# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Bourissou, Didier' _publ_contact_author_email dbouriss@chimie.ups-tlse.fr _publ_section_title ; A 1,1\^a-ferrocenyl phosphine-borane: synthesis, structure and evaluation in Rh-catalyzed hydroformylation ; loop_ _publ_author_name M.Bebbington S.Bontemps G.Bouhadir M.Hanton R.Tooze ; H.van Rensburg ; D.Bourissou # Attachment '- 2.CIF' data_mag04m _database_code_depnum_ccdc_archive 'CCDC 766316' #TrackingRef '- 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H40 B Fe P' _chemical_formula_weight 618.35 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.2786(11) _cell_length_b 42.999(5) _cell_length_c 9.2730(12) _cell_angle_alpha 90.00 _cell_angle_beta 93.458(3) _cell_angle_gamma 90.00 _cell_volume 3294.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1330 _cell_measurement_theta_min 2.251 _cell_measurement_theta_max 19.740 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 0.533 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.662254 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14541 _diffrn_reflns_av_R_equivalents 0.1484 _diffrn_reflns_av_sigmaI/netI 0.1797 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 47 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 23.26 _reflns_number_total 4681 _reflns_number_gt 2498 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0350P)^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 4681 _refine_ls_number_parameters 394 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1648 _refine_ls_R_factor_gt 0.0756 _refine_ls_wR_factor_ref 0.1269 _refine_ls_wR_factor_gt 0.1057 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.55881(11) 0.085796(18) 0.77198(9) 0.0286(3) Uani 1 1 d . . . P1 P 0.6629(2) 0.07263(3) 1.14332(17) 0.0279(4) Uani 1 1 d . . . B1 B 0.6116(9) 0.16271(15) 0.8245(8) 0.0318(19) Uani 1 1 d . . . C1 C 0.6579(8) 0.06369(12) 0.9519(6) 0.0274(16) Uani 1 1 d . . . C2 C 0.5540(8) 0.04329(12) 0.8676(6) 0.0320(17) Uani 1 1 d . . . H2 H 0.4611 0.0330 0.8997 0.038 Uiso 1 1 calc R . . C3 C 0.6127(8) 0.04099(13) 0.7293(7) 0.0350(17) Uani 1 1 d . . . H3 H 0.5656 0.0291 0.6511 0.042 Uiso 1 1 calc R . . C4 C 0.7546(8) 0.05937(13) 0.7262(7) 0.0326(16) Uani 1 1 d . . . H4 H 0.8197 0.0618 0.6460 0.039 Uiso 1 1 calc R . . C5 C 0.7826(8) 0.07355(12) 