Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Derek Woollins' 'Stephen M. Aucott' 'Colin J. Burchell' 'Heather L. Milton' 'Alexandra M. Z. Slawin' _publ_contact_author_name 'Prof Derek Woollins' _publ_contact_author_address ; School of Chemistry St Andrews St Andrews Fife KY16 9ST UNITED KINGDOM ; _publ_contact_author_email JDW3@ST-AND.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis and Characterisation of Cyanodithioimidocarbonate [C2N2S2]2- Complexes ; data_8 _database_code_depnum_ccdc_archive 'CCDC 224724' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[C34 H28 Fe P2].Pt.[C2 N2 S2]' _chemical_formula_sum 'C36 H28 Fe N2 P2 Pt S2' _chemical_formula_weight 865.60 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' 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' Pt Pt -1.7033 8.3905 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3113(13) _cell_length_b 9.5996(13) _cell_length_c 18.070(2) _cell_angle_alpha 99.062(2) _cell_angle_beta 95.808(2) _cell_angle_gamma 101.906(2) _cell_volume 1545.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 88 _cell_measurement_theta_min 12 _cell_measurement_theta_max 28 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.860 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 5.259 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.805340 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7914 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0582 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 23.32 _reflns_number_total 4411 _reflns_number_gt 3639 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0355P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4411 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0440 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0677 _refine_ls_wR_factor_gt 0.0655 _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_restrained_S_all 0.971 _refine_ls_shift/su_max 0.002 _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 Pt1 Pt 0.66584(3) 0.64428(3) 0.734441(15) 0.01669(9) Uani 1 1 d . . . S1 S 0.57879(19) 0.45442(17) 0.79668(9) 0.0220(4) Uani 1 1 d . . . S2 S 0.4913(2) 0.47327(19) 0.64380(10) 0.0279(4) Uani 1 1 d . . . C1 C 0.4680(7) 0.3655(7) 0.7118(4) 0.0201(15) Uani 1 1 d . . . N1 N 0.3792(6) 0.2377(6) 0.6986(3) 0.0260(14) Uani 1 1 d . . . C2 C 0.3676(8) 0.1663(8) 0.7553(4) 0.0306(18) Uani 1 1 d . . . N2 N 0.3473(7) 0.0901(6) 0.7998(4) 0.0410(17) Uani 1 1 d . . . P1 P 0.82385(19) 0.77185(18) 0.83826(9) 0.0168(4) Uani 1 1 d . . . C3 C 0.8245(7) 0.9611(7) 0.8627(3) 0.0187(15) Uani 1 1 d . . . C4 C 0.6953(8) 1.0175(7) 0.8560(3) 0.0206(16) Uani 1 1 d . . . H4A H 0.5970 0.9631 0.8386 0.025 Uiso 1 1 calc R . . C5 C 0.7402(8) 1.1718(7) 0.8804(3) 0.0239(17) Uani 1 1 d . . . H5A H 0.6768 1.2378 0.8827 0.029 Uiso 1 1 calc R . . C6 C 0.8938(8) 1.2067(7) 0.9000(3) 0.0235(16) Uani 1 1 d . . . H6A H 0.9524 1.3021 0.9171 0.028 Uiso 1 1 calc R . . C7 C 0.9486(7) 1.0818(7) 0.8908(3) 0.0212(16) Uani 1 1 d . . . H7A H 1.0494 1.0768 0.9012 0.025 Uiso 1 1 calc R . . Fe1 Fe 0.84220(10) 1.10050(9) 0.79050(5) 0.0185(2) Uani 1 1 d . . . C8 C 0.8025(7) 0.9900(6) 0.6834(3) 0.0174(15) Uani 1 1 d . . . C9 C 0.9570(7) 1.0377(7) 0.7081(4) 0.0210(16) Uani 1 1 d . . . H9A H 1.0263 0.9782 0.7119 0.025 Uiso 1 1 calc R . . C10 C 0.9885(8) 1.1915(7) 0.7262(4) 0.0240(17) Uani 1 1 d . . . H10A H 1.0837 1.2530 0.7439 0.029 Uiso 1 1 calc R . . C11 C 0.8566(8) 1.2375(7) 0.7135(4) 0.0250(17) Uani 1 1 d . . . H11A H 0.8470 1.3352 0.7211 0.030 Uiso 1 1 calc R . . C12 C 0.7396(7) 1.1135(7) 0.6874(3) 0.0223(16) Uani 1 1 d . . . H12A H 0.6379 1.1131 0.6749 0.027 Uiso 1 1 calc R . . C13 C 1.0136(7) 0.7563(7) 0.8367(4) 0.0186(15) Uani 1 1 d . . . C14 C 1.0543(7) 0.6820(7) 0.7740(4) 0.0199(16) Uani 1 1 d . . . H14A H 0.9835 0.6451 0.7300 0.024 Uiso 1 1 calc R . . C15 C 1.1987(8) 0.6590(7) 0.7735(5) 0.036(2) Uani 1 1 d . . . H15A H 1.2237 0.6062 0.7295 0.043 Uiso 1 1 calc R . . C16 C 1.3026(8) 0.7115(8) 0.8355(4) 0.0307(18) Uani 1 1 d . . . H16A H 1.4000 0.6956 0.8353 0.037 Uiso 1 1 calc R . . C17 C 1.2630(8) 0.7905(8) 0.9004(4) 0.0321(19) Uani 1 1 d . . . H17A H 1.3350 0.8303 0.9437 0.039 Uiso 1 1 calc R . . C18 C 1.1213(7) 0.8095(7) 0.9009(4) 0.0230(16) Uani 1 1 d . . . H18A H 1.0952 0.8596 0.9454 0.028 Uiso 1 1 calc R . . C19 C 0.7792(7) 0.7050(6) 0.9243(3) 0.0168(15) Uani 1 1 d . . . C20 C 0.8210(7) 0.5808(7) 0.9402(4) 0.0213(16) Uani 1 1 d . . . H20A H 0.8788 0.5347 0.9081 0.026 Uiso 1 1 calc R . . C21 C 0.7789(8) 0.5239(7) 1.0024(4) 0.0269(17) Uani 1 1 d . . . H21A H 0.8098 0.4400 1.0131 0.032 Uiso 1 1 calc R . . C22 C 0.6949(8) 0.5855(8) 1.0479(4) 0.0309(19) Uani 1 1 d . . . H22A H 0.6670 0.5449 1.0905 0.037 Uiso 1 1 calc R . . C23 C 0.6487(8) 0.7084(8) 1.0330(4) 0.0330(19) Uani 1 1 d . . . H23A H 0.5879 0.7512 1.0646 0.040 Uiso 1 1 calc R . . C24 C 0.6928(7) 0.7674(7) 0.9715(4) 0.0233(16) Uani 1 1 d . . . H24A H 0.6631 0.8523 0.9616 0.028 Uiso 1 1 calc R . . P2 P 0.70255(19) 0.80137(18) 0.65192(9) 0.0178(4) Uani 1 1 d . . . C25 C 0.5202(7) 0.8178(6) 0.6122(4) 0.0191(16) Uani 1 1 d . . . C26 C 0.4242(8) 0.8466(8) 0.6599(4) 0.0302(18) Uani 1 1 d . . . H26A H 0.4523 0.8590 0.7129 0.036 Uiso 1 1 calc R . . C27 C 0.2807(8) 0.8587(8) 0.6309(5) 0.036(2) Uani 1 1 d . . . H27A H 0.2135 0.8783 0.6653 0.044 Uiso 1 1 calc R . . C28 C 0.2380(8) 0.8436(7) 0.5575(5) 0.0326(19) Uani 1 1 d . . . H28A H 0.1421 0.8539 0.5393 0.039 Uiso 1 1 calc R . . C29 C 0.3390(9) 0.8112(8) 0.5059(4) 0.038(2) Uani 1 1 d . . . H29A H 0.3100 0.7993 0.4529 0.046 Uiso 1 1 calc R . . C30 C 0.4776(8) 0.7976(7) 0.5331(4) 0.0298(18) Uani 1 1 d . . . H30A H 0.5443 0.7748 0.4991 0.036 Uiso 1 1 calc R . . C31 C 0.7890(7) 0.7457(7) 0.5700(3) 0.0199(16) Uani 1 1 d . . . C32 C 0.8295(7) 0.8432(7) 0.5232(4) 0.0196(15) Uani 1 1 d . . . H32A H 0.8245 0.9415 0.5376 0.024 Uiso 1 1 calc R . . C33 C 0.8779(7) 0.7974(7) 0.4543(4) 0.0226(16) Uani 1 1 d . . . H33A H 0.9049 0.8647 0.4220 0.027 Uiso 1 1 calc R . . C34 C 0.8864(7) 0.6560(8) 0.4334(4) 0.0286(18) Uani 1 1 d . . . H34A H 0.9180 0.6244 0.3866 0.034 Uiso 1 1 calc R . . C35 C 0.8480(7) 0.5596(7) 0.4818(4) 0.0258(17) Uani 1 1 d . . . H35A H 0.8554 0.4620 0.4676 0.031 Uiso 1 1 calc R . . C36 C 0.7999(7) 0.6008(7) 0.5493(4) 0.0238(16) Uani 1 1 d . . . H36A H 0.7743 0.5331 0.5815 0.029 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 Pt1 0.01980(15) 0.01794(14) 0.01443(14) 0.00601(10) 0.00258(11) 0.00659(10) S1 0.0271(10) 0.0199(9) 0.0195(9) 0.0066(7) 0.0034(8) 0.0040(8) S2 0.0304(11) 0.0280(10) 0.0216(10) 0.0094(8) -0.0038(9) -0.0017(8) C1 0.021(4) 0.024(4) 0.020(4) 0.011(3) 0.000(3) 0.011(3) N1 0.030(4) 0.022(3) 0.028(3) 0.007(3) 0.008(3) 0.006(3) C2 0.019(4) 0.028(4) 0.040(5) -0.003(4) 0.002(4) 0.003(3) N2 0.048(4) 0.027(4) 0.047(4) 0.009(3) 0.010(4) 0.002(3) P1 0.0206(10) 0.0181(9) 0.0156(9) 0.0078(7) 0.0042(8) 0.0087(8) C3 0.026(4) 0.025(4) 0.009(3) 0.006(3) 0.005(3) 0.011(3) C4 0.028(4) 0.020(4) 0.019(4) 0.011(3) 0.009(3) 0.010(3) C5 0.044(5) 0.018(4) 0.015(4) 0.005(3) 0.011(3) 0.015(3) C6 0.033(4) 0.023(4) 0.014(4) 0.006(3) 0.002(3) 0.004(3) C7 0.024(4) 0.020(4) 0.018(4) 0.005(3) -0.005(3) 0.004(3) Fe1 0.0226(6) 0.0179(5) 0.0169(5) 0.0055(4) 0.0038(4) 0.0069(4) C8 0.022(4) 0.018(4) 0.016(3) 0.009(3) 0.003(3) 0.009(3) C9 0.024(4) 0.017(4) 0.023(4) 0.000(3) 0.005(3) 0.009(3) C10 0.029(4) 0.024(4) 0.017(4) 0.002(3) 0.008(3) -0.001(3) C11 0.032(4) 0.026(4) 0.021(4) 0.012(3) 0.014(3) 0.006(3) C12 0.025(4) 0.031(4) 0.015(4) 0.011(3) 0.006(3) 0.009(3) C13 0.018(4) 0.021(4) 0.021(4) 0.012(3) 0.005(3) 0.006(3) C14 0.016(4) 0.022(4) 0.020(4) 0.004(3) 0.002(3) 0.000(3) C15 0.037(5) 0.025(4) 0.051(5) 0.009(4) 0.028(4) 0.008(4) C16 0.015(4) 0.033(4) 0.045(5) 0.013(4) 0.004(4) 0.001(3) C17 0.029(5) 0.032(4) 0.040(5) 0.023(4) 0.002(4) 0.007(4) C18 0.032(4) 0.021(4) 0.024(4) 0.013(3) 0.013(4) 0.015(3) C19 0.018(4) 0.019(4) 0.012(3) 0.002(3) 0.003(3) 0.002(3) C20 0.029(4) 0.020(4) 0.016(4) 0.000(3) 0.006(3) 0.009(3) C21 0.037(5) 0.023(4) 0.020(4) 0.009(3) -0.002(4) 0.005(3) C22 0.036(5) 0.037(5) 0.017(4) 0.013(3) 0.003(4) -0.003(4) C23 0.038(5) 0.045(5) 0.018(4) 0.005(4) 0.010(4) 0.012(4) C24 0.025(4) 0.025(4) 0.025(4) 0.008(3) 0.007(3) 0.012(3) P2 0.0194(10) 0.0210(9) 0.0155(9) 0.0064(8) 0.0039(8) 0.0072(8) C25 0.018(4) 0.017(4) 0.021(4) 0.006(3) -0.009(3) 0.005(3) C26 0.030(4) 0.040(5) 0.019(4) 0.004(3) 0.000(4) 0.008(4) C27 0.029(5) 0.031(4) 0.050(6) 0.002(4) 0.011(4) 0.011(4) C28 0.023(4) 0.020(4) 0.054(5) 0.018(4) -0.013(4) 0.005(3) C29 0.039(5) 0.040(5) 0.030(5) 0.013(4) -0.023(4) 0.003(4) C30 0.022(4) 0.036(4) 0.032(4) 0.004(4) 0.013(4) 0.006(3) C31 0.017(4) 0.022(4) 0.019(4) 0.002(3) 0.001(3) 0.003(3) C32 0.018(4) 0.021(4) 0.020(4) 0.001(3) 0.002(3) 0.007(3) C33 0.019(4) 0.028(4) 0.018(4) 0.012(3) -0.002(3) -0.004(3) C34 0.019(4) 0.043(5) 0.021(4) -0.003(3) 0.005(3) 0.005(3) C35 0.025(4) 0.023(4) 0.026(4) -0.003(3) 0.002(3) 0.004(3) C36 0.029(4) 0.024(4) 0.025(4) 0.014(3) 0.006(3) 0.013(3) _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 Pt1 P1 2.2711(17) . ? Pt1 P2 2.2833(17) . ? Pt1 S1 2.3375(16) . ? Pt1 S2 2.3519(17) . ? S1 C1 1.747(6) . ? S2 C1 1.729(6) . ? C1 N1 1.302(8) . ? N1 C2 1.320(9) . ? C2 N2 1.173(9) . ? P1 C3 1.799(6) . ? P1 C13 1.806(7) . ? P1 C19 1.828(6) . ? C3 C4 1.419(9) . ? C3 C7 1.442(9) . ? C3 Fe1 2.005(6) . ? C4 C5 1.437(9) . ? C4 Fe1 2.020(6) . ? C4 H4A 0.9500 . ? C5 C6 1.395(9) . ? C5 Fe1 2.059(7) . ? C5 H5A 0.9500 . ? C6 C7 1.391(9) . ? C6 Fe1 2.038(6) . ? C6 H6A 0.9500 . ? C7 Fe1 2.028(6) . ? C7 H7A 0.9500 . ? Fe1 C9 2.007(7) . ? Fe1 C8 2.013(6) . ? Fe1 C10 2.030(6) . ? Fe1 C12 2.040(6) . ? Fe1 C11 2.055(6) . ? C8 C9 1.419(9) . ? C8 C12 1.422(9) . ? C8 P2 1.828(6) . ? C9 C10 1.422(9) . ? C9 H9A 0.9500 . ? C10 C11 1.398(9) . ? C10 H10A 0.9500 . ? C11 C12 1.418(9) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.370(9) . ? C13 C18 1.407(9) . ? C14 C15 1.407(9) . ? C14 H14A 0.9500 . ? C15 C16 1.358(10) . ? C15 H15A 0.9500 . ? C16 C17 1.417(10) . ? C16 H16A 0.9500 . ? C17 C18 1.370(9) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C24 1.382(9) . ? C19 C20 1.390(9) . ? C20 C21 1.381(9) . ? C20 H20A 0.9500 . ? C21 C22 1.344(9) . ? C21 H21A 0.9500 . ? C22 C23 1.392(10) . ? C22 H22A 0.9500 . ? C23 C24 1.385(9) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? P2 C31 1.815(7) . ? P2 C25 1.823(6) . ? C25 C26 1.341(9) . ? C25 C30 1.417(9) . ? C26 C27 1.419(10) . ? C26 H26A 0.9500 . ? C27 C28 1.321(10) . ? C27 H27A 0.9500 . ? C28 C29 1.435(10) . ? C28 H28A 0.9500 . ? C29 C30 1.373(10) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C32 1.379(8) . ? C31 C36 1.409(9) . ? C32 C33 1.403(9) . ? C32 H32A 0.9500 . ? C33 C34 1.372(9) . ? C33 H33A 0.9500 . ? C34 C35 1.388(9) . ? C34 H34A 0.9500 . ? C35 C36 1.370(9) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? 