe2 171.44(13) . . . . ? C17 Mo1 Fe1 Fe2 -170.6(5) . . . . ? C18 Mo1 Fe1 Fe2 -116.8(5) . . . . ? C2 Fe1 Fe2 C7 -135.3(11) . . . . ? C4 Fe1 Fe2 C7 -174.5(9) . . . . ? C3 Fe1 Fe2 C7 97.4(9) . . . . ? P1 Fe1 Fe2 C7 -3.3(8) . . . . ? Mo1 Fe1 Fe2 C7 -11.1(8) . . . . ? C2 Fe1 Fe2 C6 22.5(8) . . . . ? C4 Fe1 Fe2 C6 -16.7(7) . . . . ? C3 Fe1 Fe2 C6 -104.8(6) . . . . ? P1 Fe1 Fe2 C6 154.4(5) . . . . ? Mo1 Fe1 Fe2 C6 146.6(5) . . . . ? C2 Fe1 Fe2 C5 124.8(8) . . . . ? C4 Fe1 Fe2 C5 85.6(7) . . . . ? C3 Fe1 Fe2 C5 -2.6(6) . . . . ? P1 Fe1 Fe2 C5 -103.3(5) . . . . ? Mo1 Fe1 Fe2 C5 -111.1(5) . . . . ? C2 Fe1 Fe2 C9 -63.7(8) . . . . ? C4 Fe1 Fe2 C9 -102.9(6) . . . . ? C3 Fe1 Fe2 C9 169.0(6) . . . . ? P1 Fe1 Fe2 C9 68.2(4) . . . . ? Mo1 Fe1 Fe2 C9 60.4(4) . . . . ? C2 Fe1 Fe2 C4 39.2(8) . . . . ? C3 Fe1 Fe2 C4 -88.1(7) . . . . ? P1 Fe1 Fe2 C4 171.2(5) . . . . ? Mo1 Fe1 Fe2 C4 163.3(5) . . . . ? C2 Fe1 Fe2 Mo1 -124.1(7) . . . . ? C4 Fe1 Fe2 Mo1 -163.3(5) . . . . ? C3 Fe1 Fe2 Mo1 108.5(5) . . . . ? P1 Fe1 Fe2 Mo1 7.83(12) . . . . ? C1 Mo1 Fe2 C7 86.9(6) . . . . ? C8 Mo1 Fe2 C7 -134.3(6) . . . . ? C9 Mo1 Fe2 C7 -99.3(7) . . . . ? C20 Mo1 Fe2 C7 8.4(6) . . . . ? C19 Mo1 Fe2 C7 -28.4(6) . . . . ? C16 Mo1 Fe2 C7 29.4(7) . . . . ? P1 Mo1 Fe2 C7 166.4(5) . . . . ? C17 Mo1 Fe2 C7 -26.5(13) . . . . ? C18 Mo1 Fe2 C7 -55.2(7) . . . . ? Fe1 Mo1 Fe2 C7 173.6(5) . . . . ? C1 Mo1 Fe2 C6 -178.4(10) . . . . ? C8 Mo1 Fe2 C6 -39.6(10) . . . . ? C9 Mo1 Fe2 C6 -4.7(10) . . . . ? C20 Mo1 Fe2 C6 103.1(10) . . . . ? C19 Mo1 Fe2 C6 66.3(10) . . . . ? C16 Mo1 Fe2 C6 124.0(11) . . . . ? P1 Mo1 Fe2 C6 -98.9(9) . . . . ? C17 Mo1 Fe2 C6 68.1(15) . . . . ? C18 Mo1 Fe2 C6 39.5(10) . . . . ? Fe1 Mo1 Fe2 C6 -91.7(9) . . . . ? C1 Mo1 Fe2 C5 -2.4(7) . . . . ? C8 Mo1 Fe2 C5 136.4(6) . . . . ? C9 Mo1 Fe2 C5 171.4(7) . . . . ? C20 Mo1 Fe2 C5 -80.9(6) . . . . ? C19 Mo1 Fe2 C5 -117.7(6) . . . . ? C16 Mo1 Fe2 C5 -59.9(7) . . . . ? P1 Mo1 Fe2 C5 77.1(5) . . . . ? C17 Mo1 Fe2 C5 -115.8(13) . . . . ? C18 Mo1 Fe2 C5 -144.5(7) . . . . ? Fe1 Mo1 Fe2 C5 84.4(5) . . . . ? C1 Mo1 Fe2 C9 -173.8(6) . . . . ? C8 Mo1 Fe2 C9 -34.9(6) . . . . ? C20 Mo1 Fe2 C9 107.7(6) . . . . ? C19 Mo1 Fe2 C9 71.0(6) . . . . ? C16 Mo1 Fe2 C9 128.7(7) . . . . ? P1 Mo1 