# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 data_added_by_encifer _publ_section_references ;CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET) Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. Flack. H. D. (1983). Acta Cryst. A39, 876--881. Sheldrick, G. M. (1990a). Acta Cryst. A46, 467--473. Sheldrick, G. M. (1990b). SHELXTL/PC Software. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany Spek, A. L. (1990). Acta Cryst. A46, C-34. UNIL IC & KUMA (2000). CrysAlis CCD. Version 1.163. Kuma Diffraction Instruments GmbH, Wroc\/law, Poland. UNIL IC & KUMA (2000). CrysAlis RED. Version 1.163. Kuma Diffraction Instruments GmbH, Wroc\/law, Poland. ; data_ren211 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H25 Cl2 N3 O2 P Re, C2 H3 N' _chemical_formula_sum 'C32 H28 Cl2 N4 O2 P Re' _chemical_formula_weight 788.65 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' Cl Cl 0.1484 0.1585 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4006(4) _cell_length_b 10.5121(4) _cell_length_c 16.4277(6) _cell_angle_alpha 86.211(3) _cell_angle_beta 81.558(3) _cell_angle_gamma 63.957(4) _cell_volume 1596.22(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8353 _cell_measurement_theta_min 3.5389 _cell_measurement_theta_max 29.3187 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.14089 _exptl_crystal_size_mid 0.07330 _exptl_crystal_size_min 0.04730 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776 _exptl_absorpt_coefficient_mu 4.059 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ;CrysAlis RED, (2005) ; _exptl_absorpt_correction_T_min 0.78560 _exptl_absorpt_correction_T_max 1.00000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _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 11251 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_unetI/netI 0.0356 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 25.05 _reflns_number_total 5657 _reflns_number_gt 4816 _reflns_threshold_expression >2sigma(I) #========================================================================== # # REFINEMENT DATA _computing_data_collection 'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)' _computing_cell_refinement 'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)' _computing_data_reduction 'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;XP in SHELXTL/PC (Sheldrick, 1990b) ORTEP-3 W v. 1.062 (Farrugia 1997) ; _computing_publication_material ;SHELXL-97 (Sheldrick, 1997) and PLATON (Spek, 1990) ; _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^)+(0.0241P)^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 5657 _refine_ls_number_parameters 381 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0306 _refine_ls_R_factor_gt 0.0222 _refine_ls_wR_factor_ref 0.0459 _refine_ls_wR_factor_gt 0.0449 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.954 _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 0.265100(13) 0.344356(14) -0.342553(8) 0.03760(5) Uani 1 1 d . . . Cl1 Cl 0.12479(9) 0.56357(10) -0.40456(6) 0.0582(2) Uani 1 1 d . . . Cl2 Cl 0.45508(9) 0.13886(9) -0.29106(6) 0.0564(2) Uani 1 1 d . . . P1 P 0.14623(8) 0.44168(8) -0.20704(5) 0.03523(18) Uani 1 1 d . . . O1 O 0.4137(2) 0.4232(2) -0.34715(14) 0.0456(5) Uani 1 1 d . . . O2 O 0.6153(3) 0.4279(3) -0.41299(17) 0.0673(7) Uani 1 1 d . . . N2 N 0.3937(3) 0.2769(3) -0.45883(16) 0.0460(7) Uani 1 1 d . . . N1 N 0.1566(3) 0.2623(3) -0.34576(16) 0.0416(6) Uani 1 1 d . . . N3 N 0.5843(4) 0.1924(4) -0.6034(2) 0.0777(10) Uani 1 1 d . . . C1 C 0.1399(3) 0.3064(3) -0.13437(19) 0.0400(7) Uani 1 1 d . . . C2 C 0.2672(3) 0.2010(4) -0.1107(2) 0.0476(8) Uani 1 1 d . . . H2 H 0.3545 0.2043 -0.1295 0.057 Uiso 1 1 calc R . . C3 C 0.2658(4) 0.0929(4) -0.0603(2) 0.0621(10) Uani 1 1 d . . . H3 H 0.3519 0.0238 -0.0449 0.074 Uiso 1 1 calc R . . C4 C 0.1393(4) 0.0851(4) -0.0324(3) 0.0705(12) Uani 1 1 d . . . H4 H 0.1391 0.0102 0.0010 0.085 Uiso 1 1 calc R . . C5 C 0.0108(4) 0.1902(5) -0.0543(3) 0.0757(13) Uani 1 1 d . . . H5 H -0.0761 0.1868 -0.0345 0.091 Uiso 1 1 calc R . . C6 C 0.0113(4) 0.2991(4) -0.1051(2) 0.0590(10) Uani 1 1 d . . . H6 H -0.0751 0.3684 -0.1200 0.071 Uiso 1 1 calc R . . C7 C -0.0421(3) 0.5716(3) -0.20464(19) 0.0387(7) Uani 1 1 d . . . C8 C -0.1290(3) 0.5539(4) -0.2547(2) 0.0501(9) Uani 1 1 d . . . H8 H -0.0897 0.4783 -0.2912 0.060 Uiso 1 1 calc R . . C9 C -0.2736(3) 0.6470(4) -0.2511(3) 0.0589(10) Uani 1 1 d . . . H9 H -0.3316 0.6330 -0.2841 0.071 Uiso 1 1 calc R . . C10 C -0.3303(4) 0.7597(4) -0.1986(3) 0.0675(11) Uani 1 1 d . . . H10 H -0.4272 0.8234 -0.1967 0.081 Uiso 1 1 calc R . . C11 C -0.2464(4) 0.7800(4) -0.1490(3) 0.0750(12) Uani 1 1 d . . . H11 H -0.2860 0.8574 -0.1137 0.090 Uiso 1 1 calc R . . C12 C -0.1022(3) 0.6850(4) -0.1513(2) 0.0581(10) Uani 1 1 d . . . H12 H -0.0456 0.6979 -0.1167 0.070 Uiso 1 1 calc R . . C13 C 0.2324(3) 0.5323(3) -0.1614(2) 0.0378(7) Uani 1 1 d . . . C14 C 0.2668(3) 0.5067(4) -0.0823(2) 0.0496(9) Uani 1 1 d . . . H14 H 0.2472 0.4398 -0.0499 0.059 Uiso 1 1 calc R . . C15 C 0.3308(4) 0.5806(4) -0.0510(2) 0.0602(10) Uani 1 1 d . . . H15 H 0.3552 0.5625 0.0022 0.072 Uiso 1 1 calc R . . C16 C 0.3582(4) 0.6814(4) -0.0988(3) 0.0636(11) Uani 1 1 d . . . H16 H 0.4004 0.7316 -0.0775 0.076 Uiso 1 1 calc R . . C17 C 0.3236(4) 0.7073(4) -0.1771(3) 0.0584(10) Uani 1 1 d . . . H17 H 0.3424 0.7751 -0.2091 0.070 Uiso 1 1 calc R . . C18 C 0.2611(3) 0.6336(3) -0.2091(2) 0.0453(8) Uani 1 1 d . . . H18 H 0.2380 0.6516 -0.2626 0.054 Uiso 1 1 calc R . . C19 C 0.5186(3) 0.3921(3) -0.4078(2) 0.0478(9) Uani 1 1 d . . . C20 C 0.5059(3) 0.3087(3) -0.4735(2) 0.0465(8) Uani 1 1 d . . . C21 C 0.5990(4) 0.2667(4) -0.5469(2) 0.0644(11) Uani 1 1 d . . . H21 H 0.6749 0.2922 -0.5565 0.077 Uiso 1 1 calc R . . C22 C 0.4727(5) 0.1612(4) -0.5864(3) 0.0767(12) Uani 1 1 d . . . H22 H 0.4598 0.1068 -0.6240 0.092 Uiso 1 1 calc R . . C23 C 0.3760(4) 0.2046(4) -0.5169(2) 0.0638(10) Uani 1 1 d . . . H23 H 0.2968 0.1838 -0.5097 0.077 Uiso 1 1 calc R . . C24 C 0.0812(3) 0.1819(3) -0.3509(2) 0.0405(8) Uani 1 1 d . . . C25 C -0.0109(4) 0.2140(4) -0.4085(2) 0.0555(9) Uani 1 1 d . . . H25 H -0.0253 0.2903 -0.4440 0.067 Uiso 1 1 calc R . . C26 C -0.0823(4) 0.1315(5) -0.4130(3) 0.0687(12) Uani 1 1 d . . . H26 H -0.1433 0.1518 -0.4531 0.082 Uiso 1 1 calc R . . C27 C -0.0661(4) 0.0208(4) -0.3604(3) 0.0660(12) Uani 1 1 d . . . C28 C 0.0248(4) -0.0072(4) -0.3013(3) 0.0725(12) Uani 1 1 d . . . H28 H 0.0354 -0.0806 -0.2640 0.087 Uiso 1 1 calc R . . C29 C 0.1001(4) 0.0712(4) -0.2965(3) 0.0620(10) Uani 1 1 d . . . H29 H 0.1626 0.0501 -0.2572 0.074 Uiso 1 1 calc R . . C30 C -0.1481(4) -0.0664(5) -0.3646(4) 0.107(2) Uani 1 1 d . . . H30A H -0.1843 -0.0509 -0.4166 0.160 Uiso 1 1 calc R . . H30B H -0.2273 -0.0389 -0.3209 0.160 Uiso 1 1 calc R . . H30C H -0.0847 -0.1649 -0.3589 0.160 Uiso 1 1 calc R . . N99 N 0.6301(5) 0.1696(5) -0.0868(3) 0.1165(16) Uani 1 1 d . . . C98 C 0.6603(5) 0.3197(5) -0.2101(3) 0.0859(14) Uani 1 1 d . . . H98A H 0.5701 0.3672 -0.2320 0.129 Uiso 1 1 calc R . . H98B H 0.7334 0.2609 -0.2519 0.129 Uiso 1 1 calc R . . H98C H 0.6875 0.3885 -0.1924 0.129 Uiso 1 1 calc R . . C99 C 0.6451(4) 0.2340(5) -0.1418(3) 0.0687(11) 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 Re1 0.04060(8) 0.03961(8) 0.03342(8) -0.00295(5) -0.00341(5) -0.01826(6) Cl1 0.0600(5) 0.0555(6) 0.0494(6) 0.0155(4) -0.0095(4) -0.0176(4) Cl2 0.0537(5) 0.0441(5) 0.0540(6) -0.0026(4) -0.0070(4) -0.0050(4) P1 0.0336(4) 0.0368(5) 0.0344(5) 0.0000(4) -0.0051(3) -0.0144(3) O1 0.0441(12) 0.0479(14) 0.0457(14) -0.0089(11) 0.0025(10) -0.0221(10) O2 0.0509(14) 0.0791(19) 0.077(2) 0.0008(15) 0.0057(13) -0.0370(14) N2 0.0530(16) 0.0417(16) 0.0331(17) 0.0009(13) 0.0012(12) -0.0136(13) N1 0.0472(15) 0.0435(16) 0.0337(16) -0.0013(13) -0.0068(12) -0.0187(13) N3 0.089(3) 0.070(2) 0.042(2) -0.0104(19) 0.0095(18) -0.010(2) C1 0.0444(18) 0.0420(19) 0.0341(19) -0.0017(15) -0.0016(14) -0.0200(15) C2 0.0460(19) 0.046(2) 0.045(2) 0.0023(17) -0.0024(15) -0.0162(16) C3 0.067(2) 0.051(2) 0.056(3) 0.006(2) -0.0104(19) -0.0150(19) C4 0.086(3) 0.050(2) 0.073(3) 0.021(2) -0.003(2) -0.033(2) C5 0.064(3) 0.070(3) 0.099(4) 0.022(3) 0.000(2) -0.041(2) C6 0.054(2) 0.053(2) 0.072(3) 0.014(2) -0.0055(18) -0.0269(18) C7 0.0341(16) 0.0408(19) 0.039(2) 0.0027(15) -0.0042(13) -0.0153(14) C8 0.0448(19) 0.048(2) 0.055(2) 0.0021(18) -0.0106(16) -0.0163(16) C9 0.044(2) 0.064(3) 0.071(3) 0.011(2) -0.0195(18) -0.0234(19) C10 0.039(2) 0.065(3) 0.085(3) 0.005(2) -0.007(2) -0.0110(19) C11 0.049(2) 0.069(3) 