Supplementary Material (ESI) for Dalton Transactions This journal is (C) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Mevellec, F.' 'Noiret, N.' 'Patin, H.' 'Roucoux, Alain' _publ_contact_author_name 'Dr Alain Roucoux' _publ_contact_author_address ; Dr Alain Roucoux Lab de Chimie des Biomolecules et des Systemes Organises, CNRS UMR 6052 Ecole Nationale Superieure de Chimie de Rennes 35700 Rennes FRANCE ; _publ_contact_author_email 'ALAIN.ROUCOUX@ENSC-RENNES.FR' data_mev2 _database_code_CSD 157245 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C27 H26 Cl N2 O3 P Re S2' _chemical_formula_weight 743.24 _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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 '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 17.395(6) _cell_length_b 9.861(5) _cell_length_c 16.911(9) _cell_angle_alpha 90.00 _cell_angle_beta 102.28(3) _cell_angle_gamma 90.00 _cell_volume 2834.6(22) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 7.6 _cell_measurement_theta_max 11.2 _exptl_crystal_description gem-like blocks _exptl_crystal_colour dark _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.742 _exptl_crystal_density_method ? _exptl_crystal_F_000 1460 _exptl_absorpt_coefficient_mu 4.617 _exptl_absorpt_correction_type not applied _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 Nicolet R3m/V diffractometer _diffrn_measurement_method theta-2theta _diffrn_standards_number 2 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% no decay _diffrn_reflns_number 6373 _diffrn_reflns_av_R_equivalents 0.0621 _diffrn_reflns_av_sigmaI/netI 0.0943 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 22.06 _reflns_number_total 3315 _reflns_number_observed 2251 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'P3/P4-PC Ver.4.27, 1991' _computing_cell_refinement 'P3/P4-PC Ver.4.27, 1991' _computing_data_reduction 'P3/P4-PC Ver.4.27, 1991' _computing_structure_solution 'SHELXTL/PC Ver.5.03,Sheldrick, 1994' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL/PC Ver.5.03,Sheldrick, 1994' _computing_publication_material 'SHELXTL/PC Ver.5.03,Sheldrick, 1994' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 6 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^)+(0.0872P)^2^+18.7800P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy-atom methods _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens not found _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3309 _refine_ls_number_parameters 195 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1080 _refine_ls_R_factor_obs 0.0881 _refine_ls_wR_factor_all 0.2500 _refine_ls_wR_factor_obs 0.2312 _refine_ls_goodness_of_fit_all 1.170 _refine_ls_goodness_of_fit_obs 1.257 _refine_ls_restrained_S_all 1.186 _refine_ls_restrained_S_obs 1.257 _refine_ls_shift/esd_max -0.227 _refine_ls_shift/esd_mean 0.004 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 Re Re 0.76071(5) 0.08007(10) 0.46772(4) 0.0448(5) Uani 1 d . . Cl Cl 0.8506(3) 0.2357(7) 0.5490(3) 0.062(2) Uani 1 d . . S1 S 0.7322(3) -0.0111(7) 