Fe2 C9 -94.2(5) . . . . ? C17 Mo1 Fe2 C9 72.8(12) . . . . ? C18 Mo1 Fe2 C9 44.1(7) . . . . ? Fe1 Mo1 Fe2 C9 -87.0(5) . . . . ? C1 Mo1 Fe2 C4 -97.6(5) . . . . ? C8 Mo1 Fe2 C4 41.2(5) . . . . ? C9 Mo1 Fe2 C4 76.1(6) . . . . ? C20 Mo1 Fe2 C4 -176.1(5) . . . . ? C19 Mo1 Fe2 C4 147.1(5) . . . . ? C16 Mo1 Fe2 C4 -155.2(6) . . . . ? P1 Mo1 Fe2 C4 -18.1(4) . . . . ? C17 Mo1 Fe2 C4 148.9(12) . . . . ? C18 Mo1 Fe2 C4 120.2(6) . . . . ? Fe1 Mo1 Fe2 C4 -10.9(3) . . . . ? C1 Mo1 Fe2 Fe1 -86.7(4) . . . . ? C8 Mo1 Fe2 Fe1 52.1(4) . . . . ? C9 Mo1 Fe2 Fe1 87.0(5) . . . . ? C20 Mo1 Fe2 Fe1 -165.3(4) . . . . ? C19 Mo1 Fe2 Fe1 158.0(4) . . . . ? C16 Mo1 Fe2 Fe1 -144.3(5) . . . . ? P1 Mo1 Fe2 Fe1 -7.22(11) . . . . ? C17 Mo1 Fe2 Fe1 159.8(12) . . . . ? C18 Mo1 Fe2 Fe1 131.1(5) . . . . ? C2 Fe1 P1 C32 28.3(7) . . . . ? C4 Fe1 P1 C32 -51(4) . . . . ? C3 Fe1 P1 C32 131.9(7) . . . . ? Fe2 Fe1 P1 C32 -126.8(5) . . . . ? Mo1 Fe1 P1 C32 -118.6(6) . . . . ? C2 Fe1 P1 C21 -94.0(6) . . . . ? C4 Fe1 P1 C21 -173(4) . . . . ? C3 Fe1 P1 C21 9.6(7) . . . . ? Fe2 Fe1 P1 C21 110.9(5) . . . . ? Mo1 Fe1 P1 C21 119.2(5) . . . . ? C2 Fe1 P1 Mo1 146.8(4) . . . . ? C4 Fe1 P1 Mo1 68(4) . . . . ? C3 Fe1 P1 Mo1 -109.6(5) . . . . ? Fe2 Fe1 P1 Mo1 -8.25(12) . . . . ? C1 Mo1 P1 C32 -168.7(7) . . . . ? C8 Mo1 P1 C32 65.6(7) . . . . ? C9 Mo1 P1 C32 72.4(7) . . . . ? C20 Mo1 P1 C32 -90.5(8) . . . . ? C19 Mo1 P1 C32 -35.1(9) . . . . ? C16 Mo1 P1 C32 -87.3(7) . . . . ? C17 Mo1 P1 C32 -55.4(7) . . . . ? C18 Mo1 P1 C32 -27.1(7) . . . . ? Fe1 Mo1 P1 C32 112.7(6) . . . . ? Fe2 Mo1 P1 C32 120.5(6) . . . . ? C1 Mo1 P1 C21 -30.8(6) . . . . ? C8 Mo1 P1 C21 -156.5(6) . . . . ? C9 Mo1 P1 C21 -149.6(6) . . . . ? C20 Mo1 P1 C21 47.4(7) . . . . ? C19 Mo1 P1 C21 102.8(8) . . . . ? C16 Mo1 P1 C21 50.7(6) . . . . ? C17 Mo1 P1 C21 82.5(6) . . . . ? C18 Mo1 P1 C21 110.9(6) . . . . ? Fe1 Mo1 P1 C21 -109.4(5) . . . . ? Fe2 Mo1 P1 C21 -101.5(5) . . . . ? C1 Mo1 P1 Fe1 78.6(4) . . . . ? C8 Mo1 P1 Fe1 -47.1(3) . . . . ? C9 Mo1 P1 Fe1 -40.2(3) . . . . ? C20 Mo1 P1 Fe1 156.8(5) . . . . ? C19 Mo1 P1 Fe1 -147.8(6) . . . . ? C16 Mo1 P1 Fe1 160.1(4) . . . . ? C17 Mo1 P1 Fe1 -168.1(4) . . . . ? C18 Mo1 P1 Fe1 -139.7(4) . . . . ? Fe2 Mo1 P1 Fe1 7.86(12) . . . . ? C8 