data_k0681twin _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H30 Fe P2 Si' _chemical_formula_sum 'C18 H30 Fe P2 Si' _chemical_formula_weight 392.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 8.4191(6) _cell_length_b 14.3419(13) _cell_length_c 16.2224(11) _cell_angle_alpha 90.00 _cell_angle_beta 94.610(5) _cell_angle_gamma 90.00 _cell_volume 1952.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 3313 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 25.0 _exptl_crystal_description 'needle' _exptl_crystal_colour 'purple' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 0.993 # Absorption correction _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.484 _exptl_absorpt_correction_T_max 0.890 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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-Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3313 _diffrn_reflns_av_R_equivalents 0.162 _diffrn_reflns_av_sigmaI/netI 0.1292 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -2 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3313 _reflns_number_gt 2141 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Collect (Nonius B.V., 1997-2002)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN' _computing_structure_solution 'SIR-92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXTL V6.1(Sheldrick, 2001)' _computing_molecular_graphics 'SHELXTL V6.1' _computing_publication_material 'SHELXTL V6.1' _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^)+(0.1423P)^2^+6.7530P] 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 3313 _refine_ls_number_parameters 206 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1442 _refine_ls_R_factor_gt 0.0884 _refine_ls_wR_factor_ref 0.2716 _refine_ls_wR_factor_gt 0.2261 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.60148(16) 0.31069(9) 0.14363(7) 0.0299(4) Uani 1 1 d . . . P1 P 0.7172(3) 0.18921(17) 0.20212(14) 0.0318(6) Uani 1 1 d . . . P2 P 0.8211(3) 0.38470(17) 0.18194(15) 0.0333(6) Uani 1 1 d . . . Si1 Si 0.3418(3) 0.2329(2) -0.00310(15) 0.0338(7) Uani 1 1 d . . . C1 C 0.3601(11) 0.3044(7) 0.0934(5) 0.035(2) Uani 1 1 d . . . C2 C 0.3766(11) 0.2679(8) 0.1758(6) 0.039(2) Uani 1 1 d . . . H2A H 0.3477 0.2033 0.1924 0.047 Uiso 1 1 calc R . . C3 C 0.4382(12) 0.3402(7) 0.2310(6) 0.040(2) Uani 1 1 d . . . H3A H 0.4579 0.3357 0.2925 0.049 Uiso 1 1 calc R . . C4 C 0.4615(12) 0.4179(7) 0.1826(6) 0.044(3) Uani 1 1 d . . . H4A H 0.5031 0.4793 0.2042 0.052 Uiso 1 1 calc R . . C5 C 0.4140(12) 0.3991(6) 0.0985(6) 0.036(2) Uani 1 1 d . . . H5A H 0.4163 0.4440 0.0515 0.043 Uiso 1 1 calc R . . C6 C 0.2394(12) 0.3016(7) -0.0893(6) 0.042(2) Uani 1 1 d . . . H6A H 0.3026 0.3572 -0.0996 0.062 Uiso 1 1 calc R . . H6B H 0.1338 0.3206 -0.0742 0.062 Uiso 1 1 calc R . . H6C H 0.2281 0.2632 -0.1394 0.062 Uiso 1 1 calc R . . C7 C 0.2367(12) 0.1209(7) 0.0132(7) 0.046(3) Uani 1 1 d . . . H7A H 0.2980 0.0842 0.0556 0.069 Uiso 1 1 calc R . . H7B H 