0.5812(3) 0.058(2) Uani 1 d . . S2 S 0.7854(5) -0.2678(8) 0.6598(4) 0.075(2) Uani 1 d . . P1 P 0.6668(3) 0.2651(7) 0.4681(3) 0.0414(14) Uani 1 d . . O1 O 0.6950(8) -0.0002(16) 0.3934(8) 0.051(4) Uani 1 d . . O2 O 0.8127(8) 0.1636(19) 0.3856(7) 0.055(4) Uani 1 d . . N1 N 0.8445(10) -0.0615(26) 0.4870(8) 0.060(6) Uani 1 d . . N2 N 0.8499(10) -0.1649(17) 0.5461(10) 0.044(4) Uani 1 d . . C1 C 0.8763(12) 0.1254(27) 0.3599(12) 0.048(5) Uiso 1 d . . C2 C 0.8996(13) 0.2021(29) 0.3007(13) 0.062(6) Uiso 1 d . . H2A H 0.8725(13) 0.2808(29) 0.2816(13) 0.075 Uiso 1 calc R . C3 C 0.9661(14) 0.1592(30) 0.2691(14) 0.064(6) Uiso 1 d . . H3A H 0.9800(14) 0.2073(30) 0.2270(14) 0.077 Uiso 1 calc R . C4 C 1.0055(13) 0.0572(26) 0.2980(12) 0.053(6) Uiso 1 d . . H4A H 1.0495(13) 0.0329(26) 0.2780(12) 0.063 Uiso 1 calc R . C5 C 0.9853(14) -0.0196(33) 0.3585(14) 0.069(7) Uiso 1 d . . H5A H 1.0151(14) -0.0948(33) 0.3792(14) 0.083 Uiso 1 calc R . C6 C 0.9213(13) 0.0161(29) 0.3875(13) 0.059(6) Uiso 1 d . . C7 C 0.9089(13) -0.0779(22) 0.4513(12) 0.046(5) Uiso 1 d . . H7A H 0.9441(13) -0.1484(22) 0.4676(12) 0.055 Uiso 1 calc R . C8 C 0.7975(12) -0.1512(26) 0.5880(12) 0.048(5) Uiso 1 d . . C9 C 0.8533(18) -0.4054(34) 0.6503(19) 0.091(9) Uiso 1 d . . H9A H 0.8497(18) -0.4750(34) 0.6890(19) 0.137 Uiso 1 calc R . H9B H 0.9061(18) -0.3709(34) 0.6602(19) 0.137 Uiso 1 calc R . H9C H 0.8398(18) -0.4426(34) 0.5966(19) 0.137 Uiso 1 calc R . C1A C 0.6411(10) 0.3035(21) 0.5654(10) 0.035(4) Uiso 1 d . . C2A C 0.5646(14) 0.3188(30) 0.5682(14) 0.067(7) Uiso 1 d . . H2AA H 0.5239(14) 0.3081(30) 0.5231(14) 0.080 Uiso 1 calc R . C3A C 0.5512(18) 0.3537(38) 0.6483(17) 0.086(8) Uiso 1 d . . H3AA H 0.4994(18) 0.3539(38) 0.6546(17) 0.103 Uiso 1 calc R . C4A C 0.6005(14) 0.3819(31) 0.7059(14) 0.063(6) Uiso 1 d . . H4AA H 0.5866(14) 0.4134(31) 0.7528(14) 0.076 Uiso 1 calc R . C5A C 0.6783(14) 0.3676(33) 0.7029(14) 0.068(7) Uiso 1 d . . H5AA H 0.7175(14) 0.3828(33) 0.7488(14) 0.082 Uiso 1 calc R . C6A C 0.6975(13) 0.3308(25) 0.6314(11) 0.050(5) Uiso 1 d . . H6AA H 0.7502(13) 0.3245(25) 0.6285(11) 0.059 Uiso 1 calc R . C1B C 0.5749(12) 0.2135(25) 0.4069(12) 0.049(5) Uiso 1 d . . C2B C 0.5331(14) 0.3098(31) 0.3455(13) 0.065(6) Uiso 1 d . . H2BA H 0.5554(14) 0.3916(31) 0.3348(13) 0.078 Uiso 1 calc R . C3B C 0.4579(15) 0.2704(32) 0.3045(15) 0.072(7) Uiso 1 d . . H3BA H 0.4273(15) 0.3262(32) 0.2658(15) 0.086 Uiso 1 calc R . C4B C 0.4328(18) 0.1553(39) 0.3221(17) 0.089(9) Uiso 1 d . . H4BA H 0.3815(18) 0.1346(39) 0.2962(17) 0.107 Uiso 1 calc R . C5B C 0.4696(16) 0.0602(34) 0.3726(15) 0.074(8) Uiso 1 d . . H5BA H 0.4470(16) -0.0237(34) 0.3786(15) 0.088 Uiso 1 calc R . C6B C 0.5431(11) 0.0955(21) 0.4148(11) 0.038(5) Uiso 1 d . . H6BA H 0.5716(11) 0.0329(21) 0.4505(11) 0.046 Uiso 1 calc R . C1C C 0.6906(14) 0.4260(25) 0.4361(14) 0.054(6) Uiso 1 d . . C2C C 0.7255(14) 0.4332(27) 0.3670(14) 0.059(6) Uiso 1 d . . H2CA H 0.7348(14) 0.3548(27) 0.3400(14) 0.071 Uiso 1 calc R . C3C C 0.7456(15) 0.5600(28) 0.3410(14) 0.062(6) Uiso 1 d . . H3CA H 0.7732(15) 0.5629(28) 0.2995(14) 