Mo1 C1 O1 150(9) . . . . ? C9 Mo1 C1 O1 -169(9) . . . . ? C20 Mo1 C1 O1 -54(9) . . . . ? C19 Mo1 C1 O1 -68(9) . . . . ? C16 Mo1 C1 O1 -19(9) . . . . ? P1 Mo1 C1 O1 83(9) . . . . ? C17 Mo1 C1 O1 -3(9) . . . . ? C18 Mo1 C1 O1 -31(9) . . . . ? Fe1 Mo1 C1 O1 135(9) . . . . ? Fe2 Mo1 C1 O1 -164(9) . . . . ? C4 Fe1 C2 O2 123(69) . . . . ? C3 Fe1 C2 O2 -146(69) . . . . ? P1 Fe1 C2 O2 -49(69) . . . . ? Fe2 Fe1 C2 O2 89(69) . . . . ? Mo1 Fe1 C2 O2 -11(69) . . . . ? C2 Fe1 C3 O3 -147(24) . . . . ? C4 Fe1 C3 O3 -58(24) . . . . ? P1 Fe1 C3 O3 122(24) . . . . ? Fe2 Fe1 C3 O3 5(24) . . . . ? Mo1 Fe1 C3 O3 66(24) . . . . ? C2 Fe1 C4 O4 13(3) . . . . ? C3 Fe1 C4 O4 -91(3) . . . . ? P1 Fe1 C4 O4 92(5) . . . . ? Fe2 Fe1 C4 O4 172(4) . . . . ? Mo1 Fe1 C4 O4 155(3) . . . . ? C2 Fe1 C4 Fe2 -159.0(5) . . . . ? C3 Fe1 C4 Fe2 97.4(5) . . . . ? P1 Fe1 C4 Fe2 -80(4) . . . . ? Mo1 Fe1 C4 Fe2 -16.9(5) . . . . ? C7 Fe2 C4 O4 -25(5) . . . . ? C6 Fe2 C4 O4 -11.9(12) . . . . ? C5 Fe2 C4 O4 86.4(12) . . . . ? C9 Fe2 C4 O4 -108.2(12) . . . . ? Fe1 Fe2 C4 O4 -176.6(15) . . . . ? Mo1 Fe2 C4 O4 -161.9(11) . . . . ? C7 Fe2 C4 Fe1 152(4) . . . . ? C6 Fe2 C4 Fe1 164.7(6) . . . . ? C5 Fe2 C4 Fe1 -97.0(6) . . . . ? C9 Fe2 C4 Fe1 68.4(5) . . . . ? Mo1 Fe2 C4 Fe1 14.7(4) . . . . ? C7 Fe2 C5 O5 -9(38) . . . . ? C6 Fe2 C5 O5 -105(38) . . . . ? C9 Fe2 C5 O5 105(37) . . . . ? C4 Fe2 C5 O5 177(100) . . . . ? Fe1 Fe2 C5 O5 137(38) . . . . ? Mo1 Fe2 C5 O5 77(38) . . . . ? C7 Fe2 C6 O6 -8(25) . . . . ? C5 Fe2 C6 O6 84(25) . . . . ? C9 Fe2 C6 O6 -104(25) . . . . ? C4 Fe2 C6 O6 173(25) . . . . ? Fe1 Fe2 C6 O6 -176(25) . . . . ? Mo1 Fe2 C6 O6 -100(25) . . . . ? C6 Fe2 C7 O7 107(48) . . . . ? C5 Fe2 C7 O7 8(48) . . . . ? C9 Fe2 C7 O7 -158(48) . . . . ? C4 Fe2 C7 O7 120(47) . . . . ? Fe1 Fe2 C7 O7 -93(48) . . . . ? Mo1 Fe2 C7 O7 -103(48) . . . . ? C1 Mo1 C8 C9 94.2(8) . . . . ? C20 Mo1 C8 C9 -40.3(12) . . . . ? C19 Mo1 C8 C9 -50.4(8) . . . . ? C16 Mo1 C8 C9 -109.6(11) . . . . ? P1 Mo1 C8 C9 168.6(8) . . . . ? C17 Mo1 C8 C9 -114.3(8) . . . . ? C18 Mo1 C8 C9 -84.9(8) . . . . ? Fe1 Mo1 C8 C9 115.4(8) . . . . ? Fe2 Mo1 C8 C9 45.7(6) . . . . ? Mo1 C8 C9 C10 119.4(12) . . . . ? Mo1 C8 C9 Fe2 -70.7(7) . . . . ? C7 Fe2 C9 C8 