# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1498 data_od _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C12 H42 Fe N2 O16 P4 S' _chemical_formula_weight 682.27 _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' 'N' 'N' 0.0061 0.0033 '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' 'S' 'S' 0.1246 0.1234 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.106(4) _cell_length_b 14.103(6) _cell_length_c 15.032(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.68(2) _cell_angle_gamma 90.00 _cell_volume 2566.3(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.766 _exptl_crystal_density_method ? _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 0.995 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7820 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0360 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2914 _reflns_number_observed 2414 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens/Bruker SMART area detector ' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 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^)+(0.0494P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2912 _refine_ls_number_parameters 212 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_obs 0.0299 _refine_ls_wR_factor_all 0.0809 _refine_ls_wR_factor_obs 0.0756 _refine_ls_goodness_of_fit_all 0.946 _refine_ls_goodness_of_fit_obs 1.023 _refine_ls_restrained_S_all 0.995 _refine_ls_restrained_S_obs 1.030 _refine_ls_shift/esd_max 0.002 _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 Fe Fe 0.0000 0.17844(2) 0.2500 0.00952(11) Uani 1 d S . O O -0.08389(12) 0.06836(10) 0.31040(10) 0.0172(3) Uani 1 d D . H1 H -0.0655(26) 0.0199(18) 0.3054(22) 0.050 Uiso 1 d D . H2 H -0.1293(22) 0.0700(23) 0.3434(19) 0.050 Uiso 1 d D . P1 P -0.08611(4) 0.29629(3) 0.31236(3) 0.01057(12) Uani 1 d . . N1 N 0.12060(13) 0.37005(11) 0.36364(10) 0.0132(3) Uani 1 d . . C1 C 0.0031(2) 0.37066(13) 0.38648(13) 0.0141(4) Uani 1 d . . H1A H -0.0240(2) 0.43684(13) 0.38423(13) 0.017 Uiso 1 calc R . H1B H -0.0045(2) 0.34796(13) 0.44843(13) 0.017 Uiso 1 calc R . P2 P 0.12622(4) 0.17136(3) 0.36004(3) 0.01211(12) Uani 1 d . . C2 C 0.1800(2) 0.28668(13) 0.39908(13) 0.0147(4) Uani 1 d . . H2A H 0.1767(2) 0.28819(13) 0.46484(13) 0.018 Uiso 1 calc R . H2B H 0.2587(2) 0.29164(13) 0.38239(13) 0.018 Uiso 1 calc R . C3 C 0.1411(2) 0.38669(14) 0.26951(13) 0.0145(4) Uani 1 d D . H3A H 0.2179(16) 0.3886(16) 0.2639(14) 0.017(6) Uiso 1 d D . H3B H 0.1099(17) 0.4444(15) 0.2525(15) 0.022(6) Uiso 1 d D . O11 O -0.25869(12) 0.36251(11) 0.40852(10) 0.0226(3) Uani 1 d . . H11 H -0.3173(11) 0.3697(9) 0.3788(13) 0.034 Uiso 1 calc R . C11 C -0.2072(2) 0.27551(14) 0.38364(13) 0.0166(4) Uani 1 d . . H11A H -0.2614(2) 0.23539(14) 0.35125(13) 0.020 Uiso 1 calc R . H11B H -0.1834(2) 0.24096(14) 0.43790(13) 0.020 Uiso 1 calc R . O21 O -0.01087(14) 0.16240(13) 0.49616(11) 0.0344(4) Uani 1 d . . H21 H -0.0099(13) 0.1599(18) 0.55199(12) 0.052 Uiso 1 calc R . C21 C 