0.8634(6) 0.0315(16) Uani 1 1 d . . . H5 H 0.8691 0.0872 0.8912 0.038 Uiso 1 1 calc R . . C6 C 0.5205(7) 0.13374(12) 0.7577(7) 0.0313(16) Uani 1 1 d . . . C7 C 0.3927(7) 0.11754(12) 0.8265(6) 0.0262(15) Uani 1 1 d . . . H7 H 0.3637 0.1211 0.9226 0.031 Uiso 1 1 calc R . . C8 C 0.3188(8) 0.09616(13) 0.7329(7) 0.0356(17) Uani 1 1 d . . . H8 H 0.2296 0.0833 0.7528 0.043 Uiso 1 1 calc R . . C9 C 0.3984(8) 0.09677(12) 0.6028(7) 0.0328(17) Uani 1 1 d . . . H9 H 0.3744 0.0840 0.5205 0.039 Uiso 1 1 calc R . . C10 C 0.5208(8) 0.11979(13) 0.6168(7) 0.0328(17) Uani 1 1 d . . . H10 H 0.5921 0.1252 0.5443 0.039 Uiso 1 1 calc R . . C11 C 0.7278(7) 0.03465(12) 1.2178(6) 0.0264(15) Uani 1 1 d . . . C12 C 0.8067(7) 0.01240(13) 1.1380(7) 0.0304(16) Uani 1 1 d . . . H12 H 0.8187 0.0157 1.0380 0.037 Uiso 1 1 calc R . . C13 C 0.8677(7) -0.01444(13) 1.2031(7) 0.0348(17) Uani 1 1 d . . . H13 H 0.9192 -0.0296 1.1471 0.042 Uiso 1 1 calc R . . C14 C 0.8542(8) -0.01927(13) 1.3467(8) 0.0390(18) Uani 1 1 d . . . H14 H 0.8982 -0.0376 1.3912 0.047 Uiso 1 1 calc R . . C15 C 0.7765(9) 0.00241(14) 1.4281(7) 0.0439(19) Uani 1 1 d . . . H15 H 0.7645 -0.0012 1.5280 0.053 Uiso 1 1 calc R . . C16 C 0.7168(8) 0.02909(14) 1.3641(7) 0.0398(18) Uani 1 1 d . . . H16 H 0.6667 0.0442 1.4215 0.048 Uiso 1 1 calc R . . C17 C 0.4477(7) 0.07357(12) 1.1837(5) 0.0251(15) Uani 1 1 d . . . C18 C 0.3817(8) 0.10273(13) 1.2064(6) 0.0338(16) Uani 1 1 d . . . H18 H 0.4476 0.1208 1.2031 0.041 Uiso 1 1 calc R . . C19 C 0.2209(9) 0.10548(15) 1.2339(7) 0.0427(18) Uani 1 1 d . . . H19 H 0.1759 0.1256 1.2462 0.051 Uiso 1 1 calc R . . C20 C 0.1248(8) 0.07976(17) 1.2436(7) 0.0510(19) Uani 1 1 d . . . H20 H 0.0143 0.0820 1.2640 0.061 Uiso 1 1 calc R . . C21 C 0.1887(9) 0.05055(16) 1.2238(7) 0.049(2) Uani 1 1 d . . . H21 H 0.1227 0.0326 1.2312 0.059 Uiso 1 1 calc R . . C22 C 0.3505(8) 0.04751(14) 1.1929(7) 0.0378(17) Uani 1 1 d . . . H22 H 0.3945 0.0274 1.1779 0.045 Uiso 1 1 calc R . . C23 C 0.5638(8) 0.17210(12) 0.9813(6) 0.0280(16) Uani 1 1 d . . . C24 C 0.6788(8) 0.17084(13) 1.0996(7) 0.0312(16) Uani 1 1 d . . . C25 C 0.6364(8) 0.17685(13) 1.2386(7) 0.0352(17) Uani 1 1 d . . . H25 H 0.7165 0.1756 1.3161 0.042 Uiso 1 1 calc R . . C26 C 0.4778(9) 0.18481(13) 1.2672(7) 0.0339(17) Uani 1 1 d . . . C27 C 0.3642(8) 0.18675(12) 1.1512(7) 0.0338(17) Uani 