# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Mark Stradiotto' 'Michael J. Ferguson' 'Robert McDonald' 'Dominik Wechsler' _publ_contact_author_name 'Mark Stradiotto' _publ_contact_author_address ; Mark Stradiotto Assistant Professor Dalhousie University Department of Chemistry Halifax, Nova Scotia Canada B3H 4J3 ; _publ_contact_author_phone '902 494 7190' _publ_contact_author_fax '902 494 1310' _publ_contact_author_email mark.stradiotto@dal.ca _publ_requested_journal 'Chemical Communications' _publ_requested_coeditor_name ? _publ_section_title ; Structurally Diverse Rh(I) and Mn(I) Complexes Derived from the New Ambidentate Indene Ligand, (1-{iPr2PS}-2-{NMe2})C9H6 ; data_Compound2 _database_code_depnum_ccdc_archive 'CCDC 244733' _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H26 N P S' _chemical_formula_weight 307.42 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' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.3157(19) _cell_length_b 10.8344(12) _cell_length_c 17.787(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3337.0(6) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 4392 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 26.35 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.281 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8698 _exptl_absorpt_correction_T_max 0.9670 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 22338 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 26.42 _reflns_number_total 3424 _reflns_number_gt 2883 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1997)' _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^)+(0.0415P)^2^+1.3507P] 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 3424 _refine_ls_number_parameters 187 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0887 _refine_ls_wR_factor_gt 0.0825 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 P P 0.01997(2) 0.28897(3) 0.10468(2) 0.02134(11) Uani 1 1 d . . . S S -0.05663(2) 0.41442(4) 0.13340(3) 0.03408(13) Uani 1 1 d . . . N N 0.17391(7) 0.18671(12) -0.00144(7) 0.0264(3) Uani 1 1 d . . . C1 C 0.11556(8) 0.35876(13) 0.07984(8) 0.0219(3) Uani 1 1 d . . . H1 H 0.1089 0.4190 0.0377 0.026 Uiso 1 1 calc R . . C2 C 0.17926(8) 0.26611(14) 0.05988(8) 0.0239(3) Uani 1 1 d . . . C3 C 0.23575(9) 0.26916(15) 0.11225(9) 0.0274(3) Uani 1 1 d . . . H3 H 0.2797 0.2166 0.1130 0.033 Uiso 1 1 calc R . . C3A C 0.21944(9) 0.36460(15) 0.16718(9) 0.0263(3) Uani 1 1 d . . . C4 C 0.26157(10) 0.40317(16) 0.22964(9) 0.0334(4) Uani 1 1 d . . . H4 H 0.3076 0.3617 0.2439 0.040 Uiso 1 1 calc R . . C5 C 0.23484(10) 0.50327(18) 0.27041(9) 0.0375(4) Uani 1 1 d . . . H5 H 0.2631 0.5307 0.3130 0.045 Uiso 1 1 calc R . . C6 C 0.16770(10) 0.56414(16) 0.25023(10) 0.0355(4) Uani 1 1 d . . . H6 H 0.1511 0.6336 0.2785 0.043 Uiso 1 1 calc R . . C7 C 0.12402(9) 0.52452(15) 0.18862(9) 0.0293(4) Uani 1 1 d . . . H7 H 0.0776 0.5656 0.1751 0.035 Uiso 1 1 calc R . . C7A C 0.15012(9) 0.42388(14) 0.14776(8) 0.0246(3) Uani 1 1 d . . . C8 C 0.23396(9) 0.09221(16) -0.00513(10) 0.0337(4) Uani 1 1 d . . . H8A H 0.2352 0.0462 0.0423 0.040 Uiso 1 1 calc R . . H8B H 0.2842 0.1316 -0.0136 0.040 Uiso 1 1 calc R . . H8C H 0.2228 0.0354 -0.0466 0.040 Uiso 1 1 calc R . . C9 C 0.16266(11) 0.24473(19) -0.07476(9) 0.0388(4) Uani 1 1 d . . . H9A H 0.1251 0.3120 -0.0701 0.047 Uiso 1 1 calc R . . H9B H 0.1434 0.1833 -0.1106 0.047 Uiso 1 1 calc R . . H9C H 0.2120 0.2779 -0.0928 0.047 Uiso 1 1 calc R . . C10 C -0.01352(9) 0.20292(14) 0.02204(8) 0.0255(3) Uani 1 1 d . . . H10 H 0.0295 0.1493 0.0036 0.031 Uiso 1 1 calc R . . C11 C -0.08265(10) 0.12073(17) 0.04288(10) 0.0356(4) Uani 1 1 d . . . H11A H -0.1042 0.0838 -0.0028 0.043 Uiso 1 1 calc R . . H11B H -0.1223 0.1708 0.0677 0.043 Uiso 1 1 calc R . . H11C H -0.0655 0.0552 0.0770 0.043 Uiso 1 1 calc R . . C12 C -0.03730(10) 0.29090(17) -0.04104(9) 0.0338(4) Uani 1 1 d . . . H12A H -0.0486 0.2434 -0.0866 0.041 Uiso 1 1 calc R . . H12B H 0.0049 0.3488 -0.0512 0.041 Uiso 1 1 calc R . . H12C H -0.0834 0.3369 -0.0258 0.041 Uiso 1 1 calc R . . C13 C 0.03153(9) 0.17378(15) 0.17944(9) 0.0291(3) Uani 1 1 d . . . H13 H -0.0218 0.1420 0.1892 0.035 Uiso 1 1 calc R . . C14 C 0.07885(11) 0.05986(17) 0.15831(11) 0.0425(5) Uani 1 1 d . . . H14A H 0.0725 -0.0036 0.1971 0.051 Uiso 1 1 calc R . . H14B H 0.1335 0.0825 0.1544 0.051 Uiso 1 1 calc R . . H14C H 0.0609 0.0277 0.1099 0.051 Uiso 1 1 calc R . . C15 C 0.05807(12) 0.22850(19) 0.25434(10) 0.0448(5) Uani 1 1 d . . . H15A H 0.0512 0.1672 0.2943 0.054 Uiso 1 1 calc R . . H15B H 0.0273 0.3020 0.2658 0.054 Uiso 1 1 calc R . . H15C H 0.1127 0.2514 0.2509 0.054 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 P 0.0196(2) 0.0242(2) 0.0202(2) -0.00121(15) 0.00134(14) -0.00063(14) S 0.0256(2) 0.0340(2) 0.0427(3) -0.01074(18) 0.00590(17) 0.00334(17) N 0.0223(6) 0.0325(7) 