# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_a13643a _database_code_depnum_ccdc_archive 'CCDC 903345' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C85 H21 N O3 P Re S2' _chemical_formula_sum 'C85 H21 N O3 P Re S2' _chemical_formula_weight 1385.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1313(5) _cell_length_b 16.7505(10) _cell_length_c 17.0644(8) _cell_angle_alpha 116.909(3) _cell_angle_beta 100.253(2) _cell_angle_gamma 90.025(3) _cell_volume 2530.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.818 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 2.583 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6130 _exptl_absorpt_correction_T_max 0.9746 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18575 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.1070 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.02 _reflns_number_total 8852 _reflns_number_gt 6796 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+19.6592P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8852 _refine_ls_number_parameters 819 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0926 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1352 _refine_ls_wR_factor_gt 0.1206 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7523(7) 0.5489(6) 0.5768(6) 0.0165(11) Uani 1 1 d . . . C2 C 0.6050(7) 0.4930(6) 0.6658(6) 0.0165(11) Uani 1 1 d . . . C3 C 0.9814(7) 0.4849(6) 0.6300(6) 0.0165(11) Uani 1 1 d . . . C4 C 0.7682(7) 0.5303(6) 0.8726(5) 0.019(2) Uani 1 1 d . . . C5 C 0.7152(8) 0.6099(7) 0.8831(6) 0.026(2) Uani 1 1 d . . . H5 H 0.7252 0.6319 0.8418 0.031 Uiso 1 1 calc R . . C6 C 0.6483(9) 0.6581(8) 0.9513(7) 0.038(3) Uani 1 1 d . . . H6 H 0.6160 0.7138 0.9584 0.046 Uiso 1 1 calc R . . C7 C 0.6287(9) 0.6242(8) 1.0100(7) 0.038(3) Uani 1 1 d . . . H7 H 0.5814 0.6561 1.0568 0.046 Uiso 1 1 calc R . . C8 C 0.6780(9) 0.5448(8) 0.9995(7) 0.036(3) Uani 1 1 d . . . H8 H 0.6637 0.5214 1.0390 0.043 Uiso 1 1 calc R . . C9 C 0.7484(8) 0.4981(7) 0.9325(6) 0.029(2) Uani 1 1 d . . . H9 H 0.7835 0.4437 0.9272 0.035 Uiso 1 1 calc R . . C10 C 1.0383(8) 0.5356(7) 0.8428(6) 0.022(2) Uani 1 1 d . . . C11 C 1.0557(9) 0.6149(8) 0.9198(7) 0.036(3) Uani 1 1 d . . . H11 H 0.9817 0.6357 0.9486 0.043 Uiso 1 1 calc R . . C12 C 1.1803(9) 0.6659(8) 0.9571(8) 0.044(3) Uani 1 1 d . . . H12 H 1.1916 0.7208 1.0111 0.053 Uiso 1 1 calc R . . C13 C 1.2850(9) 0.6358(9) 0.9148(9) 0.046(3) Uani 1 1 d . . . H13 H 1.3691 0.6713 0.9382 0.055 Uiso 1 1 calc R . . C14 C 1.2716(9) 0.5548(10) 0.8387(9) 0.048(3) Uani 1 1 d . . . H14 H 1.3469 0.5342 0.8111 0.057 Uiso 1 1 calc R . . C15 C 1.1494(8) 0.5034(8) 0.8021(7) 0.033(3) Uani 1 1 d . . . H15 H 1.1403 0.4470 0.7501 0.039 Uiso 1 1 calc R . . C16 C 0.8864(8) 0.3646(7) 0.7891(6) 0.023(2) Uani 1 1 d . . . C17 C 1.0002(9) 0.3508(7) 0.8397(6) 0.031(2) Uani 1 1 d . . . H17 H 1.0735 0.3962 0.8693 0.037 Uiso 1 1 calc R . . C18 C 1.0076(10) 0.2725(8) 0.8473(7) 0.036(3) Uani 1 1 d . . . H18 H 1.0859 0.2638 0.8814 0.044 Uiso 1 1 calc R . . C19 C 0.8994(10) 0.2058(7) 0.8048(6) 0.033(2) Uani 1 1 d . . . H19 H 0.9034 0.1517 0.8099 0.039 Uiso 1 1 calc R . . C20 C 0.7883(9) 0.2195(7) 0.7560(6) 0.028(2) Uani 1 1 d . . . H20 H 0.7143 0.1746 0.7278 0.034 Uiso 1 1 calc R . . C21 C 0.7807(8) 0.2985(6) 0.7463(6) 0.022(2) Uani 1 1 d . . . C22 C 0.6582(8) 0.3082(6) 0.6867(6) 0.020(2) Uani 1 1 d . . . H22 H 0.6497 0.3739 0.7076 0.024 Uiso 1 1 calc R . . C23 C 0.4860(9) 0.3090(7) 0.7685(6) 0.029(2) Uani 1 1 d . . . H23A H 0.5483 0.2980 0.8129 0.043 Uiso 1 1 calc R . . H23B H 0.3949 0.2838 0.7618 0.043 Uiso 1 1 calc R . . H23C H 0.4862 0.3738 0.7887 0.043 Uiso 1 1 calc R . . C24 C 0.4400(8) 0.2797(7) 0.6129(6) 0.026(2) Uani 1 1 d . . . H24A H 0.4256 0.3440 0.6337 0.032 Uiso 1 1 calc R . . H24B H 0.3516 0.2445 0.5944 0.032 Uiso 1 1 calc R . . C25 C 0.5176(7) 0.2454(6) 0.5351(6) 0.019(2) Uani 1 1 d . . . C26 C 0.6732(7) 0.2650(6) 0.5854(6) 0.018(2) Uani 1 1 d . . . C27 C 0.7676(7) 0.3277(6) 0.5667(5) 0.0156(19) Uani 1 1 d . . . C28 C 0.7133(8) 0.3661(6) 0.5080(6) 0.0168(19) Uani 1 1 d . . . C29 C 0.5699(8) 0.3391(6) 0.4580(6) 0.021(2) Uani 1 1 d . . . C30 C 0.4845(7) 0.2831(6) 0.4681(6) 0.017(2) Uani 1 1 d . . . C31 C 0.3900(7) 0.2190(7) 0.3896(6) 0.022(2) Uani 1 1 d . . . C32 C 0.3813(7) 0.1360(7) 0.3946(6) 0.022(2) Uani 1 1 d . . . C33 C 0.4692(8) 0.1461(6) 0.4744(6) 0.019(2) Uani 1 1 d . . . C34 C 0.5414(8) 0.0771(7) 0.4736(6) 0.022(2) Uani 1 1 d . . . C35 C 0.6835(8) 0.0936(7) 0.5175(6) 0.021(2) Uani 1 1 d . . . C36 C 0.7469(8) 0.1800(6) 0.5597(5) 0.018(2) Uani 1 1 d . . . C39 C 0.8786(7) 0.1946(6) 0.5481(6) 0.018(2) Uani 1 1 d . . . C40 C 0.8892(7) 0.2793(6) 0.5461(5) 0.018(2) Uani 1 1 d . . . C41 C 0.9660(7) 0.2861(6) 0.4882(6) 0.019(2) Uani 1 1 d . . . C42 C 0.9132(7) 0.3305(6) 0.4339(6) 0.0159(19) Uani 1 1 d . . . C43 C 0.7879(7) 0.3629(6) 0.4393(6) 0.0166(19) Uani 1 1 d . . . C44 C 0.6967(8) 0.3508(6) 0.3599(6) 0.018(2) Uani 1 1 d . . . C45 C 0.5619(8) 0.3369(6) 0.3720(6) 0.021(2) Uani 1 1 d . . . C46 C 0.4676(8) 0.2777(6) 0.2968(6) 0.023(2) Uani 1 1 d . . . C47 C 0.3794(7) 0.2170(7) 0.3064(6) 0.020(2) Uani 1 1 d . . . C48 C 0.3590(7) 0.1326(7) 0.2259(6) 0.024(2) Uani 1 1 d . . . C49 C 0.3508(7) 0.0536(7) 0.2318(6) 0.024(2) Uani 1 1 d . . . C50 C 0.3599(7) 0.0532(7) 0.3170(6) 0.022(2) Uani 1 1 d . . . C51 C 0.4337(8) -0.0196(7) 0.3168(6) 0.026(2) Uani 1 1 d . . . C52 C 0.5227(8) -0.0078(6) 0.3934(6) 0.021(2) Uani 1 1 d . . . C53 C 0.6522(8) -0.0446(7) 0.3872(6) 0.025(2) Uani 1 1 d . . . C54 C 0.7515(8) 0.0192(7) 0.4642(6) 0.022(2) Uani 1 1 d . . . C55 C 0.8810(8) 0.0326(7) 0.4541(6) 0.024(2) Uani 1 1 d . . . C56 C 0.9479(7) 0.1217(7) 0.4965(6) 0.020(2) Uani 1 1 d . . . C57 C 1.0277(7) 0.1303(7) 0.4388(6) 0.020(2) Uani 1 1 d . . . C58 C 1.0343(7) 0.2104(6) 0.4328(6) 0.019(2) Uani 1 1 d . . . C59 C 1.0244(7) 0.2094(7) 0.3464(6) 0.021(2) Uani 1 1 d . . . C60 C 0.9496(8) 0.2831(7) 0.3467(6) 0.022(2) Uani 1 1 d . . . C61 C 0.8615(8) 0.2738(6) 0.2695(6) 0.021(2) Uani 1 1 d . . . C62 C 0.7320(8) 0.3079(7) 0.2777(6) 0.023(2) Uani 1 1 d . . . C63 C 0.6337(8) 0.2450(7) 0.1992(6) 0.0226(15) Uani 1 1 d . . . C64 C 0.5022(8) 0.2316(7) 0.2096(6) 0.0226(15) Uani 1 1 d . . . C65 C 0.4371(8) 0.1414(7) 0.1659(6) 0.025(2) Uani 1 1 d . . . C66 C 0.5028(8) 0.0689(7) 0.1134(6) 0.028(2) Uani 1 1 d . . . C67 C 0.4931(8) -0.0150(7) 0.1184(6) 0.028(2) Uani 1 1 d . . . C68 C 0.4195(8) -0.0232(7) 0.1768(6) 0.024(2) Uani 1 1 d . . . C69 C 0.4698(8) -0.0683(7) 0.2289(6) 0.027(2) Uani 1 1 d . . . C70 C 0.5959(9) -0.1026(7) 0.2233(6) 0.029(2) Uani 1 1 d . . . C71 C 0.6887(8) -0.0913(7) 0.3044(6) 0.025(2) Uani 1 1 d . . . C72 C 0.8234(9) -0.0766(7) 0.2931(6) 0.028(2) Uani 1 1 d . . . C73 C 0.9189(8) -0.0155(6) 0.3671(6) 0.022(2) Uani 1 1 d . . . C74 C 1.0091(7) 0.0446(7) 0.3574(6) 0.022(2) Uani 1 1 d . . . C75 C 0.9989(7) 0.0440(7) 0.2754(6) 0.024(2) Uani 1 1 d . . . C76 C 1.0072(8) 0.1271(7) 0.2693(6) 0.025(2) Uani 1 1 d . . . C77 C 0.9152(8) 0.1170(7) 0.1893(6) 0.024(2) Uani 1 1 d . . . C78 C 0.8442(8) 0.1876(7) 0.1896(6) 0.025(2) Uani 1 1 d . . . C79 C 0.7020(8) 0.1711(8) 0.1458(7) 0.030(2) Uani 1 1 d . . . C80 C 0.6374(8) 0.0839(7) 0.1039(6) 0.023(2) Uani 1 1 d . . . C81 C 0.7123(8) 0.0100(7) 0.1028(6) 0.024(2) Uani 1 1 d . . . C82 C 0.6234(8) -0.0517(7) 0.1126(6) 0.026(2) Uani 1 1 d . . . C83 C 0.6729(9) -0.0933(7) 0.1639(6) 0.025(2) Uani 1 1 d . . . C84 C 0.8144(8) -0.0781(7) 0.2074(6) 0.025(2) Uani 1 1 d . . . C85 C 0.9004(8) -0.0191(7) 0.1972(6) 0.026(2) Uani 1 1 d . . . C86 C 0.8480(8) 0.0269(7) 0.1457(6) 0.026(2) Uani 1 1 d . . . C87 C 1.0076(9) 0.1286(8) 0.0132(7) 0.037(3) Uani 1 1 d . . . N1 N 0.5282(6) 0.2664(6) 0.6829(5) 0.0237(18) Uani 1 1 d . . . O1 O 0.7361(7) 0.5882(5) 0.5365(5) 0.0401(19) Uani 1 1 d . . . O2 O 0.4993(7) 0.5110(5) 0.6859(5) 0.0380(18) Uani 1 1 d . . . O3 O 1.0796(6) 0.4936(5) 0.6133(4) 0.0322(17) Uani 1 1 d . . . P1 P 0.8699(2) 0.47385(18) 0.78753(16) 0.0213(6) Uani 1 1 d . . . S1 S 0.8759(2) 0.0729(2) -0.04587(19) 0.0499(9) Uani 1 1 d . . . S2 S 1.1393(3) 0.1831(3) 0.0727(3) 0.0657(10) Uani 1 1 d . . . Re1 Re 0.78921(3) 0.48175(3) 0.64604(3) 0.01818(12) Uani 1 1 d . . . H1' H 0.8290 0.5800 0.6982 0.022 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.016(2) 0.007(3) 0.030(3) 0.010(3) 0.007(2) -0.0015(19) C2 0.016(2) 0.007(3) 0.030(3) 0.010(3) 0.007(2) -0.0015(19) C3 0.016(2) 0.007(3) 0.030(3) 0.010(3) 0.007(2) -0.0015(19) C4 0.018(4) 0.022(6) 0.008(5) 0.002(4) -0.002(3) 0.000(4) C5 0.027(4) 0.025(6) 0.020(5) 0.006(5) 0.005(4) 0.005(4) C6 0.032(5) 0.036(8) 0.039(7) 0.010(6) 0.009(5) 0.011(5) C7 0.030(5) 0.057(9) 0.028(6) 0.017(6) 0.016(4) 0.009(5) C8 0.037(5) 0.050(8) 0.027(6) 0.020(6) 0.012(4) 0.003(5) C9 0.035(5) 0.037(7) 0.015(5) 0.013(5) 0.001(4) -0.002(5) C10 0.025(4) 0.024(6) 0.018(5) 0.011(5) 0.004(4) 0.001(4) C11 0.038(5) 0.034(8) 0.031(6) 0.010(6) 0.007(5) 0.004(5) C12 0.041(5) 0.036(8) 0.045(7) 0.020(6) -0.015(5) -0.007(5) C13 0.028(5) 0.062(10) 0.060(9) 0.042(8) -0.001(5) -0.008(6) C14 0.031(5) 0.080(11) 0.063(9) 0.055(9) 0.017(5) 0.012(6) C15 0.033(5) 0.048(8) 0.023(6) 0.021(6) 0.003(4) 0.001(5) C16 0.028(4) 0.025(6) 0.017(5) 0.008(5) 0.008(4) 0.001(4) C17 0.035(5) 0.027(7) 0.022(6) 0.007(5) -0.006(4) 0.002(5) C18 0.047(6) 0.030(7) 0.028(6) 0.012(6) 0.003(5) 0.012(5) C19 0.059(6) 0.025(7) 