0.075 Uiso 1 calc R . C4C C 0.7273(17) 0.6795(41) 0.3723(17) 0.090(9) Uiso 1 d . . H4CA H 0.7407(17) 0.7625(41) 0.3528(17) 0.108 Uiso 1 calc R . C5C C 0.6871(14) 0.6711(31) 0.4354(14) 0.063(6) Uiso 1 d . . H5CA H 0.6740(14) 0.7505(31) 0.4591(14) 0.076 Uiso 1 calc R . C6C C 0.6669(13) 0.5502(27) 0.4629(13) 0.051(5) Uiso 1 d . . H6CA H 0.6359(13) 0.5497(27) 0.5014(13) 0.061 Uiso 1 calc R . OW1 O 1.0349(14) 0.0457(31) 0.0795(14) 0.116(7) Uiso 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 Re 0.0425(8) 0.0472(8) 0.0461(6) 0.0057(4) 0.0128(4) 0.0095(4) Cl 0.047(3) 0.060(4) 0.074(3) -0.013(3) -0.003(3) 0.007(3) S1 0.059(4) 0.063(5) 0.053(3) 0.013(3) 0.017(3) 0.022(4) S2 0.103(5) 0.064(5) 0.060(3) 0.021(3) 0.025(3) 0.009(4) P1 0.031(3) 0.061(4) 0.026(2) -0.003(2) -0.007(2) 0.005(3) O1 0.044(8) 0.037(10) 0.060(8) -0.010(7) -0.017(7) -0.005(8) O2 0.056(9) 0.070(12) 0.035(6) 0.001(8) -0.001(6) -0.004(9) N1 0.057(11) 0.103(19) 0.014(7) -0.008(9) -0.008(7) 0.018(12) N2 0.050(10) 0.019(9) 0.061(10) -0.007(8) 0.009(9) -0.004(9) _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 Re O1 1.704(13) . ? Re O2 1.990(14) . ? Re N1 1.99(2) . ? Re S1 2.268(5) . ? Re Cl 2.403(6) . ? Re P1 2.450(6) . ? S1 C8 1.78(2) . ? S2 C8 1.72(2) . ? S2 C9 1.83(3) . ? P1 C1C 1.75(2) . ? P1 C1B 1.78(2) . ? P1 C1A 1.83(2) . ? O2 C1 1.33(2) . ? N1 C7 1.39(3) . ? N1 N2 1.42(3) . ? N2 C8 1.27(2) . ? C1 C6 1.35(4) . ? C1 C2 1.38(3) . ? C2 C3 1.44(3) . ? C3 C4 1.26(3) . ? C4 C5 1.38(3) . ? C5 C6 1.35(3) . ? C6 C7 1.47(3) . ? C1A C2A 1.35(3) . ? C1A C6A 1.35(3) . ? C2A C3A 1.46(4) . ? C3A C4A 1.19(3) . ? C4A C5A 1.37(3) . ? C5A C6A 1.37(3) . ? C1B C6B 1.31(3) . ? C1B C2B 1.48(3) . ? C2B C3B 1.40(3) . ? C3B C4B 1.27(4) . ? C4B C5B 1.34(4) . ? C5B C6B 1.37(3) . ? C1C C6C 1.40(3) . ? C1C C2C 1.43(3) . ? C2C C3C 1.39(4) . ? C3C C4C 1.36(4) . ? C4C C5C 1.40(3) . ? C5C C6C 1.35(4) . ? 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 O1 Re O2 90.6(6) . . ? O1 Re N1 98.5(7) . . ? O2 Re N1 88.8(7) . . ? O1 Re S1 101.9(5) . . ? O2 Re S1 165.6(4) . . ? N1 Re S1 82.4(5) . . ? O1 Re Cl 166.3(5) . . ? O2 Re Cl 78.4(4) . . ? N1 Re Cl 89.4(6) . . ? S1 Re Cl 90.1(2) . . ? O1 Re P1 90.3(5) . . ? O2 Re P1 95.5(5) . . ? N1 Re P1 170.2(4) . . ? S1 Re P1 91.5(2) . . ? Cl Re P1 82.8(2) . . ? C8 S1 Re 96.4(7) . . ? C8 S2 C9 104.8(12) . . ? C1C P1 C1B 108.7(11) . . ? C1C P1 C1A 102.0(10) . . ? C1B P1 C1A 102.7(8) . . ? C1C P1 Re 118.2(8) . . ? C1B P1 Re 107.6(8) . . ? C1A P1 Re 116.5(7) . . ? C1 O2 Re 130.2(16) . . ? C7 N1 N2 106.5(18) . . ? C7 N1 Re 129.7(17) . . ? N2 N1 Re 123.8(12) . . ? C8 N2 N1 111.6(18) . . ? O2 C1 C6 125.0(21) . . ? O2 C1 C2 118.3(23) . . ? C6 C1 C2 116.6(20) . . ? C1 C2 C3 119.4(26) . . ? C4 C3 C2 120.5(25) . . ? C3 C4 C5 121.6(24) . . ? C6 C5 C4 119.0(28) . . ? C1 C6 C5 122.8(25) . . ? C1 C6 C7 126.1(20) . . ? C5 C6 C7 111.2(24) . . ? N1 C7 C6 120.2(21) . . ? N2 C8 S2 122.1(19) . . ? N2 C8 S1 124.7(18) . . ? S2 C8 S1 113.1(11) . . ? C2A C1A C6A 119.8(19) . . ? C2A C1A P1 119.0(16) . . ? C6A C1A P1 120.8(14) . . ? C1A C2A C3A 114.3(23) . . ? C4A