Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Nogueira, Helena' 'Drew, Michael G. B.' 'Felix, Vitor' 'Quintal, Susanna M. O.' _publ_contact_author_name 'Dr Helena Nogueira' _publ_contact_author_address ; Department of Chemistry University of Aveiro Campus de Santiago Aveiro 3810-193 PORTUGAL ; _publ_contact_author_email 'HELENA@DQ.UA.PT' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Coordination modes of 2-mercaptonicotinic acid: synthesis and crystal structures of palladium(II), platinum(II), rhenium(III) and molybdenum(VI) complexes ; data_compound_1 _database_code_CSD 188470 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C30.50 H25 N2 O4.50 P Pd S2' _chemical_formula_weight 693.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.177(14) _cell_length_b 17.733(27) _cell_length_c 11.431(16) _cell_angle_alpha 90.00 _cell_angle_beta 115.72(1) _cell_angle_gamma 90.00 _cell_volume 1859(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'orange' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 702 _exptl_absorpt_coefficient_mu 0.687 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'MAR research image plate system' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3962 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.94 _reflns_number_total 3962 _reflns_number_gt 3163 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Platon (Spek, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1565P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.013(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(4) _refine_ls_number_reflns 3962 _refine_ls_number_parameters 383 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0923 _refine_ls_R_factor_gt 0.0679 _refine_ls_wR_factor_ref 0.2045 _refine_ls_wR_factor_gt 0.1850 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.542 _refine_ls_shift/su_mean 0.010 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.09549(7) 0.00520(5) 0.17073(6) 0.0416(3) Uani 1 d . . . S1 S -0.0280(3) 0.08895(19) 0.2444(3) 0.0506(7) Uani 1 d . . . N11 N 0.2403(10) 0.0473(6) 0.3560(9) 0.050(2) Uani 1 d . . . C16 C 0.3774(14) 0.0461(10) 0.4420(14) 0.065(4) Uani 1 d . . . H162 H 0.4429 0.0149 0.4285 0.078 Uiso 1 calc R . . C15 C 0.4265(17) 0.0908(13) 0.5528(13) 0.079(5) Uani 1 d . . . H15 H 0.5216 0.0851 0.6164 0.095 Uiso 1 calc R . . C14 C 0.3385(16) 0.1422(11) 0.5695(12) 0.072(4) Uani 1 d . . . H14 H 0.3770 0.1763 0.6380 0.086 Uiso 1 calc R . . C13 C 0.1936(15) 0.1447(8) 0.4872(12) 0.055(3) Uani 1 d . . . C12 C 0.1457(13) 0.0983(7) 0.3751(11) 0.049(3) Uani 1 d . . . C17 C 0.0890(17) 0.1960(9) 0.5121(13) 0.063(4) Uani 1 d . . . O18 O -0.0413(15) 0.1941(8) 0.4397(11) 0.088(3) Uani 1 d . . . O19 O 0.1420(14) 0.2371(8) 0.6068(12) 0.096(4) Uani 1 d . . . H19 H 0.0776 0.2629 0.6114 0.115 Uiso 1 calc R . . S2 S 0.2487(3) -0.08240(17) 0.1386(3) 0.0506(7) Uani 1 d . . . N21 N 0.3656(12) 0.0518(7) 0.1490(12) 0.054(3) Uani 1 d . . . C26 C 0.4749(16) 0.1044(8) 0.1807(13) 0.059(3) Uani 1 d . . . H26 H 0.4524 0.1554 0.1661 0.071 Uiso 1 calc R . . C25 C 0.6220(16) 0.0803(8) 0.2360(14) 0.058(3) Uani 1 d . . . H25 H 0.6964 0.1158 0.2594 0.070 Uiso 1 calc R . . C24 C 0.6556(10) 0.0062(10) 0.2550(9) 0.049(2) Uani 1 d . . . H24 H 0.7528 -0.0086 0.2886 0.059 Uiso 1 calc R . . C23 C 0.5462(12) -0.0492(7) 0.2251(10) 0.043(2) Uani 1 d . . . C22 C 0.3991(13) -0.0231(7) 0.1713(11) 0.042(3) Uani 1 d . . . C27 C 0.5859(15) -0.1256(10) 0.2479(15) 0.068(4) Uani 1 d . . . O28 O 0.7233(14) -0.1354(8) 0.3353(16) 0.112(5) Uani 1 d . . . H28 H 0.7656 -0.1627 0.3048 0.134 Uiso 1 calc R . . O29 O 0.5107(17) -0.1806(8) 0.190(2) 0.161(9) Uani 1 d . . . P1 P -0.0879(3) -0.02825(17) -0.0172(3) 0.0404(6) Uani 1 d . . . C31 C -0.0678(12) -0.0038(10) -0.1643(9) 0.049(3) Uani 1 d . . . C32 C 0.0561(13) 0.0286(8) -0.1605(11) 0.056(3) Uani 1 d . . . H32 H 0.1362 0.0360 -0.0809 0.067 Uiso 1 calc R . . C33 C 0.0633(16) 0.0504(10) -0.2727(13) 0.069(4) Uani 1 d . . . H33 H 0.1448 0.0756 -0.2696 0.083 Uiso 1 calc R . . C34 C -0.0578(19) 0.0333(12) -0.3957(16) 0.081(5) Uani 1 d . . . H34 H -0.0492 0.0414 -0.4724 0.097 Uiso 1 calc R . . C35 C -0.1829(15) 0.0058(16) -0.4000(10) 0.075(4) Uani 1 d . . . H35 H -0.2652 0.0015 -0.4789 0.091 Uiso 1 calc R . . C36 C -0.1876(13) -0.0161(9) -0.2854(10) 0.062(4) Uani 1 d . . . H36 H -0.2710 -0.0393 -0.2885 0.074 Uiso 1 calc R . . C41 C -0.2622(11) 0.0183(9) -0.0507(9) 0.050(3) Uani 1 d . . . C42 C -0.2652(15) 0.0966(9) -0.0579(11) 0.058(3) Uani 1 d . . . H42 H -0.1802 0.1225 -0.0440 0.069 Uiso 1 calc R . . C43 C -0.3927(17) 0.1371(10) -0.0855(13) 0.069(4) Uani 1 d . . . H43 H -0.3926 0.1895 -0.0889 0.083 Uiso 1 calc R . . C44 C -0.515(2) 0.0998(14) -0.1068(15) 0.093(6) Uani 1 d . . . H44 H -0.6000 0.1269 -0.1258 0.111 Uiso 1 calc R . . C45 C -0.5187(14) 0.017(2) -0.1012(14) 0.105(10) Uani 1 d . . . H45 H -0.6035 -0.0099 -0.1165 0.126 Uiso 1 calc R . . C46 C -0.3876(13) -0.0186(10) -0.0716(12) 0.064(4) Uani 1 d . . . H46 H -0.3845 -0.0710 -0.0655 0.077 Uiso 1 calc R . . C51 C -0.1213(15) -0.1285(8) -0.0262(14) 0.059(3) Uani 1 d . . . C52 C -0.0945(18) -0.1761(10) -0.1086(16) 0.073(4) Uani 1 d . . . H52 H -0.0649 -0.1574 -0.1694 0.088 Uiso 1 calc R . . C53 C -0.114(2) -0.2551(12) -0.097(2) 0.101(7) Uani 1 d . . . H53 H -0.0952 -0.2872 -0.1525 0.122 Uiso 1 calc R . . C54 C -0.156(3) -0.2856(12) -0.015(3) 0.107(7) Uani 1 d . . . H54 H -0.1717 -0.3372 -0.0143 0.129 Uiso 1 calc R . . C55 C -0.174(3) -0.2406(13) 0.065(2) 0.106(7) Uani 1 d . . . H55 H -0.1967 -0.2619 0.1284 0.127 Uiso 1 calc R . . C56 C -0.162(2) -0.1602(11) 0.0644(17) 0.085(5) Uani 1 d . . . H56 H -0.1801 -0.1303 0.1224 0.102 Uiso 1 calc R . . O91 O -0.223(3) 0.2910(13) 0.481(3) 0.096(9) Uani 0.50 d P . . H91 H -0.1677 0.2647 0.4641 0.115 Uiso 0.50 calc PR . . C92 C -0.369(4) 0.270(2) 0.401(4) 0.086(10) Uani 0.50 d P . . H92A H -0.3900 0.2230 0.4311 0.103 Uiso 0.50 calc PR . . H92B H -0.3823 0.2648 0.3135 0.103 Uiso 0.50 calc PR . . H92C H -0.4337 0.3082 0.4057 0.103 Uiso 0.50 calc PR . . 