0.021(6) 0.015(5) 0.009(5) 0.015(5) C20 0.040(5) 0.022(6) 0.017(5) 0.005(5) 0.007(4) -0.001(4) C21 0.036(4) 0.015(6) 0.006(5) 0.001(4) -0.006(4) 0.004(4) C22 0.030(4) 0.015(6) 0.013(5) 0.004(4) 0.009(4) 0.003(4) C23 0.038(5) 0.024(7) 0.031(6) 0.015(5) 0.016(4) 0.001(4) C24 0.028(4) 0.024(6) 0.024(6) 0.006(5) 0.011(4) 0.003(4) C25 0.023(4) 0.016(6) 0.014(5) 0.003(4) 0.003(3) -0.004(4) C26 0.020(4) 0.020(6) 0.014(5) 0.006(4) 0.009(3) -0.001(4) C27 0.022(4) 0.016(5) 0.005(4) 0.001(4) 0.002(3) 0.002(4) C28 0.026(4) 0.010(5) 0.012(5) 0.003(4) 0.005(3) 0.002(4) C29 0.024(4) 0.018(6) 0.018(5) 0.004(4) 0.007(4) 0.009(4) C30 0.023(4) 0.019(6) 0.019(5) 0.013(5) 0.012(4) 0.011(4) C31 0.013(4) 0.024(6) 0.027(6) 0.009(5) 0.007(4) 0.004(4) C32 0.010(3) 0.027(6) 0.031(6) 0.013(5) 0.008(4) -0.001(4) C33 0.023(4) 0.021(6) 0.017(5) 0.011(5) 0.008(4) -0.002(4) C34 0.025(4) 0.026(6) 0.016(5) 0.010(5) 0.007(4) -0.009(4) C35 0.029(4) 0.023(6) 0.009(5) 0.007(4) 0.001(4) 0.001(4) C36 0.031(4) 0.018(6) 0.005(4) 0.006(4) 0.005(4) 0.007(4) C39 0.021(4) 0.021(6) 0.012(5) 0.008(4) -0.005(3) -0.003(4) C40 0.013(3) 0.017(6) 0.010(5) -0.002(4) -0.005(3) -0.001(3) C41 0.013(3) 0.022(6) 0.019(5) 0.011(5) -0.006(3) -0.005(4) C42 0.020(4) 0.016(6) 0.013(5) 0.007(4) 0.003(3) -0.004(4) C43 0.019(4) 0.016(6) 0.021(5) 0.013(4) 0.005(3) 0.000(4) C44 0.025(4) 0.009(5) 0.024(5) 0.010(4) 0.006(4) 0.004(4) C45 0.027(4) 0.016(6) 0.024(5) 0.014(5) 0.004(4) 0.001(4) C46 0.021(4) 0.020(6) 0.024(5) 0.010(5) -0.001(4) 0.007(4) C47 0.007(3) 0.028(6) 0.021(5) 0.010(5) -0.003(3) 0.002(4) C48 0.012(4) 0.029(7) 0.023(5) 0.008(5) -0.006(3) 0.001(4) C49 0.015(4) 0.023(6) 0.022(5) 0.003(5) -0.005(3) -0.010(4) C50 0.015(4) 0.021(6) 0.027(6) 0.007(5) 0.005(4) -0.007(4) C51 0.033(5) 0.017(6) 0.022(6) 0.005(5) 0.008(4) -0.012(4) C52 0.025(4) 0.017(6) 0.022(5) 0.010(5) 0.005(4) -0.008(4) C53 0.036(5) 0.018(6) 0.029(6) 0.018(5) 0.006(4) 0.002(4) C54 0.034(4) 0.019(6) 0.015(5) 0.014(5) 0.000(4) 0.000(4) C55 0.033(4) 0.019(6) 0.021(5) 0.013(5) 0.002(4) 0.009(4) C56 0.017(4) 0.028(6) 0.017(5) 0.014(5) -0.001(3) 0.005(4) C57 0.015(4) 0.021(6) 0.022(5) 0.009(5) -0.001(3) 0.005(4) C58 0.007(3) 0.024(6) 0.023(5) 0.010(5) 0.000(3) 0.001(3) C59 0.010(3) 0.028(6) 0.024(5) 0.010(5) 0.008(3) -0.003(4) C60 0.022(4) 0.025(6) 0.019(5) 0.009(5) 0.009(4) -0.001(4) C61 0.029(4) 0.016(6) 0.025(5) 0.014(5) 0.009(4) -0.003(4) C62 0.024(4) 0.024(6) 0.025(5) 0.014(5) 0.005(4) 0.004(4) C63 0.030(3) 0.029(4) 0.017(4) 0.019(3) 0.000(3) 0.005(3) C64 0.030(3) 0.029(4) 0.017(4) 0.019(3) 0.000(3) 0.005(3) C65 0.020(4) 0.037(7) 0.016(5) 0.013(5) -0.003(4) 0.002(4) C66 0.034(5) 0.040(7) 0.009(5) 0.015(5) -0.008(4) -0.002(5) C67 0.032(4) 0.026(7) 0.011(5) 0.001(5) -0.005(4) -0.005(4) C68 0.019(4) 0.021(6) 0.024(5) 0.008(5) -0.008(4) -0.010(4) C69 0.034(5) 0.026(7) 0.014(5) 0.006(5) 0.001(4) -0.011(4) C70 0.037(5) 0.020(6) 0.022(6) 0.006(5) 0.001(4) -0.005(4) C71 0.030(4) 0.019(6) 0.026(6) 0.011(5) 0.001(4) -0.003(4) C72 0.046(5) 0.013(6) 0.024(6) 0.008(5) 0.010(4) 0.011(4) C73 0.026(4) 0.010(5) 0.030(6) 0.010(5) 0.005(4) 0.012(4) C74 0.018(4) 0.029(6) 0.019(5) 0.010(5) 0.009(4) 0.013(4) C75 0.016(4) 0.025(6) 0.031(6) 0.009(5) 0.012(4) 0.011(4) C76 0.022(4) 0.027(7) 0.026(6) 0.010(5) 0.014(4) 0.005(4) C77 0.031(4) 0.030(7) 0.010(5) 0.006(5) 0.013(4) 0.001(4) C78 0.030(4) 0.036(7) 0.022(5) 0.020(5) 0.016(4) 0.003(4) C79 0.026(4) 0.046(8) 0.040 0.038(4) 0.011(4) 0.004(4) C80 0.029(4) 0.032(7) 0.003(4) 0.006(4) 0.000(4) 0.004(4) C81 0.033(4) 0.030(7) 0.005(5) 0.003(5) 0.008(4) 0.001(4) C82 0.033(4) 0.028(7) 0.004(5) -0.003(5) 0.000(4) -0.004(4) C83 0.036(5) 0.012(6) 0.013(5) -0.007(4) 0.005(4) 0.001(4) C84 0.034(5) 0.018(6) 0.021(5) 0.004(5) 0.012(4) 0.008(4) C85 0.030(4) 0.022(6) 0.021(5) 0.001(5) 0.017(4) 0.008(4) C86 0.033(4) 0.037(7) 0.010(5) 0.010(5) 0.014(4) 0.008(5) C87 0.042(5) 0.049(8) 0.037(7) 0.029(6) 0.023(5) 0.019(5) N1 0.028(4) 0.029(5) 0.017(4) 0.012(4) 0.010(3) 0.003(3) O1 0.053(4) 0.040(5) 0.046(5) 0.033(4) 0.018(4) 0.017(4) O2 0.053(4) 0.031(5) 0.043(5) 0.024(4) 0.021(3) 0.018(4) O3 0.033(3) 0.033(5) 0.029(4) 0.013(4) 0.006(3) -0.004(3) P1 0.0250(10) 0.0196(15) 0.0186(13) 0.0084(12) 0.0038(9) 0.0009(10) S1 0.0358(13) 0.073(3) 0.0323(17) 0.0175(17) 0.0038(12) -0.0021(14) S2 0.0407(15) 0.053(3) 0.087(3) 0.024(2) -0.0059(16) -0.0103(15) Re1 0.02124(16) 0.0179(2) 0.0151(2) 0.00724(17) 0.00359(13) 0.00059(13) _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 C1 O1 1.141(10) . ? C1 Re1 1.962(9) . ? C2 O2 1.180(9) . ? C2 Re1 1.949(7) . ? C3 O3 1.108(9) . ? C3 Re1 2.018(7) . ? C4 C5 1.386(13) . ? C4 C9 1.395(12) . ? C4 P1 1.831(8) . ? C5 C6 1.378(13) . ? C5 H5 0.9500 . ? C6 C7 1.396(14) . ? C6 H6 0.9500 . ? C7 C8 1.366(15) . ? C7 H7 0.9500 . ? C8 C9 1.382(13) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.363(14) . ? C10 C15 1.407(12) . ? C10 P1 1.848(8) . ? C11 C12 1.397(13) . ? C11 H11 0.9500 . ? C12 C13 1.359(15) . ? C12 H12 0.9500 . ? C13 C14 1.373(17) . ? C13 H13 0.9500 . ? C14 C15 1.379(14) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C21 1.376(12) . ? C16 C17 1.398(12) . ? C16 P1 1.850(10) . ? C17 C18 1.376(14) . ? C17 H17 0.9500 . ? C18 C19 1.400(14) . ? C18 H18 0.9500 . ? C19 C20 1.360(13) . ? C19 H19 0.9500 . ? C20 C21 1.406(13) . ? C20 H20 0.9500 . ? C21 C22 1.518(11) . ? C22 N1 1.469(10) . ? C22 C26 1.579(11) . ? C22 H22 1.0000 . ? C23 N1 1.451(11) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 N1 1.462(11) . ? C24 C25 1.547(11) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C33 1.529(13) . ? C25 C30 1.530(12) . ? C25 C26 1.610(10) . ? C26 C36 1.527(12) . ? C26 C27 1.590(11) . ? C27 C28 1.453(11) . ? C27 C40 1.482(11) . ? C27 Re1 2.296(9) . ? C28 C43 1.485(11) . ? C28 C29 1.501(11) . ? C28 Re1 2.262(9) . ? C29 C30 1.362(12) . ? C29 C45 1.439(12) . ? C30 C31 1.450(12) . ? C31 C47 1.391(12) . ? C31 C32 1.435(13) . ? C32 C50 1.399(13) . ? C32 C33 1.426(12) . ? C33 C34 1.365(13) . ? C34 C52 1.441(13) . ? C34 C35 1.463(11) . ? C35 C36 1.384(13) . ? C35 C54 1.433(13) . ? C36 C39 1.419(11) . ? C39 C56 1.417(12) . ? C39 C40 1.439(12) . ? C40 C41 1.403(11) . ? C41 C58 1.459(12) . ? C41 C42 1.464(12) . ? C42 C43 1.383(11) . ? C42 C60 1.452(12) . ? C43 C44 1.427(11) . ? C44 C62 1.371(12) . ? C44 C45 1.450(11) . ? C45 C46 1.398(12) . ? C46 C47 1.436(12) . ? C46 C64 1.441(12) . ? C47 C48 1.439(13) . ? C48 C49 1.376(13) . ? C48 C65 1.456(12) . ? C49 C50 1.444(12) . ? C49 C68 1.471(13) . ? C50 C51 1.431(13) . ? C51 C52 1.380(12) . ? C51 C69 1.462(13) . ? C52 C53 1.450(12) . ? C53 C71 1.390(13) . ? C53 C54 1.462(13) . ? C54 C55 1.385(12) . ? C55 C56 1.435(13) . ? C55 C73 1.456(13) . ? C56 C57 1.433(11) . ? C57 C58 1.393(12) . ? C57 C74 1.459(13) . ? C58 C59 1.453(12) . ? C59 C76 1.392(13) . ? C59 C60 1.447(13) . ? C60 C61 1.397(12) . ? C61 C62 1.435(11) . ? C61 C78 1.451(13) . ? C62 C63 1.464(12) . ? C63 C64 1.406(11) . ? C63 C79 1.430(14) . ? C64 C65 1.441(13) . ? C65 C66 1.395(13) . ? C66 C80 1.437(12) . ? C66 C67 1.451(14) . ? C67 C68 1.398(12) . ? C67 C82 1.457(12) . ? C68 C69 1.438(13) . ? C69 C70 1.402(13) . ? C70 C83 1.444(13) . ? C70 C71 1.461(13) . ? C71 C72 1.447(12) . ? C72 C73 1.405(13) . ? C72 C84 1.437(13) . ? C73 C74 1.442(12) . ? C74 C75 1.381(12) . ? C75 C76 1.444(13) . ? C75 C85 1.464(13) . ? C76 C77 1.448(12) . ? C77 C78 1.384(13) . ? C77 C86 1.448(14) . ? C78 C79 1.463(12) . ? C79 C80 1.400(14) . ? C80 C81 1.446(13) . ? C81 C86 1.400(12) . ? C81 C82 1.456(13) . ? C82 C83 1.378(13) . ? C83 C84 1.457(12) . ? C84 C85 1.405(13) . ? C85 C86 1.448(13) . ? C87 S2 1.524(11) . ? C87 S1 1.529(11) . ? P1 Re1 2.470(2) . ? Re1 H1' 1.4859 . ? 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 C1 Re1 177.3(6) . . ? O2 C2 Re1 171.4(8) . . ? O3 C3 Re1 168.7(8) . . ? C5 C4 C9 117.7(8) . . ? C5 C4 P1 120.6(7) . . ? C9 C4 P1 121.6(7) . . ? C6 C5 C4 122.1(9) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C5 C6 C7 119.2(11) . . ? C5 C6 H6 120.4 . . ? C7 C6 H6 120.4 . . ? C8 C7 C6 119.5(9) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C7 C8 C9 121.1(10) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C8 C9 C4 120.4(10) . . ? C8 C9 H9 119.8 . . ? C4 C9 H9 119.8 . . ? C11 C10 C15 119.2(8) . . ? C11 C10 P1 121.1(7) . . ? C15 C10 P1 119.6(7) . . ? C10 C11 C12 121.2(9) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C13 C12 C11 118.8(11) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? C12 C13 C14 121.2(10) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C13 C14 C15 120.3(10) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C10 119.2(10) . . ? C14 C15 H15 120.4 . . ? C10 C15 H15 120.4 . . ? C21 C16 C17 119.2(9) . . ? C21 C16 P1 119.7(7) . . ? C17 C16 P1 120.8(7) . . ? C18 C17 C16 120.9(9) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 119.8(9) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C20 C19 C18 119.2(10) . . ? C20 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? C19 C20 C21 121.5(9) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C16 C21 C20 119.3(8) . . ? C16 C21 C22 121.1(8) . . ? C20 C21 C22 119.5(8) . . ? N1 C22 C21 117.1(7) . . ? N1 C22 C26 103.9(6) . . ? C21 C22 C26 111.8(7) . . ? N1 C22 H22 107.9 . . ? C21 C22 H22 107.9 . . ? C26 C22 H22 107.9 . . ? N1 C23 H23A 109.5 . . ? N1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N1 