0.0813(2) 0.11322(15) 0.46275(13) 0.0190(4) Uani 1 d . . H21A H 0.0611(2) 0.04645(15) 0.45030(13) 0.023 Uiso 1 calc R . H21B H 0.1421(2) 0.11372(15) 0.50733(13) 0.023 Uiso 1 calc R . O22 O 0.32190(13) 0.10051(13) 0.41391(11) 0.0337(4) Uani 1 d . . H22 H 0.3862(6) 0.1161(21) 0.3994(4) 0.051 Uiso 1 calc R . C22 C 0.2517(2) 0.10197(15) 0.33751(14) 0.0193(4) Uani 1 d . . H22A H 0.2310(2) 0.03631(15) 0.32108(14) 0.023 Uiso 1 calc R . H22B H 0.2915(2) 0.13040(15) 0.28690(14) 0.023 Uiso 1 calc R . S S 0.0000 0.16011(5) 0.7500 0.0161(2) Uani 1 d S . O1 O -0.0190(3) 0.1007(2) 0.6716(2) 0.0364(8) Uani 0.676(3) d P 1 O2 O 0.0966(2) 0.2218(2) 0.7394(2) 0.0454(9) Uani 0.676(3) d P 1 O3 O -0.0929(3) 0.0942(3) 0.7217(3) 0.0201(12) Uani 0.324(3) d P 2 O4 O 0.0334(4) 0.2151(3) 0.6744(3) 0.0266(14) Uani 0.324(3) d P 2 O5 O -0.0290(2) 0.3874(2) 0.6434(2) 0.0663(8) Uani 1 d D . H5A H -0.0955(19) 0.4049(22) 0.6217(19) 0.050 Uiso 1 d D . H5B H -0.0378(25) 0.3358(17) 0.6728(20) 0.050 Uiso 1 d D . O6 O -0.23109(13) 0.45326(11) 0.57763(11) 0.0247(3) Uani 1 d D . H6A H -0.2366(25) 0.4332(22) 0.5287(15) 0.050 Uiso 1 d D . H6B H -0.1997(24) 0.5023(17) 0.5761(22) 0.050 Uiso 1 d 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 Fe 0.0118(2) 0.0071(2) 0.0097(2) 0.000 0.00086(14) 0.000 O 0.0205(8) 0.0125(7) 0.0189(8) 0.0025(6) 0.0058(6) -0.0020(6) P1 0.0121(2) 0.0088(2) 0.0109(2) -0.0002(2) 0.0019(2) 0.0006(2) N1 0.0154(8) 0.0108(8) 0.0133(8) -0.0015(6) 0.0003(6) -0.0007(6) C1 0.0168(10) 0.0111(9) 0.0143(10) -0.0032(7) 0.0007(7) -0.0003(7) P2 0.0136(3) 0.0103(2) 0.0124(3) 0.0000(2) -0.0010(2) 0.0009(2) C2 0.0160(10) 0.0130(9) 0.0151(10) -0.0018(7) -0.0030(7) -0.0011(7) C3 0.0168(10) 0.0106(9) 0.0161(10) -0.0013(7) 0.0020(8) -0.0031(8) O11 0.0208(8) 0.0252(8) 0.0220(8) -0.0024(6) 0.0048(6) 0.0091(6) C11 0.0162(10) 0.0169(9) 0.0168(10) 0.0013(8) 0.0046(8) -0.0006(8) O21 0.0344(10) 0.0477(11) 0.0212(9) 0.0128(8) 0.0095(7) 0.0145(8) C21 0.0202(10) 0.0190(10) 0.0178(10) 0.0053(8) -0.0025(8) -0.0005(8) O22 0.0239(9) 0.0448(10) 0.0322(9) -0.0089(8) -0.0114(7) 0.0124(8) C22 0.0177(10) 0.0195(10) 0.0206(11) -0.0036(8) -0.0028(8) 0.0050(8) S 0.0192(4) 0.0123(3) 0.0167(4) 0.000 -0.0006(3) 0.000 O1 0.078(2) 0.0156(11) 0.0156(13) -0.0012(9) -0.0109(13) 0.0014(12) O2 0.032(2) 0.055(2) 0.049(2) -0.0001(14) 0.0032(13) -0.0212(13) O3 0.011(2) 0.020(2) 0.029(3) 0.006(2) -0.003(2) -0.005(2) O4 0.036(3) 0.021(2) 0.023(3) 0.004(2) 0.010(2) -0.008(2) O5 0.0344(12) 0.062(2) 0.102(2) 0.0480(15) 0.0027(12) 0.0095(11) O6 0.0300(9) 0.0182(8) 0.0260(9) -0.0005(7) 0.0023(7) -0.0028(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe O 2.0707(15) . ? Fe O 2.0707(15) 2 ? Fe P1 2.1797(8) . ? Fe P1 2.1797(8) 2 ? Fe P2 2.2408(8) 2 ? Fe P2 2.2408(8) . ? O H1 0.72(2) . ? O H2 0.75(2) . ? P1 C11 1.849(2) . ? P1 C1 1.865(2) . ? P1 C3 1.888(2) 2 ? N1 C3 1.458(2) . ? N1 C1 1.467(2) . ? N1 C2 1.475(2) . ? C1 H1A 0.99 . ? C1 H1B 0.99 . ? P2 C21 1.836(2) . ? P2 C22 1.842(2) . ? P2 C2 1.845(2) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 P1 1.888(2) 2 ? C3 H3A 0.94(2) . ? C3 H3B 0.93(2) . ? O11 C11 1.428(2) . ? O11 H11 0.84 . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? O21 C21 1.411(3) . ? O21 H21 0.84 . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? O22 C22 1.421(3) . ? O22 H22 0.84 . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? S O4 1.438(4) 2_556 ? S O4 1.438(4) . ? S O1 1.463(2) 2_556 ? S O1 1.463(2) . ? S O2 1.468(3) 2_556 ? S O2 1.468(3) . ? S O3 1.516(4) 2_556 ? S O3 1.516(4) . ? O5 H5A 0.90(2) . ? O5 H5B 0.86(2) . ? O6 H6A 0.79(2) . ? O6 H6B 0.79(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 O Fe O 82.87(9) . 2 ? O Fe P1 98.25(5) . . ? O Fe P1 178.87(4) 2 . ? O Fe P1 178.88(4) . 2 ? O Fe P1 98.25(5) 2 2 ? P1 Fe P1 80.63(4) . 2 ? O Fe P2 87.51(5) . 2 ? O Fe P2 88.66(5) 2 2 ? P1 Fe P2 91.49(2) . 2 ? P1 Fe P2 92.41(2) 2 2 ? O Fe P2 88.66(5) . . ? O Fe P2 87.51(5) 2 . ? P1 Fe P2 92.41(2) . . ? P1 Fe P2 91.49(2) 2 . ? P2 Fe P2 174.89(3) 2 . ? Fe O H1 120.6(26) . . ? Fe O H2 129.6(25) . . ? H1 O H2 109.3(35) . . ? C11 P1 C1 101.55(9) . . ? C11 P1 C3 102.08(9) . 2 ? C1 P1 C3 101.93(9) . 2 ? C11 P1 Fe 120.98(7) . . ? C1 P1 Fe 114.15(6) . . ? C3 P1 Fe 113.66(7) 2 . ? C3 N1 C1 113.7(2) . . ? C3 N1 C2 113.03(15) . . ? C1 N1 C2 112.96(15) . . ? N1 C1 P1 114.39(12) . . ? N1 C1 H1A 108.66(10) . . ? P1 C1 H1A 108.66(6) . . ? N1 C1 H1B 108.66(10) . . ? P1 C1 H1B 108.66(6) . . ? H1A C1 H1B 107.6 . . ? C21 P2 C22 99.82(10) . . ? C21 P2 C2 103.48(10) . . ? C22 P2 C2 103.78(10) . . ? C21 P2 Fe 115.75(7) . . ? C22 P2 Fe 116.40(7) . . ? C2 P2 Fe 115.50(7) . . ? N1 C2 P2 114.78(14) . . ? N1 C2 H2A 108.57(10) . . ? P2 C2 H2A 108.57(6) . . ? N1 C2 H2B 108.57(10) . . ? P2 C2 H2B 108.57(6) . . ? H2A C2 H2B 107.5 . . ? N1 C3 P1 117.46(13) . 2 ? N1 C3 H3A 105.9(14) . . ? P1 C3 H3A 107.7(13) 2 . ? N1 C3 H3B 109.5(14) . . ? P1 C3 H3B 105.8(14) 2 . ? H3A C3 H3B 110.4(20) . . ? C11 O11 H11 109.47(10) . . ? O11 C11 P1 111.55(13) . . ? O11 C11 H11A 109.31(10) . . ? P1 C11 H11A 109.31(7) . . ? O11 C11 H11B 109.31(10) . . ? P1 C11 H11B 109.31(7) . . ? H11A C11 H11B 108.0 . . ? C21 O21 H21 109.47(10) . . ? O21 C21 P2 108.86(14) . . ? O21 C21 H21A 109.91(12) . . ? P2 C21 H21A 109.91(7) . . ? O21 C21 H21B 109.91(11) . . ? P2 C21 H21B 109.91(7) . . ? H21A C21 H21B 108.3 . . ? C22 O22 H22 109.47(11) . . ? O22 C22 P2 110.23(14) . . ? O22 C22 H22A 109.61(11) . . ? P2 C22 H22A 109.61(7) . . ? O22 C22 H22B 109.61(12) . . ? P2 C22 H22B 109.61(7) . . ? H22A C22 H22B 108.1 . . ? O4 S O4 114.7(4) 2_556 . ? O1 S O1 110.1(2) 2_556 . ? O1 S O2 111.8(2) 2_556 2_556 ? O1 S O2 108.0(2) . 2_556 ? O1 S O2 108.0(2) 2_556 . ? O1 S O2 111.8(2) . . ? O2 S O2 107.2(3) 2_556 . ? O4 S O3 108.9(3) 2_556 2_556 ? O4 S O3 109.7(3) . 2_556 ? O4 S O3 109.7(3) 2_556 . ? O4 S O3 108.9(3) . . ? O3 S O3 104.4(3) 2_556 . ? H5A O5 H5B 107.7(28) . . ? H6A O6 H6B 108.8(32) . . ? _refine_diff_density_max 0.540 _refine_diff_density_min -0.769 _refine_diff_density_rms 0.080