C3A C2A 125.8(28) . . ? C3A C4A C5A 119.4(27) . . ? C6A C5A C4A 119.3(24) . . ? C1A C6A C5A 120.8(20) . . ? C6B C1B C2B 119.1(21) . . ? C6B C1B P1 122.8(18) . . ? C2B C1B P1 118.0(18) . . ? C3B C2B C1B 116.0(25) . . ? C4B C3B C2B 117.5(30) . . ? C3B C4B C5B 129.4(33) . . ? C4B C5B C6B 114.9(30) . . ? C1B C6B C5B 122.8(23) . . ? C6C C1C C2C 115.3(22) . . ? C6C C1C P1 126.0(16) . . ? C2C C1C P1 117.8(18) . . ? C3C C2C C1C 118.8(23) . . ? C4C C3C C2C 124.1(23) . . ? C3C C4C C5C 116.3(32) . . ? C6C C5C C4C 121.6(28) . . ? C5C C6C C1C 123.0(19) . . ? _refine_diff_density_max 1.510 _refine_diff_density_min -1.360 _refine_diff_density_rms 0.156 data_redifabs _database_code_CSD 140024 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H23 Cl N2 O2 P Re S2' _chemical_formula_weight 724.21 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 9.603(7) _cell_length_b 30.375(8) _cell_length_c 11.142(4) _cell_angle_alpha 90.00 _cell_angle_beta 114.995(5) _cell_angle_gamma 90.00 _cell_volume 2946(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 4.438 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6331 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 26.97 _reflns_number_total 5960 _reflns_number_gt 4709 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0997P)^2^+22.1013P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0008(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5960 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_gt 0.0625 _refine_ls_wR_factor_ref 0.1851 _refine_ls_wR_factor_gt 0.1727 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.51900(5) 0.090928(13) 0.67609(4) 0.04613(18) Uani 1 1 d . . . Cl1 Cl 0.4633(4) 0.13921(11) 0.8154(3) 0.0664(8) Uani 1 1 d . . . S1 S 0.7832(4) 0.08697(10) 0.8232(3) 0.0635(7) Uani 1 1 d . . . S2 S 1.0466(4) 0.05800(14) 0.7771(4) 0.0845(10) Uani 1 1 d . . . P1 P 0.5881(3) 0.18581(7) 0.5145(2) 0.0393(5) Uani 1 1 d . . . O1 O 0.4652(9) 0.0434(3) 0.7184(8) 0.062(2) Uani 1 1 d . . . O2 O 0.3002(13) 0.1091(3) 0.5229(8) 0.077(3) Uani 1 1 d . . . O3 O 0.5912(7) 0.1509(2) 0.6107(6) 0.0426(14) Uani 1 1 d . . . N1 N 0.5959(14) 0.0638(3) 0.5467(11) 0.070(3) Uani 1 1 d . . . N2 N 0.7639(10) 0.0553(3) 0.5885(9) 0.052(2) Uani 1 1 d . . . C1 C 0.2619(14) 0.0853(4) 0.4113(14) 0.069(4) Uani 1 1 d . . . C2 C 0.1026(19) 0.0893(6) 0.330(2) 0.100(6) Uani 1 1 d . . . H2 H 0.0401 0.1046 0.3604 0.120 Uiso 1 1 calc R . . C3 C 0.0504(14) 0.0737(4) 0.2263(14) 0.058(3) Uani 1 1 d . . . H3 H -0.0524 0.0808 0.1767 0.069 Uiso 1 1 calc R . . C4 C 0.113(2) 0.0453(5) 0.1592(15) 0.108(7) Uani 1 1 d . . . H4 H 0.0587 0.0326 0.0764 0.130 Uiso 1 1 calc R . . C5 C 0.265(2) 0.0401(5) 0.2360(13) 0.085(4) Uani 1 1 d . . . H5 H 0.3187 0.0221 0.2028 0.102 Uiso 1 1 calc R . . C6 C 0.3542(13) 0.0601(3) 0.3681(10) 0.051(2) Uani 1 1 d . . . C7 C 0.513(2) 0.0526(4) 0.4296(13) 0.077(4) Uani 1 1 d . . . H7 H 0.5595 0.0387 0.3813 0.093 Uiso 1 1 calc R . . C8 C 0.8430(13) 0.0662(3) 0.7125(11) 0.055(3) Uani 1 1 d . . . C9 C 1.0640(19) 0.0381(7) 0.6360(17) 0.105(6) Uani 1 1 d . . . H9A