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 Pd 0.0279(4) 0.0478(4) 0.0447(4) -0.0026(4) 0.0116(3) -0.0020(4) S1 0.0337(14) 0.0592(18) 0.0564(15) -0.0125(14) 0.0172(11) -0.0029(13) N11 0.031(4) 0.059(6) 0.049(5) 0.003(5) 0.008(4) -0.002(4) C16 0.038(6) 0.074(10) 0.071(8) -0.003(7) 0.012(6) 0.007(7) C15 0.054(8) 0.110(14) 0.051(8) -0.014(8) 0.001(6) 0.001(9) C14 0.051(8) 0.105(13) 0.041(7) -0.025(7) 0.003(6) -0.021(8) C13 0.059(8) 0.053(7) 0.050(6) -0.009(5) 0.021(6) -0.011(6) C12 0.046(7) 0.046(6) 0.056(6) 0.003(5) 0.025(5) -0.006(5) C17 0.070(10) 0.065(9) 0.055(7) -0.009(6) 0.028(7) -0.015(7) O18 0.084(8) 0.092(9) 0.078(7) -0.032(6) 0.026(6) 0.008(7) O19 0.091(9) 0.096(9) 0.104(8) -0.063(8) 0.046(7) -0.036(8) S2 0.0333(13) 0.0453(15) 0.0712(18) -0.0001(14) 0.0208(12) 0.0002(12) N21 0.031(5) 0.057(7) 0.070(7) -0.001(5) 0.017(5) -0.002(5) C26 0.068(9) 0.044(7) 0.071(8) -0.001(6) 0.034(7) 0.002(6) C25 0.053(8) 0.039(7) 0.086(9) 0.003(6) 0.032(7) -0.002(5) C24 0.028(4) 0.060(6) 0.061(6) 0.007(8) 0.021(4) 0.007(7) C23 0.036(6) 0.047(6) 0.041(6) -0.007(5) 0.012(4) -0.003(5) C22 0.035(6) 0.048(6) 0.043(5) 0.004(5) 0.016(5) 0.011(5) C27 0.030(6) 0.078(11) 0.085(10) -0.004(8) 0.015(6) 0.009(7) O28 0.065(8) 0.073(8) 0.152(12) -0.001(8) 0.005(7) 0.009(6) O29 0.058(9) 0.050(7) 0.29(2) 0.004(11) -0.007(10) 0.009(6) P1 0.0279(12) 0.0424(14) 0.0470(14) -0.0035(11) 0.0128(11) -0.0019(11) C31 0.049(6) 0.054(8) 0.045(5) 0.001(6) 0.023(4) -0.001(6) C32 0.045(6) 0.066(9) 0.049(6) 0.000(5) 0.012(5) -0.001(5) C33 0.053(8) 0.089(11) 0.062(8) 0.011(8) 0.023(6) -0.009(8) C34 0.066(9) 0.105(14) 0.070(8) 0.004(8) 0.029(7) -0.012(9) C35 0.062(7) 0.112(11) 0.040(6) 0.003(10) 0.010(5) -0.001(12) C36 0.033(5) 0.106(14) 0.040(5) 0.000(6) 0.009(4) -0.018(6) C41 0.028(5) 0.078(11) 0.041(5) -0.010(6) 0.013(4) 0.009(5) C42 0.051(7) 0.069(9) 0.047(6) 0.002(6) 0.016(5) 0.015(7) C43 0.056(9) 0.078(10) 0.057(7) -0.002(7) 0.010(6) 0.013(8) C44 0.078(12) 0.125(18) 0.058(8) 0.003(10) 0.013(7) 0.049(13) C45 0.031(6) 0.20(3) 0.071(8) -0.042(15) 0.008(5) 0.005(13) C46 0.043(7) 0.082(11) 0.063(7) -0.005(6) 0.018(5) 0.001(6) C51 0.051(7) 0.048(7) 0.072(8) -0.011(6) 0.021(6) -0.017(6) C52 0.065(9) 0.069(10) 0.082(9) -0.016(8) 0.027(7) 0.005(8) C53 0.086(14) 0.058(10) 0.134(17) -0.022(12) 0.023(12) 0.021(9) C54 0.092(15) 0.052(11) 0.136(18) -0.003(12) 0.010(12) -0.017(10) C55 0.104(16) 0.073(13) 0.115(15) 0.014(11) 0.024(12) -0.047(11) C56 0.092(13) 0.072(11) 0.084(10) -0.006(9) 0.032(9) -0.031(10) O91 0.088(18) 0.046(12) 0.112(18) -0.020(12) 0.004(14) 0.031(12) C92 0.058(18) 0.07(2) 0.10(2) -0.020(18) 0.013(16) 0.018(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd N11 2.123(10) . ? Pd P1 2.229(3) . ? Pd S1 2.326(4) . ? Pd S2 2.340(4) . ? S1 C12 1.758(13) . ? N11 C16 1.312(17) . ? N11 C12 1.406(16) . ? C16 C15 1.39(2) . ? C16 H162 0.9300 . ? C15 C14 1.35(3) . ? C15 H15 0.9300 . ? C14 C13 1.36(2) . ? C14 H14 0.9300 . ? C13 C12 1.419(17) . ? C13 C17 1.52(2) . ? C17 O19 1.219(17) . ? C17 O18 1.222(19) . ? O19 H19 0.8200 . ? S2 C22 1.759(13) . ? N21 C22 1.366(17) . ? N21 C26 1.374(18) . ? C26 C25 1.42(2) . ? C26 H26 0.9300 . ? C25 C24 1.35(2) . ? C25 H25 0.9300 . ? C24 C23 1.412(19) . ? C24 H24 0.9300 . ? C23 C27 1.41(2) . ? C23 C22 1.426(17) . ? C27 O29 1.24(2) . ? C27 O28 1.33(2) . ? O28 H28 0.8200 . ? P1 C51 1.804(14) . ? P1 C31 1.832(10) . ? P1 C41 1.840(11) . ? C31 C32 1.369(18) . ? C31 C36 1.409(16) . ? C32 C33 1.372(17) . ? C32 H32 0.9300 . ? C33 C34 1.44(2) . ? C33 H33 0.9300 . ? C34 C35 1.34(2) . ? C34 H34 0.9300 . ? C35 C36 1.387(17) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C41 C46 1.360(18) . ? C41 C42 1.39(2) . ? C42 C43 1.39(2) . ? C42 H42 0.9300 . ? C43 C44 1.33(3) . ? C43 H43 0.9300 . ? C44 C45 1.48(4) . ? C44 H44 0.9300 . ? C45 C46 1.38(2) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C51 C52 1.38(2) . ? C51 C56 1.39(2) . ? C52 C53 1.43(3) . ? C52 H52 0.9300 . ? C53 C54 1.31(3) . ? C53 H53 0.9300 . ? C54 C55 1.29(3) . ? C54 H54 0.9300 . ? C55 C56 1.43(3) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? O91 C92 1.41(4) . ? O91 H91 0.8200 . ? C92 H92A 0.9608 . ? C92 H92B 0.9608 . ? C92 H92C 0.9608 . ? 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 N11 Pd P1 169.5(3) . . ? N11 Pd S1 70.4(3) . . ? P1 Pd S1 99.25(14) . . ? N11 Pd S2 99.7(3) . . ? P1 Pd S2 90.48(14) . . ? S1 Pd S2 169.09(11) . . ? C12 S1 Pd 82.3(4) . . ? C16 N11 C12 118.1(11) . . ? C16 N11 Pd 142.5(10) . . ? C12 N11 Pd 99.0(7) . . ? N11 C16 C15 121.2(14) . . ? N11 C16 H162 119.4 . . ? C15 C16 H162 119.4 . . ? C14 C15 C16 121.1(13) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.4 . . ? C15 C14 C13 120.7(13) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C13 C12 116.7(12) . . ? C14 C13 C17 121.8(12) . . ? C12 C13 C17 121.5(12) . . ? N11 C12 C13 121.5(11) . . ? N11 C12 S1 108.1(8) . . ? C13 C12 S1 130.3(10) . . ? O19 C17 O18 123.4(16) . . ? O19 C17 C13 116.6(14) . . ? O18 C17 C13 120.0(12) . . ? C17 O19 H19 109.4 . . ? C22 S2 Pd 98.5(4) . . ? C22 N21 C26 120.1(12) . . ? N21 C26 C25 119.4(13) . . ? N21 C26 H26 120.3 . . ? C25 C26 H26 120.3 . . ? C24 C25 C26 120.7(12) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C24 C23 121.3(12) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C27 C23 C24 119.5(12) . . ? C27 C23 C22 123.8(11) . . ? C24 C23 C22 116.6(12) . . ? N21 C22 C23 121.8(11) . . ? N21 C22 S2 114.7(9) . . ? C23 C22 S2 123.4(10) . . ? O29 C27 O28 120.2(15) . . ? O29 C27 C23 126.7(13) . . ? O28 C27 C23 112.9(14) . . ? C27 O28 H28 109.5 . . ? C51 P1 C31 105.9(7) . . ? C51 P1 C41 106.8(7) . . ? C31 P1 C41 100.6(5) . . ? C51 P1 Pd 112.1(5) . . ? C31 P1 Pd 116.2(4) . . ? C41 P1 Pd 114.2(4) . . ? C32 C31 C36 119.3(10) . . ? C32 C31 P1 122.6(8) . . ? C36 C31 P1 118.1(9) . . ? C31 C32 C33 120.7(11) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C32 C33 C34 118.9(13) . . ? C32 C33 H33 120.6 . . ? C34 C33 H33 120.6 . . ? C35 C34 C33 120.5(13) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C36 119.2(12) . . ? C34 C35 H35 120.4 . . ? C36 C35 H35 120.4 . . ? C35 C36 C31 121.0(11) . . ? C35 C36 H36 119.5 . . ? C31 C36 H36 119.5 . . ? C46 C41 C42 118.4(12) . . ? C46 C41 P1 124.5(12) . . ? C42 C41 P1 117.1(10) . . ? C41 C42 C43 121.5(15) . . ? C41 C42 H42 119.2 . . ? C43 C42 H42 119.2 . . ? C44 C43 C42 119.1(18) . . ? C44 C43 H43 120.4 . . ? C42 C43 H43 120.4 . . ? C43 C44 C45 121.8(16) . . ? C43 C44 H44 119.1 . . ? C45 C44 H44 119.1 . . ? C46 C45 C44 115(2) . . ? C46 C45 H45 122.5 . . ? C44 C45 H45 122.5 . . ? C41 C46 C45 124(2) . . ? C41 C46 H46 118.0 . . ? C45 C46 H46 118.0 . . ? C52 C51 C56 118.2(15) . . ? C52 C51 P1 123.7(11) . . ? C56 C51 P1 117.7(12) . . ? C51 C52 C53 117.6(18) . . ? C51 C52 H52 121.2 . . ? C53 C52 H52 121.2 . . ? C54 C53 C52 125(2) . . ? C54 C53 H53 117.5 . . ? C52 C53 H53 117.6 . . ? C55 C54 C53 116.6(19) . . ? C55 C54 H54 121.7 . . ? C53 C54 H54 121.7 . . ? C54 C55 C56 125(2) . . ? C54 C55 H55 117.5 . . ? C56 C55 H55 117.5 . . ? C51 C56 C55 117.5(19) . . ? C51 C56 H56 121.2 . . ? C55 C56 H56 121.2 . . ? C92 O91 H91 109.4 . . ? O91 C92 H92A 109.5 . . ? O91 C92 H92B 109.7 . . ? H92A C92 H92B 109.4 . . ? O91 C92 H92C 109.5 . . ? H92A C92 H92C 109.4 . . ? H92B C92 H92C 109.4 . . ? _diffrn_measured_fraction_theta_max 0.843 _diffrn_reflns_theta_full 25.94 _diffrn_measured_fraction_theta_full 0.843 _refine_diff_density_max 1.238 _refine_diff_density_min -0.922 _refine_diff_density_rms 0.133 #==END data_compound_3 _database_code_CSD 188471 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H40 N3 O5 P Pt S2' _chemical_formula_weight 884.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 '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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.390(15) _cell_length_b 17.781(20) _cell_length_c 11.553(15) _cell_angle_alpha 90.00 _cell_angle_beta 115.540(10) _cell_angle_gamma 90.00 _cell_volume 1926(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'yellow' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.526 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 884 _exptl_absorpt_coefficient_mu 3.836 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'MAR research image plate system' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6141 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.94 _reflns_number_total 6141 _reflns_number_gt 5499 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Platon (Spek, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0836P)^2^+4.8904P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(3) _refine_ls_number_reflns 6141 _refine_ls_number_parameters 428 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1241 _refine_ls_wR_factor_gt 0.1176 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt Pt 0.42743(3) 0.46033(5) 0.32696(2) 0.03471(11) Uani 1 d . . . N11 N 0.3943(9) 0.4159(6) 0.1460(7) 0.0427(19) Uani 1 d . . . C12 C 0.2802(10) 0.3679(6) 0.1232(10) 0.042(2) Uani 1 d . . . C13 C 0.2227(13) 0.3244(6) 0.0091(10) 0.047(3) Uani 1 d . . . C14 C 0.2828(9) 0.3318(5) -0.0750(6) 0.057(3) Uani 1 d . . . H14 H 0.2472 0.3037 -0.1502 0.069 Uiso 1 calc R . . C15 C 0.3961(9) 0.3808(5) -0.0501(6) 0.071(4) Uani 1 d R . . H15 H 0.4354 0.3852 -0.1085 0.085 Uiso 1 calc R . . C16 C 0.4507(9) 0.4230(5) 0.0621(6) 0.056(3) Uani 1 d R . . H16 H 0.5261 0.4560 0.0788 0.067 Uiso 1 calc R . . C17 C 0.0992(16) 0.2722(8) -0.0237(14) 0.066(4) Uani 1 d . . . O18 O 0.0446(12) 0.2447(6) -0.1316(11) 0.081(3) Uani 1 d . . . O19 O 0.0461(17) 0.2714(10) 0.0573(14) 0.120(6) Uani 1 d . . . H19 H -0.0208 0.2417 0.0335 0.144 Uiso 1 calc R . . S1 S 0.2364(3) 0.37534(16) 0.2523(2) 0.0435(5) Uani 1 d . . . S2 S 0.6049(3) 0.54620(14) 0.3491(3) 0.0443(5) Uani 1 d . . . N21 N 0.7184(16) 0.4153(8) 0.3416(14) 0.057(3) Uani 1 d . . . C22 C 0.7252(12) 0.4918(8) 0.3227(14) 0.039(3) Uani 1 d . . . C23 C 0.8175(13) 0.5178(7) 0.2668(10) 0.042(2) Uani 1 d . . . C24 C 0.9052(9) 0.4625(12) 0.2435(9) 0.049(2) Uani 1 d . . . H24 H 0.9701 0.4788 0.2132 0.059 Uiso 1 calc R . . C25 C 0.8973(15) 0.3890(8) 0.2635(13) 0.058(3) Uani 1 d . . . H25 H 0.9517 0.3539 0.2444 0.070 Uiso 1 calc R . . C26 C 0.8046(13) 0.3682(7) 0.3137(13) 0.054(3) Uani 1 d . . . H26 H 0.8003 0.3173 0.3302 0.064 Uiso 1 calc R . . C27 C 0.8275(13) 0.5983(6) 0.2370(12) 0.050(3) Uani 1 d . . . O28 O 0.9186(16) 0.6110(7) 0.1924(17) 0.111(5) Uani 1 d . . . H28 H 0.9175 0.6558 0.1754 0.133 Uiso 1 calc R . . O29 O 0.762(2) 0.6469(7) 0.257(3) 0.159(9) Uani 1 d . . . P1 P 0.4302(3) 0.49454(15) 0.5125(2) 0.0345(5) Uani 1 d . . . C31 C 0.5923(10) 0.4677(14) 0.6547(8) 0.050(3) Uani 1 d . . . C32 C 0.7098(12) 0.4376(7) 0.6496(11) 0.054(3) Uani 1 d . . . H32 H 0.7118 0.4307 0.5706 0.065 Uiso 1 calc R . . C33 C 0.8254(15) 0.4171(10) 0.7599(14) 0.068(4) Uani 1 d . . . H33 H 0.9037 0.3941 0.7559 0.081 Uiso 1 calc R . . C34 C 0.8244(16) 0.4314(9) 0.8790(13) 0.068(3) Uani 1 d . . . H34 H 0.9033 0.4186 0.9542 0.082 Uiso 1 calc R . . C35 C 0.7118(12) 0.4629(14) 0.8854(12) 0.078(4) Uani 1 d . . . H35 H 0.7124 0.4709 0.9652 0.093 Uiso 1 calc R . . C36 C 0.5947(12) 0.4838(9) 0.7769(10) 0.065(5) Uani 1 d . . . H36 H 0.5183 0.5081 0.7825 0.078 Uiso 1 calc R . . C41 C 0.2942(10) 0.4469(8) 0.5480(9) 0.045(4) Uani 1 d . . . C42 C 0.1940(12) 0.4834(7) 0.5724(12) 0.055(3) Uani 1 d . . . H42 H 0.1939 0.5357 0.5722 0.066 Uiso 1 calc R . . C43 C 0.0901(14) 0.446(2) 0.5980(14) 0.119(13) Uani 1 d . . . H43 H 0.0186 0.4712 0.6097 0.143 Uiso 1 calc R . . C44 C 0.1009(17) 0.3653(10) 0.6051(14) 0.074(4) Uani 1 d . . . H44 H 0.0361 0.3376 0.6236 0.088 Uiso 1 calc R . . C45 C 0.2046(16) 0.3289(9) 0.5850(12) 0.066(4) Uani 1 d . . . H45 H 0.2110 0.2768 0.5908 0.079 Uiso 1 calc R . . C46 C 0.3017(14) 0.3696(7) 0.5557(12) 0.055(3) Uani 1 d . . . H46 H 0.3718 0.3444 0.5412 0.065 Uiso 1 calc R . . C51 C 0.4000(13) 0.5948(6) 0.5188(11) 0.047(2) Uani 1 d . . . C52 C 0.2706(17) 0.6251(9) 0.4268(16) 0.071(4) Uani 1 d . . . H52 H 0.2036 0.5939 0.3659 0.085 Uiso 1 calc R . . C53 C 0.244(3) 0.7003(11) 0.427(2) 0.108(8) Uani 1 d . . . H53 H 0.1572 