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 P1 Pt1 P2 101.04(6) . . ? P1 Pt1 S1 92.68(6) . . ? P2 Pt1 S1 165.98(6) . . ? P1 Pt1 S2 167.33(6) . . ? P2 Pt1 S2 91.63(6) . . ? S1 Pt1 S2 74.68(6) . . ? C1 S1 Pt1 87.7(2) . . ? C1 S2 Pt1 87.7(2) . . ? N1 C1 S2 122.9(5) . . ? N1 C1 S1 127.3(5) . . ? S2 C1 S1 109.9(3) . . ? C1 N1 C2 117.6(6) . . ? N2 C2 N1 172.4(8) . . ? C3 P1 C13 107.8(3) . . ? C3 P1 C19 102.4(3) . . ? C13 P1 C19 102.4(3) . . ? C3 P1 Pt1 116.4(2) . . ? C13 P1 Pt1 114.2(2) . . ? C19 P1 Pt1 112.0(2) . . ? C4 C3 C7 107.4(6) . . ? C4 C3 P1 123.9(5) . . ? C7 C3 P1 128.7(5) . . ? C4 C3 Fe1 69.9(3) . . ? C7 C3 Fe1 69.9(3) . . ? P1 C3 Fe1 124.9(3) . . ? C3 C4 C5 107.6(6) . . ? C3 C4 Fe1 68.8(4) . . ? C5 C4 Fe1 70.8(4) . . ? C3 C4 H4A 126.2 . . ? C5 C4 H4A 126.2 . . ? Fe1 C4 H4A 125.8 . . ? C6 C5 C4 107.4(6) . . ? C6 C5 Fe1 69.3(4) . . ? C4 C5 Fe1 67.9(4) . . ? C6 C5 H5A 126.3 . . ? C4 C5 H5A 126.3 . . ? Fe1 C5 H5A 128.0 . . ? C7 C6 C5 110.2(6) . . ? C7 C6 Fe1 69.6(4) . . ? C5 C6 Fe1 70.9(4) . . ? C7 C6 H6A 124.9 . . ? C5 C6 H6A 124.9 . . ? Fe1 C6 H6A 126.2 . . ? C6 C7 C3 107.4(6) . . ? C6 C7 Fe1 70.4(4) . . ? C3 C7 Fe1 68.2(3) . . ? C6 C7 H7A 126.3 . . ? C3 C7 H7A 126.3 . . ? Fe1 C7 H7A 126.7 . . ? C3 Fe1 C9 110.2(3) . . ? C3 Fe1 C8 109.6(2) . . ? C9 Fe1 C8 41.3(3) . . ? C3 Fe1 C4 41.3(2) . . ? C9 Fe1 C4 140.9(3) . . ? C8 Fe1 C4 112.7(3) . . ? C3 Fe1 C7 41.9(2) . . ? C9 Fe1 C7 108.4(3) . . ? C8 Fe1 C7 136.7(3) . . ? C4 Fe1 C7 69.4(3) . . ? C3 Fe1 C10 140.2(3) . . ? C9 Fe1 C10 41.3(2) . . ? C8 Fe1 C10 68.8(3) . . ? C4 Fe1 C10 177.8(3) . . ? C7 Fe1 C10 110.7(3) . . ? C3 Fe1 C6 68.8(3) . . ? C9 Fe1 C6 135.7(3) . . ? C8 Fe1 C6 176.4(3) . . ? C4 Fe1 C6 68.4(3) . . ? C7 Fe1 C6 40.0(3) . . ? C10 Fe1 C6 110.2(3) . . ? C3 Fe1 C12 137.6(3) . . ? C9 Fe1 C12 69.4(3) . . ? C8 Fe1 C12 41.1(2) . . ? C4 Fe1 C12 111.6(3) . . ? C7 Fe1 C12 177.7(3) . . ? C10 Fe1 C12 68.3(3) . . ? C6 Fe1 C12 142.2(3) . . ? C3 Fe1 C11 178.0(3) . . ? C9 Fe1 C11 68.8(3) . . ? C8 Fe1 C11 68.4(3) . . ? C4 Fe1 C11 138.6(3) . . ? C7 Fe1 C11 139.9(3) . . ? C10 Fe1 C11 40.0(3) . . ? C6 Fe1 C11 113.2(3) . . ? C12 Fe1 C11 40.5(3) . . ? C3 Fe1 C5 69.1(3) . . ? C9 Fe1 C5 175.5(3) . . ? C8 Fe1 C5 143.2(3) . . ? C4 Fe1 C5 41.2(2) . . ? C7 Fe1 C5 68.0(3) . . ? C10 Fe1 C5 136.7(3) . . ? C6 Fe1 C5 39.8(3) . . ? C12 Fe1 C5 114.3(3) . . ? C11 Fe1 C5 112.1(3) . . ? C9 C8 C12 108.4(6) . . ? C9 C8 P2 125.4(5) . . ? C12 C8 P2 126.2(5) . . ? C9 C8 Fe1 69.1(4) . . ? C12 C8 Fe1 70.5(4) . . ? P2 C8 Fe1 126.2(3) . . ? C8 C9 C10 107.0(6) . . ? C8 C9 Fe1 69.6(4) . . ? C10 C9 Fe1 70.3(4) . . ? C8 C9 H9A 126.5 . . ? C10 C9 H9A 126.5 . . ? Fe1 C9 H9A 125.2 . . ? C11 C10 C9 108.8(6) . . ? C11 C10 Fe1 70.9(4) . . ? C9 C10 Fe1 68.5(4) . . ? C11 C10 H10A 125.6 . . ? C9 C10 H10A 125.6 . . ? Fe1 C10 H10A 126.6 . . ? C10 C11 C12 108.4(6) . . ? C10 C11 Fe1 69.0(4) . . ? C12 C11 Fe1 69.2(4) . . ? C10 C11 H11A 125.8 . . ? C12 C11 H11A 125.8 . . ? Fe1 C11 H11A 127.6 . . ? C11 C12 C8 107.4(6) . . ? C11 C12 Fe1 70.3(4) . . ? C8 C12 Fe1 68.5(4) . . ? C11 C12 H12A 126.3 . . ? C8 C12 H12A 126.3 . . ? Fe1 C12 H12A 126.5 . . ? C14 C13 C18 117.8(6) . . ? C14 C13 P1 120.4(5) . . ? C18 C13 P1 121.6(5) . . ? C13 C14 C15 121.4(6) . . ? C13 C14 H14A 119.3 . . ? C15 C14 H14A 119.3 . . ? C16 C15 C14 120.6(7) . . ? C16 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? C15 C16 C17 118.7(7) . . ? C15 C16 H16A 120.6 . . ? C17 C16 H16A 120.6 . . ? C18 C17 C16 120.3(7) . . ? C18 C17 H17A 119.9 . . ? C16 C17 H17A 119.9 . . ? C17 C18 C13 121.1(6) . . ? C17 C18 H18A 119.4 . . ? C13 C18 H18A 119.4 . . ? C24 C19 C20 118.1(6) . . ? C24 C19 P1 121.6(5) . . ? C20 C19 P1 120.0(5) . . ? C21 C20 C19 120.4(6) . . ? C21 C20 H20A 119.8 . . ? C19 C20 H20A 119.8 . . ? C22 C21 C20 121.0(7) . . ? C22 C21 H21A 119.5 . . ? C20 C21 H21A 119.5 . . ? C21 C22 C23 120.2(6) . . ? C21 C22 H22A 119.9 . . ? C23 C22 H22A 119.9 . . ? C24 C23 C22 119.0(7) . . ? C24 C23 H23A 120.5 . . ? C22 C23 H23A 120.5 . . ? C19 C24 C23 121.2(6) . . ? C19 C24 H24A 119.4 . . ? C23 C24 H24A 119.4 . . ? C31 P2 C25 104.4(3) . . ? C31 P2 C8 102.1(3) . . ? C25 P2 C8 102.9(3) . . ? C31 P2 Pt1 116.7(2) . . ? C25 P2 Pt1 107.0(2) . . ? C8 P2 Pt1 121.7(2) . . ? C26 C25 C30 120.0(6) . . ? C26 C25 P2 118.4(5) . . ? C30 C25 P2 121.6(5) . . ? C25 C26 C27 119.9(7) . . ? C25 C26 H26A 120.0 . . ? C27 C26 H26A 120.0 . . ? C28 C27 C26 121.9(8) . . ? C28 C27 H27A 119.1 . . ? C26 C27 H27A 119.1 . . ? C27 C28 C29 118.8(7) . . ? C27 C28 H28A 120.6 . . ? C29 C28 H28A 120.6 . . ? C30 C29 C28 120.0(7) . . ? C30 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? C29 C30 C25 119.4(7) . . ? C29 C30 H30A 120.3 . . ? C25 C30 H30A 120.3 . . ? C32 C31 C36 119.8(6) . . ? C32 C31 P2 119.0(5) . . ? C36 C31 P2 120.8(5) . . ? C31 C32 C33 120.1(6) . . ? C31 C32 H32A 120.0 . . ? C33 C32 H32A 120.0 . . ? C34 C33 C32 120.3(6) . . ? C34 C33 H33A 119.9 . . ? C32 C33 H33A 119.9 . . ? C33 C34 C35 119.1(6) . . ? C33 C34 H34A 120.5 . . ? C35 C34 H34A 120.5 . . ? C36 C35 C34 122.1(6) . . ? C36 C35 H35A 119.0 . . ? C34 C35 H35A 119.0 . . ? C35 C36 C31 118.7(6) . . ? C35 C36 H36A 120.6 . . ? C31 C36 H36A 120.6 . . ? 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 P1 Pt1 S1 C1 -177.9(2) . . . . ? P2 Pt1 S1 C1 14.0(4) . . . . ? S2 Pt1 S1 C1 1.2(2) . . . . ? P1 Pt1 S2 C1 2.6(4) . . . . ? P2 Pt1 S2 C1 -178.2(2) . . . . ? S1 Pt1 S2 C1 -1.3(2) . . . . ? Pt1 S2 C1 N1 -178.3(6) . . . . ? Pt1 S2 C1 S1 1.7(3) . . . . ? Pt1 S1 C1 N1 178.3(6) . . . . ? Pt1 S1 C1 S2 -1.7(3) . . . . ? S2 C1 N1 C2 -178.5(5) . . . . ? S1 C1 N1 C2 1.5(10) . . . . ? C1 N1 C2 N2 -175(6) . . . . ? P2 Pt1 P1 C3 43.7(2) . . . . ? S1 Pt1 P1 C3 -133.4(2) . . . . ? S2 Pt1 P1 C3 -137.1(4) . . . . ? P2 Pt1 P1 C13 -83.1(2) . . . . ? S1 Pt1 P1 C13 99.8(2) . . . . ? S2 Pt1 P1 C13 96.1(4) . . . . ? P2 Pt1 P1 C19 161.1(2) . . . . ? S1 Pt1 P1 C19 -16.0(2) . . . . ? S2 Pt1 P1 C19 -19.7(4) . . . . ? C13 P1 C3 C4 168.0(5) . . . . ? C19 P1 C3 C4 -84.5(5) . . . . ? Pt1 P1 C3 C4 38.1(6) . . . . ? C13 P1 C3 C7 -11.3(6) . . . . ? C19 P1 C3 C7 96.2(6) . . . . ? Pt1 P1 C3 C7 -141.2(5) . . . . ? C13 P1 C3 Fe1 80.0(4) . . . . ? C19 P1 C3 Fe1 -172.4(4) . . . . ? Pt1 P1 C3 Fe1 -49.8(5) . . . . ? C7 C3 C4 C5 -0.3(7) . . . . ? P1 C3 C4 C5 -179.8(4) . . . . ? Fe1 C3 C4 C5 -60.5(4) . . . . ? C7 C3 C4 Fe1 60.2(4) . . . . ? P1 C3 C4 Fe1 -119.3(5) . . . . ? C3 C4 C5 C6 1.0(7) . . . . ? Fe1 C4 C5 C6 -58.2(4) . . . . ? C3 C4 C5 Fe1 59.2(4) . . . . ? C4 C5 C6 C7 -1.3(7) . . . . ? Fe1 C5 C6 C7 -58.7(5) . . . . ? C4 C5 C6 Fe1 57.4(4) . . . . ? C5 C6 C7 C3 1.1(7) . . . . ? Fe1 C6 C7 C3 -58.3(4) . . . . ? C5 C6 C7 Fe1 59.4(5) . . . . ? C4 C3 C7 C6 -0.4(7) . . . . ? P1 C3 C7 C6 179.0(5) . . . . ? Fe1 C3 C7 C6 59.7(4) . . . . ? C4 C3 C7 Fe1 -60.2(4) . . . . ? P1 C3 C7 Fe1 119.2(5) . . . . ? C4 C3 Fe1 C9 -146.5(4) . . . . ? C7 C3 Fe1 C9 95.3(4) . . . . ? P1 C3 Fe1 C9 -28.5(5) . . . . ? C4 C3 Fe1 C8 -102.4(4) . . . . ? C7 C3 Fe1 C8 139.4(4) . . . . ? P1 C3 Fe1 C8 15.6(5) . . . . ? C7 C3 Fe1 C4 -118.2(5) . . . . ? P1 C3 Fe1 C4 118.0(6) . . . . ? C4 C3 Fe1 C7 118.2(5) . . . . ? P1 C3 Fe1 C7 -123.8(6) . . . . ? C4 C3 Fe1 C10 177.6(4) . . . . ? C7 C3 Fe1 C10 59.4(5) . . . . ? P1 C3 Fe1 C10 -64.5(6) . . . . ? C4 C3 Fe1 C6 81.1(4) . . . . ? C7 C3 Fe1 C6 -37.1(4) . . . . ? P1 C3 Fe1 C6 -161.0(5) . . . . ? C4 C3 Fe1 C12 -65.2(5) . . . . ? C7 C3 Fe1 C12 176.6(4) . . . . ? P1 C3 Fe1 C12 52.7(6) . . . . ? C4 C3 Fe1 C11 -87(8) . . . . ? C7 C3 Fe1 C11 155(8) . . . . ? P1 C3 Fe1 C11 31(8) . . . . ? C4 C3 Fe1 C5 38.3(4) . . . . ? C7 C3 Fe1 C5 -79.9(4) . . . . ? P1 C3 Fe1 C5 156.2(5) . . . . ? C5 C4 Fe1 C3 118.6(5) . . . . ? C3 C4 Fe1 C9 55.2(6) . . . . ? C5 C4 Fe1 C9 173.8(4) . . . . ? C3 C4 Fe1 C8 94.3(4) . . . . ? C5 C4 Fe1 C8 -147.1(4) . . . . ? C3 C4 Fe1 C7 -38.9(4) . . . . ? C5 C4 Fe1 C7 79.6(4) . . . . ? C3 C4 Fe1 C10 -134(7) . . . . ? C5 C4 Fe1 C10 -16(7) . . . . ? C3 C4 Fe1 C6 -81.9(4) . . . . ? C5 C4 Fe1 C6 36.6(4) . . . . ? C3 C4 Fe1 C12 138.8(4) . . . . ? C5 C4 Fe1 C12 -102.6(4) . . . . ? C3 C4 Fe1 C11 177.0(4) . . . . ? C5 C4 Fe1 C11 -64.5(6) . . . . ? C3 C4 Fe1 C5 -118.6(5) . . . . ? C6 C7 Fe1 C3 -119.0(6) . . . . ? C6 C7 Fe1 C9 140.9(4) . . . . ? C3 C7 Fe1 C9 -100.1(4) . . . . ? C6 C7 Fe1 C8 177.7(4) . . . . ? C3 C7 Fe1 C8 -63.3(5) . . . . ? C6 C7 Fe1 C4 -80.6(4) . . . . ? C3 C7 Fe1 C4 38.4(4) . . . . ? C6 C7 Fe1 C10 97.1(4) . . . . ? C3 C7 Fe1 C10 -143.9(4) . . . . ? C3 C7 Fe1 C6 119.0(6) . . . . ? C6 C7 Fe1 C12 161(6) . . . . ? C3 C7 Fe1 C12 -80(6) . . . . ? C6 C7 Fe1 C11 62.3(6) . . . . ? C3 C7 Fe1 C11 -178.7(4) . . . . ? C6 C7 Fe1 C5 -36.2(4) . . . . ? C3 C7 Fe1 C5 82.8(4) . . . . ? C7 C6 Fe1 C3 38.8(4) . . . . ? C5 C6 Fe1 C3 -82.4(4) . . . . ? C7 C6 Fe1 C9 -58.8(5) . . . . ? C5 C6 Fe1 C9 179.9(4) . . . . ? C7 C6 Fe1 C8 -25(4) . . . . ? C5 C6 Fe1 C8 -147(4) . . . . ? C7 C6 Fe1 C4 83.3(4) . . . . ? C5 C6 Fe1 C4 -37.9(4) . . . . ? C5 C6 Fe1 C7 -121.2(6) . . . . ? C7 C6 Fe1 C10 -98.5(4) . . . . ? C5 C6 Fe1 C10 140.2(4) . . . . ? C7 C6 Fe1 C12 -178.8(4) . . . . ? C5 C6 Fe1 C12 60.0(6) . . . . ? C7 C6 Fe1 C11 -141.6(4) . . . . ? C5 C6 Fe1 C11 97.1(4) . . . . ? C7 C6 Fe1 C5 121.2(6) . . . . ? C6 C5 Fe1 C3 81.5(4) . . . . ? C4 C5 Fe1 C3 -38.4(4) . . . . ? C6 C5 Fe1 C9 -1(3) . . . . ? C4 C5 Fe1 C9 -120(3) . . . . ? C6 C5 Fe1 C8 176.7(4) . . . . ? C4 C5 Fe1 C8 56.8(6) . . . . ? C6 C5 Fe1 C4 119.9(6) . . . . ? C6 C5 Fe1 C7 36.4(4) . . . . ? C4 C5 Fe1 C7 -83.5(4) . . . . ? C6 C5 Fe1 C10 -61.0(6) . . . . ? C4 C5 Fe1 C10 179.1(4) . . . . ? C4 C5 Fe1 C6 -119.9(6) . . . . ? C6 C5 Fe1 C12 -144.4(4) . . . . ? C4 C5 Fe1 C12 95.7(4) . . . . ? C6 C5 Fe1 C11 -100.2(4) . . . . ? C4 C5 Fe1 C11 139.9(4) . . . . ? C3 Fe1 C8 C9 -98.7(4) . . . . ? C4 Fe1 C8 C9 -143.0(4) . . . . ? C7 Fe1 C8 C9 -59.4(5) . . . . ? C10 Fe1 C8 C9 38.8(4) . . . . ? C6 Fe1 C8 C9 -36(4) . . . . ? C12 Fe1 C8 C9 119.6(5) . . . . ? C11 Fe1 C8 C9 81.9(4) . . . . ? C5 Fe1 C8 C9 -179.7(4) . . . . ? C3 Fe1 C8 C12 141.7(4) . . . . ? C9 Fe1 C8 C12 -119.6(5) . . . . ? C4 Fe1 C8 C12 97.4(4) . . . . ? C7 Fe1 C8 C12 -179.0(4) . . . . ? C10 Fe1 C8 C12 -80.8(4) . . . . ? C6 Fe1 C8 C12 -155(4) . . . . ? C11 Fe1 C8 C12 -37.7(4) . . . . ? C5 Fe1 C8 C12 60.7(5) . . . . ? C3 Fe1 C8 P2 20.6(5) . . . . ? C9 Fe1 C8 P2 119.3(6) . . . . ? C4 Fe1 C8 P2 -23.7(5) . . . . ? C7 Fe1 C8 P2 59.9(6) . . . . ? C10 Fe1 C8 P2 158.0(5) . . . . ? C6 Fe1 C8 P2 84(4) . . . . ? C12 Fe1 C8 P2 -121.1(6) . . . . ? C11 Fe1 C8 P2 -158.8(5) . . . . ? C5 Fe1 C8 P2 -60.4(6) . . . . ? C12 C8 C9 C10 -0.9(7) . . . . ? P2 C8 C9 C10 179.1(4) . . . . ? Fe1 C8 C9 C10 -60.6(4) . . . . ? C12 C8 C9 Fe1 59.7(4) . . . . ? P2 C8 C9 Fe1 -120.2(5) . . . . ? C3 Fe1 C9 C8 97.1(4) . . . . ? C4 Fe1 C9 C8 61.8(6) . . . . ? C7 Fe1 C9 C8 141.5(4) . . . . ? C10 Fe1 C9 C8 -117.7(5) . . . . ? C6 Fe1 C9 C8 177.0(4) . . . . ? C12 Fe1 C9 C8 -37.6(4) . . . . ? C11 Fe1 C9 C8 -81.1(4) . . . . ? C5 Fe1 C9 C8 177(3) . . . . ? C3 Fe1 C9 C10 -145.3(4) . . . . ? C8 Fe1 C9 C10 117.7(5) . . . . ? C4 Fe1 C9 C10 179.4(4) . . . . ? C7 Fe1 C9 C10 -100.8(4) . . . . ? C6 Fe1 C9 C10 -65.3(5) . . . . ? C12 Fe1 C9 C10 