0.0243(7) -0.0026(5) 0.0017(5) 0.0029(5) C1 0.0212(7) 0.0245(7) 0.0201(7) 0.0024(6) 0.0009(6) -0.0011(6) C2 0.0211(7) 0.0269(8) 0.0237(8) 0.0037(6) 0.0038(6) -0.0008(6) C3 0.0221(8) 0.0313(8) 0.0288(8) 0.0026(7) 0.0002(6) -0.0001(6) C3A 0.0233(7) 0.0306(8) 0.0250(8) 0.0038(6) 0.0008(6) -0.0062(6) C4 0.0291(9) 0.0416(10) 0.0296(9) 0.0037(7) -0.0048(7) -0.0085(7) C5 0.0385(10) 0.0479(10) 0.0261(9) -0.0040(8) -0.0019(7) -0.0176(8) C6 0.0397(10) 0.0356(9) 0.0312(9) -0.0083(7) 0.0079(7) -0.0134(8) C7 0.0287(8) 0.0289(8) 0.0303(9) -0.0011(7) 0.0043(7) -0.0060(7) C7A 0.0249(7) 0.0268(8) 0.0220(8) 0.0026(6) 0.0019(6) -0.0079(6) C8 0.0261(8) 0.0344(9) 0.0405(10) -0.0062(7) 0.0026(7) 0.0034(7) C9 0.0424(10) 0.0507(11) 0.0234(9) -0.0010(8) 0.0020(7) 0.0090(9) C10 0.0243(8) 0.0294(8) 0.0229(8) -0.0037(6) 0.0003(6) -0.0005(6) C11 0.0330(9) 0.0397(9) 0.0339(9) -0.0061(8) -0.0005(7) -0.0117(8) C12 0.0294(9) 0.0454(10) 0.0267(9) 0.0021(8) -0.0051(7) -0.0002(7) C13 0.0291(8) 0.0359(9) 0.0224(8) 0.0062(7) 0.0015(6) -0.0063(7) C14 0.0466(11) 0.0395(10) 0.0414(10) 0.0178(9) 0.0025(9) 0.0061(8) C15 0.0555(12) 0.0558(12) 0.0230(9) 0.0101(8) -0.0030(8) -0.0214(10) _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 P C13 1.8346(16) . ? P C10 1.8347(15) . ? P C1 1.8728(15) . ? P S 1.9665(6) . ? N C2 1.392(2) . ? N C8 1.461(2) . ? N C9 1.461(2) . ? C1 C7A 1.522(2) . ? C1 C2 1.533(2) . ? C2 C3 1.351(2) . ? C3 C3A 1.450(2) . ? C3A C4 1.393(2) . ? C3A C7A 1.405(2) . ? C4 C5 1.384(3) . ? C5 C6 1.384(3) . ? C6 C7 1.399(2) . ? C7 C7A 1.386(2) . ? C10 C12 1.529(2) . ? C10 C11 1.537(2) . ? C13 C14 1.528(2) . ? C13 C15 1.529(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 C13 P C10 105.64(7) . . ? C13 P C1 110.44(7) . . ? C10 P C1 107.19(7) . . ? C13 P S 110.82(6) . . ? C10 P S 110.25(5) . . ? C1 P S 112.23(5) . . ? C2 N C8 114.89(13) . . ? C2 N C9 116.26(13) . . ? C8 N C9 110.88(13) . . ? C7A C1 C2 101.80(12) . . ? C7A C1 P 110.33(10) . . ? C2 C1 P 115.23(10) . . ? C3 C2 N 127.11(14) . . ? C3 C2 C1 110.20(13) . . ? N C2 C1 122.55(13) . . ? C2 C3 C3A 109.93(14) . . ? C4 C3A C7A 120.42(15) . . ? C4 C3A C3 130.47(15) . . ? C7A C3A C3 109.07(13) . . ? C5 C4 C3A 118.54(16) . . ? C6 C5 C4 121.22(16) . . ? C5 C6 C7 120.74(16) . . ? C7A C7 C6 118.41(16) . . ? C7 C7A C3A 120.63(15) . . ? C7 C7A C1 130.75(15) . . ? C3A C7A C1 108.62(13) . . ? C12 C10 C11 109.18(13) . . ? C12 C10 P 110.88(11) . . ? C11 C10 P 110.32(11) . . ? C14 C13 C15 111.49(15) . . ? C14 C13 P 115.44(12) . . ? C15 C13 P 113.62(12) . . ? 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 C13 P C1 C7A -61.12(12) . . . . ? C10 P C1 C7A -175.73(10) . . . . ? S P C1 C7A 63.08(11) . . . . ? C13 P C1 C2 53.44(13) . . . . ? C10 P C1 C2 -61.17(12) . . . . ? S P C1 C2 177.64(9) . . . . ? C8 N C2 C3 4.4(2) . . . . ? C9 N C2 C3 -127.42(17) . . . . ? C8 N C2 C1 -170.92(13) . . . . ? C9 N C2 C1 57.24(19) . . . . ? C7A C1 C2 C3 5.79(16) . . . . ? P C1 C2 C3 -113.61(13) . . . . ? C7A C1 C2 N -178.17(13) . . . . ? P C1 C2 N 62.44(17) . . . . ? N C2 C3 C3A -179.41(14) . . . . ? C1 C2 C3 C3A -3.58(17) . . . . ? C2 C3 C3A C4 -178.41(16) . . . . ? C2 C3 C3A C7A -0.42(18) . . . . ? C7A C3A C4 C5 -2.0(2) . . . . ? C3 C3A C4 C5 175.77(16) . . . . ? C3A C4 C5 C6 0.2(2) . . . . ? C4 C5 C6 C7 1.2(3) . . . . ? C5 C6 C7 C7A -0.8(2) . . . . ? C6 C7 C7A C3A -1.0(2) . . . . ? C6 C7 C7A C1 178.99(15) . . . . ? C4 C3A C7A C7 2.5(2) . . . . ? C3 C3A C7A C7 -175.76(13) . . . . ? C4 C3A C7A C1 -177.54(14) . . . . ? C3 C3A C7A C1 4.23(16) . . . . ? C2 C1 C7A C7 174.08(15) . . . . ? P C1 C7A C7 -63.12(19) . . . . ? C2 C1 C7A C3A -5.91(15) . . . . ? P C1 C7A C3A 116.89(12) . . . . ? C13 P C10 C12 171.32(11) . . . . ? C1 P C10 C12 -70.89(12) . . . . ? S P C10 C12 51.54(12) . . . . ? C13 P C10 C11 50.25(13) . . . . ? C1 P C10 C11 168.04(11) . . . . ? S P C10 C11 -69.54(12) . . . . ? C10 P C13 C14 50.45(14) . . . . ? C1 P C13 C14 -65.13(14) . . . . ? S P C13 C14 169.86(11) . . . . ? C10 P C13 C15 -178.96(13) . . . . ? C1 P C13 C15 65.46(14) . . . . ? S P C13 C15 -59.55(14) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.433 _refine_diff_density_min -0.178 _refine_diff_density_rms 0.046 #===END data_compound4 _database_code_depnum_ccdc_archive 'CCDC 244734' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H37 N P Rh S' _chemical_formula_weight 517.50 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' 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' Rh Rh -1.1178 0.9187 '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' 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 10.1379(7) _cell_length_b 12.4282(8) _cell_length_c 18.8478(13) _cell_angle_alpha 90.00 _cell_angle_beta 93.7628(11) _cell_angle_gamma 90.00 _cell_volume 2369.