0.7209 0.3710 0.130 Uiso 1 calc R . . C54 C 0.359(3) 0.7480(9) 0.522(2) 0.094(6) Uani 1 d . . . H54 H 0.3431 0.7994 0.5238 0.113 Uiso 1 calc R . . C55 C 0.483(2) 0.7203(9) 0.6031(19) 0.086(5) Uani 1 d . . . H55 H 0.5548 0.7520 0.6581 0.103 Uiso 1 calc R . . C56 C 0.5069(17) 0.6411(7) 0.6055(14) 0.064(3) Uani 1 d . . . H56 H 0.5925 0.6205 0.6642 0.077 Uiso 1 calc R . . N61 N 0.2642(15) 0.6693(7) 0.0124(12) 0.073(3) Uani 1 d . . . C61 C 0.210(2) 0.6215(11) 0.085(2) 0.093(6) Uani 1 d . . . H61A H 0.1583 0.6528 0.1190 0.111 Uiso 1 calc R . . H61B H 0.2913 0.6003 0.1573 0.111 Uiso 1 calc R . . C62 C 0.116(2) 0.5591(15) 0.011(3) 0.119(8) Uani 1 d . . . H62A H 0.0590 0.5753 -0.0750 0.143 Uiso 1 calc R . . H62B H 0.0554 0.5448 0.0510 0.143 Uiso 1 calc R . . H62C H 0.1734 0.5169 0.0107 0.143 Uiso 1 calc R . . C71 C 0.390(3) 0.6320(14) -0.003(3) 0.115(7) Uani 1 d . . . H71A H 0.4745 0.6336 0.0777 0.138 Uiso 1 calc R . . H71B H 0.3673 0.5797 -0.0274 0.138 Uiso 1 calc R . . C72 C 0.418(4) 0.6720(17) -0.104(3) 0.158(13) Uani 1 d . . . H72A H 0.3917 0.6401 -0.1780 0.189 Uiso 1 calc R . . H72B H 0.5182 0.6837 -0.0708 0.189 Uiso 1 calc R . . H72C H 0.3638 0.7176 -0.1281 0.189 Uiso 1 calc R . . C81 C 0.307(2) 0.7447(11) 0.0747(18) 0.089(5) Uani 1 d . . . H81A H 0.3329 0.7765 0.0201 0.107 Uiso 1 calc R . . H81B H 0.2242 0.7674 0.0797 0.107 Uiso 1 calc R . . C82 C 0.4219(19) 0.7441(8) 0.2005(13) 0.104(6) Uani 1 d . . . H82A H 0.4243 0.6966 0.2407 0.125 Uiso 1 calc R . . H82B H 0.4087 0.7837 0.2508 0.125 Uiso 1 calc R . . H82C H 0.5103 0.7517 0.1944 0.125 Uiso 1 calc R . . OW1 O -0.0320(17) 0.2081(8) 0.2089(11) 0.116(5) Uani 1 d 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 Pt 0.03502(16) 0.03530(17) 0.03446(16) -0.0014(3) 0.01560(11) 0.0001(2) N11 0.049(5) 0.052(5) 0.026(4) -0.008(4) 0.016(3) -0.001(4) C12 0.034(5) 0.047(6) 0.043(5) 0.004(4) 0.016(4) 0.002(4) C13 0.057(7) 0.030(5) 0.038(5) 0.001(4) 0.005(5) 0.004(4) C14 0.068(8) 0.065(8) 0.030(5) -0.021(5) 0.012(5) 0.002(6) C15 0.075(9) 0.093(11) 0.045(6) -0.002(7) 0.027(6) 0.000(8) C16 0.074(8) 0.061(7) 0.044(6) -0.011(5) 0.035(6) -0.017(6) C17 0.070(8) 0.046(7) 0.063(8) -0.001(6) 0.010(7) -0.010(6) O18 0.073(6) 0.060(6) 0.084(7) -0.036(6) 0.008(5) 0.004(5) O19 0.117(11) 0.134(13) 0.092(8) -0.013(9) 0.027(8) -0.072(10) S1 0.0393(12) 0.0464(13) 0.0452(12) -0.0056(11) 0.0186(10) -0.0073(10) S2 0.0452(13) 0.0349(12) 0.0573(14) -0.0037(11) 0.0264(12) -0.0042(10) N21 0.067(8) 0.043(6) 0.070(8) -0.008(6) 0.038(6) 0.005(5) C22 0.016(4) 0.045(6) 0.055(6) 0.006(5) 0.012(4) 0.000(4) C23 0.046(6) 0.040(5) 0.035(5) -0.003(4) 0.011(4) -0.007(5) C24 0.040(4) 0.055(6) 0.059(5) -0.023(10) 0.027(4) -0.010(9) C25 0.057(7) 0.053(8) 0.068(8) -0.001(6) 0.029(6) 0.012(6) C26 0.051(6) 0.040(6) 0.065(7) 0.008(6) 0.019(6) 0.008(5) C27 0.050(6) 0.041(6) 0.060(6) 0.003(5) 0.026(5) -0.001(5) O28 0.126(11) 0.071(7) 0.188(15) 0.059(9) 0.118(11) 0.033(7) O29 0.200(18) 0.047(7) 0.33(3) 0.026(11) 0.21(2) 0.019(8) P1 0.0340(12) 0.0351(11) 0.0342(11) -0.0045(9) 0.0146(10) -0.0015(9) C31 0.039(4) 0.068(10) 0.035(4) -0.019(8) 0.009(3) -0.012(7) C32 0.050(6) 0.064(9) 0.052(6) 0.003(5) 0.026(5) 0.005(5) C33 0.053(7) 0.080(10) 0.065(8) 0.009(7) 0.020(6) 0.012(7) C34 0.069(8) 0.068(8) 0.058(7) -0.005(6) 0.018(6) -0.005(6) C35 0.056(6) 0.098(10) 0.063(7) -0.054(10) 0.010(5) -0.015(11) C36 0.041(5) 0.113(15) 0.036(5) -0.016(6) 0.013(4) -0.004(6) C41 0.033(4) 0.066(12) 0.035(4) 0.000(5) 0.012(3) -0.003(5) C42 0.045(6) 0.056(8) 0.064(7) 0.000(5) 0.024(5) 0.006(4) C43 0.045(7) 0.24(4) 0.075(8) -0.076(17) 0.030(6) -0.063(15) C44 0.075(10) 0.081(11) 0.061(8) -0.006(8) 0.026(7) -0.036(8) C45 0.077(9) 0.060(8) 0.049(6) 0.008(6) 0.017(6) -0.019(7) C46 0.059(7) 0.048(6) 0.060(7) -0.008(6) 0.030(6) -0.015(5) C51 0.066(7) 0.036(5) 0.050(6) -0.002(4) 0.036(5) 0.007(5) C52 0.070(9) 0.063(8) 0.081(9) 0.011(7) 0.034(8) 0.012(7) C53 0.17(2) 0.073(11) 0.128(16) 0.043(12) 0.107(17) 0.063(13) C54 0.157(19) 0.044(8) 0.114(14) 0.005(9) 0.090(15) 0.007(10) C55 0.113(14) 0.047(8) 0.094(11) -0.013(8) 0.041(11) -0.013(9) C56 0.079(9) 0.041(6) 0.066(8) -0.006(6) 0.026(7) -0.008(6) N61 0.090(9) 0.052(6) 0.064(7) 0.010(6) 0.020(6) -0.001(6) C61 0.086(12) 0.072(11) 0.089(12) 0.034(10) 0.008(10) -0.002(9) C62 0.101(15) 0.116(18) 0.139(19) 0.023(16) 0.051(14) -0.024(14) C71 0.16(2) 0.087(14) 0.132(18) -0.007(13) 0.090(17) 0.012(14) C72 0.25(4) 0.11(2) 0.19(3) -0.05(2) 0.16(3) -0.03(2) C81 0.105(14) 0.074(10) 0.087(11) -0.015(9) 0.039(10) -0.016(9) C82 0.101(14) 0.095(14) 0.095(12) -0.028(11) 0.023(11) -0.007(11) OW1 0.152(14) 0.096(10) 0.081(8) 0.007(8) 0.034(9) -0.015(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 Pt N11 2.120(8) . ? Pt P1 2.216(4) . ? Pt S2 2.322(3) . ? Pt S1 2.343(3) . ? N11 C16 1.337(11) . ? N11 C12 1.390(14) . ? C12 C13 1.419(15) . ? C12 S1 1.742(10) . ? C13 C14 1.370(15) . ? C13 C17 1.495(18) . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C17 O18 1.227(18) . ? C17 O19 1.27(2) . ? S2 C22 1.709(13) . ? N21 C26 1.363(18) . ? N21 C22 1.384(16) . ? C22 C23 1.444(18) . ? C23 C24 1.44(2) . ? C23 C27 1.485(16) . ? C24 C25 1.34(2) . ? C25 C26 1.37(2) . ? C27 O29 1.179(18) . ? C27 O28 1.278(16) . ? P1 C51 1.817(11) . ? P1 C31 1.838(12) . ? P1 C41 1.839(11) . ? C31 C32 1.356(18) . ? C31 C36 1.430(14) . ? C32 C33 1.371(18) . ? C33 C34 1.40(2) . ? C34 C35 1.33(2) . ? C35 C36 1.370(19) . ? C41 C42 1.356(16) . ? C41 C46 1.377(19) . ? C42 C43 1.41(2) . ? C43 C44 1.43(4) . ? C44 C45 1.36(2) . ? C45 C46 1.396(18) . ? C51 C56 1.398(18) . ? C51 C52 1.412(19) . ? C52 C53 1.37(2) . ? C53 C54 1.49(3) . ? C54 C55 1.32(3) . ? C55 C56 1.43(2) . ? N61 C61 1.46(2) . ? N61 C81 1.50(2) . ? N61 C71 1.54(3) . ? C61 C62 1.48(3) . ? C71 C72 1.50(3) . ? C81 C82 1.43(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Pt P1 170.1(3) . . ? N11 Pt S2 97.9(3) . . ? P1 Pt S2 91.97(10) . . ? N11 Pt S1 69.2(3) . . ? P1 Pt S1 100.88(10) . . ? S2 Pt S1 166.20(10) . . ? C16 N11 C12 121.6(8) . . ? C16 N11 Pt 138.1(7) . . ? C12 N11 Pt 