0.084(3) -0.021(2) 0.000(2) -0.004(2) C12 0.0421(19) 0.062(2) 0.062(3) -0.017(2) -0.0059(17) -0.0132(17) C13 0.0335(16) 0.0378(18) 0.039(2) -0.0055(15) -0.0048(13) -0.0118(14) C14 0.053(2) 0.056(2) 0.042(2) -0.0008(18) -0.0105(16) -0.0244(17) C15 0.058(2) 0.073(3) 0.052(3) -0.012(2) -0.0170(18) -0.026(2) C16 0.050(2) 0.069(3) 0.081(3) -0.026(2) -0.009(2) -0.030(2) C17 0.056(2) 0.051(2) 0.074(3) -0.012(2) -0.001(2) -0.0289(18) C18 0.0494(19) 0.042(2) 0.044(2) -0.0053(17) -0.0073(15) -0.0181(16) C19 0.0411(19) 0.043(2) 0.050(2) 0.0056(17) 0.0010(16) -0.0124(16) C20 0.0457(19) 0.0404(19) 0.038(2) 0.0030(16) 0.0020(15) -0.0074(15) C21 0.059(2) 0.062(3) 0.049(3) 0.008(2) 0.0089(19) -0.010(2) C22 0.108(4) 0.063(3) 0.044(3) -0.015(2) -0.003(2) -0.024(3) C23 0.083(3) 0.064(3) 0.044(2) -0.013(2) -0.007(2) -0.030(2) C24 0.0410(17) 0.0380(19) 0.044(2) -0.0017(16) -0.0053(15) -0.0179(15) C25 0.068(2) 0.056(2) 0.051(2) 0.0099(19) -0.0264(19) -0.0310(19) C26 0.058(2) 0.072(3) 0.085(3) -0.013(3) -0.024(2) -0.030(2) C27 0.044(2) 0.044(2) 0.110(4) -0.021(2) 0.004(2) -0.0196(18) C28 0.070(3) 0.042(2) 0.106(4) 0.020(2) -0.014(2) -0.026(2) C29 0.059(2) 0.052(2) 0.077(3) 0.018(2) -0.0249(19) -0.0241(19) C30 0.063(3) 0.075(3) 0.194(6) -0.042(4) 0.011(3) -0.044(2) N99 0.147(4) 0.104(4) 0.104(4) 0.029(3) -0.056(3) -0.052(3) C98 0.086(3) 0.097(4) 0.082(4) 0.007(3) -0.020(3) -0.044(3) C99 0.075(3) 0.061(3) 0.069(3) 0.007(2) -0.035(2) -0.022(2) _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 N1 1.702(2) . ? Re1 O1 2.0410(19) . ? Re1 N2 2.130(2) . ? Re1 Cl1 2.3771(9) . ? Re1 Cl2 2.4058(9) . ? Re1 P1 2.4317(8) . ? P1 C1 1.813(3) . ? P1 C13 1.821(3) . ? P1 C7 1.827(3) . ? O1 C19 1.303(4) . ? O2 C19 1.211(4) . ? N2 C20 1.334(4) . ? N2 C23 1.339(4) . ? N1 C24 1.396(4) . ? N3 C21 1.318(5) . ? N3 C22 1.326(5) . ? C1 C6 1.386(4) . ? C1 C2 1.392(4) . ? C2 C3 1.365(5) . ? C2 H2 0.9300 . ? C3 C4 1.364(5) . ? C3 H3 0.9300 . ? C4 C5 1.388(6) . ? C4 H4 0.9300 . ? C5 C6 1.372(5) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.380(4) . ? C7 C8 1.383(4) . ? C8 C9 1.382(5) . ? C8 H8 0.9300 . ? C9 C10 1.366(5) . ? C9 H9 0.9300 . ? C10 C11 1.367(5) . ? C10 H10 0.9300 . ? C11 C12 1.386(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.376(5) . ? C13 C18 1.393(4) . ? C14 C15 1.385(4) . ? C14 H14 0.9300 . ? C15 C16 1.382(5) . ? C15 H15 0.9300 . ? C16 C17 1.365(5) . ? C16 H16 0.9300 . ? C17 C18 1.376(4) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.490(5) . ? C20 C21 1.393(5) . ? C21 H21 0.9300 . ? C22 C23 1.360(5) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.366(5) . ? C24 C29 1.380(5) . ? C25 C26 1.378(5) . ? C25 H25 0.9300 . ? C26 C27 1.367(6) . ? C26 H26 0.9300 . ? C27 C28 1.383(6) . ? C27 C30 1.511(5) . ? C28 C29 1.375(5) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? N99 C99 1.127(6) . ? C98 C99 1.425(6) . ? C98 H98A 0.9600 . ? C98 H98B 0.9600 . ? C98 H98C 0.9600 . ? 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 N1 Re1 O1 173.13(10) . . ? N1 Re1 N2 98.48(11) . . ? O1 Re1 N2 75.62(9) . . ? N1 Re1 Cl1 99.20(9) . . ? O1 Re1 Cl1 84.30(7) . . ? N2 Re1 Cl1 88.50(8) . . ? N1 Re1 Cl2 93.98(9) . . ? O1 Re1 Cl2 82.04(7) . . ? N2 Re1 Cl2 84.17(8) . . ? Cl1 Re1 Cl2 165.74(3) . . ? N1 Re1 P1 91.84(8) . . ? O1 Re1 P1 94.05(6) . . ? N2 Re1 P1 169.67(7) . . ? Cl1 Re1 P1 90.34(3) . . ? Cl2 Re1 P1 94.69(3) . . ? C1 P1 C13 106.73(15) . . ? C1 P1 C7 104.37(14) . . ? C13 P1 C7 104.76(14) . . ? C1 P1 Re1 112.11(10) . . ? C13 P1 Re1 113.56(10) . . ? C7 P1 Re1 114.49(11) . . ? C19 O1 Re1 121.1(2) . . ? C20 N2 C23 117.4(3) . . ? C20 N2 Re1 115.2(2) . . ? C23 N2 Re1 127.4(2) . . ? C24 N1 Re1 173.8(2) . . ? C21 N3 C22 115.5(3) . . ? C6 C1 C2 118.2(3) . . ? C6 C1 P1 121.6(3) . . ? C2 C1 P1 120.0(2) . . ? C3 C2 C1 121.0(3) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C4 C3 C2 120.7(4) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 119.3(4) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C6 C5 C4 120.4(3) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C1 120.4(4) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C12 C7 C8 118.7(3) . . ? C12 C7 P1 121.4(2) . . ? C8 C7 P1 119.9(2) . . ? C9 C8 C7 120.9(3) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C10 C9 C8 119.4(3) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 120.7(3) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C10 C11 C12 119.9(4) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C7 C12 C11 120.4(3) . . ? C7 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C14 C13 C18 119.5(3) . . ? C14 C13 P1 122.9(2) . . ? C18 C13 P1 117.5(2) . . ? C13 C14 C15 120.0(3) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C16 C15 C14 120.0(4) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 C15 120.1(3) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 120.4(4) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C13 120.0(3) . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? O2 C19 O1 125.3(3) . . ? O2 C19 C20 122.1(3) . . ? O1 C19 C20 112.6(3) . . ? N2 C20 C21 119.9(3) . . ? N2 C20 C19 115.2(3) . . ? C21 C20 C19 124.9(3) . . ? N3 C21 C20 123.0(4) . . ? N3 C21 H21 118.5 . . ? C20 C21 H21 118.5 . . ? N3 C22 C23 123.6(4) . . ? N3 C22 H22 118.2 . . ? C23 C22 H22 118.2 . . ? N2 C23 C22 120.6(4) . . ? N2 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C25 C24 C29 120.9(3) . . ? C25 C24 N1 120.2(3) . . ? C29 C24 N1 118.9(3) . . ? C24 C25 C26 119.0(4) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C27 C26 C25 121.9(4) . . ? C27 C26 H26 119.1 . . ? C25 C26 H26 119.1 . . ? C26 C27 C28 118.0(3) . . ? C26 C27 C30 121.4(4) . . ? C28 C27 C30 120.6(4) . . ? C29 C28 C27 121.4(4) . . ? C29 C28 H28 119.3 . . ? C27 C28 H28 119.3 . . ? C28 C29 C24 118.8(4) . . ? C28 C29 H29 120.6 . . ? C24 C29 H29 120.6 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C99 C98 H98A 109.5 . . ? C99 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? C99 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? N99 C99 C98 178.1(6) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C2 H2 Cl2 0.93 2.72 3.233(3) 115.6 . C22 H22 Cl2 0.93 2.74 3.589(4) 152.3 2_654 C30 H30B Cl2 0.96 2.98 3.770(4) 140.6 1_455 C98 H98A O1 0.96 2.55 3.428(5) 152.5 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.679 _refine_diff_density_min -0.655 _refine_diff_density_rms 0.070 _database_code_depnum_ccdc_archive 'CCDC 973294' data_added_by_encifer _publ_section_references ;CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET) Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. Flack. H. D. (1983). Acta Cryst. A39, 876--881. Sheldrick, G. M. (1990a). Acta Cryst. A46, 467--473. Sheldrick, G. M. (1990b). SHELXTL/PC Software. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany Spek, A. L. (1990). Acta Cryst. A46, C-34. UNIL IC & KUMA (2000). CrysAlis CCD. Version 1.163. Kuma Diffraction Instruments GmbH, Wroc\/law, Poland. UNIL IC & KUMA (2000). CrysAlis RED. Version 1.163. Kuma Diffraction Instruments GmbH, Wroc\/law, Poland. ; data_ren267 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H25 Cl2 N3 O2 P Re' _chemical_formula_sum 'C30 H25 Cl2 N3 O2 P Re' _chemical_formula_weight 747.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7169(5) _cell_length_b 14.4692(9) _cell_length_c 22.3218(12) _cell_angle_alpha 97.987(5) _cell_angle_beta 90.759(5) _cell_angle_gamma 105.589(5) _cell_volume 2989.