C24 C25 103.7(7) . . ? N1 C24 H24A 111.0 . . ? C25 C24 H24A 111.0 . . ? N1 C24 H24B 111.0 . . ? C25 C24 H24B 111.0 . . ? H24A C24 H24B 109.0 . . ? C33 C25 C30 100.5(7) . . ? C33 C25 C24 107.4(7) . . ? C30 C25 C24 116.4(7) . . ? C33 C25 C26 115.1(7) . . ? C30 C25 C26 114.1(6) . . ? C24 C25 C26 103.6(6) . . ? C36 C26 C22 111.6(7) . . ? C36 C26 C27 102.4(6) . . ? C22 C26 C27 112.4(7) . . ? C36 C26 C25 113.0(7) . . ? C22 C26 C25 100.9(6) . . ? C27 C26 C25 117.0(7) . . ? C28 C27 C40 115.4(7) . . ? C28 C27 C26 120.7(6) . . ? C40 C27 C26 105.3(7) . . ? C28 C27 Re1 70.1(5) . . ? C40 C27 Re1 119.5(5) . . ? C26 C27 Re1 123.2(5) . . ? C27 C28 C43 119.5(7) . . ? C27 C28 C29 119.2(7) . . ? C43 C28 C29 103.6(7) . . ? C27 C28 Re1 72.7(5) . . ? C43 C28 Re1 113.8(6) . . ? C29 C28 Re1 127.1(6) . . ? C30 C29 C45 120.4(8) . . ? C30 C29 C28 123.3(8) . . ? C45 C29 C28 108.3(7) . . ? C29 C30 C31 118.5(8) . . ? C29 C30 C25 125.1(7) . . ? C31 C30 C25 109.1(7) . . ? C47 C31 C32 119.4(9) . . ? C47 C31 C30 121.8(8) . . ? C32 C31 C30 108.4(8) . . ? C50 C32 C33 120.5(9) . . ? C50 C32 C31 121.2(9) . . ? C33 C32 C31 108.8(8) . . ? C34 C33 C32 120.1(9) . . ? C34 C33 C25 123.7(8) . . ? C32 C33 C25 109.9(8) . . ? C33 C34 C52 119.8(8) . . ? C33 C34 C35 120.8(9) . . ? C52 C34 C35 108.3(8) . . ? C36 C35 C54 120.2(7) . . ? C36 C35 C34 120.0(8) . . ? C54 C35 C34 107.9(8) . . ? C35 C36 C39 119.6(8) . . ? C35 C36 C26 124.3(7) . . ? C39 C36 C26 111.3(8) . . ? C56 C39 C36 120.9(8) . . ? C56 C39 C40 121.3(7) . . ? C36 C39 C40 108.3(7) . . ? C41 C40 C39 117.7(8) . . ? C41 C40 C27 123.1(8) . . ? C39 C40 C27 111.3(7) . . ? C40 C41 C58 121.2(8) . . ? C40 C41 C42 119.1(7) . . ? C58 C41 C42 107.0(7) . . ? C43 C42 C60 119.2(7) . . ? C43 C42 C41 119.4(7) . . ? C60 C42 C41 108.6(8) . . ? C42 C43 C44 120.1(8) . . ? C42 C43 C28 121.8(7) . . ? C44 C43 C28 110.7(6) . . ? C62 C44 C43 120.8(7) . . ? C62 C44 C45 121.7(8) . . ? C43 C44 C45 107.1(7) . . ? C46 C45 C29 121.5(8) . . ? C46 C45 C44 118.0(8) . . ? C29 C45 C44 109.3(7) . . ? C45 C46 C47 118.5(8) . . ? C45 C46 C64 121.5(7) . . ? C47 C46 C64 108.2(8) . . ? C31 C47 C46 119.3(8) . . ? C31 C47 C48 120.4(9) . . ? C46 C47 C48 108.5(8) . . ? C49 C48 C47 119.5(9) . . ? C49 C48 C65 120.4(9) . . ? C47 C48 C65 107.4(8) . . ? C48 C49 C50 121.6(9) . . ? C48 C49 C68 120.3(8) . . ? C50 C49 C68 106.8(8) . . ? C32 C50 C51 119.2(8) . . ? C32 C50 C49 118.0(9) . . ? C51 C50 C49 109.3(8) . . ? C52 C51 C50 119.6(9) . . ? C52 C51 C69 120.4(8) . . ? C50 C51 C69 107.9(8) . . ? C51 C52 C34 120.6(9) . . ? C51 C52 C53 120.3(8) . . ? C34 C52 C53 107.8(7) . . ? C71 C53 C52 120.5(8) . . ? C71 C53 C54 119.7(8) . . ? C52 C53 C54 107.9(8) . . ? C55 C54 C35 120.6(9) . . ? C55 C54 C53 119.8(8) . . ? C35 C54 C53 108.1(7) . . ? C54 C55 C56 120.0(9) . . ? C54 C55 C73 120.6(8) . . ? C56 C55 C73 107.3(8) . . ? C39 C56 C57 120.2(8) . . ? C39 C56 C55 118.6(7) . . ? C57 C56 C55 109.4(8) . . ? C58 C57 C56 119.3(8) . . ? C58 C57 C74 119.7(8) . . ? C56 C57 C74 107.5(8) . . ? C57 C58 C59 120.7(8) . . ? C57 C58 C41 120.1(7) . . ? C59 C58 C41 108.1(7) . . ? C76 C59 C60 120.3(8) . . ? C76 C59 C58 119.0(9) . . ? C60 C59 C58 108.6(7) . . ? C61 C60 C59 120.9(9) . . ? C61 C60 C42 120.4(8) . . ? C59 C60 C42 107.6(8) . . ? C60 C61 C62 118.7(8) . . ? C60 C61 C78 118.3(9) . . ? C62 C61 C78 108.3(8) . . ? C44 C62 C61 120.7(8) . . ? C44 C62 C63 120.2(7) . . ? C61 C62 C63 107.8(8) . . ? C64 C63 C79 121.1(9) . . ? C64 C63 C62 118.7(8) . . ? C79 C63 C62 108.2(7) . . ? C63 C64 C65 118.7(9) . . ? C63 C64 C46 119.9(8) . . ? C65 C64 C46 108.0(8) . . ? C66 C65 C64 120.6(8) . . ? C66 C65 C48 119.9(9) . . ? C64 C65 C48 107.9(8) . . ? C65 C66 C80 119.9(9) . . ? C65 C66 C67 120.1(8) . . ? C80 C66 C67 107.7(8) . . ? C68 C67 C66 120.2(9) . . ? C68 C67 C82 118.6(9) . . ? C66 C67 C82 108.4(8) . . ? C67 C68 C69 120.9(8) . . ? C67 C68 C49 119.2(9) . . ? C69 C68 C49 108.3(8) . . ? C70 C69 C68 119.9(8) . . ? C70 C69 C51 119.3(8) . . ? C68 C69 C51 107.7(9) . . ? C69 C70 C83 119.3(9) . . ? C69 C70 C71 120.1(9) . . ? C83 C70 C71 108.6(8) . . ? C53 C71 C72 120.8(8) . . ? C53 C71 C70 119.5(8) . . ? C72 C71 C70 107.1(8) . . ? C73 C72 C84 119.6(8) . . ? C73 C72 C71 119.6(9) . . ? C84 C72 C71 108.6(8) . . ? C72 C73 C74 120.5(8) . . ? C72 C73 C55 119.6(8) . . ? C74 C73 C55 108.2(8) . . ? C75 C74 C73 119.8(8) . . ? C75 C74 C57 119.4(9) . . ? C73 C74 C57 107.7(7) . . ? C74 C75 C76 120.9(9) . . ? C74 C75 C85 120.7(8) . . ? C76 C75 C85 107.2(8) . . ? C59 C76 C75 120.4(9) . . ? C59 C76 C77 119.0(9) . . ? C75 C76 C77 109.1(8) . . ? C78 C77 C86 119.7(8) . . ? C78 C77 C76 120.6(9) . . ? C86 C77 C76 107.4(9) . . ? C77 C78 C61 120.9(8) . . ? C77 C78 C79 120.0(9) . . ? C61 C78 C79 107.5(8) . . ? C80 C79 C63 119.5(7) . . ? C80 C79 C78 120.1(9) . . ? C63 C79 C78 108.1(9) . . ? C79 C80 C66 120.2(9) . . ? C79 C80 C81 119.8(8) . . ? C66 C80 C81 108.7(9) . . ? C86 C81 C80 119.6(9) . . ? C86 C81 C82 119.7(8) . . ? C80 C81 C82 108.0(7) . . ? C83 C82 C81 120.0(8) . . ? C83 C82 C67 120.5(8) . . ? C81 C82 C67 107.1(9) . . ? C82 C83 C70 120.8(8) . . ? C82 C83 C84 121.1(8) . . ? C70 C83 C84 107.3(8) . . ? C85 C84 C72 120.5(8) . . ? C85 C84 C83 118.8(9) . . ? C72 C84 C83 108.4(7) . . ? C84 C85 C86 120.3(8) . . ? C84 C85 C75 118.9(8) . . ? C86 C85 C75 107.8(8) . . ? C81 C86 C77 120.8(9) . . ? C81 C86 C85 120.1(8) . . ? C77 C86 C85 108.5(8) . . ? S2 C87 S1 179.1(8) . . ? C23 N1 C24 112.8(7) . . ? C23 N1 C22 111.8(7) . . ? C24 N1 C22 101.7(6) . . ? C4 P1 C10 103.0(4) . . ? C4 P1 C16 102.1(4) . . ? C10 P1 C16 104.4(4) . . ? C4 P1 Re1 113.8(3) . . ? C10 P1 Re1 110.4(3) . . ? C16 P1 Re1 121.2(3) . . ? C2 Re1 C1 88.9(3) . . ? C2 Re1 C3 173.6(4) . . ? C1 Re1 C3 86.9(3) . . ? C2 Re1 C28 89.6(3) . . ? C1 Re1 C28 80.4(3) . . ? C3 Re1 C28 94.5(3) . . ? C2 Re1 C27 96.0(3) . . ? C1 Re1 C27 117.1(3) . . ? C3 Re1 C27 90.2(3) . . ? C28 Re1 C27 37.2(3) . . ? C2 Re1 P1 92.0(3) . . ? C1 Re1 P1 151.9(3) . . ? C3 Re1 P1 89.4(2) . . ? C28 Re1 P1 127.6(2) . . ? C27 Re1 P1 90.7(2) . . ? C2 Re1 H1' 93.9 . . ? C1 Re1 H1' 65.3 . . ? C3 Re1 H1' 80.0 . . ? C28 Re1 H1' 145.4 . . ? C27 Re1 H1' 169.9 . . ? P1 Re1 H1' 86.7 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 4.189 _refine_diff_density_min -1.353 _refine_diff_density_rms 0.181 data_a13609 _database_code_depnum_ccdc_archive 'CCDC 903346' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C88 H19 N O7 P Re2' _chemical_formula_sum 'C88 H19 N O7 P Re2' _chemical_formula_weight 1605.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 32.402(3) _cell_length_b 18.559(2) _cell_length_c 22.676(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.232(8) _cell_angle_gamma 90.00 _cell_volume 13275(3) _cell_formula_units_Z 8 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour brown(dark) _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.607 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6200 _exptl_absorpt_coefficient_mu 3.729 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5081 _exptl_absorpt_correction_T_max 0.9637 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43871 _diffrn_reflns_av_R_equivalents 0.1622 _diffrn_reflns_av_sigmaI/netI 0.2517 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 25.02 _reflns_number_total 11665 _reflns_number_gt 4149 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0648P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11665 _refine_ls_number_parameters 577 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2002 _refine_ls_R_factor_gt 0.0725 _refine_ls_wR_factor_ref 0.1765 _refine_ls_wR_factor_gt 0.1471 _refine_ls_goodness_of_fit_ref 0.868 _refine_ls_restrained_S_all 0.868 _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 C1 C 0.8502(6) 0.1798(10) 0.2232(9) 0.081(5) Uani 1 1 d . . . C2 C 0.8072(5) 0.1040(12) 0.2924(9) 0.081(5) Uani 1 1 d . . . C3 C 0.7688(4) 0.2122(9) 0.2339(7) 0.052(5) Uani 1 1 d . . . C4 C 0.8817(5) 0.4024(10) 0.3154(9) 0.070(6) Uani 1 1 d . . . C5 C 0.8231(6) 0.3605(10) 0.1982(13) 0.096(6) Uani 1 1 d . . . C6 C 0.8096(6) 0.4809(11) 0.2778(11) 0.096(6) Uani 1 1 d . . . C7 C 0.7574(5) 0.3632(10) 0.2689(8) 0.067(6) Uani 1 1 d . . . C8 C 0.8200(4) 0.3745(9) 0.3822(7) 0.043(4) Uani 1 1 d . . . C9 C 0.8316(5) 0.4373(10) 0.4164(9) 0.061(5) Uani 1 1 d . . . H9 H 0.8383 0.4790 0.3960 0.073 Uiso 1 1 calc R . . C10 C 0.8338(5) 0.4424(10) 0.4784(10) 0.065(5) Uani 1 1 d . . . H10 H 0.8407 0.4872 0.4985 0.078 Uiso 1 1 calc R . . C11 C 0.8261(4) 0.3825(9) 0.5112(8) 0.044(4) Uani 1 1 d . . . H11 H 0.8290 0.3845 0.5538 0.053 Uiso 1 1 calc R . . C12 C 0.8139(4) 0.3190(8) 0.4783(7) 0.031(4) Uani 1 1 d . . . H12 H 0.8076 0.2770 0.4985 0.038 Uiso 1 1 calc R . . C13 C 0.8110(4) 0.3175(7) 0.4163(7) 0.027(4) Uani 1 1 d . . . C14 C 0.7356(4) 0.2315(8) 0.3673(7) 0.038(4) Uani 1 1 d . . . C15 C 0.7147(4) 0.2876(8) 0.3892(7) 0.049(4) Uani 1 1 d . . . H15 H 0.7305 0.3262 0.4112 0.059 Uiso 1 1 calc R . . C16 C 0.6698(4) 0.2868(9) 0.3787(7) 0.052(4) Uani 1 1 d . . . H16 H 0.6551 0.3255 0.3923 0.062 Uiso 1 1 calc R . . C17 C 0.6481(4) 0.2302(10) 0.3490(8) 0.055(5) Uani 1 1 d . . . H17 H 0.6182 0.2282 0.3444 0.066 Uiso 1 1 calc R . . C18 C 0.6676(4) 0.1758(9) 0.3253(7) 0.046(4) Uani 1 1 d . . . H18 H 0.6512 0.1380 0.3034 0.055 Uiso 1 1 calc R . . C19 C 0.7128(4) 0.1757(8) 0.3335(7) 0.049(5) Uani 1 1 d . . . H19 H 0.7268 