H 1.1701 0.0323 0.6574 0.137 Uiso 1 1 calc R . . H9B H 1.0254 0.0597 0.5667 0.137 Uiso 1 1 calc R . . H9C H 1.0058 0.0114 0.6067 0.137 Uiso 1 1 calc R . . C10 C 0.4965(11) 0.1685(3) 0.3449(10) 0.047(2) Uani 1 1 d . . . C11 C 0.3366(13) 0.1689(3) 0.2742(10) 0.052(2) Uani 1 1 d . . . H11 H 0.2763 0.1793 0.3152 0.062 Uiso 1 1 calc R . . C12 C 0.2664(14) 0.1543(4) 0.1447(11) 0.063(3) Uani 1 1 d . . . H12 H 0.1602 0.1558 0.0980 0.075 Uiso 1 1 calc R . . C13 C 0.3530(18) 0.1379(4) 0.0867(13) 0.074(4) Uani 1 1 d . . . H13 H 0.3060 0.1275 0.0002 0.089 Uiso 1 1 calc R . . C14 C 0.5120(18) 0.1364(5) 0.1548(13) 0.082(4) Uani 1 1 d . . . H14 H 0.5700 0.1252 0.1128 0.098 Uiso 1 1 calc R . . C15 C 0.5856(16) 0.1512(4) 0.2835(13) 0.068(3) Uani 1 1 d . . . H15 H 0.6921 0.1498 0.3287 0.082 Uiso 1 1 calc R . . C16 C 0.7814(12) 0.2008(3) 0.5449(10) 0.046(2) Uani 1 1 d . . . C17 C 0.9008(15) 0.1736(4) 0.6180(17) 0.082(4) Uani 1 1 d . . . H17 H 0.8817 0.1492 0.6593 0.098 Uiso 1 1 calc R . . C18 C 1.0486(17) 0.1812(6) 0.632(2) 0.107(6) Uani 1 1 d . . . H18 H 1.1252 0.1604 0.6728 0.129 Uiso 1 1 calc R . . C19 C 1.0809(18) 0.2195(6) 0.5862(19) 0.094(5) Uani 1 1 d . . . H19 H 1.1815 0.2265 0.6019 0.113 Uiso 1 1 calc R . . C20 C 0.9626(19) 0.2479(5) 0.5160(17) 0.088(5) Uani 1 1 d . . . H20 H 0.9844 0.2736 0.4819 0.106 Uiso 1 1 calc R . . C21 C 0.8134(16) 0.2395(4) 0.4946(15) 0.073(4) Uani 1 1 d . . . H21 H 0.7354 0.2593 0.4475 0.087 Uiso 1 1 calc R . . C22 C 0.4920(11) 0.2345(3) 0.5314(10) 0.045(2) Uani 1 1 d . . . C23 C 0.4219(13) 0.2635(3) 0.4256(12) 0.061(3) Uani 1 1 d . . . H23 H 0.4203 0.2575 0.3432 0.073 Uiso 1 1 calc R . . C24 C 0.3546(14) 0.3016(4) 0.4462(14) 0.072(4) Uani 1 1 d . . . H24 H 0.3057 0.3209 0.3759 0.087 Uiso 1 1 calc R . . C25 C 0.3589(14) 0.3113(4) 0.5664(15) 0.068(3) Uani 1 1 d . . . H25 H 0.3140 0.3370 0.5786 0.082 Uiso 1 1 calc R . . C26 C 0.4294(15) 0.2830(4) 0.6691(15) 0.072(4) Uani 1 1 d . . . H26 H 0.4323 0.2896 0.7516 0.086 Uiso 1 1 calc R . . C27 C 0.4967(12) 0.2448(4) 0.6530(11) 0.055(3) Uani 1 1 d . . . H27 H 0.5453 0.2259 0.7245 0.066 Uiso 1 1 calc R . . O4 O 0.3567 -0.0244 0.9318 0.092 Uiso 0.70 1 d P . . C28 C 0.5342 -0.0232 0.9975 0.050 Uiso 0.70 1 d P . . 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 Re1 0.0557(3) 0.0475(2) 0.0444(2) -0.00196(17) 0.03013(19) -0.00717(18) Cl1 0.081(2) 0.0791(19) 0.0583(16) -0.0016(13) 0.0481(16) 0.0092(15) S1 0.0683(19) 0.0628(17) 0.0590(16) -0.0011(13) 0.0265(15) 0.0042(14) S2 0.066(2) 0.090(2) 0.093(3) 0.002(2) 0.0293(19) 0.0085(18) P1 0.0421(13) 0.0375(11) 0.0450(12) -0.0011(9) 0.0250(10) -0.0021(9) O1 0.069(5) 0.065(5) 0.057(4) 0.014(4) 0.031(4) -0.005(4) O2 0.143(9) 0.058(4) 0.044(4) -0.010(4) 0.052(5) -0.033(5) O3 0.046(4) 0.039(3) 0.051(4) 0.003(3) 0.028(3) 0.000(3) N1 0.114(9) 0.044(5) 0.070(7) -0.004(4) 0.055(7) -0.006(5) N2 0.055(5) 0.049(5) 0.061(5) 0.002(4) 0.033(4) 0.011(4) C1 0.045(6) 0.076(8) 0.083(9) 0.033(7) 0.024(6) -0.001(5) C2 0.064(10) 0.110(13) 0.128(16) 0.049(12) 0.042(10) -0.004(9) C3 0.053(7) 0.049(6) 0.059(7) 0.007(5) 