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293.0(2) _cell_measurement_reflns_used 8700 _cell_measurement_theta_min 3.3717 _cell_measurement_theta_max 29.3294 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.091 _exptl_crystal_size_mid 0.077 _exptl_crystal_size_min 0.016 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.661 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 4.329 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ;CrysAlis RED, (2005) ; _exptl_absorpt_correction_T_min 0.50725 _exptl_absorpt_correction_T_max 1.00000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293.0(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 'Xcalibur, Atlas, Gemini ultra' _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 28030 _diffrn_reflns_av_R_equivalents 0.0712 _diffrn_reflns_av_unetI/netI 0.0987 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 25.05 _reflns_number_total 10568 _reflns_number_gt 7544 _reflns_threshold_expression >2sigma(I) #========================================================================== # # REFINEMENT DATA _computing_data_collection 'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)' _computing_cell_refinement 'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)' _computing_data_reduction 'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;XP in SHELXTL/PC (Sheldrick, 1990b) ORTEP-3 W v. 1.062 (Farrugia 1997) ; _computing_publication_material ;SHELXL-97 (Sheldrick, 1997) and PLATON (Spek, 1990) ; _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^)+(0.0436P)^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 10568 _refine_ls_number_parameters 705 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0785 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1166 _refine_ls_wR_factor_gt 0.1057 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _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 Re1 Re 0.45574(3) 0.31812(2) 0.168947(15) 0.03251(11) Uani 1 1 d . . . Re2 Re -0.09098(3) 0.84519(2) 0.327419(15) 0.03281(11) Uani 1 1 d . . . N2 N 0.3990(7) 0.4048(4) 0.2445(3) 0.0322(16) Uani 1 1 d . . . N1 N 0.5856(7) 0.3999(4) 0.1372(3) 0.0345(17) Uani 1 1 d . . . N3 N 0.3201(9) 0.4952(5) 0.3523(3) 0.049(2) Uani 1 1 d . . . N4 N -0.2123(8) 0.9288(5) 0.2901(3) 0.0418(19) Uani 1 1 d . . . N5 N 0.0620(7) 0.9375(5) 0.3439(3) 0.0393(18) Uani 1 1 d . . . N6 N -0.3995(10) 1.0235(7) 0.2474(4) 0.064(2) Uani 1 1 d . . . O1 O 0.2858(6) 0.2246(4) 0.2031(3) 0.0449(15) Uani 1 1 d . . . O2 O 0.1191(7) 0.2056(4) 0.2711(3) 0.0583(18) Uani 1 1 d . . . O3 O -0.2924(6) 0.7507(4) 0.3086(3) 0.0421(14) Uani 1 1 d . . . O4 O -0.5055(7) 0.7257(5) 0.2608(4) 0.077(2) Uani 1 1 d . . . Cl1 Cl 0.6029(3) 0.27776(17) 0.24147(10) 0.0504(6) Uani 1 1 d . . . Cl2 Cl 0.2673(3) 0.35346(19) 0.11329(11) 0.0559(6) Uani 1 1 d . . . Cl3 Cl -0.1866(2) 0.88288(16) 0.42354(11) 0.0506(6) Uani 1 1 d . . . Cl4 Cl -0.0582(3) 0.78826(17) 0.22511(11) 0.0573(7) Uani 1 1 d . . . P1 P 0.4802(2) 0.18338(15) 0.09453(10) 0.0347(5) Uani 1 1 d . . . P2 P 0.0030(2) 0.72387(15) 0.36776(10) 0.0331(5) Uani 1 1 d . . . C1 C 0.3349(9) 0.0743(6) 0.0967(4) 0.038(2) Uani 1 1 d . . . C2 C 0.2432(10) 0.0280(6) 0.0481(4) 0.046(2) Uani 1 1 d . . . H2 H 0.2582 0.0528 0.0117 0.056 Uiso 1 1 calc R . . C3 C 0.1306(10) -0.0525(6) 0.0495(5) 0.054(3) Uani 1 1 d . . . H3 H 0.0704 -0.0824 0.0156 0.064 Uiso 1 1 calc R . . C4 C 0.1120(10) -0.0869(7) 0.1053(5) 0.056(3) Uani 1 1 d . . . H4 H 0.0358 -0.1404 0.1088 0.067 Uiso 1 1 calc R . . C5 C 0.2028(10) -0.0439(7) 0.1549(5) 0.054(3) Uani 1 1 d . . . H5 H 0.1884 -0.0690 0.1912 0.065 Uiso 1 1 calc R . . C6 C 0.3166(9) 0.0371(6) 0.1509(4) 0.044(2) Uani 1 1 d . . . H6 H 0.3795 0.0659 0.1842 0.053 Uiso 1 1 calc R . . C7 C 0.4810(9) 0.2063(6) 0.0158(4) 0.042(2) Uani 1 1 d . . . C8 C 0.5967(10) 0.2017(6) -0.0184(4) 0.052(3) Uani 1 1 d . . . H8 H 0.6739 0.1849 -0.0024 0.062 Uiso 1 1 calc R . . C9 C 0.5959(12) 0.2229(7) -0.0780(5) 0.066(3) Uani 1 1 d . . . H9 H 0.6728 0.2182 -0.1014 0.079 Uiso 1 1 calc R . . C10 C 0.4868(14) 0.2500(8) -0.1024(5) 0.072(3) Uani 1 1 d . . . H10 H 0.4895 0.2654 -0.1416 0.087 Uiso 1 1 calc R . . C11 C 0.3716(12) 0.2540(7) -0.0675(5) 0.063(3) Uani 1 1 d . . . H11 H 0.2946 0.2710 -0.0835 0.076 Uiso 1 1 calc R . . C12 C 0.3699(10) 0.2326(6) -0.0085(4) 0.047(2) Uani 1 1 d . . . H12 H 0.2922 0.2363 0.0147 0.056 Uiso 1 1 calc R . . C13 C 0.6463(9) 0.1501(6) 0.1068(4) 0.041(2) Uani 1 1 d . . . C14 C 0.7718(9) 0.2227(7) 0.1181(5) 0.053(3) Uani 1 1 d . . . H14 H 0.7715 0.2871 0.1189 0.064 Uiso 1 1 calc R . . C15 C 0.8999(10) 0.1996(7) 0.1285(5) 0.061(3) Uani 1 1 d . . . H15 H 0.9843 0.2490 0.1378 0.074 Uiso 1 1 calc R . . C16 C 0.9021(11) 0.1051(8) 0.1250(5) 0.060(3) Uani 1 1 d . . . H16 H 0.9878 0.0897 0.1309 0.072 Uiso 1 1 calc R . . C17 C 0.7790(12) 0.0346(7) 0.1130(5) 0.057(3) Uani 1 1 d . . . H17 H 0.7810 -0.0296 0.1115 0.069 Uiso 1 1 calc R . . C18 C 0.6477(10) 0.0540(6) 0.1028(4) 0.046(2) Uani 1 1 d . . . H18 H 0.5641 0.0039 0.0935 0.055 Uiso 1 1 calc R . . C19 C 0.2227(9) 0.2537(6) 0.2501(4) 0.036(2) Uani 1 1 d . . . C20 C 0.2931(9) 0.3564(6) 0.2761(4) 0.035(2) Uani 1 1 d . . . C21 C 0.2583(10) 0.4028(7) 0.3289(4) 0.048(2) Uani 1 1 d . . . H21 H 0.1861 0.3673 0.3502 0.058 Uiso 1 1 calc R . . C22 C 0.4179(10) 0.5400(6) 0.3181(4) 0.048(2) Uani 1 1 d . . . H22 H 0.4602 0.6059 0.3302 0.058 Uiso 1 1 calc R . . C23 C 0.4615(9) 0.4976(6) 0.2670(4) 0.042(2) Uani 1 1 d . . . H23 H 0.5361 0.5335 0.2470 0.051 Uiso 1 1 calc R . . C24 C 0.6788(9) 0.4636(5) 0.1063(4) 0.035(2) Uani 1 1 d . . . C25 C 0.8015(10) 0.5274(6) 0.1364(4) 0.050(2) Uani 1 1 d . . . H25 H 0.8178 0.5300 0.1778 0.060 Uiso 1 1 calc R . . C26 C 0.8999(10) 0.5874(7) 0.1036(4) 0.050(2) Uani 1 1 d . . . H26 H 0.9816 0.6306 0.1235 0.060 Uiso 1 1 calc R . . C27 C 0.8772(9) 0.5831(6) 0.0418(4) 0.044(2) Uani 1 1 d . . . C28 C 0.7504(10) 0.5194(6) 0.0129(4) 0.051(3) Uani 1 1 d . . . H28 H 0.7321 0.5165 -0.0284 0.061 Uiso 1 1 calc R . . C29 C 0.6545(9) 0.4620(6) 0.0456(4) 0.040(2) Uani 1 1 d . . . H29 H 0.5706 0.4208 0.0262 0.048 Uiso 1 1 calc R . . C30 C 0.9878(10) 0.6447(7) 0.0049(5) 0.067(3) Uani 1 1 d . . . H30A H 1.0062 0.6044 -0.0303 0.100 Uiso 1 1 calc R . . H30B H 1.0750 0.6732 0.0293 0.100 Uiso 1 1 calc R . . H30C H 0.9517 0.6951 -0.0074 0.100 Uiso 1 1 calc R . . C31 C 0.1706(8) 0.7813(6) 0.4113(4) 0.036(2) Uani 1 1 d . . . C32 C 0.1809(9) 0.8587(6) 0.4571(4) 0.044(2) Uani 1 1 d . . . H32 H 0.1023 0.8833 0.4633 0.053 Uiso 1 1 calc R . . C33 C 0.3004(11) 0.8994(7) 0.4926(5) 0.058(3) Uani 1 1 d . . . H33 H 0.3014 0.9494 0.5239 0.069 Uiso 1 1 calc R . . C34 C 0.4223(11) 0.8679(8) 0.4835(6) 0.070(3) Uani 1 1 d . . . H34 H 0.5060 0.8982 0.5072 0.084 Uiso 1 1 calc R . . C35 C 0.4175(10) 0.7916(8) 0.4390(6) 0.075(3) Uani 1 1 d . . . H35 H 0.4973 0.7681 0.4334 0.090 Uiso 1 1 calc R . . C36 C 0.2922(9) 0.7486(7) 0.4016(5) 0.056(3) Uani 1 1 d . . . H36 H 0.2906 0.6983 0.3705 0.068 Uiso 1 1 calc R . . C37 C 0.0336(9) 0.6288(6) 0.3105(4) 0.040(2) Uani 1 1 d . . . C38 C 0.1359(9) 0.6541(7) 0.2693(4) 0.050(2) Uani 1 1 d . . . H38 H 0.1893 0.7184 0.2714 0.060 Uiso 1 1 calc R . . C39 C 0.1602(10) 0.5832(8) 0.2243(5) 0.059(3) Uani 1 1 d . . . H39 H 0.2295 0.6007 0.1965 0.071 Uiso 1 1 calc R . . C40 C 0.0819(12) 0.4883(8) 0.2211(5) 0.064(3) Uani 1 1 d . . . H40 H 0.0983 0.4411 0.1915 0.077 Uiso 1 1 calc R . . C41 C -0.0177(12) 0.4646(7) 0.2607(5) 0.066(3) Uani 1 1 d . . . H41 H -0.0725 0.4005 0.2575 0.079 Uiso 1 1 calc R . . C42 C -0.0431(10) 0.5325(6) 0.3072(5) 0.051(2) Uani 1 1 d . . . H42 H -0.1105 0.5133 0.3354 0.061 Uiso 1 1 calc R . . C43 C -0.1068(8) 0.6554(5) 0.4214(4) 0.0334(19) Uani 1 1 d . . . C44 C -0.0448(10) 0.6278(7) 0.4694(4) 0.053(3) Uani 1 1 d . . . H44 H 0.0537 0.6490 0.4773 0.063 Uiso 1 1 calc R . . C45 C -0.1290(11) 0.5690(7) 0.5053(5) 0.060(3) Uani 1 1 d . . . H45 H -0.0865 0.5498 0.5373 0.072 Uiso 1 1 calc R . . C46 C -0.2720(11) 0.5383(7) 0.4955(4) 0.056(3) Uani 1 1 d . . . H46 H -0.3276 0.4994 0.5209 0.067 Uiso 1 1 calc R . . C47 C -0.3366(12) 0.5651(8) 0.4470(6) 0.077(4) Uani 1 1 d . . . H47 H -0.4351 0.5432 0.4389 0.092 Uiso 1 1 calc R . . C48 C -0.2529(9) 0.6236(7) 0.4120(5) 0.057(3) Uani 1 1 d . . . H48 H -0.2958 0.6431 0.3803 0.069 Uiso 1 1 calc R . . C49 C -0.3899(10) 0.7779(7) 0.2798(4) 0.047(2) Uani 1 1 d . . . C50 C -0.3473(9) 0.8817(6) 0.2731(4) 0.043(2) Uani 1 1 d . . . C51 C -0.4382(10) 0.9304(7) 0.2512(4) 0.056(3) Uani 1 1 d . . . H51 H -0.5314 0.8951 0.2386 0.068 Uiso 1 1 calc R . . C52 C -0.2648(13) 1.0674(7) 0.2626(5) 0.062(3) Uani 1 1 d . . . H52 H -0.2323 1.1330 0.2592 0.074 Uiso 1 1 calc R . . C53 C -0.1654(10) 1.0229(6) 0.2839(4) 0.050(2) Uani 1 1 d . . . H53 H -0.0704 1.0575 0.2933 0.060 Uiso 1 1 calc R . . C54 C 0.1695(8) 1.0242(6) 0.3617(4) 0.037(2) Uani 1 1 d . . . C55 C 0.2935(9) 1.0438(7) 0.3311(5) 0.054(3) Uani 1 1 d . . . H55 H 0.3093 0.9989 0.2998 0.064 Uiso 1 1 calc R . . C56 C 0.3940(10) 1.1321(7) 0.3481(5) 0.059(3) Uani 1 1 d . . . H56 H 0.4766 1.1465 0.3267 0.071 Uiso 1 1 calc R . . C57 C 0.3771(10) 1.1989(6) 0.3949(5) 0.052(3) Uani 1 1 d . . . C58 C 0.2521(11) 1.1766(7) 0.4253(5) 0.059(3) Uani 1 1 d . . . H58 H 0.2375 1.2208 0.4574 0.071 Uiso 1 1 calc R . . C59 C 0.1486(10) 1.0900(6) 0.4090(4) 0.053(3) Uani 1 1 d . . . H59 H 0.0651 1.0761 0.4299 0.064 Uiso 1 1 calc R . . C60 C 0.4867(11) 1.2925(7) 0.4125(5) 0.073(3) Uani 1 1 d . . . H60A H 0.5030 1.3047 0.4558 0.109 Uiso 1 1 calc R . . H60B H 0.4539 1.3437 0.3993 0.109 Uiso 1 1 calc R . . H60C H 0.5743 1.2898 0.3939 0.109 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 0.0317(2) 0.03059(19) 0.0359(2) 0.00792(16) 