0.2262 0.0857 -0.0387 0.069 Uiso 1 1 calc R . . H7C H 0.1306 0.1338 0.0312 0.069 Uiso 1 1 calc R . . C8 C 0.9331(12) 0.2047(6) 0.2138(6) 0.038(2) Uani 1 1 d . . . H8A H 0.9809 0.1626 0.2574 0.046 Uiso 1 1 calc R . . H8B H 0.9797 0.1898 0.1613 0.046 Uiso 1 1 calc R . . C9 C 0.9671(12) 0.3067(7) 0.2377(6) 0.039(2) Uani 1 1 d . . . H9A H 1.0759 0.3236 0.2241 0.047 Uiso 1 1 calc R . . H9B H 0.9616 0.3145 0.2980 0.047 Uiso 1 1 calc R . . C10 C 0.6954(15) 0.0716(7) 0.1587(6) 0.047(3) Uani 1 1 d . . . H10A H 0.7648 0.0285 0.1917 0.070 Uiso 1 1 calc R . . H10B H 0.7253 0.0720 0.1016 0.070 Uiso 1 1 calc R . . H10C H 0.5843 0.0514 0.1596 0.070 Uiso 1 1 calc R . . C11 C 0.6727(13) 0.1689(7) 0.3095(5) 0.044(3) Uani 1 1 d . . . H11A H 0.7293 0.1131 0.3307 0.066 Uiso 1 1 calc R . . H11B H 0.5577 0.1599 0.3117 0.066 Uiso 1 1 calc R . . H11C H 0.7073 0.2228 0.3434 0.066 Uiso 1 1 calc R . . C12 C 0.8140(13) 0.4797(6) 0.2571(6) 0.041(2) Uani 1 1 d . . . H12A H 0.9220 0.4932 0.2812 0.062 Uiso 1 1 calc R . . H12B H 0.7470 0.4612 0.3010 0.062 Uiso 1 1 calc R . . H12C H 0.7691 0.5355 0.2293 0.062 Uiso 1 1 calc R . . C13 C 0.9406(13) 0.4420(7) 0.1058(6) 0.045(3) Uani 1 1 d . . . H13A H 1.0357 0.4701 0.1346 0.068 Uiso 1 1 calc R . . H13B H 0.8767 0.4907 0.0766 0.068 Uiso 1 1 calc R . . H13C H 0.9728 0.3957 0.0660 0.068 Uiso 1 1 calc R . . C14 C 0.6752(11) 0.2759(7) 0.0171(5) 0.035(2) Uani 1 1 d . . . H14A H 0.6675 0.3345 -0.0164 0.042 Uiso 1 1 calc R . . C15 C 0.8276(12) 0.2330(7) 0.0043(5) 0.038(2) Uani 1 1 d . . . H15 H 0.9297 0.2593 0.0185 0.045 Uiso 1 1 calc R . . C16 C 0.7977(12) 0.1474(7) -0.0319(6) 0.038(2) Uani 1 1 d . . . H16 H 0.8762 0.1043 -0.0468 0.045 Uiso 1 1 calc R . . C17 C 0.6293(12) 0.1340(7) -0.0436(5) 0.035(2) Uani 1 1 d . . . H17 H 0.5783 0.0792 -0.0654 0.042 Uiso 1 1 calc R . . C18 C 0.5521(11) 0.2119(7) -0.0186(5) 0.035(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0369(8) 0.0240(7) 0.0289(7) -0.0016(5) 0.0025(6) 0.0019(6) P1 0.0445(15) 0.0228(13) 0.0277(12) -0.0003(10) 0.0007(11) 0.0009(11) P2 0.0401(15) 0.0233(13) 0.0362(13) -0.0013(10) 0.0020(12) -0.0021(11) Si1 0.0354(15) 0.0321(15) 0.0332(13) -0.0023(11) -0.0013(12) 0.0024(12) C1 0.035(5) 0.041(6) 0.030(5) -0.005(4) 0.005(4) -0.002(5) C2 0.033(5) 0.048(6) 0.036(5) 0.001(5) 0.005(5) 0.011(5) C3 0.046(6) 0.043(6) 0.033(5) -0.006(5) 0.006(5) 0.003(5) C4 0.037(6) 0.042(6) 0.051(6) -0.017(5) 0.000(5) 0.003(5) C5 0.045(6) 0.023(5) 0.039(5) -0.007(4) 0.000(5) 0.010(4) C6 0.043(6) 0.044(6) 0.037(5) -0.003(5) 0.003(5) 0.006(5) C7 0.035(6) 0.047(7) 0.056(6) -0.011(5) 0.001(5) 0.001(5) C8 0.046(6) 0.029(6) 0.040(5) -0.003(4) 0.000(5) 0.006(5) C9 0.036(5) 0.033(6) 0.047(6) 0.002(5) -0.007(5) 0.002(5) C10 0.078(8) 0.027(5) 0.034(5) -0.005(4) 0.003(5) -0.007(5) C11 0.064(7) 0.041(6) 0.026(5) 0.003(4) -0.006(5) -0.004(5) C12 0.055(6) 0.021(5) 0.047(6) -0.006(4) -0.003(5) -0.005(5) C13 0.049(6) 0.034(6) 0.053(6) -0.004(5) 0.003(5) -0.010(5) C14 0.035(5) 0.038(6) 