0.011(6) -0.007(5) C4 0.119(13) 0.074(9) 0.072(9) 0.022(8) -0.020(9) -0.046(9) C5 0.112(12) 0.064(8) 0.062(8) 0.005(6) 0.020(8) -0.010(8) C6 0.057(7) 0.046(5) 0.043(5) -0.002(4) 0.014(5) -0.009(5) C7 0.133(13) 0.045(6) 0.069(8) 0.001(6) 0.057(9) -0.005(7) C8 0.054(6) 0.048(5) 0.058(6) 0.006(5) 0.018(5) -0.009(5) C9 0.078(11) 0.151(17) 0.095(11) 0.003(11) 0.044(9) -0.003(10) C10 0.051(6) 0.049(5) 0.049(5) 0.002(4) 0.029(5) -0.004(4) C11 0.057(7) 0.051(5) 0.052(6) 0.002(4) 0.027(5) -0.001(5) C12 0.060(7) 0.074(7) 0.046(6) 0.006(5) 0.016(5) -0.007(6) C13 0.098(11) 0.079(8) 0.053(6) -0.018(6) 0.039(7) -0.027(7) C14 0.103(12) 0.099(10) 0.069(8) -0.028(7) 0.060(9) -0.035(8) C15 0.077(8) 0.076(8) 0.066(7) -0.019(6) 0.045(7) -0.018(6) C16 0.048(6) 0.046(5) 0.056(6) -0.005(4) 0.034(5) -0.005(4) C17 0.053(8) 0.068(8) 0.128(12) 0.033(8) 0.041(8) 0.004(6) C18 0.052(8) 0.099(12) 0.170(18) 0.047(12) 0.046(10) 0.015(8) C19 0.066(9) 0.096(11) 0.134(14) -0.014(10) 0.055(10) -0.027(8) C20 0.094(11) 0.070(8) 0.117(12) 0.004(8) 0.060(10) -0.031(8) C21 0.077(9) 0.056(7) 0.104(10) 0.013(7) 0.056(8) -0.003(6) C22 0.038(5) 0.047(5) 0.050(5) -0.002(4) 0.019(4) -0.003(4) C23 0.065(7) 0.041(5) 0.062(6) -0.001(5) 0.013(6) 0.007(5) C24 0.065(8) 0.042(6) 0.084(9) 0.000(6) 0.007(7) 0.013(5) C25 0.053(7) 0.042(6) 0.108(11) -0.007(6) 0.033(7) 0.010(5) C26 0.070(8) 0.061(7) 0.106(10) -0.022(7) 0.059(8) -0.007(6) C27 0.058(7) 0.054(6) 0.059(6) 0.001(5) 0.032(6) 0.005(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 Re1 O1 1.666(7) . ? Re1 N1 2.051(10) . ? Re1 O2 2.145(11) . ? Re1 O3 2.180(6) . ? Re1 Cl1 2.355(3) . ? Re1 S1 2.372(4) . ? S1 C8 1.689(12) . ? S2 C9 1.758(18) . ? S2 C8 1.792(12) . ? P1 O3 1.500(6) . ? P1 C10 1.794(10) . ? P1 C22 1.794(10) . ? P1 C16 1.799(10) . ? O2 C1 1.348(17) . ? N1 C7 1.254(17) . ? N1 N2 1.500(15) . ? N2 C8 1.306(14) . ? C1 C6 1.402(18) . ? C1 C2 1.42(2) . ? C2 C3 1.15(2) . ? C2 H2 0.9300 . ? C3 C4 1.43(2) . ? C3 H3 0.9300 . ? C4 C5 1.35(2) . ? C4 H4 0.9300 . ? C5 C6 1.485(16) . ? C5 H5 0.9300 . ? C6 C7 1.403(19) . ? C7 H7 0.9300 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.399(14) . ? C10 C15 1.403(15) . ? C11 C12 1.384(15) . ? C11 H11 0.9300 . ? C12 C13 1.346(18) . ? C12 H12 0.9300 . ? C13 C14 1.390(19) . ? C13 H13 0.9300 . ? C14 C15 1.380(17) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.368(16) . ? C16 C21 1.392(14) . ? C17 C18 1.379(19) . ? C17 H17 0.9300 . ? C18 C19 1.36(2) . ? C18 H18 0.9300 . ? C19 C20 1.38(2) . ? C19 H19 0.9300 . ? C20 C21 1.373(19) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C27 1.372(14) . ? C22 C23 1.396(14) . ? C23 C24 1.392(15) . ? C23 H23 0.9300 . ? C24 C25 1.354(19) . ? C24 H24 0.9300 . ? C25 C26 1.361(19) . ? C25 H25 0.9300 . ? C26 C27 1.376(15) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? O4 C28 1.5453 . ? O4 C28 1.7628 3_657 ? C28 C28 1.5659 3_657 ? C28 O4 1.7629 3_657 ? 