80.1(4) . . . . ? C11 Fe1 C9 C10 36.6(4) . . . . ? C5 Fe1 C9 C10 -65(3) . . . . ? C8 C9 C10 C11 0.5(7) . . . . ? Fe1 C9 C10 C11 -59.7(5) . . . . ? C8 C9 C10 Fe1 60.2(4) . . . . ? C3 Fe1 C10 C11 176.9(4) . . . . ? C9 Fe1 C10 C11 120.2(6) . . . . ? C8 Fe1 C10 C11 81.3(4) . . . . ? C4 Fe1 C10 C11 -51(7) . . . . ? C7 Fe1 C10 C11 -145.2(4) . . . . ? C6 Fe1 C10 C11 -102.4(4) . . . . ? C12 Fe1 C10 C11 37.1(4) . . . . ? C5 Fe1 C10 C11 -65.8(5) . . . . ? C3 Fe1 C10 C9 56.7(6) . . . . ? C8 Fe1 C10 C9 -38.9(4) . . . . ? C4 Fe1 C10 C9 -171(7) . . . . ? C7 Fe1 C10 C9 94.6(4) . . . . ? C6 Fe1 C10 C9 137.4(4) . . . . ? C12 Fe1 C10 C9 -83.2(4) . . . . ? C11 Fe1 C10 C9 -120.2(6) . . . . ? C5 Fe1 C10 C9 174.0(4) . . . . ? C9 C10 C11 C12 0.1(7) . . . . ? Fe1 C10 C11 C12 -58.1(4) . . . . ? C9 C10 C11 Fe1 58.2(4) . . . . ? C3 Fe1 C11 C10 -98(8) . . . . ? C9 Fe1 C11 C10 -37.7(4) . . . . ? C8 Fe1 C11 C10 -82.2(4) . . . . ? C4 Fe1 C11 C10 177.4(4) . . . . ? C7 Fe1 C11 C10 56.0(6) . . . . ? C6 Fe1 C11 C10 94.3(4) . . . . ? C12 Fe1 C11 C10 -120.5(6) . . . . ? C5 Fe1 C11 C10 137.5(4) . . . . ? C3 Fe1 C11 C12 22(8) . . . . ? C9 Fe1 C11 C12 82.8(4) . . . . ? C8 Fe1 C11 C12 38.2(4) . . . . ? C4 Fe1 C11 C12 -62.1(6) . . . . ? C7 Fe1 C11 C12 176.4(4) . . . . ? C10 Fe1 C11 C12 120.5(6) . . . . ? C6 Fe1 C11 C12 -145.3(4) . . . . ? C5 Fe1 C11 C12 -102.0(4) . . . . ? C10 C11 C12 C8 -0.6(7) . . . . ? Fe1 C11 C12 C8 -58.6(4) . . . . ? C10 C11 C12 Fe1 58.0(4) . . . . ? C9 C8 C12 C11 1.0(7) . . . . ? P2 C8 C12 C11 -179.1(5) . . . . ? Fe1 C8 C12 C11 59.8(4) . . . . ? C9 C8 C12 Fe1 -58.8(4) . . . . ? P2 C8 C12 Fe1 121.1(5) . . . . ? C3 Fe1 C12 C11 -178.9(4) . . . . ? C9 Fe1 C12 C11 -81.0(4) . . . . ? C8 Fe1 C12 C11 -118.8(6) . . . . ? C4 Fe1 C12 C11 141.0(4) . . . . ? C7 Fe1 C12 C11 -102(6) . . . . ? C10 Fe1 C12 C11 -36.6(4) . . . . ? C6 Fe1 C12 C11 58.7(6) . . . . ? C5 Fe1 C12 C11 96.1(4) . . . . ? C3 Fe1 C12 C8 -60.0(5) . . . . ? C9 Fe1 C12 C8 37.8(4) . . . . ? C4 Fe1 C12 C8 -100.2(4) . . . . ? C7 Fe1 C12 C8 17(6) . . . . ? C10 Fe1 C12 C8 82.2(4) . . . . ? C6 Fe1 C12 C8 177.5(4) . . . . ? C11 Fe1 C12 C8 118.8(6) . . . . ? C5 Fe1 C12 C8 -145.0(4) . . . . ? C3 P1 C13 C14 -126.2(5) . . . . ? C19 P1 C13 C14 126.2(5) . . . . ? Pt1 P1 C13 C14 4.9(6) . . . . ? C3 P1 C13 C18 58.8(6) . . . . ? C19 P1 C13 C18 -48.8(6) . . . . ? Pt1 P1 C13 C18 -170.1(4) . . . . ? C18 C13 C14 C15 0.1(9) . . . . ? P1 C13 C14 C15 -175.1(5) . . . . ? C13 C14 C15 C16 -0.6(10) . . . . ? C14 C15 C16 C17 -0.3(10) . . . . ? C15 C16 C17 C18 1.8(10) . . . . ? C16 C17 C18 C13 -2.3(9) . . . . ? C14 C13 C18 C17 1.4(9) . . . . ? P1 C13 C18 C17 176.5(5) . . . . ? C3 P1 C19 C24 30.0(6) . . . . ? C13 P1 C19 C24 141.7(5) . . . . ? Pt1 P1 C19 C24 -95.5(5) . . . . ? C3 P1 C19 C20 -155.8(5) . . . . ? C13 P1 C19 C20 -44.1(6) . . . . ? Pt1 P1 C19 C20 78.6(5) . . . . ? C24 C19 C20 C21 -1.2(9) . . . . ? P1 C19 C20 C21 -175.5(5) . . . . ? C19 C20 C21 C22 1.2(10) . . . . ? C20 C21 C22 C23 0.0(10) . . . . ? C21 C22 C23 C24 -1.1(10) . . . . ? C20 C19 C24 C23 0.0(9) . . . . ? P1 C19 C24 C23 174.3(5) . . . . ? C22 C23 C24 C19 1.1(10) . . . . ? C9 C8 P2 C31 -61.8(6) . . . . ? C12 C8 P2 C31 118.3(6) . . . . ? Fe1 C8 P2 C31 -150.5(4) . . . . ? C9 C8 P2 C25 -169.8(5) . . . . ? C12 C8 P2 C25 10.2(6) . . . . ? Fe1 C8 P2 C25 101.5(4) . . . . ? C9 C8 P2 Pt1 70.5(6) . . . . ? C12 C8 P2 Pt1 -109.4(5) . . . . ? Fe1 C8 P2 Pt1 -18.2(5) . . . . ? P1 Pt1 P2 C31 113.2(2) . . . . ? S1 Pt1 P2 C31 -78.9(4) . . . . ? S2 Pt1 P2 C31 -66.6(2) . . . . ? P1 Pt1 P2 C25 -130.4(2) . . . . ? S1 Pt1 P2 C25 37.5(4) . . . . ? S2 Pt1 P2 C25 49.8(2) . . . . ? P1 Pt1 P2 C8 -12.8(3) . . . . ? S1 Pt1 P2 C8 155.2(3) . . . . ? S2 Pt1 P2 C8 167.4(3) . . . . ? C31 P2 C25 C26 174.7(5) . . . . ? C8 P2 C25 C26 -79.0(6) . . . . ? Pt1 P2 C25 C26 50.4(6) . . . . ? C31 P2 C25 C30 -3.9(6) . . . . ? C8 P2 C25 C30 102.4(6) . . . . ? Pt1 P2 C25 C30 -128.2(5) . . . . ? C30 C25 C26 C27 -0.8(10) . . . . ? P2 C25 C26 C27 -179.4(5) . . . . ? C25 C26 C27 C28 -0.6(11) . . . . ? C26 C27 C28 C29 1.2(10) . . . . ? C27 C28 C29 C30 -0.4(10) . . . . ? C28 C29 C30 C25 -0.9(10) . . . . ? C26 C25 C30 C29 1.5(10) . . . . ? P2 C25 C30 C29 -179.9(5) . . . . ? C25 P2 C31 C32 69.6(5) . . . . ? C8 P2 C31 C32 -37.3(6) . . . . ? Pt1 P2 C31 C32 -172.5(4) . . . . ? C25 P2 C31 C36 -103.3(6) . . . . ? C8 P2 C31 C36 149.8(5) . . . . ? Pt1 P2 C31 C36 14.6(6) . . . . ? C36 C31 C32 C33 1.5(9) . . . . ? P2 C31 C32 C33 -171.4(5) . . . . ? C31 C32 C33 C34 -0.5(10) . . . . ? C32 C33 C34 C35 -0.7(10) . . . . ? C33 C34 C35 C36 1.0(10) . . . . ? C34 C35 C36 C31 0.0(10) . . . . ? C32 C31 C36 C35 -1.3(9) . . . . ? P2 C31 C36 C35 171.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 23.32 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.780 _refine_diff_density_min -1.084 _refine_diff_density_rms 0.135 data_3 _database_code_depnum_ccdc_archive 'CCDC 224725' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[C24 H20 P]2.[(C2 N2 S2)2]Pd' _chemical_formula_sum 'C52 H40 N4 P2 Pd S4' _chemical_formula_weight 1017.46 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.861(2) _cell_length_b 14.540(3) _cell_length_c 15.163(3) _cell_angle_alpha 88.894(11) _cell_angle_beta 88.705(10) _cell_angle_gamma 83.598(10) _cell_volume 2378.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4370 _cell_measurement_theta_min 2.2257 _cell_measurement_theta_max 21.9658 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max .1 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 0.673 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7777 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _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_type ccd _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 0.85 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8060 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0667 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 21.97 _reflns_number_total 5365 _reflns_number_gt 3831 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0364P)^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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0001(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5365 _refine_ls_number_parameters 572 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0706 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0790 _refine_ls_wR_factor_gt 0.0715 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.940 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 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 Pd1 Pd 0.5000 0.0000 0.0000 0.04474(19) Uani 1 2 d S . . S1 S 0.59735(11) 0.12993(9) 0.03194(9) 0.0560(4) Uani 1 1 d . . . S2 S 0.37228(13) 0.07808(9) 0.10447(10) 0.0638(4) Uani 1 1 d . . . C1 C 0.4737(4) 0.1617(3) 0.1030(3) 0.0435(13) Uani 1 1 d . . . N1 N 0.4519(4) 0.2369(3) 0.1484(3) 0.0522(11) Uani 1 1 d . . . C2 C 0.5290(5) 0.3016(4) 0.1420(3) 0.0530(15) Uani 1 1 d . . . N2 N 0.5849(5) 0.3633(3) 0.1413(3) 0.0818(16) Uani 1 1 d . . . P1 P 0.47375(11) 0.21698(8) 0.46004(8) 0.0415(3) Uani 1 1 d . . . C3 C 0.4691(4) 0.3372(3) 0.4286(3) 0.0421(12) Uani 1 1 d . . . C4 C 0.5693(5) 0.3726(4) 0.3889(3) 0.0602(15) Uani 1 1 d . . . H4A H 0.6415 0.3338 0.3768 0.072 Uiso 1 1 calc R . . C5 C 0.5626(6) 0.4658(4) 0.3671(3) 0.0677(16) Uani 1 1 d . . . H5A H 0.6302 0.4893 0.3397 0.081 Uiso 1 1 calc R . . C6 C 0.4574(7) 0.5236(4) 0.3855(4) 0.0666(16) Uani 1 1 d . . . H6A H 0.4544 0.5865 0.3721 0.080 Uiso 1 1 calc R . . C7 C 0.3578(6) 0.4891(4) 0.4232(3) 0.0619(16) Uani 1 1 d . . . H7A H 0.2856 0.5283 0.4340 0.074 Uiso 1 1 calc R . . C8 C 0.3621(5) 0.3965(4) 0.4457(3) 0.0556(14) Uani 1 1 d . . . H8A H 0.2935 0.3737 0.4724 0.067 Uiso 1 1 calc R . . C9 C 0.6063(4) 0.1532(3) 0.4103(3) 0.0417(12) Uani 1 1 d . . . C10 C 0.5909(4) 0.0903(3) 0.3460(3) 0.0512(14) Uani 1 1 d . . . H10A H 0.5117 0.0822 0.3275 0.061 Uiso 1 1 calc R . . C11 C 0.6945(6) 0.0385(3) 0.3083(4) 0.0645(16) Uani 1 1 d . . . H11A H 0.6849 -0.0029 0.2636 0.077 Uiso 1 1 calc R . . C12 C 0.8108(5) 0.0491(4) 0.3381(4) 0.0663(17) Uani 1 1 d . . . H12A H 0.8793 0.0126 0.3150 0.080 Uiso 1 1 calc R . . C13 C 0.8273(5) 0.1125(4) 0.4009(4) 0.0681(17) Uani 1 1 d . . . H13A H 0.9067 0.1203 0.4190 0.082 Uiso 1 1 calc R . . C14 C 0.7252(5) 0.1652(3) 0.4376(3) 0.0579(15) Uani 1 1 d . . . H14A H 0.7361 0.2084 0.4804 0.069 Uiso 1 1 calc R . . C15 C 0.3380(4) 0.1753(3) 0.4198(3) 0.0379(12) Uani 1 1 d . . . C16 C 0.2987(4) 0.2017(3) 0.3360(3) 0.0462(13) Uani 1 1 d . . . H16A H 0.3345 0.2484 0.3054 0.055 Uiso 1 1 calc R . . C17 C 0.2061(4) 0.1588(4) 0.2977(3) 0.0537(14) Uani 1 1 d . . . H17A H 0.1796 0.1761 0.2412 0.064 Uiso 1 1 calc R . . C18 C 0.1542(4) 0.0908(4) 0.3438(4) 0.0562(15) Uani 1 1 d . . . H18A H 0.0943 0.0603 0.3173 0.067 Uiso 1 1 calc R . . C19 C 0.1880(5) 0.0667(3) 0.4271(4) 0.0575(15) Uani 1 1 d . . . H19A H 0.1481 0.0227 0.4585 0.069 Uiso 1 1 calc R . . C20 C 0.2813(4) 0.1073(3) 0.4653(3) 0.0474(13) Uani 1 1 d . . . H20A H 0.3066 0.0891 0.5218 0.057 Uiso 1 1 calc R . . C21 C 0.4763(4) 0.1997(3) 0.5771(3) 0.0410(12) Uani 1 1 d . . . C22 C 0.3825(5) 0.2426(3) 0.6296(3) 0.0574(15) Uani 1 1 d . . . H22A H 0.3205 0.2825 0.6033 0.069 Uiso 1 1 calc R . . C23 C 0.3774(5) 0.2283(4) 0.7193(4) 0.0710(17) Uani 1 1 d . . . H23A H 0.3124 0.2574 0.7530 0.085 Uiso 1 1 calc R . . C24 C 0.4688(6) 0.1708(4) 0.7585(4) 0.0817(19) Uani 1 1 d . . . H24A H 0.4670 0.1607 0.8192 0.098 Uiso 1 1 calc R . . C25 C 0.5633(6) 0.1282(4) 0.7074(4) 0.091(2) Uani 1 1 d . . . H25A H 0.6258 0.0892 0.7341 0.109 Uiso 1 1 calc R . . C26 C 0.5676(5) 0.1417(4) 0.6175(4) 0.0666(17) Uani 1 1 d . . . H26A H 0.6322 0.1117 0.5841 0.080 Uiso 1 1 calc R . . Pd31 Pd 0.0000 0.5000 0.5000 0.04423(19) Uani 1 2 d S . . S31 S -0.05247(14) 0.34963(9) 0.50597(9) 0.0650(4) Uani 1 1 d . . . S32 S 0.09847(12) 0.43343(9) 0.62333(9) 0.0568(4) Uani 1 1 d . . . C31 C 0.0334(4) 0.3340(3) 0.5999(3) 0.0408(12) Uani 1 1 d . . . N31 N 0.0508(4) 0.2598(3) 0.6505(3) 0.0497(11) Uani 1 1 d . . . C32 C -0.0057(6) 0.1876(4) 0.6288(4) 0.0586(16) Uani 1 1 d . . . N32 N -0.0507(5) 0.1211(3) 0.6176(4) 0.0979(19) Uani 1 1 d . . . P31 P 0.00637(10) 0.29527(8) 0.95925(8) 0.0352(3) Uani 1 1 d . . . C33 C -0.0151(4) 0.3008(3) 1.0762(3) 0.0365(12) Uani 1 1 d . . . C34 C 0.0480(4) 0.3556(3) 1.1276(3) 0.0499(13) Uani 1 1 d . . . H34A H 0.1089 0.3880 1.1018 0.060 Uiso 1 1 calc R . . C35 C 0.0224(5) 0.3636(3) 1.2181(4) 0.0628(16) Uani 1 1 d . . . H35A H 0.0653 0.4013 1.2523 0.075 Uiso 1 1 calc R . . C36 C -0.0663(6) 0.3155(4) 1.2551(4) 0.0636(16) Uani 1 1 d . . . H36A H -0.0817 0.3189 1.3156 0.076 Uiso 1 1 calc R . . C37 C -0.1332(5) 0.2623(4) 1.2060(4) 0.0570(15) Uani 1 1 d . . . H37A H -0.1960 0.2319 1.2322 0.068 Uiso 1 1 calc R . . C38 C -0.1066(4) 0.2538(3) 1.1158(3) 0.0484(13) Uani 1 1 d . . . H38A H -0.1505 0.2164 1.0821 0.058 Uiso 1 1 calc R . . C39 C -0.1190(4) 0.3647(3) 0.9080(3) 0.0328(11) Uani 1 1 d . . . C40 C -0.1226(4) 0.3670(3) 0.8169(3) 0.0486(14) Uani 