0.031(5) 0.011(4) -0.001(4) -0.004(4) C15 0.042(6) 0.038(6) 0.033(5) 0.007(4) 0.002(5) -0.001(5) C16 0.043(6) 0.037(6) 0.033(5) -0.001(4) 0.006(5) 0.005(5) C17 0.044(6) 0.033(6) 0.028(5) -0.002(4) 0.004(4) -0.006(5) C18 0.037(5) 0.043(6) 0.024(4) 0.002(4) -0.005(4) -0.004(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C4 2.067(10) . ? Fe1 C2 2.095(10) . ? Fe1 C3 2.096(9) . ? Fe1 C5 2.110(10) . ? Fe1 C1 2.130(10) . ? Fe1 P1 2.176(3) . ? Fe1 P2 2.179(3) . ? Fe1 C14 2.249(9) . ? P1 C8 1.826(11) . ? P1 C10 1.831(9) . ? P1 C11 1.834(9) . ? P2 C12 1.832(9) . ? P2 C9 1.844(10) . ? P2 C13 1.847(10) . ? Si1 C18 1.833(10) . ? Si1 C7 1.863(11) . ? Si1 C6 1.864(10) . ? Si1 C1 1.867(9) . ? C1 C5 1.432(13) . ? C1 C2 1.432(13) . ? C2 C3 1.440(14) . ? C3 C4 1.387(14) . ? C4 C5 1.416(13) . ? C8 C9 1.534(13) . ? C14 C15 1.453(14) . ? C14 C18 1.468(13) . ? C15 C16 1.375(14) . ? C16 C17 1.429(14) . ? C17 C18 1.371(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Fe1 C2 66.0(4) . . ? C4 Fe1 C3 38.9(4) . . ? C2 Fe1 C3 40.2(4) . . ? C4 Fe1 C5 39.6(4) . . ? C2 Fe1 C5 66.2(4) . . ? C3 Fe1 C5 66.4(4) . . ? C4 Fe1 C1 66.3(4) . . ? C2 Fe1 C1 39.6(3) . . ? C3 Fe1 C1 67.0(4) . . ? C5 Fe1 C1 39.5(4) . . ? C4 Fe1 P1 135.1(3) . . ? C2 Fe1 P1 92.2(3) . . ? C3 Fe1 P1 99.3(3) . . ? C5 Fe1 P1 158.2(3) . . ? C1 Fe1 P1 120.9(3) . . ? C4 Fe1 P2 92.4(3) . . ? C2 Fe1 P2 146.6(3) . . ? C3 Fe1 P2 107.2(3) . . ? C5 Fe1 P2 113.6(3) . . ? C1 Fe1 P2 153.0(3) . . ? P1 Fe1 P2 85.74(11) . . ? C4 Fe1 C14 130.6(4) . . ? C2 Fe1 C14 118.9(4) . . ? C3 Fe1 C14 155.1(4) . . ? C5 Fe1 C14 94.1(3) . . ? C1 Fe1 C14 88.1(3) . . ? P1 Fe1 C14 94.2(3) . . ? P2 Fe1 C14 94.5(3) . . ? C8 P1 C10 102.7(5) . . ? C8 P1 C11 101.4(5) . . ? C10 P1 C11 101.4(5) . . ? C8 P1 Fe1 110.8(3) . . ? C10 P1 Fe1 122.8(4) . . ? C11 P1 Fe1 115.0(4) . . ? C12 P2 C9 100.4(5) . . ? C12 P2 C13 99.3(5) . . ? C9 P2 C13 102.7(5) . . ? C12 P2 Fe1 118.7(4) . . ? C9 P2 Fe1 111.2(3) . . ? C13 P2 Fe1 121.4(3) . . ? C18 Si1 C7 110.7(5) . . ? C18 Si1 C6 112.1(4) . . ? C7 Si1 C6 111.5(5) . . ? C18 Si1 C1 100.9(4) . . ? C7 Si1 C1 111.3(5) . . ? C6 Si1 C1 109.9(5) . . ? C5 C1 C2 106.6(8) . . ? C5 C1 Si1 125.1(7) . . ? C2 C1 Si1 125.2(8) . . ? C5 C1 Fe1 69.5(6) . . ? C2 C1 Fe1 68.9(6) . . ? Si1 C1 Fe1 110.8(5) . . ? C1 C2 C3 108.7(9) . . ? C1 C2 Fe1 71.5(6) . . ? C3 C2 Fe1 69.9(6) . . ? C4 C3 C2 106.7(9) . . ? C4 C3 Fe1 69.5(6) . . ? C2 C3 Fe1 69.9(5) . . ? C3 C4 C5 110.5(9) . . ? C3 C4 Fe1 71.6(6) . . ? C5 C4 Fe1 71.8(6) . . ? C4 C5 C1 107.5(9) . . ? C4 C5 Fe1 68.6(6) . . ? C1 C5 Fe1 71.0(5) . . ? C9 C8 P1 107.8(7) . . ? C8 C9 P2 110.6(7) . . ? C15 C14 C18 106.4(8) . . ? C15 C14 Fe1 122.4(6) . . ? C18 C14 Fe1 105.1(6) . . ? C16 C15 C14 107.8(9) . . ? C15 C16 C17 108.8(9) . . ? C18 C17 C16 109.9(9) . . ? C17 C18 C14 106.8(8) . . ? C17 C18 Si1 131.3(8) . . ? C14 C18 Si1 120.2(7) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.936 _refine_diff_density_min -1.155 _refine_diff_density_rms 0.165