Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Marchi, Andrea' 'Bergamini, Paola' 'Bertolasi, V.' 'Ferretti, V.' 'Lazzaro, Antonio' 'Mantovani, Nicoletta' 'Marvelli, Lorenza' 'Rossi, Roberto' 'Vetruani, Gianni' _publ_contact_author_name 'Prof Andrea Marchi' _publ_contact_author_address ; Dipartimento di Chimica Universita di Ferrara Laboratorio di Chimica Inorganica e via L. Borsari 46 Ferrara 44100 ITALY ; _publ_contact_author_email 'MHA@DNS.UNIFE.IT' _publ_section_title ; Synthesis, Characterization, Properties and Structures of Rhenium(II), -(III), and- (V) Complexes with Derivatized Amino Acids ; data_(9) _database_code_CSD 179466 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H37 Cl N2 O2 P2 Re S' _chemical_formula_sum 'C47 H37 Cl N2 O2 P2 Re S' _chemical_formula_weight 977.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Re' 'Re' -1.0185 7.2310 '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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'O' 'O' 0.0106 0.0060 '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' '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' _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 9.7671(1) _cell_length_b 11.7999(2) _cell_length_c 19.8616(3) _cell_angle_alpha 76.5863(8) _cell_angle_beta 89.1218(10) _cell_angle_gamma 68.3395(9) _cell_volume 2063.17(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24506 _cell_measurement_theta_min 1.0 _cell_measurement_theta_max 30.03 _exptl_crystal_description 'prism' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 974 _exptl_absorpt_coefficient_mu 3.179 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.64 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_process_details ; SORTAV (R.H. Blessing, Acta Crystallogr., 1995, A51, 33. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method 'phi scan plus omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'none' _diffrn_reflns_number 24506 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0327 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 30.03 _reflns_number_total 11830 _reflns_number_gt 10995 _reflns_threshold_expression 'I>2sigma(I)' _computing_data_collection 'Kappa-CCD software (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski, Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski, Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1976)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+2.4383P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11830 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0734 _refine_ls_wR_factor_gt 0.0701 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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 Re1 Re 0.146512(10) 0.015378(9) 0.215556(5) 0.02321(4) Uani 1 1 d . . . P1 P 0.09811(8) 0.20305(7) 0.11794(4) 0.02708(13) Uani 1 1 d . . . P2 P 0.19737(8) -0.16628(7) 0.31616(4) 0.02751(13) Uani 1 1 d . . . Cl1 Cl 0.40505(8) -0.02873(8) 0.20988(5) 0.04089(17) Uani 1 1 d . . . S1 S -0.32828(9) 0.17882(10) 0.27864(5) 0.0483(2) Uani 1 1 d . . . O1 O 0.1149(3) -0.1467(3) 0.12355(14) 0.0569(7) Uani 1 1 d . . . O2 O 0.1561(2) 0.1267(2) 0.28463(11) 0.0311(4) Uani 1 1 d . . . N1 N -0.0848(3) 0.2012(2) 0.31645(14) 0.0350(5) Uani 1 1 d . . . N2 N -0.0779(2) 0.0763(2) 0.23229(12) 0.0283(5) Uani 1 1 d . . . C1 C 0.1300(3) -0.0831(3) 0.15793(15) 0.0344(6) Uani 1 1 d . . . C2 C 0.0562(3) 0.1881(3) 0.31811(14) 0.0290(5) Uani 1 1 d . . . C3 C -0.1406(3) 0.1495(3) 0.27594(15) 0.0311(6) Uani 1 1 d . . . C4 C -0.3187(4) 0.0921(4) 0.2191(2) 0.0482(8) Uani 1 1 d . . . H4 H -0.3984 0.0793 0.2019 0.058 Uiso 1 1 calc R . . C5 C -0.1809(3) 0.0456(3) 0.20093(18) 0.0389(7) Uani 1 1 d . . . H5 H -0.1553 -0.0043 0.1692 0.047 Uiso 1 1 calc R . . C6 C 0.1037(4) 0.2501(3) 0.36559(16) 0.0361(6) Uani 1 1 d . . . C7 C 0.2463(4) 0.2476(4) 0.3660(2) 0.0531(9) Uani 1 1 d . . . H7 H 0.3116 0.2083 0.3364 0.064 Uiso 1 1 calc R . . C8 C 0.2923(6) 0.3037(5) 0.4108(3) 0.0702(13) Uani 1 1 d . . . H8 H 0.3876 0.3035 0.4101 0.084 Uiso 1 1 calc R . . C9 C 0.1992(6) 0.3589(5) 0.4556(3) 0.0764(15) Uani 1 1 d . . . H9 H 0.2312 0.3956 0.4856 0.092 Uiso 1 1 calc R . . C10 C 0.0588(6) 0.3604(5) 0.4567(3) 0.0748(14) Uani 1 1 d . . . H10 H -0.0041 0.3966 0.4880 0.090 Uiso 1 1 calc R . . C11 C 0.0095(5) 0.3079(4) 0.4110(2) 0.0541(10) Uani 1 1 d . . . H11 H -0.0873 0.3116 0.4109 0.065 Uiso 1 1 calc R . . C12 C 0.1281(3) 0.3367(3) 0.13752(15) 0.0326(6) Uani 1 1 d . . . C13 C 0.2519(4) 0.3128(3) 0.18029(19) 0.0408(7) Uani 1 1 d . . . H13 H 0.3120 0.2304 0.2016 0.049 Uiso 1 1 calc R . . C14 C 0.2859(4) 0.4116(4) 0.1912(2) 0.0508(9) Uani 1 1 d . . . H14 H 0.3696 0.3948 0.2195 0.061 Uiso 1 1 calc R . . C15 C 0.1982(5) 0.5335(4) 0.1609(2) 0.0555(10) Uani 1 1 d . . . H15 H 0.2221 0.5990 0.1685 0.067 Uiso 1 1 calc R . . C16 C 0.0742(5) 0.5587(3) 0.1191(2) 0.0567(10) Uani 1 1 d . . . H16 H 0.0137 0.6416 0.0989 0.068 Uiso 1 1 calc R . . C17 C 0.0391(4) 0.4609(3) 0.1069(2) 0.0468(8) Uani 1 1 d . . . H17 H -0.0442 0.4786 0.0782 0.056 Uiso 1 1 calc R . . C18 C 0.2043(3) 0.1810(3) 0.04210(15) 0.0352(6) Uani 1 1 d . . . C19 C 0.2327(5) 0.0746(4) 0.0175(2) 0.0566(10) Uani 1 1 d . . . H19 H 0.2014 0.0117 0.0410 0.068 Uiso 1 1 calc R . . C20 C 0.3075(6) 0.0607(5) -0.0422(2) 0.0701(13) Uani 1 1 d . . . H20 H 0.3257 -0.0111 -0.0582 0.084 Uiso 1 1 calc R . . C21 C 0.3544(5) 0.1523(5) -0.0771(2) 0.0688(13) Uani 1 1 d . . . H21 H 0.4028 0.1435 -0.1174 0.083 Uiso 1 1 calc R . . C22 C 0.3300(5) 0.2568(5) -0.0527(2) 0.0665(12) Uani 1 1 d . . . H22 H 0.3642 0.3180 -0.0759 0.080 Uiso 1 1 calc R . . C23 C 0.2548(4) 0.2723(4) 0.00632(19) 0.0498(8) Uani 1 1 d . . . H23 H 0.2380 0.3443 0.0221 0.060 Uiso 1 1 calc R . . C24 C -0.0955(3) 0.2665(3) 0.08453(15) 0.0322(6) Uani 1 1 d . . . C25 C -0.2038(4) 0.3388(3) 0.12030(18) 0.0400(7) Uani 1 1 d . . . H25 H -0.1763 0.3612 0.1583 0.048 Uiso 1 1 calc R . . C26 C -0.3518(4) 0.3773(4) 0.0998(2) 0.0515(9) Uani 1 1 d . . . H26 H -0.4233 0.4267 0.1235 0.062 Uiso 1 1 calc R . . C27 C -0.3935(4) 0.3426(4) 0.0441(2) 0.0604(11) Uani 1 1 d . . . H27 H -0.4932 0.3684 0.0305 0.073 Uiso 1 1 calc R . . C28 C -0.2888(5) 0.2704(4) 0.0088(2) 0.0567(10) Uani 1 1 d . . . H28 H -0.3176 0.2469 -0.0286 0.068 Uiso 1 1 calc R . . C29 C -0.1392(4) 0.2321(4) 0.02858(18) 0.0439(7) Uani 1 1 d . . . H29 H -0.0685 0.1833 0.0044 0.053 Uiso 1 1 calc R . . C30 C 0.2386(3) -0.1354(3) 0.39793(15) 0.0340(6) Uani 1 1 d . . . C31 C 0.1649(5) -0.1478(4) 0.45700(19) 0.0549(10) Uani 1 1 d . . . H31 H 0.0863 -0.1745 0.4576 0.066 Uiso 1 1 calc R . . C32 C 0.2077(5) -0.1203(5) 0.5162(2) 0.0664(12) Uani 1 1 d . . . H32 H 0.1560 -0.1274 0.5557 0.080 Uiso 1 1 calc R . . C33 C 0.3231(6) -0.0835(5) 0.5167(2) 0.0669(12) Uani 1 1 d . . . H33 H 0.3510 -0.0656 0.5563 0.080 Uiso 1 1 calc R . . C34 C 0.3988(6) -0.0729(6) 0.4584(2) 0.0728(14) Uani 1 1 d . . . H34 H 0.4796 -0.0494 0.4590 0.087 Uiso 1 1 calc R . . C35 C 0.3567(4) -0.0965(4) 0.3989(2) 0.0550(10) Uani 1 1 d . . . H35 H 0.4072 -0.0865 0.3592 0.066 Uiso 1 1 calc R . . C36 C 0.0449(4) -0.2208(3) 0.32866(17) 0.0372(6) Uani 1 1 d . . . C37 C -0.0861(4) -0.1519(4) 0.3530(2) 0.0466(8) Uani 1 1 d . . . H37 H -0.0922 -0.0819 0.3686 0.056 Uiso 1 1 calc R . . C38 C -0.2079(5) -0.1855(5) 0.3544(3) 0.0651(12) Uani 1 1 d . . . H38 H -0.2949 -0.1380 0.3707 0.078 Uiso 1 1 calc R . . C39 C -0.2007(6) -0.2880(6) 0.3321(3) 0.0809(16) Uani 1 1 d . . . H39 H -0.2826 -0.3104 0.3329 0.097 Uiso 1 1 calc R . . C40 C -0.0720(7) -0.3583(6) 0.3083(3) 0.0893(18) Uani 1 1 d . . . H40 H -0.0672 -0.4287 0.2934 0.107 Uiso 1 1 calc R . . C41 C 0.0516(5) -0.3256(4) 0.3063(3) 0.0620(11) Uani 1 1 d . . . H41 H 0.1381 -0.3738 0.2900 0.074 Uiso 1 1 calc R . . C42 C 0.3589(3) -0.3079(3) 0.31499(19) 0.0403(7) Uani 1 1 d . . . C43 C 0.4252(4) -0.3261(3) 0.2544(2) 0.0498(9) Uani 1 1 d . . . H43 H 0.3860 -0.2668 0.2127 0.060 Uiso 1 1 calc R . . C44 C 0.5506(5) -0.4331(4) 0.2556(3) 0.0714(14) Uani 1 1 d . . . H44 H 0.5949 -0.4447 0.2146 0.086 Uiso 1 1 calc R . . C45 C 0.6090(5) -0.5210(4) 0.3162(3) 0.0776(16) Uani 1 1 d . . . H45 H 0.6929 -0.5920 0.3165 0.093 Uiso 1 1 calc R . . C46 C 0.5446(6) -0.5051(4) 0.3763(3) 0.0814(16) Uani 1 1 d . . . H46 H 0.5842 -0.5653 0.4176 0.098 Uiso 1 1 calc R . . C47 C 0.4190(5) -0.3982(4) 0.3760(3) 0.0641(11) Uani 1 1 d . . . H47 H 0.3753 -0.3878 0.4172 0.077 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 Re1 0.02345(5) 0.02356(6) 0.02638(5) -0.01098(4) 0.00376(3) -0.01024(4) P1 0.0302(3) 0.0261(3) 0.0273(3) -0.0089(3) 0.0042(2) -0.0119(3) P2 0.0276(3) 0.0250(3) 0.0303(3) -0.0075(3) 0.0013(2) -0.0099(3) Cl1 0.0300(3) 0.0430(4) 0.0559(5) -0.0211(4) 0.0128(3) -0.0157(3) S1 0.0235(3) 0.0594(5) 0.0631(5) -0.0213(4) 0.0093(3) -0.0132(3) O1 0.082(2) 0.0509(15) 0.0549(15) -0.0318(13) 0.0033(14) -0.0330(14) O2 0.0293(9) 0.0372(11) 0.0357(10) -0.0216(9) 0.0069(8) -0.0151(8) N1 0.0294(12) 0.0379(13) 0.0403(13) -0.0204(11) 0.0067(10) -0.0091(10) N2 0.0238(10) 0.0298(12) 0.0330(11) -0.0087(9) 0.0023(8) -0.0113(9) C1 0.0387(15) 0.0327(15) 0.0322(14) -0.0092(12) 0.0032(11) -0.0133(12) C2 0.0317(13) 0.0274(13) 0.0303(13) -0.0113(10) 0.0033(10) -0.0111(11) C3 0.0222(12) 0.0335(14) 0.0383(14) -0.0100(12) 0.0050(10) -0.0108(11) C4 0.0289(15) 0.056(2) 0.066(2) -0.0147(18) -0.0026(14) -0.0227(15) C5 0.0339(15) 0.0430(17) 0.0479(17) -0.0166(14) -0.0017(12) -0.0201(13) C6 0.0438(16) 0.0326(15) 0.0366(15) -0.0162(12) 0.0022(12) -0.0153(13) C7 0.050(2) 0.063(2) 0.061(2) -0.035(2) 0.0029(17) -0.0256(18) C8 0.069(3) 0.084(3) 0.082(3) -0.041(3) -0.005(2) -0.042(3) C9 0.104(4) 0.077(3) 0.076(3) -0.048(3) -0.002(3) -0.048(3) C10 0.097(4) 0.076(3) 0.075(3) -0.058(3) 0.022(3) -0.037(3) C11 0.063(2) 0.055(2) 0.061(2) -0.0394(19) 0.0178(18) -0.0254(19) C12 0.0386(15) 0.0290(14) 0.0352(14) -0.0106(11) 0.0068(11) -0.0168(12) C13 0.0405(16) 0.0344(16) 0.0515(18) -0.0122(14) -0.0001(14) -0.0173(13) C14 0.052(2) 0.046(2) 0.065(2) -0.0182(18) -0.0025(17) -0.0273(17) C15 0.072(3) 0.0407(19) 0.069(3) -0.0205(18) 0.008(2) -0.0345(19) C16 0.068(3) 0.0272(16) 0.073(3) -0.0069(17) -0.003(2) -0.0192(16) C17 0.053(2) 0.0299(16) 