0.00549(16) 0.00799(15) Re2 0.02987(19) 0.02833(19) 0.0403(2) 0.00733(16) 0.00368(16) 0.00695(15) N2 0.039(4) 0.031(4) 0.030(4) 0.004(3) 0.002(3) 0.016(3) N1 0.039(4) 0.028(3) 0.041(4) 0.010(3) 0.007(3) 0.013(3) N3 0.065(5) 0.041(4) 0.042(5) 0.003(4) 0.005(4) 0.017(4) N4 0.051(5) 0.032(4) 0.047(5) 0.018(4) 0.010(4) 0.012(4) N5 0.039(4) 0.035(4) 0.048(5) 0.004(3) 0.006(4) 0.018(4) N6 0.067(6) 0.067(6) 0.069(6) 0.019(5) -0.005(5) 0.033(5) O1 0.044(4) 0.035(3) 0.048(4) 0.000(3) 0.011(3) 0.000(3) O2 0.051(4) 0.054(4) 0.061(5) 0.012(4) 0.023(4) -0.003(3) O3 0.035(3) 0.034(3) 0.054(4) 0.012(3) -0.004(3) 0.001(3) O4 0.044(4) 0.077(5) 0.102(6) 0.043(5) -0.025(4) -0.009(4) Cl1 0.0580(15) 0.0542(14) 0.0464(14) 0.0146(12) -0.0010(12) 0.0243(12) Cl2 0.0502(14) 0.0844(17) 0.0440(14) 0.0088(13) 0.0028(12) 0.0370(14) Cl3 0.0484(14) 0.0571(14) 0.0514(15) 0.0078(12) 0.0155(12) 0.0227(12) Cl4 0.0732(17) 0.0576(14) 0.0423(14) 0.0091(12) 0.0113(13) 0.0185(14) P1 0.0333(12) 0.0333(12) 0.0372(13) 0.0055(10) 0.0047(10) 0.0080(10) P2 0.0270(11) 0.0306(11) 0.0424(14) 0.0064(10) 0.0051(10) 0.0086(10) C1 0.033(5) 0.035(5) 0.048(6) 0.005(4) 0.001(5) 0.013(4) C2 0.045(6) 0.037(5) 0.052(6) 0.008(5) 0.009(5) 0.002(5) C3 0.052(6) 0.044(6) 0.054(7) 0.000(5) -0.001(5) -0.002(5) C4 0.040(6) 0.047(6) 0.071(8) 0.001(6) 0.008(6) -0.003(5) C5 0.052(6) 0.048(6) 0.059(7) 0.017(5) 0.005(6) 0.003(5) C6 0.042(5) 0.040(5) 0.049(6) 0.013(5) 0.004(5) 0.004(4) C7 0.047(5) 0.036(5) 0.042(5) 0.004(4) 0.006(5) 0.011(4) C8 0.058(6) 0.054(6) 0.044(6) 0.009(5) 0.009(5) 0.015(5) C9 0.081(8) 0.065(7) 0.052(7) 0.011(6) 0.032(6) 0.018(6) C10 0.102(10) 0.064(7) 0.055(7) 0.007(6) -0.003(7) 0.032(7) C11 0.084(8) 0.060(6) 0.050(7) 0.001(5) -0.010(6) 0.030(6) C12 0.049(6) 0.057(6) 0.035(5) -0.002(5) 0.001(5) 0.020(5) C13 0.032(5) 0.046(5) 0.048(6) 0.010(5) 0.013(4) 0.011(4) C14 0.038(5) 0.051(6) 0.073(7) 0.007(5) 0.011(5) 0.015(5) C15 0.027(5) 0.066(7) 0.082(8) -0.010(6) 0.003(5) 0.008(5) C16 0.054(7) 0.076(8) 0.056(7) -0.003(6) 0.003(6) 0.036(6) C17 0.071(7) 0.048(6) 0.064(7) 0.009(5) 0.002(6) 0.033(6) C18 0.059(6) 0.043(5) 0.046(6) 0.009(5) 0.016(5) 0.029(5) C19 0.034(5) 0.038(5) 0.036(5) 0.010(4) 0.006(4) 0.009(4) C20 0.036(5) 0.046(5) 0.026(5) 0.008(4) 0.000(4) 0.012(4) C21 0.045(6) 0.053(6) 0.044(6) 0.006(5) 0.010(5) 0.009(5) C22 0.065(7) 0.034(5) 0.044(6) 0.003(5) -0.002(5) 0.012(5) C23 0.048(6) 0.031(5) 0.046(6) 0.006(4) 0.005(5) 0.009(4) C24 0.038(5) 0.027(4) 0.042(5) 0.013(4) 0.006(4) 0.008(4) C25 0.055(6) 0.048(6) 0.037(6) 0.003(5) -0.011(5) 0.001(5) C26 0.038(5) 0.053(6) 0.047(6) 0.005(5) -0.008(5) -0.007(5) C27 0.032(5) 0.034(5) 0.062(7) 0.017(5) 0.009(5) 0.000(4) C28 0.069(7) 0.042(5) 0.042(6) 0.016(5) 0.002(5) 0.011(5) C29 0.037(5) 0.036(5) 0.039(6) 0.008(4) -0.006(4) -0.007(4) C30 0.056(7) 0.062(7) 0.075(8) 0.030(6) 0.006(6) -0.005(6) C31 0.026(4) 0.033(5) 0.047(6) 0.014(4) 0.002(4) 0.003(4) C32 0.039(5) 0.037(5) 0.054(6) -0.003(5) -0.006(5) 0.014(4) C33 0.064(7) 0.041(5) 0.059(7) -0.013(5) -0.020(6) 0.010(5) C34 0.053(7) 0.054(7) 0.099(10) 0.018(7) -0.016(6) 0.005(6) C35 0.030(6) 0.078(8) 0.113(11) -0.011(7) -0.007(6) 0.020(6) C36 0.033(5) 0.062(6) 0.070(7) -0.005(5) 0.000(5) 0.015(5) C37 0.032(5) 0.049(5) 0.046(6) 0.004(4) 0.004(4) 0.022(4) C38 0.042(5) 0.053(6) 0.054(6) 0.001(5) 0.018(5) 0.014(5) C39 0.042(6) 0.094(9) 0.048(6) -0.002(6) 0.005(5) 0.035(6) C40 0.059(7) 0.064(7) 0.070(8) -0.021(6) -0.008(6) 0.035(6) C41 0.069(7) 0.036(5) 0.085(9) -0.019(6) -0.026(7) 0.017(5) C42 0.049(6) 0.030(5) 0.070(7) 0.008(5) 0.000(5) 0.005(5) C43 0.034(5) 0.026(4) 0.039(5) 0.001(4) 0.004(4) 0.008(4) C44 0.043(5) 0.062(6) 0.054(6) 0.024(5) 0.004(5) 0.008(5) C45 0.068(7) 0.066(7) 0.053(7) 0.019(6) -0.001(6) 0.025(6) C46 0.056(7) 0.068(7) 0.047(6) 0.022(6) 0.019(6) 0.014(6) C47 0.053(7) 0.072(8) 0.101(10) 0.031(7) 0.014(7) -0.001(6) C48 0.036(5) 0.074(7) 0.065(7) 0.041(6) 0.008(5) 0.003(5) C49 0.032(5) 0.057(6) 0.052(6) 0.023(5) 0.000(5) 0.005(5) C50 0.036(5) 0.050(6) 0.045(6) 0.015(5) -0.003(5) 0.009(5) C51 0.047(6) 0.065(7) 0.061(7) 0.014(6) 0.002(5) 0.020(5) C52 0.091(9) 0.046(6) 0.056(7) 0.008(5) 0.002(7) 0.032(7) C53 0.045(5) 0.035(5) 0.067(7) 0.014(5) 0.001(5) 0.002(4) C54 0.032(5) 0.031(5) 0.043(5) 0.001(4) -0.003(4) 0.002(4) C55 0.039(5) 0.050(6) 0.065(7) -0.004(5) 0.005(5) 0.006(5) C56 0.040(6) 0.055(6) 0.069(8) 0.001(6) 0.013(5) -0.007(5) C57 0.055(6) 0.035(5) 0.058(7) 0.003(5) 0.006(5) 0.000(5) C58 0.075(7) 0.040(6) 0.059(7) -0.003(5) 0.011(6) 0.015(6) C59 0.054(6) 0.040(5) 0.061(7) 0.001(5) 0.016(5) 0.011(5) C60 0.069(7) 0.040(6) 0.089(9) -0.004(6) -0.007(7) -0.013(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 N1 1.718(6) . ? Re1 O1 2.063(5) . ? Re1 N2 2.129(6) . ? Re1 Cl1 2.378(2) . ? Re1 Cl2 2.404(2) . ? Re1 P1 2.445(2) . ? Re2 N5 1.706(7) . ? Re2 O3 2.063(6) . ? Re2 N4 2.137(6) . ? Re2 Cl4 2.373(2) . ? Re2 Cl3 2.401(2) . ? Re2 P2 2.4507(19) . ? N2 C23 1.338(10) . ? N2 C20 1.347(9) . ? N1 C24 1.374(9) . ? N3 C22 1.316(10) . ? N3 C21 1.337(11) . ? N4 C50 1.328(11) . ? N4 C53 1.343(10) . ? N5 C54 1.404(10) . ? N6 C52 1.309(13) . ? N6 C51 1.313(12) . ? O1 C19 1.299(9) . ? O2 C19 1.202(8) . ? O3 C49 1.311(10) . ? O4 C49 1.206(11) . ? P1 C1 1.820(8) . ? P1 C13 1.832(8) . ? P1 C7 1.833(9) . ? P2 C31 1.815(9) . ? P2 C43 1.830(7) . ? P2 C37 1.832(8) . ? C1 C2 1.368(12) . ? C1 C6 1.386(11) . ? C2 C3 1.372(12) . ? C2 H2 0.9300 . ? C3 C4 1.399(13) . ? C3 H3 0.9300 . ? C4 C5 1.370(14) . ? C4 H4 0.9300 . ? C5 C6 1.393(12) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.365(12) . ? C7 C8 1.378(11) . ? C8 C9 1.406(13) . ? C8 H8 0.9300 . ? C9 C10 1.357(14) . ? C9 H9 0.9300 . ? C10 C11 1.382(14) . ? C10 H10 0.9300 . ? C11 C12 1.394(12) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.373(12) . ? C13 C18 1.384(11) . ? C14 C15 1.397(12) . ? C14 H14 0.9300 . ? C15 C16 1.366(13) . ? C15 H15 0.9300 . ? C16 C17 1.343(14) . ? C16 H16 0.9300 . ? C17 C18 1.401(12) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.488(12) . ? C20 C21 1.367(11) . ? C21 H21 0.9300 . ? C22 C23 1.347(11) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C29 1.368(11) . ? C24 C25 1.393(12) . ? C25 C26 1.397(11) . ? C25 H25 0.9300 . ? C26 C27 1.385(13) . ? C26 H26 0.9300 . ? C27 C28 1.409(13) . ? C27 C30 1.529(11) . ? C28 C29 1.364(10) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C32 1.388(12) . ? C31 C36 1.395(11) . ? C32 C33 1.343(13) . ? C32 H32 0.9300 . ? C33 C34 1.386(13) . ? C33 H33 0.9300 . ? C34 C35 1.369(15) . ? C34 H34 0.9300 . ? C35 C36 1.409(14) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.374(10) . ? C37 C42 1.383(11) . ? C38 C39 1.403(12) . ? C38 H38 0.9300 . ? C39 C40 1.371(13) . ? C39 H39 0.9300 . ? C40 C41 1.329(13) . ? C40 H40 0.9300 . ? C41 C42 1.399(13) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C48 1.374(12) . ? C43 C44 1.379(12) . ? C44 C45 1.368(11) . ? C44 H44 0.9300 . ? C45 C46 1.345(13) . ? C45 H45 0.9300 . ? C46 C47 1.396(15) . ? C46 H46 0.9300 . ? C47 C48 1.347(12) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C50 1.478(12) . ? C50 C51 1.390(12) . ? C51 H51 0.9300 . ? C52 C53 1.407(13) . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? C54 C59 1.374(11) . ? C54 C55 1.376(11) . ? C55 C56 1.383(13) . ? C55 H55 0.9300 . ? C56 C57 1.365(13) . ? C56 H56 0.9300 . ? C57 C58 1.383(12) . ? C57 C60 1.480(13) . ? C58 C59 1.378(13) . ? C58 H58 0.9300 . ? C59 H59 0.9300 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? 