1 1 d . . . H27 H 0.2563 0.1925 1.1685 0.041 Uiso 1 1 calc R . . C28 C 0.4033(8) 0.18050(12) 1.0104(7) 0.0281(16) Uani 1 1 d . . . C29 C 0.8516(8) 0.16133(14) 1.0778(7) 0.0475(19) Uani 1 1 d . . . H29A H 0.9177 0.1644 1.1680 0.071 Uiso 1 1 calc R . . H29B H 0.8947 0.1741 1.0014 0.071 Uiso 1 1 calc R . . H29C H 0.8545 0.1394 1.0499 0.071 Uiso 1 1 calc R . . C30 C 0.4302(9) 0.19164(15) 1.4190(6) 0.054(2) Uani 1 1 d . . . H30A H 0.3534 0.2090 1.4168 0.081 Uiso 1 1 calc R . . H30B H 0.5269 0.1972 1.4798 0.081 Uiso 1 1 calc R . . H30C H 0.3796 0.1732 1.4587 0.081 Uiso 1 1 calc R . . C31 C 0.2687(8) 0.18407(13) 0.8921(7) 0.0412(18) Uani 1 1 d . . . H31A H 0.1773 0.1707 0.9139 0.062 Uiso 1 1 calc R . . H31B H 0.3091 0.1780 0.7990 0.062 Uiso 1 1 calc R . . H31C H 0.2330 0.2058 0.8875 0.062 Uiso 1 1 calc R . . C32 C 0.7296(8) 0.18311(13) 0.7363(6) 0.0326(16) Uani 1 1 d . . . C33 C 0.8652(8) 0.17100(14) 0.6664(7) 0.0350(17) Uani 1 1 d . . . C34 C 0.9617(8) 0.19023(15) 0.5872(7) 0.0455(19) Uani 1 1 d . . . H34 H 1.0528 0.1816 0.5441 0.055 Uiso 1 1 calc R . . C35 C 0.9287(10) 0.22157(17) 0.5696(8) 0.053(2) Uani 1 1 d . . . C36 C 0.7992(10) 0.23341(15) 0.6364(8) 0.050(2) Uani 1 1 d . . . H36 H 0.7752 0.2549 0.6252 0.060 Uiso 1 1 calc R . . C37 C 0.7018(8) 0.21550(14) 0.7192(7) 0.0398(18) Uani 1 1 d . . . C38 C 0.9195(8) 0.13771(13) 0.6818(7) 0.0474(19) Uani 1 1 d . . . H38A H 0.9500 0.1299 0.5880 0.071 Uiso 1 1 calc R . . H38B H 0.8309 0.1251 0.7158 0.071 Uiso 1 1 calc R . . H38C H 1.0129 0.1365 0.7517 0.071 Uiso 1 1 calc R . . C39 C 1.0342(10) 0.24242(17) 0.4811(10) 0.086(3) Uani 1 1 d . . . H39A H 0.9750 0.2615 0.4545 0.128 Uiso 1 1 calc R . . H39B H 1.0619 0.2314 0.3934 0.128 Uiso 1 1 calc R . . H39C H 1.1337 0.2477 0.5386 0.128 Uiso 1 1 calc R . . C40 C 0.5622(10) 0.23193(13) 0.7828(8) 0.062(2) Uani 1 1 d . . . H40A H 0.5629 0.2539 0.7552 0.093 Uiso 1 1 calc R . . H40B H 0.5724 0.2302 0.8884 0.093 Uiso 1 1 calc R . . H40C H 0.4602 0.2224 0.7463 0.093 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 Fe1 0.0275(6) 0.0236(5) 0.0340(5) -0.0010(5) -0.0025(4) 0.0021(5) P1 0.0245(10) 0.0223(9) 0.0362(10) 0.0001(8) -0.0041(9) -0.0015(7) B1 0.024(5) 0.030(4) 0.040(5) 0.003(4) -0.005(4) 0.013(3) C1 0.031(4) 0.019(3) 0.031(4) 0.005(3) -0.003(4) 0.006(3) C2 0.038(5) 0.021(4) 0.037(4) 