1 1 d . . . H40A H -0.0627 0.3304 0.7846 0.058 Uiso 1 1 calc R . . C41 C -0.2131(5) 0.4224(4) 0.7736(3) 0.0621(16) Uani 1 1 d . . . H41A H -0.2132 0.4247 0.7123 0.075 Uiso 1 1 calc R . . C42 C -0.3034(4) 0.4745(3) 0.8210(4) 0.0580(15) Uani 1 1 d . . . H42A H -0.3650 0.5122 0.7919 0.070 Uiso 1 1 calc R . . C43 C -0.3029(4) 0.4712(3) 0.9111(4) 0.0502(14) Uani 1 1 d . . . H43A H -0.3648 0.5064 0.9430 0.060 Uiso 1 1 calc R . . C44 C -0.2108(4) 0.4157(3) 0.9558(3) 0.0402(12) Uani 1 1 d . . . H44A H -0.2114 0.4131 1.0171 0.048 Uiso 1 1 calc R . . C45 C 0.1482(4) 0.3399(3) 0.9285(3) 0.0315(11) Uani 1 1 d . . . C46 C 0.2610(4) 0.3010(3) 0.9626(3) 0.0427(12) Uani 1 1 d . . . H46A H 0.2623 0.2519 1.0029 0.051 Uiso 1 1 calc R . . C47 C 0.3710(4) 0.3347(3) 0.9372(3) 0.0503(14) Uani 1 1 d . . . H47A H 0.4458 0.3073 0.9591 0.060 Uiso 1 1 calc R . . C48 C 0.3693(5) 0.4081(4) 0.8801(3) 0.0544(14) Uani 1 1 d . . . H48A H 0.4430 0.4308 0.8629 0.065 Uiso 1 1 calc R . . C49 C 0.2589(5) 0.4486(3) 0.8478(3) 0.0488(13) Uani 1 1 d . . . H49A H 0.2584 0.4993 0.8094 0.059 Uiso 1 1 calc R . . C50 C 0.1499(4) 0.4154(3) 0.8712(3) 0.0417(12) Uani 1 1 d . . . H50A H 0.0759 0.4437 0.8486 0.050 Uiso 1 1 calc R . . C51 C 0.0024(4) 0.1791(3) 0.9224(3) 0.0362(12) Uani 1 1 d . . . C52 C -0.1078(5) 0.1499(3) 0.8981(3) 0.0554(14) Uani 1 1 d . . . H52A H -0.1795 0.1913 0.8993 0.066 Uiso 1 1 calc R . . C53 C -0.1138(5) 0.0610(4) 0.8721(4) 0.0680(16) Uani 1 1 d . . . H53A H -0.1891 0.0428 0.8551 0.082 Uiso 1 1 calc R . . C54 C -0.0108(6) -0.0006(4) 0.8708(3) 0.0605(15) Uani 1 1 d . . . H54A H -0.0152 -0.0609 0.8527 0.073 Uiso 1 1 calc R . . C55 C 0.0995(6) 0.0258(4) 0.8961(3) 0.0625(16) Uani 1 1 d . . . H55A H 0.1698 -0.0170 0.8963 0.075 Uiso 1 1 calc R . . C56 C 0.1075(5) 0.1159(3) 0.9216(3) 0.0525(14) Uani 1 1 d . . . H56A H 0.1831 0.1338 0.9381 0.063 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 Pd1 0.0456(4) 0.0368(3) 0.0515(4) -0.0006(3) 0.0024(3) -0.0036(3) S1 0.0493(8) 0.0470(8) 0.0723(11) -0.0112(7) 0.0122(7) -0.0094(7) S2 0.0669(10) 0.0502(9) 0.0766(11) -0.0107(8) 0.0234(8) -0.0196(7) C1 0.052(3) 0.044(3) 0.034(3) 0.007(3) 0.002(2) -0.006(3) N1 0.070(3) 0.042(3) 0.046(3) -0.013(2) 0.014(2) -0.014(2) C2 0.063(4) 0.044(4) 0.051(4) -0.014(3) 0.003(3) -0.002(3) N2 0.082(4) 0.056(3) 0.110(5) -0.024(3) 0.008(3) -0.016(3) P1 0.0412(8) 0.0465(8) 0.0372(9) -0.0008(6) 0.0022(6) -0.0067(6) C3 0.049(3) 0.043(3) 0.035(3) -0.002(2) 0.003(2) -0.013(3) C4 0.065(4) 0.062(4) 0.054(4) 0.000(3) 0.004(3) -0.013(3) C5 0.077(4) 0.079(5) 0.054(4) 0.009(3) 0.002(3) -0.039(4) C6 0.100(5) 0.059(4) 0.045(4) 0.006(3) -0.016(3) -0.025(4) C7 0.080(4) 0.054(4) 0.048(4) 0.003(3) -0.019(3) 0.010(3) C8 0.056(4) 0.060(4) 0.050(4) 0.006(3) 0.002(3) -0.004(3) C9 0.041(3) 0.045(3) 0.040(3) 0.000(3) -0.003(2) -0.010(2) C10 0.042(3) 0.051(3) 0.063(4) 0.003(3) 0.007(3) -0.014(3) C11 0.071(4) 0.059(4) 0.064(4) -0.009(3) 0.015(3) -0.008(3) C12 0.058(4) 0.065(4) 0.069(5) 0.008(3) 0.021(3) 0.018(3) C13 0.043(4) 0.096(5) 0.063(4) 0.019(4) 0.012(3) -0.002(4) C14 0.048(3) 0.074(4) 0.052(4) 0.001(3) -0.003(3) -0.010(3) C15 0.033(3) 0.045(3) 0.036(3) 0.000(2) 0.006(2) -0.008(2) C16 0.040(3) 0.064(4) 0.035(3) 0.008(3) 0.007(3) -0.010(3) C17 0.039(3) 0.076(4) 0.046(4) -0.003(3) -0.004(3) 0.000(3) C18 0.043(3) 0.075(4) 0.052(4) -0.019(3) 0.000(3) -0.011(3) C19 0.049(3) 0.068(4) 0.058(4) 0.003(3) 0.002(3) -0.018(3) C20 0.051(3) 0.057(3) 0.033(3) 0.005(3) -0.008(3) -0.004(3) C21 0.039(3) 0.037(3) 0.048(3) -0.004(2) 0.001(3) -0.009(2) C22 0.068(4) 0.055(3) 0.046(4) 0.002(3) -0.005(3) 0.009(3) C23 0.088(4) 0.075(4) 0.045(4) -0.006(3) 0.004(3) 0.012(4) C24 0.113(5) 0.096(5) 0.034(4) 0.001(3) -0.004(4) -0.005(4) C25 0.087(5) 0.116(5) 0.060(5) 0.009(4) -0.014(4) 0.030(4) C26 0.061(4) 0.092(4) 0.042(4) 0.004(3) 0.003(3) 0.012(3) Pd31 0.0541(4) 0.0431(3) 0.0366(4) 0.0004(3) -0.0009(3) -0.0107(3) S31 0.0968(11) 0.0500(9) 0.0525(10) 0.0038(7) -0.0232(8) -0.0240(8) S32 0.0717(10) 0.0539(9) 0.0477(9) 0.0045(7) -0.0134(7) -0.0190(7) C31 0.044(3) 0.041(3) 0.036(3) -0.006(2) 0.004(2) -0.003(2) N31 0.059(3) 0.039(3) 0.051(3) 0.003(2) -0.002(2) -0.005(2) C32 0.082(5) 0.041(4) 0.051(4) 0.010(3) 0.001(3) 0.001(3) N32 0.135(5) 0.058(3) 0.105(5) 0.015(3) -0.019(4) -0.030(4) P31 0.0362(7) 0.0356(7) 0.0337(8) 0.0020(6) -0.0013(6) -0.0045(6) C33 0.042(3) 0.031(3) 0.038(3) 0.009(2) -0.008(2) -0.006(2) C34 0.061(4) 0.045(3) 0.045(4) 0.005(3) -0.003(3) -0.010(3) C35 0.099(5) 0.049(3) 0.041(4) -0.007(3) -0.017(3) -0.009(3) C36 0.088(5) 0.069(4) 0.031(4) 0.008(3) -0.006(3) 0.001(4) C37 0.066(4) 0.062(4) 0.041(4) 0.017(3) 0.012(3) -0.002(3) C38 0.061(4) 0.043(3) 0.041(4) 0.001(3) -0.005(3) -0.005(3) C39 0.029(3) 0.035(3) 0.034(3) -0.001(2) -0.002(2) -0.002(2) C40 0.034(3) 0.068(4) 0.041(4) -0.006(3) 0.000(2) 0.007(3) C41 0.051(3) 0.093(4) 0.039(3) 0.001(3) -0.006(3) 0.006(3) C42 0.044(3) 0.070(4) 0.058(4) 0.010(3) -0.015(3) 0.002(3) C43 0.035(3) 0.049(3) 0.065(4) -0.016(3) -0.003(3) 0.004(3) C44 0.044(3) 0.045(3) 0.032(3) -0.006(2) -0.004(2) -0.006(3) C45 0.031(3) 0.031(3) 0.033(3) 0.001(2) 0.003(2) -0.010(2) C46 0.050(3) 0.037(3) 0.042(3) 0.004(2) -0.007(3) -0.010(3) C47 0.035(3) 0.058(4) 0.059(4) -0.002(3) -0.007(3) -0.007(3) C48 0.049(4) 0.065(4) 0.054(4) -0.009(3) 0.014(3) -0.026(3) C49 0.056(4) 0.050(3) 0.041(3) 0.003(3) 0.011(3) -0.016(3) C50 0.044(3) 0.048(3) 0.034(3) -0.002(2) 0.005(2) -0.005(3) C51 0.037(3) 0.032(3) 0.039(3) -0.002(2) 0.005(2) -0.003(3) C52 0.049(4) 0.042(3) 0.077(4) -0.013(3) 0.003(3) -0.011(3) C53 0.063(4) 0.062(4) 0.085(5) -0.012(3) -0.010(3) -0.027(3) C54 0.091(5) 0.042(3) 0.051(4) -0.009(3) -0.007(3) -0.014(4) C55 0.077(4) 0.055(4) 0.052(4) -0.009(3) -0.008(3) 0.013(3) C56 0.059(4) 0.044(3) 0.055(4) -0.006(3) -0.004(3) -0.007(3) _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 Pd1 S2 2.3111(13) 2_655 ? Pd1 S2 2.3111(13) . ? Pd1 S1 2.3293(14) . ? Pd1 S1 2.3293(14) 2_655 ? S1 C1 1.730(4) . ? S2 C1 1.729(5) . ? C1 N1 1.300(5) . ? N1 C2 1.328(7) . ? C2 N2 1.138(6) . ? P1 C15 1.780(5) . ? P1 C9 1.784(4) . ? P1 C21 1.788(5) . ? P1 C3 1.799(4) . ? C3 C4 1.375(6) . ? C3 C8 1.390(6) . ? C4 C5 1.384(6) . ? C4 H4A 0.9300 . ? C5 C6 1.368(7) . ? C5 H5A 0.9300 . ? C6 C7 1.354(7) . ? C6 H6A 0.9300 . ? C7 C8 1.379(6) . ? C7 H7A 0.9300 . ? C8 H8A 0.9300 . ? C9 C10 1.376(6) . ? C9 C14 1.396(6) . ? C10 C11 1.400(6) . ? C10 H10A 0.9300 . ? C11 C12 1.376(7) . ? C11 H11A 0.9300 . ? C12 C13 1.367(7) . ? C12 H12A 0.9300 . ? C13 C14 1.387(6) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 C16 1.383(6) . ? C15 C20 1.387(6) . ? C16 C17 1.386(6) . ? C16 H16A 0.9300 . ? C17 C18 1.365(6) . ? C17 H17A 0.9300 . ? C18 C19 1.352(6) . ? C18 H18A 0.9300 . ? C19 C20 1.372(6) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C26 1.375(6) . ? C21 C22 1.379(6) . ? C22 C23 1.374(6) . ? C22 H22A 0.9300 . ? C23 C24 1.362(7) . ? C23 H23A 0.9300 . ? C24 C25 1.371(7) . ? C24 H24A 0.9300 . ? C25 C26 1.373(7) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? Pd31 S32 2.3167(13) 2_566 ? Pd31 S32 2.3167(13) . ? Pd31 S31 2.3197(14) 2_566 ? Pd31 S31 2.3197(14) . ? S31 C31 1.717(5) . ? S32 C31 1.726(5) . ? C31 N31 1.310(5) . ? N31 C32 1.325(7) . ? C32 N32 1.147(7) . ? P31 C39 1.786(4) . ? P31 C33 1.786(5) . ? P31 C45 1.786(4) . ? P31 C51 1.795(4) . ? C33 C34 1.371(6) . ? C33 C38 1.387(6) . ? C34 C35 1.398(6) . ? C34 H34A 0.9300 . ? C35 C36 1.358(7) . ? C35 H35A 0.9300 . ? C36 C37 1.362(7) . ? C36 H36A 0.9300 . ? C37 C38 1.396(6) . ? C37 H37A 0.9300 . ? C38 H38A 0.9300 . ? C39 C44 1.376(5) . ? C39 C40 1.381(6) . ? C40 C41 1.371(6) . ? C40 H40A 0.9300 . ? C41 C42 1.370(6) . ? C41 H41A 0.9300 . ? C42 C43 1.366(6) . ? C42 H42A 0.9300 . ? C43 C44 1.393(5) . ? C43 H43A 0.9300 . ? C44 H44A 0.9300 . ? C45 C50 1.389(5) . ? C45 C46 1.396(5) . ? C46 C47 1.386(6) . ? C46 H46A 0.9300 . ? C47 C48 1.359(6) . ? C47 H47A 0.9300 . ? C48 C49 1.372(6) . ? C48 H48A 0.9300 . ? C49 C50 1.365(6) . ? C49 H49A 0.9300 . ? C50 H50A 0.9300 . ? C51 C52 1.374(6) . ? C51 C56 1.383(5) . ? C52 C53 1.368(6) . ? C52 H52A 0.9300 . ? C53 C54 1.353(6) . ? C53 H53A 0.9300 . ? C54 C55 1.363(7) . ? C54 H54A 0.9300 . ? C55 C56 1.386(6) . ? C55 H55A 0.9300 . ? C56 H56A 0.9300 . ? 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 S2 Pd1 S2 180.00(5) 2_655 . ? S2 Pd1 S1 104.83(5) 2_655 . ? S2 Pd1 S1 75.17(5) . . ? S2 Pd1 S1 75.17(5) 2_655 2_655 ? S2 Pd1 S1 104.83(5) . 2_655 ? S1 Pd1 S1 180.00(7) . 2_655 ? C1 S1 Pd1 87.16(17) . . ? C1 S2 Pd1 87.78(16) . . ? N1 C1 S2 121.9(4) . . ? N1 C1 S1 128.2(4) . . ? S2 C1 S1 109.8(3) . . ? C1 N1 C2 120.0(4) . . ? N2 C2 N1 172.3(6) . . ? C15 P1 C9 108.8(2) . . ? C15 P1 C21 108.5(2) . . ? C9 P1 C21 109.8(2) . . ? C15 P1 C3 107.8(2) . . ? C9 P1 C3 109.6(2) . . ? C21 P1 C3 112.3(2) . . ? C4 C3 C8 118.9(4) . . ? C4 C3 P1 121.8(4) . . ? C8 C3 P1 119.3(4) . . ? C3 C4 C5 120.0(5) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C6 C5 C4 120.5(5) . . ? C6 C5 H5A 119.8 . . ? C4 C5 H5A 119.8 . . ? C7 C6 C5 119.9(5) . . ? C7 C6 H6A 120.0 . . ? C5 C6 H6A 120.0 . . ? C6 C7 C8 120.7(5) . . ? C6 C7 H7A 119.6 . . ? C8 C7 H7A 119.6 . . ? C7 C8 C3 120.0(5) . . ? C7 C8 H8A 120.0 . . ? C3 C8 H8A 120.0 . . ? C10 C9 C14 119.9(4) . . ? C10 C9 P1 119.7(4) . . ? C14 C9 P1 120.4(4) . . ? C9 C10 C11 119.8(5) . . ? C9 C10 H10A 120.1 . . ? C11 C10 H10A 120.1 . . ? C12 C11 C10 119.5(5) . . ? C12 C11 H11A 120.3 . . ? C10 C11 H11A 120.3 . . ? C13 C12 C11 121.1(5) . . ? C13 C12 H12A 119.5 . . ? C11 C12 H12A 119.5 . . ? C12 C13 C14 119.8(5) . . ? C12 C13 H13A 120.1 . . ? C14 C13 H13A 120.1 . . ? C13 C14 C9 119.9(5) . . ? C13 C14 H14A 120.1 . . ? C9 C14 H14A 120.1 . . ? C16 C15 C20 119.1(4) . . ? C16 C15 P1 119.0(4) . . ? C20 C15 P1 121.2(4) . . ? C17 C16 C15 120.1(5) . . ? C17 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C18 C17 C16 119.1(5) . . ? C18 C17 H17A 120.4 . . ? C16 C17 H17A 120.4 . . ? C19 C18 C17 121.6(5) . . ? C19 C18 H18A 119.2 . . ? C17 C18 H18A 119.2 . . ? C18 C19 C20 119.9(5) . . ? C18 C19 H19A 120.0 . . ? C20 C19 H19A 120.0 . . ? C19 C20 C15 120.1(5) . . ? C19 C20 H20A 119.9 . . ? C15 C20 H20A 119.9 . . ? C26 C21 C22 117.8(4) . . ? C26 C21 P1 122.1(4) . . ? C22 C21 P1 120.1(4) . . ? C23 C22 C21 122.3(4) . . ? C23 C22 H22A 118.9 . . ? C21 C22 H22A 118.9 . . ? C24 C23 C22 119.2(5) . . ? C24 C23 H23A 120.4 . . ? C22 C23 H23A 120.4 . . ? C23 C24 C25 119.3(5) . . ? C23 C24 H24A 120.3 . . ? C25 C24 H24A 120.3 . . ? C26 C25 C24 121.4(5) . . ? C26 C25 H25A 119.3 . . ? C24 C25 H25A 119.3 . . ? C25 C26 C21 120.0(5) . . ? C25 C26 H26A 120.0 . . ? C21 C26 H26A 120.0 . . ? S32 Pd31 S32 180.000(1) 2_566 . ? S32 Pd31 S31 75.19(5) 2_566 2_566 ? S32 Pd31 S31 104.81(5) . 