0.055(2) -0.0033(14) -0.0060(16) -0.0165(14) C18 0.0339(14) 0.0417(16) 0.0285(13) -0.0101(12) 0.0069(11) -0.0119(12) C19 0.077(3) 0.051(2) 0.047(2) -0.0216(17) 0.0258(19) -0.025(2) C20 0.090(3) 0.068(3) 0.054(2) -0.031(2) 0.030(2) -0.022(3) C21 0.066(3) 0.089(3) 0.046(2) -0.023(2) 0.0266(19) -0.022(2) C22 0.073(3) 0.083(3) 0.052(2) -0.015(2) 0.031(2) -0.040(3) C23 0.057(2) 0.057(2) 0.0426(18) -0.0145(16) 0.0178(16) -0.0296(18) C24 0.0338(14) 0.0306(14) 0.0311(13) -0.0050(11) 0.0006(11) -0.0122(11) C25 0.0395(16) 0.0366(16) 0.0418(16) -0.0108(13) 0.0023(13) -0.0111(13) C26 0.0376(18) 0.047(2) 0.061(2) -0.0137(17) 0.0031(15) -0.0057(15) C27 0.0409(19) 0.060(2) 0.074(3) -0.006(2) -0.0158(18) -0.0163(18) C28 0.052(2) 0.068(3) 0.053(2) -0.0179(19) -0.0099(17) -0.0235(19) C29 0.0435(17) 0.050(2) 0.0421(17) -0.0161(15) 0.0004(13) -0.0193(15) C30 0.0367(15) 0.0357(15) 0.0303(13) -0.0074(11) -0.0017(11) -0.0149(12) C31 0.061(2) 0.081(3) 0.0411(18) -0.0218(19) 0.0111(16) -0.044(2) C32 0.077(3) 0.104(4) 0.0398(19) -0.029(2) 0.0176(19) -0.052(3) C33 0.085(3) 0.097(4) 0.042(2) -0.026(2) 0.002(2) -0.055(3) C34 0.082(3) 0.123(4) 0.048(2) -0.028(3) 0.005(2) -0.073(3) C35 0.057(2) 0.085(3) 0.0414(18) -0.0191(19) 0.0062(16) -0.045(2) C36 0.0420(16) 0.0358(16) 0.0387(15) -0.0040(12) -0.0002(12) -0.0229(13) C37 0.0427(18) 0.0450(19) 0.057(2) -0.0083(16) 0.0091(15) -0.0246(15) C38 0.050(2) 0.076(3) 0.076(3) -0.007(2) 0.010(2) -0.037(2) C39 0.072(3) 0.100(4) 0.098(4) -0.020(3) 0.011(3) -0.066(3) C40 0.101(4) 0.094(4) 0.118(5) -0.049(4) 0.019(4) -0.075(4) C41 0.070(3) 0.059(3) 0.080(3) -0.032(2) 0.015(2) -0.042(2) C42 0.0340(15) 0.0252(14) 0.061(2) -0.0135(14) -0.0013(13) -0.0084(12) C43 0.0432(18) 0.0388(18) 0.070(2) -0.0298(17) 0.0034(16) -0.0081(15) C44 0.051(2) 0.056(3) 0.110(4) -0.053(3) 0.007(2) -0.003(2) C45 0.048(2) 0.039(2) 0.140(5) -0.044(3) -0.012(3) 0.0036(18) C46 0.069(3) 0.036(2) 0.111(4) 0.000(2) -0.026(3) 0.002(2) C47 0.059(2) 0.040(2) 0.073(3) -0.0011(19) -0.008(2) -0.0024(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C1 1.857(3) . ? Re1 N2 2.087(2) . ? Re1 O2 2.1322(18) . ? Re1 Cl1 2.3891(7) . ? Re1 P2 2.4682(7) . ? Re1 P1 2.4799(7) . ? P1 C24 1.828(3) . ? P1 C18 1.829(3) . ? P1 C12 1.831(3) . ? P2 C36 1.821(3) . ? P2 C30 1.827(3) . ? P2 C42 1.831(3) . ? S1 C4 1.715(4) . ? S1 C3 1.738(3) . ? O1 C1 1.172(4) . ? O2 C2 1.265(3) . ? N1 C2 1.328(4) . ? N1 C3 1.343(4) . ? N2 C3 1.346(4) . ? N2 C5 1.387(4) . ? C2 C6 1.492(4) . ? C4 C5 1.332(5) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.382(5) . ? C6 C11 1.386(5) . ? C7 C8 1.392(5) . ? C7 H7 0.9300 . ? C8 C9 1.360(7) . ? C8 H8 0.9300 . ? C9 C10 1.365(7) . ? C9 H9 0.9300 . ? C10 C11 1.390(5) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.390(4) . ? C12 C17 1.391(4) . ? C13 C14 1.387(5) . ? C13 H13 0.9300 . ? C14 C15 1.367(6) . ? C14 H14 0.9300 . ? C15 C16 1.377(6) . ? C15 H15 0.9300 . ? C16 C17 1.390(5) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.384(5) . ? C18 C23 1.392(5) . ? C19 C20 1.393(5) . ? C19 H19 0.9300 . ? C20 C21 1.366(7) . ? C20 H20 0.9300 . ? C21 C22 1.367(7) . ? C21 H21 0.9300 . ? C22 C23 1.386(5) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C29 1.391(4) . ? C24 C25 1.394(4) . ? C25 C26 1.381(5) . ? C25 H25 0.9300 . ? C26 C27 1.380(6) . ? C26 H26 0.9300 . ? C27 C28 1.369(6) . ? C27 H27 0.9300 . ? C28 C29 1.393(5) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.374(5) . ? C30 C35 1.390(5) . ? C31 C32 1.398(5) . ? C31 H31 0.9300 . ? C32 C33 1.350(6) . ? C32 H32 0.9300 . ? C33 C34 1.371(6) . ? C33 H33 0.9300 . ? C34 C35 1.377(5) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C41 1.387(5) . ? C36 C37 1.389(5) . ? C37 C38 1.384(5) . ? C37 H37 0.9300 . ? C38 C39 1.360(7) . ? C38 H38 0.9300 . ? C39 C40 1.373(8) . ? C39 H39 0.9300 . ? C40 C41 1.393(6) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C43 1.381(5) . ? C42 C47 1.382(5) . ? C43 C44 1.393(5) . ? C43 H43 0.9300 . ? C44 C45 1.363(8) . ? C44 H44 0.9300 . ? C45 C46 1.359(8) . ? C45 H45 0.9300 . ? C46 C47 1.396(6) . ? C46 H46 0.9300 . ? C47 H47 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 C1 Re1 N2 93.08(12) . . ? C1 Re1 O2 176.96(11) . . ? N2 Re1 O2 84.31(8) . . ? C1 Re1 Cl1 97.78(10) . . ? N2 Re1 Cl1 169.13(7) . . ? O2 Re1 Cl1 84.84(6) . . ? C1 Re1 P2 89.30(10) . . ? N2 Re1 P2 89.96(7) . . ? O2 Re1 P2 89.13(6) . . ? Cl1 Re1 P2 90.56(3) . . ? C1 Re1 P1 93.24(10) . . ? N2 Re1 P1 90.25(7) . . ? O2 Re1 P1 88.34(6) . . ? Cl1 Re1 P1 88.75(3) . . ? P2 Re1 P1 177.43(2) . . ? C24 P1 C18 105.20(14) . . ? C24 P1 C12 104.54(14) . . ? C18 P1 C12 101.93(14) . . ? C24 P1 Re1 109.94(10) . . ? C18 P1 Re1 117.15(11) . . ? C12 P1 Re1 116.74(10) . . ? C36 P2 C30 107.23(15) . . ? C36 P2 C42 104.30(15) . . ? C30 P2 C42 101.02(15) . . ? C36 P2 Re1 112.65(10) . . ? C30 P2 Re1 113.50(10) . . ? C42 P2 Re1 116.96(12) . . ? C4 S1 C3 90.76(15) . . ? C2 O2 Re1 130.10(18) . . ? C2 N1 C3 122.3(2) . . ? C3 N2 C5 111.4(2) . . ? C3 N2 Re1 123.95(18) . . ? C5 N2 Re1 124.7(2) . . ? O1 C1 Re1 176.8(3) . . ? O2 C2 N1 127.2(3) . . ? O2 C2 C6 116.0(2) . . ? N1 C2 C6 116.8(2) . . ? N1 C3 N2 132.0(2) . . ? N1 C3 S1 116.4(2) . . ? N2 C3 S1 111.6(2) . . ? C5 C4 S1 110.5(2) . . ? C5 C4 H4 124.8 . . ? S1 C4 H4 124.8 . . ? C4 C5 N2 115.8(3) . . ? C4 C5 H5 122.1 . . ? N2 C5 H5 122.1 . . ? C7 C6 C11 118.7(3) . . ? C7 C6 C2 119.6(3) . . ? C11 C6 C2 121.7(3) . . ? C6 C7 C8 120.1(4) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C9 C8 C7 120.6(4) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 120.1(4) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C9 C10 C11 120.1(4) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C6 C11 C10 120.4(4) . . ? C6 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C13 C12 C17 118.7(3) . . ? C13 C12 P1 118.4(2) . . ? C17 C12 P1 122.7(2) . . ? C14 C13 C12 120.1(3) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C15 C14 C13 120.8(4) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 119.7(3) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C15 C16 C17 120.3(3) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C16 C17 C12 120.2(3) . . ? C16 C17 H17 119.9 . . ? C12 C17 H17 119.9 . . ? C19 C18 C23 118.2(3) . . ? C19 C18 P1 120.8(3) . . ? C23 C18 P1 121.0(3) . . ? C18 C19 C20 120.7(4) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C21 C20 C19 120.2(4) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 119.8(4) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C21 C22 C23 120.6(4) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C22 C23 C18 120.4(4) . . ? C22 C23 H23 119.8 . . ? C18 C23 H23 119.8 . . ? C29 C24 C25 118.8(3) . . ? C29 C24 P1 121.1(2) . . ? C25 C24 P1 119.7(2) . . ? C26 C25 C24 120.6(3) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C27 C26 C25 120.0(4) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C28 C27 C26 120.3(4) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C29 120.2(4) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C24 C29 C28 120.1(3) . . ? C24 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C31 C30 C35 118.6(3) . . ? C31 C30 P2 126.0(3) . . ? C35 C30 P2 115.4(2) . . ? C30 C31 C32 120.1(4) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C33 C32 C31 120.8(4) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C32 C33 C34 119.4(4) . . ? C32 C33 H33 120.3 . . ? C34 C33 H33 120.3 . . ? C33 C34 C35 120.9(4) . . ? C33 C34 H34 119.5 . . ? C35 C34 H34 119.5 . . ? C34 C35 C30 120.1(4) . . ? C34 C35 H35 120.0 . . ? C30 C35 H35 120.0 . . ? C41 C36 C37 118.3(3) . . ? C41 C36 P2 119.9(3) . . ? C37 C36 P2 121.5(3) . . ? C38 C37 C36 121.2(4) . . ? C38 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? C39 C38 C37 120.1(4) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C38 C39 C40 119.8(4) . . ? C38 C39 H39 120.1 . . ? C40 C39 H39 120.1 . . ? C39 C40 C41 120.9(5) . . ? C39 C40 H40 119.6 . . ? C41 C40 H40 119.6 . . ? C36 C41 C40 119.7(4) . . ? C36 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C43 C42 C47 118.6(3) . . ? C43 C42 P2 121.5(3) . . ? C47 C42 P2 119.9(3) . . ? C42 C43 C44 120.1(4) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C45 C44 C43 120.6(5) . . ? C45 C44 H44 119.7 . . ? C43 C44 H44 119.7 . . ? C46 C45 C44 120.1(4) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C47 120.1(5) . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C42 C47 C46 120.6(5) . . ? C42 C47 H47 119.7 . . ? C46 C47 H47 119.7 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.968 _refine_diff_density_min -1.770 _refine_diff_density_rms 0.107 ###END data_(11) _database_code_CSD 179467 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C53 H42 Cl N4 O2 P2 Re S' _chemical_formula_sum 'C53 H42 Cl N4 O2 P2 Re S' _chemical_formula_weight 1082.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Re' 'Re' -1.0185 7.2310 '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' 'O' 'O' 0.0106 0.0060 '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' '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 20.8074(6) _cell_length_b 9.9213(2) _cell_length_c 23.4766(8) _cell_angle_alpha 90.00 _cell_angle_beta 108.7751(11) _cell_angle_gamma 90.00 _cell_volume 4588.