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 5212 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 26.37 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 0.888 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6002 _exptl_absorpt_correction_T_max 0.9323 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15830 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4830 _reflns_number_gt 4087 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'DIRDIF-96 (Beurskens et al., 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1997)' _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^)+(0.0406P)^2^+1.2457P] 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 4830 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0349 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0770 _refine_ls_wR_factor_gt 0.0735 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 Rh Rh 0.226552(17) -0.003238(13) 0.215617(9) 0.02248(7) Uani 1 1 d . . . S S 0.09809(6) -0.11269(6) 0.28852(3) 0.03435(16) Uani 1 1 d . . . P P 0.25200(6) -0.08424(5) 0.35896(3) 0.02176(13) Uani 1 1 d . . . N N 0.2118(2) 0.17774(17) 0.37100(11) 0.0349(5) Uani 1 1 d . . . C1 C 0.3412(2) 0.02132(18) 0.31956(12) 0.0234(5) Uani 1 1 d . . . C2 C 0.3289(2) 0.13444(19) 0.34671(12) 0.0274(5) Uani 1 1 d . . . C3 C 0.4491(3) 0.1841(2) 0.35001(13) 0.0338(6) Uani 1 1 d . . . H3 H 0.4653 0.2560 0.3654 0.041 Uiso 1 1 calc R . . C3A C 0.5471(2) 0.1114(2) 0.32673(13) 0.0313(5) Uani 1 1 d . . . C4 C 0.6827(3) 0.1259(3) 0.31788(15) 0.0428(7) Uani 1 1 d . . . H4 H 0.7236 0.1932 0.3288 0.051 Uiso 1 1 calc R . . C5 C 0.7554(3) 0.0427(3) 0.29348(16) 0.0485(8) Uani 1 1 d . . . H5 H 0.8475 0.0518 0.2891 0.058 Uiso 1 1 calc R . . C6 C 0.6962(3) -0.0542(3) 0.27513(16) 0.0427(7) Uani 1 1 d . . . H6 H 0.7482 -0.1111 0.2581 0.051 Uiso 1 1 calc R . . C7 C 0.5614(3) -0.0697(2) 0.28122(14) 0.0344(6) Uani 1 1 d . . . H7 H 0.5209 -0.1356 0.2663 0.041 Uiso 1 1 calc R . . C7A C 0.4866(2) 0.01174(18) 0.30924(13) 0.0262(5) Uani 1 1 d . . . C11 C 0.2953(3) 0.1388(2) 0.16838(13) 0.0319(5) Uani 1 1 d . . . H11 H 0.3428 0.1890 0.2027 0.038 Uiso 1 1 calc R . . C12 C 0.3723(3) 0.0529(2) 0.14751(13) 0.0341(6) Uani 1 1 d . . . H12 H 0.4643 0.0528 0.1702 0.041 Uiso 1 1 calc R . . C13 C 0.3606(3) 0.0016(2) 0.07429(16) 0.0466(7) Uani 1 1 d . . . H13A H 0.4483 -0.0259 0.0628 0.056 Uiso 1 1 calc R . . H13B H 0.3336 0.0572 0.0386 0.056 Uiso 1 1 calc R . . C14 C 0.2611(4) -0.0904(3) 0.06878(15) 0.0534(8) Uani 1 1 d . . . H14A H 0.2195 -0.0924 0.0198 0.064 Uiso 1 1 calc R . . H14B H 0.3090 -0.1591 0.0772 0.064 Uiso 1 1 calc R . . C15 C 0.1539(3) -0.0822(2) 0.12031(13) 0.0372(6) Uani 1 1 d . . . H15 H 0.1073 -0.1515 0.1284 0.045 Uiso 1 1 calc R . . C16 C 0.0772(3) 0.0087(2) 0.12930(15) 0.0374(6) Uani 1 1 d . . . H16 H -0.0147 -0.0066 0.1428 0.045 Uiso 1 1 calc R . . C17 C 0.0910(3) 0.1101(2) 0.08596(16) 0.0460(7) Uani 1 1 d . . . H17A H 0.0029 0.1437 0.0772 0.055 Uiso 1 1 calc R . . H17B H 0.1240 0.0909 0.0393 0.055 Uiso 1 1 calc R . . C18 C 0.1848(3) 0.1911(2) 0.12292(14) 0.0409(6) Uani 1 1 d . . . H18A H 0.2236 0.2365 0.0865 0.049 Uiso 1 1 calc R . . H18B H 0.1339 0.2387 0.1532 0.049 Uiso 1 1 calc R . . C21 C 0.1903(3) -0.0435(2) 0.44514(13) 0.0314(5) Uani 1 1 d . . . H21 H 0.1291 0.0181 0.4338 0.038 Uiso 1 1 calc R . . C22 C 0.2964(3) 0.0013(2) 0.49817(14) 0.0432(7) Uani 1 1 d . . . H22A H 0.3485 0.0555 0.4747 0.052 Uiso 1 1 calc R . . H22B H 0.3545 -0.0573 0.5157 0.052 Uiso 1 1 calc R . . H22C H 0.2543 0.0343 0.5382 0.052 Uiso 1 1 calc R . . C23 C 0.1056(3) -0.1288(2) 0.47806(16) 0.0466(7) Uani 1 1 d . . . H23A H 0.0369 -0.1532 0.4427 0.056 Uiso 1 1 calc R . . H23B H 0.0641 -0.0982 0.5190 0.056 Uiso 1 1 calc R . . H23C H 0.1612 -0.1900 0.4936 0.056 Uiso 1 1 calc R . . C24 C 0.3506(3) -0.20822(19) 0.36877(13) 0.0306(5) Uani 1 1 d . . . H24 H 0.3962 -0.2158 0.3235 0.037 Uiso 1 1 calc R . . C25 C 0.4607(3) -0.2031(2) 0.42805(15) 0.0418(7) Uani 1 1 d . . . H25A H 0.5120 -0.1370 0.4232 0.050 Uiso 1 1 calc R . . H25B H 0.5189 -0.2656 0.4247 0.050 Uiso 1 1 calc R . . H25C H 0.4218 -0.2035 0.4743 0.050 Uiso 1 1 calc R . . C26 C 0.2675(3) -0.3094(2) 0.37451(15) 0.0412(6) Uani 1 1 d . . . H26A H 0.1980 -0.3106 0.3358 0.049 Uiso 1 1 calc R . . H26B H 0.2270 -0.3099 0.4203 0.049 Uiso 1 1 calc R . . H26C H 0.3239 -0.3730 0.3711 0.049 Uiso 1 1 calc R . . C27 C 0.0953(3) 0.1839(2) 0.32269(15) 0.0391(6) Uani 1 1 d . . . H27A H 0.0227 0.2162 0.3472 0.047 Uiso 1 1 calc R . . H27B H 0.0700 0.1114 0.3066 0.047 Uiso 1 1 calc R . . H27C H 0.1142 0.2283 0.2816 0.047 Uiso 1 1 calc R . . C28 C 0.2277(3) 0.2760(3) 0.41268(17) 0.0543(9) Uani 1 1 d . . . H28A H 0.1412 0.2998 0.4271 0.065 Uiso 1 1 calc R . . H28B H 0.2661 0.3322 0.3839 0.065 Uiso 1 1 calc R . . H28C H 0.2864 0.2622 0.4551 0.065 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 Rh 0.02220(11) 0.02516(11) 0.02009(11) -0.00030(7) 0.00159(7) -0.00246(7) S 0.0280(3) 0.0438(4) 0.0306(3) 