0.1389 0.3164 0.059 Uiso 1 1 calc R . . C20 C 0.8108(4) 0.1626(7) 0.4372(7) 0.036(4) Uani 1 1 d . . . C21 C 0.7822(4) 0.1214(8) 0.4615(8) 0.045(4) Uani 1 1 d . . . H21 H 0.7530 0.1333 0.4505 0.054 Uiso 1 1 calc R . . C22 C 0.7945(5) 0.0654(8) 0.4999(7) 0.046(4) Uani 1 1 d . . . H22 H 0.7744 0.0420 0.5178 0.055 Uiso 1 1 calc R . . C23 C 0.8364(4) 0.0420(8) 0.5133(7) 0.051(5) Uani 1 1 d . . . H23 H 0.8447 0.0001 0.5373 0.061 Uiso 1 1 calc R . . C24 C 0.8667(4) 0.0827(7) 0.4900(7) 0.043(4) Uani 1 1 d . . . H24 H 0.8957 0.0689 0.5002 0.052 Uiso 1 1 calc R . . C25 C 0.8545(4) 0.1426(7) 0.4524(6) 0.028(4) Uani 1 1 d . . . C26 C 0.8843(3) 0.1879(7) 0.4269(7) 0.032(4) Uani 1 1 d . . . H26 H 0.8722 0.2377 0.4241 0.039 Uiso 1 1 calc R . . C27 C 0.8973(4) 0.0909(7) 0.3574(7) 0.045(5) Uani 1 1 d . . . H27A H 0.8971 0.0808 0.3149 0.067 Uiso 1 1 calc R . . H27B H 0.8772 0.0588 0.3708 0.067 Uiso 1 1 calc R . . H27C H 0.9259 0.0828 0.3824 0.067 Uiso 1 1 calc R . . C28 C 0.9199(4) 0.2105(8) 0.3498(7) 0.051(4) Uani 1 1 d . . . H28A H 0.9095 0.2590 0.3355 0.061 Uiso 1 1 calc R . . H28B H 0.9311 0.1868 0.3175 0.061 Uiso 1 1 calc R . . C29 C 0.9557(4) 0.2170(7) 0.4086(6) 0.033(3) Uiso 1 1 d . . . C30 C 0.9317(4) 0.1959(7) 0.4632(6) 0.026(3) Uiso 1 1 d . . . C31 C 0.9320(4) 0.2561(7) 0.5106(6) 0.034(4) Uiso 1 1 d . . . C32 C 0.9411(4) 0.2285(7) 0.5699(6) 0.035(4) Uiso 1 1 d . . . C33 C 0.9545(4) 0.1528(7) 0.5661(6) 0.033(4) Uiso 1 1 d . . . C34 C 0.9544(4) 0.1386(7) 0.5060(6) 0.033(4) Uiso 1 1 d . . . C35 C 0.9873(4) 0.0967(7) 0.4942(6) 0.031(4) Uiso 1 1 d . . . C36 C 1.0077(4) 0.1129(7) 0.4445(6) 0.032(4) Uiso 1 1 d . . . C37 C 0.9958(4) 0.1728(8) 0.4107(7) 0.042(4) Uiso 1 1 d . . . C38 C 1.0277(5) 0.2211(9) 0.3946(7) 0.059(5) Uiso 1 1 d . . . C39 C 1.0153(4) 0.2935(8) 0.3988(6) 0.042(4) Uiso 1 1 d . . . C40 C 0.9740(4) 0.2967(8) 0.4157(7) 0.045(4) Uiso 1 1 d . . . C41 C 0.9640(4) 0.3478(8) 0.4535(7) 0.043(4) Uiso 1 1 d . . . C42 C 0.9445(4) 0.3286(8) 0.5027(7) 0.047 Uiso 1 1 d . . . C43 C 0.9624(4) 0.3706(8) 0.5553(7) 0.043 Uiso 1 1 d . . . C44 C 0.9681(4) 0.3439(8) 0.6114(7) 0.044(4) Uiso 1 1 d . . . C45 C 0.9580(4) 0.2677(7) 0.6206(6) 0.036(4) Uiso 1 1 d . . . C46 C 0.9891(5) 0.2368(8) 0.6698(7) 0.049(4) Uiso 1 1 d . . . C47 C 1.0032(4) 0.1669(8) 0.6681(7) 0.047(4) Uiso 1 1 d . . . C48 C 0.9853(4) 0.1255(7) 0.6144(6) 0.033(4) Uiso 1 1 d . . . C49 C 1.0182(4) 0.0804(7) 0.6015(6) 0.035(4) Uiso 1 1 d . . . C50 C 1.0188(4) 0.0667(7) 0.5431(6) 0.036(4) Uiso 1 1 d . . . C51 C 1.0588(4) 0.0675(8) 0.5235(7) 0.048(4) Uiso 1 1 d . . . C52 C 1.0535(4) 0.0959(7) 0.4652(7) 0.037(4) Uiso 1 1 d . . . C53 C 1.0832(5) 0.1397(9) 0.4492(7) 0.056(5) Uiso 1 1 d . . . C54 C 1.0720(5) 0.2010(9) 0.4137(7) 0.057(5) Uiso 1 1 d . . . C55 C 1.1026(5) 0.2613(10) 0.4350(8) 0.072(6) Uiso 1 1 d . . . C56 C 1.0887(5) 0.3314(9) 0.4373(7) 0.049(4) Uiso 1 1 d . . . C57 C 1.0427(5) 0.3501(9) 0.4210(8) 0.057(5) Uiso 1 1 d . . . C58 C 1.0340(5) 0.4017(8) 0.4585(7) 0.047(4) Uiso 1 1 d . . . C59 C 0.9953(4) 0.4041(8) 0.4769(7) 0.042(4) Uiso 1 1 d . . . C60 C 0.9955(4) 0.4176(8) 0.5348(7) 0.045(4) Uiso 1 1 d . . . C61 C 1.0315(4) 0.4330(8) 0.5812(7) 0.045(4) Uiso 1 1 d . . . C62 C 1.0386(5) 0.4056(9) 0.6387(8) 0.059(5) Uiso 1 1 d . . . C63 C 1.0092(5) 0.3592(9) 0.6580(7) 0.057(5) Uiso 1 1 d . . . C64 C 1.0208(5) 0.2939(8) 0.6925(7) 0.053(4) Uiso 1 1 d . . . C65 C 1.0632(5) 0.2755(9) 0.7105(7) 0.051(4) Uiso 1 1 d . . . C66 C 1.0766(5) 0.2057(9) 0.7085(7) 0.052(4) Uiso 1 1 d . . . C67 C 1.0486(5) 0.1519(9) 0.6880(7) 0.056(5) Uiso 1 1 d . . . C68 C 1.0580(5) 0.0951(8) 0.6485(8) 0.054(5) Uiso 1 1 d . . . C69 C 1.0941(5) 0.0970(8) 0.6279(7) 0.046(4) Uiso 1 1 d . . . C70 C 1.0961(4) 0.0840(8) 0.5677(7) 0.045(4) Uiso 1 1 d . . . C71 C 1.1286(5) 0.1303(8) 0.5523(8) 0.051(4) Uiso 1 1 d . . . C72 C 1.1225(4) 0.1564(9) 0.4965(7) 0.050(4) Uiso 1 1 d . . . C73 C 1.1343(5) 0.2299(9) 0.4839(8) 0.062(5) Uiso 1 1 d . . . C74 C 1.1516(5) 0.2724(9) 0.5356(8) 0.056(5) Uiso 1 1 d . . . C75 C 1.1375(5) 0.3459(9) 0.5375(7) 0.050(4) Uiso 1 1 d . . . C76 C 1.1064(5) 0.3742(9) 0.4870(8) 0.061(5) Uiso 1 1 d . . . C77 C 1.0734(5) 0.4205(8) 0.5057(7) 0.051(4) Uiso 1 1 d . . . C78 C 1.0721(5) 0.4335(9) 0.5631(8) 0.060(5) Uiso 1 1 d . . . C79 C 1.1030(5) 0.4047(8) 0.6122(7) 0.048(4) Uiso 1 1 d . . . C80 C 1.1363(5) 0.3603(9) 0.5977(7) 0.052(5) Uiso 1 1 d . . . C81 C 1.1485(4) 0.2931(8) 0.6342(7) 0.044(4) Uiso 1 1 d . . . C82 C 1.1579(4) 0.2416(8) 0.5918(7) 0.044(4) Uiso 1 1 d . . . C83 C 1.1470(4) 0.1718(8) 0.6034(7) 0.046(4) Uiso 1 1 d . . . C84 C 1.1274(5) 0.1550(9) 0.6487(8) 0.056(5) Uiso 1 1 d . . . C85 C 1.1165(4) 0.2052(8) 0.6881(7) 0.048(4) Uiso 1 1 d . . . C86 C 1.1283(4) 0.2806(9) 0.6803(7) 0.054(4) Uiso 1 1 d . . . C87 C 1.0932(5) 0.3246(9) 0.6933(7) 0.052(5) Uiso 1 1 d . . . C88 C 1.0830(5) 0.3865(9) 0.6611(8) 0.055(5) Uiso 1 1 d . . . N1 N 0.8847(3) 0.1672(7) 0.3635(6) 0.042(3) Uani 1 1 d . . . O1 O 0.8651(4) 0.1687(9) 0.1852(7) 0.108(5) Uani 1 1 d . . . O2 O 0.7935(3) 0.0371(6) 0.2949(6) 0.077(4) Uani 1 1 d . . . O3 O 0.7397(3) 0.2205(7) 0.1977(5) 0.080(4) Uani 1 1 d . . . O4 O 0.9144(4) 0.4216(7) 0.3325(6) 0.089(5) Uani 1 1 d . . . O5 O 0.8227(5) 0.3545(11) 0.1470(7) 0.144(8) Uani 1 1 d . . . O6 O 0.8054(4) 0.5363(8) 0.2687(6) 0.101(5) Uani 1 1 d . . . O7 O 0.7231(4) 0.3636(7) 0.2582(6) 0.094(5) Uani 1 1 d . . . P1 P 0.79318(10) 0.2308(2) 0.37879(19) 0.0391(11) Uani 1 1 d . . . Re1 Re 0.822164(19) 0.19496(4) 0.29247(3) 0.0454(2) Uani 1 1 d . . . Re2 Re 0.82099(2) 0.37456(4) 0.28483(4) 0.0573(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.054(8) 0.085(12) 0.085(12) -0.048(9) -0.025(7) 0.050(8) C2 0.054(8) 0.085(12) 0.085(12) -0.048(9) -0.025(7) 0.050(8) C3 0.029(8) 0.072(13) 0.048(11) 0.001(11) -0.007(8) -0.001(10) C4 0.025(9) 0.085(15) 0.094(16) 0.044(12) 0.000(10) 0.002(10) C5 0.068(9) 0.055(11) 0.140(16) 0.061(11) -0.027(10) -0.025(8) C6 0.068(9) 0.055(11) 0.140(16) 0.061(11) -0.027(10) -0.025(8) C7 0.042(10) 0.084(15) 0.070(14) 0.009(12) 0.002(10) -0.027(11) C8 0.025(8) 0.048(12) 0.051(12) 0.008(11) -0.003(7) -0.003(8) C9 0.055(11) 0.068(15) 0.062(15) 0.015(12) 0.016(10) -0.029(10) C10 0.061(11) 0.039(13) 0.088(17) -0.012(13) 0.004(11) -0.018(10) C11 0.031(8) 0.038(12) 0.056(12) 0.015(10) -0.004(8) -0.015(8) C12 0.033(8) 0.015(9) 0.051(11) 0.018(9) 0.019(8) -0.003(7) C13 0.022(7) 0.017(9) 0.042(10) 0.014(8) 0.010(7) -0.006(6) C14 0.011(6) 0.043(11) 0.054(11) 0.013(9) -0.003(7) -0.001(7) C15 0.030(8) 0.042(11) 0.073(12) -0.014(10) 0.004(7) 0.012(9) C16 0.040(9) 0.044(11) 0.074(13) -0.012(11) 0.022(8) 0.005(9) C17 0.019(8) 0.079(15) 0.067(13) -0.002(11) 0.011(8) 0.006(9) C18 0.020(8) 0.063(12) 0.049(11) 0.010(9) -0.004(7) -0.010(8) C19 0.020(8) 0.044(11) 0.087(14) 0.010(10) 0.020(8) -0.001(7) C20 0.023(7) 0.015(9) 0.065(12) 0.001(8) 0.002(7) 0.013(7) C21 0.023(8) 0.027(10) 0.087(14) -0.004(10) 0.020(8) -0.011(7) C22 0.047(10) 0.034(11) 0.062(12) 0.017(10) 0.021(9) -0.005(8) C23 0.032(9) 0.021(10) 0.092(14) 0.012(9) 0.000(9) 0.008(7) C24 0.038(9) 0.016(10) 0.075(13) 0.005(9) 0.009(8) -0.008(8) C25 0.019(7) 0.025(10) 0.041(10) -0.003(8) 0.012(6) 0.000(6) C26 0.014(6) 0.034(10) 0.051(11) 0.022(9) 0.011(6) 0.005(6) C27 0.024(8) 0.035(11) 0.069(13) 0.006(9) -0.002(8) 0.001(7) C28 0.033(8) 0.056(12) 0.057(11) 0.005(10) -0.004(7) -0.002(9) N1 0.025(6) 0.028(9) 0.071(11) 0.011(8) 0.009(6) -0.008(6) O1 0.074(9) 0.160(14) 0.103(12) -0.017(11) 0.046(8) 0.040(9) O2 0.054(7) 0.057(9) 0.113(11) -0.036(8) 0.002(7) -0.017(6) O3 0.047(7) 0.113(11) 0.068(9) 0.004(8) -0.013(6) -0.004(8) O4 0.039(7) 0.085(10) 0.132(13) 0.041(9) 0.000(8) -0.010(7) O5 0.128(13) 0.24(2) 0.060(11) 0.068(13) 0.010(10) -0.009(12) O6 0.084(9) 0.094(11) 0.110 0.068(10) -0.009(8) -0.035(9) O7 0.036(7) 0.105(11) 0.123(12) 0.035(9) -0.020(7) -0.009(8) P1 0.0200(18) 0.040(3) 0.054(3) 0.002(2) 0.0014(18) -0.0004(19) Re1 0.0263(3) 0.0582(6) 0.0497(5) -0.0012(4) 0.0043(3) 0.0010(4) Re2 0.0342(4) 0.0651(6) 0.0674(6) 0.0215(5) 0.0011(4) -0.0047(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 C1 O1 1.10(2) . ? C1 Re1 2.01(2) . ? C2 O2 1.32(2) . ? C2 Re1 1.76(2) . ? C3 O3 1.110(14) . ? C3 Re1 1.949(15) . ? C4 O4 1.101(16) . ? C4 Re2 1.997(17) . ? C5 O5 1.16(3) . ? C5 Re2 2.00(3) . ? C6 O6 1.052(18) . ? C6 Re2 2.01(2) . ? C7 O7 1.082(16) . ? C7 Re2 2.021(17) . ? C8 C13 1.382(18) . ? C8 C9 1.40(2) . ? C8 Re2 2.214(16) . ? C9 C10 1.40(2) . ? C9 H9 0.9500 . ? C10 C11 1.39(2) . ? C10 H10 0.9500 . ? C11 C12 1.401(18) . ? C11 H11 0.9500 . ? C12 C13 1.388(18) . ? C12 H12 0.9500 . ? C13 P1 1.849(14) . ? C14 C19 1.395(18) . ? C14 C15 1.395(18) . ? C14 P1 1.823(12) . ? C15 C16 1.421(17) . ? C15 H15 0.9500 . ? C16 C17 1.355(19) . ? C16 H16 0.9500 . ? C17 C18 1.363(19) . ? C17 H17 0.9500 . ? C18 C19 1.435(17) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.408(18) . ? C20 C25 1.426(15) . ? C20 P1 1.826(14) . ? C21 C22 1.355(18) . ? C21 H21 0.9500 . ? C22 C23 1.391(17) . ? C22 H22 0.9500 . ? C23 C24 1.434(18) . ? C23 H23 0.9500 . ? C24 C25 1.401(17) . ? C24 H24 0.9500 . ? C25 C26 1.494(16) . ? C26 N1 1.491(16) . ? C26 C30 1.576(15) . ? C26 H26 1.0000 . ? C27 N1 1.489(16) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 N1 1.485(16) . ? C28 C29 1.557(17) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C37 1.530(17) . ? C29 C40 