100.3(6) . . ? N11 C12 C13 119.6(9) . . ? N11 C12 S1 107.9(7) . . ? C13 C12 S1 132.5(9) . . ? C14 C13 C12 117.9(10) . . ? C14 C13 C17 119.0(10) . . ? C12 C13 C17 123.1(12) . . ? C13 C14 C15 121.2(6) . . ? C14 C15 C16 120.0 . . ? N11 C16 C15 119.7(5) . . ? O18 C17 O19 125.8(15) . . ? O18 C17 C13 118.3(15) . . ? O19 C17 C13 114.7(12) . . ? C12 S1 Pt 82.6(4) . . ? C22 S2 Pt 102.4(5) . . ? C26 N21 C22 118.8(14) . . ? N21 C22 C23 118.3(12) . . ? N21 C22 S2 115.9(12) . . ? C23 C22 S2 125.2(11) . . ? C24 C23 C22 117.4(12) . . ? C24 C23 C27 120.0(12) . . ? C22 C23 C27 122.6(12) . . ? C25 C24 C23 122.9(12) . . ? C24 C25 C26 116.3(12) . . ? N21 C26 C25 126.0(13) . . ? O29 C27 O28 122.3(13) . . ? O29 C27 C23 124.0(12) . . ? O28 C27 C23 113.7(11) . . ? C51 P1 C31 109.0(8) . . ? C51 P1 C41 106.3(6) . . ? C31 P1 C41 100.2(6) . . ? C51 P1 Pt 112.2(3) . . ? C31 P1 Pt 114.7(5) . . ? C41 P1 Pt 113.5(4) . . ? C32 C31 C36 119.2(10) . . ? C32 C31 P1 124.0(8) . . ? C36 C31 P1 116.7(11) . . ? C31 C32 C33 120.6(11) . . ? C32 C33 C34 119.3(13) . . ? C35 C34 C33 120.7(14) . . ? C34 C35 C36 121.3(12) . . ? C35 C36 C31 118.7(12) . . ? C42 C41 C46 119.4(11) . . ? C42 C41 P1 124.0(11) . . ? C46 C41 P1 116.5(9) . . ? C41 C42 C43 122.8(18) . . ? C42 C43 C44 116.1(18) . . ? C45 C44 C43 120.8(13) . . ? C44 C45 C46 120.2(14) . . ? C41 C46 C45 120.4(13) . . ? C56 C51 C52 121.2(12) . . ? C56 C51 P1 120.6(10) . . ? C52 C51 P1 118.0(10) . . ? C53 C52 C51 119.9(19) . . ? C52 C53 C54 117(2) . . ? C55 C54 C53 122.5(15) . . ? C54 C55 C56 119.3(17) . . ? C51 C56 C55 119.4(15) . . ? C61 N61 C81 110.6(15) . . ? C61 N61 C71 111.6(15) . . ? C81 N61 C71 110.7(17) . . ? N61 C61 C62 115.3(19) . . ? C72 C71 N61 110(2) . . ? C82 C81 N61 115.2(16) . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 25.94 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 2.371 _refine_diff_density_min -1.096 _refine_diff_density_rms 0.132 #==END data_compound_7 _database_code_CSD 188472 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H42.50 I2 N2 O3.50 P2 Re S' _chemical_formula_weight 1201.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 '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 Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, z+1/2' '-x, -y, -z' '-x, y-1/2, -z-1/2' _cell_length_a 11.068(16) _cell_length_b 23.579(26) _cell_length_c 18.371(24) _cell_angle_alpha 90.00 _cell_angle_beta 96.26(10) _cell_angle_gamma 90.00 _cell_volume 4764(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'dark red' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.675 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2326 _exptl_absorpt_coefficient_mu 3.998 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mar research image plate system' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8431 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 26.04 _reflns_number_total 8431 _reflns_number_gt 6691 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Platon (Spek, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0004P)^2^+148.8310P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8431 _refine_ls_number_parameters 503 _refine_ls_number_restraints 153 _refine_ls_R_factor_all 0.1259 _refine_ls_R_factor_gt 0.0973 _refine_ls_wR_factor_ref 0.1860 _refine_ls_wR_factor_gt 0.1750 _refine_ls_goodness_of_fit_ref 1.211 _refine_ls_restrained_S_all 1.205 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re Re 0.61309(5) 0.48138(2) 0.78954(3) 0.03531(17) Uani 1 d U . . I1 I 0.66057(9) 0.52129(4) 0.92814(6) 0.0460(3) Uani 1 d U . . I2 I 0.82386(10) 0.50427(5) 0.73168(7) 0.0567(3) Uani 1 d U . . P1 P 0.6910(4) 0.38597(16) 0.8304(2) 0.0400(7) Uani 1 d U . . C41 C 0.5713(14) 0.3472(6) 0.8717(9) 0.042(2) Uani 1 d U . . C42 C 0.4868(15) 0.3155(6) 0.8265(10) 0.052(4) Uani 1 d U . . H42 H 0.4970 0.3102 0.7774 0.063 Uiso 1 calc R . . C43 C 0.3864(18) 0.2918(8) 0.8559(13) 0.074(5) Uani 1 d U . . H43 H 0.3279 0.2718 0.8260 0.089 Uiso 1 calc R . . C44 C 0.375(2) 0.2985(9) 0.9292(14) 0.096(7) Uani 1 d U . . H44 H 0.3122 0.2801 0.9492 0.115 Uiso 1 calc R . . C45 C 0.452(2) 0.3305(8) 0.9728(13) 0.076(5) Uani 1 d U . . H15 H 0.4406 0.3366 1.0215 0.092 Uiso 1 calc R . . C46 C 0.5511(17) 0.3546(7) 0.9426(10) 0.056(4) Uani 1 d U . . H46 H 0.6054 0.3767 0.9725 0.068 Uiso 1 calc R . . C21 C 0.8210(14) 0.3820(7) 0.9006(9) 0.046(3) Uani 1 d U . . C22 C 0.9041(13) 0.4274(7) 0.9118(9) 0.043(3) Uani 1 d U . . H22 H 0.8912 0.4600 0.8835 0.052 Uiso 1 calc R . . C23 C 1.0062(15) 0.4245(8) 0.9648(10) 0.058(4) Uani 1 d U . . H23 H 1.0595 0.4550 0.9725 0.069 Uiso 1 calc R . . C24 C 1.0250(19) 0.3749(8) 1.0053(12) 0.069(5) Uiso 1 d U . . H24 H 1.0927 0.3722 1.0400 0.083 Uiso 1 calc R . . C25 C 0.949(2) 0.3308(9) 0.9961(12) 0.082(6) Uani 1 d U . . H25 H 0.9652 0.2979 1.0234 0.098 Uiso 1 calc R . . C26 C 0.8432(17) 0.3336(8) 0.9450(11) 0.061(4) Uani 1 d U . . H26 H 0.7886 0.3035 0.9408 0.073 Uiso 1 calc R . . C31 C 0.7338(14) 0.3354(7) 0.7599(9) 0.046(3) Uani 1 d U . . C32 C 0.7448(19) 0.2776(7) 0.7763(12) 0.072(5) Uani 1 d U . . H32 H 0.7300 0.2649 0.8225 0.086 Uiso 1 calc R . . C33 C 0.7772(19) 0.2390(8) 0.7257(13) 0.074(5) Uani 1 d U . . H33 H 0.7808 0.2005 0.7370 0.088 Uiso 1 calc R . . C34 C 0.804(2) 0.2576(10) 0.6579(14) 0.095(7) Uani 1 d U . . H34 H 0.8316 0.2321 0.6247 0.114 Uiso 1 calc R . . C35 C 0.791(2) 0.3136(10) 0.6401(14) 0.094(7) Uani 1 d U . . H35 H 0.8060 0.3260 0.5939 0.113 Uiso 1 calc R . . C36 C 0.755(2) 0.3525(8) 0.6912(11) 0.072(5) Uani 1 d U . . H36 H 0.7453 0.3905 0.6783 0.086 Uiso 1 calc R . . P2 P 0.5276(4) 0.57663(16) 0.7544(2) 0.0407(6) Uani 1 d U . . C61 C 0.5107(14) 0.5976(7) 0.6576(9) 0.045(2) Uani 1 d U . . C62 C 0.5566(16) 0.5671(7) 0.6040(9) 0.054(4) Uani 1 d U . . H62 H 0.5946 0.5326 0.6160 0.064 Uiso 1 calc R . . C63 C 0.5483(19) 0.5857(9) 0.5329(10) 0.069(4) Uani 1 d U . . H63 H 0.5828 0.5646 0.4977 0.082 Uiso 1 calc R . . C64 C 0.489(2) 0.6356(9) 0.5139(12) 0.083(6) Uani 1 d U . . H64 H 0.4785 0.6474 0.4653 0.100 Uiso 1 calc R . . C65 C 0.446(2) 0.6673(9) 