0.0072(3) -0.0031(3) -0.0139(3) P 0.0190(3) 0.0247(3) 0.0218(3) -0.0012(2) 0.0027(2) -0.0014(2) N 0.0428(13) 0.0321(11) 0.0299(11) -0.0058(9) 0.0022(10) 0.0101(10) C1 0.0207(11) 0.0250(11) 0.0245(11) -0.0026(9) 0.0013(9) 0.0010(9) C2 0.0323(13) 0.0285(12) 0.0212(11) 0.0001(9) 0.0008(10) 0.0015(10) C3 0.0438(16) 0.0294(12) 0.0276(12) -0.0047(10) -0.0019(11) -0.0089(11) C3A 0.0280(13) 0.0382(13) 0.0270(12) 0.0028(10) -0.0033(10) -0.0073(10) C4 0.0310(15) 0.0548(17) 0.0420(16) 0.0008(13) -0.0020(12) -0.0178(13) C5 0.0234(14) 0.072(2) 0.0503(18) 0.0104(16) 0.0041(13) -0.0053(14) C6 0.0286(14) 0.0518(17) 0.0490(16) 0.0138(13) 0.0129(12) 0.0101(12) C7 0.0272(13) 0.0347(13) 0.0421(14) 0.0070(11) 0.0090(11) 0.0029(10) C7A 0.0216(12) 0.0326(12) 0.0244(11) 0.0046(9) 0.0003(9) -0.0027(9) C11 0.0398(15) 0.0313(12) 0.0248(12) 0.0032(10) 0.0040(11) -0.0102(11) C12 0.0285(14) 0.0475(15) 0.0269(12) 0.0049(11) 0.0064(10) -0.0043(11) C13 0.0527(19) 0.0581(19) 0.0306(14) -0.0002(12) 0.0161(13) 0.0083(14) C14 0.079(2) 0.0504(18) 0.0312(15) -0.0108(13) 0.0081(15) 0.0040(17) C15 0.0478(17) 0.0361(14) 0.0267(12) -0.0042(11) -0.0052(11) -0.0103(12) C16 0.0305(14) 0.0484(16) 0.0319(13) 0.0069(11) -0.0080(11) -0.0092(12) C17 0.0427(17) 0.0483(16) 0.0459(16) 0.0152(13) -0.0064(13) 0.0032(13) C18 0.0528(18) 0.0353(14) 0.0348(14) 0.0066(11) 0.0050(13) 0.0025(13) C21 0.0348(14) 0.0342(12) 0.0261(12) 0.0000(10) 0.0098(11) 0.0028(11) C22 0.0549(19) 0.0510(17) 0.0238(13) -0.0067(11) 0.0039(12) -0.0009(14) C23 0.0571(19) 0.0427(16) 0.0432(16) 0.0010(13) 0.0278(14) -0.0028(14) C24 0.0350(14) 0.0303(12) 0.0276(12) 0.0018(10) 0.0092(10) 0.0032(10) C25 0.0372(16) 0.0457(16) 0.0421(15) 0.0062(13) -0.0008(12) 0.0107(12) C26 0.0511(18) 0.0310(13) 0.0431(15) 0.0046(11) 0.0149(13) 0.0010(12) C27 0.0312(14) 0.0411(15) 0.0457(16) -0.0078(12) 0.0068(12) 0.0067(11) C28 0.062(2) 0.0528(18) 0.0475(17) -0.0230(15) -0.0029(15) 0.0177(16) _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 Rh C11 2.116(2) . ? Rh C15 2.135(2) . ? Rh C12 2.137(3) . ? Rh C16 2.153(3) . ? Rh C1 2.233(2) . ? Rh S 2.3811(7) . ? S P 2.0127(8) . ? P C1 1.783(2) . ? P C24 1.840(2) . ? P C21 1.849(2) . ? N C2 1.407(3) . ? N C27 1.445(3) . ? N C28 1.455(3) . ? C1 C7A 1.504(3) . ? C1 C2 1.504(3) . ? C2 C3 1.364(4) . ? C3 C3A 1.434(4) . ? C3A C4 1.407(4) . ? C3A C7A 1.411(3) . ? C4 C5 1.366(5) . ? C5 C6 1.379(5) . ? C6 C7 1.392(4) . ? C7 C7A 1.390(4) . ? C11 C12 1.394(4) . ? C11 C18 1.512(4) . ? C12 C13 1.518(4) . ? C13 C14 1.524(5) . ? C14 C15 1.508(4) . ? C15 C16 1.388(4) . ? C16 C17 1.513(4) . ? C17 C18 1.522(4) . ? C21 C23 1.522(4) . ? C21 C22 1.525(4) . ? C24 C26 1.522(4) . ? C24 C25 1.528(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 C11 Rh C15 97.72(10) . . ? C11 Rh C12 38.26(10) . . ? C15 Rh C12 81.87(11) . . ? C11 Rh C16 81.92(10) . . ? C15 Rh C16 37.76(11) . . ? C12 Rh C16 90.19(10) . . ? C11 Rh C1 95.06(9) . . ? C15 Rh C1 158.78(10) . . ? C12 Rh C1 98.14(9) . . ? C16 Rh C1 162.44(10) . . ? C11 Rh S 158.03(8) . . ? C15 Rh S 92.96(8) . . ? C12 Rh S 163.56(8) . . ? C16 Rh S 95.23(8) . . ? C1 Rh S 81.07(6) . . ? P S Rh 81.41(3) . . ? C1 P C24 111.77(11) . . ? C1 P C21 111.99(11) . . ? C24 P C21 110.75(11) . . ? C1 P S 104.30(8) . . ? C24 P S 108.17(9) . . ? C21 P S 109.58(9) . . ? C2 N C27 119.2(2) . . ? C2 N C28 115.5(2) . . ? C27 N C28 110.7(2) . . ? C7A C1 C2 102.85(19) . . ? C7A C1 P 121.59(16) . . ? C2 C1 P 119.35(17) . . ? C7A C1 Rh 109.51(15) . . ? C2 C1 Rh 112.09(15) . . ? P C1 Rh 90.90(10) . . ? C3 C2 N 125.6(2) . . ? C3 C2 C1 110.1(2) . . ? N C2 C1 124.0(2) . . ? C2 C3 C3A 109.7(2) . . ? C4 C3A C7A 119.9(3) . . ? C4 C3A C3 131.1(2) . . ? C7A C3A C3 109.0(2) . . ? C5 C4 C3A 119.7(3) . . ? C4 C5 C6 120.7(3) . . ? C5 C6 C7 120.9(3) . . ? C7A C7 C6 119.6(3) . . ? C7 C7A C3A 119.2(2) . . ? C7 C7A C1 132.1(2) . . ? C3A C7A C1 108.4(2) . . ? C12 C11 C18 125.2(2) . . ? C12 C11 Rh 71.71(15) . . ? C18 C11 Rh 110.17(17) . . ? C11 C12 C13 124.5(2) . . ? C11 C12 Rh 70.03(14) . . ? C13 C12 Rh 113.13(19) . . ? C12 C13 C14 112.9(2) . . ? C15 C14 C13 114.0(2) . . ? C16 C15 C14 124.6(3) . . ? C16 C15 Rh 71.85(15) . . ? C14 C15 Rh 110.49(19) . . ? C15 C16 C17 122.6(3) . . ? C15 C16 Rh 70.39(14) . . ? C17 C16 Rh 112.32(18) . . ? C16 C17 C18 112.4(2) . . ? C11 C18 C17 113.1(2) . . ? C23 C21 C22 112.3(2) . . ? C23 C21 P 113.56(19) . . ? C22 C21 P 114.26(19) . . ? C26 C24 C25 111.3(2) . . ? C26 C24 P 113.54(18) . . ? C25 C24 P 113.88(18) . . ? 