1.588(18) . ? C29 C30 1.652(17) . ? C30 C34 1.511(16) . ? C30 C31 1.549(17) . ? C31 C32 1.406(17) . ? C31 C42 1.428(18) . ? C32 C45 1.365(17) . ? C32 C33 1.479(17) . ? C33 C34 1.387(17) . ? C33 C48 1.398(17) . ? C34 C35 1.395(16) . ? C35 C50 1.435(17) . ? C35 C36 1.463(18) . ? C36 C37 1.354(17) . ? C36 C52 1.485(16) . ? C37 C38 1.478(19) . ? C38 C39 1.412(19) . ? C38 C54 1.449(19) . ? C39 C57 1.392(18) . ? C39 C40 1.476(17) . ? C40 C41 1.367(18) . ? C41 C42 1.446(19) . ? C41 C59 1.469(18) . ? C42 C43 1.431(18) . ? C43 C44 1.338(18) . ? C43 C60 1.535(18) . ? C44 C45 1.476(18) . ? C44 C63 1.526(19) . ? C45 C46 1.439(18) . ? C46 C47 1.378(18) . ? C46 C64 1.484(18) . ? C47 C48 1.444(18) . ? C47 C67 1.463(18) . ? C48 C49 1.436(17) . ? C49 C50 1.355(17) . ? C49 C68 1.499(18) . ? C50 C51 1.463(17) . ? C51 C52 1.396(18) . ? C51 C70 1.418(18) . ? C52 C53 1.370(18) . ? C53 C54 1.393(19) . ? C53 C72 1.499(19) . ? C54 C55 1.50(2) . ? C55 C56 1.38(2) . ? C55 C73 1.45(2) . ? C56 C76 1.391(19) . ? C56 C57 1.492(19) . ? C57 C58 1.353(19) . ? C58 C59 1.409(18) . ? C58 C77 1.507(19) . ? C59 C60 1.335(18) . ? C60 C61 1.411(18) . ? C61 C62 1.369(19) . ? C61 C78 1.462(19) . ? C62 C63 1.42(2) . ? C62 C88 1.458(19) . ? C63 C64 1.445(19) . ? C64 C65 1.384(18) . ? C65 C66 1.371(18) . ? C65 C87 1.450(19) . ? C66 C67 1.357(18) . ? C66 C85 1.469(18) . ? C67 C68 1.46(2) . ? C68 C69 1.354(19) . ? C69 C70 1.403(19) . ? C69 C84 1.520(19) . ? C70 C71 1.461(19) . ? C71 C72 1.327(19) . ? C71 C83 1.405(18) . ? C72 C73 1.46(2) . ? C73 C74 1.42(2) . ? C74 C82 1.369(19) . ? C74 C75 1.44(2) . ? C75 C80 1.401(19) . ? C75 C76 1.44(2) . ? C76 C77 1.50(2) . ? C77 C78 1.34(2) . ? C78 C79 1.421(19) . ? C79 C88 1.44(2) . ? C79 C80 1.455(19) . ? C80 C81 1.500(19) . ? C81 C86 1.374(18) . ? C81 C82 1.437(18) . ? C82 C83 1.384(19) . ? C83 C84 1.364(19) . ? C84 C85 1.391(19) . ? C85 C86 1.472(19) . ? C86 C87 1.484(19) . ? C87 C88 1.361(19) . ? N1 Re1 2.340(11) . ? P1 Re1 2.449(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 Re1 177(2) . . ? O2 C2 Re1 175.2(16) . . ? O3 C3 Re1 175.5(15) . . ? O4 C4 Re2 176.0(17) . . ? O5 C5 Re2 177(2) . . ? O6 C6 Re2 172(2) . . ? O7 C7 Re2 173.1(17) . . ? C13 C8 C9 113.0(15) . . ? C13 C8 Re2 127.7(12) . . ? C9 C8 Re2 119.2(13) . . ? C10 C9 C8 124.0(17) . . ? C10 C9 H9 118.0 . . ? C8 C9 H9 118.0 . . ? C11 C10 C9 120.7(17) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 116.8(16) . . ? C10 C11 H11 121.6 . . ? C12 C11 H11 121.6 . . ? C13 C12 C11 120.1(13) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C8 C13 C12 125.3(14) . . ? C8 C13 P1 119.5(12) . . ? C12 C13 P1 115.2(11) . . ? C19 C14 C15 120.7(12) . . ? C19 C14 P1 118.0(11) . . ? C15 C14 P1 121.2(11) . . ? C14 C15 C16 119.7(14) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C17 C16 C15 119.1(14) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C16 C17 C18 122.4(14) . . ? C16 C17 H17 118.8 . . ? C18 C17 H17 118.8 . . ? C17 C18 C19 120.2(14) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C14 C19 C18 117.8(14) . . ? C14 C19 H19 121.1 . . ? C18 C19 H19 121.1 . . ? C21 C20 C25 117.9(13) . . ? C21 C20 P1 122.4(10) . . ? C25 C20 P1 119.0(11) . . ? C22 C21 C20 123.0(13) . . ? C22 C21 H21 118.5 . . ? C20 C21 H21 118.5 . . ? C21 C22 C23 120.7(14) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C22 C23 C24 118.0(14) . . ? C22 C23 H23 121.0 . . ? C24 C23 H23 121.0 . . ? C25 C24 C23 121.3(13) . . ? C25 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? C24 C25 C20 118.8(12) . . ? C24 C25 C26 124.3(11) . . ? C20 C25 C26 116.9(12) . . ? N1 C26 C25 112.2(11) . . ? N1 C26 C30 107.7(10) . . ? C25 C26 C30 119.3(11) . . ? N1 C26 H26 105.5 . . ? C25 C26 H26 105.5 . . ? C30 C26 H26 105.5 . . ? N1 C27 H27A 109.5 . . ? N1 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N1 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N1 C28 C29 108.6(12) . . ? N1 C28 H28A 110.0 . . ? C29 C28 H28A 110.0 . . ? N1 C28 H28B 110.0 . . ? C29 C28 H28B 110.0 . . ? H28A C28 H28B 108.3 . . ? C37 C29 C28 116.5(12) . . ? C37 C29 C40 101.6(10) . . ? C28 C29 C40 110.3(11) . . ? C37 C29 C30 113.0(11) . . ? C28 C29 C30 103.8(10) . . ? C40 C29 C30 111.9(10) . . ? C34 C30 C31 97.9(10) . . ? C34 C30 C26 122.8(10) . . ? C31 C30 C26 106.3(10) . . ? C34 C30 C29 113.9(10) . . ? C31 C30 C29 114.8(10) . . ? C26 C30 C29 101.5(9) . . ? C32 C31 C42 117.3(13) . . ? C32 C31 C30 111.5(12) . . ? C42 C31 C30 123.4(13) . . ? C45 C32 C31 124.6(13) . . ? C45 C32 C33 119.3(12) . . ? C31 C32 C33 106.9(12) . . ? C34 C33 C48 122.8(13) . . ? C34 C33 C32 107.7(12) . . ? C48 C33 C32 117.7(13) . . ? C33 C34 C35 117.7(12) . . ? C33 C34 C30 112.8(12) . . ? C35 C34 C30 123.3(12) . . ? C34 C35 C50 120.5(13) . . ? C34 C35 C36 122.3(12) . . ? C50 C35 C36 108.0(11) . . ? C37 C36 C35 118.9(13) . . ? C37 C36 C52 119.2(13) . . ? C35 C36 C52 107.9(12) . . ? C36 C37 C38 120.9(13) . . ? C36 C37 C29 126.0(13) . . ? C38 C37 C29 107.7(12) . . ? C39 C38 C54 120.2(15) . . ? C39 C38 C37 109.6(13) . . ? C54 C38 C37 118.0(15) . . ? C57 C39 C38 125.0(14) . . ? C57 C39 C40 114.7(14) . . ? C38 C39 C40 110.2(13) . . ? C41 C40 C39 123.3(13) . . ? C41 C40 C29 125.0(12) . . ? C39 C40 C29 106.1(12) . . ? C40 C41 C42 121.3(14) . . ? C40 C41 C59 118.5(13) . . ? C42 C41 C59 106.5(13) . . ? C31 C42 C43 118.8(14) . . ? C31 C42 C41 121.0(14) . . ? C43 C42 C41 110.1(13) . . ? C44 C43 C42 122.1(14) . . ? C44 C43 C60 123.1(13) . . ? C42 C43 C60 103.6(13) . . ? C43 C44 C45 120.2(14) . . ? C43 C44 C63 119.8(14) . . ? C45 C44 C63 105.4(13) . . ? C32 C45 C46 121.0(13) . . ? C32 C45 C44 116.7(13) . . ? C46 C45 C44 110.8(13) . . ? C47 C46 C45 122.1(14) . . ? C47 C46 C64 118.2(13) . . ? C45 C46 C64 106.8(13) . . ? C46 C47 C48 116.9(14) . . ? C46 C47 C67 119.2(15) . . ? C48 C47 C67 110.0(13) . . ? C33 C48 C49 118.8(13) . . ? C33 C48 C47 123.0(13) . . ? C49 C48 C47 107.9(12) . . ? C50 C49 C48 119.1(13) . . ? C50 C49 C68 121.7(13) . . ? C48 C49 C68 107.9(13) . . ? C49 C50 C35 121.1(13) . . ? C49 C50 C51 120.6(13) . . ? C35 C50 C51 106.5(13) . . ? C52 C51 C70 119.2(14) . . ? C52 C51 C50 111.5(13) . . ? C70 C51 C50 117.4(14) . . ? C53 C52 C51 122.3(14) . . ? C53 C52 C36 120.1(14) . . ? C51 C52 C36 106.1(13) . . ? C52 C53 C54 122.2(15) . . ? C52 C53 C72 117.8(15) . . ? C54 C53 C72 108.1(14) . . ? C53 C54 C38 119.5(15) . . ? C53 C54 C55 111.0(14) . . ? C38 C54 C55 116.1(15) . . ? C56 C55 C73 121.9(17) . . ? C56 C55 C54 121.3(16) . . ? C73 C55 C54 104.3(15) . . ? C55 C56 C76 119.5(16) . . ? C55 C56 C57 121.6(16) . . ? C76 C56 C57 105.6(14) . . ? C58 C57 C39 123.6(15) . . ? C58 C57 C56 110.5(15) . . ? C39 C57 C56 115.6(14) . . ? C57 C58 C59 122.5(15) . . ? C57 C58 C77 110.2(14) . . ? C59 C58 C77 116.5(14) . . ? C60 C59 C58 119.6(14) . . ? C60 C59 C41 109.5(13) . . ? C58 C59 C41 117.3(14) . . ? C59 C60 C61 126.0(14) . . ? C59 C60 C43 110.2(13) . . ? C61 C60 C43 113.9(14) . . ? C62 C61 C60 124.3(15) . . ? C62 C61 C78 107.8(14) . . ? C60 C61 C78 115.8(14) . . ? C61 C62 C63 122.7(15) . . ? C61 C62 C88 110.9(15) . . ? C63 C62 C88 115.0(15) . . ? C62 C63 C64 124.4(15) . . ? C62 C63 C44 116.1(15) . . ? C64 C63 C44 107.2(13) . . ? C65 C64 C63 118.9(15) . . ? C65 C64 C46 119.2(14) . . ? C63 C64 C46 109.7(13) . . ? C66 C65 C64 121.6(15) . . ? C66 C65 C87 110.3(14) . . ? C64 C65 C87 116.6(15) . . ? C67 C66 C65 121.0(15) . . ? C67 C66 C85 117.1(15) . . ? C65 C66 C85 109.0(14) . . ? C66 C67 C68 121.6(15) . . ? C66 C67 C47 120.7(15) . . ? C68 C67 C47 106.4(14) . . ? C69 C68 C67 120.7(15) . . ? C69 C68 C49 115.6(15) . . ? C67 C68 C49 107.5(13) . . ? C68 C69 C70 124.5(15) . . ? C68 C69 C84 121.2(15) . . ? C70 C69 C84 103.6(13) . . ? C69 C70 C51 120.2(14) . . ? C69 C70 C71 109.2(14) . . ? C51 C70 C71 120.1(14) . . ? C72 C71 C83 121.9(16) . . ? C72 C71 C70 119.1(15) . . ? C83 C71 C70 108.6(15) . . ? C71 C72 C73 122.6(16) . . ? C71 C72 C53 121.5(15) . . ? C73 C72 C53 105.7(14) . . ? C74 C73 C55 119.0(16) . . ? C74 C73 C72 115.4(16) . . ? C55 C73 C72 110.7(15) . . ? C82 C74 C73 119.0(16) . . ? C82 C74 C75 110.3(15) . . ? C73 C74 C75 118.9(15) . . ? C80 C75 C74 106.8(15) . . ? C80 C75 C76 122.2(15) . . ? C74 C75 C76 119.4(15) . . ? C56 C76 C75 121.2(15) . . ? C56 C76 C77 111.6(14) . . ? C75 C76 C77 113.5(15) . . ? C78 C77 C58 121.6(15) . . ? C78 C77 C76 124.1(15) . . ? C58 C77 C76 102.0(14) . . ? C77 C78 C79 121.5(16) . . ? C77 C78 C61 120.2(15) . . ? C79 C78 C61 107.1(15) . . ? C78 C79 C88 109.3(14) . . ? C78 C79 C80 117.5(15) . . ? C88 C79 C80 121.8(14) . . ? C75 C80 C79 121.2(15) . . ? C75 C80 C81 108.5(14) . . ? C79 C80 C81 117.5(14) . . ? C86 C81 C82 127.5(15) . . ? C86 C81 C80 116.7(14) . . ? C82 C81 C80 104.6(13) . . ? C74 C82 C83 125.2(15) . . ? C74 C82 C81 109.7(14) . . ? C83 C82 C81 113.1(14) . . ? C84 C83 C82 122.8(16) . . ? C84 C83 C71 108.2(15) . . ? C82 C83 C71 115.8(15) . . ? C83 C84 C85 124.1(16) . . ? C83 C84 C69 110.4(15) . . ? C85 C84 C69 114.1(14) . . ? C84 C85 C66 125.2(14) . . ? C84 C85 C86 116.7(14) . . ? C66 C85 C86 107.6(13) . . ? C81 C86 C85 115.7(15) . . ? C81 C86 C87 125.3(15) . . ? C85 C86 C87 105.5(13) . . ? C88 C87 C65 125.5(15) . . ? C88 C87 C86 117.5(15) . . ? C65 C87 C86 107.5(14) . . ? C87 C88 C79 120.8(15) . . ? C87 C88 C62 119.4(15) . . ? C79 C88 C62 104.9(15) . . ? C28 N1 C27 104.8(11) . . ? C28 N1 C26 103.9(10) . . ? C27 N1 C26 113.5(11) . . ? C28 N1 Re1 108.8(8) . . ? C27 N1 Re1 110.9(8) . . ? C26 N1 Re1 114.1(8) . . ? C14 P1 C20 104.4(6) . . ? C14 P1 C13 105.1(6) . . ? C20 P1 C13 104.9(6) . . ? C14 P1 Re1 117.0(5) . . ? C20 P1 Re1 106.1(5) . . ? C13 P1 Re1 117.9(5) . . ? C2 Re1 C3 87.4(7) . . ? C2 Re1 C1 92.2(9) . . ? C3 Re1 C1 88.8(6) . . ? C2 Re1 N1 89.1(6) . . ? C3 Re1 N1 176.5(6) . . ? C1 Re1 N1 91.8(5) . . ? C2 Re1 P1 96.1(7) . . ? C3 Re1 P1 93.3(5) . . ? C1 Re1 P1 171.5(6) . . ? N1 Re1 P1 86.6(3) . . ? C5 Re2 C4 97.0(8) . . ? C5 Re2 C6 95.6(9) . . ? C4 Re2 C6 85.5(7) . . ? C5 Re2 C7 94.2(7) . . ? C4 Re2 C7 166.4(8) . . ? C6 Re2 C7 85.8(7) . . ? C5 Re2 C8 172.4(7) . . ? C4 Re2 C8 83.7(7) . . ? C6 Re2 C8 92.0(8) . . ? C7 Re2 C8 86.1(6) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.206 _refine_diff_density_min -1.049 _refine_diff_density_rms 0.175 data_a13832 _database_code_depnum_ccdc_archive 'CCDC 903347' #TrackingRef '4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C173 H42 N2 O12 P2 Re4 S6' _chemical_formula_sum 'C173 H42 N2 O12 P2 Re4 S6' _chemical_formula_weight 3339.