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 29480 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 27.88 _exptl_crystal_description 'plate' _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_absorpt_coefficient_mu 2.869 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_T_max 0.94 _exptl_absorpt_process_details ; SORTAV (R.H. Blessing, Acta Crystallogr., 1995, A51, 33) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '\f scans and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29480 _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_av_sigmaI/netI 0.0659 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 27.88 _reflns_number_total 10883 _reflns_number_gt 8217 _reflns_threshold_expression 'I>2sigma(I)' _computing_data_collection 'Kappa CCD server software, 1997' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997' _computing_data_reduction 'Denzo-SMN' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP II (Johnson, 1976)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+13.0693P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10883 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0961 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1209 _refine_ls_wR_factor_gt 0.1038 _refine_ls_goodness_of_fit_ref 1.181 _refine_ls_restrained_S_all 1.181 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.006 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 Re1 Re 0.249145(12) 0.07869(2) -0.014201(11) 0.03462(8) Uani 1 1 d . . . Cl1 Cl 0.32876(9) 0.22130(17) -0.04260(9) 0.0554(4) Uani 1 1 d . . . S1 S 0.15158(10) -0.32416(18) 0.01372(10) 0.0600(5) Uani 1 1 d . . . P1 P 0.16991(8) 0.09928(15) -0.11854(7) 0.0376(4) Uani 1 1 d . . . P2 P 0.32904(8) 0.06146(15) 0.08917(8) 0.0394(4) Uani 1 1 d . . . O1 O 0.2991(2) -0.0718(4) -0.0423(2) 0.0423(10) Uani 1 1 d . . . O2 O 0.0741(3) 0.2400(6) -0.0031(3) 0.0782(17) Uani 1 1 d . . . N1 N 0.1923(2) -0.0862(5) 0.0011(2) 0.0383(11) Uani 1 1 d . . . N2 N 0.2615(3) -0.2735(5) -0.0144(2) 0.0449(13) Uani 1 1 d . . . N3 N 0.2078(3) 0.2005(5) 0.0149(2) 0.0397(12) Uani 1 1 d . . . N4 N 0.1865(3) 0.2890(5) 0.0444(3) 0.0484(14) Uani 1 1 d . . . C1 C 0.1321(3) -0.0730(7) 0.0146(3) 0.0481(16) Uani 1 1 d . . . H1 H 0.1130 0.0103 0.0177 0.058 Uiso 1 1 calc R . . C2 C 0.1037(4) -0.1903(7) 0.0228(3) 0.0561(19) Uani 1 1 d . . . H2 H 0.0637 -0.1976 0.0321 0.067 Uiso 1 1 calc R . . C3 C 0.2089(3) -0.2151(6) -0.0014(3) 0.0433(15) Uani 1 1 d . . . C4 C 0.3021(3) -0.2021(6) -0.0348(3) 0.0399(14) Uani 1 1 d . . . C5 C 0.3554(3) -0.2716(6) -0.0525(3) 0.0481(16) Uani 1 1 d . . . C6 C 0.3667(4) -0.4092(7) -0.0423(4) 0.062(2) Uani 1 1 d . . . H6 H 0.3399 -0.4583 -0.0249 0.074 Uiso 1 1 calc R . . C7 C 0.4173(4) -0.4728(8) -0.0578(5) 0.081(3) Uani 1 1 d . . . H7 H 0.4251 -0.5644 -0.0502 0.097 Uiso 1 1 calc R . . C8 C 0.4563(5) -0.4020(9) -0.0844(5) 0.088(3) Uani 1 1 d . . . H8 H 0.4906 -0.4457 -0.0946 0.105 Uiso 1 1 calc R . . C9 C 0.4453(4) -0.2665(9) -0.0961(5) 0.088(3) Uani 1 1 d . . . H9 H 0.4718 -0.2191 -0.1146 0.105 Uiso 1 1 calc R . . C10 C 0.3947(4) -0.2010(7) -0.0803(4) 0.066(2) Uani 1 1 d . . . H10 H 0.3871 -0.1095 -0.0883 0.079 Uiso 1 1 calc R . . C11 C 0.1182(3) 0.2991(6) 0.0359(3) 0.0471(16) Uani 1 1 d . . . C12 C 0.1020(3) 0.3910(6) 0.0797(3) 0.0423(15) Uani 1 1 d . . . C13 C 0.1493(4) 0.4310(7) 0.1330(3) 0.0536(17) Uani 1 1 d . . . H13 H 0.1944 0.4042 0.1423 0.064 Uiso 1 1 calc R . . C14 C 0.1295(4) 0.5112(8) 0.1726(4) 0.068(2) Uani 1 1 d . . . H14 H 0.1610 0.5355 0.2092 0.082 Uiso 1 1 calc R . . C15 C 0.0642(5) 0.5549(8) 0.1583(4) 0.068(2) Uani 1 1 d . . . H15 H 0.0519 0.6111 0.1848 0.082 Uiso 1 1 calc R . . C16 C 0.0169(4) 0.5177(8) 0.1063(4) 0.067(2) Uani 1 1 d . . . H16 H -0.0275 0.5484 0.0968 0.081 Uiso 1 1 calc R . . C17 C 0.0353(4) 0.4336(7) 0.0673(4) 0.0551(17) Uani 1 1 d . . . H17 H 0.0025 0.4051 0.0321 0.066 Uiso 1 1 calc R . . C18 C 0.1461(3) 0.2714(6) -0.1442(3) 0.0431(15) Uani 1 1 d . . . C19 C 0.1746(3) 0.3835(6) -0.1096(3) 0.0465(16) Uani 1 1 d . . . H19 H 0.2048 0.3716 -0.0710 0.056 Uiso 1 1 calc R . . C20 C 0.1585(4) 0.5121(7) -0.1321(4) 0.059(2) Uani 1 1 d . . . H20 H 0.1784 0.5861 -0.1088 0.070 Uiso 1 1 calc R . . C21 C 0.1136(5) 0.5308(8) -0.1883(4) 0.071(2) Uani 1 1 d . . . H21 H 0.1037 0.6178 -0.2034 0.085 Uiso 1 1 calc R . . C22 C 0.0826(4) 0.4221(8) -0.2231(4) 0.070(2) Uani 1 1 d . . . H22 H 0.0506 0.4358 -0.2608 0.084 Uiso 1 1 calc R . . C23 C 0.0994(4) 0.2932(7) -0.2016(3) 0.0593(19) Uani 1 1 d . . . H23 H 0.0795 0.2198 -0.2255 0.071 Uiso 1 1 calc R . . C24 C 0.0882(3) 0.0172(6) -0.1297(3) 0.0427(15) Uani 1 1 d . . . C25 C 0.0341(3) 0.0873(8) -0.1224(3) 0.0550(17) Uani 1 1 d . . . H25 H 0.0380 0.1791 -0.1140 0.066 Uiso 1 1 calc R . . C26 C -0.0260(4) 0.0214(9) -0.1275(3) 0.063(2) Uani 1 1 d . . . H26 H -0.0618 0.0692 -0.1218 0.075 Uiso 1 1 calc R . . C27 C -0.0335(4) -0.1112(9) -0.1406(4) 0.078(3) Uani 1 1 d . . . H27 H -0.0750 -0.1539 -0.1465 0.094 Uiso 1 1 calc R . . C28 C 0.0210(5) -0.1812(9) -0.1450(5) 0.101(4) Uani 1 1 d . . . H28 H 0.0173 -0.2736 -0.1518 0.121 Uiso 1 1 calc R . . C29 C 0.0817(5) -0.1175(7) -0.1396(5) 0.084(3) Uani 1 1 d . . . H29 H 0.1182 -0.1673 -0.1427 0.100 Uiso 1 1 calc R . . C30 C 0.1973(4) 0.0280(7) -0.1783(3) 0.0504(17) Uani 1 1 d . . . C31 C 0.1526(7) -0.0193(14) -0.2297(5) 0.124(4) Uani 1 1 d . . . H31 H 0.1059 -0.0084 -0.2397 0.149 Uiso 1 1 calc R . . C32 C 0.1842(13) -0.088(2) -0.2672(11) 0.35(2) Uani 1 1 d . . . H32 H 0.1611 -0.1624 -0.2882 0.425 Uiso 1 1 calc R . . C33 C 0.2332(9) -0.063(2) -0.2742(5) 0.189(10) Uani 1 1 d . . . H33 H 0.2398 -0.0669 -0.3115 0.227 Uiso 1 1 calc R . . C34 C 0.2830(10) -0.024(2) -0.2223(10) 0.207(9) Uani 1 1 d . . . H34 H 0.3285 -0.0336 -0.2191 0.248 Uiso 1 1 calc R . . C35 C 0.2647(6) 0.0321(14) -0.1723(6) 0.127(5) Uani 1 1 d . . . H35 H 0.2968 0.0683 -0.1384 0.152 Uiso 1 1 calc R . . C36 C 0.3616(3) 0.2231(6) 0.1258(3) 0.0454(15) Uani 1 1 d . . . C37 C 0.4032(4) 0.2248(8) 0.1847(3) 0.063(2) Uani 1 1 d . . . H37 H 0.4156 0.1440 0.2055 0.075 Uiso 1 1 calc R . . C38 C 0.4268(4) 0.3463(9) 0.2137(4) 0.075(2) Uani 1 1 d . . . H38 H 0.4548 0.3466 0.2536 0.090 Uiso 1 1 calc R . . C39 C 0.4087(5) 0.4650(8) 0.1833(4) 0.074(2) Uani 1 1 d . . . H39 H 0.4240 0.5461 0.2028 0.088 Uiso 1 1 calc R . . C40 C 0.3690(5) 0.4656(8) 0.1253(4) 0.074(2) Uani 1 1 d . . . H40 H 0.3578 0.5470 0.1048 0.089 Uiso 1 1 calc R . . C41 C 0.3444(4) 0.3444(7) 0.0957(4) 0.0573(19) Uani 1 1 d . . . H41 H 0.3166 0.3455 0.0558 0.069 Uiso 1 1 calc R . . C42 C 0.4060(3) -0.0412(6) 0.1036(3) 0.0457(16) Uani 1 1 d . . . C43 C 0.4383(4) -0.0395(7) 0.0603(4) 0.0566(19) Uani 1 1 d . . . H43 H 0.4199 0.0099 0.0251 0.068 Uiso 1 1 calc R . . C44 C 0.4979(4) -0.1113(9) 0.0693(5) 0.075(2) Uani 1 1 d . . . H44 H 0.5191 -0.1110 0.0399 0.090 Uiso 1 1 calc R . . C45 C 0.5257(4) -0.1826(8) 0.1213(5) 0.075(3) Uani 1 1 d . . . H45 H 0.5660 -0.2299 0.1273 0.090 Uiso 1 1 calc R . . C46 C 0.4950(4) -0.1845(8) 0.1640(4) 0.072(2) Uani 1 1 d . . . H46 H 0.5145 -0.2330 0.1992 0.086 Uiso 1 1 calc R . . C47 C 0.4346(4) -0.1148(7) 0.1560(4) 0.0598(19) Uani 1 1 d . . . H47 H 0.4136 -0.1175 0.1855 0.072 Uiso 1 1 calc R . . C48 C 0.2856(3) -0.0081(7) 0.1379(3) 0.0491(17) Uani 1 1 d . . . C49 C 0.2516(4) 0.0718(9) 0.1669(3) 0.063(2) Uani 1 1 d . . . H49 H 0.2547 0.1651 0.1647 0.076 Uiso 1 1 calc R . . C50 C 0.2126(4) 0.0165(12) 0.1994(4) 0.083(3) Uani 1 1 d . . . H50 H 0.1901 0.0720 0.2187 0.099 Uiso 1 1 calc R . . C51 C 0.2079(5) -0.1220(14) 0.2026(4) 0.095(4) Uani 1 1 d . . . H51 H 0.1831 -0.1605 0.2251 0.114 Uiso 1 1 calc R . . C52 C 0.2393(5) -0.2017(12) 0.1730(5) 0.097(4) Uani 1 1 d . . . H52 H 0.2347 -0.2948 0.1746 0.117 Uiso 1 1 calc R . . C53 C 0.2779(4) -0.1492(8) 0.1407(3) 0.065(2) Uani 1 1 d . . . H53 H 0.2989 -0.2063 0.1207 0.078 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 Re1 0.03364(13) 0.03368(12) 0.03943(14) 0.00106(11) 0.01581(10) -0.00263(10) Cl1 0.0511(10) 0.0469(9) 0.0778(13) 0.0095(8) 0.0341(9) -0.0060(7) S1 0.0677(12) 0.0480(10) 0.0770(14) -0.0044(9) 0.0410(11) -0.0227(8) P1 0.0392(9) 0.0366(8) 0.0402(9) 0.0001(7) 0.0169(7) -0.0003(6) P2 0.0363(8) 0.0384(8) 0.0431(10) 0.0003(7) 0.0122(7) -0.0051(6) O1 0.045(2) 0.036(2) 0.053(3) 0.0028(19) 0.026(2) 0.0008(18) O2 0.050(3) 0.093(4) 0.086(4) -0.041(3) 0.014(3) 0.001(3) N1 0.039(3) 0.042(3) 0.037(3) -0.002(2) 0.017(2) -0.009(2) N2 0.047(3) 0.036(3) 0.056(3) 0.000(2) 0.022(3) -0.008(2) N3 0.040(3) 0.037(3) 0.043(3) -0.005(2) 0.013(2) -0.005(2) N4 0.045(3) 0.046(3) 0.058(4) -0.013(3) 0.023(3) 0.000(2) C1 0.045(4) 0.053(4) 0.053(4) -0.003(3) 0.026(3) -0.008(3) C2 0.055(4) 0.061(4) 0.065(5) -0.009(4) 0.037(4) -0.017(3) C3 0.051(4) 0.040(3) 0.043(4) -0.001(3) 0.020(3) -0.014(3) C4 0.034(3) 0.036(3) 0.050(4) -0.003(3) 0.013(3) -0.005(2) C5 0.044(4) 0.040(3) 0.066(5) -0.005(3) 0.025(3) -0.003(3) C6 0.059(5) 0.045(4) 0.086(6) -0.005(4) 0.030(4) 0.001(3) C7 0.074(6) 0.043(4) 0.139(9) -0.007(5) 0.052(6) 0.008(4) C8 0.065(6) 0.066(6) 0.145(10) -0.019(6) 0.053(6) 0.009(4) C9 0.072(6) 0.071(6) 0.144(9) -0.010(6) 0.070(6) -0.004(5) C10 0.059(5) 0.048(4) 0.105(7) 0.002(4) 0.047(5) 0.000(3) C11 0.047(4) 0.045(4) 0.051(4) -0.007(3) 0.018(3) 0.002(3) C12 0.049(4) 0.040(3) 0.045(4) 0.000(3) 0.024(3) -0.002(3) C13 0.051(4) 0.057(4) 0.051(4) -0.007(3) 0.014(3) -0.002(3) C14 0.075(6) 0.069(5) 0.063(5) -0.023(4) 0.024(5) -0.007(4) C15 0.079(6) 0.065(5) 0.071(6) -0.017(4) 0.038(5) 0.003(4) C16 0.058(5) 0.073(5) 0.080(6) -0.010(4) 0.034(5) 0.008(4) C17 0.046(4) 0.058(4) 0.062(5) -0.006(4) 0.018(3) -0.002(3) C18 0.044(4) 0.041(3) 0.045(4) 0.005(3) 0.016(3) 0.001(3) C19 0.051(4) 0.044(3) 0.048(4) 0.001(3) 0.021(3) 0.004(3) C20 0.075(5) 0.037(4) 0.069(5) 0.001(3) 0.029(4) 0.008(3) C21 0.095(7) 0.046(4) 0.069(6) 0.014(4) 0.020(5) 0.019(4) C22 0.078(6) 0.056(5) 0.061(5) 0.018(4) 0.003(4) 0.009(4) C23 0.066(5) 0.048(4) 0.056(5) 0.004(3) 0.009(4) -0.001(3) C24 0.041(4) 0.044(3) 0.042(4) 0.005(3) 0.012(3) -0.004(3) C25 0.044(4) 0.065(4) 0.058(5) -0.005(4) 0.021(3) -0.002(3) C26 0.043(4) 0.091(6) 0.058(5) -0.001(4) 0.021(4) -0.006(4) C27 0.057(5) 0.080(6) 0.097(7) 0.020(5) 0.025(5) -0.018(4) C28 0.095(8) 0.057(5) 0.159(11) -0.012(6) 0.055(7) -0.032(5) C29 0.077(6) 0.039(4) 0.153(10) -0.008(5) 0.062(6) -0.009(4) C30 0.045(4) 0.061(4) 0.048(4) -0.009(3) 0.018(3) -0.003(3) C31 0.111(9) 0.163(12) 0.096(9) -0.036(8) 0.031(8) 0.003(9) C32 0.43(3) 0.42(3) 0.38(3) -0.35(3) 0.37(3) -0.33(3) C33 0.161(14) 0.38(3) 0.048(7) -0.058(12) 0.064(8) -0.093(16) C34 0.186(18) 0.31(2) 0.20(2) 0.006(18) 0.166(18) 0.047(17) C35 0.113(10) 0.179(13) 0.109(10) -0.044(9) 0.064(8) -0.032(9) C36 0.042(4) 0.050(4) 0.046(4) -0.006(3) 0.015(3) -0.008(3) C37 0.070(5) 0.058(4) 0.052(5) -0.005(4) 0.009(4) 0.001(4) C38 0.079(6) 0.074(6) 0.065(6) -0.029(5) 0.015(5) -0.013(5) C39 0.084(6) 0.055(5) 0.084(7) -0.028(5) 0.030(5) -0.021(4) C40 0.080(6) 0.048(4) 0.091(7) -0.012(4) 0.024(5) -0.011(4) C41 0.059(5) 0.050(4) 0.060(5) -0.001(3) 0.014(4) -0.011(3) C42 0.040(4) 0.039(3) 0.053(4) 0.002(3) 0.007(3) -0.005(3) C43 