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 N1 Re1 O1 174.6(3) . . ? N1 Re1 N2 103.4(3) . . ? O1 Re1 N2 75.7(2) . . ? N1 Re1 Cl1 98.9(2) . . ? O1 Re1 Cl1 86.36(18) . . ? N2 Re1 Cl1 84.60(18) . . ? N1 Re1 Cl2 92.2(2) . . ? O1 Re1 Cl2 82.48(18) . . ? N2 Re1 Cl2 85.78(18) . . ? Cl1 Re1 Cl2 166.77(7) . . ? N1 Re1 P1 91.8(2) . . ? O1 Re1 P1 89.37(16) . . ? N2 Re1 P1 164.67(17) . . ? Cl1 Re1 P1 90.93(8) . . ? Cl2 Re1 P1 96.01(8) . . ? N5 Re2 O3 170.9(2) . . ? N5 Re2 N4 96.1(3) . . ? O3 Re2 N4 75.7(2) . . ? N5 Re2 Cl4 100.6(2) . . ? O3 Re2 Cl4 82.89(17) . . ? N4 Re2 Cl4 85.25(19) . . ? N5 Re2 Cl3 92.9(2) . . ? O3 Re2 Cl3 82.96(17) . . ? N4 Re2 Cl3 88.10(18) . . ? Cl4 Re2 Cl3 165.48(9) . . ? N5 Re2 P2 95.2(2) . . ? O3 Re2 P2 92.92(15) . . ? N4 Re2 P2 168.6(2) . . ? Cl4 Re2 P2 93.91(8) . . ? Cl3 Re2 P2 90.06(7) . . ? C23 N2 C20 116.7(7) . . ? C23 N2 Re1 128.6(5) . . ? C20 N2 Re1 114.5(5) . . ? C24 N1 Re1 173.6(6) . . ? C22 N3 C21 113.0(8) . . ? C50 N4 C53 118.4(7) . . ? C50 N4 Re2 115.4(5) . . ? C53 N4 Re2 126.2(7) . . ? C54 N5 Re2 168.7(5) . . ? C52 N6 C51 115.0(8) . . ? C19 O1 Re1 121.2(5) . . ? C49 O3 Re2 119.3(5) . . ? C1 P1 C13 106.3(4) . . ? C1 P1 C7 105.9(4) . . ? C13 P1 C7 104.9(4) . . ? C1 P1 Re1 111.6(3) . . ? C13 P1 Re1 112.9(3) . . ? C7 P1 Re1 114.6(3) . . ? C31 P2 C43 102.9(4) . . ? C31 P2 C37 107.7(4) . . ? C43 P2 C37 103.3(4) . . ? C31 P2 Re2 110.7(2) . . ? C43 P2 Re2 116.4(2) . . ? C37 P2 Re2 114.8(3) . . ? C2 C1 C6 118.8(8) . . ? C2 C1 P1 123.5(6) . . ? C6 C1 P1 117.7(7) . . ? C1 C2 C3 124.2(9) . . ? C1 C2 H2 117.9 . . ? C3 C2 H2 117.9 . . ? C2 C3 C4 115.8(10) . . ? C2 C3 H3 122.1 . . ? C4 C3 H3 122.1 . . ? C5 C4 C3 121.9(9) . . ? C5 C4 H4 119.0 . . ? C3 C4 H4 119.0 . . ? C4 C5 C6 120.1(9) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C1 C6 C5 119.1(9) . . ? C1 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C12 C7 C8 119.5(8) . . ? C12 C7 P1 120.2(6) . . ? C8 C7 P1 120.2(7) . . ? C7 C8 C9 118.8(9) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C10 C9 C8 122.3(9) . . ? C10 C9 H9 118.8 . . ? C8 C9 H9 118.8 . . ? C9 C10 C11 118.1(10) . . ? C9 C10 H10 121.0 . . ? C11 C10 H10 121.0 . . ? C10 C11 C12 120.5(10) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C7 C12 C11 120.8(8) . . ? C7 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C14 C13 C18 120.1(8) . . ? C14 C13 P1 118.5(6) . . ? C18 C13 P1 121.4(7) . . ? C13 C14 C15 119.8(8) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 120.4(9) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C17 C16 C15 119.2(9) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C16 C17 C18 122.5(9) . . ? C16 C17 H17 118.7 . . ? C18 C17 H17 118.7 . . ? C13 C18 C17 117.9(9) . . ? C13 C18 H18 121.1 . . ? C17 C18 H18 121.1 . . ? O2 C19 O1 125.6(8) . . ? O2 C19 C20 122.4(7) . . ? O1 C19 C20 112.0(6) . . ? N2 C20 C21 119.2(8) . . ? N2 C20 C19 116.3(7) . . ? C21 C20 C19 124.6(7) . . ? N3 C21 C20 125.0(8) . . ? N3 C21 H21 117.5 . . ? C20 C21 H21 117.5 . . ? N3 C22 C23 124.9(9) . . ? N3 C22 H22 117.5 . . ? C23 C22 H22 117.5 . . ? N2 C23 C22 121.0(8) . . ? N2 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C29 C24 N1 120.3(8) . . ? C29 C24 C25 119.8(7) . . ? N1 C24 C25 119.9(8) . . ? C24 C25 C26 119.3(9) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? C27 C26 C25 120.7(9) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C26 C27 C28 118.7(7) . . ? C26 C27 C30 121.1(9) . . ? C28 C27 C30 120.2(9) . . ? C29 C28 C27 120.0(9) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C24 121.5(9) . . ? C28 C29 H29 119.2 . . ? C24 C29 H29 119.2 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C36 117.4(8) . . ? C32 C31 P2 120.6(6) . . ? C36 C31 P2 122.0(7) . . ? C33 C32 C31 122.4(8) . . ? C33 C32 H32 118.8 . . ? C31 C32 H32 118.8 . . ? C32 C33 C34 120.9(10) . . ? C32 C33 H33 119.5 . . ? C34 C33 H33 119.5 . . ? C35 C34 C33 118.9(11) . . ? C35 C34 H34 120.6 . . ? C33 C34 H34 120.6 . . ? C34 C35 C36 120.3(9) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C31 C36 C35 120.0(9) . . ? C31 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C38 C37 C42 118.9(8) . . ? C38 C37 P2 118.9(7) . . ? C42 C37 P2 122.2(6) . . ? C37 C38 C39 120.2(9) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C40 C39 C38 120.1(9) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C41 C40 C39 119.3(9) . . ? C41 C40 H40 120.4 . . ? C39 C40 H40 120.4 . . ? C40 C41 C42 122.4(10) . . ? C40 C41 H41 118.8 . . ? C42 C41 H41 118.8 . . ? C37 C42 C41 118.9(9) . . ? C37 C42 H42 120.5 . . ? C41 C42 H42 120.5 . . ? C48 C43 C44 118.2(7) . . ? C48 C43 P2 120.6(7) . . ? C44 C43 P2 121.1(6) . . ? C45 C44 C43 119.7(9) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C46 C45 C44 121.4(9) . . ? C46 C45 H45 119.3 . . ? C44 C45 H45 119.3 . . ? C45 C46 C47 119.8(9) . . ? C45 C46 H46 120.1 . . ? C47 C46 H46 120.1 . . ? C48 C47 C46 118.4(10) . . ? C48 C47 H47 120.8 . . ? C46 C47 H47 120.8 . . ? C47 C48 C43 122.5(9) . . ? C47 C48 H48 118.7 . . ? C43 C48 H48 118.7 . . ? O4 C49 O3 125.1(8) . . ? O4 C49 C50 121.2(8) . . ? O3 C49 C50 113.7(8) . . ? N4 C50 C51 120.2(8) . . ? N4 C50 C49 115.3(7) . . ? C51 C50 C49 124.5(9) . . ? N6 C51 C50 123.5(10) . . ? N6 C51 H51 118.2 . . ? C50 C51 H51 118.2 . . ? N6 C52 C53 124.9(9) . . ? N6 C52 H52 117.6 . . ? C53 C52 H52 117.6 . . ? N4 C53 C52 117.8(9) . . ? N4 C53 H53 121.1 . . ? C52 C53 H53 121.1 . . ? C59 C54 C55 120.5(8) . . ? C59 C54 N5 119.6(7) . . ? C55 C54 N5 119.9(8) . . ? C54 C55 C56 118.2(9) . . ? C54 C55 H55 120.9 . . ? C56 C55 H55 120.9 . . ? C57 C56 C55 122.8(8) . . ? C57 C56 H56 118.6 . . ? C55 C56 H56 118.6 . . ? C56 C57 C58 117.6(9) . . ? C56 C57 C60 121.8(9) . . ? C58 C57 C60 120.6(9) . . ? C59 C58 C57 121.2(9) . . ? C59 C58 H58 119.4 . . ? C57 C58 H58 119.4 . . ? C54 C59 C58 119.7(8) . . ? C54 C59 H59 120.1 . . ? C58 C59 H59 120.1 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C12 H12 Cl2 0.93 2.64 3.336(9) 132.0 . C22 H22 O4 0.93 2.44 3.053(10) 123.2 1_655 C48 H48 O3 0.93 2.38 3.224(10) 151.2 . C53 H53 O2 0.93 2.53 3.318(10) 142.2 1_565 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.038 _refine_diff_density_min -1.144 _refine_diff_density_rms 0.159 _database_code_depnum_ccdc_archive 'CCDC 973295' data_added_by_encifer _publ_section_references ;CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET) Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. Flack. H. D. (1983). Acta Cryst. A39, 876--881. Sheldrick, G. M. (1990a). Acta Cryst. A46, 467--473. Sheldrick, G. M. (1990b). SHELXTL/PC Software. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany Spek, A. L. (1990). Acta Cryst. A46, C-34. UNIL IC & KUMA (2000). CrysAlis CCD. Version 1.163. Kuma Diffraction Instruments GmbH, Wroc\/law, Poland. UNIL IC & KUMA (2000). CrysAlis RED. Version 1.163. Kuma Diffraction Instruments GmbH, Wroc\/law, Poland. ; data_re173 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H25 Br2 N3 O2 P Re' _chemical_formula_sum 'C30 H25 Br2 N3 O2 P Re' _chemical_formula_weight 836.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' O O 0.0106 0.0060 '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 10.3301(10) _cell_length_b 11.3982(10) _cell_length_c 13.2930(10) _cell_angle_alpha 92.707(6) _cell_angle_beta 104.825(8) _cell_angle_gamma 104.41 _cell_volume 1455.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7015 _cell_measurement_theta_min 3.4924 _cell_measurement_theta_max 29.3175 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.15271 _exptl_crystal_size_mid 0.10183 _exptl_crystal_size_min 0.08524 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.909 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 804 _exptl_absorpt_coefficient_mu 7.009 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ;CrysAlis RED, (2005) ; _exptl_absorpt_correction_T_min 0.34107 _exptl_absorpt_correction_T_max 1.00000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _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 9640 _diffrn_reflns_av_R_equivalents 0.0396 _diffrn_reflns_av_unetI/netI 0.0522 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.50 _diffrn_reflns_theta_max 25.05 _reflns_number_total 5134 _reflns_number_gt 4148 _reflns_threshold_expression >2sigma(I) #========================================================================== # # REFINEMENT DATA _computing_data_collection 'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)' _computing_cell_refinement 'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)' _computing_data_reduction 'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;XP in SHELXTL/PC (Sheldrick, 1990b) ORTEP-3 W v. 1.062 (Farrugia 1997) ; _computing_publication_material ;SHELXL-97 (Sheldrick, 1997) and PLATON (Spek, 1990) ; _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^)+(0.1102P)^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 5134 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1590 _refine_ls_wR_factor_gt 0.1541 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.22130(4) 0.20188(3) 0.21825(3) 0.03028(17) Uani 1 1 d . . . N2 N 0.0200(8) 0.2083(7) 0.1387(6) 0.0325(18) Uani 1 1 d . . . N1 N 0.1771(8) 0.0537(7) 0.2450(5) 0.0323(18) Uani 1 1 d . . . N3 N -0.2345(10) 0.2382(9) 0.0213(7) 0.050(2) Uani 1 1 d . . . O1 O 0.2426(7) 0.3788(6) 0.1925(5) 0.0424(17) Uani 1 1 d . . . O2 O 0.1395(10) 0.5207(7) 0.1327(7) 0.071(3) Uani 1 1 d . . . Br1 Br 0.25151(15) 0.17478(12) 0.03819(9) 0.0604(4) Uani 1 1 d . . . Br2 Br 0.17950(15) 0.27818(12) 0.38692(10) 0.0648(4) Uani 1 1 d . . . P1 P 0.4716(3) 0.2477(2) 0.29192(17) 