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 10.0769(2) _cell_length_b 22.5349(7) _cell_length_c 24.5205(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.086(2) _cell_angle_gamma 90.00 _cell_volume 5512.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.012 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3232 _exptl_absorpt_coefficient_mu 4.602 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4751 _exptl_absorpt_correction_T_max 0.8373 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36284 _diffrn_reflns_av_R_equivalents 0.0829 _diffrn_reflns_av_sigmaI/netI 0.0975 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.04 _reflns_number_total 9680 _reflns_number_gt 6362 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0794P)^2^+2.2425P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9680 _refine_ls_number_parameters 891 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1084 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1637 _refine_ls_wR_factor_gt 0.1378 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4453(14) 0.0213(6) 0.1549(5) 0.049(4) Uani 1 1 d . . . C2 C 0.3608(12) 0.1352(6) 0.1609(5) 0.037(3) Uani 1 1 d . . . C3 C 0.4377(13) -0.0796(6) 0.2476(6) 0.042(3) Uani 1 1 d . . . C4 C 0.3114(12) -0.0542(6) 0.3409(5) 0.033(3) Uani 1 1 d . . . C5 C 0.5913(13) -0.0501(6) 0.3415(5) 0.036(3) Uani 1 1 d . . . C6 C 0.6735(18) 0.0801(7) 0.1122(6) 0.064(5) Uani 1 1 d . . . C7 C 0.5910(17) 0.1176(10) 0.0782(6) 0.092(7) Uani 1 1 d . . . H7 H 0.5477 0.1504 0.0924 0.110 Uiso 1 1 calc R . . C8 C 0.574(3) 0.1047(16) 0.0217(8) 0.153(16) Uani 1 1 d . . . H8 H 0.5171 0.1288 -0.0034 0.184 Uiso 1 1 calc R . . C9 C 0.638(5) 0.059(2) 0.0033(12) 0.23(3) Uani 1 1 d . . . H9 H 0.6259 0.0517 -0.0353 0.278 Uiso 1 1 calc R . . C10 C 0.716(5) 0.0226(13) 0.0345(11) 0.21(3) Uani 1 1 d . . . H10 H 0.7565 -0.0103 0.0191 0.253 Uiso 1 1 calc R . . C11 C 0.739(3) 0.0335(8) 0.0924(8) 0.121(9) Uani 1 1 d . . . H11 H 0.7978 0.0091 0.1164 0.145 Uiso 1 1 calc R . . C12 C 0.7872(13) 0.0391(6) 0.2246(5) 0.041(3) Uani 1 1 d . . . C13 C 0.7658(15) -0.0220(6) 0.2167(7) 0.056(4) Uani 1 1 d . . . H13 H 0.6992 -0.0343 0.1875 0.067 Uiso 1 1 calc R . . C14 C 0.8331(17) -0.0640(7) 0.2475(8) 0.062(5) Uani 1 1 d . . . H14 H 0.8132 -0.1047 0.2400 0.075 Uiso 1 1 calc R . . C15 C 0.9272(18) -0.0494(8) 0.2884(9) 0.075(6) Uani 1 1 d . . . H15 H 0.9773 -0.0794 0.3094 0.090 Uiso 1 1 calc R . . C16 C 0.9517(16) 0.0081(9) 0.3001(7) 0.079(6) Uani 1 1 d . . . H16 H 1.0177 0.0177 0.3304 0.095 Uiso 1 1 calc R . . C17 C 0.8835(13) 0.0557(6) 0.2694(6) 0.044(3) Uani 1 1 d . . . H17 H 0.9020 0.0961 0.2786 0.053 Uiso 1 1 calc R . . C18 C 0.7803(12) 0.1637(5) 0.1946(5) 0.033(3) Uani 1 1 d . . . C19 C 0.9144(13) 0.1563(6) 0.1870(5) 0.043(3) Uani 1 1 d . . . H19 H 0.9456 0.1179 0.1791 0.051 Uiso 1 1 calc R . . C20 C 1.0020(12) 0.2036(6) 0.1906(5) 0.038(3) Uani 1 1 d . . . H20 H 1.0930 0.1976 0.1858 0.045 Uiso 1 1 calc R . . C21 C 0.9566(12) 0.2599(6) 0.2012(5) 0.040(3) Uani 1 1 d . . . H21 H 1.0162 0.2927 0.2042 0.048 Uiso 1 1 calc R . . C22 C 0.8236(13) 0.2677(5) 0.2073(5) 0.039(3) Uani 1 1 d . . . H22 H 0.7919 0.3062 0.2145 0.047 Uiso 1 1 calc R . . C23 C 0.7344(12) 0.2194(5) 0.2031(4) 0.033(3) Uani 1 1 d . . . C24 C 0.5888(12) 0.2296(5) 0.2091(5) 0.034(3) Uani 1 1 d . . . H24 H 0.5342 0.2012 0.1839 0.041 Uiso 1 1 calc R . . C25 C 0.5327(14) 0.3038(5) 0.1364(5) 0.042(3) Uani 1 1 d . . . H25A H 0.6242 0.3051 0.1272 0.063 Uiso 1 1 calc R . . H25B H 0.4898 0.3425 0.1289 0.063 Uiso 1 1 calc R . . H25C H 0.4812 0.2734 0.1141 0.063 Uiso 1 1 calc R . . C26 C 0.4034(12) 0.2870(5) 0.2110(4) 0.032(3) Uani 1 1 d . . . H26A H 0.3439 0.2611 0.1857 0.039 Uiso 1 1 calc R . . H26B H 0.3635 0.3271 0.2109 0.039 Uiso 1 1 calc R . . C27 C 0.4264(11) 0.2606(5) 0.2704(4) 0.030(3) Uani 1 1 d . . . C28 C 0.5547(10) 0.2183(5) 0.2688(4) 0.022(3) Uani 1 1 d . . . C29 C 0.5352(10) 0.1509(5) 0.2812(4) 0.021(2) Uani 1 1 d . . . C30 C 0.4074(10) 0.1277(5) 0.2900(4) 0.022(3) Uani 1 1 d . . . C31 C 0.3967(10) 0.0821(5) 0.3342(4) 0.023(3) Uani 1 1 d . . . C32 C 0.5137(11) 0.0590(5) 0.3662(4) 0.023(3) Uani 1 1 d . . . C33 C 0.6450(11) 0.0878(5) 0.3615(5) 0.028(3) Uani 1 1 d . . . C34 C 0.6480(10) 0.1328(5) 0.3230(4) 0.022(3) Uani 1 1 d . . . C35 C 0.7343(10) 0.1835(5) 0.3374(4) 0.021(2) Uani 1 1 d . . . C36 C 0.6713(11) 0.2353(5) 0.3131(4) 0.027(3) Uani 1 1 d . . . C37 C 0.6841(11) 0.2882(5) 0.3406(4) 0.030(3) Uani 1 1 d . . . C38 C 0.5694(12) 0.3280(5) 0.3407(5) 0.034(3) Uani 1 1 d . . . C39 C 0.4475(12) 0.3107(5) 0.3124(4) 0.031(3) Uani 1 1 d . . . C40 C 0.3267(12) 0.3185(5) 0.3368(5) 0.036(3) Uani 1 1 d . . . C41 C 0.2370(11) 0.2687(5) 0.3232(5) 0.031(3) Uani 1 1 d . . . C42 C 0.3047(10) 0.2299(5) 0.2881(4) 0.030(3) Uani 1 1 d . . . C43 C 0.2951(10) 0.1686(5) 0.2944(4) 0.028(3) Uani 1 1 d . . . C44 C 0.2146(10) 0.1469(5) 0.3353(4) 0.028(3) Uani 1 1 d . . . C45 C 0.2815(10) 0.0935(5) 0.3599(5) 0.025(3) Uani 1 1 d . . . C46 C 0.2752(11) 0.0804(5) 0.4147(5) 0.028(3) Uani 1 1 d . . . C47 C 0.3960(12) 0.0585(5) 0.4472(5) 0.032(3) Uani 1 1 d . . . C48 C 0.5109(11) 0.0504(5) 0.4251(4) 0.026(3) Uani 1 1 d . . . C49 C 0.6399(11) 0.0676(5) 0.4538(4) 0.026(3) Uani 1 1 d . . . C50 C 0.7183(11) 0.0920(5) 0.4151(4) 0.026(3) Uani 1 1 d . . . C51 C 0.8054(9) 0.1393(5) 0.4298(4) 0.023(3) Uani 1 1 d . . . C52 C 0.8126(9) 0.1865(5) 0.3901(4) 0.024(3) Uani 1 1 d . . . C53 C 0.8264(10) 0.2421(5) 0.4185(5) 0.028(3) Uani 1 1 d . . . C54 C 0.7611(11) 0.2921(5) 0.3950(5) 0.032(3) Uani 1 1 d . . . C55 C 0.6951(11) 0.3317(5) 0.4277(5) 0.029(3) Uani 1 1 d . . . C56 C 0.5766(13) 0.3540(5) 0.3949(5) 0.036(3) Uani 1 1 d . . . C57 C 0.4584(13) 0.3632(6) 0.4182(5) 0.043(3) Uani 1 1 d . . . C58 C 0.3347(13) 0.3463(5) 0.3889(5) 0.039(3) Uani 1 1 d . . . C59 C 0.2524(13) 0.3228(6) 0.4274(6) 0.046(4) Uani 1 1 d . . . C60 C 0.1654(11) 0.2746(6) 0.4144(5) 0.038(3) Uani 1 1 d . . . C61 C 0.1588(11) 0.2477(6) 0.3599(5) 0.037(3) Uani 1 1 d . . . C62 C 0.1471(11) 0.1852(6) 0.3664(5) 0.036(3) Uani 1 1 d . . . C63 C 0.1449(11) 0.1713(6) 0.4245(5) 0.038(3) Uani 1 1 d . . . C64 C 0.2096(10) 0.1211(6) 0.4475(5) 0.031(3) Uani 1 1 d . . . C65 C 0.2881(11) 0.1248(6) 0.5016(5) 0.034(3) Uani 1 1 d . . . C66 C 0.4018(11) 0.0858(5) 0.5016(5) 0.029(3) Uani 1 1 d . . . C67 C 0.5252(11) 0.1034(5) 0.5308(4) 0.030(3) Uani 1 1 d . . . C68 C 0.6474(11) 0.0939(5) 0.5071(4) 0.027(3) Uani 1 1 d . . . C69 C 0.7358(10) 0.1441(5) 0.5201(4) 0.030(3) Uani 1 1 d . . . C70 C 0.8140(10) 0.1668(5) 0.4835(4) 0.027(3) Uani 1 1 d . . . C71 C 0.8252(11) 0.2301(6) 0.4772(5) 0.032(3) Uani 1 1 d . . . C72 C 0.7613(11) 0.2686(5) 0.5080(5) 0.031(3) Uani 1 1 d . . . C73 C 0.6966(12) 0.3208(5) 0.4833(5) 0.035(3) Uani 1 1 d . . . C74 C 0.5722(14) 0.3293(6) 0.5078(5) 0.046(4) Uani 1 1 d . . . C75 C 0.4560(13) 0.3509(5) 0.4761(5) 0.039(3) Uani 1 1 d . . . C76 C 0.3296(12) 0.3261(6) 0.4828(5) 0.040(3) Uani 1 1 d . . . C77 C 0.3189(13) 0.2799(7) 0.5202(5) 0.046(4) Uani 1 1 d . . . C78 C 0.4420(13) 0.2578(6) 0.5532(4) 0.039(3) Uani 1 1 d . . . C79 C 0.5641(13) 0.2833(6) 0.5475(5) 0.037(3) Uani 1 1 d . . . C80 C 0.6816(13) 0.2450(6) 0.5474(5) 0.041(3) Uani 1 1 d . . . C81 C 0.6660(11) 0.1839(6) 0.5539(4) 0.033(3) Uani 1 1 d . . . C82 C 0.5379(11) 0.1589(6) 0.5604(4) 0.033(3) Uani 1 1 d . . . C83 C 0.4268(12) 0.1956(6) 0.5601(4) 0.035(3) Uani 1 1 d . . . C84 C 0.2972(11) 0.1775(6) 0.5298(5) 0.036(3) Uani 1 1 d . . . C85 C 0.2334(12) 0.2296(6) 0.5056(5) 0.039(3) Uani 1 1 d . . . C86 C 0.1578(11) 0.2266(6) 0.4537(5) 0.037(3) Uani 1 1 d . . . C87 C 0.0000 0.0000 0.5000 0.055(6) Uani 1 2 d S . . N1 N 0.5369(10) 0.2893(4) 0.1954(4) 0.033(3) Uani 1 1 d . . . O1 O 0.4378(13) -0.0138(5) 0.1214(4) 0.086(4) Uani 1 1 d . . . O2 O 0.2971(10) 0.1625(5) 0.1283(4) 0.066(3) Uani 1 1 d . . . O3 O 0.4498(10) -0.1178(5) 0.2189(4) 0.062(3) Uani 1 1 d . . . O4 O 0.2343(10) -0.0762(4) 0.3644(4) 0.055(3) Uani 1 1 d . . . O5 O 0.6797(9) -0.0728(4) 0.3653(4) 0.050(3) Uani 1 1 d . . . O6 O 0.0276(11) 0.0082(5) 0.1371(5) 0.083 Uiso 1 1 d . . . H6' H -0.0147 -0.0170 0.1162 0.125 Uiso 1 1 calc R . . P1 P 0.6786(4) 0.09467(15) 0.18744(13) 0.0372(8) Uani 1 1 d . . . Re1 Re 0.45561(5) 0.08173(2) 0.213086(19) 0.03066(16) Uani 1 1 d . . . Re2 Re 