0.000(3) 0.000(4) 0.000(3) C3 0.051(5) 0.022(4) 0.032(4) -0.004(3) -0.006(4) 0.004(3) C4 0.030(4) 0.030(4) 0.038(4) 0.004(3) 0.006(4) 0.012(3) C5 0.037(4) 0.020(3) 0.037(4) -0.002(3) 0.001(4) 0.002(3) C6 0.027(4) 0.027(4) 0.040(4) 0.005(3) 0.003(4) 0.009(3) C7 0.025(4) 0.024(3) 0.030(4) 0.001(3) -0.001(3) 0.003(3) C8 0.023(4) 0.034(4) 0.048(4) -0.008(3) -0.005(4) 0.001(3) C9 0.039(5) 0.027(4) 0.032(4) 0.001(3) -0.008(4) 0.008(3) C10 0.038(5) 0.025(4) 0.035(4) 0.007(3) 0.002(4) 0.005(3) C11 0.018(4) 0.029(4) 0.031(4) -0.005(3) -0.009(3) -0.005(3) C12 0.019(4) 0.034(4) 0.038(4) 0.005(3) -0.001(3) -0.001(3) C13 0.027(4) 0.028(4) 0.048(5) -0.008(3) -0.004(4) 0.004(3) C14 0.041(5) 0.026(4) 0.049(5) -0.002(3) -0.014(4) 0.006(3) C15 0.063(6) 0.035(4) 0.032(4) 0.002(3) -0.009(4) 0.012(4) C16 0.053(5) 0.034(4) 0.031(4) -0.011(3) -0.008(4) 0.012(3) C17 0.034(4) 0.019(3) 0.022(3) 0.003(3) -0.002(3) 0.000(3) C18 0.033(5) 0.027(4) 0.041(4) -0.001(3) -0.001(4) -0.001(3) C19 0.038(5) 0.040(4) 0.051(4) 0.005(4) 0.005(4) 0.012(4) C20 0.017(4) 0.067(6) 0.068(5) 0.016(4) -0.003(4) 0.003(4) C21 0.033(5) 0.049(5) 0.065(5) 0.008(4) -0.002(4) -0.010(4) C22 0.035(5) 0.031(4) 0.046(4) 0.010(3) -0.010(4) -0.001(3) C23 0.035(5) 0.012(3) 0.037(4) -0.002(3) 0.004(4) -0.002(3) C24 0.031(5) 0.023(3) 0.040(4) -0.005(3) -0.001(4) -0.004(3) C25 0.027(5) 0.032(4) 0.045(5) -0.001(3) -0.016(4) -0.006(3) C26 0.046(5) 0.019(3) 0.036(5) -0.003(3) -0.009(4) -0.003(3) C27 0.029(4) 0.022(4) 0.050(5) -0.008(3) 0.001(4) 0.002(3) C28 0.028(4) 0.014(3) 0.041(4) -0.009(3) -0.005(4) 0.009(3) C29 0.030(5) 0.057(5) 0.054(5) 0.005(4) -0.012(4) 0.001(4) C30 0.069(6) 0.049(5) 0.042(5) 0.001(4) 0.000(4) 0.003(4) C31 0.043(5) 0.031(4) 0.049(4) -0.008(3) -0.008(4) 0.011(3) C32 0.035(4) 0.031(4) 0.031(4) 0.003(3) -0.006(4) -0.003(3) C33 0.029(4) 0.034(4) 0.042(4) 0.008(3) -0.003(4) -0.007(3) C34 0.029(4) 0.048(5) 0.060(5) 0.020(4) 0.005(4) -0.005(4) C35 0.044(6) 0.048(5) 0.067(5) 0.022(4) -0.005(5) -0.018(4) C36 0.055(6) 0.029(4) 0.065(5) 0.014(4) -0.011(5) -0.007(4) C37 0.037(5) 0.030(4) 0.052(5) -0.003(3) -0.010(4) -0.006(4) C38 0.030(5) 0.047(4) 0.065(5) 0.010(4) 0.004(4) 0.008(3) C39 0.062(6) 0.070(6) 0.126(8) 0.049(5) 0.008(6) -0.009(5) C40 0.096(7) 0.023(4) 0.066(5) 0.011(4) 0.013(5) 0.022(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 