0.5663(12) 0.088(6) Uani 1 d U . . H65 H 0.4116 0.7025 0.5542 0.105 Uiso 1 calc R . . C66 C 0.453(2) 0.6488(8) 0.6365(12) 0.077(6) Uani 1 d U . . H66 H 0.4179 0.6704 0.6712 0.093 Uiso 1 calc R . . C51 C 0.3691(15) 0.5802(7) 0.7778(10) 0.048(2) Uani 1 d U . . C52 C 0.2760(15) 0.5667(7) 0.7254(11) 0.057(4) Uani 1 d U . . H52 H 0.2901 0.5593 0.6774 0.069 Uiso 1 calc R . . C53 C 0.1560(18) 0.5645(9) 0.7476(13) 0.075(5) Uani 1 d U . . H53 H 0.0913 0.5550 0.7131 0.090 Uiso 1 calc R . . C54 C 0.1336(19) 0.5758(10) 0.8170(15) 0.084(6) Uani 1 d U . . H54 H 0.0543 0.5748 0.8293 0.101 Uiso 1 calc R . . C55 C 0.2278(17) 0.5888(8) 0.8691(13) 0.070(4) Uani 1 d U . . H55 H 0.2129 0.5959 0.9171 0.083 Uiso 1 calc R . . C56 C 0.3448(16) 0.5912(7) 0.8498(10) 0.056(4) Uani 1 d U . . H56 H 0.4085 0.6004 0.8851 0.067 Uiso 1 calc R . . C71 C 0.5988(16) 0.6410(6) 0.7973(9) 0.047(3) Uani 1 d U . . C72 C 0.7273(19) 0.6424(8) 0.8106(12) 0.073(5) Uani 1 d U . . H72 H 0.7739 0.6110 0.8008 0.088 Uiso 1 calc R . . C73 C 0.782(2) 0.6925(9) 0.8391(13) 0.094(6) Uani 1 d U . . H73 H 0.8660 0.6951 0.8449 0.113 Uiso 1 calc R . . C74 C 0.714(3) 0.7386(8) 0.8589(12) 0.103(7) Uani 1 d U . . H74 H 0.7518 0.7708 0.8796 0.124 Uiso 1 calc R . . C75 C 0.591(3) 0.7357(8) 0.8477(12) 0.092(6) Uani 1 d U . . H75 H 0.5450 0.7663 0.8611 0.110 Uiso 1 calc R . . C76 C 0.530(2) 0.6874(7) 0.8159(12) 0.072(5) Uani 1 d U . . H76 H 0.4457 0.6865 0.8077 0.086 Uiso 1 calc R . . N11 N 0.4366(10) 0.4549(5) 0.8078(7) 0.0359(9) Uani 1 d U . . S1 S 0.5004(4) 0.43873(16) 0.6828(2) 0.0427(7) Uani 1 d U . . C12 C 0.3903(13) 0.4338(6) 0.7411(9) 0.038(2) Uani 1 d U . . C13 C 0.2724(14) 0.4116(6) 0.7314(10) 0.046(3) Uani 1 d U . . C14 C 0.2030(16) 0.4121(7) 0.7901(11) 0.062(4) Uani 1 d U . . H14 H 0.1234 0.3989 0.7845 0.074 Uiso 1 calc R . . C15 C 0.2552(16) 0.4330(8) 0.8582(12) 0.065(5) Uani 1 d U . . H15' H 0.2136 0.4320 0.8995 0.078 Uiso 1 calc R . . C16 C 0.3759(13) 0.4559(5) 0.8607(9) 0.040(3) Uani 1 d U . . H16 H 0.4101 0.4724 0.9041 0.047 Uiso 1 calc R . . C17 C 0.2238(16) 0.3873(7) 0.6598(11) 0.055(3) Uani 1 d U . . O19 O 0.2812(13) 0.3848(6) 0.6078(8) 0.078(4) Uani 1 d U . . O18 O 0.1099(12) 0.3686(7) 0.6596(9) 0.092(5) Uani 1 d U . . H18 H 0.0835 0.3591 0.6179 0.110 Uiso 1 calc R . . O90 O 0.0377(16) 0.3214(8) 0.5324(10) 0.109(6) Uani 1 d U . . C91 C 0.097(3) 0.3313(10) 0.4831(15) 0.092(7) Uani 1 d U . . H91 H 0.1738 0.3464 0.4977 0.111 Uiso 1 calc R . . N92 N 0.074(2) 0.3248(8) 0.4143(12) 0.093(6) Uani 1 d U . . C93 C 0.152(3) 0.3379(15) 0.3598(18) 0.152(12) Uani 1 d U . . H93A H 0.1207 0.3705 0.3326 0.182 Uiso 1 calc R . . H93B H 0.1546 0.3062 0.3273 0.182 Uiso 1 calc R . . H93C H 0.2318 0.3458 0.3829 0.182 Uiso 1 calc R . . C94 C -0.044(3) 0.3072(15) 0.391(2) 0.27(3) Uani 1 d U . . H94A H -0.0690 0.2797 0.4250 0.329 Uiso 1 calc R . . H94B H -0.0459 0.2904 0.3434 0.329 Uiso 1 calc R . . H94C H -0.0974 0.3393 0.3891 0.329 Uiso 1 calc R . . OW1 O -0.108(3) 0.4780(15) 0.505(2) 0.143(15) Uiso 0.50 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re 0.0370(3) 0.0336(3) 0.0353(3) -0.0026(2) 0.0041(2) -0.0057(3) I1 0.0522(6) 0.0465(6) 0.0381(5) -0.0073(4) -0.0017(4) -0.0008(5) I2 0.0437(6) 0.0643(7) 0.0641(8) 0.0069(5) 0.0156(5) -0.0108(5) P1 0.0345(19) 0.0362(10) 0.049(2) -0.0034(8) 0.0023(12) -0.0025(11) C41 0.046(5) 0.035(4) 0.046(5) 0.002(4) 0.003(4) -0.005(4) C42 0.057(9) 0.037(8) 0.063(7) -0.005(7) 0.008(6) -0.018(6) C43 0.060(10) 0.065(12) 0.098(10) -0.002(10) 0.017(8) -0.026(8) C44 0.113(16) 0.079(15) 0.101(12) 0.016(11) 0.043(12) -0.051(12) C45 0.101(14) 0.063(12) 0.072(8) 0.012(9) 0.037(9) -0.016(9) C46 0.080(11) 0.040(9) 0.051(6) 0.000(6) 0.018(6) -0.013(7) C21 0.042(5) 0.046(5) 0.050(6) 0.000(4) -0.002(4) 0.001(4) C22 0.039(7) 0.056(7) 0.035(9) -0.009(6) 0.002(5) -0.003(5) C23 0.035(8) 0.074(10) 0.062(12) -0.007(8) -0.006(6) 0.005(6) C25 0.079(13) 0.079(12) 0.081(16) 0.020(10) -0.024(9) 0.008(9) C26 0.062(10) 0.057(8) 0.060(12) 0.011(7) -0.006(7) 0.003(7) C31 0.038(7) 0.045(4) 0.053(5) -0.007(3) 0.001(4) 0.007(5) C32 0.096(15) 0.044(4) 0.076(10) -0.008(5) 0.015(11) 0.015(10) C33 0.079(14) 0.054(5) 0.086(11) -0.023(6) 0.000(11) 0.017(10) C34 0.113(19) 0.082(8) 0.095(13) -0.027(10) 0.032(15) 0.027(14) C35 0.13(2) 0.079(9) 0.078(11) -0.024(7) 0.046(14) -0.003(14) C36 0.101(16) 0.061(7) 0.056(8) -0.011(5) 0.020(11) 0.002(10) P2 0.0469(15) 0.0334(10) 0.0413(15) 0.0018(11) 0.0028(14) -0.0086(11) C61 0.039(8) 0.053(6) 0.041(2) 0.004(3) -0.011(4) 0.002(6) C62 0.070(12) 0.051(8) 0.038(3) 0.001(5) -0.002(7) -0.006(7) C63 0.089(14) 0.077(11) 0.037(4) 0.003(6) -0.008(8) -0.020(9) C64 0.121(19) 0.078(12) 0.048(9) 0.028(7) -0.001(10) -0.018(10) C65 0.13(2) 0.068(11) 0.057(7) 0.021(7) -0.019(11) 0.004(10) C66 0.120(18) 0.051(9) 0.062(6) 0.021(7) 0.014(11) 0.018(9) C51 0.045(2) 0.043(6) 0.054(5) 0.000(6) 0.001(3) 0.004(2) C52 0.045(2) 0.053(10) 0.071(8) -0.008(8) -0.006(5) 0.008(8) C53 0.048(3) 0.074(13) 0.100(10) 0.004(11) 0.001(6) -0.012(10) C54 0.047(7) 0.096(16) 0.111(13) 0.002(14) 0.019(7) -0.007(11) C55 0.055(7) 0.065(12) 0.092(9) -0.008(10) 0.024(6) 0.006(9) C56 0.047(6) 0.064(11) 0.056(6) 0.006(8) 0.007(4) 0.013(8) C71 0.067(5) 0.0325(12) 0.039(6) 0.004(4) -0.001(6) -0.012(4) C72 0.069(5) 0.048(8) 0.096(16) 0.003(8) -0.020(10) -0.023(5) C73 0.118(8) 0.058(9) 0.095(18) 0.020(9) -0.038(13) -0.053(8) C74 0.184(15) 0.041(8) 0.069(15) 0.005(8) -0.052(16) -0.046(10) C75 0.178(14) 0.037(7) 0.056(14) -0.006(7) -0.014(14) -0.011(9) C76 0.103(8) 0.029(6) 0.082(15) -0.001(6) 0.007(11) -0.003(6) N11 0.0374(13) 0.026(3) 0.045(3) -0.006(4) 0.009(2) -0.0025(13) S1 0.0489(15) 0.0420(15) 0.0365(14) -0.0054(12) 0.0019(11) -0.0074(14) C12 0.034(4) 0.030(7) 0.050(4) -0.007(6) 0.000(3) 0.001(5) C13 0.045(5) 0.025(7) 0.066(5) -0.004(6) 0.002(3) -0.011(6) C14 0.047(7) 0.059(10) 0.080(7) -0.006(9) 0.013(5) -0.020(8) C15 0.050(7) 0.074(12) 0.076(7) -0.015(10) 0.025(6) -0.021(8) C16 0.050(5) 0.015(6) 0.057(4) -0.009(6) 0.020(4) -0.009(5) C17 0.045(6) 0.041(9) 