145.9(11) . . . . ? C6 Fe2 C9 C8 -117.3(11) . . . . ? C5 Fe2 C9 C8 33(3) . . . . ? C4 Fe2 C9 C8 -40.7(10) . . . . ? Fe1 Fe2 C9 C8 -1.2(9) . . . . ? Mo1 Fe2 C9 C8 65.0(9) . . . . ? C7 Fe2 C9 C10 -45.3(13) . . . . ? C6 Fe2 C9 C10 51.6(13) . . . . ? C5 Fe2 C9 C10 -158(2) . . . . ? C4 Fe2 C9 C10 128.1(13) . . . . ? Fe1 Fe2 C9 C10 167.6(13) . . . . ? Mo1 Fe2 C9 C10 -126.1(13) . . . . ? C7 Fe2 C9 Mo1 80.9(5) . . . . ? C6 Fe2 C9 Mo1 177.7(5) . . . . ? C5 Fe2 C9 Mo1 -32(2) . . . . ? C4 Fe2 C9 Mo1 -105.8(5) . . . . ? Fe1 Fe2 C9 Mo1 -66.2(2) . . . . ? C1 Mo1 C9 C8 -107.0(8) . . . . ? C20 Mo1 C9 C8 155.6(7) . . . . ? C19 Mo1 C9 C8 133.3(8) . . . . ? C16 Mo1 C9 C8 132.1(9) . . . . ? P1 Mo1 C9 C8 -11.5(8) . . . . ? C17 Mo1 C9 C8 88.3(9) . . . . ? C18 Mo1 C9 C8 98.5(8) . . . . ? Fe1 Mo1 C9 C8 -45.1(7) . . . . ? Fe2 Mo1 C9 C8 -113.9(8) . . . . ? C1 Mo1 C9 C10 137.4(11) . . . . ? C8 Mo1 C9 C10 -115.6(14) . . . . ? C20 Mo1 C9 C10 40.1(12) . . . . ? C19 Mo1 C9 C10 17.8(11) . . . . ? C16 Mo1 C9 C10 16.5(16) . . . . ? P1 Mo1 C9 C10 -127.0(10) . . . . ? C17 Mo1 C9 C10 -27.2(13) . . . . ? C18 Mo1 C9 C10 -17.1(11) . . . . ? Fe1 Mo1 C9 C10 -160.7(12) . . . . ? Fe2 Mo1 C9 C10 130.6(13) . . . . ? C1 Mo1 C9 Fe2 6.8(7) . . . . ? C8 Mo1 C9 Fe2 113.9(8) . . . . ? C20 Mo1 C9 Fe2 -90.5(5) . . . . ? C19 Mo1 C9 Fe2 -112.8(5) . . . . ? C16 Mo1 C9 Fe2 -114.1(7) . . . . ? P1 Mo1 C9 Fe2 102.4(3) . . . . ? C17 Mo1 C9 Fe2 -157.8(5) . . . . ? C18 Mo1 C9 Fe2 -147.6(5) . . . . ? Fe1 Mo1 C9 Fe2 68.7(3) . . . . ? C8 C9 C10 C11 -12(2) . . . . ? Fe2 C9 C10 C11 -179.2(11) . . . . ? Mo1 C9 C10 C11 75.4(16) . . . . ? C8 C9 C10 C15 164.3(14) . . . . ? Fe2 C9 C10 C15 -3(2) . . . . ? Mo1 C9 C10 C15 -108.5(14) . . . . ? C15 C10 C11 C12 0(2) . . . . ? C9 C10 C11 C12 176.4(13) . . . . ? C10 C11 C12 C13 -1(2) . . . . ? C11 C12 C13 C14 1(2) . . . . ? C12 C13 C14 C15 0(2) . . . . ? C13 C14 C15 C10 -1(2) . . . . ? C11 C10 C15 C14 1(2) . . . . ? C9 C10 C15 C14 -175.5(14) . . . . ? C1 Mo1 C16 C20 -91.2(9) . . . . ? C8 Mo1 C16 C20 108.8(12) . . . . ? C9 Mo1 C16 C20 39.3(13) . . . . ? C19 Mo1 C16 C20 37.8(8) . . . . ? P1 Mo1 C16 C20 -176.1(8) . . . . ? C17 Mo1 C16 C20 116.0(13) . . . . ? C18 Mo1 C16 C20 79.7(9) . . . . ? Fe1 Mo1 C16 C20 -145.6(7) . . . . ? Fe2 