0.043(4) 0.055(4) 0.074(5) 0.008(4) 0.021(4) 0.002(3) C44 0.049(5) 0.084(6) 0.096(7) 0.005(5) 0.029(5) 0.010(4) C45 0.053(5) 0.064(5) 0.102(8) -0.012(5) 0.016(5) 0.009(4) C46 0.063(5) 0.055(5) 0.077(6) 0.007(4) -0.005(5) 0.014(4) C47 0.060(5) 0.056(4) 0.055(5) 0.001(3) 0.006(4) 0.000(3) C48 0.040(4) 0.066(4) 0.038(4) 0.008(3) 0.007(3) -0.011(3) C49 0.041(4) 0.091(6) 0.055(5) 0.016(4) 0.012(3) -0.002(4) C50 0.051(5) 0.147(9) 0.054(5) -0.003(6) 0.022(4) -0.013(6) C51 0.057(6) 0.167(11) 0.056(6) 0.025(6) 0.013(5) -0.047(6) C52 0.094(8) 0.114(8) 0.078(7) 0.029(6) 0.021(6) -0.049(7) C53 0.072(5) 0.065(5) 0.056(5) 0.010(4) 0.017(4) -0.026(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 N3 1.744(5) . ? Re1 O1 2.045(4) . ? Re1 N1 2.116(5) . ? Re1 Cl1 2.4292(15) . ? Re1 P2 2.4668(17) . ? Re1 P1 2.4819(17) . ? S1 C2 1.715(7) . ? S1 C3 1.729(6) . ? P1 C30 1.818(7) . ? P1 C24 1.826(6) . ? P1 C18 1.825(6) . ? P2 C48 1.808(7) . ? P2 C42 1.834(7) . ? P2 C36 1.842(6) . ? O1 C4 1.304(7) . ? O2 C11 1.218(8) . ? N1 C3 1.330(8) . ? N1 C1 1.394(8) . ? N2 C4 1.305(7) . ? N2 C3 1.358(8) . ? N3 N4 1.284(7) . ? N4 C11 1.374(8) . ? C1 C2 1.346(9) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C4 C5 1.475(9) . ? C5 C10 1.389(9) . ? C5 C6 1.392(9) . ? C6 C7 1.373(10) . ? C6 H6 0.9300 . ? C7 C8 1.365(12) . ? C7 H7 0.9300 . ? C8 C9 1.377(12) . ? C8 H8 0.9300 . ? C9 C10 1.386(10) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.491(9) . ? C12 C13 1.379(9) . ? C12 C17 1.388(9) . ? C13 C14 1.384(10) . ? C13 H13 0.9300 . ? C14 C15 1.362(11) . ? C14 H14 0.9300 . ? C15 C16 1.349(11) . ? C15 H15 0.9300 . ? C16 C17 1.381(10) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.392(9) . ? C18 C23 1.402(9) . ? C19 C20 1.380(9) . ? C19 H19 0.9300 . ? C20 C21 1.363(11) . ? C20 H20 0.9300 . ? C21 C22 1.382(11) . ? C21 H21 0.9300 . ? C22 C23 1.378(9) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C29 1.356(9) . ? C24 C25 1.381(9) . ? C25 C26 1.381(10) . ? C25 H25 0.9300 . ? C26 C27 1.349(11) . ? C26 H26 0.9300 . ? C27 C28 1.362(13) . ? C27 H27 0.9300 . ? C28 C29 1.380(11) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.349(13) . ? C30 C35 1.364(13) . ? C31 C32 1.430(18) . ? C31 H31 0.9300 . ? C32 C33 1.11(2) . ? C32 H32 0.9300 . ? C33 C34 1.38(2) . ? C33 H33 0.9300 . ? C34 C35 1.457(18) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C37 1.376(10) . ? C36 C41 1.383(9) . ? C37 C38 1.394(10) . ? C37 H37 0.9300 . ? C38 C39 1.365(12) . ? C38 H38 0.9300 . ? C39 C40 1.346(12) . ? C39 H39 0.9300 . ? C40 C41 1.401(10) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C43 1.388(10) . ? C42 C47 1.390(10) . ? C43 C44 1.386(10) . ? C43 H43 0.9300 . ? C44 C45 1.367(12) . ? C44 H44 0.9300 . ? C45 C46 1.352(12) . ? C45 H45 0.9300 . ? C46 C47 1.393(11) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C48 C49 1.381(10) . ? C48 C53 1.412(10) . ? C49 C50 1.392(11) . ? C49 H49 0.9300 . ? C50 C51 1.382(15) . ? C50 H50 0.9300 . ? C51 C52 1.352(15) . ? C51 H51 0.9300 . ? C52 C53 1.372(12) . ? C52 H52 0.9300 . ? C53 H53 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 N3 Re1 O1 175.7(2) . . ? N3 Re1 N1 95.5(2) . . ? O1 Re1 N1 81.96(17) . . ? N3 Re1 Cl1 99.75(16) . . ? O1 Re1 Cl1 82.79(12) . . ? N1 Re1 Cl1 164.71(14) . . ? N3 Re1 P2 85.64(17) . . ? O1 Re1 P2 90.85(13) . . ? N1 Re1 P2 90.90(14) . . ? Cl1 Re1 P2 90.41(6) . . ? N3 Re1 P1 94.29(17) . . ? O1 Re1 P1 89.27(13) . . ? N1 Re1 P1 90.08(14) . . ? Cl1 Re1 P1 88.64(6) . . ? P2 Re1 P1 179.02(5) . . ? C2 S1 C3 90.4(3) . . ? C30 P1 C24 103.0(3) . . ? C30 P1 C18 103.2(3) . . ? C24 P1 C18 103.2(3) . . ? C30 P1 Re1 117.1(2) . . ? C24 P1 Re1 113.4(2) . . ? C18 P1 Re1 115.2(2) . . ? C48 P2 C42 104.8(3) . . ? C48 P2 C36 102.8(3) . . ? C42 P2 C36 103.2(3) . . ? C48 P2 Re1 109.5(2) . . ? C42 P2 Re1 119.5(2) . . ? C36 P2 Re1 115.4(2) . . ? C4 O1 Re1 133.5(4) . . ? C3 N1 C1 111.3(5) . . ? C3 N1 Re1 124.7(4) . . ? C1 N1 Re1 123.9(4) . . ? C4 N2 C3 121.0(5) . . ? N4 N3 Re1 170.1(5) . . ? N3 N4 C11 119.6(5) . . ? C2 C1 N1 114.8(6) . . ? C2 C1 H1 122.6 . . ? N1 C1 H1 122.6 . . ? C1 C2 S1 110.6(5) . . ? C1 C2 H2 124.7 . . ? S1 C2 H2 124.7 . . ? N1 C3 N2 131.2(5) . . ? N1 C3 S1 112.8(5) . . ? N2 C3 S1 116.0(4) . . ? O1 C4 N2 125.3(6) . . ? O1 C4 C5 115.7(5) . . ? N2 C4 C5 119.0(5) . . ? C10 C5 C6 118.9(6) . . ? C10 C5 C4 120.4(6) . . ? C6 C5 C4 120.7(6) . . ? C7 C6 C5 120.4(7) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C8 C7 C6 120.2(8) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C7 C8 C9 120.6(8) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C8 C9 C10 119.7(8) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C9 C10 C5 120.1(7) . . ? C9 C10 H10 119.9 . . ? C5 C10 H10 119.9 . . ? O2 C11 N4 124.6(6) . . ? O2 C11 C12 122.0(6) . . ? N4 C11 C12 113.4(6) . . ? C13 C12 C17 118.5(6) . . ? C13 C12 C11 123.1(6) . . ? C17 C12 C11 118.3(6) . . ? C12 C13 C14 119.7(7) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C15 C14 C13 120.5(8) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C16 C15 C14 120.9(8) . . ? C16 C15 H15 119.5 . . ? C14 C15 H15 119.5 . . ? C15 C16 C17 119.3(8) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C16 C17 C12 121.1(7) . . ? C16 C17 H17 119.4 . . ? C12 C17 H17 119.4 . . ? C19 C18 C23 118.1(6) . . ? C19 C18 P1 122.4(5) . . ? C23 C18 P1 119.5(5) . . ? C20 C19 C18 120.7(7) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C21 C20 C19 120.2(7) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 120.7(7) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C23 C22 C21 119.5(7) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 C18 120.8(7) . . ? C22 C23 H23 119.6 . . ? C18 C23 H23 119.6 . . ? C29 C24 C25 118.5(7) . . ? C29 C24 P1 120.1(6) . . ? C25 C24 P1 121.1(5) . . ? C26 C25 C24 120.1(7) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C27 C26 C25 121.2(8) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C26 C27 C28 118.4(8) . . ? C26 C27 H27 120.8 . . ? C28 C27 H27 120.8 . . ? C27 C28 C29 121.3(8) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C24 C29 C28 120.4(8) . . ? C24 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C31 C30 C35 119.5(9) . . ? C31 C30 P1 121.9(7) . . ? C35 C30 P1 118.4(7) . . ? C30 C31 C32 113.4(14) . . ? C30 C31 H31 123.3 . . ? C32 C31 H31 123.3 . . ? C33 C32 C31 127.3(17) . . ? C33 C32 H32 116.4 . . ? C31 C32 H32 116.3 . . ? C32 C33 C34 113.5(15) . . ? C32 C33 H33 123.3 . . ? C34 C33 H33 123.2 . . ? C33 C34 C35 120.1(15) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 119.8 . . ? C30 C35 C34 115.7(13) . . ? C30 C35 H35 122.1 . . ? C34 C35 H35 122.2 . . ? C37 C36 C41 118.6(6) . . ? C37 C36 P2 119.8(5) . . ? C41 C36 P2 121.6(5) . . ? C36 C37 C38 120.7(8) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? C39 C38 C37 119.7(8) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? C40 C39 C38 120.6(8) . . ? C40 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? C39 C40 C41 120.3(8) . . ? C39 C40 H40 119.8 . . ? C41 C40 H40 119.8 . . ? C36 C41 C40 120.0(7) . . ? C36 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C43 C42 C47 119.0(7) . . ? C43 C42 P2 117.3(5) . . ? C47 C42 P2 123.7(6) . . ? C44 C43 C42 120.2(8) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C45 C44 C43 120.2(9) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? C46 C45 C44 120.3(8) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C45 C46 C47 121.0(8) . . ? C45 C46 H46 119.5 . . ? C47 C46 H46 119.5 . . ? C46 C47 C42 119.3(8) . . ? C46 C47 H47 120.3 . . ? C42 C47 H47 120.3 . . ? C49 C48 C53 117.5(7) . . ? C49 C48 P2 122.2(6) . . ? C53 C48 P2 119.7(6) . . ? C48 C49 C50 121.7(9) . . ? C48 C49 H49 119.2 . . ? C50 C49 H49 119.2 . . ? C51 C50 C49 119.1(10) . . ? C51 C50 H50 120.5 . . ? C49 C50 H50 120.5 . . ? C52 C51 C50 120.0(9) . . ? C52 C51 H51 120.0 . . ? C50 C51 H51 120.0 . . ? C51 C52 C53 121.8(10) . . ? C51 C52 H52 119.1 . . ? C53 C52 H52 119.1 . . ? C52 C53 C48 119.9(9) . . ? C52 C53 H53 120.1 . . ? C48 C53 H53 120.1 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.334 _refine_diff_density_min -0.924 _refine_diff_density_rms 0.122 ###END data_(12) _database_code_CSD 179468 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H34 N6 O3 P Re S2' _chemical_formula_sum 'C45 H34 N6 O3 P Re S2' _chemical_formula_weight 988.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Re' 'Re' -1.0185 7.2310 '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' 'O' 'O' 0.0106 0.0060 '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' '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' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.4175(6) _cell_length_b 21.6210(18) _cell_length_c 18.4750(12) _cell_angle_alpha 90.00 _cell_angle_beta 98.805(5) _cell_angle_gamma 90.00 _cell_volume 4112.