0.0294(5) Uani 1 1 d . . . C1 C 0.5338(10) 0.2657(9) 0.4351(7) 0.034(2) Uani 1 1 d . . . C2 C 0.4820(12) 0.1687(10) 0.4832(8) 0.048(3) Uani 1 1 d . . . H2 H 0.4142 0.1015 0.4432 0.058 Uiso 1 1 calc R . . C3 C 0.5279(14) 0.1686(12) 0.5890(8) 0.057(3) Uani 1 1 d . . . H3 H 0.4924 0.1014 0.6205 0.068 Uiso 1 1 calc R . . C4 C 0.6260(13) 0.2677(13) 0.6484(8) 0.057(3) Uani 1 1 d . . . H4 H 0.6586 0.2677 0.7205 0.069 Uiso 1 1 calc R . . C5 C 0.6758(12) 0.3657(11) 0.6026(8) 0.052(3) Uani 1 1 d . . . H5 H 0.7390 0.4343 0.6443 0.062 Uiso 1 1 calc R . . C6 C 0.6355(12) 0.3665(9) 0.4954(8) 0.047(3) Uani 1 1 d . . . H6 H 0.6748 0.4324 0.4642 0.056 Uiso 1 1 calc R . . C7 C 0.5550(11) 0.1317(8) 0.2596(7) 0.035(2) Uani 1 1 d . . . C8 C 0.4821(11) 0.0259(8) 0.1946(7) 0.035(2) Uani 1 1 d . . . H8 H 0.3884 0.0135 0.1605 0.042 Uiso 1 1 calc R . . C9 C 0.5482(12) -0.0619(9) 0.1800(8) 0.044(3) Uani 1 1 d . . . H9 H 0.4978 -0.1330 0.1355 0.052 Uiso 1 1 calc R . . C10 C 0.6796(12) -0.0484(9) 0.2268(8) 0.047(3) Uani 1 1 d . . . H10 H 0.7218 -0.1091 0.2154 0.057 Uiso 1 1 calc R . . C11 C 0.7571(13) 0.0591(11) 0.2950(9) 0.055(3) Uani 1 1 d . . . H11 H 0.8501 0.0693 0.3300 0.066 Uiso 1 1 calc R . . C12 C 0.6933(11) 0.1474(10) 0.3084(8) 0.045(3) Uani 1 1 d . . . H12 H 0.7443 0.2195 0.3514 0.054 Uiso 1 1 calc R . . C13 C 0.5513(10) 0.3845(8) 0.2435(7) 0.033(2) Uani 1 1 d . . . C14 C 0.5452(12) 0.4988(9) 0.2858(9) 0.047(3) Uani 1 1 d . . . H14 H 0.5117 0.5051 0.3438 0.056 Uiso 1 1 calc R . . C15 C 0.5907(14) 0.6014(10) 0.2381(11) 0.064(4) Uani 1 1 d . . . H15 H 0.5902 0.6775 0.2663 0.077 Uiso 1 1 calc R . . C16 C 0.6359(13) 0.5927(11) 0.1508(10) 0.063(3) Uani 1 1 d . . . H16 H 0.6668 0.6625 0.1206 0.076 Uiso 1 1 calc R . . C17 C 0.6357(13) 0.4798(12) 0.1073(10) 0.058(3) Uani 1 1 d . . . H17 H 0.6636 0.4731 0.0465 0.069 Uiso 1 1 calc R . . C18 C 0.5939(11) 0.3772(10) 0.1547(8) 0.044(3) Uani 1 1 d . . . H18 H 0.5948 0.3017 0.1256 0.053 Uiso 1 1 calc R . . C19 C 0.1357(12) 0.4168(9) 0.1456(8) 0.046(3) Uani 1 1 d . . . C20 C 0.0043(11) 0.3174(9) 0.1110(8) 0.039(2) Uani 1 1 d . . . C21 C -0.1198(12) 0.3312(10) 0.0537(9) 0.051(3) Uani 1 1 d . . . H21 H -0.1247 0.4084 0.0366 0.062 Uiso 1 1 calc R . . C22 C -0.2193(12) 0.1303(11) 0.0495(8) 0.048(3) Uani 1 1 d . . . H22 H -0.2968 0.0632 0.0277 0.058 Uiso 1 1 calc R . . C23 C -0.0990(11) 0.1117(9) 0.1076(8) 0.040(2) Uani 1 1 d . . . H23 H -0.0964 0.0346 0.1264 0.048 Uiso 1 1 calc R . . C24 C 0.1185(10) -0.0588(8) 0.2727(7) 0.034(2) Uani 1 1 d . . . C25 C 0.0735(12) -0.1605(9) 0.2007(9) 0.045(3) Uani 1 1 d . . . H25 H 0.0802 -0.1554 0.1325 0.054 Uiso 1 1 calc R . . C26 C 0.0175(13) -0.2718(9) 0.2329(9) 0.052(3) Uani 1 1 d . . . H26 H -0.0120 -0.3417 0.1850 0.062 Uiso 1 1 calc R . . C27 C 0.0041(11) -0.2823(9) 0.3328(10) 0.052(3) Uani 1 1 d . . . C28 C 0.0469(14) -0.1744(12) 0.4040(9) 0.061(3) Uani 1 1 d . . . H28 H 0.0348 -0.1790 0.4708 0.073 Uiso 1 1 calc R . . C29 C 0.1050(13) -0.0652(10) 0.3770(8) 0.051(3) Uani 1 1 d . . . H29 H 0.1357 0.0045 0.4251 0.062 Uiso 1 1 calc R . . C30 C -0.0575(14) -0.4024(11) 0.3692(11) 0.075(4) Uani 1 1 d . . . H30A H -0.1170 -0.3903 0.4113 0.112 Uiso 1 1 calc R . . H30B H 0.0161 -0.4322 0.4100 0.112 Uiso 1 1 calc R . . H30C H -0.1106 -0.4608 0.3094 0.112 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 0.0326(3) 0.0211(2) 0.0349(3) 0.00245(14) 0.00947(17) 0.00320(15) N2 0.028(5) 0.026(4) 0.040(4) -0.002(3) 0.006(3) 0.007(3) N1 0.044(5) 0.025(4) 0.028(4) 0.008(3) 0.012(3) 0.006(3) N3 0.044(6) 0.054(6) 0.052(5) 0.007(4) 0.011(4) 0.018(5) O1 0.037(4) 0.026(3) 0.057(4) 0.007(3) 0.006(3) 0.003(3) O2 0.080(7) 0.033(5) 0.083(6) 0.013(4) -0.004(5) 0.012(4) Br1 0.0699(9) 0.0570(7) 0.0512(7) 0.0038(5) 0.0169(6) 0.0118(6) Br2 0.0718(9) 0.0629(8) 0.0617(8) -0.0040(6) 0.0250(6) 0.0175(7) P1 0.0356(15) 0.0210(11) 0.0308(12) 0.0022(9) 0.0110(10) 0.0044(10) C1 0.037(6) 0.035(5) 0.031(5) 0.001(4) 0.011(4) 0.009(4) C2 0.052(7) 0.048(6) 0.040(6) 0.013(5) 0.012(5) 0.004(5) C3 0.068(9) 0.065(8) 0.044(7) 0.017(6) 0.021(6) 0.022(7) C4 0.060(9) 0.086(10) 0.034(6) 0.007(6) 0.007(5) 0.041(7) C5 0.044(7) 0.063(8) 0.034(6) -0.017(5) -0.004(5) 0.009(6) C6 0.043(7) 0.032(5) 0.052(7) -0.005(4) 0.007(5) -0.006(5) C7 0.041(6) 0.033(5) 0.034(5) 0.007(4) 0.013(4) 0.009(4) C8 0.040(6) 0.024(5) 0.041(5) 0.007(4) 0.012(4) 0.006(4) C9 0.048(7) 0.029(5) 0.048(6) -0.001(4) 0.007(5) 0.008(5) C10 0.057(8) 0.038(6) 0.055(6) 0.008(5) 0.023(6) 0.021(5) C11 0.043(7) 0.060(8) 0.060(7) -0.005(6) 0.008(5) 0.018(6) C12 0.030(6) 0.048(6) 0.051(6) -0.007(5) 0.000(5) 0.014(5) C13 0.028(5) 0.027(5) 0.047(6) 0.013(4) 0.014(4) 0.008(4) C14 0.042(7) 0.028(5) 0.076(7) 0.009(5) 0.029(5) 0.005(4) C15 0.064(9) 0.026(6) 0.114(11) 0.011(6) 0.045(8) 0.013(5) C16 0.058(8) 0.054(8) 0.086(9) 0.035(7) 0.036(7) 0.008(6) C17 0.053(8) 0.066(8) 0.064(7) 0.028(6) 0.030(6) 0.017(6) C18 0.046(7) 0.043(6) 0.051(6) 0.010(5) 0.022(5) 0.015(5) C19 0.045(7) 0.031(6) 0.055(6) 0.006(5) 0.001(5) 0.009(5) C20 0.038(6) 0.028(5) 0.051(6) 0.001(4) 0.012(5) 0.010(4) C21 0.049(8) 0.040(6) 0.066(7) 0.012(5) 0.013(6) 0.017(5) C22 0.037(7) 0.055(7) 0.048(6) 0.001(5) 0.012(5) 0.004(5) C23 0.038(6) 0.032(5) 0.057(6) 0.010(4) 0.019(5) 0.013(4) C24 0.031(6) 0.026(5) 0.040(5) 0.012(4) 0.007(4) 0.002(4) C25 0.045(7) 0.034(5) 0.051(6) 0.000(4) 0.017(5) 0.001(5) C26 0.063(8) 0.026(5) 0.063(7) -0.001(5) 0.023(6) 0.000(5) C27 0.036(6) 0.032(6) 0.077(8) 0.024(5) 0.006(6) -0.004(5) C28 0.069(9) 0.064(8) 0.044(6) 0.025(6) 0.019(6) 0.002(6) C29 0.063(8) 0.038(6) 0.045(6) 0.002(5) 0.021(5) -0.007(5) C30 0.062(9) 0.043(7) 0.101(10) 0.034(7) 0.008(8) -0.010(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 N1 1.716(7) . ? Re1 O1 2.028(6) . ? Re1 N2 2.099(8) . ? Re1 P1 2.429(3) . ? Re1 Br1 2.5064(13) . ? Re1 Br2 2.5433(13) . ? N2 C20 1.349(12) . ? N2 C23 1.385(13) . ? N1 C24 1.385(11) . ? N3 C21 1.336(15) . ? N3 C22 1.337(14) . ? O1 C19 1.306(12) . ? O2 C19 1.198(12) . ? P1 C13 1.803(9) . ? P1 C1 1.830(9) . ? P1 C7 1.838(10) . ? C1 C2 1.366(14) . ? C1 C6 1.395(13) . ? C2 C3 1.364(15) . ? C3 C4 1.365(18) . ? C4 C5 1.350(18) . ? C5 C6 1.380(15) . ? C7 C12 1.372(14) . ? C7 C8 1.373(12) . ? C8 C9 1.376(14) . ? C9 C10 1.307(15) . ? C10 C11 1.414(15) . ? C11 C12 1.360(15) . ? C13 C18 1.368(14) . ? C13 C14 1.417(13) . ? C14 C15 1.392(16) . ? C15 C16 1.366(18) . ? C16 C17 1.386(18) . ? C17 C18 1.381(15) . ? C19 C20 1.485(14) . ? C20 C21 1.364(15) . ? C22 C23 1.358(14) . ? C24 C25 1.369(13) . ? C24 C29 1.432(14) . ? C25 C26 1.392(15) . ? C26 C27 1.379(17) . ? C27 C28 1.417(17) . ? C27 C30 1.516(14) . ? C28 C29 1.349(15) . ? 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 N1 Re1 O1 170.1(3) . . ? N1 Re1 N2 97.0(3) . . ? O1 Re1 N2 75.4(3) . . ? N1 Re1 P1 98.5(3) . . ? O1 Re1 P1 89.4(2) . . ? N2 Re1 P1 164.3(2) . . ? N1 Re1 Br1 101.7(2) . . ? O1 Re1 Br1 84.2(2) . . ? N2 Re1 Br1 84.6(2) . . ? P1 Re1 Br1 89.64(6) . . ? N1 Re1 Br2 91.2(2) . . ? O1 Re1 Br2 82.3(2) . . ? N2 Re1 Br2 88.3(2) . . ? P1 Re1 Br2 94.08(6) . . ? Br1 Re1 Br2 165.93(5) . . ? C20 N2 C23 115.7(8) . . ? C20 N2 Re1 117.0(6) . . ? C23 N2 Re1 127.2(6) . . ? C24 N1 Re1 167.7(7) . . ? C21 N3 C22 115.2(9) . . ? C19 O1 Re1 121.3(6) . . ? C13 P1 C1 109.4(4) . . ? C13 P1 C7 106.0(5) . . ? C1 P1 C7 100.1(4) . . ? C13 P1 Re1 108.2(3) . . ? C1 P1 Re1 115.9(3) . . ? C7 P1 Re1 116.5(3) . . ? C2 C1 C6 119.3(9) . . ? C2 C1 P1 116.1(8) . . ? C6 C1 P1 124.4(8) . . ? C3 C2 C1 121.2(11) . . ? C2 C3 C4 119.7(12) . . ? C5 C4 C3 120.0(10) . . ? C4 C5 C6 121.7(10) . . ? C5 C6 C1 118.1(10) . . ? C12 C7 C8 118.7(9) . . ? C12 C7 P1 118.5(7) . . ? C8 C7 P1 122.6(8) . . ? C7 C8 C9 119.8(10) . . ? C10 C9 C8 122.0(10) . . ? C9 C10 C11 119.5(10) . . ? C12 C11 C10 118.9(11) . . ? C11 C12 C7 121.0(10) . . ? C18 C13 C14 119.4(9) . . ? C18 C13 P1 120.4(7) . . ? C14 C13 P1 119.2(8) . . ? C15 C14 C13 118.3(11) . . ? C16 C15 C14 121.4(11) . . ? C15 C16 C17 119.9(11) . . ? C18 C17 C16 119.6(11) . . ? C13 C18 C17 121.3(11) . . ? O2 C19 O1 124.9(10) . . ? O2 C19 C20 122.1(10) . . ? O1 C19 C20 113.1(8) . . ? N2 C20 C21 122.2(9) . . ? N2 C20 C19 113.0(9) . . ? C21 C20 C19 124.7(9) . . ? N3 C21 C20 122.6(10) . . ? N3 C22 C23 124.7(10) . . ? C22 C23 N2 119.6(9) . . ? C25 C24 N1 120.1(9) . . ? C25 C24 C29 121.4(9) . . ? N1 C24 C29 118.5(8) . . ? C24 C25 C26 117.9(10) . . ? C27 C26 C25 122.6(10) . . ? C26 C27 C28 117.9(9) . . ? C26 C27 C30 123.4(11) . . ? C28 C27 C30 118.6(11) . . ? C29 C28 C27 121.4(11) . . ? C28 C29 C24 118.7(10) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 3.346 _refine_diff_density_min -2.388 _refine_diff_density_rms 0.220 _database_code_depnum_ccdc_archive 'CCDC 973296' data_added_by_encifer _publ_section_references ;CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET) Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. Flack. H. D. (1983). Acta Cryst. A39, 876--881. Sheldrick, G. M. (1990a). Acta Cryst. A46, 467--473. Sheldrick, G. M. (1990b). SHELXTL/PC Software. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany Spek, A. L. (1990). Acta Cryst. A46, C-34. UNIL IC & KUMA (2000). CrysAlis CCD. Version 1.163. Kuma Diffraction Instruments GmbH, Wroc\/law, Poland. UNIL IC & KUMA (2000). CrysAlis RED. Version 1.163. Kuma Diffraction Instruments GmbH, Wroc\/law, Poland. ; data_ren228 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H27 Cl2 N3 O2 P Re, 2(C H4 O)' _chemical_formula_sum 'C35 H35 Cl2 N3 O4 P Re' _chemical_formula_weight 849.73 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' Cl Cl 0.1484 0.1585 '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 8.2043(16) _cell_length_b 11.196(2) _cell_length_c 18.785(4) _cell_angle_alpha 84.91(3) _cell_angle_beta 84.90(3) _cell_angle_gamma 85.40(3) _cell_volume 1707.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8968 _cell_measurement_theta_min 3.4793 _cell_measurement_theta_max 29.2182 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.83585 _exptl_crystal_size_mid 0.50223 _exptl_crystal_size_min 0.38390 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 3.805 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ;CrysAlis RED, (2005) ; _exptl_absorpt_correction_T_min 0.39224 _exptl_absorpt_correction_T_max 1.00000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _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 15941 _diffrn_reflns_av_R_equivalents 0.0525 _diffrn_reflns_av_unetI/netI 0.0563 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6001 _reflns_number_gt 5345 _reflns_threshold_expression >2sigma(I) #========================================================================== # # REFINEMENT DATA _computing_data_collection 'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)' _computing_cell_refinement 'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)' _computing_data_reduction 'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;XP in SHELXTL/PC (Sheldrick, 1990b) ORTEP-3 W v. 1.062 (Farrugia 1997) ; _computing_publication_material ;SHELXL-97 (Sheldrick, 1997) and PLATON (Spek, 1990) ; _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^)+(0.0310P)^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 6001 _refine_ls_number_parameters 420 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0650 _refine_ls_wR_factor_gt 0.0626 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 0.816198(18) 0.668862(15) 0.743677(8) 0.02963(7) Uani 1 1 d . . . N1 N 0.9491(4) 0.6317(3) 0.83465(16) 0.0299(8) Uani 1 1 d . . . N2 N 0.9643(4) 0.6007(3) 0.68814(16) 0.0340(8) Uani 1 1 d . . . N3 N 1.0956(4) 0.5708(3) 0.84592(17) 0.0341(8) Uani 1 1 d . . . H3A H 1.1550 0.5302 0.8151 0.041 Uiso 1 1 calc R . . O1 O 0.6616(4) 0.8003(3) 0.93956(15) 0.0533(9) Uani 1 1 d . . . O2 O 0.6865(3) 0.7596(3) 0.82500(14) 0.0342(7) Uani 1 1 d . . . P1 P 0.92710(12) 0.86506(10) 0.71834(5) 0.0280(2) Uani 1 1 d . . . Cl1 Cl 0.61045(13) 0.72560(11) 0.66383(6) 0.0458(3) Uani 1 1 d . . . Cl2 Cl 0.66119(15) 0.50022(12) 0.78513(7) 0.0536(3) Uani 1 1 d . . . C1 C 0.7831(5) 0.9974(4) 0.70974(19) 0.0300(9) Uani 1 1 d . . . C2 C 0.8456(5) 1.1089(4) 0.6897(2) 0.0409(11) Uani 1 1 d . . . H2 H 0.9573 1.1128 0.6769 0.049 Uiso 1 1 calc R . . C3 C 0.7445(7) 1.2132(5) 0.6887(3) 0.0543(13) Uani 1 1 d . . . H3 H 0.7877 1.2870 0.6753 0.065 Uiso 1 1 calc R . . C4 C 0.5786(6) 1.2077(5) 0.7076(3) 0.0551(13) Uani 1 1 d . . . H4 H 0.5099 1.2779 0.7074 0.066 Uiso 1 1 calc R . . C5 C 0.5155(6) 1.0990(5) 0.7265(3) 0.0529(13) Uani 1 1 d . . . H5 H 0.4036 1.0956 0.7389 0.063 Uiso 1 1 calc R . . C6 C 0.6171(5) 0.9936(4) 0.7275(2) 0.0409(11) Uani 1 1 d . . . H6 H 0.5727 0.9200 0.7402 0.049 Uiso 1 1 calc R . . C7 C 1.0456(5) 0.8995(4) 0.7905(2) 0.0316(9) Uani 1 1 d . . . C8 C 1.2010(5) 0.8423(4) 0.7990(2) 0.0422(11) Uani 1 1 d . . . H8 H 1.2493 0.7910 0.7655 0.051 Uiso 1 1 calc R . . C9 C 1.2827(6) 0.8624(5) 0.8576(3) 0.0573(15) Uani 1 1 d . . . H9 H 1.3868 0.8252 0.8632 0.069 Uiso 1 1 calc R . . C10 C 1.2108(7) 0.9374(5) 0.9078(3) 0.0627(16) Uani 1 1 d . . . H10 H 1.2667 0.9505 0.9470 0.075 Uiso 1 1 calc R . . C11 C 1.0586(7) 0.9922(5) 0.9002(2) 0.0546(13) Uani 1 1 d . . . H11 H 1.0102 1.0419 0.9345 0.065 Uiso 1 1 calc R . . C12 C 0.9759(5) 0.9742(4) 0.8416(2) 0.0386(10) Uani 1 1 d . . . H12 H 0.8723 1.0126 0.8365 0.046 Uiso 1 1 calc R . . C13 C 1.0598(5) 0.8788(4) 0.6355(2) 0.0323(9) Uani 1 1 d . . . C14 C 1.0066(6) 0.8373(4) 0.5750(2) 0.0445(11) Uani 1 1 d . . . H14 H 0.9099 0.7984 0.5784 0.053 Uiso 1 1 calc R . . C15 C 1.0966(7) 0.8533(5) 0.5093(2) 0.0570(14) Uani 1 1 d . . . H15 H 1.0590 0.8263 0.4687 0.068 Uiso 1 1 calc R . . C16 C 1.2404(6) 0.9086(5) 0.5039(3) 0.0599(15) Uani 1 1 d . . . H16 H 1.3004 0.9193 0.4597 0.072 Uiso 1 1 calc R . . C17 C 1.2957(6) 0.9481(6) 0.5631(3) 0.0695(17) Uani 1 1 d . . . H17 H 1.3938 0.9852 0.5593 0.083 Uiso 1 1 calc R . . C18 C 1.2061(5) 0.9333(5) 0.6296(2) 0.0548(14) Uani 1 1 d . . . H18 H 1.2450 0.9601 0.6699 0.066 Uiso 1 1 calc R . . C19 C 0.7356(5) 0.7525(4) 0.8896(2) 0.0354(10) Uani 1 1 d . . . C20 C 0.8945(4) 0.6821(4) 0.8944(2) 0.0291(9) Uani 1 1 d . . . C21 C 1.0081(5) 0.6553(4) 0.9468(2) 0.0329(9) Uani 1 1 d . . . C22 C 1.0168(5) 0.6846(4) 1.0182(2) 0.0403(11) Uani 1 1 d . . . H22 H 0.9346 0.7328 1.0413 0.048 Uiso 1 1 calc R . . C23 C 1.1523(6) 0.6383(5) 1.0515(2) 0.0492(12) Uani 1 1 d . . . H23 H 1.1618 0.6553 1.0984 0.059 Uiso 1 1 calc R . . C24 C 1.2771(6) 0.5662(5) 1.0174(3) 0.0541(14) Uani 1 1 d . . . H24 H 1.3667 0.5371 1.0425 0.065 Uiso 1 1 calc R . . C25 C 1.2727(5) 0.5369(5) 0.9487(3) 0.0473(12) Uani 1 1 d . . . H25 H 1.3561 0.4889 0.9263 0.057 Uiso 1 1 calc R . . C26 C 1.1335(5) 0.5842(4) 0.9140(2) 0.0343(10) Uani 1 1 d . . . C27 C 1.0891(5) 0.5398(4) 0.6482(2) 0.0328(9) Uani 1 1 d . . . C28 C 1.2523(5) 0.5479(4) 0.6585(2) 0.0399(10) Uani 1 1 d . . . H28 H 1.2826 0.5988 0.6908 0.048 Uiso 1 1 calc R . . C29 C 1.3695(6) 0.4788(4) 0.6198(2) 0.0465(12) Uani 1 1 d . . . H29 H 1.4795 0.4830 0.6271 0.056 Uiso 1 1 calc R . . C30 C 1.3290(6) 0.4039(4) 0.5707(2) 0.0498(12) Uani 1 1 d . . . C31 C 1.1658(7) 0.4010(5) 0.5602(2) 0.0559(13) Uani 1 1 d . . . H31 H 1.1364 0.3522 0.5266 0.067 Uiso 1 1 calc R . . C32 C 1.0449(6) 0.4673(4) 0.5974(2) 0.0470(12) Uani 1 1 d . . . H32 H 0.9354 0.4641 0.5890 0.056 Uiso 1 1 calc R . . C33 C 1.4597(8) 0.3261(6) 0.5311(3) 0.0787(19) Uani 1 1 d . . . H33C H 1.5658 0.3527 0.5368 0.118 Uiso 1 1 calc R . . H33B H 1.4414 0.3321 0.4811 0.118 Uiso 1 1 calc R . . H33A H 1.4548 0.2439 0.5503 0.118 Uiso 1 1 calc R . . O98 O 1.2337(4) 0.3543(3) 0.80292(18) 0.0559(9) Uani 1 1 d . . . H98 H 1.2963 0.3807 0.7699 0.084 Uiso 1 1 calc R . . O99 O 0.6058(5) 0.7714(4) 1.08777(18) 0.0771(12) Uani 1 1 d . . . H99 H 0.6390 0.7696 1.0454 0.116 Uiso 1 1 calc R . . C98 C 1.1264(7) 0.2809(5) 0.7764(3) 0.0630(15) Uani 1 1 d . . . H98A H 1.1167 0.2090 0.8080 0.094 Uiso 1 1 calc R . . H98B H 1.1686 0.2600 0.7295 0.094 Uiso 1 1 calc R . . H98C H 1.0204 0.3234 0.7737 0.094 Uiso 1 1 calc R . . C99 C 0.4560(6) 0.8383(6) 1.0935(3) 0.0729(17) Uani 1 1 d . . . H99A H 0.3985 0.8170 1.1390 0.109 Uiso 1 1 calc R . . H99B H 0.3917 0.8218 1.0557 0.109 Uiso 1 1 calc R . . H99C H 0.4741 0.9224 1.0896 0.109 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 0.02725(10) 0.03129(11) 0.03068(10) -0.00436(7) -0.00401(7) -0.00041(7) N1 0.0263(17) 0.030(2) 0.0326(17) -0.0004(15) -0.0068(14) 0.0050(15) N2 0.0403(19) 0.035(2) 0.0271(17) -0.0034(15) -0.0039(15) 0.0008(16) N3 0.0291(18) 0.036(2) 0.0360(18) -0.0072(16) -0.0016(15) 0.0079(16) O1 0.0471(18) 0.078(3) 0.0312(16) -0.0118(16) 0.0015(14) 0.0239(18) O2 0.0269(14) 0.0416(18) 0.0330(15) -0.0015(13) -0.0058(12) 0.0062(13) P1 0.0251(5) 0.0314(6) 0.0275(5) -0.0041(4) -0.0015(4) -0.0005(4) Cl1 0.0420(6) 0.0513(7) 0.0471(6) -0.0050(5) -0.0199(5) -0.0030(5) Cl2 0.0569(7) 0.0473(7) 0.0588(7) 0.0058(6) -0.0106(6) -0.0212(6) C1 0.036(2) 0.030(2) 0.0253(19) -0.0062(17) -0.0060(17) 0.0039(18) C2 0.044(3) 0.039(3) 0.038(2) 0.001(2) 0.000(2) -0.001(2) C3 0.073(4) 0.036(3) 0.052(3) 0.004(2) -0.004(3) 0.002(3) C4 0.064(3) 0.046(3) 0.053(3) -0.004(2) -0.011(3) 