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 C11 Rh S P -91.07(18) . . . . ? C15 Rh S P 149.77(8) . . . . ? C12 Rh S P 78.7(3) . . . . ? C16 Rh S P -172.44(8) . . . . ? C1 Rh S P -9.75(6) . . . . ? Rh S P C1 12.48(8) . . . . ? Rh S P C24 -106.63(9) . . . . ? Rh S P C21 132.54(9) . . . . ? C24 P C1 C7A -10.2(2) . . . . ? C21 P C1 C7A 114.7(2) . . . . ? S P C1 C7A -126.87(18) . . . . ? C24 P C1 C2 -140.42(18) . . . . ? C21 P C1 C2 -15.5(2) . . . . ? S P C1 C2 102.94(18) . . . . ? C24 P C1 Rh 103.46(10) . . . . ? C21 P C1 Rh -131.60(10) . . . . ? S P C1 Rh -13.18(8) . . . . ? C11 Rh C1 C7A -66.75(16) . . . . ? C15 Rh C1 C7A 60.1(3) . . . . ? C12 Rh C1 C7A -28.34(17) . . . . ? C16 Rh C1 C7A -145.9(3) . . . . ? S Rh C1 C7A 135.05(15) . . . . ? C11 Rh C1 C2 46.73(18) . . . . ? C15 Rh C1 C2 173.6(2) . . . . ? C12 Rh C1 C2 85.14(18) . . . . ? C16 Rh C1 C2 -32.4(4) . . . . ? S Rh C1 C2 -111.47(17) . . . . ? C11 Rh C1 P 169.10(10) . . . . ? C15 Rh C1 P -64.0(3) . . . . ? C12 Rh C1 P -152.50(10) . . . . ? C16 Rh C1 P 89.9(3) . . . . ? S Rh C1 P 10.89(7) . . . . ? C27 N C2 C3 125.5(3) . . . . ? C28 N C2 C3 -10.1(4) . . . . ? C27 N C2 C1 -60.7(3) . . . . ? C28 N C2 C1 163.8(2) . . . . ? C7A C1 C2 C3 1.3(3) . . . . ? P C1 C2 C3 139.41(19) . . . . ? Rh C1 C2 C3 -116.25(19) . . . . ? C7A C1 C2 N -173.4(2) . . . . ? P C1 C2 N -35.3(3) . . . . ? Rh C1 C2 N 69.1(3) . . . . ? N C2 C3 C3A 174.3(2) . . . . ? C1 C2 C3 C3A -0.3(3) . . . . ? C2 C3 C3A C4 177.1(3) . . . . ? C2 C3 C3A C7A -1.0(3) . . . . ? C7A C3A C4 C5 -1.1(4) . . . . ? C3 C3A C4 C5 -179.0(3) . . . . ? C3A C4 C5 C6 2.2(4) . . . . ? C4 C5 C6 C7 -0.2(5) . . . . ? C5 C6 C7 C7A -3.0(4) . . . . ? C6 C7 C7A C3A 4.1(4) . . . . ? C6 C7 C7A C1 177.0(3) . . . . ? C4 C3A C7A C7 -2.1(4) . . . . ? C3 C3A C7A C7 176.2(2) . . . . ? C4 C3A C7A C1 -176.5(2) . . . . ? C3 C3A C7A C1 1.8(3) . . . . ? C2 C1 C7A C7 -175.3(3) . . . . ? P C1 C7A C7 47.8(4) . . . . ? Rh C1 C7A C7 -56.0(3) . . . . ? C2 C1 C7A C3A -1.8(2) . . . . ? P C1 C7A C3A -138.76(18) . . . . ? Rh C1 C7A C3A 117.50(18) . . . . ? C15 Rh C11 C12 -66.28(17) . . . . ? C16 Rh C11 C12 -100.69(16) . . . . ? C1 Rh C11 C12 96.73(15) . . . . ? S Rh C11 C12 175.37(14) . . . . ? C15 Rh C11 C18 55.5(2) . . . . ? C12 Rh C11 C18 121.7(2) . . . . ? C16 Rh C11 C18 21.05(19) . . . . ? C1 Rh C11 C18 -141.53(18) . . . . ? S Rh C11 C18 -62.9(3) . . . . ? C18 C11 C12 C13 2.7(4) . . . . ? Rh C11 C12 C13 104.9(3) . . . . ? C18 C11 C12 Rh -102.2(2) . . . . ? C15 Rh C12 C11 113.59(16) . . . . ? C16 Rh C12 C11 76.63(16) . . . . ? C1 Rh C12 C11 -87.85(15) . . . . ? S Rh C12 C11 -173.87(19) . . . . ? C11 Rh C12 C13 -120.0(3) . . . . ? C15 Rh C12 C13 -6.4(2) . . . . ? C16 Rh C12 C13 -43.4(2) . . . . ? C1 Rh C12 C13 152.2(2) . . . . ? S Rh C12 C13 66.1(3) . . . . ? C11 C12 C13 C14 -89.5(3) . . . . ? Rh C12 C13 C14 -8.5(3) . . . . ? C12 C13 C14 C15 26.1(4) . . . . ? C13 C14 C15 C16 50.7(4) . . . . ? C13 C14 C15 Rh -30.8(3) . . . . ? C11 Rh C15 C16 -66.02(18) . . . . ? C12 Rh C15 C16 -100.96(17) . . . . ? C1 Rh C15 C16 167.5(2) . . . . ? S Rh C15 C16 94.73(16) . . . . ? C11 Rh C15 C14 55.0(2) . . . . ? C12 Rh C15 C14 20.0(2) . . . . ? C16 Rh C15 C14 121.0(3) . . . . ? C1 Rh C15 C14 -71.5(3) . . . . ? S Rh C15 C14 -144.3(2) . . . . ? C14 C15 C16 C17 1.7(4) . . . . ? Rh C15 C16 C17 104.5(2) . . . . ? C14 C15 C16 Rh -102.8(3) . . . . ? C11 Rh C16 C15 113.87(18) . . . . ? C12 Rh C16 C15 76.39(17) . . . . ? C1 Rh C16 C15 -164.9(3) . . . . ? S Rh C16 C15 -88.07(16) . . . . ? C11 Rh C16 C17 -4.3(2) . . . . ? C15 Rh C16 C17 -118.2(3) . . . . ? C12 Rh C16 C17 -41.8(2) . . . . ? C1 Rh C16 C17 76.8(4) . . . . ? S Rh C16 C17 153.7(2) . . . . ? C15 C16 C17 C18 -93.7(3) . . . . ? Rh C16 C17 C18 -13.3(3) . . . . ? C12 C11 C18 C17 46.5(4) . . . . ? Rh C11 C18 C17 -34.9(3) . . . . ? C16 C17 C18 C11 31.8(4) . . . . ? C1 P C21 C23 176.1(2) . . . . ? C24 P C21 C23 -58.4(2) . . . . ? S P C21 C23 60.8(2) . . . . ? C1 P C21 C22 -53.3(2) . . . . ? C24 P C21 C22 72.2(2) . . . . ? S P C21 C22 -168.59(17) . . . . ? C1 P C24 C26 -157.76(18) . . . . ? C21 P C24 C26 76.6(2) . . . . ? S P C24 C26 -43.5(2) . . . . ? C1 P C24 C25 73.4(2) . . . . ? C21 P C24 C25 -52.2(2) . . . . ? S P C24 C25 -172.29(17) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.734 _refine_diff_density_min -0.274 _refine_diff_density_rms 0.078 #===END data_compound5 _database_code_depnum_ccdc_archive 'CCDC 244735' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H25 Mn N O3 P S' _chemical_formula_weight 445.38 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' Mn Mn 0.3368 0.7283 '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 9.688(2) _cell_length_b 15.570(4) _cell_length_c 13.898(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.494(4) _cell_angle_gamma 90.00 _cell_volume 2095.