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 17191 _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 25.08 _exptl_crystal_description 'plate' _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.014 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 3.145 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.792 _exptl_absorpt_correction_T_max 0.955 _exptl_absorpt_process_details ; SORTAV (R.H. Blessing, Acta Crystallogr., 1995, A51, 33) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '\f scan plus \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17191 _diffrn_reflns_av_R_equivalents 0.048 _diffrn_reflns_av_sigmaI/netI 0.0574 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 25.08 _reflns_number_total 6345 _reflns_number_gt 4968 _reflns_threshold_expression 'I>2sigma(I)' _computing_data_collection 'Kappa-CCD Software (Nonius, 1997)' _computing_cell_refinement 'DENZO-SMN (Otwinowski, Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski, Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP II(Johnson, 1976)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+30.7241P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6345 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0923 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1435 _refine_ls_wR_factor_gt 0.1309 _refine_ls_goodness_of_fit_ref 1.184 _refine_ls_restrained_S_all 1.184 _refine_ls_shift/su_max 0.014 _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 Re1 Re 0.43037(4) 0.16247(2) 0.14487(2) 0.04785(16) Uani 1 1 d . . . S1 S 0.5883(4) 0.2812(2) 0.34292(17) 0.0924(14) Uani 1 1 d . . . S2 S 0.8175(3) 0.0583(2) 0.14647(17) 0.0743(11) Uani 1 1 d . . . P1 P 0.2329(2) 0.22021(16) 0.11083(13) 0.0465(7) Uani 1 1 d . . . O1 O 0.5389(6) 0.2288(4) 0.1065(4) 0.056(2) Uani 1 1 d . . . O2 O 0.4192(6) 0.1277(4) 0.0414(4) 0.053(2) Uani 1 1 d . . . O3 O 0.1828(9) 0.0079(6) 0.1492(5) 0.092(3) Uani 1 1 d . . . N1 N 0.4771(7) 0.2089(5) 0.2445(4) 0.054(3) Uani 1 1 d . . . N2 N 0.6297(10) 0.2869(6) 0.2063(5) 0.072(3) Uani 1 1 d . . . N3 N 0.6108(7) 0.1143(5) 0.1676(4) 0.049(2) Uani 1 1 d . . . N4 N 0.6202(7) 0.0798(5) 0.0425(4) 0.055(3) Uani 1 1 d . . . N5 N 0.3355(7) 0.1093(4) 0.1851(4) 0.041(2) Uani 1 1 d . . . N6 N 0.2712(9) 0.0846(6) 0.2313(6) 0.069(3) Uani 1 1 d . . . C1 C 0.4336(11) 0.1901(7) 0.3089(5) 0.059(3) Uani 1 1 d . . . H1 H 0.3767 0.1570 0.3089 0.071 Uiso 1 1 calc R . . C2 C 0.4791(11) 0.2234(7) 0.3749(6) 0.074(4) Uani 1 1 d . . . H2 H 0.4589 0.2175 0.4217 0.089 Uiso 1 1 calc R . . C3 C 0.5626(11) 0.2560(7) 0.2553(6) 0.065(4) Uani 1 1 d . . . C4 C 0.6132(10) 0.2722(7) 0.1339(6) 0.056(3) Uani 1 1 d . . . C5 C 0.6849(11) 0.3057(7) 0.0870(6) 0.064(3) Uani 1 1 d . . . C6 C 0.7813(13) 0.3493(8) 0.1167(8) 0.084(5) Uani 1 1 d . . . H6 H 0.7994 0.3542 0.1672 0.100 Uiso 1 1 calc R . . C7 C 0.8475(16) 0.3840(10) 0.0736(10) 0.106(6) Uani 1 1 d . . . H7 H 0.9114 0.4117 0.0937 0.127 Uiso 1 1 calc R . . C8 C 0.8148(17) 0.3761(10) -0.0053(9) 0.099(5) Uani 1 1 d . . . H8 H 0.8550 0.4003 -0.0369 0.118 Uiso 1 1 calc R . . C9 C 0.7290(14) 0.3351(10) -0.0310(8) 0.095(6) Uani 1 1 d . . . H9 H 0.7109 0.3303 -0.0816 0.114 Uiso 1 1 calc R . . C10 C 0.6599(12) 0.2964(9) 0.0134(7) 0.084(5) Uani 1 1 d . . . H10 H 0.6012 0.2665 -0.0072 0.100 Uiso 1 1 calc R . . C11 C 0.6920(9) 0.1112(7) 0.2348(6) 0.061(3) Uani 1 1 d . . . H11 H 0.6698 0.1276 0.2778 0.073 Uiso 1 1 calc R . . C12 C 0.8030(11) 0.0830(8) 0.2320(6) 0.075(4) Uani 1 1 d . . . H12 H 0.8667 0.0771 0.2726 0.090 Uiso 1 1 calc R . . C13 C 0.6650(8) 0.0884(7) 0.1155(5) 0.056(3) Uani 1 1 d . . . C14 C 0.5041(9) 0.0980(6) 0.0120(5) 0.045(3) Uani 1 1 d . . . C15 C 0.4672(9) 0.0837(6) -0.0672(5) 0.050(3) Uani 1 1 d . . . C16 C 0.5412(10) 0.0462(6) -0.1043(6) 0.057(3) Uani 1 1 d . . . H16 H 0.6170 0.0288 -0.0795 0.068 Uiso 1 1 calc R . . C17 C 0.5045(12) 0.0340(7) -0.1779(6) 0.069(4) Uani 1 1 d . . . H17 H 0.5577 0.0102 -0.2029 0.082 Uiso 1 1 calc R . . C18 C 0.3906(13) 0.0568(8) -0.2137(6) 0.080(5) Uani 1 1 d . . . H18 H 0.3634 0.0471 -0.2627 0.096 Uiso 1 1 calc R . . C19 C 0.3165(13) 0.0942(8) -0.1771(6) 0.082(5) Uani 1 1 d . . . H19 H 0.2401 0.1111 -0.2019 0.098 Uiso 1 1 calc R . . C20 C 0.3535(10) 0.1073(7) -0.1037(5) 0.063(4) Uani 1 1 d . . . H20 H 0.3014 0.1322 -0.0791 0.075 Uiso 1 1 calc R . . C21 C 0.1906(11) 0.0290(8) 0.2098(7) 0.073(4) Uani 1 1 d . . . C22 C 0.1261(10) 0.0078(7) 0.2677(6) 0.059(3) Uani 1 1 d . . . C23 C 0.0557(11) -0.0486(8) 0.2579(8) 0.075(4) Uani 1 1 d . . . H23 H 0.0524 -0.0707 0.2144 0.090 Uiso 1 1 calc R . . C24 C -0.0063(15) -0.0700(9) 0.3117(9) 0.097(5) Uani 1 1 d . . . H24 H -0.0549 -0.1061 0.3036 0.117 Uiso 1 1 calc R . . C25 C -0.0009(16) -0.0411(12) 0.3773(9) 0.117(7) Uani 1 1 d . . . H25 H -0.0408 -0.0578 0.4146 0.140 Uiso 1 1 calc R . . C26 C 0.0686(16) 0.0158(10) 0.3865(9) 0.107(6) Uani 1 1 d . . . H26 H 0.0683 0.0390 0.4288 0.128 Uiso 1 1 calc R . . C27 C 0.1347(15) 0.0358(10) 0.3338(7) 0.099(6) Uani 1 1 d . . . H27 H 0.1882 0.0702 0.3432 0.119 Uiso 1 1 calc R . . C28 C 0.2475(9) 0.2864(6) 0.0530(6) 0.052(3) Uani 1 1 d . . . C29 C 0.3167(10) 0.2819(8) -0.0034(6) 0.068(4) Uani 1 1 d . . . H29 H 0.3585 0.2449 -0.0104 0.081 Uiso 1 1 calc R . . C30 C 0.3269(13) 0.3307(9) -0.0508(7) 0.082(5) Uani 1 1 d . . . H30 H 0.3749 0.3256 -0.0889 0.099 Uiso 1 1 calc R . . C31 C 0.2675(15) 0.3868(9) -0.0427(9) 0.089(5) Uani 1 1 d . . . H31 H 0.2758 0.4199 -0.0737 0.106 Uiso 1 1 calc R . . C32 C 0.1954(15) 0.3912(9) 0.0134(9) 0.093(5) Uani 1 1 d . . . H32 H 0.1554 0.4286 0.0212 0.111 Uiso 1 1 calc R . . C33 C 0.1809(15) 0.3426(10) 0.0580(11) 0.112(6) Uani 1 1 d . . . H33 H 0.1256 0.3464 0.0927 0.134 Uiso 1 1 calc R . . C34 C 0.1671(9) 0.2490(7) 0.1894(5) 0.056(3) Uani 1 1 d . . . C35 C 0.0659(12) 0.2187(8) 0.2153(6) 0.073(4) Uani 1 1 d . . . H35 H 0.0269 0.1845 0.1906 0.087 Uiso 1 1 calc R . . C36 C 0.0236(17) 0.2402(11) 0.2785(8) 0.107(7) Uani 1 1 d . . . H36 H -0.0452 0.2206 0.2959 0.129 Uiso 1 1 calc R . . C37 C 0.083(2) 0.2904(12) 0.3158(8) 0.120(8) Uani 1 1 d . . . H37 H 0.0540 0.3043 0.3581 0.143 Uiso 1 1 calc R . . C38 C 0.1837(17) 0.3197(10) 0.2910(8) 0.100(6) Uani 1 1 d . . . H38 H 0.2231 0.3538 0.3158 0.120 Uiso 1 1 calc R . . C39 C 0.2255(12) 0.2982(8) 0.2294(6) 0.076(4) Uani 1 1 d . . . H39 H 0.2963 0.3173 0.2136 0.091 Uiso 1 1 calc R . . C40 C 0.1004(9) 0.1776(6) 0.0574(5) 0.048(3) Uani 1 1 d . . . C41 C -0.0233(9) 0.2032(6) 0.0405(5) 0.053(3) Uani 1 1 d . . . H41 H -0.0403 0.2424 0.0577 0.063 Uiso 1 1 calc R . . C42 C -0.1219(10) 0.1695(8) -0.0025(6) 0.068(4) Uani 1 1 d . . . H42 H -0.2048 0.1864 -0.0128 0.082 Uiso 1 1 calc R . . C43 C -0.0996(11) 0.1140(7) -0.0288(6) 0.065(4) Uani 1 1 d . . . H43 H -0.1661 0.0927 -0.0579 0.078 Uiso 1 1 calc R . . C44 C 0.0220(10) 0.0879(7) -0.0128(6) 0.060(3) Uani 1 1 d . . . H44 H 0.0379 0.0492 -0.0315 0.073 Uiso 1 1 calc R . . C45 C 0.1209(10) 0.1192(7) 0.0312(6) 0.060(3) Uani 1 1 d . . . H45 H 0.2020 0.1007 0.0432 0.072 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 Re1 0.0393(2) 0.0623(3) 0.0405(2) -0.0014(2) 0.00151(14) 0.0061(2) S1 0.112(3) 0.110(4) 0.0533(18) -0.0171(19) 0.0061(17) -0.038(3) S2 0.0466(15) 0.105(3) 0.0692(18) 0.0112(18) 0.0012(13) 0.0251(17) P1 0.0391(12) 0.056(2) 0.0429(13) -0.0048(12) 0.0023(10) 0.0030(12) O1 0.045(4) 0.063(7) 0.056(4) 0.011(4) -0.003(3) -0.004(4) O2 0.041(3) 0.060(6) 0.057(4) -0.010(4) 0.006(3) 0.008(4) O3 0.100(7) 0.084(10) 0.092(6) -0.017(6) 0.014(5) -0.024(6) N1 0.040(4) 0.068(8) 0.053(5) -0.003(5) 0.005(4) -0.006(5) N2 0.077(6) 0.082(10) 0.058(6) 0.005(5) 0.015(5) -0.018(6) N3 0.043(4) 0.058(8) 0.045(4) 0.002(4) 0.002(4) -0.004(4) N4 0.041(4) 0.084(9) 0.041(4) 0.006(4) 0.008(4) 0.011(5) N5 0.040(4) 0.052(7) 0.033(4) -0.004(4) 0.013(3) 0.004(4) N6 0.064(6) 0.061(9) 0.086(7) 0.000(6) 0.020(5) 0.006(6) C1 0.065(6) 0.069(10) 0.043(5) 0.009(5) 0.009(5) 0.001(6) C2 0.066(7) 0.078(12) 0.069(7) -0.037(7) -0.023(6) -0.004(7) C3 0.054(6) 0.079(12) 0.058(6) 0.002(6) -0.002(5) -0.001(7) C4 0.048(6) 0.059(10) 0.062(6) -0.011(6) 0.011(5) 0.002(6) C5 0.059(7) 0.062(11) 0.072(7) -0.002(6) 0.012(6) -0.008(6) C6 0.085(9) 0.079(14) 0.090(9) -0.022(8) 0.020(7) -0.015(8) C7 0.099(11) 0.097(18) 0.128(14) 0.022(11) 0.038(10) 0.000(10) C8 0.108(12) 0.093(17) 0.103(12) 0.029(10) 0.039(10) 0.008(11) C9 0.076(9) 0.135(19) 0.074(8) 0.023(10) 0.008(7) -0.016(10) C10 0.060(7) 0.123(16) 0.070(8) 0.034(8) 0.019(6) 0.036(8) C11 0.042(6) 0.072(11) 0.062(6) 0.008(6) -0.010(5) 0.011(6) C12 0.054(7) 0.106(14) 0.061(7) 0.009(7) -0.006(5) 0.011(7) C13 0.029(5) 0.083(11) 0.054(6) 0.011(6) 0.004(4) 0.003(5) C14 0.039(5) 0.050(8) 0.047(5) 0.007(5) 0.008(4) -0.002(5) C15 0.042(5) 0.066(9) 0.044(5) -0.001(5) 0.006(4) 0.003(5) C16 0.049(6) 0.063(10) 0.061(6) -0.002(6) 0.015(5) 0.005(6) C17 0.078(8) 0.075(12) 0.056(6) -0.009(6) 0.018(6) 0.013(7) C18 0.090(9) 0.108(15) 0.039(6) -0.003(7) 0.002(6) 0.024(9) C19 0.081(8) 0.096(15) 0.063(7) -0.012(7) -0.008(6) 0.028(8) C20 0.062(7) 0.078(11) 0.046(6) -0.009(6) 0.000(5) 0.014(6) C21 0.055(7) 0.089(14) 0.076(8) 0.011(8) 0.014(6) 0.011(7) C22 0.057(6) 0.041(9) 0.078(8) 0.004(6) 0.005(5) -0.004(6) C23 0.059(7) 0.070(12) 0.092(9) 0.001(8) -0.001(6) -0.009(7) C24 0.103(11) 0.074(15) 0.107(12) 0.018(10) -0.005(9) -0.026(10) C25 0.104(12) 0.15(2) 0.094(11) 0.020(12) -0.005(9) -0.033(13) C26 0.110(12) 0.102(18) 0.102(11) -0.009(10) -0.002(9) -0.048(12) C27 0.102(11) 0.123(19) 0.070(9) 0.005(9) 0.003(8) -0.038(11) C28 0.039(5) 0.056(9) 0.060(6) -0.015(6) 0.006(4) -0.003(5) C29 0.057(6) 0.092(13) 0.053(6) 0.005(7) 0.003(5) 0.001(7) C30 0.079(8) 0.102(16) 0.068(8) 0.026(8) 0.015(6) -0.001(9) C31 0.091(10) 0.069(15) 0.103(11) 0.022(9) 0.003(8) -0.013(9) C32 0.100(11) 0.051(13) 0.122(13) 0.009(9) 0.002(10) 0.002(9) C33 0.087(10) 0.077(15) 0.183(18) 0.028(13) 0.055(11) 0.001(10) C34 0.046(5) 0.076(11) 0.044(5) -0.010(5) 0.001(4) 0.015(6) C35 0.079(8) 0.089(13) 0.053(6) -0.001(7) 0.018(6) 0.006(8) C36 0.121(13) 0.14(2) 0.067(9) 0.022(10) 0.045(9) 0.032(13) C37 0.151(17) 0.15(2) 0.062(9) -0.028(11) 0.026(10) 0.050(16) C38 0.106(12) 0.115(19) 0.072(9) -0.030(9) -0.009(8) 0.034(11) C39 0.067(7) 0.092(14) 0.063(7) -0.024(7) -0.007(6) 0.017(8) C40 0.051(5) 0.053(9) 0.039(5) 0.000(5) 0.007(4) 0.000(5) C41 0.044(5) 0.057(9) 0.054(6) 0.000(5) -0.002(4) 0.012(5) C42 0.037(5) 0.084(13) 0.077(7) 0.004(7) -0.011(5) 0.003(6) C43 0.052(6) 0.074(12) 0.063(7) 0.000(7) -0.010(5) -0.016(6) C44 0.064(7) 0.057(10) 0.059(6) -0.017(6) 0.004(5) -0.015(6) C45 0.045(6) 0.077(11) 0.058(6) -0.006(6) 0.008(5) -0.006(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 N5 1.753(8) . ? Re1 O1 2.021(8) . ? Re1 O2 2.041(7) . ? Re1 N1 2.087(9) . ? Re1 N3 2.134(8) . ? Re1 P1 2.406(3) . ? S1 C3 1.689(12) . ? S1 C2 1.846(16) . ? S2 C12 1.696(13) . ? S2 C13 1.731(10) . ? P1 C28 1.807(13) . ? P1 C34 1.807(10) . ? P1 C40 1.820(10) . ? O1 C4 1.271(14) . ? O2 C14 1.280(12) . ? O3 C21 1.200(15) . ? N1 C3 1.348(16) . ? N1 C1 1.397(12) . ? N2 C4 1.360(14) . ? N2 C3 1.397(15) . ? N3 C13 1.313(13) . ? N3 C11 1.393(12) . ? N4 C14 1.314(12) . ? N4 C13 1.371(12) . ? N5 N6 1.279(12) . ? N6 C21 1.485(19) . ? C1 C2 1.432(15) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C4 C5 1.425(17) . ? C5 C10 1.360(16) . ? C5 C6 1.425(19) . ? C6 C7 1.36(2) . ? C6 H6 0.9300 . ? C7 C8 1.46(2) . ? C7 H7 0.9300 . ? C8 C9 1.30(2) . ? C8 H8 0.9300 . ? C9 C10 1.44(2) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.315(16) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C14 