2_566 ? S32 Pd31 S31 104.81(5) 2_566 . ? S32 Pd31 S31 75.19(5) . . ? S31 Pd31 S31 180.0 2_566 . ? C31 S31 Pd31 87.21(16) . . ? C31 S32 Pd31 87.11(16) . . ? N31 C31 S31 128.1(4) . . ? N31 C31 S32 121.4(4) . . ? S31 C31 S32 110.5(3) . . ? C31 N31 C32 117.2(4) . . ? N32 C32 N31 173.3(6) . . ? C39 P31 C33 109.0(2) . . ? C39 P31 C45 109.0(2) . . ? C33 P31 C45 109.2(2) . . ? C39 P31 C51 106.8(2) . . ? C33 P31 C51 110.7(2) . . ? C45 P31 C51 112.1(2) . . ? C34 C33 C38 118.5(5) . . ? C34 C33 P31 122.7(4) . . ? C38 C33 P31 118.5(4) . . ? C33 C34 C35 121.2(5) . . ? C33 C34 H34A 119.4 . . ? C35 C34 H34A 119.4 . . ? C36 C35 C34 118.8(5) . . ? C36 C35 H35A 120.6 . . ? C34 C35 H35A 120.6 . . ? C35 C36 C37 121.7(5) . . ? C35 C36 H36A 119.2 . . ? C37 C36 H36A 119.2 . . ? C36 C37 C38 119.3(5) . . ? C36 C37 H37A 120.4 . . ? C38 C37 H37A 120.4 . . ? C33 C38 C37 120.4(5) . . ? C33 C38 H38A 119.8 . . ? C37 C38 H38A 119.8 . . ? C44 C39 C40 119.4(4) . . ? C44 C39 P31 122.4(3) . . ? C40 C39 P31 118.2(3) . . ? C41 C40 C39 120.9(4) . . ? C41 C40 H40A 119.5 . . ? C39 C40 H40A 119.5 . . ? C42 C41 C40 119.7(5) . . ? C42 C41 H41A 120.1 . . ? C40 C41 H41A 120.1 . . ? C43 C42 C41 120.0(4) . . ? C43 C42 H42A 120.0 . . ? C41 C42 H42A 120.0 . . ? C42 C43 C44 120.7(4) . . ? C42 C43 H43A 119.6 . . ? C44 C43 H43A 119.6 . . ? C39 C44 C43 119.2(4) . . ? C39 C44 H44A 120.4 . . ? C43 C44 H44A 120.4 . . ? C50 C45 C46 117.7(4) . . ? C50 C45 P31 121.2(3) . . ? C46 C45 P31 121.1(3) . . ? C47 C46 C45 120.9(4) . . ? C47 C46 H46A 119.6 . . ? C45 C46 H46A 119.6 . . ? C48 C47 C46 119.8(4) . . ? C48 C47 H47A 120.1 . . ? C46 C47 H47A 120.1 . . ? C47 C48 C49 120.1(5) . . ? C47 C48 H48A 120.0 . . ? C49 C48 H48A 120.0 . . ? C50 C49 C48 120.8(4) . . ? C50 C49 H49A 119.6 . . ? C48 C49 H49A 119.6 . . ? C49 C50 C45 120.7(4) . . ? C49 C50 H50A 119.7 . . ? C45 C50 H50A 119.7 . . ? C52 C51 C56 118.5(4) . . ? C52 C51 P31 120.0(3) . . ? C56 C51 P31 121.4(4) . . ? C53 C52 C51 121.1(5) . . ? C53 C52 H52A 119.4 . . ? C51 C52 H52A 119.4 . . ? C54 C53 C52 120.3(5) . . ? C54 C53 H53A 119.8 . . ? C52 C53 H53A 119.8 . . ? C53 C54 C55 119.9(5) . . ? C53 C54 H54A 120.1 . . ? C55 C54 H54A 120.0 . . ? C54 C55 C56 120.5(5) . . ? C54 C55 H55A 119.8 . . ? C56 C55 H55A 119.8 . . ? C51 C56 C55 119.6(5) . . ? C51 C56 H56A 120.2 . . ? C55 C56 H56A 120.2 . . ? 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 S2 Pd1 S1 C1 178.42(14) 2_655 . . . ? S2 Pd1 S1 C1 -1.58(14) . . . . ? S1 Pd1 S1 C1 -21(100) 2_655 . . . ? S2 Pd1 S2 C1 177(100) 2_655 . . . ? S1 Pd1 S2 C1 1.58(15) . . . . ? S1 Pd1 S2 C1 -178.42(15) 2_655 . . . ? Pd1 S2 C1 N1 176.0(4) . . . . ? Pd1 S2 C1 S1 -2.2(2) . . . . ? Pd1 S1 C1 N1 -175.8(4) . . . . ? Pd1 S1 C1 S2 2.2(2) . . . . ? S2 C1 N1 C2 -176.6(4) . . . . ? S1 C1 N1 C2 1.3(7) . . . . ? C1 N1 C2 N2 168(4) . . . . ? C15 P1 C3 C4 -131.3(4) . . . . ? C9 P1 C3 C4 -13.1(5) . . . . ? C21 P1 C3 C4 109.3(4) . . . . ? C15 P1 C3 C8 49.6(4) . . . . ? C9 P1 C3 C8 167.8(4) . . . . ? C21 P1 C3 C8 -69.9(4) . . . . ? C8 C3 C4 C5 0.2(8) . . . . ? P1 C3 C4 C5 -178.9(4) . . . . ? C3 C4 C5 C6 0.7(8) . . . . ? C4 C5 C6 C7 -1.8(8) . . . . ? C5 C6 C7 C8 1.9(8) . . . . ? C6 C7 C8 C3 -0.9(8) . . . . ? C4 C3 C8 C7 -0.1(7) . . . . ? P1 C3 C8 C7 179.0(4) . . . . ? C15 P1 C9 C10 5.5(5) . . . . ? C21 P1 C9 C10 124.1(4) . . . . ? C3 P1 C9 C10 -112.1(4) . . . . ? C15 P1 C9 C14 -173.0(4) . . . . ? C21 P1 C9 C14 -54.4(4) . . . . ? C3 P1 C9 C14 69.4(4) . . . . ? C14 C9 C10 C11 0.1(7) . . . . ? P1 C9 C10 C11 -178.4(3) . . . . ? C9 C10 C11 C12 1.9(7) . . . . ? C10 C11 C12 C13 -3.0(8) . . . . ? C11 C12 C13 C14 2.0(8) . . . . ? C12 C13 C14 C9 0.0(8) . . . . ? C10 C9 C14 C13 -1.1(7) . . . . ? P1 C9 C14 C13 177.4(4) . . . . ? C9 P1 C15 C16 -76.9(4) . . . . ? C21 P1 C15 C16 163.7(3) . . . . ? C3 P1 C15 C16 41.9(4) . . . . ? C9 P1 C15 C20 93.9(4) . . . . ? C21 P1 C15 C20 -25.5(4) . . . . ? C3 P1 C15 C20 -147.3(4) . . . . ? C20 C15 C16 C17 -1.6(6) . . . . ? P1 C15 C16 C17 169.4(3) . . . . ? C15 C16 C17 C18 0.3(7) . . . . ? C16 C17 C18 C19 2.4(7) . . . . ? C17 C18 C19 C20 -3.7(7) . . . . ? C18 C19 C20 C15 2.3(7) . . . . ? C16 C15 C20 C19 0.3(6) . . . . ? P1 C15 C20 C19 -170.5(4) . . . . ? C15 P1 C21 C26 116.3(4) . . . . ? C9 P1 C21 C26 -2.4(5) . . . . ? C3 P1 C21 C26 -124.7(4) . . . . ? C15 P1 C21 C22 -61.3(4) . . . . ? C9 P1 C21 C22 180.0(4) . . . . ? C3 P1 C21 C22 57.7(4) . . . . ? C26 C21 C22 C23 -0.6(8) . . . . ? P1 C21 C22 C23 177.0(4) . . . . ? C21 C22 C23 C24 0.9(9) . . . . ? C22 C23 C24 C25 -0.4(9) . . . . ? C23 C24 C25 C26 -0.3(10) . . . . ? C24 C25 C26 C21 0.5(10) . . . . ? C22 C21 C26 C25 -0.1(8) . . . . ? P1 C21 C26 C25 -177.7(5) . . . . ? S32 Pd31 S31 C31 -179.24(14) 2_566 . . . ? S32 Pd31 S31 C31 0.76(14) . . . . ? S31 Pd31 S31 C31 87(100) 2_566 . . . ? S32 Pd31 S32 C31 -21(100) 2_566 . . . ? S31 Pd31 S32 C31 179.24(14) 2_566 . . . ? S31 Pd31 S32 C31 -0.76(14) . . . . ? Pd31 S31 C31 N31 178.4(4) . . . . ? Pd31 S31 C31 S32 -1.06(19) . . . . ? Pd31 S32 C31 N31 -178.5(4) . . . . ? Pd31 S32 C31 S31 1.1(2) . . . . ? S31 C31 N31 C32 -1.4(6) . . . . ? S32 C31 N31 C32 178.1(4) . . . . ? C31 N31 C32 N32 -173(5) . . . . ? C39 P31 C33 C34 -101.3(4) . . . . ? C45 P31 C33 C34 17.7(4) . . . . ? C51 P31 C33 C34 141.5(4) . . . . ? C39 P31 C33 C38 73.2(4) . . . . ? C45 P31 C33 C38 -167.8(3) . . . . ? C51 P31 C33 C38 -43.9(4) . . . . ? C38 C33 C34 C35 0.7(7) . . . . ? P31 C33 C34 C35 175.2(3) . . . . ? C33 C34 C35 C36 0.4(7) . . . . ? C34 C35 C36 C37 -2.2(8) . . . . ? C35 C36 C37 C38 2.8(8) . . . . ? C34 C33 C38 C37 -0.1(6) . . . . ? P31 C33 C38 C37 -174.8(3) . . . . ? C36 C37 C38 C33 -1.6(7) . . . . ? C33 P31 C39 C44 2.8(4) . . . . ? C45 P31 C39 C44 -116.4(4) . . . . ? C51 P31 C39 C44 122.3(4) . . . . ? C33 P31 C39 C40 -177.6(4) . . . . ? C45 P31 C39 C40 63.3(4) . . . . ? C51 P31 C39 C40 -58.0(4) . . . . ? C44 C39 C40 C41 2.9(7) . . . . ? P31 C39 C40 C41 -176.8(4) . . . . ? C39 C40 C41 C42 -1.7(8) . . . . ? C40 C41 C42 C43 0.1(8) . . . . ? C41 C42 C43 C44 0.5(8) . . . . ? C40 C39 C44 C43 -2.3(6) . . . . ? P31 C39 C44 C43 177.4(3) . . . . ? C42 C43 C44 C39 0.7(7) . . . . ? C39 P31 C45 C50 -1.6(4) . . . . ? C33 P31 C45 C50 -120.6(4) . . . . ? C51 P31 C45 C50 116.4(4) . . . . ? C39 P31 C45 C46 177.1(3) . . . . ? C33 P31 C45 C46 58.2(4) . . . . ? C51 P31 C45 C46 -64.8(4) . . . . ? C50 C45 C46 C47 -2.5(6) . . . . ? P31 C45 C46 C47 178.7(4) . . . . ? C45 C46 C47 C48 1.7(7) . . . . ? C46 C47 C48 C49 0.1(8) . . . . ? C47 C48 C49 C50 -0.9(7) . . . . ? C48 C49 C50 C45 0.1(7) . . . . ? C46 C45 C50 C49 1.6(6) . . . . ? P31 C45 C50 C49 -179.6(3) . . . . ? C39 P31 C51 C52 -27.4(4) . . . . ? C33 P31 C51 C52 91.1(4) . . . . ? C45 P31 C51 C52 -146.7(4) . . . . ? C39 P31 C51 C56 155.6(4) . . . . ? C33 P31 C51 C56 -85.9(4) . . . . ? C45 P31 C51 C56 36.3(4) . . . . ? C56 C51 C52 C53 -1.1(7) . . . . ? P31 C51 C52 C53 -178.2(4) . . . . ? C51 C52 C53 C54 0.8(8) . . . . ? C52 C53 C54 C55 0.4(8) . . . . ? C53 C54 C55 C56 -1.2(8) . . . . ? C52 C51 C56 C55 0.3(7) . . . . ? P31 C51 C56 C55 177.3(4) . . . . ? C54 C55 C56 C51 0.9(8) . . . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 21.97 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 0.238 _refine_diff_density_min -0.298 _refine_diff_density_rms 0.055 data_4 _database_code_depnum_ccdc_archive 'CCDC 224726' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[C2 N2 S2].[C8 H11 P]2.Pt' _chemical_formula_sum 'C18 H22 N2 P2 Pt S2' _chemical_formula_weight 587.53 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' Pt Pt -1.7033 8.3905 '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 33.846(10) _cell_length_b 11.431(7) _cell_length_c 11.030(7) _cell_angle_alpha 90.00 _cell_angle_beta 92.792(9) _cell_angle_gamma 90.00 _cell_volume 4262(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5262 _cell_measurement_theta_min 2.2553 _cell_measurement_theta_max 24.7121 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.1500 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.0600 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.831 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 6.934 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6684 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _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_type CCD _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 0.85 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7744 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 24.71 _reflns_number_total 3264 _reflns_number_gt 2747 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+9.4807P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00023(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3264 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0712 _refine_ls_wR_factor_gt 0.0676 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.002 _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 Pt1 Pt 0.634292(7) 0.08693(2) 0.09288(2) 0.03006(12) Uani 1 1 d . . . S1 S 0.61269(5) -0.09719(14) 0.15758(17) 0.0420(4) Uani 1 1 d . . . S2 S 0.67414(5) -0.05024(17) -0.00376(17) 0.0472(5) Uani 1 1 d . . . C1 C 0.64754(19) -0.1583(6) 0.0663(6) 0.0377(16) Uani 1 1 d . . . N1 N 0.65352(19) -0.2687(5) 0.0456(5) 0.0516(16) Uani 1 1 d . . . C2 C 0.6293(3) -0.3442(7) 0.0920(7) 0.053(2) Uani 1 1 d . . . N2 N 0.6080(3) -0.4181(6) 0.1242(7) 0.076(2) Uani 1 1 d . . . P1 P 0.58818(5) 0.18810(15) 0.19230(15) 0.0336(4) Uani 1 1 d . . . C3 C 0.5664(2) 0.1025(6) 0.3099(6) 0.0453(18) Uani 1 1 d . . . H3A H 0.5472 0.1489 0.3492 0.068 Uiso 1 1 calc R . . H3B H 0.5867 0.0785 0.3684 0.068 Uiso 1 1 calc R . . H3C H 0.5538 0.0346 0.2744 0.068 Uiso 1 1 calc R . . C4 C 0.6026(2) 0.3214(6) 0.2708(6) 0.0442(17) Uani 1 1 d . . . H4A H 0.5802 0.3542 0.3083 0.066 Uiso 1 1 calc R . . H4B H 0.6125 0.3764 0.2138 0.066 Uiso 1 1 calc R . . H4C H 0.6230 0.3043 0.3319 0.066 Uiso 1 1 calc R . . C5 C 0.54606(18) 0.2245(6) 0.0910(6) 0.0367(15) Uani 1 1 d . . . C6 C 0.5339(2) 0.1424(8) 0.0037(7) 0.063(2) Uani 1 1 d . . . H6A H 0.5478 0.0725 -0.0009 0.075 Uiso 1 1 calc R . . C7 C 0.5025(3) 0.1612(10) -0.0749(8) 0.079(3) Uani 1 1 d . . . H7A H 0.4950 0.1041 -0.1315 0.094 Uiso 1 1 calc R . . C8 C 0.4818(3) 0.2635(9) -0.0712(8) 0.076(3) Uani 1 1 d . . . H8A H 0.4609 0.2772 -0.1270 0.091 Uiso 1 1 calc R . . C9 C 0.4920(2) 0.3462(8) 0.0151(9) 0.073(3) Uani 1 1 d . . . H9A H 0.4774 0.4148 0.0195 0.088 Uiso 1 1 calc R . . C10 C 0.5245(2) 0.3272(7) 0.0967(8) 0.060(2) Uani 1 1 d . . . H10A H 0.5315 0.3836 0.1546 0.073 Uiso 1 1 calc R . . P2 P 0.66116(5) 0.24751(15) 0.00876(14) 0.0333(4) Uani 1 1 d . . . C11 C 0.6261(2) 0.3447(6) -0.0680(6) 0.0431(17) Uani 1 1 d . . . H11A H 0.6399 0.4099 -0.1007 0.065 Uiso 1 1 calc R . . H11B H 0.6075 0.3724 -0.0113 0.065 Uiso 1 1 calc R . . H11C H 0.6121 0.3033 -0.1326 0.065 Uiso 1 1 calc R . . C12 C 0.6948(2) 0.2130(7) -0.1081(6) 0.054(2) Uani 1 1 d . . . H12A H 0.7052 0.2841 -0.1402 0.080 Uiso 1 1 calc R . . H12B H 0.6810 0.1704 -0.1720 0.080 Uiso 1 1 calc R . . H12C H 0.7161 0.1662 -0.0742 0.080 Uiso 1 1 calc R . . C13 C 0.69052(18) 0.3373(6) 0.1156(5) 0.0325(15) Uani 1 1 d . . . C14 C 0.7014(2) 0.4507(6) 0.0872(6) 0.0423(17) Uani 1 1 d . . . H14A H 0.6927 0.4826 0.0130 0.051 Uiso 1 1 calc R . . C15 C 0.7246(2) 