0.075(7) -0.010(8) -0.009(4) -0.008(7) O19 0.073(8) 0.096(10) 0.061(6) -0.015(7) -0.006(5) -0.040(8) O18 0.051(6) 0.112(12) 0.110(10) -0.037(9) -0.003(5) -0.031(7) O90 0.096(13) 0.137(15) 0.090(10) -0.018(11) -0.002(9) -0.046(11) C91 0.106(18) 0.086(16) 0.081(10) -0.003(13) -0.005(9) -0.020(14) N92 0.115(13) 0.076(12) 0.081(9) 0.013(10) -0.020(9) -0.031(11) C93 0.19(2) 0.17(3) 0.097(15) 0.02(2) 0.030(18) -0.01(3) C94 0.23(3) 0.39(7) 0.18(3) 0.01(4) -0.06(2) -0.24(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re N11 2.111(12) . ? Re S1 2.425(4) . ? Re P2 2.494(5) . ? Re P1 2.495(5) . ? Re I1 2.711(3) . ? Re I2 2.721(3) . ? P1 C21 1.827(16) . ? P1 C41 1.840(16) . ? P1 C31 1.859(16) . ? C41 C46 1.36(2) . ? C41 C42 1.40(2) . ? C42 C43 1.40(2) . ? C43 C44 1.38(3) . ? C44 C45 1.34(3) . ? C45 C46 1.40(2) . ? C21 C26 1.41(2) . ? C21 C22 1.41(2) . ? C22 C23 1.41(2) . ? C23 C24 1.39(3) . ? C24 C25 1.34(3) . ? C25 C26 1.42(3) . ? C31 C36 1.37(3) . ? C31 C32 1.40(2) . ? C32 C33 1.38(3) . ? C33 C34 1.38(3) . ? C34 C35 1.36(3) . ? C35 C36 1.40(3) . ? P2 C61 1.837(17) . ? P2 C71 1.847(15) . ? P2 C51 1.852(17) . ? C61 C62 1.36(2) . ? C61 C66 1.40(2) . ? C62 C63 1.37(2) . ? C63 C64 1.38(3) . ? C64 C65 1.34(3) . ? C65 C66 1.36(3) . ? C51 C52 1.37(2) . ? C51 C56 1.40(2) . ? C52 C53 1.43(3) . ? C53 C54 1.35(3) . ? C54 C55 1.37(3) . ? C55 C56 1.38(2) . ? C71 C76 1.39(2) . ? C71 C72 1.42(3) . ? C72 C73 1.40(2) . ? C73 C74 1.39(4) . ? C74 C75 1.35(4) . ? C75 C76 1.42(3) . ? N11 C16 1.241(18) . ? N11 C12 1.369(18) . ? S1 C12 1.712(16) . ? C12 C13 1.40(2) . ? C13 C14 1.39(2) . ? C13 C17 1.48(2) . ? C14 C15 1.41(3) . ? C15 C16 1.44(2) . ? C17 O19 1.21(2) . ? C17 O18 1.33(2) . ? O90 C91 1.20(3) . ? C91 N92 1.27(3) . ? N92 C94 1.39(3) . ? N92 C93 1.42(3) . ? 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 N11 Re S1 66.6(3) . . ? N11 Re P2 88.6(3) . . ? S1 Re P2 90.97(15) . . ? N11 Re P1 88.9(3) . . ? S1 Re P1 90.01(15) . . ? P2 Re P1 176.73(14) . . ? N11 Re I1 92.4(3) . . ? S1 Re I1 158.96(11) . . ? P2 Re I1 87.70(11) . . ? P1 Re I1 90.27(12) . . ? N11 Re I2 165.4(3) . . ? S1 Re I2 98.82(13) . . ? P2 Re I2 92.17(12) . . ? P1 Re I2 90.77(11) . . ? I1 Re I2 102.21(7) . . ? C21 P1 C41 103.3(8) . . ? C21 P1 C31 102.6(7) . . ? C41 P1 C31 102.6(7) . . ? C21 P1 Re 118.6(5) . . ? C41 P1 Re 109.3(5) . . ? C31 P1 Re 118.3(6) . . ? C46 C41 C42 118.0(16) . . ? C46 C41 P1 122.2(12) . . ? C42 C41 P1 119.1(13) . . ? C41 C42 C43 119.5(18) . . ? C44 C43 C42 119(2) . . ? C45 C44 C43 122.1(19) . . ? C44 C45 C46 118(2) . . ? C41 C46 C45 123.1(18) . . ? C26 C21 C22 117.4(15) . . ? C26 C21 P1 121.6(13) . . ? C22 C21 P1 121.0(12) . . ? C23 C22 C21 121.6(16) . . ? C24 C23 C22 118.2(18) . . ? C25 C24 C23 122(2) . . ? C24 C25 C26 120.7(19) . . ? C21 C26 C25 120.0(18) . . ? C36 C31 C32 117.7(16) . . ? C36 C31 P1 122.5(13) . . ? C32 C31 P1 119.8(14) . . ? C33 C32 C31 121(2) . . ? C32 C33 C34 120(2) . . ? C35 C34 C33 120(2) . . ? C34 C35 C36 120(2) . . ? C31 C36 C35 121(2) . . ? C61 P2 C71 100.7(7) . . ? C61 P2 C51 102.4(8) . . ? C71 P2 C51 103.6(8) . . ? C61 P2 Re 119.2(5) . . ? C71 P2 Re 119.8(6) . . ? C51 P2 Re 108.8(5) . . ? C62 C61 C66 116.8(16) . . ? C62 C61 P2 123.5(13) . . ? C66 C61 P2 119.6(14) . . ? C61 C62 C63 121.9(18) . . ? C62 C63 C64 120(2) . . ? C65 C64 C63 119(2) . . ? C64 C65 C66 121(2) . . ? C65 C66 C61 121(2) . . ? C52 C51 C56 119.9(17) . . ? C52 C51 P2 119.1(14) . . ? C56 C51 P2 120.7(13) . . ? C51 C52 C53 117.3(19) . . ? C54 C53 C52 122(2) . . ? C53 C54 C55 120(2) . . ? C54 C55 C56 120(2) . . ? C55 C56 C51 121.0(18) . . ? C76 C71 C72 120.3(16) . . ? C76 C71 P2 122.0(14) . . ? C72 C71 P2 117.7(13) . . ? C73 C72 C71 118(2) . . ? C74 C73 C72 122(2) . . ? C75 C74 C73 118.9(19) . . ? C74 C75 C76 122(2) . . ? C71 C76 C75 119(2) . . ? C16 N11 C12 121.7(13) . . ? C16 N11 Re 135.1(11) . . ? C12 N11 Re 103.2(9) . . ? C12 S1 Re 82.0(5) . . ? N11 C12 C13 120.2(14) . . ? N11 C12 S1 108.2(10) . . ? C13 C12 S1 131.6(12) . . ? C14 C13 C12 119.0(15) . . ? C14 C13 C17 120.9(15) . . ? C12 C13 C17 120.1(15) . . ? C13 C14 C15 119.0(16) . . ? C14 C15 C16 116.7(16) . . ? N11 C16 C15 123.3(16) . . ? O19 C17 O18 124.1(17) . . ? O19 C17 C13 123.4(16) . . ? O18 C17 C13 112.5(17) . . ? O90 C91 N92 131(3) . . ? C91 N92 C94 115(3) . . ? C91 N92 C93 127(3) . . ? C94 N92 C93 118(3) . . ? _diffrn_measured_fraction_theta_max 0.895 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.895 _refine_diff_density_max 2.094 _refine_diff_density_min -1.720 _refine_diff_density_rms 0.207 #==END data_compound_8 _database_code_CSD 188473 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H12 Mo N2 O6 S2' _chemical_formula_weight 464.32 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' 'x-1/2, y, -z-1/2' _cell_length_a 8.128(14) _cell_length_b 28.616(35) _cell_length_c 14.941(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3475(8) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour 'brown' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.775 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 1.028 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Mar research imgale plate system' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11034 _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_sigmaI/netI 0.0201 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 26.06 _reflns_number_total 3113 _reflns_number_gt 2577 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Platon (Spek, 1999)' _computing_publication_material 'Platon (Spek, 1999)' _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 w=1/[\s^2^(Fo^2^)+(0.0127P)^2^+12.8947P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00105(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3113 _refine_ls_number_parameters 229 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0584 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.0909 _refine_ls_wR_factor_gt 0.0843 _refine_ls_goodness_of_fit_ref 1.191 _refine_ls_restrained_S_all 1.191 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo Mo 0.09002(5) 