C15 1.487(13) . ? C15 C20 1.369(14) . ? C15 C16 1.371(15) . ? C16 C17 1.380(15) . ? C16 H16 0.9300 . ? C17 C18 1.360(16) . ? C17 H17 0.9300 . ? C18 C19 1.367(18) . ? C18 H18 0.9300 . ? C19 C20 1.382(15) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.424(16) . ? C22 C27 1.355(19) . ? C22 C23 1.42(2) . ? C23 C24 1.348(18) . ? C23 H23 0.9300 . ? C24 C25 1.36(2) . ? C24 H24 0.9300 . ? C25 C26 1.42(3) . ? C25 H25 0.9300 . ? C26 C27 1.347(19) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.358(14) . ? C28 C33 1.41(2) . ? C29 C30 1.38(2) . ? C29 H29 0.9300 . ? C30 C31 1.38(2) . ? C30 H30 0.9300 . ? C31 C32 1.374(19) . ? C31 H31 0.9300 . ? C32 C33 1.36(2) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C39 1.383(19) . ? C34 C35 1.387(17) . ? C35 C36 1.390(18) . ? C35 H35 0.9300 . ? C36 C37 1.38(3) . ? C36 H36 0.9300 . ? C37 C38 1.36(3) . ? C37 H37 0.9300 . ? C38 C39 1.362(18) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C45 1.380(17) . ? C40 C41 1.393(14) . ? C41 C42 1.403(16) . ? C41 H41 0.9300 . ? C42 C43 1.329(19) . ? C42 H42 0.9300 . ? C43 C44 1.377(17) . ? C43 H43 0.9300 . ? C44 C45 1.387(15) . ? C44 H44 0.9300 . ? C45 H45 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 N5 Re1 O1 174.7(3) . . ? N5 Re1 O2 101.6(3) . . ? O1 Re1 O2 83.5(3) . . ? N5 Re1 N1 90.7(4) . . ? O1 Re1 N1 84.3(3) . . ? O2 Re1 N1 167.2(3) . . ? N5 Re1 N3 97.7(4) . . ? O1 Re1 N3 83.8(3) . . ? O2 Re1 N3 85.8(3) . . ? N1 Re1 N3 88.9(3) . . ? N5 Re1 P1 86.3(3) . . ? O1 Re1 P1 92.4(2) . . ? O2 Re1 P1 91.3(2) . . ? N1 Re1 P1 93.2(3) . . ? N3 Re1 P1 175.4(2) . . ? C3 S1 C2 94.2(6) . . ? C12 S2 C13 89.0(5) . . ? C28 P1 C34 106.2(6) . . ? C28 P1 C40 101.9(5) . . ? C34 P1 C40 105.1(5) . . ? C28 P1 Re1 114.8(3) . . ? C34 P1 Re1 112.5(3) . . ? C40 P1 Re1 115.2(4) . . ? C4 O1 Re1 136.3(7) . . ? C14 O2 Re1 129.7(6) . . ? C3 N1 C1 112.7(9) . . ? C3 N1 Re1 123.7(7) . . ? C1 N1 Re1 123.3(8) . . ? C4 N2 C3 121.7(12) . . ? C13 N3 C11 111.2(9) . . ? C13 N3 Re1 121.9(6) . . ? C11 N3 Re1 126.6(7) . . ? C14 N4 C13 122.3(8) . . ? N6 N5 Re1 160.6(8) . . ? N5 N6 C21 119.5(10) . . ? N1 C1 C2 118.1(12) . . ? N1 C1 H1 121.0 . . ? C2 C1 H1 121.0 . . ? C1 C2 S1 102.0(9) . . ? C1 C2 H2 129.0 . . ? S1 C2 H2 129.0 . . ? N1 C3 N2 130.6(11) . . ? N1 C3 S1 113.0(8) . . ? N2 C3 S1 116.5(10) . . ? O1 C4 N2 122.9(11) . . ? O1 C4 C5 118.5(10) . . ? N2 C4 C5 118.6(12) . . ? C10 C5 C6 119.9(13) . . ? C10 C5 C4 119.6(13) . . ? C6 C5 C4 120.5(11) . . ? C7 C6 C5 122.1(14) . . ? C7 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? C6 C7 C8 117.5(18) . . ? C6 C7 H7 121.2 . . ? C8 C7 H7 121.2 . . ? C9 C8 C7 119.3(15) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C10 124.5(15) . . ? C8 C9 H9 117.8 . . ? C10 C9 H9 117.8 . . ? C5 C10 C9 116.6(16) . . ? C5 C10 H10 121.7 . . ? C9 C10 H10 121.7 . . ? C12 C11 N3 113.9(11) . . ? C12 C11 H11 123.1 . . ? N3 C11 H11 123.1 . . ? C11 C12 S2 112.7(9) . . ? C11 C12 H12 123.6 . . ? S2 C12 H12 123.6 . . ? N3 C13 N4 131.3(9) . . ? N3 C13 S2 113.2(7) . . ? N4 C13 S2 115.5(8) . . ? O2 C14 N4 128.2(9) . . ? O2 C14 C15 115.6(8) . . ? N4 C14 C15 116.3(9) . . ? C20 C15 C16 119.0(9) . . ? C20 C15 C14 118.7(9) . . ? C16 C15 C14 122.3(9) . . ? C15 C16 C17 120.8(10) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C18 C17 C16 120.0(11) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 119.4(11) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C18 C19 C20 120.9(12) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C15 C20 C19 119.8(11) . . ? C15 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? O3 C21 C22 127.3(16) . . ? O3 C21 N6 120.8(12) . . ? C22 C21 N6 111.9(12) . . ? C27 C22 C23 117.5(13) . . ? C27 C22 C21 124.0(14) . . ? C23 C22 C21 118.4(13) . . ? C24 C23 C22 119.8(15) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C25 122.9(18) . . ? C23 C24 H24 118.6 . . ? C25 C24 H24 118.6 . . ? C24 C25 C26 117.1(17) . . ? C24 C25 H25 121.5 . . ? C26 C25 H25 121.5 . . ? C27 C26 C25 119.9(18) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C26 C27 C22 122.5(17) . . ? C26 C27 H27 118.8 . . ? C22 C27 H27 118.8 . . ? C29 C28 C33 115.9(13) . . ? C29 C28 P1 120.0(10) . . ? C33 C28 P1 123.9(9) . . ? C28 C29 C30 122.1(15) . . ? C28 C29 H29 118.9 . . ? C30 C29 H29 118.9 . . ? C31 C30 C29 121.4(14) . . ? C31 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C32 C31 C30 116.7(14) . . ? C32 C31 H31 121.6 . . ? C30 C31 H31 121.6 . . ? C33 C32 C31 121.8(18) . . ? C33 C32 H32 119.1 . . ? C31 C32 H32 119.1 . . ? C32 C33 C28 121.8(16) . . ? C32 C33 H33 119.1 . . ? C28 C33 H33 119.1 . . ? C39 C34 C35 118.3(11) . . ? C39 C34 P1 120.3(9) . . ? C35 C34 P1 121.1(11) . . ? C34 C35 C36 119.3(16) . . ? C34 C35 H35 120.4 . . ? C36 C35 H35 120.4 . . ? C37 C36 C35 120.4(17) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C38 C37 C36 120.6(15) . . ? C38 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C37 C38 C39 118.8(18) . . ? C37 C38 H38 120.6 . . ? C39 C38 H38 120.6 . . ? C38 C39 C34 122.6(15) . . ? C38 C39 H39 118.7 . . ? C34 C39 H39 118.7 . . ? C45 C40 C41 118.3(10) . . ? C45 C40 P1 120.5(8) . . ? C41 C40 P1 121.2(9) . . ? C40 C41 C42 119.4(12) . . ? C40 C41 H41 120.3 . . ? C42 C41 H41 120.3 . . ? C43 C42 C41 121.5(11) . . ? C43 C42 H42 119.2 . . ? C41 C42 H42 119.2 . . ? C42 C43 C44 119.8(11) . . ? C42 C43 H43 120.1 . . ? C44 C43 H43 120.1 . . ? C43 C44 C45 120.2(13) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C40 C45 C44 120.7(11) . . ? C40 C45 H45 119.7 . . ? C44 C45 H45 119.7 . . ? _diffrn_measured_fraction_theta_max 0.870 _diffrn_reflns_theta_full 25.08 _diffrn_measured_fraction_theta_full 0.870 _refine_diff_density_max 0.870 _refine_diff_density_min -1.404 _refine_diff_density_rms 0.112 ###END data_(14) _database_code_CSD 179469 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H56 N6 O9 P2 Re2 S2' _chemical_formula_sum 'C56 H56 N6 O9 P2 Re2 S2' _chemical_formula_weight 1455.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' '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' 'O' 'O' 0.0106 0.0060 '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' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 14.9495(4) _cell_length_b 17.8488(5) _cell_length_c 21.3756(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5703.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15529 _cell_measurement_theta_min 1.36 _cell_measurement_theta_max 30.03 _exptl_crystal_description 'needle' _exptl_crystal_colour 'purple' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.695 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2872 _exptl_absorpt_coefficient_mu 4.430 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.608 _exptl_absorpt_correction_T_max 0.661 _exptl_absorpt_process_details ; SORTAV (R. H. Blessing, Acta Crystallogr., 1995, A51, 33) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '\f scans and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15529 _diffrn_reflns_av_R_equivalents 0.0648 _diffrn_reflns_av_sigmaI/netI 0.0674 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 30.07 _reflns_number_total 8629 _reflns_number_gt 7129 _reflns_threshold_expression 'I>2sigma(I)' _computing_data_collection 'Kappa CCD server software (Nonius, 1997)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN' _computing_structure_solution 'SIR92(Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP II (Johnson, 1976)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+11.6278P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00106(13) _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 0.402(14) _refine_ls_number_reflns 8629 _refine_ls_number_parameters 695 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0670 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1103 _refine_ls_wR_factor_gt 0.0999 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.027 _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 Re1 Re 0.75382(3) 0.95172(2) 0.800839(14) 0.03358(10) Uani 1 1 d . . . Re2 Re 0.52502(3) 0.98936(2) 0.837067(15) 0.03562(10) Uani 1 1 d . . . P1 P 0.81689(19) 0.98060(16) 0.90445(11) 0.0414(6) Uani 1 1 d . . . P2 P 0.50290(18) 1.09396(16) 0.76346(12) 0.0408(6) Uani 1 1 d . . . S1 S 0.5746(2) 0.85786(19) 0.64439(12) 0.0552(7) Uani 1 1 d . . . S2 S 0.5956(3) 0.75914(18) 0.91459(14) 0.0589(8) Uani 1 1 d . . . O1 O 0.8387(5) 0.8899(4) 0.7926(3) 0.0444(16) Uani 1 1 d . . . O2 O 0.4155(5) 0.9703(5) 0.8275(3) 0.0486(19) Uani 1 1 d . . . O3 O 0.6496(4) 1.0063(4) 0.8276(3) 0.0366(13) Uani 1 1 d . . . O4 O 0.7107(7) 0.9580(6) 0.6108(3) 0.064(2) Uani 1 1 d . . . O5 O 0.8304(8) 1.1253(5) 0.8261(4) 0.065(2) Uani 1 1 d . . . O6 O 0.8440(7) 1.1563(5) 0.7243(3) 0.056(2) Uani 1 1 d . . . O7 O 0.5320(10) 0.8679(5) 1.0003(4) 0.077(3) Uani 1 1 d . . . O8 O 0.5466(7) 1.1636(5) 0.8879(3) 0.061(2) Uani 1 1 d . . . O9 O 0.5334(8) 1.1382(4) 0.9893(3) 0.057(2) Uani 1 1 d . . . N1 N 0.5416(6) 0.9112(5) 0.7534(3) 0.0395(19) Uani 1 1 d . . . N2 N 0.6855(6) 0.9445(5) 0.7165(3) 0.0383(18) Uani 1 1 d . . . N3 N 0.8072(6) 1.0369(5) 0.7503(3) 0.0407(18) Uani 1 1 d . . . N4 N 0.6839(6) 0.8511(5) 0.8448(4) 0.0413(18) Uani 1 1 d . . . N5 N 0.5668(7) 0.9092(5) 0.9012(4) 0.0425(19) Uani 1 1 d . . . N6 N 0.5150(6) 1.0446(5) 0.9195(3) 0.0398(17) Uani 1 1 d . . . C1 C 0.4715(9) 0.8646(7) 0.7375(5) 0.051(3) Uani 1 1 d . . . H1 H 0.4232 0.8567 0.7641 0.061 Uiso 1 1 calc R . . C2 C 0.4776(10) 0.8318(6) 0.6817(5) 0.054(3) Uani 1 1 d . . . H2 H 0.4352 0.7992 0.6652 0.065 Uiso 1 1 calc R . . C3 C 0.6030(7) 0.9111(5) 0.7089(4) 0.038(2) Uani 1 1 d . . . C4 C 0.7304(8) 0.9727(6) 0.6654(4) 0.045(2) Uani 1 1 d . . . C5 C 0.8099(8) 1.0207(7) 0.6828(4) 0.046(2) Uani 1 1 d . . . H5 H 0.8060 1.0681 0.6598 0.055 Uiso 1 1 calc R . . C6 C 0.8957(8) 0.9796(8) 0.6628(6) 0.058(3) Uani 1 1 d . . . H61 H 0.8952 0.9300 0.6814 0.070 Uiso 1 1 calc R . . H62 H 0.8943 0.9731 0.6177 0.070 Uiso 1 1 calc R . . C7 C 0.9825(8) 1.0178(8) 0.6802(5) 0.054(3) Uani 1 1 d . . . C8 C 1.0117(9) 1.0792(7) 0.6466(6) 0.056(3) Uani 1 1 d . . . H8 H 0.9759 1.0995 0.6153 0.067 Uiso 1 1 calc R . . C9 C 1.0943(10) 