Mo1 C16 C20 -36.5(11) . . . . ? C1 Mo1 C16 C17 152.8(9) . . . . ? C8 Mo1 C16 C17 -7.2(15) . . . . ? C9 Mo1 C16 C17 -76.8(12) . . . . ? C20 Mo1 C16 C17 -116.0(13) . . . . ? C19 Mo1 C16 C17 -78.2(9) . . . . ? P1 Mo1 C16 C17 67.9(8) . . . . ? C18 Mo1 C16 C17 -36.3(8) . . . . ? Fe1 Mo1 C16 C17 98.4(10) . . . . ? Fe2 Mo1 C16 C17 -152.6(7) . . . . ? C20 C16 C17 C18 0.3(16) . . . . ? Mo1 C16 C17 C18 63.7(10) . . . . ? C20 C16 C17 Mo1 -63.4(10) . . . . ? C1 Mo1 C17 C16 -29.5(10) . . . . ? C8 Mo1 C17 C16 176.3(8) . . . . ? C9 Mo1 C17 C16 135.8(8) . . . . ? C20 Mo1 C17 C16 37.4(8) . . . . ? C19 Mo1 C17 C16 79.7(9) . . . . ? P1 Mo1 C17 C16 -114.5(8) . . . . ? C18 Mo1 C17 C16 117.8(13) . . . . ? Fe1 Mo1 C17 C16 -128.6(8) . . . . ? Fe2 Mo1 C17 C16 77.6(15) . . . . ? C1 Mo1 C17 C18 -147.3(9) . . . . ? C8 Mo1 C17 C18 58.5(10) . . . . ? C9 Mo1 C17 C18 18.0(11) . . . . ? C20 Mo1 C17 C18 -80.4(9) . . . . ? C19 Mo1 C17 C18 -38.1(8) . . . . ? C16 Mo1 C17 C18 -117.8(13) . . . . ? P1 Mo1 C17 C18 127.7(8) . . . . ? Fe1 Mo1 C17 C18 113.6(8) . . . . ? Fe2 Mo1 C17 C18 -40.2(17) . . . . ? C16 C17 C18 C19 -0.7(15) . . . . ? Mo1 C17 C18 C19 62.3(9) . . . . ? C16 C17 C18 Mo1 -63.0(10) . . . . ? C1 Mo1 C18 C17 50.3(12) . . . . ? C8 Mo1 C18 C17 -131.0(9) . . . . ? C9 Mo1 C18 C17 -165.7(9) . . . . ? C20 Mo1 C18 C17 77.4(9) . . . . ? C19 Mo1 C18 C17 115.5(13) . . . . ? C16 Mo1 C18 C17 36.2(8) . . . . ? P1 Mo1 C18 C17 -56.2(9) . . . . ? Fe1 Mo1 C18 C17 -108.2(9) . . . . ? Fe2 Mo1 C18 C17 164.6(7) . . . . ? C1 Mo1 C18 C19 -65.2(12) . . . . ? C8 Mo1 C18 C19 113.6(9) . . . . ? C9 Mo1 C18 C19 78.9(9) . . . . ? C20 Mo1 C18 C19 -38.0(8) . . . . ? C16 Mo1 C18 C19 -79.2(9) . . . . ? P1 Mo1 C18 C19 -171.7(8) . . . . ? C17 Mo1 C18 C19 -115.5(13) . . . . ? Fe1 Mo1 C18 C19 136.4(7) . . . . ? Fe2 Mo1 C18 C19 49.1(10) . . . . ? C17 C18 C19 C20 0.8(15) . . . . ? Mo1 C18 C19 C20 64.5(9) . . . . ? C17 C18 C19 Mo1 -63.7(9) . . . . ? C1 Mo1 C19 C20 23.3(10) . . . . ? C8 Mo1 C19 C20 169.9(8) . . . . ? C9 Mo1 C19 C20 143.8(9) . . . . ? C16 Mo1 C19 C20 -37.1(8) . . . . ? P1 Mo1 C19 C20 -102.0(9) . . . . ? C17 Mo1 C19 C20 -78.0(9) . . . . ? C18 Mo1 C19 C20 -115.2(12) . . . . ? Fe1 Mo1 C19 C20 146.9(7) . . . . ? Fe2 Mo1 C19 C20 