0.378115(13) 0.05336(3) 0.03375(14) Uani 1 d . . . S1 S 0.11858(18) 0.44396(4) 0.15721(8) 0.0432(3) Uani 1 d . . . C12 C 0.2064(6) 0.47343(14) 0.0654(3) 0.0313(10) Uani 1 d . . . N11 N 0.2128(5) 0.44410(13) -0.0054(2) 0.0361(9) Uani 1 d . . . C16 C 0.2684(7) 0.45975(17) -0.0844(3) 0.0418(12) Uani 1 d . . . H16 H 0.2701 0.4396 -0.1332 0.050 Uiso 1 calc R . . C15 C 0.3230(7) 0.50493(17) -0.0951(3) 0.0445(12) Uani 1 d . . . H15 H 0.3591 0.5154 -0.1506 0.053 Uiso 1 calc R . . C14 C 0.3235(6) 0.53455(17) -0.0221(3) 0.0418(12) Uani 1 d . . . H14 H 0.3628 0.5649 -0.0279 0.050 Uiso 1 calc R . . C13 C 0.2653(6) 0.51899(14) 0.0599(3) 0.0336(10) Uani 1 d . . . C17 C 0.2649(7) 0.54978(15) 0.1405(3) 0.0390(11) Uani 1 d . . . O18 O 0.3752(5) 0.58414(11) 0.1328(2) 0.0451(8) Uani 1 d . . . O19 O 0.1776(5) 0.54432(12) 0.2045(2) 0.0595(11) Uani 1 d . . . C20 C 0.3836(8) 0.61631(17) 0.2075(4) 0.0582(15) Uani 1 d . . . H20A H 0.2794 0.6317 0.2145 0.070 Uiso 1 calc R . . H20B H 0.4674 0.6392 0.1963 0.070 Uiso 1 calc R . . H20C H 0.4095 0.5994 0.2611 0.070 Uiso 1 calc R . . S2 S 0.22311(16) 0.33025(4) -0.06119(8) 0.0392(3) Uani 1 d . . . C22 C 0.3965(6) 0.33181(14) 0.0091(3) 0.0315(9) Uani 1 d . . . N21 N 0.3633(5) 0.36002(12) 0.0806(2) 0.0324(8) Uani 1 d . . . C26 C 0.4748(6) 0.36462(17) 0.1459(3) 0.0386(11) Uani 1 d . . . H26 H 0.4503 0.3832 0.1952 0.046 Uiso 1 calc R . . C25 C 0.6247(6) 0.34251(18) 0.1419(3) 0.0453(12) Uani 1 d . . . H25 H 0.7000 0.3456 0.1884 0.054 Uiso 1 calc R . . C24 C 0.6621(6) 0.31570(17) 0.0678(3) 0.0416(11) Uani 1 d . . . H24 H 0.7643 0.3013 0.0637 0.050 Uiso 1 calc R . . C23 C 0.5478(6) 0.31016(15) -0.0007(3) 0.0333(10) Uani 1 d . . . C27 C 0.5859(7) 0.28265(16) -0.0831(3) 0.0426(12) Uani 1 d . . . O28 O 0.7461(5) 0.27645(13) -0.0937(2) 0.0548(10) Uani 1 d . . . O29 O 0.4830(5) 0.26982(14) -0.1353(3) 0.0623(11) Uani 1 d . . . C30 C 0.7958(8) 0.2545(2) -0.1766(4) 0.0687(19) Uani 1 d . . . H30A H 0.7453 0.2243 -0.1813 0.082 Uiso 1 calc R . . H30B H 0.9133 0.2511 -0.1774 0.082 Uiso 1 calc R . . H30C H 0.7620 0.2736 -0.2261 0.082 Uiso 1 calc R . . O1 O 0.0312(4) 0.34182(11) 0.1373(2) 0.0442(8) Uani 1 d . . . O2 O -0.0789(5) 0.38748(12) -0.0114(2) 0.0512(9) Uani 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 Mo 0.0293(3) 0.0368(2) 0.0352(2) 0.00094(16) -0.00193(16) 0.00056(16) S1 0.0583(9) 0.0415(6) 0.0297(6) -0.0004(5) 0.0121(5) -0.0047(6) C12 0.035(3) 0.031(2) 0.027(2) 0.0035(17) -0.0009(18) 0.0036(17) N11 0.041(3) 0.039(2) 0.0285(19) -0.0037(15) 0.0011(16) 0.0025(17) C16 0.049(3) 0.052(3) 0.024(2) 0.000(2) 0.003(2) 0.007(2) C15 0.056(4) 0.052(3) 0.026(2) 0.008(2) 0.008(2) 0.002(2) C14 0.046(3) 0.045(3) 0.034(2) 0.009(2) 0.006(2) 0.000(2) C13 0.036(3) 0.034(2) 0.032(2) -0.0023(18) 0.0013(19) 0.0057(18) C17 0.051(3) 0.033(2) 0.033(2) 0.0021(18) 0.000(2) 0.004(2) O18 0.051(2) 0.0385(17) 0.0460(19) -0.0020(14) 0.0026(16) -0.0042(15) O19 0.090(3) 0.051(2) 0.0375(19) -0.0060(16) 0.022(2) -0.013(2) C20 0.075(5) 0.041(3) 0.059(3) -0.008(2) 0.003(3) -0.008(3) S2 0.0359(8) 0.0461(6) 0.0355(6) -0.0074(5) -0.0115(5) 0.0053(5) C22 0.032(3) 0.033(2) 0.030(2) 0.0015(17) -0.0056(18) -0.0058(18) N21 0.029(2) 0.0389(19) 0.0290(18) -0.0013(15) -0.0042(15) -0.0010(15) C26 0.037(3) 0.053(3) 0.026(2) -0.0007(19) -0.0020(19) -0.011(2) C25 0.031(3) 0.070(3) 0.035(3) 0.004(2) -0.008(2) -0.011(2) C24 0.026(3) 0.054(3) 0.045(3) 0.010(2) 0.000(2) 0.000(2) C23 0.033(3) 0.035(2) 0.032(2) 0.0042(18) 0.0017(18) -0.0017(18) C27 0.045(4) 0.040(2) 0.042(3) 0.005(2) 0.004(2) 0.006(2) O28 0.044(3) 0.070(2) 0.051(2) -0.0008(18) 0.0126(18) 0.0148(18) O29 0.056(3) 0.078(3) 0.053(2) -0.025(2) -0.006(2) 0.012(2) C30 0.076(5) 0.071(4) 0.060(4) 0.008(3) 0.027(3) 0.025(3) O1 0.040(2) 0.0443(18) 0.048(2) 0.0043(15) 0.0006(16) -0.0056(15) O2 0.040(2) 0.059(2) 0.055(2) 0.0012(17) -0.0130(17) 0.0092(17) _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 Mo O1 1.697(3) . ? Mo O2 1.701(4) . ? Mo N11 2.309(4) . ? Mo N21 2.317(5) . ? Mo S2 2.445(2) . ? Mo S1 2.452(2) . ? S1 C12 1.761(4) . ? C12 N11 1.352(5) . ? C12 C13 1.391(6) . ? N11 C16 1.340(6) . ? C16 C15 1.376(7) . ? C15 C14 1.381(7) . ? C14 C13 1.387(6) . ? C13 C17 1.492(6) . ? C17 O19 1.201(6) . ? C17 O18 1.336(6) . ? O18 C20 1.448(6) . ? S2 C22 1.759(5) . ? C22 N21 1.366(5) . ? C22 C23 1.385(7) . ? N21 C26 1.339(6) . ? C26 C25 1.374(7) . ? C25 C24 1.380(7) . ? C24 C23 1.392(6) . ? C23 C27 1.493(6) . ? C27 O29 1.202(6) . ? C27 O28 1.324(7) . ? O28 C30 1.446(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo O2 106.80(19) . . ? O1 Mo N11 154.59(14) . . ? O2 Mo N11 90.21(18) . . ? O1 Mo N21 90.21(16) . . ? O2 Mo N21 155.39(16) . . ? N11 Mo N21 80.52(15) . . ? O1 Mo S2 107.41(14) . . ? O2 Mo S2 92.72(15) . . ? N11 Mo S2 90.03(12) . . ? N21 Mo S2 64.76(10) . . ? O1 Mo S1 91.68(15) . . ? O2 Mo S1 108.37(13) . . ? N11 Mo S1 64.63(12) . . ? N21 Mo S1 88.27(10) . . ? S2 Mo S1 146.28(7) . . ? C12 S1 Mo 85.04(16) . . ? N11 C12 C13 121.5(4) . . ? N11 C12 S1 109.2(3) . . ? C13 C12 S1 129.3(3) . . ? C16 N11 C12 119.7(4) . . ? C16 N11 Mo 138.9(3) . . ? C12 N11 Mo 101.1(3) . . ? N11 C16 C15 121.6(4) . . ? C16 C15 C14 119.1(4) . . ? C15 C14 C13 120.0(4) . . ? C14 C13 C12 118.1(4) . . ? C14 C13 C17 121.6(4) . . ? C12 C13 C17 120.3(4) . . ? O19 C17 O18 124.1(4) . . ? O19 C17 C13 124.5(4) . . ? O18 C17 C13 111.3(4) . . ? C17 O18 C20 115.6(4) . . ? C22 S2 Mo 85.53(18) . . ? N21 C22 C23 121.6(4) . . ? N21 C22 S2 108.9(3) . . ? C23 C22 S2 129.5(3) . . ? C26 N21 C22 119.7(4) . . ? C26 N21 Mo 139.0(3) . . ? C22 N21 Mo 100.6(3) . . ? N21 C26 C25 121.5(4) . . ? C26 C25 C24 119.1(4) . . ? C25 C24 C23 120.4(5) . . ? C22 C23 C24 117.6(4) . . ? C22 C23 C27 120.5(4) . . ? C24 C23 C27 121.9(5) . . ? O29 C27 O28 124.4(5) . . ? O29 C27 C23 123.5(5) . . ? O28 C27 C23 111.9(4) . . ? C27 O28 C30 115.9(5) . . ? _diffrn_measured_fraction_theta_max 0.803 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 0.803 _refine_diff_density_max 0.701 _refine_diff_density_min -0.758 _refine_diff_density_rms 0.093 #==END