1.1101(9) 0.6598(8) 0.073(4) Uani 1 1 d . . . H9 H 1.1149 1.1505 0.6363 0.087 Uiso 1 1 calc R . . C10 C 1.1458(11) 1.0821(11) 0.7067(8) 0.080(5) Uani 1 1 d . . . H10 H 1.2007 1.1042 0.7156 0.096 Uiso 1 1 calc R . . C11 C 1.1173(13) 1.0210(12) 0.7416(8) 0.089(5) Uani 1 1 d . . . H11 H 1.1527 1.0011 0.7733 0.107 Uiso 1 1 calc R . . C12 C 1.0343(12) 0.9906(11) 0.7276(7) 0.080(4) Uani 1 1 d . . . H12 H 1.0133 0.9505 0.7513 0.096 Uiso 1 1 calc R . . C13 C 0.8283(8) 1.1053(7) 0.7714(5) 0.044(2) Uani 1 1 d . . . C14 C 0.8673(18) 1.2304(8) 0.7440(6) 0.107(8) Uani 1 1 d . . . H141 H 0.9295 1.2319 0.7568 0.128 Uiso 1 1 calc R . . H142 H 0.8304 1.2453 0.7792 0.128 Uiso 1 1 calc R . . C15 C 0.8522(11) 1.2826(6) 0.6896(6) 0.057(3) Uani 1 1 d . . . C16 C 0.9035(13) 1.2784(10) 0.6362(7) 0.079(5) Uani 1 1 d . . . H16 H 0.9499 1.2438 0.6337 0.094 Uiso 1 1 calc R . . C17 C 0.8866(13) 1.3250(12) 0.5867(7) 0.083(5) Uani 1 1 d . . . H17 H 0.9189 1.3196 0.5498 0.100 Uiso 1 1 calc R . . C18 C 0.8234(13) 1.3787(10) 0.5910(9) 0.086(5) Uani 1 1 d . . . H18 H 0.8142 1.4113 0.5577 0.103 Uiso 1 1 calc R . . C19 C 0.7735(16) 1.3852(13) 0.6432(9) 0.107(7) Uani 1 1 d . . . H19 H 0.7296 1.4220 0.6460 0.128 Uiso 1 1 calc R . . C20 C 0.7888(12) 1.3360(12) 0.6932(7) 0.080(5) Uani 1 1 d . . . H20 H 0.7546 1.3403 0.7293 0.096 Uiso 1 1 calc R . . C21 C 0.7167(8) 0.7791(6) 0.8362(5) 0.048(2) Uani 1 1 d . . . H21 H 0.7638 0.7697 0.8089 0.058 Uiso 1 1 calc R . . C22 C 0.6786(11) 0.7247(6) 0.8680(5) 0.059(3) Uani 1 1 d . . . H22 H 0.6947 0.6744 0.8655 0.070 Uiso 1 1 calc R . . C23 C 0.6156(8) 0.8479(6) 0.8856(4) 0.040(2) Uani 1 1 d . . . C24 C 0.5323(10) 0.9177(6) 0.9604(4) 0.050(3) Uani 1 1 d . . . C25 C 0.4950(8) 0.9953(6) 0.9734(4) 0.048(3) Uani 1 1 d . . . H25 H 0.5248 1.0156 1.0105 0.057 Uiso 1 1 calc R . . C26 C 0.3942(9) 0.9880(10) 0.9875(6) 0.066(4) Uani 1 1 d . . . H231 H 0.3641 0.9705 0.9501 0.080 Uiso 1 1 calc R . . H232 H 0.3860 0.9503 1.0197 0.080 Uiso 1 1 calc R . . C27 C 0.3512(9) 1.0585(9) 1.0084(6) 0.065(3) Uani 1 1 d . . . C28 C 0.3625(11) 1.0826(9) 1.0689(7) 0.072(4) Uani 1 1 d . . . H28 H 0.3978 1.0539 1.0955 0.086 Uiso 1 1 calc R . . C29 C 0.3257(19) 1.1443(16) 1.0911(14) 0.137(11) Uani 1 1 d . . . H29 H 0.3330 1.1567 1.1331 0.164 Uiso 1 1 calc R . . C30 C 0.278(3) 1.189(2) 1.054(2) 0.20(2) Uani 1 1 d . . . H30 H 0.2512 1.2320 1.0701 0.241 Uiso 1 1 calc R . . C31 C 0.269(3) 1.172(3) 0.990(3) 0.24(3) Uani 1 1 d . . . H31 H 0.2396 1.2042 0.9625 0.284 Uiso 1 1 calc R . . C32 C 0.303(2) 1.106(2) 0.9690(14) 0.163(14) Uani 1 1 d . . . H32 H 0.2946 1.0923 0.9275 0.195 Uiso 1 1 calc R . . C33 C 0.5316(8) 1.1177(6) 0.9282(4) 0.042(2) Uani 1 1 d . . . C34 C 0.5337(16) 1.2174(7) 1.0007(6) 0.086(6) Uani 1 1 d . . . H341 H 0.4735 1.2370 0.9964 0.103 Uiso 1 1 calc R . . H342 H 0.5714 1.2422 0.9701 0.103 Uiso 1 1 calc R . . C35 C 0.5681(10) 1.2335(6) 1.0654(5) 0.054(3) Uani 1 1 d . . . C36 C 0.5284(13) 1.2888(10) 1.0997(7) 0.087(6) Uani 1 1 d . . . H36 H 0.4760 1.3110 1.0854 0.104 Uiso 1 1 calc R . . C37 C 0.5660(18) 1.3123(13) 1.1565(8) 0.111(8) Uani 1 1 d . . . H37 H 0.5437 1.3537 1.1778 0.133 Uiso 1 1 calc R . . C38 C 0.6363(15) 1.2724(11) 1.1792(7) 0.093(6) Uani 1 1 d . . . H38 H 0.6571 1.2834 1.2192 0.112 Uiso 1 1 calc R . . C39 C 0.6769(13) 1.2181(10) 1.1471(8) 0.086(5) Uani 1 1 d . . . H39 H 0.7278 1.1949 1.1629 0.103 Uiso 1 1 calc R . . C40 C 0.6419(11) 1.1965(8) 1.0892(6) 0.061(3) Uani 1 1 d . . . H40 H 0.6681 1.1576 1.0668 0.073 Uiso 1 1 calc R . . C41 C 0.9320(9) 1.0084(9) 0.9038(6) 0.064(4) Uani 1 1 d . . . H411 H 0.9666 0.9720 0.8812 0.077 Uiso 1 1 calc R . . H412 H 0.9536 1.0119 0.9460 0.077 Uiso 1 1 calc R . . H413 H 0.9375 1.0564 0.8837 0.077 Uiso 1 1 calc R . . C42 C 0.7564(13) 1.0517(8) 0.9487(5) 0.067(4) Uani 1 1 d . . . H421 H 0.6940 1.0390 0.9499 0.080 Uiso 1 1 calc R . . H422 H 0.7638 1.0995 0.9288 0.080 Uiso 1 1 calc R . . H423 H 0.7795 1.0539 0.9905 0.080 Uiso 1 1 calc R . . C43 C 0.8185(9) 0.8993(7) 0.9562(5) 0.049(3) Uani 1 1 d . . . C44 C 0.7691(11) 0.8946(9) 1.0106(6) 0.068(4) Uani 1 1 d . . . H44 H 0.7314 0.9337 1.0222 0.081 Uiso 1 1 calc R . . C45 C 0.7760(13) 0.8312(11) 1.0479(6) 0.079(5) Uani 1 1 d . . . H45 H 0.7421 0.8278 1.0842 0.095 Uiso 1 1 calc R . . C46 C 0.8317(13) 0.7740(9) 1.0320(7) 0.079(5) Uani 1 1 d . . . H46 H 0.8371 0.7331 1.0586 0.094 Uiso 1 1 calc R . . C47 C 0.8792(11) 0.7755(9) 0.9783(6) 0.067(4) Uani 1 1 d . . . H47 H 0.9158 0.7355 0.9673 0.080 Uiso 1 1 calc R . . C48 C 0.8725(11) 0.8386(9) 0.9395(6) 0.066(4) Uani 1 1 d . . . H48 H 0.9045 0.8401 0.9022 0.079 Uiso 1 1 calc R . . C49 C 0.6012(9) 1.1505(8) 0.7501(5) 0.056(3) Uani 1 1 d . . . H491 H 0.6234 1.1687 0.7894 0.068 Uiso 1 1 calc R . . H492 H 0.5861 1.1921 0.7237 0.068 Uiso 1 1 calc R . . H493 H 0.6464 1.1206 0.7302 0.068 Uiso 1 1 calc R . . C50 C 0.4095(9) 1.1561(8) 0.7836(5) 0.055(3) Uani 1 1 d . . . H501 H 0.3567 1.1267 0.7910 0.066 Uiso 1 1 calc R . . H502 H 0.3988 1.1902 0.7497 0.066 Uiso 1 1 calc R . . H503 H 0.4241 1.1838 0.8207 0.066 Uiso 1 1 calc R . . C51 C 0.4683(8) 1.0645(6) 0.6853(4) 0.044(2) Uani 1 1 d . . . C52 C 0.3889(10) 1.0246(9) 0.6781(6) 0.066(4) Uani 1 1 d . . . H52 H 0.3550 1.0127 0.7133 0.079 Uiso 1 1 calc R . . C53 C 0.3599(12) 1.0026(11) 0.6203(6) 0.080(4) Uani 1 1 d . . . H53 H 0.3069 0.9757 0.6168 0.096 Uiso 1 1 calc R . . C54 C 0.4080(14) 1.0198(10) 0.5669(6) 0.083(5) Uani 1 1 d . . . H54 H 0.3873 1.0056 0.5276 0.099 Uiso 1 1 calc R . . C55 C 0.4867(14) 1.0584(12) 0.5733(6) 0.086(5) Uani 1 1 d . . . H55 H 0.5205 1.0696 0.5379 0.103 Uiso 1 1 calc R . . C56 C 0.5171(12) 1.0811(9) 0.6322(6) 0.071(4) Uani 1 1 d . . . H56 H 0.5705 1.1075 0.6356 0.085 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 Re1 0.04057(19) 0.03224(17) 0.02794(15) 0.00060(11) 0.00031(14) -0.00076(17) Re2 0.0414(2) 0.03323(18) 0.03229(16) -0.00232(13) 0.00206(14) -0.00112(16) P1 0.0488(15) 0.0415(13) 0.0340(11) 0.0006(9) -0.0070(9) -0.0021(12) P2 0.0424(15) 0.0396(14) 0.0404(12) 0.0015(9) 0.0006(10) 0.0064(11) S1 0.071(2) 0.0548(18) 0.0393(12) -0.0158(11) -0.0053(12) -0.0068(15) S2 0.082(2) 0.0337(14) 0.0609(16) 0.0070(11) 0.0150(15) -0.0042(15) O1 0.039(4) 0.041(4) 0.053(4) -0.004(3) 0.004(3) 0.014(3) O2 0.030(3) 0.068(6) 0.048(4) -0.006(3) 0.007(3) -0.010(3) O3 0.043(3) 0.029(3) 0.038(3) 0.000(2) -0.001(2) -0.008(3) O4 0.092(6) 0.077(6) 0.022(3) -0.002(3) 0.001(3) -0.011(6) O5 0.098(7) 0.049(5) 0.047(4) -0.005(3) -0.013(4) -0.011(5) O6 0.076(6) 0.048(5) 0.043(4) 0.002(3) -0.003(4) -0.014(4) O7 0.137(10) 0.049(5) 0.046(4) 0.011(3) 0.035(6) 0.005(6) O8 0.097(7) 0.040(4) 0.046(4) 0.002(3) -0.002(4) -0.003(5) O9 0.092(6) 0.036(4) 0.043(4) -0.005(3) 0.004(4) 0.007(5) N1 0.047(5) 0.030(4) 0.041(4) -0.003(3) -0.010(3) -0.009(4) N2 0.050(5) 0.042(4) 0.023(3) -0.002(3) 0.001(3) -0.007(4) N3 0.055(5) 0.036(4) 0.031(4) -0.001(3) 0.002(3) -0.006(4) N4 0.056(5) 0.030(4) 0.037(4) 0.001(3) -0.002(3) 0.013(4) N5 0.054(5) 0.034(4) 0.039(4) -0.001(3) 0.010(4) 0.004(4) N6 0.052(5) 0.037(4) 0.030(3) -0.004(3) 0.004(3) 0.004(4) C1 0.058(7) 0.053(6) 0.042(5) -0.003(4) -0.012(5) -0.011(6) C2 0.066(7) 0.036(5) 0.061(6) -0.009(4) 0.001(6) -0.013(6) C3 0.053(6) 0.030(4) 0.030(4) -0.004(3) -0.001(4) 0.006(4) C4 0.059(7) 0.045(5) 0.032(4) 0.001(4) 0.006(4) 0.000(5) C5 0.059(6) 0.041(5) 0.037(4) 0.002(4) 0.017(4) -0.002(5) C6 0.060(7) 0.056(7) 0.058(6) -0.014(6) 0.022(5) -0.004(6) C7 0.048(6) 0.060(7) 0.054(6) 0.002(5) 0.011(4) 0.013(6) C8 0.058(7) 0.047(7) 0.063(7) 0.002(5) 0.008(5) -0.006(6) C9 0.063(9) 0.053(8) 0.102(11) -0.005(8) 0.019(8) 0.004(7) C10 0.057(8) 0.084(12) 0.098(11) -0.035(9) -0.010(8) 0.010(8) C11 0.093(13) 0.091(14) 0.084(10) 0.018(9) -0.003(9) 0.023(11) C12 0.083(10) 0.084(11) 0.073(8) 0.015(8) 0.010(7) -0.003(10) C13 0.043(6) 0.048(6) 0.041(5) 0.000(4) -0.002(4) -0.010(5) C14 0.22(3) 0.044(8) 0.058(8) 0.014(6) -0.041(11) -0.041(12) C15 0.084(9) 0.030(5) 0.057(6) 0.000(4) -0.004(6) -0.020(6) C16 0.084(11) 0.066(10) 0.086(10) 0.001(7) 0.012(8) 0.029(9) C17 0.081(11) 0.106(15) 0.063(9) 0.015(8) 0.006(7) -0.005(11) C18 0.091(13) 0.066(10) 0.101(12) 0.033(9) -0.006(10) -0.004(10) C19 0.125(19) 0.104(16) 0.091(12) -0.012(10) 0.006(11) 0.047(14) C20 0.076(10) 0.105(14) 0.060(8) -0.005(8) 0.006(7) 0.000(10) C21 0.060(7) 0.034(5) 0.050(5) -0.009(4) -0.005(5) 0.009(5) C22 0.093(10) 0.025(5) 0.058(6) -0.006(4) 0.006(6) -0.002(6) C23 0.054(6) 0.027(5) 0.039(5) -0.004(3) 0.000(4) 0.000(4) C24 0.074(8) 0.045(6) 0.031(4) 0.005(4) 0.008(5) -0.007(6) C25 0.078(8) 0.041(5) 0.023(4) -0.003(3) 0.010(4) -0.005(5) C26 0.054(7) 0.093(11) 0.053(6) -0.012(7) 0.012(5) -0.017(8) C27 0.057(7) 0.073(10) 0.066(7) 0.010(6) 0.001(6) 0.013(7) C28 0.074(10) 0.061(9) 0.080(9) -0.007(7) 0.015(7) 0.012(8) C29 0.13(2) 0.11(2) 0.17(2) -0.009(17) 0.093(19) 0.013(17) C30 0.18(4) 0.12(3) 0.30(5) 0.04(3) 0.09(4) 0.10(3) C31 0.17(4) 0.23(5) 0.31(5) 0.13(5) 0.00(4) 0.13(4) C32 0.14(2) 0.21(4) 0.14(2) 0.06(2) -0.014(18) 0.09(3) C33 0.053(6) 0.031(5) 0.041(5) 0.000(3) -0.001(4) 0.008(5) C34 0.156(17) 0.037(6) 0.064(8) -0.012(5) -0.048(10) 0.021(9) C35 0.075(8) 0.031(5) 0.056(6) -0.008(4) -0.012(6) 0.001(6) C36 0.087(11) 0.080(11) 0.095(10) -0.037(8) -0.039(9) 0.038(10) C37 0.16(2) 0.102(15) 0.075(10) -0.035(10) -0.016(12) 0.033(14) C38 0.127(17) 0.082(12) 0.069(9) -0.024(8) -0.031(9) 0.041(12) C39 0.092(12) 0.075(11) 0.090(10) -0.013(8) -0.038(9) 0.015(10) C40 0.080(9) 0.046(7) 0.056(7) -0.002(5) 0.010(6) 0.011(7) C41 0.058(7) 0.068(9) 0.065(7) 0.029(6) -0.016(5) -0.014(7) C42 0.111(11) 0.054(7) 0.035(5) -0.007(4) -0.008(6) 0.018(9) C43 0.061(7) 0.049(6) 0.036(5) -0.002(4) -0.009(4) 0.000(6) C44 0.079(10) 0.073(9) 0.051(6) 0.019(6) 0.001(6) 0.000(8) C45 0.101(13) 0.087(12) 0.050(7) 0.021(6) 0.012(7) -0.013(10) C46 0.118(14) 0.053(8) 0.066(8) 0.026(6) -0.032(9) -0.006(9) C47 0.077(10) 0.056(8) 0.067(8) 0.009(6) -0.015(7) 0.002(7) C48 0.093(11) 0.059(8) 0.044(6) 0.002(5) -0.012(6) -0.011(8) C49 0.059(7) 0.052(7) 0.058(7) 0.012(5) -0.006(5) -0.006(6) C50 0.054(7) 0.058(8) 0.054(6) -0.003(5) -0.007(5) 0.020(6) C51 0.039(5) 0.045(6) 0.047(5) 0.000(4) -0.005(4) 0.018(5) C52 