Fe1 C3 2.022(5) . ? Fe1 C7 2.023(6) . ? Fe1 C2 2.033(5) . ? Fe1 C4 2.045(6) . ? Fe1 C8 2.048(6) . ? Fe1 C9 2.048(6) . ? Fe1 C1 2.049(6) . ? Fe1 C5 2.059(6) . ? Fe1 C10 2.062(6) . ? Fe1 C6 2.089(5) . ? P1 C1 1.814(6) . ? P1 C11 1.840(6) . ? P1 C17 1.843(6) . ? B1 C6 1.565(9) . ? B1 C32 1.578(9) . ? B1 C23 1.582(9) . ? C1 C5 1.422(7) . ? C1 C2 1.428(8) . ? C2 C3 1.403(7) . ? C3 C4 1.417(8) . ? C4 C5 1.418(8) . ? C6 C10 1.438(8) . ? C6 C7 1.446(7) . ? C7 C8 1.382(7) . ? C8 C9 1.410(7) . ? C9 C10 1.417(8) . ? C11 C16 1.386(8) . ? C11 C12 1.396(7) . ? C12 C13 1.383(7) . ? C13 C14 1.359(8) . ? C14 C15 1.382(8) . ? C15 C16 1.370(8) . ? C17 C22 1.385(7) . ? C17 C18 1.389(7) . ? C18 C19 1.375(8) . ? C19 C20 1.368(8) . ? C20 C21 1.380(8) . ? C21 C22 1.393(8) . ? C23 C24 1.410(8) . ? C23 C28 1.418(8) . ? C24 C25 1.380(8) . ? C24 C29 1.514(8) . ? C25 C26 1.398(8) . ? C26 C27 1.388(8) . ? C26 C30 1.513(8) . ? C27 C28 1.390(8) . ? C28 C31 1.524(8) . ? C32 C37 1.419(8) . ? C32 C33 1.428(8) . ? C33 C34 1.390(8) . ? C33 C38 1.504(8) . ? C34 C35 1.383(9) . ? C35 C36 1.368(9) . ? C35 C39 1.526(9) . ? C36 C37 1.382(8) . ? C37 C40 1.505(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Fe1 C7 148.6(3) . . ? C3 Fe1 C2 40.5(2) . . ? C7 Fe1 C2 117.8(2) . . ? C3 Fe1 C4 40.8(2) . . ? C7 Fe1 C4 170.4(3) . . ? C2 Fe1 C4 68.1(2) . . ? C3 Fe1 C8 113.3(3) . . ? C7 Fe1 C8 39.7(2) . . ? C2 Fe1 C8 103.2(3) . . ? C4 Fe1 C8 149.0(3) . . ? C3 Fe1 C9 102.1(2) . . ? C7 Fe1 C9 67.5(2) . . ? C2 Fe1 C9 120.8(2) . . ? C4 Fe1 C9 117.0(2) . . ? C8 Fe1 C9 40.3(2) . . ? C3 Fe1 C1 68.6(2) . . ? C7 Fe1 C1 110.8(2) . . ? C2 Fe1 C1 41.0(2) . . ? C4 Fe1 C1 68.2(2) . . ? C8 Fe1 C1 125.6(3) . . ? C9 Fe1 C1 160.1(2) . . ? C3 Fe1 C5 68.5(2) . . ? C7 Fe1 C5 132.7(2) . . ? C2 Fe1 C5 68.4(2) . . ? C4 Fe1 C5 40.4(2) . . ? C8 Fe1 C5 165.5(2) . . ? C9 Fe1 C5 154.1(2) . . ? C1 Fe1 C5 40.5(2) . . ? C3 Fe1 C10 124.4(2) . . ? C7 Fe1 C10 67.6(2) . . ? C2 Fe1 C10 159.3(2) . . ? C4 Fe1 C10 109.8(2) . . ? C8 Fe1 C10 67.4(2) . . ? C9 Fe1 C10 40.3(2) . . ? C1 Fe1 C10 159.1(2) . . ? C5 Fe1 C10 124.4(2) . . ? C3 Fe1 C6 164.2(2) . . ? C7 Fe1 C6 41.1(2) . . ? C2 Fe1 C6 155.2(2) . . ? C4 Fe1 C6 130.9(2) . . ? C8 Fe1 C6 68.4(2) . . ? C9 Fe1 C6 68.6(2) . . ? C1 Fe1 C6 124.2(2) . . ? C5 Fe1 C6 114.1(2) . . ? C10 Fe1 C6 40.5(2) . . ? C1 