0.5168(7) 0.1662(7) 0.0529(19) Uani 1 1 d . . . H15A H 0.7310 0.5934 0.1466 0.063 Uiso 1 1 calc R . . C16 C 0.7384(2) 0.4688(8) 0.2748(7) 0.057(2) Uani 1 1 d . . . H16A H 0.7550 0.5122 0.3273 0.069 Uiso 1 1 calc R . . C17 C 0.7278(2) 0.3576(7) 0.3056(6) 0.053(2) Uani 1 1 d . . . H17A H 0.7367 0.3263 0.3797 0.064 Uiso 1 1 calc R . . C18 C 0.7037(2) 0.2916(6) 0.2268(6) 0.0434(17) Uani 1 1 d . . . H18A H 0.6964 0.2163 0.2485 0.052 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 Pt1 0.03023(16) 0.02497(16) 0.03484(19) -0.00032(11) -0.00004(10) 0.00032(11) S1 0.0473(10) 0.0262(9) 0.0529(11) 0.0040(8) 0.0067(9) 0.0004(8) S2 0.0447(11) 0.0374(10) 0.0603(12) -0.0061(9) 0.0095(9) 0.0062(8) C1 0.039(4) 0.032(4) 0.041(4) -0.005(3) -0.011(3) 0.002(3) N1 0.071(4) 0.032(4) 0.051(4) 0.001(3) -0.009(3) 0.009(3) C2 0.075(6) 0.035(5) 0.046(5) -0.005(4) -0.007(4) 0.023(4) N2 0.118(7) 0.037(4) 0.073(5) 0.000(4) 0.012(5) 0.007(4) P1 0.0380(10) 0.0283(10) 0.0346(10) 0.0007(7) 0.0030(8) -0.0003(8) C3 0.053(4) 0.039(4) 0.045(4) 0.001(3) 0.012(3) -0.003(3) C4 0.046(4) 0.042(4) 0.045(4) -0.012(3) 0.007(3) -0.006(3) C5 0.031(3) 0.036(4) 0.043(4) 0.006(3) 0.006(3) 0.001(3) C6 0.049(5) 0.087(7) 0.051(5) -0.016(5) -0.010(4) 0.021(5) C7 0.066(6) 0.100(8) 0.068(6) -0.021(6) -0.016(5) 0.008(6) C8 0.064(6) 0.090(8) 0.070(6) 0.032(6) -0.019(5) -0.014(6) C9 0.045(5) 0.049(6) 0.125(8) 0.034(6) -0.005(5) 0.003(4) C10 0.049(5) 0.034(4) 0.097(6) 0.007(4) -0.009(4) -0.001(4) P2 0.0350(9) 0.0314(10) 0.0338(9) 0.0001(7) 0.0035(7) -0.0041(8) C11 0.053(4) 0.038(4) 0.038(4) 0.006(3) -0.008(3) -0.005(3) C12 0.066(5) 0.048(5) 0.048(4) -0.011(4) 0.023(4) -0.009(4) C13 0.032(3) 0.033(4) 0.033(4) -0.004(3) 0.005(3) -0.003(3) C14 0.044(4) 0.036(4) 0.048(4) -0.002(3) 0.007(3) 0.000(3) C15 0.051(5) 0.034(4) 0.074(5) -0.006(4) 0.006(4) -0.001(4) C16 0.049(5) 0.054(5) 0.069(6) -0.022(4) -0.002(4) -0.005(4) C17 0.052(5) 0.064(6) 0.043(5) -0.011(4) -0.007(4) 0.006(4) C18 0.048(4) 0.043(4) 0.039(4) 0.000(3) 0.000(3) -0.004(3) _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 Pt1 P2 2.2670(19) . ? Pt1 P1 2.2677(18) . ? Pt1 S1 2.350(2) . ? Pt1 S2 2.3566(19) . ? S1 C1 1.734(7) . ? S2 C1 1.733(7) . ? C1 N1 1.300(8) . ? N1 C2 1.312(11) . ? C2 N2 1.176(11) . ? P1 C4 1.808(7) . ? P1 C3 1.810(6) . ? P1 C5 1.816(6) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C10 1.386(9) . ? C5 C6 1.392(10) . ? C6 C7 1.356(11) . ? C6 H6A 0.9300 . ? C7 C8 1.365(12) . ? C7 H7A 0.9300 . ? C8 C9 1.374(12) . ? C8 H8A 0.9300 . ? C9 C10 1.402(10) . ? C9 H9A 0.9300 . ? C10 H10A 0.9300 . ? P2 C12 1.804(6) . ? P2 C11 1.806(7) . ? P2 C13 1.821(6) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C18 1.386(9) . ? C13 C14 1.388(9) . ? C14 C15 1.371(10) . ? C14 H14A 0.9300 . ? C15 C16 1.379(11) . ? C15 H15A 0.9300 . ? C16 C17 1.368(11) . ? C16 H16A 0.9300 . ? C17 C18 1.386(9) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? 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 P2 Pt1 P1 94.83(7) . . ? P2 Pt1 S1 170.48(6) . . ? P1 Pt1 S1 94.49(7) . . ? P2 Pt1 S2 95.96(8) . . ? P1 Pt1 S2 168.68(6) . . ? S1 Pt1 S2 74.62(7) . . ? C1 S1 Pt1 87.4(2) . . ? C1 S2 Pt1 87.2(2) . . ? N1 C1 S2 121.7(6) . . ? N1 C1 S1 127.5(6) . . ? S2 C1 S1 110.7(4) . . ? C1 N1 C2 117.6(7) . . ? N2 C2 N1 173.8(8) . . ? C4 P1 C3 102.9(3) . . ? C4 P1 C5 106.7(3) . . ? C3 P1 C5 103.3(3) . . ? C4 P1 Pt1 119.0(2) . . ? C3 P1 Pt1 112.6(2) . . ? C5 P1 Pt1 110.9(2) . . ? P1 C3 H3A 109.5 . . ? P1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? P1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? P1 C4 H4A 109.5 . . ? P1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? P1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C10 C5 C6 117.7(7) . . ? C10 C5 P1 124.5(6) . . ? C6 C5 P1 117.9(5) . . ? C7 C6 C5 122.1(8) . . ? C7 C6 H6A 119.0 . . ? C5 C6 H6A 119.0 . . ? C6 C7 C8 120.3(9) . . ? C6 C7 H7A 119.9 . . ? C8 C7 H7A 119.9 . . ? C7 C8 C9 119.9(8) . . ? C7 C8 H8A 120.0 . . ? C9 C8 H8A 120.0 . . ? C8 C9 C10 120.0(9) . . ? C8 C9 H9A 120.0 . . ? C10 C9 H9A 120.0 . . ? C5 C10 C9 120.0(8) . . ? C5 C10 H10A 120.0 . . ? C9 C10 H10A 120.0 . . ? C12 P2 C11 102.9(3) . . ? C12 P2 C13 104.0(3) . . ? C11 P2 C13 106.4(3) . . ? C12 P2 Pt1 113.3(3) . . ? C11 P2 Pt1 115.0(2) . . ? C13 P2 Pt1 114.1(2) . . ? P2 C11 H11A 109.5 . . ? P2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P2 C12 H12A 109.5 . . ? P2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 118.4(6) . . ? C18 C13 P2 120.1(5) . . ? C14 C13 P2 121.5(5) . . ? C15 C14 C13 121.4(7) . . ? C15 C14 H14A 119.3 . . ? C13 C14 H14A 119.3 . . ? C14 C15 C16 119.6(7) . . ? C14 C15 H15A 120.2 . . ? C16 C15 H15A 120.2 . . ? C17 C16 C15 120.2(7) . . ? C17 C16 H16A 119.9 . . ? C15 C16 H16A 119.9 . . ? C16 C17 C18 120.3(7) . . ? C16 C17 H17A 119.9 . . ? C18 C17 H17A 119.9 . . ? C17 C18 C13 120.2(7) . . ? C17 C18 H18A 119.9 . . ? C13 C18 H18A 119.9 . . ? 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 P2 Pt1 S1 C1 7.6(5) . . . . ? P1 Pt1 S1 C1 175.8(2) . . . . ? S2 Pt1 S1 C1 -1.1(2) . . . . ? P2 Pt1 S2 C1 -177.5(2) . . . . ? P1 Pt1 S2 C1 -15.2(4) . . . . ? S1 Pt1 S2 C1 1.1(2) . . . . ? Pt1 S2 C1 N1 176.2(6) . . . . ? Pt1 S2 C1 S1 -1.5(3) . . . . ? Pt1 S1 C1 N1 -176.1(6) . . . . ? Pt1 S1 C1 S2 1.5(3) . . . . ? S2 C1 N1 C2 -172.8(5) . . . . ? S1 C1 N1 C2 4.6(10) . . . . ? C1 N1 C2 N2 146(8) . . . . ? P2 Pt1 P1 C4 -43.5(3) . . . . ? S1 Pt1 P1 C4 138.4(3) . . . . ? S2 Pt1 P1 C4 154.1(4) . . . . ? P2 Pt1 P1 C3 -164.0(3) . . . . ? S1 Pt1 P1 C3 18.0(3) . . . . ? S2 Pt1 P1 C3 33.7(4) . . . . ? P2 Pt1 P1 C5 80.8(2) . . . . ? S1 Pt1 P1 C5 -97.3(2) . . . . ? S2 Pt1 P1 C5 -81.5(4) . . . . ? C4 P1 C5 C10 -13.7(7) . . . . ? C3 P1 C5 C10 94.4(6) . . . . ? Pt1 P1 C5 C10 -144.7(5) . . . . ? C4 P1 C5 C6 168.1(6) . . . . ? C3 P1 C5 C6 -83.8(6) . . . . ? Pt1 P1 C5 C6 37.1(6) . . . . ? C10 C5 C6 C7 0.9(12) . . . . ? P1 C5 C6 C7 179.2(7) . . . . ? C5 C6 C7 C8 0.7(14) . . . . ? C6 C7 C8 C9 -2.2(14) . . . . ? C7 C8 C9 C10 2.2(13) . . . . ? C6 C5 C10 C9 -0.9(11) . . . . ? P1 C5 C10 C9 -179.1(6) . . . . ? C8 C9 C10 C5 -0.6(12) . . . . ? P1 Pt1 P2 C12 -168.4(3) . . . . ? S1 Pt1 P2 C12 -0.2(5) . . . . ? S2 Pt1 P2 C12 8.2(3) . . . . ? P1 Pt1 P2 C11 -50.5(2) . . . . ? S1 Pt1 P2 C11 117.7(4) . . . . ? S2 Pt1 P2 C11 126.1(2) . . . . ? P1 Pt1 P2 C13 72.9(2) . . . . ? S1 Pt1 P2 C13 -119.0(4) . . . . ? S2 Pt1 P2 C13 -110.6(2) . . . . ? C12 P2 C13 C18 -106.7(6) . . . . ? C11 P2 C13 C18 145.1(5) . . . . ? Pt1 P2 C13 C18 17.2(6) . . . . ? C12 P2 C13 C14 71.2(6) . . . . ? C11 P2 C13 C14 -37.0(6) . . . . ? Pt1 P2 C13 C14 -164.9(4) . . . . ? C18 C13 C14 C15 0.2(10) . . . . ? P2 C13 C14 C15 -177.8(5) . . . . ? C13 C14 C15 C16 1.7(11) . . . . ? C14 C15 C16 C17 -2.5(11) . . . . ? C15 C16 C17 C18 1.4(11) . . . . ? C16 C17 C18 C13 0.6(11) . . . . ? C14 C13 C18 C17 -1.3(10) . . . . ? P2 C13 C18 C17 176.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.898 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.898 _refine_diff_density_max 0.673 _refine_diff_density_min -0.653 _refine_diff_density_rms 0.122 data_10 _database_code_depnum_ccdc_archive 'CCDC 224727' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H30 Rh2.[C2 N2 S2]2.[C H Cl3]2' _chemical_formula_sum 'C26 H32 Cl6 N4 Rh2 S4' _chemical_formula_weight 947.32 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' 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' 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 P2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 19.181(4) _cell_length_b 8.8430(19) _cell_length_c 21.576(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.771(3) _cell_angle_gamma 90.00 _cell_volume 3569.2(13) _cell_formula_units_Z 4 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used 125 _cell_measurement_theta_min 12 _cell_measurement_theta_max 28 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max .15 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.763 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 1.633 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.625713 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 0.9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16908 _diffrn_reflns_av_R_equivalents 0.1637 _diffrn_reflns_av_sigmaI/netI 0.1220 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 23.35 _reflns_number_total 5062 _reflns_number_gt 3478 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0120P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef - _refine_ls_number_reflns 5062 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0782 _refine_ls_R_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.0761 _refine_ls_wR_factor_gt 0.0672 _refine_ls_goodness_of_fit_ref 0.934 _refine_ls_restrained_S_all 0.934 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.001 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 Rh1 Rh 0.30095(2) 0.40761(5) 0.18935(2) 0.02104(13) Uani 1 1 d . . . S1 S 0.32245(8) 0.38012(16) 0.30270(7) 0.0239(3) Uani 1 1 d . . . S2 S 0.32995(8) 0.15071(16) 0.21184(7) 0.0247(4) Uani 1 1 d . . . C1 C 0.3382(3) 0.1832(6) 0.2906(3) 0.0235(14) Uani 1 1 d . . . N1 N 0.3554(2) 0.0820(5) 0.3349(2) 0.0286(12) Uani 1 1 d . . . C2 C 0.3593(3) 0.1218(7) 0.3954(3) 0.0356(16) Uani 1 1 d . . . N2 N 0.3645(3) 0.1431(6) 0.4487(3) 0.0537(17) Uani 1 1 d . . . C3 C 0.3937(3) 0.4886(7) 0.1604(3) 0.0346(17) Uani 1 1 d . . . C4 C 0.3450(3) 0.4256(7) 0.1050(3) 0.0324(16) Uani 1 1 d . . . C5 C 0.2814(3) 0.5111(6) 0.0957(3) 0.0242(14) Uani 1 1 d . . . C6 C 0.2909(3) 0.6302(6) 0.1433(3) 0.0276(15) Uani 1 1 d . . . C7 C 0.3593(3) 0.6154(7) 0.1820(3) 0.0315(15) Uani 1 1 d . . . C8 C 0.4706(3) 0.4371(9) 0.1875(4) 0.065(3) Uani 1 1 d . . . H8A H 0.5036 0.5008 0.1703 0.098 Uiso 1 1 calc R . . H8B H 0.4761 0.3315 0.1756 0.098 Uiso 1 1 calc R . . H8C H 0.4813 0.4460 0.2339 0.098 Uiso 1 1 calc R . . C9 C 0.3588(4) 0.2952(7) 0.0657(3) 0.049(2) Uani 1 1 d . . . H9A H 0.3133 0.2483 0.0451 0.073 Uiso 1 1 calc R . . H9B H 0.3888 0.2207 0.0930 0.073 Uiso 1 1 calc R . . H9C H 0.3835 0.3308 0.0332 0.073 Uiso 1 1 calc R . . C10 C 0.2158(3) 0.4921(7) 0.0436(3) 0.0393(18) Uani 1 1 d . . . H10A H 0.2245 0.5346 0.0040 0.059 Uiso 1 1 calc R . . H10B H 0.1756 0.5449 0.0551 0.059 Uiso 1 1 calc R . . H10C H 0.2045 0.3843 0.0376 0.059 Uiso 1 1 calc R . . C11 C 0.2382(3) 0.7532(6) 0.1453(3) 0.0413(18) Uani 1 1 d . . . H11A H 0.2492 0.8012 0.1873 0.062 Uiso 1 1 calc R . . H11B H 0.1899 0.7103 0.1373 0.062 Uiso 1 1 calc R . . H11C H 0.2408 0.8288 0.1127 0.062 Uiso 1 1 calc R . . C12 C 0.3941(4) 0.7171(7) 0.2367(3) 0.048(2) Uani 1 1 d . . . H12A H 0.4315 0.7776 0.2242 0.072 Uiso 1 1 calc R . . H12B H 0.4152 0.6549 0.2736 0.072 Uiso 1 1 calc R . . H12C H 0.3580 0.7844 0.2475 0.072 Uiso 1 1 calc R . . Rh21 Rh 0.69019(2) 0.13106(5) 0.30361(2) 0.01897(13) Uani 1 1 d . . . S21 S 0.68317(8) 0.16387(16) 0.19224(7) 0.0231(4) Uani 1 1 d . . . S22 S 0.66071(8) 0.38776(16) 0.28061(7) 0.0250(4) Uani 1 1 d . . . C21 C 