0.067(8) 0.077(10) 0.054(7) -0.002(6) -0.011(5) -0.003(7) C53 0.094(11) 0.078(11) 0.067(8) 0.000(7) -0.034(7) 0.001(10) C54 0.119(14) 0.082(11) 0.048(7) -0.010(7) -0.017(7) 0.018(11) C55 0.109(13) 0.109(14) 0.039(6) -0.005(7) 0.007(7) 0.013(12) C56 0.081(10) 0.078(10) 0.054(7) 0.003(6) 0.014(7) 0.002(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 O1 1.690(7) . ? Re1 O3 1.925(7) . ? Re1 N3 2.028(8) . ? Re1 N2 2.075(7) . ? Re1 N4 2.280(9) . ? Re1 P1 2.462(2) . ? Re2 O2 1.684(7) . ? Re2 O3 1.897(7) . ? Re2 N6 2.025(7) . ? Re2 N5 2.078(9) . ? Re2 N1 2.282(8) . ? Re2 P2 2.464(3) . ? P1 C41 1.791(13) . ? P1 C42 1.822(13) . ? P1 C43 1.824(12) . ? P2 C49 1.805(13) . ? P2 C51 1.827(10) . ? P2 C50 1.834(12) . ? S1 C2 1.720(14) . ? S1 C3 1.727(9) . ? S2 C22 1.705(14) . ? S2 C23 1.728(11) . ? O4 C4 1.233(12) . ? O5 C13 1.223(12) . ? O6 C13 1.377(13) . ? O6 C14 1.430(17) . ? O7 C24 1.231(13) . ? O8 C33 1.210(13) . ? O9 C33 1.358(12) . ? O9 C34 1.434(14) . ? N1 C3 1.323(13) . ? N1 C1 1.379(14) . ? N2 C4 1.376(12) . ? N2 C3 1.380(14) . ? N3 C13 1.340(14) . ? N3 C5 1.472(12) . ? N4 C23 1.344(13) . ? N4 C21 1.387(13) . ? N5 C23 1.357(14) . ? N5 C24 1.375(12) . ? N6 C33 1.340(13) . ? N6 C25 1.481(12) . ? C1 C2 1.332(15) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C4 C5 1.511(16) . ? C5 C6 1.539(17) . ? C5 H5 0.9800 . ? C6 C7 1.514(19) . ? C6 H61 0.9700 . ? C6 H62 0.9700 . ? C7 C12 1.36(2) . ? C7 C8 1.380(18) . ? C8 C9 1.38(2) . ? C8 H8 0.9300 . ? C9 C10 1.36(2) . ? C9 H9 0.9300 . ? C10 C11 1.39(3) . ? C10 H10 0.9300 . ? C11 C12 1.39(3) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C14 C15 1.507(17) . ? C14 H141 0.9700 . ? C14 H142 0.9700 . ? C15 C20 1.35(2) . ? C15 C16 1.379(19) . ? C16 C17 1.37(2) . ? C16 H16 0.9300 . ? C17 C18 1.35(3) . ? C17 H17 0.9300 . ? C18 C19 1.35(3) . ? C18 H18 0.9300 . ? C19 C20 1.40(3) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.317(17) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C24 C25 1.519(16) . ? C25 C26 1.541(17) . ? C25 H25 0.9800 . ? C26 C27 1.48(2) . ? C26 H231 0.9700 . ? C26 H232 0.9700 . ? C27 C28 1.37(2) . ? C27 C32 1.39(3) . ? C28 C29 1.32(3) . ? C28 H28 0.9300 . ? C29 C30 1.33(5) . ? C29 H29 0.9300 . ? C30 C31 1.42(5) . ? C30 H30 0.9300 . ? C31 C32 1.35(6) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C34 C35 1.503(16) . ? C34 H341 0.9700 . ? C34 H342 0.9700 . ? C35 C36 1.366(18) . ? C35 C40 1.38(2) . ? C36 C37 1.40(2) . ? C36 H36 0.9300 . ? C37 C38 1.36(3) . ? C37 H37 0.9300 . ? C38 C39 1.33(2) . ? C38 H38 0.9300 . ? C39 C40 1.397(19) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 H411 0.9600 . ? C41 H412 0.9600 . ? C41 H413 0.9600 . ? C42 H421 0.9600 . ? C42 H422 0.9600 . ? C42 H423 0.9600 . ? C43 C44 1.379(17) . ? C43 C48 1.40(2) . ? C44 C45 1.39(2) . ? C44 H44 0.9300 . ? C45 C46 1.36(3) . ? C45 H45 0.9300 . ? C46 C47 1.35(2) . ? C46 H46 0.9300 . ? C47 C48 1.402(19) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 H491 0.9600 . ? C49 H492 0.9600 . ? C49 H493 0.9600 . ? C50 H501 0.9600 . ? C50 H502 0.9600 . ? C50 H503 0.9600 . ? C51 C56 1.382(17) . ? C51 C52 1.39(2) . ? C52 C53 1.368(17) . ? C52 H52 0.9300 . ? C53 C54 1.38(2) . ? C53 H53 0.9300 . ? C54 C55 1.37(3) . ? C54 H54 0.9300 . ? C55 C56 1.40(2) . ? C55 H55 0.9300 . ? C56 H56 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 O1 Re1 O3 165.7(3) . . ? O1 Re1 N3 97.9(4) . . ? O3 Re1 N3 95.6(3) . . ? O1 Re1 N2 103.8(3) . . ? O3 Re1 N2 83.8(3) . . ? N3 Re1 N2 77.2(3) . . ? O1 Re1 N4 82.7(3) . . ? O3 Re1 N4 84.5(3) . . ? N3 Re1 N4 171.8(3) . . ? N2 Re1 N4 94.8(3) . . ? O1 Re1 P1 86.7(3) . . ? O3 Re1 P1 86.37(19) . . ? N3 Re1 P1 99.9(2) . . ? N2 Re1 P1 169.3(3) . . ? N4 Re1 P1 88.3(2) . . ? O2 Re2 O3 166.7(3) . . ? O2 Re2 N6 97.6(4) . . ? O3 Re2 N6 95.0(3) . . ? O2 Re2 N5 103.5(4) . . ? O3 Re2 N5 83.4(3) . . ? N6 Re2 N5 77.4(3) . . ? O2 Re2 N1 83.5(3) . . ? O3 Re2 N1 84.7(3) . . ? N6 Re2 N1 171.1(3) . . ? N5 Re2 N1 93.7(3) . . ? O2 Re2 P2 86.9(3) . . ? O3 Re2 P2 86.8(2) . . ? N6 Re2 P2 100.2(3) . . ? N5 Re2 P2 169.6(3) . . ? N1 Re2 P2 88.7(2) . . ? C41 P1 C42 106.7(8) . . ? C41 P1 C43 102.3(6) . . ? C42 P1 C43 104.2(6) . . ? C41 P1 Re1 114.8(4) . . ? C42 P1 Re1 115.0(5) . . ? C43 P1 Re1 112.6(4) . . ? C49 P2 C51 104.3(6) . . ? C49 P2 C50 108.6(7) . . ? C51 P2 C50 100.0(5) . . ? C49 P2 Re2 114.5(4) . . ? C51 P2 Re2 113.8(4) . . ? C50 P2 Re2 114.2(4) . . ? C2 S1 C3 89.2(5) . . ? C22 S2 C23 89.7(5) . . ? Re2 O3 Re1 138.3(4) . . ? C13 O6 C14 115.9(9) . . ? C33 O9 C34 115.4(9) . . ? C3 N1 C1 110.5(8) . . ? C3 N1 Re2 129.8(6) . . ? C1 N1 Re2 118.6(7) . . ? C4 N2 C3 120.0(8) . . ? C4 N2 Re1 115.2(7) . . ? C3 N2 Re1 124.7(6) . . ? C13 N3 C5 120.2(8) . . ? C13 N3 Re1 126.6(6) . . ? C5 N3 Re1 112.7(6) . . ? C23 N4 C21 108.4(9) . . ? C23 N4 Re1 130.4(6) . . ? C21 N4 Re1 120.8(7) . . ? C23 N5 C24 121.1(9) . . ? C23 N5 Re2 123.7(6) . . ? C24 N5 Re2 114.8(7) . . ? C33 N6 C25 120.6(7) . . ? C33 N6 Re2 125.5(6) . . ? C25 N6 Re2 113.7(6) . . ? C2 C1 N1 115.7(12) . . ? C2 C1 H1 122.2 . . ? N1 C1 H1 122.1 . . ? C1 C2 S1 110.7(10) . . ? C1 C2 H2 124.6 . . ? S1 C2 H2 124.6 . . ? N1 C3 N2 122.3(7) . . ? N1 C3 S1 113.9(8) . . ? N2 C3 S1 123.5(7) . . ? O4 C4 N2 123.9(10) . . ? O4 C4 C5 122.8(9) . . ? N2 C4 C5 113.3(8) . . ? N3 C5 C4 109.3(8) . . ? N3 C5 C6 112.9(10) . . ? C4 C5 C6 108.4(9) . . ? N3 C5 H5 108.7 . . ? C4 C5 H5 108.7 . . ? C6 C5 H5 108.7 . . ? C7 C6 C5 115.5(10) . . ? C7 C6 H61 108.4 . . ? C5 C6 H61 108.4 . . ? C7 C6 H62 108.4 . . ? C5 C6 H62 108.4 . . ? H61 C6 H62 107.5 . . ? C12 C7 C8 119.4(14) . . ? C12 C7 C6 120.6(14) . . ? C8 C7 C6 120.0(12) . . ? C7 C8 C9 119.5(14) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C10 C9 C8 120.6(16) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 120.8(17) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C12 C11 C10 117.8(16) . . ? C12 C11 H11 121.1 . . ? C10 C11 H11 121.1 . . ? C7 C12 C11 121.9(16) . . ? C7 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? O5 C13 N3 126.4(10) . . ? O5 C13 O6 120.1(11) . . ? N3 C13 O6 113.3(8) . . ? O6 C14 C15 108.0(10) . . ? O6 C14 H141 110.1 . . ? C15 C14 H141 110.1 . . ? O6 C14 H142 110.1 . . ? C15 C14 H142 110.1 . . ? H141 C14 H142 108.4 . . ? C20 C15 C16 118.4(13) . . ? C20 C15 C14 120.0(15) . . ? C16 C15 C14 121.5(16) . . ? C17 C16 C15 120.3(15) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C18 C17 C16 120.6(15) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C19 120.4(16) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C18 C19 C20 119.1(18) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C15 C20 C19 121.1(14) . . ? C15 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C22 C21 N4 117.5(11) . . ? C22 C21 H21 121.2 . . ? N4 C21 H21 121.2 . . ? C21 C22 S2 110.5(9) . . ? C21 C22 H22 124.7 . . ? S2 C22 H22 124.7 . . ? N4 C23 N5 122.3(9) . . ? N4 C23 S2 113.8(7) . . ? N5 C23 S2 123.9(8) . . ? O7 C24 N5 124.0(11) . . ? O7 C24 C25 122.1(9) . . ? N5 C24 C25 113.9(8) . . ? N6 C25 C24 109.0(7) . . ? N6 C25 C26 113.5(10) . . ? C24 C25 C26 108.6(11) . . ? N6 C25 H25 108.5 . . ? C24 C25 H25 108.5 . . ? C26 C25 H25 108.5 . . ? C27 C26 C25 114.3(13) . . ? C27 C26 H231 108.7 . . ? C25 C26 H231 108.7 . . ? C27 C26 H232 108.7 . . ? C25 C26 H232 108.7 . . ? H231 C26 H232 107.6 . . ? C28 C27 C32 116(2) . . ? C28 C27 C26 119.8(13) . . ? C32 C27 C26 123.9(19) . . ? C29 C28 C27 123(2) . . ? C29 C28 H28 118.3 . . ? C27 C28 H28 118.3 . . ? C28 C29 C30 121(3) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C29 C30 C31 120(3) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.1 . . ? C32 C31 C30 118(3) . . ? C32 C31 H31 121.0 . . ? C30 C31 H31 121.0 . . ? C31 C32 C27 122(3) . . ? C31 C32 H32 119.1 . . ? C27 C32 H32 119.1 . . ? O8 C33 N6 126.5(9) . . ? O8 C33 O9 119.9(10) . . ? N6 C33 O9 113.6(8) . . ? O9 C34 C35 110.2(10) . . ? O9 C34 H341 109.6 . . ? C35 C34 H341 109.6 . . ? O9 C34 H342 109.6 . . ? C35 C34 H342 109.6 . . ? H341 C34 H342 108.1 . . ? C36 C35 C40 119.6(12) . . ? C36 C35 C34 118.9(13) . . ? C40 C35 C34 121.3(12) . . ? C35 C36 C37 120.5(16) . . ? C35 C36 H36 119.8 . . ? C37 C36 H36 119.8 . . ? C38 C37 C36 117.5(17) . . ? C38 C37 H37 121.2 . . ? C36 C37 H37 121.2 . . ? C39 C38 C37 123.3(16) . . ? C39 C38 H38 118.4 . . ? C37 C38 H38 118.4 . . ? C38 C39 C40 119.1(16) . . ? C38 C39 H39 120.5 . . ? C40 C39 H39 120.5 . . ? C35 C40 C39 119.5(13) . . ? C35 C40 H40 120.2 . . ? C39 C40 H40 120.2 . . ? P1 C41 H411 109.5 . . ? P1 C41 H412 109.5 . . ? H411 C41 H412 109.5 . . ? P1 C41 H413 109.5 . . ? H411 C41 H413 109.5 . . ? H412 C41 H413 109.5 . . ? P1 C42 H421 109.5 . . ? P1 C42 H422 109.5 . . ? H421 C42 H422 109.5 . . ? P1 C42 H423 109.5 . . ? H421 C42 H423 109.5 . . ? H422 C42 H423 109.5 . . ? C44 C43 C48 118.4(12) . . ? C44 C43 P1 123.5(10) . . ? C48 C43 P1 118.0(9) . . ? C43 C44 C45 119.6(15) . . ? C43 C44 H44 120.2 . . ? C45 C44 H44 120.2 . . ? C46 C45 C44 120.9(13) . . ? C46 C45 H45 119.5 . . ? C44 C45 H45 119.5 . . ? C47 C46 C45 121.3(13) . . ? C47 C46 H46 119.3 . . ? C45 C46 H46 119.3 . . ? C46 C47 C48 118.7(15) . . ? C46 C47 H47 120.7 . . ? C48 C47 H47 120.7 . . ? C43 C48 C47 120.9(13) . . ? C43 C48 H48 119.5 . . ? C47 C48 H48 119.5 . . ? P2 C49 H491 109.5 . . ? P2 C49 H492 109.5 . . ? H491 C49 H492 109.5 . . ? P2 C49 H493 109.5 . . ? H491 C49 H493 109.5 . . ? H492 C49 H493 109.5 . . ? P2 C50 H501 109.5 . . ? P2 C50 H502 109.5 . . ? H501 C50 H502 109.5 . . ? P2 C50 H503 109.5 . . ? H501 C50 H503 109.5 . . ? H502 C50 H503 109.5 . . ? C56 C51 C52 118.0(11) . . ? C56 C51 P2 122.7(10) . . ? C52 C51 P2 119.3(9) . . ? C53 C52 C51 121.0(14) . . ? C53 C52 H52 119.5 . . ? C51 C52 H52 119.5 . . ? C52 C53 C54 121.2(17) . . ? C52 C53 H53 119.4 . . ? C54 C53 H53 119.4 . . ? C55 C54 C53 118.4(13) . . ? C55 C54 H54 120.8 . . ? C53 C54 H54 120.8 . . ? C54 C55 C56 120.9(15) . . ? C54 C55 H55 119.5 . . ? C56 C55 H55 119.5 . . ? C51 C56 C55 120.4(16) . . ? C51 C56 H56 119.8 . . ? C55 C56 H56 119.8 . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 30.07 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 1.183 _refine_diff_density_min -1.421 _refine_diff_density_rms 0.145 ###END