101.3(8) . . . . ? C1 Mo1 C19 C18 138.6(9) . . . . ? C8 Mo1 C19 C18 -74.8(9) . . . . ? C9 Mo1 C19 C18 -101.0(9) . . . . ? C20 Mo1 C19 C18 115.2(12) . . . . ? C16 Mo1 C19 C18 78.2(9) . . . . ? P1 Mo1 C19 C18 13.2(12) . . . . ? C17 Mo1 C19 C18 37.3(8) . . . . ? Fe1 Mo1 C19 C18 -97.8(10) . . . . ? Fe2 Mo1 C19 C18 -143.4(8) . . . . ? C17 C16 C20 C19 0.2(16) . . . . ? Mo1 C16 C20 C19 -64.7(10) . . . . ? C17 C16 C20 Mo1 64.9(10) . . . . ? C18 C19 C20 C16 -0.6(16) . . . . ? Mo1 C19 C20 C16 65.5(10) . . . . ? C18 C19 C20 Mo1 -66.1(9) . . . . ? C1 Mo1 C20 C16 84.6(9) . . . . ? C8 Mo1 C20 C16 -132.5(9) . . . . ? C9 Mo1 C20 C16 -156.5(8) . . . . ? C19 Mo1 C20 C16 -116.0(12) . . . . ? P1 Mo1 C20 C16 5.6(11) . . . . ? C17 Mo1 C20 C16 -37.1(8) . . . . ? C18 Mo1 C20 C16 -78.2(9) . . . . ? Fe1 Mo1 C20 C16 113.1(11) . . . . ? Fe2 Mo1 C20 C16 155.2(7) . . . . ? C1 Mo1 C20 C19 -159.4(9) . . . . ? C8 Mo1 C20 C19 -16.5(13) . . . . ? C9 Mo1 C20 C19 -40.4(9) . . . . ? C16 Mo1 C20 C19 116.0(12) . . . . ? P1 Mo1 C20 C19 121.6(8) . . . . ? C17 Mo1 C20 C19 78.9(9) . . . . ? C18 Mo1 C20 C19 37.9(8) . . . . ? Fe1 Mo1 C20 C19 -130.9(10) . . . . ? Fe2 Mo1 C20 C19 -88.7(8) . . . . ? C32 P1 C21 C26 97.5(12) . . . . ? Fe1 P1 C21 C26 -132.3(10) . . . . ? Mo1 P1 C21 C26 -47.4(13) . . . . ? C32 P1 C21 C22 -85.3(12) . . . . ? Fe1 P1 C21 C22 44.9(12) . . . . ? Mo1 P1 C21 C22 129.8(10) . . . . ? C26 C21 C22 C23 -1(2) . . . . ? P1 C21 C22 C23 -178.5(10) . . . . ? C21 C22 C23 C24 1(2) . . . . ? C22 C23 C24 C25 0(2) . . . . ? C23 C24 C25 C26 0(2) . . . . ? C22 C21 C26 C25 1(2) . . . . ? P1 C21 C26 C25 178.6(11) . . . . ? C24 C25 C26 C21 -1(2) . . . . ? C32 C27 C28 C29 1(2) . . . . ? C27 C28 C29 C30 -1(2) . . . . ? C28 C29 C30 C31 -1(2) . . . . ? C29 C30 C31 C32 4(2) . . . . ? C28 C27 C32 C31 1(2) . . . . ? C28 C27 C32 P1 -176.0(11) . . . . ? C30 C31 C32 C27 -3(2) . . . . ? C30 C31 C32 P1 173.7(12) . . . . ? C21 P1 C32 C27 35.9(14) . . . . ? Fe1 P1 C32 C27 -92.7(13) . . . . ? Mo1 P1 C32 C27 -179.1(10) . . . . ? C21 P1 C32 C31 -141.0(13) . . . . ? Fe1 P1 C32 C31 90.4(13) . . . . ? Mo1 P1 C32 C31 4.0(16) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.646 _refine_diff_density_min -1.600 _refine_diff_density_rms 0.215