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 7660 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 26.39 _exptl_crystal_description fragment _exptl_crystal_colour yellow _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.412 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 0.825 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7027 _exptl_absorpt_correction_T_max 0.7781 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16327 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 26.39 _reflns_number_total 4273 _reflns_number_gt 3966 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'DIRDIF-96 (Beurskens et al., 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1997)' _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^)+(0.0401P)^2^+0.9334P] 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 4273 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0295 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0764 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 Mn Mn 0.06815(2) 0.099911(14) 0.306505(16) 0.02317(8) Uani 1 1 d . . . S S 0.31575(5) -0.07947(3) 0.14839(4) 0.04335(13) Uani 1 1 d . . . P P 0.38519(4) 0.01383(2) 0.23071(3) 0.02378(10) Uani 1 1 d . . . O11 O -0.04313(15) -0.06912(8) 0.24892(11) 0.0494(3) Uani 1 1 d . . . O12 O 0.13100(15) 0.04632(12) 0.50537(10) 0.0584(4) Uani 1 1 d . . . O13 O -0.20489(14) 0.16081(12) 0.36398(13) 0.0639(5) Uani 1 1 d . . . N N 0.34625(13) 0.18218(8) 0.39201(9) 0.0258(3) Uani 1 1 d . . . C1 C 0.14592(16) 0.22685(9) 0.28541(12) 0.0280(3) Uani 1 1 d . . . H1 H 0.1182 0.2791 0.3220 0.034 Uiso 1 1 calc R . . C2 C 0.25821(14) 0.17224(9) 0.30975(10) 0.0226(3) Uani 1 1 d . . . C3 C 0.26328(15) 0.10292(8) 0.23924(10) 0.0211(3) Uani 1 1 d . . . C3A C 0.15826(15) 0.12409(9) 0.16515(11) 0.0237(3) Uani 1 1 d . . . C4 C 0.11889(17) 0.08601(10) 0.07500(11) 0.0298(3) Uani 1 1 d . . . H4 H 0.1662 0.0369 0.0521 0.036 Uiso 1 1 calc R . . C5 C 0.01190(18) 0.12137(12) 0.02217(12) 0.0358(4) Uani 1 1 d . . . H5 H -0.0140 0.0963 -0.0379 0.043 Uiso 1 1 calc R . . C6 C -0.06117(18) 0.19420(12) 0.05457(14) 0.0401(4) Uani 1 1 d . . . H6 H -0.1357 0.2162 0.0163 0.048 Uiso 1 1 calc R . . C7 C -0.02684(18) 0.23310(11) 0.13917(14) 0.0370(4) Uani 1 1 d . . . H7 H -0.0765 0.2818 0.1604 0.044 Uiso 1 1 calc R . . C7A C 0.08602(15) 0.19900(9) 0.19571(12) 0.0276(3) Uani 1 1 d . . . C11 C 0.00171(17) -0.00439(10) 0.27097(12) 0.0322(3) Uani 1 1 d . . . C12 C 0.10476(17) 0.06551(12) 0.42715(13) 0.0370(4) Uani 1 1 d . . . C13 C -0.09917(17) 0.13613(12) 0.34092(13) 0.0378(4) Uani 1 1 d . . . C21 C 0.54608(16) 0.06146(11) 0.18435(11) 0.0315(3) Uani 1 1 d . . . H21 H 0.5994 0.0861 0.2404 0.038 Uiso 1 1 calc R . . C22 C 0.6378(2) -0.00594(15) 0.13697(15) 0.0496(5) Uani 1 1 d . . . H22A H 0.6577 -0.0524 0.1828 0.060 Uiso 1 1 calc R . . H22B H 0.7244 0.0209 0.1180 0.060 Uiso 1 1 calc R . . H22C H 0.5897 -0.0293 0.0798 0.060 Uiso 1 1 calc R . . C23 C 0.5143(2) 0.13472(13) 0.11375(13) 0.0424(4) Uani 1 1 d . . . H23A H 0.4561 0.1775 0.1448 0.051 Uiso 1 1 calc R . . H23B H 0.4656 0.1118 0.0566 0.051 Uiso 1 1 calc R . . H23C H 0.6008 0.1617 0.0947 0.051 Uiso 1 1 calc R . . C24 C 0.42284(17) -0.02219(10) 0.35535(11) 0.0298(3) Uani 1 1 d . . . H24 H 0.4079 0.0278 0.3990 0.036 Uiso 1 1 calc R . . C25 C 0.3246(2) -0.09365(13) 0.38473(17) 0.0501(5) Uani 1 1 d . . . H25A H 0.2290 -0.0744 0.3749 0.060 Uiso 1 1 calc R . . H25B H 0.3411 -0.1077 0.4528 0.060 Uiso 1 1 calc R . . H25C H 0.3406 -0.1447 0.3454 0.060 Uiso 1 1 calc R . . C26 C 0.5715(2) -0.05270(14) 0.37152(14) 0.0450(4) Uani 1 1 d . . . H26A H 0.6352 -0.0070 0.3531 0.054 Uiso 1 1 calc R . . H26B H 0.5876 -0.1038 0.3322 0.054 Uiso 1 1 calc R . . H26C H 0.5872 -0.0668 0.4396 0.054 Uiso 1 1 calc R . . C27 C 0.48224(18) 0.21501(13) 0.36935(14) 0.0435(4) Uani 1 1 d . . . H27A H 0.5381 0.2209 0.4288 0.052 Uiso 1 1 calc R . . H27B H 0.4726 0.2712 0.3381 0.052 Uiso 1 1 calc R . . H27C H 0.5276 0.1750 0.3259 0.052 Uiso 1 1 calc R . . C28 C 0.28801(19) 0.23584(12) 0.46704(13) 0.0394(4) Uani 1 1 d . . . H28A H 0.3536 0.2396 0.5217 0.047 Uiso 1 1 calc R . . H28B H 0.2015 0.2104 0.4883 0.047 Uiso 1 1 calc R . . H28C H 0.2699 0.2935 0.4414 0.047 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 Mn 0.01762(12) 0.02378(13) 0.02805(13) 0.00005(8) -0.00052(9) -0.00234(8) S 0.0462(3) 0.0317(2) 0.0512(3) -0.01946(19) -0.0177(2) 0.01067(18) P 0.02365(19) 0.02203(18) 0.02543(19) -0.00339(14) -0.00396(14) 0.00527(14) O11 0.0505(8) 0.0306(7) 0.0665(9) -0.0011(6) -0.0090(7) -0.0149(6) O12 0.0454(8) 0.0931(12) 0.0363(7) 0.0205(7) -0.0085(6) -0.0283(8) O13 0.0245(7) 0.0851(12) 0.0827(11) -0.0200(9) 0.0111(7) 0.0044(7) N 0.0222(6) 0.0238(6) 0.0311(6) -0.0065(5) -0.0038(5) -0.0009(5) C1 0.0242(7) 0.0198(7) 0.0400(8) -0.0017(6) -0.0015(6) 0.0007(5) C2 0.0192(7) 0.0189(6) 0.0297(7) -0.0004(5) 0.0009(5) -0.0017(5) C3 0.0182(7) 0.0193(6) 0.0255(7) 0.0005(5) -0.0008(5) -0.0001(5) C3A 0.0208(7) 0.0222(7) 0.0280(7) 0.0043(6) -0.0012(5) -0.0019(5) C4 0.0302(8) 0.0308(8) 0.0281(8) 0.0025(6) -0.0027(6) -0.0041(6) C5 0.0360(9) 0.0401(9) 0.0308(8) 0.0091(7) -0.0090(7) -0.0096(7) C6 0.0307(9) 0.0401(9) 0.0486(10) 0.0177(8) -0.0146(7) -0.0023(7) C7 0.0291(8) 0.0281(8) 0.0534(10) 0.0093(7) -0.0086(7) 0.0043(6) C7A 