0.43303(5) -0.01361(2) 0.298899(19) 0.03043(16) Uani 1 1 d . . . S1 S 0.2499(3) 0.03529(15) 0.23674(13) 0.0381(8) Uani 1 1 d . . . S2 S 0.1662(4) -0.02838(19) 0.18109(17) 0.0661(12) Uani 1 1 d . . . S3 S -0.0220(6) -0.0353(3) 0.4475(2) 0.0998(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.077(10) 0.037(9) 0.033(8) 0.005(7) 0.010(7) -0.027(7) C2 0.035(7) 0.038(9) 0.039(8) -0.001(7) 0.005(6) -0.014(6) C3 0.045(8) 0.034(9) 0.042(8) 0.008(7) -0.007(7) -0.009(6) C4 0.040(8) 0.032(8) 0.024(6) 0.011(6) -0.007(6) -0.006(6) C5 0.051(8) 0.025(8) 0.032(7) 0.001(6) 0.007(6) -0.012(6) C6 0.102(13) 0.062(11) 0.036(8) -0.023(8) 0.038(9) -0.061(10) C7 0.075(12) 0.17(2) 0.031(9) 0.022(11) -0.004(8) -0.058(13) C8 0.15(2) 0.28(5) 0.028(13) 0.027(17) 0.005(14) -0.14(3) C9 0.32(6) 0.34(7) 0.050(18) -0.07(2) 0.08(2) -0.29(6) C10 0.44(7) 0.12(3) 0.11(2) -0.09(2) 0.16(3) -0.17(3) C11 0.24(3) 0.061(13) 0.082(13) -0.050(11) 0.109(16) -0.050(15) C12 0.053(8) 0.035(8) 0.040(8) -0.009(7) 0.026(7) -0.012(6) C13 0.070(10) 0.030(9) 0.078(11) -0.011(8) 0.044(9) -0.015(8) C14 0.070(12) 0.026(9) 0.104(14) 0.005(10) 0.061(11) 0.016(8) C15 0.076(13) 0.030(11) 0.125(17) 0.024(11) 0.035(12) 0.031(9) C16 0.061(11) 0.123(18) 0.060(11) 0.039(12) 0.032(9) 0.034(11) C17 0.051(8) 0.029(8) 0.059(9) 0.017(7) 0.032(7) 0.014(6) C18 0.045(8) 0.024(8) 0.028(7) -0.004(6) -0.001(6) -0.003(6) C19 0.056(9) 0.042(9) 0.030(7) 0.000(6) 0.007(6) 0.007(7) C20 0.030(7) 0.054(10) 0.028(7) 0.000(7) 0.001(6) -0.005(7) C21 0.035(8) 0.045(9) 0.038(8) -0.004(7) 0.001(6) -0.015(6) C22 0.066(10) 0.022(7) 0.031(7) 0.002(6) 0.009(6) -0.013(6) C23 0.059(9) 0.026(8) 0.013(6) 0.004(5) 0.000(6) -0.006(6) C24 0.048(8) 0.031(8) 0.025(6) 0.005(6) 0.006(6) -0.005(6) C25 0.072(9) 0.028(8) 0.026(7) 0.013(6) 0.009(6) -0.004(7) C26 0.042(7) 0.023(7) 0.029(7) 0.003(5) -0.003(6) 0.005(5) C27 0.037(7) 0.026(7) 0.024(6) 0.004(5) -0.004(5) 0.002(5) C28 0.034(6) 0.022(7) 0.011(5) 0.003(5) 0.001(5) -0.006(5) C29 0.038(7) 0.009(6) 0.015(5) 0.003(5) -0.001(5) 0.002(5) C30 0.032(7) 0.014(6) 0.019(6) 0.002(5) -0.002(5) -0.002(5) C31 0.018(6) 0.034(7) 0.018(6) -0.003(5) 0.005(5) -0.009(5) C32 0.040(7) 0.008(6) 0.018(6) -0.002(5) -0.001(5) 0.003(5) C33 0.039(7) 0.020(7) 0.028(6) 0.001(5) 0.014(5) -0.003(5) C34 0.026(6) 0.028(7) 0.014(5) -0.003(5) 0.007(5) 0.000(5) C35 0.024(6) 0.022(7) 0.016(5) -0.001(5) 0.005(5) 0.002(5) C36 0.038(7) 0.021(7) 0.021(6) 0.007(5) 0.005(5) -0.008(5) C37 0.040(7) 0.027(7) 0.024(6) -0.001(6) 0.010(5) -0.011(6) C38 0.050(8) 0.008(6) 0.042(7) 0.004(6) 0.001(6) 0.003(5) C39 0.045(8) 0.023(7) 0.022(6) 0.011(5) -0.003(6) 0.009(5) C40 0.047(8) 0.020(7) 0.039(7) 0.012(6) -0.004(6) 0.019(6) C41 0.028(7) 0.028(8) 0.033(7) 0.008(6) -0.006(6) 0.009(5) C42 0.023(6) 0.036(8) 0.026(6) 0.008(6) -0.010(5) 0.003(5) C43 0.011(6) 0.038(8) 0.029(6) 0.003(6) -0.013(5) 0.002(5) C44 0.014(6) 0.043(8) 0.026(6) 0.002(6) -0.006(5) -0.004(5) C45 0.014(6) 0.030(7) 0.031(7) -0.003(5) -0.003(5) -0.012(5) C46 0.024(6) 0.029(7) 0.031(7) 0.008(6) 0.001(5) -0.004(5) C47 0.041(8) 0.020(7) 0.034(7) 0.007(6) 0.008(6) -0.007(5) C48 0.044(7) 0.006(6) 0.027(6) 0.006(5) 0.003(6) 0.001(5) C49 0.036(7) 0.017(7) 0.023(6) 0.012(5) -0.006(5) 0.014(5) C50 0.032(6) 0.021(7) 0.025(6) 0.002(5) 0.006(5) 0.013(5) C51 0.011(5) 0.030(7) 0.028(6) -0.002(5) 0.003(5) 0.004(5) C52 0.012(5) 0.024(7) 0.034(7) 0.003(5) 0.002(5) 0.002(5) C53 0.020(6) 0.033(8) 0.029(7) -0.005(6) 0.001(5) -0.009(5) C54 0.035(7) 0.021(7) 0.040(7) 0.001(6) 0.004(6) -0.007(5) C55 0.037(7) 0.015(7) 0.035(7) -0.006(5) 0.004(6) -0.009(5) C56 0.057(9) 0.015(7) 0.032(7) -0.003(6) -0.004(6) -0.009(6) C57 0.046(8) 0.033 0.050(8) -0.010(7) 0.006(7) 0.009(6) C58 0.049(8) 0.020(7) 0.049(8) -0.005(6) 0.009(7) 0.020(6) C59 0.040(8) 0.041(9) 0.056(9) 0.005(7) 0.005(7) 0.026(7) C60 0.028(7) 0.037(9) 0.050(8) -0.005(7) 0.005(6) 0.019(6) C61 0.024(7) 0.040(9) 0.045(8) 0.006(7) -0.001(6) 0.018(6) C62 0.019(6) 0.055(10) 0.032(7) 0.004(7) 0.001(5) 0.004(6) C63 0.018(6) 0.056(10) 0.041(8) -0.001(7) 0.005(6) 0.005(6) C64 0.010(6) 0.046(8) 0.035(7) 0.008(6) 0.000(5) -0.002(5) C65 0.033(7) 0.042(9) 0.031(7) 0.004(6) 0.015(6) -0.001(6) C66 0.036(7) 0.026(7) 0.028(6) 0.007(5) 0.010(5) -0.003(5) C67 0.037(7) 0.040(8) 0.011(6) 0.008(5) -0.004(5) 0.002(6) C68 0.032(7) 0.023(7) 0.025(6) 0.016(5) 0.004(5) 0.005(5) C69 0.019(6) 0.040(8) 0.025(6) 0.000(6) -0.017(5) 0.014(5) C70 0.016(6) 0.041(8) 0.024(6) -0.007(6) -0.001(5) 0.003(5) C71 0.024(6) 0.044(9) 0.027(7) 0.000(6) -0.004(5) -0.002(6) C72 0.032(7) 0.035(8) 0.023(6) -0.006(6) -0.008(6) -0.006(6) C73 0.048(8) 0.017(7) 0.037(7) -0.010(6) -0.003(6) -0.001(6) C74 0.062(10) 0.034(9) 0.041(8) -0.025(7) 0.006(7) -0.001(7) C75 0.059(9) 0.023(7) 0.034(7) -0.015(6) 0.007(7) 0.022(6) C76 0.034(8) 0.043(9) 0.044(8) -0.015(7) 0.009(6) 0.018(6) C77 0.052(9) 0.060(10) 0.027(7) -0.014(7) 0.008(6) 0.015(7) C78 0.045(8) 0.059(10) 0.015(6) -0.002(6) 0.009(6) 0.009(7) C79 0.052(8) 0.039(8) 0.019(6) -0.005(6) 0.000(6) 0.005(7) C80 0.049(8) 0.051(10) 0.018(6) -0.012(6) -0.016(6) 0.007(7) C81 0.037(7) 0.048(9) 0.010(6) 0.001(6) -0.006(5) 0.009(6) C82 0.033(7) 0.052(9) 0.016(6) 0.004(6) 0.016(5) 0.009(6) C83 0.049(8) 0.040(9) 0.017(6) -0.001(6) 0.015(6) 0.003(6) C84 0.028(7) 0.052(9) 0.031(7) 0.009(7) 0.011(6) 0.010(6) C85 0.037(7) 0.049(9) 0.034(7) -0.011(7) 0.017(6) 0.007(6) C86 0.022(6) 0.048(9) 0.041(8) 0.000(7) 0.005(6) 0.005(6) C87 0.071(14) 0.041(14) 0.055(13) 0.023(11) 0.018(11) 0.023(10) N1 0.053(7) 0.019(6) 0.026(5) 0.009(4) 0.000(5) -0.009(5) O1 0.139(11) 0.080(9) 0.050(7) -0.048(7) 0.048(7) -0.061(8) O2 0.078(7) 0.062(7) 0.046(6) 0.024(5) -0.031(5) -0.012(6) O3 0.071(7) 0.050(7) 0.063(7) -0.022(6) 0.001(6) -0.002(5) O4 0.059(6) 0.056(7) 0.047(6) 0.028(5) 0.001(5) -0.014(5) O5 0.054(6) 0.044(6) 0.048(6) 0.011(5) -0.003(5) 0.007(5) P1 0.057(2) 0.033(2) 0.0225(16) -0.0057(15) 0.0084(16) -0.0108(16) Re1 0.0437(3) 0.0256(3) 0.0212(3) 0.0004(2) -0.0004(2) -0.0090(2) Re2 0.0399(3) 0.0223(3) 0.0286(3) 0.0018(2) 0.0028(2) -0.0067(2) S1 0.0418(19) 0.036(2) 0.0350(18) -0.0010(15) -0.0014(15) -0.0103(15) S2 0.062(3) 0.066(3) 0.069(3) -0.025(2) 0.003(2) -0.027(2) S3 0.130(5) 0.092(4) 0.078(3) -0.007(3) 0.018(3) 0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.133(15) . ? C1 Re1 1.965(15) . ? C2 O2 1.132(14) . ? C2 Re1 1.914(13) . ? C3 O3 1.129(15) . ? C3 Re2 1.952(15) . ? C4 O4 1.144(13) . ? C4 Re2 1.937(13) . ? C5 O5 1.119(13) . ? C5 Re2 1.959(14) . ? C6 C11 1.36(2) . ? C6 C7 1.38(2) . ? C6 P1 1.868(14) . ? C7 C8 1.40(2) . ? C7 H7 0.9500 . ? C8 C9 1.33(6) . ? C8 H8 0.9500 . ? C9 C10 1.30(7) . ? C9 H9 0.9500 . ? C10 C11 1.43(3) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.404(17) . ? C12 C17 1.409(17) . ? C12 P1 1.821(14) . ? C13 C14 1.34(2) . ? C13 H13 0.9500 . ? C14 C15 1.32(2) . ? C14 H14 0.9500 . ? C15 C16 1.34(2) . ? C15 H15 0.9500 . ? C16 C17 1.430(19) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C23 1.364(16) . ? C18 C19 1.400(17) . ? C18 P1 1.858(12) . ? C19 C20 1.378(17) . ? C19 H19 0.9500 . ? C20 C21 1.386(17) . ? C20 H20 0.9500 . ? C21 C22 1.380(17) . ? C21 H21 0.9500 . ? C22 C23 1.405(15) . ? C22 H22 0.9500 . ? C23 C24 1.513(17) . ? C24 N1 1.465(15) . ? C24 C28 1.571(14) . ? C24 H24 1.0000 . ? C25 N1 1.477(13) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 N1 1.450(15) . ? C26 C27 1.559(14) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C42 1.523(16) . ? C27 C39 1.524(16) . ? C27 C28 1.611(15) . ? C28 C36 1.531(14) . ? C28 C29 1.567(14) . ? C29 C30 1.434(14) . ? C29 C34 1.476(13) . ? C29 Re1 2.343(10) . ? C30 C43 1.476(15) . ? C30 C31 1.509(14) . ? C30 Re1 2.264(11) . ? C31 C32 1.421(14) . ? C31 C45 1.419(15) . ? C31 Re2 2.373(11) . ? C32 C48 1.461(14) . ? C32 C33 1.493(15) . ? C32 Re2 2.385(10) . ? C33 C34 1.389(14) . ? C33 C50 1.419(15) . ? C34 C35 1.448(14) . ? C35 C52 1.417(14) . ? C35 C36 1.418(14) . ? C36 C37 1.367(15) . ? C37 C54 1.448(15) . ? C37 C38 1.463(16) . ? C38 C39 1.379(15) . ? C38 C56 1.446(16) . ? C39 C40 1.440(17) . ? C40 C58 1.414(16) . ? C40 C41 1.452(16) . ? C41 C61 1.362(16) . ? C41 C42 1.461(16) . ? C42 C43 1.394(15) . ? C43 C44 1.461(16) . ? C44 C62 1.391(16) . ? C44 C45 1.467(15) . ? C45 C46 1.387(15) . ? C46 C64 1.440(16) . ? C46 C47 1.444(15) . ? C47 C48 1.359(15) . ? C47 C66 1.462(16) . ? C48 C49 1.441(15) . ? C49 C50 1.427(16) . ? C49 C68 1.429(15) . ? C50 C51 1.396(15) . ? C51 C70 1.448(14) . ? C51 C52 1.452(15) . ? C52 C53 1.430(15) . ? C53 C54 1.389(15) . ? C53 C71 1.467(15) . ? C54 C55 1.426(16) . ? C55 C73 1.383(15) . ? C55 C56 1.434(15) . ? C56 C57 1.407(17) . ? C57 C58 1.401(17) . ? C57 C75 1.452(17) . ? C58 C59 1.441(18) . ? C59 C60 1.403(18) . ? C59 C76 1.470(17) . ? C60 C61 1.460(17) . ? C60 C86 1.460(17) . ? C61 C62 1.423(17) . ? C62 C63 1.463(16) . ? C63 C64 1.386(16) . ? C63 C86 1.433(17) . ? C64 C65 1.450(15) . ? C65 C84 1.370(17) . ? C65 C66 1.444(16) . ? C66 C67 1.403(15) . ? C67 C82 1.442(16) . ? C67 C68 1.449(16) . ? C68 C69 1.446(15) . ? C69 C70 1.373(16) . ? C69 C81 1.468(16) . ? C70 C71 1.442(16) . ? C71 C72 1.369(16) . ? C72 C73 1.438(16) . ? C72 C80 1.441(17) . ? C73 C74 1.476(17) . ? C74 C75 1.397(17) . ? C74 C79 1.432(17) . ? C75 C76 1.422(18) . ? C76 C77 1.401(18) . ? C77 C85 1.438(18) . ? C77 C78 1.469(17) . ? C78 C79 1.383(17) . ? C78 C83 1.423(17) . ? C79 C80 1.467(17) . ? C80 C81 1.397(17) . ? C81 C82 1.438(16) . ? C82 C83 1.391(16) . ? C83 C84 1.467(16) . ? C84 C85 1.426(17) . ? C85 C86 1.390(16) . ? C87 S3 1.502(5) 3_556 ? C87 S3 1.502(5) . ? O6 S2 1.836(11) . ? O6 H6' 0.8400 . ? P1 Re1 2.435(4) . ? Re1 S1 2.464(3) . ? Re1 Re2 3.0381(7) . ? Re2 S1 2.481(3) . ? S1 S2 2.076(5) . ? 