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 O1 Re1 N1 95.6(4) . . ? O1 Re1 O2 97.5(3) . . ? N1 Re1 O2 93.8(4) . . ? O1 Re1 O3 176.4(3) . . ? N1 Re1 O3 80.9(3) . . ? O2 Re1 O3 82.1(3) . . ? O1 Re1 Cl1 99.7(3) . . ? N1 Re1 Cl1 164.5(3) . . ? O2 Re1 Cl1 86.9(2) . . ? O3 Re1 Cl1 83.84(18) . . ? O1 Re1 S1 97.5(3) . . ? N1 Re1 S1 82.4(4) . . ? O2 Re1 S1 164.8(2) . . ? O3 Re1 S1 82.80(19) . . ? Cl1 Re1 S1 92.88(11) . . ? C8 S1 Re1 96.2(4) . . ? C9 S2 C8 100.8(7) . . ? O3 P1 C10 113.5(4) . . ? O3 P1 C22 111.3(4) . . ? C10 P1 C22 107.9(5) . . ? O3 P1 C16 109.7(4) . . ? C10 P1 C16 106.3(4) . . ? C22 P1 C16 107.9(4) . . ? C1 O2 Re1 112.9(8) . . ? P1 O3 Re1 156.4(4) . . ? C7 N1 N2 113.7(11) . . ? C7 N1 Re1 125.7(11) . . ? N2 N1 Re1 120.6(7) . . ? C8 N2 N1 110.7(9) . . ? O2 C1 C6 130.1(11) . . ? O2 C1 C2 110.1(15) . . ? C6 C1 C2 119.7(15) . . ? C3 C2 C1 120(2) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 C4 132.3(16) . . ? C2 C3 H3 113.9 . . ? C4 C3 H3 113.9 . . ? C5 C4 C3 108.6(14) . . ? C5 C4 H4 125.7 . . ? C3 C4 H4 125.7 . . ? C4 C5 C6 126.7(16) . . ? C4 C5 H5 116.6 . . ? C6 C5 H5 116.6 . . ? C1 C6 C7 129.6(11) . . ? C1 C6 C5 112.3(12) . . ? C7 C6 C5 118.1(12) . . ? N1 C7 C6 122.9(13) . . ? N1 C7 H7 118.6 . . ? C6 C7 H7 118.6 . . ? N2 C8 S1 129.9(9) . . ? N2 C8 S2 116.0(9) . . ? S1 C8 S2 114.1(6) . . ? S2 C9 H9A 109.5 . . ? S2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? S2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 118.7(10) . . ? C11 C10 P1 121.5(7) . . ? C15 C10 P1 119.6(9) . . ? C12 C11 C10 121.3(10) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C13 C12 C11 119.5(12) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C12 C13 C14 120.6(11) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C15 C14 C13 121.3(13) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C10 118.6(13) . . ? C14 C15 H15 120.7 . . ? C10 C15 H15 120.7 . . ? C17 C16 C21 118.6(10) . . ? C17 C16 P1 119.8(8) . . ? C21 C16 P1 121.6(9) . . ? C16 C17 C18 122.0(12) . . ? C16 C17 H17 119.0 . . ? C18 C17 H17 119.0 . . ? C19 C18 C17 119.2(14) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C18 C19 C20 119.0(13) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C21 C20 C19 122.3(13) . . ? C21 C20 H20 118.9 . . ? C19 C20 H20 118.9 . . ? C20 C21 C16 118.5(13) . . ? C20 C21 H21 120.7 . . ? C16 C21 H21 120.7 . . ? C27 C22 C23 119.5(10) . . ? C27 C22 P1 119.2(8) . . ? C23 C22 P1 121.1(8) . . ? C24 C23 C22 118.6(12) . . ? C24 C23 H23 120.7 . . ? C22 C23 H23 120.7 . . ? C25 C24 C23 121.4(12) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C24 C25 C26 119.4(11) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C25 C26 C27 121.2(12) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C22 C27 C26 120.0(11) . . ? C22 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C28 O4 C28 56.0 . 3_657 ? O4 C28 C28 69.0 . 3_657 ? O4 C28 O4 124.0 . 3_657 ? C28 C28 O4 54.9 3_657 3_657 ? 