0.0232(7) 0.0216(7) 0.0379(8) 0.0045(6) -0.0030(6) -0.0003(5) C11 0.0290(8) 0.0309(8) 0.0366(9) 0.0049(6) -0.0036(7) -0.0038(6) C12 0.0245(8) 0.0489(10) 0.0375(9) 0.0049(7) -0.0004(7) -0.0146(7) C13 0.0237(8) 0.0457(10) 0.0440(10) -0.0068(8) 0.0005(7) -0.0042(7) C21 0.0238(8) 0.0425(9) 0.0282(8) -0.0001(7) 0.0011(6) 0.0062(6) C22 0.0387(10) 0.0667(13) 0.0438(10) -0.0043(9) 0.0086(8) 0.0215(9) C23 0.0375(10) 0.0535(11) 0.0367(9) 0.0113(8) 0.0072(7) 0.0039(8) C24 0.0371(9) 0.0241(7) 0.0281(7) 0.0024(6) -0.0034(6) 0.0044(6) C25 0.0504(12) 0.0394(10) 0.0603(13) 0.0219(9) -0.0050(10) -0.0019(8) C26 0.0424(10) 0.0529(11) 0.0391(10) 0.0111(8) -0.0125(8) 0.0084(8) C27 0.0249(8) 0.0559(11) 0.0499(10) -0.0198(9) 0.0011(7) -0.0108(8) C28 0.0356(9) 0.0435(10) 0.0390(9) -0.0176(8) -0.0007(7) -0.0016(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 Mn C12 1.7869(18) . ? Mn C13 1.7930(18) . ? Mn C11 1.8109(17) . ? Mn C3 2.1312(15) . ? Mn C1 2.1381(15) . ? Mn C2 2.1579(14) . ? Mn C7A 2.1899(15) . ? Mn C3A 2.2030(15) . ? S P 1.9575(6) . ? P C3 1.8277(14) . ? P C24 1.8481(16) . ? P C21 1.8566(17) . ? O11 C11 1.136(2) . ? O12 C12 1.150(2) . ? O13 C13 1.147(2) . ? N C2 1.4169(19) . ? N C27 1.455(2) . ? N C28 1.461(2) . ? C1 C2 1.415(2) . ? C1 C7A 1.429(2) . ? C2 C3 1.4595(19) . ? C3 C3A 1.466(2) . ? C3A C4 1.429(2) . ? C3A C7A 1.431(2) . ? C4 C5 1.370(2) . ? C5 C6 1.416(3) . ? C6 C7 1.356(3) . ? C7 C7A 1.432(2) . ? C21 C23 1.531(2) . ? C21 C22 1.534(2) . ? C24 C25 1.527(2) . ? C24 C26 1.528(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 C12 Mn C13 90.16(8) . . ? C12 Mn C11 92.72(8) . . ? C13 Mn C11 92.15(8) . . ? C12 Mn C3 105.16(7) . . ? C13 Mn C3 158.21(7) . . ? C11 Mn C3 102.31(7) . . ? C12 Mn C1 110.11(7) . . ? C13 Mn C1 94.02(7) . . ? C11 Mn C1 156.30(7) . . ? C3 Mn C1 66.41(5) . . ? C12 Mn C2 89.34(6) . . ? C13 Mn C2 127.38(7) . . ? C11 Mn C2 140.43(7) . . ? C3 Mn C2 39.78(5) . . ? C1 Mn C2 38.45(5) . . ? C12 Mn C7A 148.61(7) . . ? C13 Mn C7A 93.13(7) . . ? C11 Mn C7A 118.30(7) . . ? C3 Mn C7A 65.72(5) . . ? C1 Mn C7A 38.53(6) . . ? C2 Mn C7A 64.15(6) . . ? C12 Mn C3A 144.53(7) . . ? C13 Mn C3A 124.48(7) . . ? C11 Mn C3A 93.23(7) . . ? C3 Mn C3A 39.50(5) . . ? C1 Mn C3A 64.56(6) . . ? C2 Mn C3A 64.64(5) . . ? C7A Mn C3A 38.01(5) . . ? C3 P C24 106.36(7) . . ? C3 P C21 105.61(7) . . ? C24 P C21 107.43(8) . . ? C3 P S 112.85(5) . . ? C24 P S 112.28(6) . . ? C21 P S 111.86(6) . . ? C2 N C27 113.14(13) . . ? C2 N C28 113.75(12) . . ? C27 N C28 108.80(13) . . ? C2 C1 C7A 108.58(13) . . ? C2 C1 Mn 71.53(8) . . ? C7A C1 Mn 72.70(8) . . ? C1 C2 N 124.77(13) . . ? C1 C2 C3 108.85(13) . . ? N C2 C3 126.33(12) . . ? C1 C2 Mn 70.02(8) . . ? N C2 Mn 124.70(10) . . ? C3 C2 Mn 69.12(8) . . ? C2 C3 C3A 105.69(12) . . ? C2 C3 P 129.64(11) . . ? C3A C3 P 124.25(11) . . ? C2 C3 Mn 71.09(8) . . ? C3A C3 Mn 72.89(8) . . ? P C3 Mn 126.43(7) . . ? C4 C3A C7A 118.50(14) . . ? C4 C3A C3 133.40(14) . . ? C7A C3A C3 108.10(13) . . ? C4 C3A Mn 127.45(10) . . ? C7A C3A Mn 70.50(8) . . ? C3 C3A Mn 67.61(8) . . ? C5 C4 C3A 118.96(16) . . ? C4 C5 C6 121.92(16) . . ? C7 C6 C5 121.32(15) . . ? C6 C7 C7A 118.47(16) . . ? C1 C7A C3A 108.41(13) . . ? C1 C7A C7 130.80(15) . . ? C3A C7A C7 120.79(15) . . ? C1 C7A Mn 68.77(9) . . ? C3A C7A Mn 71.49(8) . . ? C7 C7A Mn 125.03(11) . . ? O11 C11 Mn 178.35(16) . . ? O12 C12 Mn 177.34(17) . . ? O13 C13 Mn 178.49(18) . . ? C23 C21 C22 110.10(15) . . ? C23 C21 P 111.30(11) . . ? C22 C21 P 112.11(14) . . ? C25 C24 C26 109.03(15) . . ? C25 C24 P 111.26(12) . . ? C26 C24 P 113.24(12) . . ? 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 C12 Mn C1 C2 61.27(11) . . . . ? C13 Mn C1 C2 152.91(10) . . . . ? C11 Mn C1 C2 -102.42(18) . . . . ? C3 Mn C1 C2 -37.02(9) . . . . ? C7A Mn C1 C2 -117.12(13) . . . . ? C3A Mn C1 C2 -80.57(9) . . . . ? C12 Mn C1 C7A 178.39(10) . . . . ? C13 Mn C1 C7A -89.97(10) . . . . ? C11 Mn C1 C7A 14.7(2) . . . . ? C3 Mn C1 C7A 80.10(9) . . . . ? C2 Mn C1 C7A 117.12(13) . . . . ? C3A Mn C1 C7A 36.55(8) . . . . ? C7A C1 C2 N 177.29(13) . . . . ? Mn C1 C2 N -119.01(14) . . . . ? C7A C1 C2 C3 -5.36(17) . . . . ? Mn C1 C2 C3 58.35(10) . . . . ? C7A C1 C2 Mn -63.70(10) . . . . ? C27 N C2 C1 -105.97(17) . . . . ? C28 N C2 C1 18.8(2) . . . . ? C27 N C2 C3 77.14(18) . . . . ? C28 N C2 C3 -158.04(14) . . . . ? C27 N C2 Mn 165.48(11) . . . . ? C28 N C2 Mn -69.70(16) . . . . ? C12 Mn C2 C1 -124.56(11) . . . . ? C13 Mn C2 C1 -34.87(13) . . . . ? C11 Mn C2 C1 141.96(11) . . . . ? C3 Mn C2 C1 120.43(12) . . . . ? C7A Mn C2 C1 38.03(9) . . . . ? C3A Mn C2 C1 80.36(10) . . . . ? C12 Mn C2 N -5.47(13) . . . . ? C13 Mn C2 N 84.22(14) . . . . ? C11 Mn C2 N -98.95(14) . . . . ? C3 Mn C2 N -120.47(15) . . . . ? C1 Mn C2 N 119.09(15) . . . . ? C7A Mn C2 N 157.13(13) . . . . ? C3A Mn C2 N -160.54(13) . . . . ? C12 Mn C2 C3 115.00(10) . . . . ? C13 