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 C1 Re1 179.1(13) . . ? O2 C2 Re1 173.5(11) . . ? O3 C3 Re2 175.2(12) . . ? O4 C4 Re2 176.3(11) . . ? O5 C5 Re2 177.5(11) . . ? C11 C6 C7 122.5(17) . . ? C11 C6 P1 122.6(16) . . ? C7 C6 P1 114.8(14) . . ? C6 C7 C8 117(2) . . ? C6 C7 H7 121.6 . . ? C8 C7 H7 121.6 . . ? C9 C8 C7 120(3) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C10 C9 C8 124(3) . . ? C10 C9 H9 117.8 . . ? C8 C9 H9 117.8 . . ? C9 C10 C11 119(4) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? C6 C11 C10 118(3) . . ? C6 C11 H11 121.1 . . ? C10 C11 H11 121.1 . . ? C13 C12 C17 116.3(13) . . ? C13 C12 P1 122.4(11) . . ? C17 C12 P1 120.5(10) . . ? C14 C13 C12 124.1(16) . . ? C14 C13 H13 117.9 . . ? C12 C13 H13 117.9 . . ? C15 C14 C13 120.4(16) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 119.5(17) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C15 C16 C17 123.5(18) . . ? C15 C16 H16 118.3 . . ? C17 C16 H16 118.3 . . ? C12 C17 C16 116.0(14) . . ? C12 C17 H17 122.0 . . ? C16 C17 H17 122.0 . . ? C23 C18 C19 118.9(12) . . ? C23 C18 P1 126.2(10) . . ? C19 C18 P1 114.7(10) . . ? C20 C19 C18 121.4(13) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C19 C20 C21 119.6(12) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C22 C21 C20 119.2(12) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C21 C22 C23 120.9(12) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C18 C23 C22 119.8(12) . . ? C18 C23 C24 120.6(11) . . ? C22 C23 C24 119.6(11) . . ? N1 C24 C23 115.9(10) . . ? N1 C24 C28 104.1(9) . . ? C23 C24 C28 114.1(9) . . ? N1 C24 H24 107.4 . . ? C23 C24 H24 107.4 . . ? C28 C24 H24 107.4 . . ? N1 C25 H25A 109.5 . . ? N1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N1 C26 C27 103.8(8) . . ? N1 C26 H26A 111.0 . . ? C27 C26 H26A 111.0 . . ? N1 C26 H26B 111.0 . . ? C27 C26 H26B 111.0 . . ? H26A C26 H26B 109.0 . . ? C42 C27 C39 100.6(9) . . ? C42 C27 C26 114.8(9) . . ? C39 C27 C26 109.8(9) . . ? C42 C27 C28 114.8(9) . . ? C39 C27 C28 114.7(8) . . ? C26 C27 C28 102.6(9) . . ? C36 C28 C29 102.0(8) . . ? C36 C28 C24 111.9(9) . . ? C29 C28 C24 112.8(9) . . ? C36 C28 C27 112.0(9) . . ? C29 C28 C27 116.5(9) . . ? C24 C28 C27 102.0(8) . . ? C30 C29 C34 114.6(9) . . ? C30 C29 C28 121.5(9) . . ? C34 C29 C28 107.3(8) . . ? C30 C29 Re1 68.9(6) . . ? C34 C29 Re1 117.6(7) . . ? C28 C29 Re1 123.1(6) . . ? C29 C30 C43 119.8(9) . . ? C29 C30 C31 120.8(9) . . ? C43 C30 C31 103.8(9) . . ? C29 C30 Re1 74.9(6) . . ? C43 C30 Re1 127.1(7) . . ? C31 C30 Re1 109.4(7) . . ? C32 C31 C45 119.3(9) . . ? C32 C31 C30 120.6(9) . . ? C45 C31 C30 110.0(9) . . ? C32 C31 Re2 73.1(6) . . ? C45 C31 Re2 120.2(7) . . ? C30 C31 Re2 109.0(7) . . ? C31 C32 C48 117.7(10) . . ? C31 C32 C33 118.3(9) . . ? C48 C32 C33 106.0(9) . . ? C31 C32 Re2 72.2(6) . . ? C48 C32 Re2 122.7(7) . . ? C33 C32 Re2 117.6(7) . . ? C34 C33 C50 121.6(10) . . ? C34 C33 C32 118.4(10) . . ? C50 C33 C32 107.9(10) . . ? C33 C34 C35 118.7(9) . . ? C33 C34 C29 125.8(10) . . ? C35 C34 C29 109.2(9) . . ? C52 C35 C36 120.1(10) . . ? C52 C35 C34 119.9(10) . . ? C36 C35 C34 109.2(9) . . ? C37 C36 C35 120.3(10) . . ? C37 C36 C28 125.2(10) . . ? C35 C36 C28 110.2(9) . . ? C36 C37 C54 120.6(11) . . ? C36 C37 C38 121.0(10) . . ? C54 C37 C38 106.4(10) . . ? C39 C38 C56 120.1(11) . . ? C39 C38 C37 118.3(10) . . ? C56 C38 C37 108.1(10) . . ? C38 C39 C40 120.1(11) . . ? C38 C39 C27 125.4(11) . . ? C40 C39 C27 109.1(10) . . ? C58 C40 C39 119.1(11) . . ? C58 C40 C41 120.3(12) . . ? C39 C40 C41 110.1(11) . . ? C61 C41 C40 121.1(12) . . ? C61 C41 C42 122.9(11) . . ? C40 C41 C42 105.7(11) . . ? C43 C42 C41 118.7(11) . . ? C43 C42 C27 123.6(10) . . ? C41 C42 C27 111.0(10) . . ? C42 C43 C44 117.6(11) . . ? C42 C43 C30 123.0(10) . . ? C44 C43 C30 110.3(10) . . ? C62 C44 C43 122.0(11) . . ? C62 C44 C45 121.1(10) . . ? C43 C44 C45 106.8(10) . . ? C46 C45 C31 122.9(9) . . ? C46 C45 C44 119.5(11) . . ? C31 C45 C44 108.9(10) . . ? C45 C46 C64 119.5(10) . . ? C45 C46 C47 117.3(10) . . ? C64 C46 C47 109.1(10) . . ? C48 C47 C46 121.7(10) . . ? C48 C47 C66 119.6(10) . . ? C46 C47 C66 106.4(10) . . ? C47 C48 C49 122.0(10) . . ? C47 C48 C32 120.8(10) . . ? C49 C48 C32 107.7(9) . . ? C50 C49 C68 119.0(10) . . ? C50 C49 C48 109.0(9) . . ? C68 C49 C48 119.1(10) . . ? C51 C50 C33 121.1(10) . . ? C51 C50 C49 120.7(10) . . ? C33 C50 C49 109.0(10) . . ? C50 C51 C70 121.1(10) . . ? C50 C51 C52 118.4(9) . . ? C70 C51 C52 107.1(10) . . ? C35 C52 C53 119.3(10) . . ? C35 C52 C51 120.2(10) . . ? C53 C52 C51 109.0(9) . . ? C54 C53 C52 120.0(10) . . ? C54 C53 C71 119.1(11) . . ? C52 C53 C71 107.7(10) . . ? C53 C54 C55 120.4(11) . . ? C53 C54 C37 119.6(11) . . ? C55 C54 C37 109.0(10) . . ? C73 C55 C54 120.2(11) . . ? C73 C55 C56 120.5(11) . . ? C54 C55 C56 108.7(10) . . ? C57 C56 C55 120.7(11) . . ? C57 C56 C38 119.8(11) . . ? C55 C56 C38 107.8(11) . . ? C58 C57 C56 119.7(11) . . ? C58 C57 C75 108.2(12) . . ? C56 C57 C75 120.0(11) . . ? C57 C58 C40 121.1(12) . . ? C57 C58 C59 108.5(12) . . ? C40 C58 C59 117.6(12) . . ? C60 C59 C58 122.2(13) . . ? C60 C59 C76 118.8(13) . . ? C58 C59 C76 107.9(12) . . ? C59 C60 C61 118.5(13) . . ? C59 C60 C86 120.8(12) . . ? C61 C60 C86 107.2(11) . . ? C41 C61 C62 118.8(12) . . ? C41 C61 C60 120.2(12) . . ? C62 C61 C60 107.7(11) . . ? C44 C62 C61 119.9(12) . . ? C44 C62 C63 118.5(11) . . ? C61 C62 C63 109.4(12) . . ? C64 C63 C86 120.2(11) . . ? C64 C63 C62 120.0(12) . . ? C86 C63 C62 106.8(12) . . ? C63 C64 C46 121.4(11) . . ? C63 C64 C65 119.3(12) . . ? C46 C64 C65 108.2(10) . . ? C84 C65 C66 122.1(11) . . ? C84 C65 C64 120.0(12) . . ? C66 C65 C64 107.2(11) . . ? C67 C66 C65 118.3(11) . . ? C67 C66 C47 120.2(10) . . ? C65 C66 C47 109.0(10) . . ? C66 C67 C82 120.7(11) . . ? C66 C67 C68 119.8(10) . . ? C82 C67 C68 108.0(10) . . ? C49 C68 C69 118.5(10) . . ? C49 C68 C67 119.3(10) . . ? C69 C68 C67 109.2(10) . . ? C70 C69 C68 122.7(10) . . ? C70 C69 C81 120.4(11) . . ? C68 C69 C81 105.8(10) . . ? C69 C70 C71 120.0(11) . . ? C69 C70 C51 117.9(10) . . ? C71 C70 C51 108.8(10) . . ? C72 C71 C70 121.1(11) . . ? C72 C71 C53 119.7(11) . . ? C70 C71 C53 107.4(10) . . ? C71 C72 C73 120.4(11) . . ? C71 C72 C80 119.1(12) . . ? C73 C72 C80 108.8(11) . . ? C55 C73 C72 120.1(11) . . ? C55 C73 C74 119.1(11) . . ? C72 C73 C74 107.2(11) . . ? C75 C74 C79 120.4(13) . . ? C75 C74 C73 120.8(12) . . ? C79 C74 C73 108.3(12) . . ? C74 C75 C76 119.5(12) . . ? C74 C75 C57 118.8(12) . . ? C76 C75 C57 109.0(11) . . ? C77 C76 C75 121.4(11) . . ? C77 C76 C59 119.2(13) . . ? C75 C76 C59 106.2(12) . . ? C76 C77 C85 121.5(12) . . ? C76 C77 C78 118.4(13) . . ? C85 C77 C78 107.4(13) . . ? C79 C78 C83 122.3(12) . . ? C79 C78 C77 119.8(12) . . ? C83 C78 C77 107.6(12) . . ? C78 C79 C74 120.4(11) . . ? C78 C79 C80 119.0(12) . . ? C74 C79 C80 107.6(12) . . ? C81 C80 C72 121.5(12) . . ? C81 C80 C79 118.5(12) . . ? C72 C80 C79 108.0(12) . . ? C80 C81 C82 121.0(11) . . ? C80 C81 C69 117.8(11) . . ? C82 C81 C69 109.4(11) . . ? C83 C82 C81 120.1(12) . . ? C83 C82 C67 120.0(11) . . ? C81 C82 C67 107.5(10) . . ? C82 C83 C78 119.0(12) . . ? C82 C83 C84 119.6(12) . . ? C78 C83 C84 108.5(11) . . ? C65 C84 C85 120.7(11) . . ? C65 C84 C83 119.2(11) . . ? C85 C84 C83 107.4(12) . . ? C86 C85 C84 119.8(12) . . ? C86 C85 C77 119.8(13) . . ? C84 C85 C77 109.0(11) . . ? C85 C86 C63 119.9(12) . . ? C85 C86 C60 119.8(12) . . ? C63 C86 C60 108.9(11) . . ? S3 C87 S3 180.000(1) 3_556 . ? C26 N1 C24 102.8(9) . . ? C26 N1 C25 111.5(9) . . ? C24 N1 C25 112.8(10) . . ? S2 O6 H6' 109.5 . . ? C12 P1 C18 104.1(6) . . ? C12 P1 C6 107.7(8) . . ? C18 P1 C6 100.3(6) . . ? C12 P1 Re1 107.5(4) . . ? C18 P1 Re1 126.4(4) . . ? C6 P1 Re1 109.6(5) . . ? C2 Re1 C1 88.9(5) . . ? C2 Re1 C30 97.1(4) . . ? C1 Re1 C30 158.0(5) . . ? C2 Re1 C29 98.4(4) . . ? C1 Re1 C29 163.1(5) . . ? C30 Re1 C29 36.2(4) . . ? C2 Re1 P1 98.3(4) . . ? C1 Re1 P1 81.5(4) . . ? C30 Re1 P1 118.3(3) . . ? C29 Re1 P1 82.4(3) . . ? C2 Re1 S1 93.9(3) . . ? C1 Re1 S1 85.2(4) . . ? C30 Re1 S1 73.3(3) . . ? C29 Re1 S1 109.3(3) . . ? P1 Re1 S1 161.74(11) . . ? C2 Re1 Re2 146.1(3) . . ? C1 Re1 Re2 90.7(4) . . ? C30 Re1 Re2 72.6(3) . . ? C29 Re1 Re2 91.6(2) . . ? P1 Re1 Re2 115.17(8) . . ? S1 Re1 Re2 52.34(7) . . ? C4 Re2 C3 93.3(5) . . ? C4 Re2 C5 92.7(5) . . ? C3 Re2 C5 86.1(5) . . ? C4 Re2 C31 95.4(5) . . ? C3 Re2 C31 161.2(4) . . ? C5 Re2 C31 110.0(4) . . ? C4 Re2 C32 97.8(4) . . ? C3 Re2 C32 158.7(5) . . ? C5 Re2 C32 75.3(4) . . ? C31 Re2 C32 34.7(3) . . ? C4 Re2 S1 93.7(3) . . ? C3 Re2 S1 91.5(4) . . ? C5 Re2 S1 173.3(4) . . ? C31 Re2 S1 71.4(2) . . ? C32 Re2 S1 105.8(3) . . ? C4 Re2 Re1 144.7(3) . . ? C3 Re2 Re1 94.7(4) . . ? C5 Re2 Re1 122.1(3) . . ? C31 Re2 Re1 68.9(3) . . ? C32 Re2 Re1 86.7(2) . . ? S1 Re2 Re1 51.83(8) . . ? S2 S1 Re1 114.61(19) . . ? S2 S1 Re2 107.18(19) . . ? Re1 S1 Re2 75.83(9) . . ? O6 S2 S1 106.3(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.501 _refine_diff_density_min -1.596 _refine_diff_density_rms 0.376