0.6657(3) 0.3594(6) 0.2030(3) 0.0210(13) Uani 1 1 d . . . N21 N 0.6583(2) 0.4680(5) 0.1612(2) 0.0249(12) Uani 1 1 d . . . C22 C 0.6691(3) 0.4378(6) 0.1038(3) 0.0302(15) Uani 1 1 d . . . N22 N 0.6786(3) 0.4297(6) 0.0528(3) 0.0437(15) Uani 1 1 d . . . C23 C 0.6939(3) 0.0288(6) 0.3971(3) 0.0267(15) Uani 1 1 d . . . C24 C 0.6275(3) 0.1012(6) 0.3760(3) 0.0264(14) Uani 1 1 d . . . C25 C 0.5924(3) 0.0337(6) 0.3159(3) 0.0222(14) Uani 1 1 d . . . C26 C 0.6361(3) -0.0862(6) 0.3030(3) 0.0220(14) Uani 1 1 d . . . C27 C 0.6992(3) -0.0890(6) 0.3519(3) 0.0216(14) Uani 1 1 d . . . C28 C 0.7475(3) 0.0574(8) 0.4576(3) 0.050(2) Uani 1 1 d . . . H28A H 0.7451 0.1636 0.4699 0.075 Uiso 1 1 calc R . . H28B H 0.7956 0.0350 0.4514 0.075 Uiso 1 1 calc R . . H28C H 0.7372 -0.0077 0.4912 0.075 Uiso 1 1 calc R . . C29 C 0.5986(4) 0.2253(7) 0.4116(3) 0.051(2) Uani 1 1 d . . . H29A H 0.5715 0.1802 0.4405 0.077 Uiso 1 1 calc R . . H29B H 0.5672 0.2914 0.3812 0.077 Uiso 1 1 calc R . . H29C H 0.6384 0.2846 0.4362 0.077 Uiso 1 1 calc R . . C30 C 0.5182(3) 0.0727(7) 0.2790(3) 0.0373(17) Uani 1 1 d . . . H30A H 0.5156 0.0582 0.2335 0.056 Uiso 1 1 calc R . . H30B H 0.5076 0.1784 0.2870 0.056 Uiso 1 1 calc R . . H30C H 0.4833 0.0067 0.2926 0.056 Uiso 1 1 calc R . . C31 C 0.6155(3) -0.1922(7) 0.2474(3) 0.0379(17) Uani 1 1 d . . . H31A H 0.5776 -0.2603 0.2544 0.057 Uiso 1 1 calc R . . H31B H 0.6572 -0.2518 0.2432 0.057 Uiso 1 1 calc R . . H31C H 0.5981 -0.1337 0.2085 0.057 Uiso 1 1 calc R . . C32 C 0.7590(3) -0.2048(7) 0.3610(3) 0.049(2) Uani 1 1 d . . . H32A H 0.7554 -0.2725 0.3962 0.074 Uiso 1 1 calc R . . H32B H 0.8052 -0.1528 0.3708 0.074 Uiso 1 1 calc R . . H32C H 0.7548 -0.2640 0.3220 0.074 Uiso 1 1 calc R . . C41 C 0.5285(3) 0.6810(6) 0.4389(3) 0.0331(16) Uani 1 1 d . . . H41A H 0.5489 0.6770 0.4858 0.040 Uiso 1 1 calc R . . Cl1 Cl 0.48584(11) 0.8541(2) 0.41914(11) 0.0699(6) Uani 1 1 d . . . Cl2 Cl 0.46412(9) 0.53360(19) 0.41685(9) 0.0460(5) Uani 1 1 d . . . Cl3 Cl 0.59657(9) 0.6525(2) 0.39790(8) 0.0464(5) Uani 1 1 d . . . C51 C 0.5536(3) 0.2433(7) -0.0317(3) 0.0431(18) Uani 1 1 d . . . H51A H 0.5888 0.3283 -0.0223 0.052 Uiso 1 1 calc R . . Cl4 Cl 0.58243(10) 0.1144(2) -0.08288(9) 0.0555(5) Uani 1 1 d . . . Cl5 Cl 0.46999(11) 0.3167(3) -0.06983(10) 0.0753(7) Uani 1 1 d . . . Cl6 Cl 0.54810(10) 0.1560(2) 0.04019(8) 0.0543(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0198(3) 0.0182(3) 0.0253(3) 0.0028(2) 0.0053(2) -0.0005(2) S1 0.0208(8) 0.0210(9) 0.0304(9) -0.0014(7) 0.0069(7) -0.0007(7) S2 0.0258(9) 0.0214(9) 0.0286(9) 0.0031(7) 0.0093(7) 0.0067(7) C1 0.017(3) 0.014(3) 0.041(4) 0.000(3) 0.009(3) 0.006(3) N1 0.026(3) 0.032(3) 0.029(3) 0.000(3) 0.009(2) 0.003(2) C2 0.035(4) 0.029(4) 0.041(5) 0.006(3) 0.005(4) 0.009(3) N2 0.069(5) 0.052(4) 0.039(4) 0.013(3) 0.009(3) 0.013(3) C3 0.014(3) 0.045(4) 0.046(4) 0.024(3) 0.008(3) -0.004(3) C4 0.032(4) 0.027(4) 0.042(4) 0.022(3) 0.017(3) 0.004(3) C5 0.023(3) 0.022(4) 0.027(4) 0.014(3) 0.003(3) -0.001(3) C6 0.029(4) 0.022(4) 0.033(4) 0.005(3) 0.008(3) -0.001(3) C7 0.031(4) 0.023(4) 0.041(4) 0.006(3) 0.009(3) -0.012(3) C8 0.021(4) 0.087(6) 0.089(6) 0.054(5) 0.017(4) 0.004(4) C9 0.068(5) 0.038(4) 0.053(5) 0.002(3) 0.042(4) 0.012(4) C10 0.035(4) 0.050(5) 0.030(4) 0.019(3) 0.002(3) -0.003(3) C11 0.058(5) 0.017(4) 0.052(5) 0.014(3) 0.021(4) 0.018(3) C12 0.055(5) 0.029(4) 0.054(5) 0.004(3) -0.002(4) -0.027(4) Rh21 0.0178(3) 0.0160(3) 0.0239(3) 0.0019(2) 0.0063(2) 0.0006(2) S21 0.0182(8) 0.0195(8) 0.0314(9) -0.0010(7) 0.0053(7) -0.0003(6) S22 0.0262(9) 0.0197(8) 0.0306(9) 0.0025(7) 0.0094(7) 0.0055(7) C21 0.009(3) 0.017(3) 0.037(4) 0.002(3) 0.005(3) 0.001(2) N21 0.018(3) 0.027(3) 0.029(3) 0.006(2) 0.002(2) 0.002(2) C22 0.036(4) 0.019(4) 0.038(4) 0.008(3) 0.014(3) -0.002(3) N22 0.051(4) 0.034(3) 0.047(4) 0.011(3) 0.014(3) -0.004(3) C23 0.026(4) 0.028(4) 0.025(4) 0.014(3) 0.003(3) -0.005(3) C24 0.036(4) 0.015(3) 0.032(4) 0.003(3) 0.017(3) -0.003(3) C25 0.019(3) 0.016(3) 0.030(4) 0.006(3) 0.001(3) -0.005(3) C26 0.027(3) 0.012(3) 0.031(3) 0.004(3) 0.012(3) -0.005(3) C27 0.022(3) 0.016(3) 0.030(4) 0.005(3) 0.011(3) 0.000(3) C28 0.058(5) 0.057(5) 0.028(4) 0.017(3) -0.007(4) -0.024(4) C29 0.064(5) 0.043(5) 0.060(5) -0.014(4) 0.041(4) -0.007(4) C30 0.020(4) 0.036(4) 0.053(5) 0.016(3) 0.001(3) -0.003(3) C31 0.049(4) 0.020(4) 0.046(4) -0.008(3) 0.012(4) -0.012(3) C32 0.032(4) 0.043(5) 0.078(6) 0.035(4) 0.026(4) 0.017(3) C41 0.031(4) 0.025(4) 0.044(4) 0.004(3) 0.012(3) 0.001(3) Cl1 0.0594(13) 0.0367(12) 0.1125(19) 0.0168(11) 0.0164(13) 0.0169(10) Cl2 0.0338(10) 0.0455(11) 0.0583(12) 0.0020(9) 0.0092(9) -0.0107(8) Cl3 0.0406(11) 0.0509(11) 0.0530(11) 0.0107(9) 0.0220(9) -0.0018(9) C51 0.044(4) 0.036(4) 0.047(5) 0.000(3) 0.004(4) -0.003(3) Cl4 0.0649(13) 0.0524(12) 0.0567(12) 0.0049(9) 0.0294(10) -0.0025(10) Cl5 0.0532(13) 0.1020(18) 0.0720(15) 0.0331(13) 0.0163(12) 0.0317(12) Cl6 0.0563(12) 0.0685(13) 0.0371(11) 0.0112(9) 0.0079(9) -0.0173(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 Rh1 C3 2.135(5) . ? Rh1 C4 2.175(6) . ? Rh1 C5 2.175(5) . ? Rh1 C7 2.175(5) . ? Rh1 C6 2.195(6) . ? Rh1 S2 2.3635(16) . ? Rh1 S1 2.4008(16) . ? Rh1 S1 2.4230(15) 2 ? S1 C1 1.796(6) . ? S1 Rh1 2.4230(15) 2 ? S2 C1 1.695(6) . ? C1 N1 1.299(7) . ? N1 C2 1.337(8) . ? C2 N2 1.149(8) . ? C3 C7 1.430(8) . ? C3 C4 1.454(9) . ? C3 C8 1.532(8) . ? C4 C5 1.412(7) . ? C4 C9 1.489(8) . ? C5 C6 1.454(8) . ? C5 C10 1.499(8) . ? C6 C7 1.396(8) . ? C6 C11 1.492(7) . ? C7 C12 1.516(8) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? Rh21 C25 2.134(5) . ? Rh21 C26 2.182(5) . ? Rh21 C24 2.187(5) . ? Rh21 C27 2.196(5) . ? Rh21 C23 2.198(5) . ? Rh21 S22 2.3654(16) . ? Rh21 S21 2.3944(16) . ? Rh21 S21 2.4284(15) 2_655 ? S21 C21 1.786(5) . ? S21 Rh21 2.4284(15) 2_655 ? S22 C21 1.716(6) . ? C21 N21 1.305(7) . ? N21 C22 1.327(7) . ? C22 N22 1.156(7) . ? C23 C24 1.408(8) . ? C23 C27 1.446(8) . ? C23 C28 1.493(8) . ? C24 C25 1.450(8) . ? C24 C29 1.513(8) . ? C25 C26 1.418(7) . ? C25 C30 1.508(7) . ? C26 C27 1.419(7) . ? C26 C31 1.504(8) . ? C27 C32 1.517(7) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C41 Cl1 1.743(6) . ? C41 Cl3 1.750(6) . ? C41 Cl2 1.787(6) . ? C41 H41A 1.0000 . ? C51 Cl6 1.756(6) . ? C51 Cl5 1.758(6) . ? C51 Cl4 1.759(7) . ? C51 H51A 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Rh1 C4 39.4(2) . . ? C3 Rh1 C5 64.5(2) . . ? C4 Rh1 C5 37.9(2) . . ? C3 Rh1 C7 38.7(2) . . ? C4 Rh1 C7 64.9(2) . . ? C5 Rh1 C7 64.0(2) . . ? C3 Rh1 C6 64.0(2) . . ? C4 Rh1 C6 64.3(2) . . ? C5 Rh1 C6 38.9(2) . . ? C7 Rh1 C6 37.3(2) . . ? C3 Rh1 S2 102.07(17) . . ? C4 Rh1 S2 97.15(16) . . ? C5 Rh1 S2 125.43(16) . . ? C7 Rh1 S2 136.51(17) . . ? C6 Rh1 S2 161.47(15) . . ? C3 Rh1 S1 111.45(18) . . ? C4 Rh1 S1 148.04(17) . . ? C5 Rh1 S1 160.90(16) . . ? C7 Rh1 S1 100.65(17) . . ? C6 Rh1 S1 122.05(16) . . ? S2 Rh1 S1 73.38(5) . . ? C3 Rh1 S1 160.79(16) . 2 ? C4 Rh1 S1 129.28(17) . 2 ? C5 Rh1 S1 97.90(15) . 2 ? C7 Rh1 S1 128.04(17) . 2 ? C6 Rh1 S1 97.64(15) . 2 ? S2 Rh1 S1 94.49(5) . 2 ? S1 Rh1 S1 82.43(5) . 2 ? C1 S1 Rh1 86.9(2) . . ? C1 S1 Rh1 107.83(18) . 2 ? Rh1 S1 Rh1 96.39(5) . 2 ? C1 S2 Rh1 90.5(2) . . ? N1 C1 S2 125.0(4) . . ? N1 C1 S1 125.7(5) . . ? S2 C1 S1 109.2(3) . . ? C1 N1 C2 119.2(5) . . ? N2 C2 N1 174.0(7) . . ? C7 C3 C4 108.0(5) . . ? C7 C3 C8 125.7(6) . . ? C4 C3 C8 126.1(6) . . ? C7 C3 Rh1 72.1(3) . . ? C4 C3 Rh1 71.8(3) . . ? C8 C3 Rh1 125.6(4) . . ? C5 C4 C3 106.8(5) . . ? C5 C4 C9 126.2(6) . . ? C3 C4 C9 127.0(6) . . ? C5 C4 Rh1 71.0(3) . . ? C3 C4 Rh1 68.8(3) . . ? C9 C4 Rh1 124.8(4) . . ? C4 C5 C6 108.5(5) . . ? C4 C5 C10 127.1(6) . . ? C6 C5 C10 124.3(5) . . ? C4 C5 Rh1 71.1(3) . . ? C6 C5 Rh1 71.3(3) . . ? C10 C5 Rh1 126.4(4) . . ? C7 C6 C5 108.0(5) . . ? C7 C6 C11 127.1(6) . . ? C5 C6 C11 124.6(5) . . ? C7 C6 Rh1 70.6(3) . . ? C5 C6 Rh1 69.8(3) . . ? C11 C6 Rh1 129.2(4) . . ? C6 C7 C3 108.6(5) . . ? C6 C7 C12 127.1(6) . . ? C3 C7 C12 124.3(6) . . ? C6 C7 Rh1 72.1(3) . . ? C3 C7 Rh1 69.1(3) . . ? C12 C7 Rh1 126.1(4) . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C25 Rh21 C26 38.35(19) . . ? C25 Rh21 C24 39.2(2) . . ? C26 Rh21 C24 64.1(2) . . ? C25 Rh21 C27 64.1(2) . . ? C26 Rh21 C27 37.81(19) . . ? C24 Rh21 C27 63.4(2) . . ? C25 Rh21 C23 64.6(2) . . ? C26 Rh21 C23 64.0(2) . . ? C24 Rh21 C23 37.5(2) . . ? C27 Rh21 C23 38.4(2) . . ? C25 Rh21 S22 103.72(15) . . ? C26 Rh21 S22 138.81(15) . . ? C24 Rh21 S22 97.01(15) . . ? C27 Rh21 S22 160.07(14) . . ? C23 Rh21 S22 123.05(16) . . ? C25 Rh21 S21 108.55(16) . . ? C26 Rh21 S21 100.34(15) . . ? C24 Rh21 S21 144.43(16) . . ? C27 Rh21 S21 124.36(15) . . ? C23 Rh21 S21 162.62(16) . . ? S22 Rh21 S21 73.46(5) . . ? C25 Rh21 S21 160.68(15) . 2_655 ? C26 Rh21 S21 125.15(15) . 2_655 ? C24 Rh21 S21 133.73(16) . 2_655 ? C27 Rh21 S21 96.62(14) . 2_655 ? C23 Rh21 S21 100.72(15) . 2_655 ? S22 Rh21 S21 94.81(5) . 2_655 ? S21 Rh21 S21 81.75(5) . 2_655 ? C21 S21 Rh21 87.53(19) . . ? C21 S21 Rh21 108.99(18) . 2_655 ? Rh21 S21 Rh21 96.58(5) . 2_655 ? C21 S22 Rh21 90.13(19) . . ? N21 C21 S22 123.2(4) . . ? N21 C21 S21 128.1(5) . . ? S22 C21 S21 108.7(3) . . ? C21 N21 C22 118.8(5) . . ? N22 C22 N21 171.9(7) . . ? C24 C23 C27 107.6(5) . . ? C24 C23 C28 127.2(6) . . ? C27 C23 C28 125.0(5) . . ? C24 C23 Rh21 70.9(3) . . ? C27 C23 Rh21 70.7(3) . . ? C28 C23 Rh21 127.5(4) . . ? C23 C24 C25 108.1(5) . . ? C23 C24 C29 124.9(6) . . ? C25 C24 C29 127.0(5) . . ? C23 C24 Rh21 71.7(3) . . ? C25 C24 Rh21 68.4(3) . . ? C29 C24 Rh21 126.6(4) . . ? C26 C25 C24 107.7(5) . . ? C26 C25 C30 126.6(5) . . ? C24 C25 C30 125.2(5) . . ? C26 C25 Rh21 72.6(3) . . ? C24 C25 Rh21 72.4(3) . . ? C30 C25 Rh21 126.5(4) . . ? C25 C26 C27 108.2(5) . . ? C25 C26 C31 124.1(5) . . ? C27 C26 C31 127.8(5) . . ? C25 C26 Rh21 69.0(3) . . ? C27 C26 Rh21 71.6(3) . . ? C31 C26 Rh21 126.5(4) . . ? C26 C27 C23 108.3(5) . . ? C26 C27 C32 127.2(5) . . ? C23 C27 C32 124.2(6) . . ? C26 C27 Rh21 70.5(3) . . ? C23 C27 Rh21 70.9(3) . . ? C32 C27 Rh21 129.6(4) . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Cl1 C41 Cl3 111.4(3) . . ? Cl1 C41 Cl2 108.4(3) . . ? Cl3 C41 Cl2 108.0(3) . . ? Cl1 C41 H41A 109.7 . . ? Cl3 C41 H41A 109.7 . . ? Cl2 C41 H41A 109.7 . . ? Cl6 C51 Cl5 110.4(4) . . ? Cl6 C51 Cl4 111.0(3) . . ? Cl5 C51 Cl4 109.0(4) . . ? Cl6 C51 H51A 108.8 . . ? Cl5 C51 H51A 108.8 . . ? Cl4 C51 H51A 108.8 . . ? 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 C3 Rh1 S1 C1 -97.7(3) . . . . ? C4 Rh1 S1 C1 -77.5(4) . . . . ? C5 Rh1 S1 C1 -171.6(5) . . . . ? C7 Rh1 S1 C1 -136.5(2) . . . . ? C6 Rh1 S1 C1 -169.6(2) . . . . ? S2 Rh1 S1 C1 -0.95(18) . . . . ? S1 Rh1 S1 C1 96.06(18) 2 . . . ? C3 Rh1 S1 Rh1 154.71(19) . . . 2 ? C4 Rh1 S1 Rh1 174.9(3) . . . 2 ? C5 Rh1 S1 Rh1 80.8(5) . . . 2 ? C7 Rh1 S1 Rh1 115.86(17) . . . 2 ? C6 Rh1 S1 Rh1 82.76(18) . . . 2 ? S2 Rh1 S1 Rh1 -108.56(6) . . . 2 ? S1 Rh1 S1 Rh1 -11.54(7) 2 . . 