Mn C2 C3 -155.31(10) . . . . ? C11 Mn C2 C3 21.52(13) . . . . ? C1 Mn C2 C3 -120.43(12) . . . . ? C7A Mn C2 C3 -82.40(9) . . . . ? C3A Mn C2 C3 -40.07(8) . . . . ? C1 C2 C3 C3A 6.32(15) . . . . ? N C2 C3 C3A -176.38(13) . . . . ? Mn C2 C3 C3A 65.22(9) . . . . ? C1 C2 C3 P 179.01(11) . . . . ? N C2 C3 P -3.7(2) . . . . ? Mn C2 C3 P -122.10(12) . . . . ? C1 C2 C3 Mn -58.89(10) . . . . ? N C2 C3 Mn 118.41(14) . . . . ? C24 P C3 C2 38.87(15) . . . . ? C21 P C3 C2 -75.09(14) . . . . ? S P C3 C2 162.41(11) . . . . ? C24 P C3 C3A -149.66(12) . . . . ? C21 P C3 C3A 96.38(13) . . . . ? S P C3 C3A -26.12(13) . . . . ? C24 P C3 Mn -56.20(11) . . . . ? C21 P C3 Mn -170.16(9) . . . . ? S P C3 Mn 67.33(10) . . . . ? C12 Mn C3 C2 -69.87(10) . . . . ? C13 Mn C3 C2 63.4(2) . . . . ? C11 Mn C3 C2 -166.16(9) . . . . ? C1 Mn C3 C2 35.81(8) . . . . ? C7A Mn C3 C2 78.12(9) . . . . ? C3A Mn C3 C2 113.86(11) . . . . ? C12 Mn C3 C3A 176.27(9) . . . . ? C13 Mn C3 C3A -50.5(2) . . . . ? C11 Mn C3 C3A 79.98(9) . . . . ? C1 Mn C3 C3A -78.05(9) . . . . ? C2 Mn C3 C3A -113.86(11) . . . . ? C7A Mn C3 C3A -35.74(8) . . . . ? C12 Mn C3 P 55.95(11) . . . . ? C13 Mn C3 P -170.79(15) . . . . ? C11 Mn C3 P -40.34(11) . . . . ? C1 Mn C3 P 161.63(11) . . . . ? C2 Mn C3 P 125.82(13) . . . . ? C7A Mn C3 P -156.06(11) . . . . ? C3A Mn C3 P -120.32(13) . . . . ? C2 C3 C3A C4 174.98(15) . . . . ? P C3 C3A C4 1.8(2) . . . . ? Mn C3 C3A C4 -121.04(17) . . . . ? C2 C3 C3A C7A -4.95(15) . . . . ? P C3 C3A C7A -178.13(10) . . . . ? Mn C3 C3A C7A 59.04(10) . . . . ? C2 C3 C3A Mn -63.99(9) . . . . ? P C3 C3A Mn 122.83(11) . . . . ? C12 Mn C3A C4 122.13(16) . . . . ? C13 Mn C3A C4 -71.98(16) . . . . ? C11 Mn C3A C4 22.85(14) . . . . ? C3 Mn C3A C4 128.35(17) . . . . ? C1 Mn C3A C4 -148.53(15) . . . . ? C2 Mn C3A C4 168.71(15) . . . . ? C7A Mn C3A C4 -111.49(17) . . . . ? C12 Mn C3A C7A -126.38(13) . . . . ? C13 Mn C3A C7A 39.51(12) . . . . ? C11 Mn C3A C7A 134.35(10) . . . . ? C3 Mn C3A C7A -120.16(12) . . . . ? C1 Mn C3A C7A -37.04(9) . . . . ? C2 Mn C3A C7A -79.80(9) . . . . ? C12 Mn C3A C3 -6.22(15) . . . . ? C13 Mn C3A C3 159.67(9) . . . . ? C11 Mn C3A C3 -105.50(9) . . . . ? C1 Mn C3A C3 83.12(9) . . . . ? C2 Mn C3A C3 40.36(8) . . . . ? C7A Mn C3A C3 120.16(12) . . . . ? C7A C3A C4 C5 -1.3(2) . . . . ? C3 C3A C4 C5 178.74(15) . . . . ? Mn C3A C4 C5 85.07(18) . . . . ? C3A C4 C5 C6 -0.3(2) . . . . ? C4 C5 C6 C7 1.0(3) . . . . ? C5 C6 C7 C7A 0.1(3) . . . . ? C2 C1 C7A C3A 2.17(17) . . . . ? Mn C1 C7A C3A -60.78(10) . . . . ? C2 C1 C7A C7 -178.49(16) . . . . ? Mn C1 C7A C7 118.56(18) . . . . ? C2 C1 C7A Mn 62.95(10) . . . . ? C4 C3A C7A C1 -178.11(13) . . . . ? C3 C3A C7A C1 1.83(16) . . . . ? Mn C3A C7A C1 59.08(10) . . . . ? C4 C3A C7A C7 2.5(2) . . . . ? C3 C3A C7A C7 -177.59(14) . . . . ? Mn C3A C7A C7 -120.34(15) . . . . ? C4 C3A C7A Mn 122.81(13) . . . . ? C3 C3A C7A Mn -57.25(10) . . . . ? C6 C7 C7A C1 178.86(16) . . . . ? C6 C7 C7A C3A -1.9(2) . . . . ? C6 C7 C7A Mn -89.9(2) . . . . ? C12 Mn C7A C1 -2.91(17) . . . . ? C13 Mn C7A C1 92.53(10) . . . . ? C11 Mn C7A C1 -173.35(9) . . . . ? C3 Mn C7A C1 -82.05(9) . . . . ? C2 Mn C7A C1 -37.95(9) . . . . ? C3A Mn C7A C1 -119.16(12) . . . . ? C12 Mn C7A C3A 116.25(15) . . . . ? C13 Mn C7A C3A -148.32(10) . . . . ? C11 Mn C7A C3A -54.19(11) . . . . ? C3 Mn C7A C3A 37.11(8) . . . . ? C1 Mn C7A C3A 119.16(12) . . . . ? C2 Mn C7A C3A 81.20(9) . . . . ? C12 Mn C7A C7 -128.62(17) . . . . ? C13 Mn C7A C7 -33.19(16) . . . . ? C11 Mn C7A C7 60.94(16) . . . . ? C3 Mn C7A C7 152.24(16) . . . . ? C1 Mn C7A C7 -125.72(18) . . . . ? C2 Mn C7A C7 -163.67(16) . . . . ? C3A Mn C7A C7 115.13(18) . . . . ? C12 Mn C11 O11 99(5) . . . . ? C13 Mn C11 O11 9(5) . . . . ? C3 Mn C11 O11 -154(5) . . . . ? C1 Mn C11 O11 -96(5) . . . . ? C2 Mn C11 O11 -168(5) . . . . ? C7A Mn C11 O11 -85(5) . . . . ? C3A Mn C11 O11 -116(5) . . . . ? C13 Mn C12 O12 -97(4) . . . . ? C11 Mn C12 O12 171(4) . . . . ? C3 Mn C12 O12 67(4) . . . . ? C1 Mn C12 O12 -3(4) . . . . ? C2 Mn C12 O12 30(4) . . . . ? C7A Mn C12 O12 -1(4) . . . . ? C3A Mn C12 O12 71(4) . . . . ? C12 Mn C13 O13 73(8) . . . . ? C11 Mn C13 O13 166(8) . . . . ? C3 Mn C13 O13 -62(8) . . . . ? C1 Mn C13 O13 -37(8) . . . . ? C2 Mn C13 O13 -16(8) . . . . ? C7A Mn C13 O13 -76(8) . . . . ? C3A Mn C13 O13 -99(8) . . . . ? C3 P C21 C23 -34.28(14) . . . . ? C24 P C21 C23 -147.50(12) . . . . ? S P C21 C23 88.85(13) . . . . ? C3 P C21 C22 -158.10(12) . . . . ? C24 P C21 C22 88.68(13) . . . . ? S P C21 C22 -34.97(14) . . . . ? C3 P C24 C25 91.61(14) . . . . ? C21 P C24 C25 -155.67(13) . . . . ? S P C24 C25 -32.28(14) . . . . ? C3 P C24 C26 -145.16(12) . . . . ? C21 P C24 C26 -32.45(14) . . . . ? S P C24 C26 90.95(13) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.364 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.049 #===END