P1 C11 99.7(3) . . ? C1 P1 C17 103.8(3) . . ? C11 P1 C17 102.0(3) . . ? C6 B1 C32 122.4(5) . . ? C6 B1 C23 115.2(5) . . ? C32 B1 C23 122.1(5) . . ? C5 C1 C2 107.5(5) . . ? C5 C1 P1 121.8(5) . . ? C2 C1 P1 130.0(5) . . ? C5 C1 Fe1 70.1(3) . . ? C2 C1 Fe1 68.9(3) . . ? P1 C1 Fe1 133.1(3) . . ? C3 C2 C1 108.3(6) . . ? C3 C2 Fe1 69.4(3) . . ? C1 C2 Fe1 70.1(3) . . ? C2 C3 C4 108.2(6) . . ? C2 C3 Fe1 70.2(3) . . ? C4 C3 Fe1 70.5(3) . . ? C3 C4 C5 108.2(6) . . ? C3 C4 Fe1 68.8(3) . . ? C5 C4 Fe1 70.3(3) . . ? C4 C5 C1 107.8(5) . . ? C4 C5 Fe1 69.3(4) . . ? C1 C5 Fe1 69.4(3) . . ? C10 C6 C7 104.0(5) . . ? C10 C6 B1 131.7(6) . . ? C7 C6 B1 123.8(5) . . ? C10 C6 Fe1 68.7(3) . . ? C7 C6 Fe1 67.0(3) . . ? B1 C6 Fe1 133.8(4) . . ? C8 C7 C6 110.6(5) . . ? C8 C7 Fe1 71.1(3) . . ? C6 C7 Fe1 71.9(3) . . ? C7 C8 C9 108.2(5) . . ? C7 C8 Fe1 69.2(3) . . ? C9 C8 Fe1 69.9(3) . . ? C8 C9 C10 107.6(5) . . ? C8 C9 Fe1 69.8(3) . . ? C10 C9 Fe1 70.3(4) . . ? C9 C10 C6 109.6(5) . . ? C9 C10 Fe1 69.3(3) . . ? C6 C10 Fe1 70.8(3) . . ? C16 C11 C12 117.4(5) . . ? C16 C11 P1 119.0(4) . . ? C12 C11 P1 123.0(5) . . ? C13 C12 C11 120.7(6) . . ? C14 C13 C12 120.4(6) . . ? C13 C14 C15 120.0(6) . . ? C16 C15 C14 119.7(6) . . ? C15 C16 C11 121.7(6) . . ? C22 C17 C18 119.1(6) . . ? C22 C17 P1 124.5(5) . . ? C18 C17 P1 116.4(4) . . ? C19 C18 C17 120.0(6) . . ? C20 C19 C18 121.1(6) . . ? C19 C20 C21 119.9(6) . . ? C20 C21 C22 119.6(6) . . ? C17 C22 C21 120.4(6) . . ? C24 C23 C28 117.2(5) . . ? C24 C23 B1 120.7(6) . . ? C28 C23 B1 122.0(6) . . ? C25 C24 C23 121.5(6) . . ? C25 C24 C29 118.1(6) . . ? C23 C24 C29 120.4(6) . . ? C24 C25 C26 121.2(6) . . ? C27 C26 C25 117.9(6) . . ? C27 C26 C30 120.5(6) . . ? C25 C26 C30 121.6(6) . . ? C26 C27 C28 122.1(6) . . ? C27 C28 C23 120.1(6) . . ? C27 C28 C31 117.0(5) . . ? C23 C28 C31 122.8(5) . . ? C37 C32 C33 115.8(5) . . ? C37 C32 B1 120.1(6) . . ? C33 C32 B1 124.1(5) . . ? C34 C33 C32 121.0(6) . . ? C34 C33 C38 116.0(6) . . ? C32 C33 C38 122.9(5) . . ? C35 C34 C33 121.8(7) . . ? C36 C35 C34 117.6(6) . . ? C36 C35 C39 121.0(7) . . ? C34 C35 C39 121.4(7) . . ? C35 C36 C37 122.9(6) . . ? C36 C37 C32 120.8(6) . . ? C36 C37 C40 116.4(6) . . ? C32 C37 C40 122.7(6) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.435 _refine_diff_density_min -0.302 _refine_diff_density_rms 0.068