2 ? C3 Rh1 S2 C1 110.1(3) . . . . ? C4 Rh1 S2 C1 149.8(3) . . . . ? C5 Rh1 S2 C1 177.3(3) . . . . ? C7 Rh1 S2 C1 89.0(3) . . . . ? C6 Rh1 S2 C1 149.4(5) . . . . ? S1 Rh1 S2 C1 1.01(19) . . . . ? S1 Rh1 S2 C1 -79.71(19) 2 . . . ? Rh1 S2 C1 N1 -179.5(5) . . . . ? Rh1 S2 C1 S1 -1.4(3) . . . . ? Rh1 S1 C1 N1 179.4(5) . . . . ? Rh1 S1 C1 N1 -84.9(5) 2 . . . ? Rh1 S1 C1 S2 1.3(3) . . . . ? Rh1 S1 C1 S2 97.1(3) 2 . . . ? S2 C1 N1 C2 -179.2(4) . . . . ? S1 C1 N1 C2 3.0(8) . . . . ? C1 N1 C2 N2 -179(100) . . . . ? C4 Rh1 C3 C7 116.7(5) . . . . ? C5 Rh1 C3 C7 79.5(4) . . . . ? C6 Rh1 C3 C7 36.2(3) . . . . ? S2 Rh1 C3 C7 -156.8(3) . . . . ? S1 Rh1 C3 C7 -80.1(3) . . . . ? S1 Rh1 C3 C7 54.2(8) 2 . . . ? C5 Rh1 C3 C4 -37.1(3) . . . . ? C7 Rh1 C3 C4 -116.7(5) . . . . ? C6 Rh1 C3 C4 -80.5(3) . . . . ? S2 Rh1 C3 C4 86.6(3) . . . . ? S1 Rh1 C3 C4 163.3(3) . . . . ? S1 Rh1 C3 C4 -62.5(7) 2 . . . ? C4 Rh1 C3 C8 -121.8(8) . . . . ? C5 Rh1 C3 C8 -158.9(7) . . . . ? C7 Rh1 C3 C8 121.6(8) . . . . ? C6 Rh1 C3 C8 157.8(7) . . . . ? S2 Rh1 C3 C8 -35.2(7) . . . . ? S1 Rh1 C3 C8 41.5(7) . . . . ? S1 Rh1 C3 C8 175.8(4) 2 . . . ? C7 C3 C4 C5 -2.2(6) . . . . ? C8 C3 C4 C5 -177.5(5) . . . . ? Rh1 C3 C4 C5 61.2(4) . . . . ? C7 C3 C4 C9 178.2(5) . . . . ? C8 C3 C4 C9 3.0(9) . . . . ? Rh1 C3 C4 C9 -118.3(6) . . . . ? C7 C3 C4 Rh1 -63.5(4) . . . . ? C8 C3 C4 Rh1 121.3(6) . . . . ? C3 Rh1 C4 C5 -117.5(5) . . . . ? C7 Rh1 C4 C5 -79.3(4) . . . . ? C6 Rh1 C4 C5 -37.9(3) . . . . ? S2 Rh1 C4 C5 142.2(3) . . . . ? S1 Rh1 C4 C5 -147.9(3) . . . . ? S1 Rh1 C4 C5 40.4(4) 2 . . . ? C5 Rh1 C4 C3 117.5(5) . . . . ? C7 Rh1 C4 C3 38.1(3) . . . . ? C6 Rh1 C4 C3 79.6(4) . . . . ? S2 Rh1 C4 C3 -100.3(3) . . . . ? S1 Rh1 C4 C3 -30.4(5) . . . . ? S1 Rh1 C4 C3 157.9(3) 2 . . . ? C3 Rh1 C4 C9 121.1(7) . . . . ? C5 Rh1 C4 C9 -121.4(7) . . . . ? C7 Rh1 C4 C9 159.3(6) . . . . ? C6 Rh1 C4 C9 -159.3(6) . . . . ? S2 Rh1 C4 C9 20.8(5) . . . . ? S1 Rh1 C4 C9 90.7(6) . . . . ? S1 Rh1 C4 C9 -81.0(6) 2 . . . ? C3 C4 C5 C6 2.0(6) . . . . ? C9 C4 C5 C6 -178.4(5) . . . . ? Rh1 C4 C5 C6 61.8(4) . . . . ? C3 C4 C5 C10 178.4(5) . . . . ? C9 C4 C5 C10 -2.0(9) . . . . ? Rh1 C4 C5 C10 -121.8(5) . . . . ? C3 C4 C5 Rh1 -59.8(4) . . . . ? C9 C4 C5 Rh1 119.8(5) . . . . ? C3 Rh1 C5 C4 38.6(4) . . . . ? C7 Rh1 C5 C4 81.8(4) . . . . ? C6 Rh1 C5 C4 118.0(5) . . . . ? S2 Rh1 C5 C4 -48.3(4) . . . . ? S1 Rh1 C5 C4 120.7(5) . . . . ? S1 Rh1 C5 C4 -149.6(3) 2 . . . ? C3 Rh1 C5 C6 -79.4(4) . . . . ? C4 Rh1 C5 C6 -118.0(5) . . . . ? C7 Rh1 C5 C6 -36.2(3) . . . . ? S2 Rh1 C5 C6 -166.3(3) . . . . ? S1 Rh1 C5 C6 2.7(7) . . . . ? S1 Rh1 C5 C6 92.4(3) 2 . . . ? C3 Rh1 C5 C10 161.2(6) . . . . ? C4 Rh1 C5 C10 122.6(7) . . . . ? C7 Rh1 C5 C10 -155.6(6) . . . . ? C6 Rh1 C5 C10 -119.4(6) . . . . ? S2 Rh1 C5 C10 74.3(5) . . . . ? S1 Rh1 C5 C10 -116.7(5) . . . . ? S1 Rh1 C5 C10 -27.0(5) 2 . . . ? C4 C5 C6 C7 -1.1(6) . . . . ? C10 C5 C6 C7 -177.6(5) . . . . ? Rh1 C5 C6 C7 60.6(4) . . . . ? C4 C5 C6 C11 173.9(5) . . . . ? C10 C5 C6 C11 -2.6(9) . . . . ? Rh1 C5 C6 C11 -124.4(5) . . . . ? C4 C5 C6 Rh1 -61.7(4) . . . . ? C10 C5 C6 Rh1 121.8(5) . . . . ? C3 Rh1 C6 C7 -37.6(4) . . . . ? C4 Rh1 C6 C7 -81.6(4) . . . . ? C5 Rh1 C6 C7 -118.6(5) . . . . ? S2 Rh1 C6 C7 -81.3(6) . . . . ? S1 Rh1 C6 C7 62.4(4) . . . . ? S1 Rh1 C6 C7 148.3(3) 2 . . . ? C3 Rh1 C6 C5 81.0(4) . . . . ? C4 Rh1 C6 C5 37.0(3) . . . . ? C7 Rh1 C6 C5 118.6(5) . . . . ? S2 Rh1 C6 C5 37.3(7) . . . . ? S1 Rh1 C6 C5 -179.0(3) . . . . ? S1 Rh1 C6 C5 -93.1(3) 2 . . . ? C3 Rh1 C6 C11 -160.2(6) . . . . ? C4 Rh1 C6 C11 155.8(6) . . . . ? C5 Rh1 C6 C11 118.8(7) . . . . ? C7 Rh1 C6 C11 -122.6(7) . . . . ? S2 Rh1 C6 C11 156.1(4) . . . . ? S1 Rh1 C6 C11 -60.2(6) . . . . ? S1 Rh1 C6 C11 25.7(6) 2 . . . ? C5 C6 C7 C3 -0.3(6) . . . . ? C11 C6 C7 C3 -175.2(5) . . . . ? Rh1 C6 C7 C3 59.8(4) . . . . ? C5 C6 C7 C12 177.8(5) . . . . ? C11 C6 C7 C12 2.9(10) . . . . ? Rh1 C6 C7 C12 -122.1(6) . . . . ? C5 C6 C7 Rh1 -60.1(4) . . . . ? C11 C6 C7 Rh1 125.0(6) . . . . ? C4 C3 C7 C6 1.5(6) . . . . ? C8 C3 C7 C6 176.8(5) . . . . ? Rh1 C3 C7 C6 -61.7(4) . . . . ? C4 C3 C7 C12 -176.6(5) . . . . ? C8 C3 C7 C12 -1.3(9) . . . . ? Rh1 C3 C7 C12 120.2(6) . . . . ? C4 C3 C7 Rh1 63.2(4) . . . . ? C8 C3 C7 Rh1 -121.5(6) . . . . ? C3 Rh1 C7 C6 118.8(5) . . . . ? C4 Rh1 C7 C6 80.0(4) . . . . ? C5 Rh1 C7 C6 37.8(3) . . . . ? S2 Rh1 C7 C6 152.8(3) . . . . ? S1 Rh1 C7 C6 -130.1(3) . . . . ? S1 Rh1 C7 C6 -41.4(4) 2 . . . ? C4 Rh1 C7 C3 -38.8(3) . . . . ? C5 Rh1 C7 C3 -81.0(4) . . . . ? C6 Rh1 C7 C3 -118.8(5) . . . . ? S2 Rh1 C7 C3 34.1(5) . . . . ? S1 Rh1 C7 C3 111.1(3) . . . . ? S1 Rh1 C7 C3 -160.2(3) 2 . . . ? C3 Rh1 C7 C12 -117.9(7) . . . . ? C4 Rh1 C7 C12 -156.7(6) . . . . ? C5 Rh1 C7 C12 161.1(6) . . . . ? C6 Rh1 C7 C12 123.4(7) . . . . ? S2 Rh1 C7 C12 -83.8(6) . . . . ? S1 Rh1 C7 C12 -6.8(6) . . . . ? S1 Rh1 C7 C12 81.9(6) 2 . . . ? C25 Rh21 S21 C21 101.7(2) . . . . ? C26 Rh21 S21 C21 140.5(2) . . . . ? C24 Rh21 S21 C21 81.1(3) . . . . ? C27 Rh21 S21 C21 172.5(2) . . . . ? C23 Rh21 S21 C21 165.4(5) . . . . ? S22 Rh21 S21 C21 2.45(17) . . . . ? S21 Rh21 S21 C21 -95.10(17) 2_655 . . . ? C25 Rh21 S21 Rh21 -149.42(16) . . . 2_655 ? C26 Rh21 S21 Rh21 -110.65(15) . . . 2_655 ? C24 Rh21 S21 Rh21 -170.0(2) . . . 2_655 ? C27 Rh21 S21 Rh21 -78.66(18) . . . 2_655 ? C23 Rh21 S21 Rh21 -85.8(5) . . . 2_655 ? S22 Rh21 S21 Rh21 111.29(6) . . . 2_655 ? S21 Rh21 S21 Rh21 13.74(7) 2_655 . . 2_655 ? C25 Rh21 S22 C21 -108.2(2) . . . . ? C26 Rh21 S22 C21 -89.4(3) . . . . ? C24 Rh21 S22 C21 -147.5(2) . . . . ? C27 Rh21 S22 C21 -157.8(5) . . . . ? C23 Rh21 S22 C21 -176.5(2) . . . . ? S21 Rh21 S22 C21 -2.55(18) . . . . ? S21 Rh21 S22 C21 77.35(18) 2_655 . . . ? Rh21 S22 C21 N21 -175.8(5) . . . . ? Rh21 S22 C21 S21 3.5(2) . . . . ? Rh21 S21 C21 N21 175.8(5) . . . . ? Rh21 S21 C21 N21 79.7(5) 2_655 . . . ? Rh21 S21 C21 S22 -3.4(2) . . . . ? Rh21 S21 C21 S22 -99.5(2) 2_655 . . . ? S22 C21 N21 C22 174.4(4) . . . . ? S21 C21 N21 C22 -4.8(8) . . . . ? C21 N21 C22 N22 -166(5) . . . . ? C25 Rh21 C23 C24 -37.8(3) . . . . ? C26 Rh21 C23 C24 -80.5(4) . . . . ? C27 Rh21 C23 C24 -117.4(5) . . . . ? S22 Rh21 C23 C24 52.4(4) . . . . ? S21 Rh21 C23 C24 -107.9(5) . . . . ? S21 Rh21 C23 C24 155.4(3) 2_655 . . . ? C25 Rh21 C23 C27 79.6(3) . . . . ? C26 Rh21 C23 C27 36.9(3) . . . . ? C24 Rh21 C23 C27 117.4(5) . . . . ? S22 Rh21 C23 C27 169.9(3) . . . . ? S21 Rh21 C23 C27 9.5(7) . . . . ? S21 Rh21 C23 C27 -87.1(3) 2_655 . . . ? C25 Rh21 C23 C28 -160.5(6) . . . . ? C26 Rh21 C23 C28 156.8(6) . . . . ? C24 Rh21 C23 C28 -122.7(7) . . . . ? C27 Rh21 C23 C28 119.9(7) . . . . ? S22 Rh21 C23 C28 -70.3(6) . . . . ? S21 Rh21 C23 C28 129.4(6) . . . . ? S21 Rh21 C23 C28 32.7(6) 2_655 . . . ? C27 C23 C24 C25 -2.6(6) . . . . ? C28 C23 C24 C25 -178.0(5) . . . . ? Rh21 C23 C24 C25 58.9(4) . . . . ? C27 C23 C24 C29 176.2(5) . . . . ? C28 C23 C24 C29 0.7(9) . . . . ? Rh21 C23 C24 C29 -122.3(5) . . . . ? C27 C23 C24 Rh21 -61.5(4) . . . . ? C28 C23 C24 Rh21 123.0(6) . . . . ? C25 Rh21 C24 C23 118.9(5) . . . . ? C26 Rh21 C24 C23 80.5(4) . . . . ? C27 Rh21 C24 C23 38.1(3) . . . . ? S22 Rh21 C24 C23 -138.0(3) . . . . ? S21 Rh21 C24 C23 150.8(3) . . . . ? S21 Rh21 C24 C23 -34.4(4) 2_655 . . . ? C26 Rh21 C24 C25 -38.4(3) . . . . ? C27 Rh21 C24 C25 -80.8(3) . . . . ? C23 Rh21 C24 C25 -118.9(5) . . . . ? S22 Rh21 C24 C25 103.1(3) . . . . ? S21 Rh21 C24 C25 31.9(4) . . . . ? S21 Rh21 C24 C25 -153.3(3) 2_655 . . . ? C25 Rh21 C24 C29 -120.8(7) . . . . ? C26 Rh21 C24 C29 -159.2(6) . . . . ? C27 Rh21 C24 C29 158.4(6) . . . . ? C23 Rh21 C24 C29 120.3(7) . . . . ? S22 Rh21 C24 C29 -17.7(6) . . . . ? S21 Rh21 C24 C29 -88.9(6) . . . . ? S21 Rh21 C24 C29 85.9(6) 2_655 . . . ? C23 C24 C25 C26 3.5(6) . . . . ? C29 C24 C25 C26 -175.2(5) . . . . ? Rh21 C24 C25 C26 64.5(4) . . . . ? C23 C24 C25 C30 176.4(5) . . . . ? C29 C24 C25 C30 -2.3(9) . . . . ? Rh21 C24 C25 C30 -122.6(5) . . . . ? C23 C24 C25 Rh21 -61.0(4) . . . . ? C29 C24 C25 Rh21 120.3(6) . . . . ? C24 Rh21 C25 C26 -115.7(5) . . . . ? C27 Rh21 C25 C26 -36.8(3) . . . . ? C23 Rh21 C25 C26 -79.6(3) . . . . ? S22 Rh21 C25 C26 160.0(3) . . . . ? S21 Rh21 C25 C26 83.2(3) . . . . ? S21 Rh21 C25 C26 -36.8(7) 2_655 . . . ? C26 Rh21 C25 C24 115.7(5) . . . . ? C27 Rh21 C25 C24 79.0(3) . . . . ? C23 Rh21 C25 C24 36.1(3) . . . . ? S22 Rh21 C25 C24 -84.2(3) . . . . ? S21 Rh21 C25 C24 -161.1(3) . . . . ? S21 Rh21 C25 C24 78.9(6) 2_655 . . . ? C26 Rh21 C25 C30 -123.1(7) . . . . ? C24 Rh21 C25 C30 121.1(6) . . . . ? C27 Rh21 C25 C30 -159.9(6) . . . . ? C23 Rh21 C25 C30 157.3(6) . . . . ? S22 Rh21 C25 C30 36.9(5) . . . . ? S21 Rh21 C25 C30 -40.0(5) . . . . ? S21 Rh21 C25 C30 -159.9(4) 2_655 . . . ? C24 C25 C26 C27 -3.1(6) . . . . ? C30 C25 C26 C27 -175.8(5) . . . . ? Rh21 C25 C26 C27 61.3(4) . . . . ? C24 C25 C26 C31 175.0(5) . . . . ? C30 C25 C26 C31 2.3(8) . . . . ? Rh21 C25 C26 C31 -120.6(5) . . . . ? C24 C25 C26 Rh21 -64.3(4) . . . . ? C30 C25 C26 Rh21 122.9(6) . . . . ? C24 Rh21 C26 C25 39.3(3) . . . . ? C27 Rh21 C26 C25 118.6(5) . . . . ? C23 Rh21 C26 C25 81.1(3) . . . . ? S22 Rh21 C26 C25 -30.2(4) . . . . ? S21 Rh21 C26 C25 -106.9(3) . . . . ? S21 Rh21 C26 C25 166.0(3) 2_655 . . . ? C25 Rh21 C26 C27 -118.6(5) . . . . ? C24 Rh21 C26 C27 -79.3(3) . . . . ? C23 Rh21 C26 C27 -37.5(3) . . . . ? S22 Rh21 C26 C27 -148.9(3) . . . . ? S21 Rh21 C26 C27 134.5(3) . . . . ? S21 Rh21 C26 C27 47.4(3) 2_655 . . . ? C25 Rh21 C26 C31 117.5(7) . . . . ? C24 Rh21 C26 C31 156.8(6) . . . . ? C27 Rh21 C26 C31 -123.9(6) . . . . ? C23 Rh21 C26 C31 -161.3(6) . . . . ? S22 Rh21 C26 C31 87.3(5) . . . . ? S21 Rh21 C26 C31 10.6(5) . . . . ? S21 Rh21 C26 C31 -76.5(5) 2_655 . . . ? C25 C26 C27 C23 1.5(6) . . . . ? C31 C26 C27 C23 -176.5(5) . . . . ? Rh21 C26 C27 C23 61.1(4) . . . . ? C25 C26 C27 C32 174.9(5) . . . . ? C31 C26 C27 C32 -3.1(9) . . . . ? Rh21 C26 C27 C32 -125.5(5) . . . . ? C25 C26 C27 Rh21 -59.6(3) . . . . ? C31 C26 C27 Rh21 122.4(6) . . . . ? C24 C23 C27 C26 0.7(6) . . . . ? C28 C23 C27 C26 176.3(5) . . . . ? Rh21 C23 C27 C26 -60.9(4) . . . . ? C24 C23 C27 C32 -172.9(5) . . . . ? C28 C23 C27 C32 2.7(9) . . . . ? Rh21 C23 C27 C32 125.5(5) . . . . ? C24 C23 C27 Rh21 61.6(4) . . . . ? C28 C23 C27 Rh21 -122.8(5) . . . . ? C25 Rh21 C27 C26 37.3(3) . . . . ? C24 Rh21 C27 C26 81.2(3) . . . . ? C23 Rh21 C27 C26 118.3(4) . . . . ? S22 Rh21 C27 C26 92.7(5) . . . . ? S21 Rh21 C27 C26 -58.2(3) . . . . ? S21 Rh21 C27 C26 -142.7(3) 2_655 . . . ? C25 Rh21 C27 C23 -81.1(3) . . . . ? C26 Rh21 C27 C23 -118.3(4) . . . . ? C24 Rh21 C27 C23 -37.1(3) . . . . ? S22 Rh21 C27 C23 -25.7(6) . . . . ? S21 Rh21 C27 C23 -176.6(3) . . . . ? S21 Rh21 C27 C23 98.9(3) 2_655 . . . ? C25 Rh21 C27 C32 159.9(6) . . . . ? C26 Rh21 C27 C32 122.7(7) . . . . ? C24 Rh21 C27 C32 -156.1(6) . . . . ? C23 Rh21 C27 C32 -119.0(7) . . . . ? S22 Rh21 C27 C32 -144.7(5) . . . . ? S21 Rh21 C27 C32 64.4(6) . . . . ? S21 Rh21 C27 C32 -20.1(6) 2_655 . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 23.35 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.556 _refine_diff_density_min -1.415 _refine_diff_density_rms 0.138