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 O1 Re1 S1 C8 96.5(5) . . . . ? N1 Re1 S1 C8 1.8(4) . . . . ? O2 Re1 S1 C8 -74.7(10) . . . . ? O3 Re1 S1 C8 -79.9(4) . . . . ? Cl1 Re1 S1 C8 -163.4(4) . . . . ? O1 Re1 O2 C1 -74.1(8) . . . . ? N1 Re1 O2 C1 22.1(7) . . . . ? O3 Re1 O2 C1 102.3(7) . . . . ? Cl1 Re1 O2 C1 -173.5(7) . . . . ? S1 Re1 O2 C1 97.1(10) . . . . ? C10 P1 O3 Re1 -21.2(11) . . . . ? C22 P1 O3 Re1 100.7(10) . . . . ? C16 P1 O3 Re1 -139.9(9) . . . . ? O1 Re1 O3 P1 54(6) . . . . ? N1 Re1 O3 P1 64.8(10) . . . . ? O2 Re1 O3 P1 -30.4(10) . . . . ? Cl1 Re1 O3 P1 -118.1(10) . . . . ? S1 Re1 O3 P1 148.2(10) . . . . ? O1 Re1 N1 C7 80.5(10) . . . . ? O2 Re1 N1 C7 -17.4(10) . . . . ? O3 Re1 N1 C7 -98.8(10) . . . . ? Cl1 Re1 N1 C7 -109.5(14) . . . . ? S1 Re1 N1 C7 177.3(10) . . . . ? O1 Re1 N1 N2 -99.2(7) . . . . ? O2 Re1 N1 N2 162.9(7) . . . . ? O3 Re1 N1 N2 81.5(7) . . . . ? Cl1 Re1 N1 N2 70.8(16) . . . . ? S1 Re1 N1 N2 -2.4(7) . . . . ? C7 N1 N2 C8 -177.7(10) . . . . ? Re1 N1 N2 C8 2.0(11) . . . . ? Re1 O2 C1 C6 -18.6(14) . . . . ? Re1 O2 C1 C2 163.1(8) . . . . ? O2 C1 C2 C3 174.8(13) . . . . ? C6 C1 C2 C3 -4(2) . . . . ? C1 C2 C3 C4 7(3) . . . . ? C2 C3 C4 C5 -5(2) . . . . ? C3 C4 C5 C6 -0.1(19) . . . . ? O2 C1 C6 C7 0(2) . . . . ? C2 C1 C6 C7 178.0(12) . . . . ? O2 C1 C6 C5 -178.4(11) . . . . ? C2 C1 C6 C5 -0.2(15) . . . . ? C4 C5 C6 C1 1.9(18) . . . . ? C4 C5 C6 C7 -176.6(13) . . . . ? N2 N1 C7 C6 -176.0(9) . . . . ? Re1 N1 C7 C6 4.3(17) . . . . ? C1 C6 C7 N1 10.0(19) . . . . ? C5 C6 C7 N1 -171.8(11) . . . . ? N1 N2 C8 S1 0.0(14) . . . . ? N1 N2 C8 S2 -179.9(6) . . . . ? Re1 S1 C8 N2 -1.6(10) . . . . ? Re1 S1 C8 S2 178.4(5) . . . . ? C9 S2 C8 N2 1.5(11) . . . . ? C9 S2 C8 S1 -178.5(8) . . . . ? O3 P1 C10 C11 81.6(9) . . . . ? C22 P1 C10 C11 -42.2(9) . . . . ? C16 P1 C10 C11 -157.7(8) . . . . ? O3 P1 C10 C15 -94.0(9) . . . . ? C22 P1 C10 C15 142.2(9) . . . . ? C16 P1 C10 C15 26.7(10) . . . . ? C15 C10 C11 C12 -2.4(16) . . . . ? P1 C10 C11 C12 -178.0(8) . . . . ? C10 C11 C12 C13 2.3(17) . . . . ? C11 C12 C13 C14 -1(2) . . . . ? C12 C13 C14 C15 1(2) . . . . ? C13 C14 C15 C10 -1(2) . . . . ? C11 C10 C15 C14 1.6(17) . . . . ? P1 C10 C15 C14 177.3(10) . . . . ? O3 P1 C16 C17 17.4(12) . . . . ? C10 P1 C16 C17 -105.7(11) . . . . ? C22 P1 C16 C17 138.8(11) . . . . ? O3 P1 C16 C21 -163.2(9) . . . . ? C10 P1 C16 C21 73.7(10) . . . . ? C22 P1 C16 C21 -41.8(11) . . . . ? C21 C16 C17 C18 -6(2) . . . . ? P1 C16 C17 C18 173.0(15) . . . . ? C16 C17 C18 C19 8(3) . . . . ? C17 C18 C19 C20 -6(3) . . . . ? C18 C19 C20 C21 2(3) . . . . ? C19 C20 C21 C16 -1(2) . . . . ? C17 C16 C21 C20 3(2) . . . . ? P1 C16 C21 C20 -176.8(11) . . . . ? O3 P1 C22 C27 30.1(10) . . . . ? C10 P1 C22 C27 155.2(8) . . . . ? C16 P1 C22 C27 -90.4(9) . . . . ? O3 P1 C22 C23 -154.5(8) . . . . ? C10 P1 C22 C23 -29.4(10) . . . . ? C16 P1 C22 C23 85.1(9) . . . . ? C27 C22 C23 C24 -1.9(17) . . . . ? P1 C22 C23 C24 -177.4(9) . . . . ? C22 C23 C24 C25 1.4(19) . . . . ? C23 C24 C25 C26 0(2) . . . . ? C24 C25 C26 C27 0.1(19) . . . . ? C23 C22 C27 C26 1.6(16) . . . . ? P1 C22 C27 C26 177.1(9) . . . . ? C25 C26 C27 C22 -0.6(18) . . . . ? C28 O4 C28 O4 0.0 3_657 . . 3_657 ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 26.97 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 3.467 _refine_diff_density_min -1.839 _refine_diff_density_rms 0.202