0.023(3) C5 0.037(3) 0.051(3) 0.067(3) -0.003(3) -0.002(2) 0.015(2) C6 0.035(2) 0.035(3) 0.054(3) -0.013(2) -0.005(2) 0.001(2) C7 0.033(2) 0.033(2) 0.030(2) -0.0041(18) -0.0032(17) -0.0081(19) C8 0.027(2) 0.052(3) 0.046(3) 0.002(2) -0.002(2) -0.004(2) C9 0.035(3) 0.075(4) 0.063(3) 0.018(3) -0.017(2) -0.019(3) C10 0.081(4) 0.069(4) 0.044(3) 0.009(3) -0.028(3) -0.034(3) C11 0.080(4) 0.049(3) 0.037(2) -0.007(2) -0.010(3) -0.008(3) C12 0.047(3) 0.036(3) 0.034(2) -0.001(2) -0.010(2) -0.003(2) C13 0.032(2) 0.029(2) 0.033(2) -0.0015(18) 0.0044(18) 0.0054(18) C14 0.050(3) 0.048(3) 0.035(2) -0.002(2) 0.002(2) -0.005(2) C15 0.076(4) 0.060(4) 0.033(2) -0.004(2) 0.007(2) -0.003(3) C16 0.056(3) 0.072(4) 0.043(3) 0.001(3) 0.021(3) 0.011(3) C17 0.045(3) 0.101(5) 0.059(3) 0.004(3) 0.017(3) -0.015(3) C18 0.044(3) 0.081(4) 0.040(3) -0.004(3) 0.004(2) -0.017(3) C19 0.030(2) 0.039(3) 0.036(2) 0.000(2) -0.0013(19) 0.0035(19) C20 0.027(2) 0.031(2) 0.029(2) -0.0013(17) -0.0023(17) -0.0007(18) C21 0.031(2) 0.033(2) 0.035(2) 0.0007(19) -0.0041(18) -0.0039(19) C22 0.040(2) 0.045(3) 0.038(2) -0.006(2) -0.006(2) -0.007(2) C23 0.046(3) 0.063(4) 0.042(3) -0.005(2) -0.017(2) -0.013(3) C24 0.034(3) 0.078(4) 0.052(3) 0.001(3) -0.021(2) 0.001(3) C25 0.034(2) 0.052(3) 0.056(3) -0.007(2) -0.009(2) 0.003(2) C26 0.030(2) 0.035(3) 0.038(2) 0.0015(19) -0.0059(18) -0.0019(19) C27 0.038(2) 0.027(2) 0.032(2) -0.0042(18) 0.0032(18) 0.0027(19) C28 0.044(3) 0.038(3) 0.040(2) -0.015(2) -0.004(2) 0.001(2) C29 0.039(3) 0.050(3) 0.048(3) -0.002(2) 0.000(2) 0.007(2) C30 0.064(3) 0.044(3) 0.037(2) -0.004(2) 0.005(2) 0.014(3) C31 0.081(4) 0.048(3) 0.040(3) -0.019(2) -0.007(3) 0.005(3) C32 0.058(3) 0.043(3) 0.043(2) -0.014(2) -0.012(2) 0.000(2) C33 0.102(5) 0.073(4) 0.054(3) -0.014(3) 0.007(3) 0.035(4) O98 0.061(2) 0.049(2) 0.056(2) -0.0062(18) -0.0036(17) 0.0077(18) O99 0.078(3) 0.103(3) 0.0438(19) -0.002(2) -0.0075(19) 0.032(2) C98 0.069(4) 0.052(4) 0.066(3) -0.001(3) -0.003(3) -0.001(3) C99 0.063(4) 0.098(5) 0.057(3) -0.014(3) -0.003(3) 0.000(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 Re1 N2 1.707(3) . ? Re1 O2 2.076(3) . ? Re1 N1 2.101(3) . ? Re1 Cl1 2.3688(12) . ? Re1 Cl2 2.3952(14) . ? Re1 P1 2.4367(13) . ? N1 C20 1.328(5) . ? N1 N3 1.357(4) . ? N2 C27 1.385(5) . ? N3 C26 1.366(5) . ? N3 H3A 0.8600 . ? O1 C19 1.212(5) . ? O2 C19 1.307(5) . ? P1 C13 1.820(4) . ? P1 C7 1.821(4) . ? P1 C1 1.824(4) . ? C1 C6 1.376(6) . ? C1 C2 1.396(6) . ? C2 C3 1.377(6) . ? C2 H2 0.9300 . ? C3 C4 1.380(7) . ? C3 H3 0.9300 . ? C4 C5 1.366(7) . ? C4 H4 0.9300 . ? C5 C6 1.389(6) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.385(6) . ? C7 C8 1.396(6) . ? C8 C9 1.382(6) . ? C8 H8 0.9300 . ? C9 C10 1.379(8) . ? C9 H9 0.9300 . ? C10 C11 1.360(7) . ? C10 H10 0.9300 . ? C11 C12 1.381(6) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C18 1.381(6) . ? C13 C14 1.384(6) . ? C14 C15 1.385(6) . ? C14 H14 0.9300 . ? C15 C16 1.368(7) . ? C15 H15 0.9300 . ? C16 C17 1.359(8) . ? C16 H16 0.9300 . ? C17 C18 1.395(6) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.473(5) . ? C20 C21 1.411(5) . ? C21 C26 1.384(6) . ? C21 C22 1.419(6) . ? C22 C23 1.367(6) . ? C22 H22 0.9300 . ? C23 C24 1.397(7) . ? C23 H23 0.9300 . ? C24 C25 1.362(7) . ? C24 H24 0.9300 . ? C25 C26 1.408(6) . ? C25 H25 0.9300 . ? C27 C28 1.381(6) . ? C27 C32 1.395(6) . ? C28 C29 1.382(6) . ? C28 H28 0.9300 . ? C29 C30 1.378(7) . ? C29 H29 0.9300 . ? C30 C31 1.374(7) . ? C30 C33 1.512(7) . ? C31 C32 1.369(6) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 H33C 0.9600 . ? C33 H33B 0.9600 . ? C33 H33A 0.9600 . ? O98 C98 1.401(6) . ? O98 H98 0.8200 . ? O99 C99 1.388(6) . ? O99 H99 0.8200 . ? C98 H98A 0.9600 . ? C98 H98B 0.9600 . ? C98 H98C 0.9600 . ? C99 H99A 0.9600 . ? C99 H99B 0.9600 . ? C99 H99C 0.9600 . ? 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 N2 Re1 O2 165.49(13) . . ? N2 Re1 N1 93.86(14) . . ? O2 Re1 N1 73.53(11) . . ? N2 Re1 Cl1 100.96(11) . . ? O2 Re1 Cl1 92.07(8) . . ? N1 Re1 Cl1 164.93(9) . . ? N2 Re1 Cl2 99.86(12) . . ? O2 Re1 Cl2 87.10(9) . . ? N1 Re1 Cl2 88.02(10) . . ? Cl1 Re1 Cl2 86.79(5) . . ? N2 Re1 P1 93.05(12) . . ? O2 Re1 P1 80.38(9) . . ? N1 Re1 P1 91.46(10) . . ? Cl1 Re1 P1 90.46(5) . . ? Cl2 Re1 P1 167.09(4) . . ? C20 N1 N3 107.9(3) . . ? C20 N1 Re1 118.8(2) . . ? N3 N1 Re1 133.1(3) . . ? C27 N2 Re1 175.1(3) . . ? N1 N3 C26 109.1(3) . . ? N1 N3 H3A 125.4 . . ? C26 N3 H3A 125.4 . . ? C19 O2 Re1 121.6(2) . . ? C13 P1 C7 107.24(19) . . ? C13 P1 C1 103.07(18) . . ? C7 P1 C1 102.18(19) . . ? C13 P1 Re1 113.83(14) . . ? C7 P1 Re1 111.16(14) . . ? C1 P1 Re1 118.17(14) . . ? C6 C1 C2 118.5(4) . . ? C6 C1 P1 122.9(3) . . ? C2 C1 P1 118.4(3) . . ? C3 C2 C1 121.0(4) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C2 C3 C4 119.6(5) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 120.0(5) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 120.6(5) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C1 C6 C5 120.3(4) . . ? C1 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C12 C7 C8 119.0(4) . . ? C12 C7 P1 120.1(3) . . ? C8 C7 P1 120.6(3) . . ? C9 C8 C7 119.5(5) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C10 C9 C8 120.4(5) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C11 C10 C9 120.3(4) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 120.1(5) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C7 120.7(4) . . ? C11 C12 H12 119.7 . . ? C7 C12 H12 119.7 . . ? C18 C13 C14 118.7(4) . . ? C18 C13 P1 123.4(3) . . ? C14 C13 P1 117.8(3) . . ? C13 C14 C15 120.4(4) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 120.3(5) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C17 C16 C15 120.0(4) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 120.4(5) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C13 C18 C17 120.1(5) . . ? C13 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? O1 C19 O2 124.3(4) . . ? O1 C19 C20 123.7(4) . . ? O2 C19 C20 112.0(3) . . ? N1 C20 C21 110.1(3) . . ? N1 C20 C19 113.7(3) . . ? C21 C20 C19 136.2(4) . . ? C26 C21 C20 104.6(3) . . ? C26 C21 C22 120.1(4) . . ? C20 C21 C22 135.2(4) . . ? C23 C22 C21 116.6(4) . . ? C23 C22 H22 121.7 . . ? C21 C22 H22 121.7 . . ? C22 C23 C24 122.3(4) . . ? C22 C23 H23 118.8 . . ? C24 C23 H23 118.8 . . ? C25 C24 C23 122.6(4) . . ? C25 C24 H24 118.7 . . ? C23 C24 H24 118.7 . . ? C24 C25 C26 115.6(4) . . ? C24 C25 H25 122.2 . . ? C26 C25 H25 122.2 . . ? N3 C26 C21 108.3(3) . . ? N3 C26 C25 128.9(4) . . ? C21 C26 C25 122.8(4) . . ? C28 C27 N2 121.8(4) . . ? C28 C27 C32 120.4(4) . . ? N2 C27 C32 117.8(4) . . ? C27 C28 C29 118.5(4) . . ? C27 C28 H28 120.7 . . ? C29 C28 H28 120.7 . . ? C30 C29 C28 122.3(4) . . ? C30 C29 H29 118.9 . . ? C28 C29 H29 118.9 . . ? C31 C30 C29 117.6(4) . . ? C31 C30 C33 121.4(5) . . ? C29 C30 C33 121.0(5) . . ? C32 C31 C30 122.4(5) . . ? C32 C31 H31 118.8 . . ? C30 C31 H31 118.8 . . ? C31 C32 C27 118.8(4) . . ? C31 C32 H32 120.6 . . ? C27 C32 H32 120.6 . . ? C30 C33 H33C 109.5 . . ? C30 C33 H33B 109.5 . . ? H33C C33 H33B 109.5 . . ? C30 C33 H33A 109.5 . . ? H33C C33 H33A 109.5 . . ? H33B C33 H33A 109.5 . . ? C98 O98 H98 109.5 . . ? C99 O99 H99 109.5 . . ? O98 C98 H98A 109.5 . . ? O98 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? O98 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? O99 C99 H99A 109.5 . . ? O99 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? O99 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3A O98 0.86 2.05 2.748(5) 138.0 . O99 H99 O1 0.82 1.98 2.775(4) 162.9 . C6 H6 Cl1 0.93 2.69 3.333(5) 126.6 . C6 H6 O2 0.93 2.47 3.104(5) 125.1 . C9 H9 O2 0.93 2.57 3.439(6) 156.3 1_655 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.754 _refine_diff_density_min -1.025 _refine_diff_density_rms 0.108 _database_code_depnum_ccdc_archive 'CCDC 973297' data_added_by_encifer _publ_section_references ;CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET) Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. Flack. H. D. (1983). Acta Cryst. A39, 876--881. Sheldrick, G. M. (1990a). Acta Cryst. A46, 467--473. Sheldrick, G. M. (1990b). SHELXTL/PC Software. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany Spek, A. L. (1990). Acta Cryst. A46, C-34. UNIL IC & KUMA (2000). CrysAlis CCD. Version 1.163. Kuma Diffraction Instruments GmbH, Wroc\/law, Poland. UNIL IC & KUMA (2000). CrysAlis RED. Version 1.163. Kuma Diffraction Instruments GmbH, Wroc\/law, Poland. ; data_ren266 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C33 H27 Cl2 N3 O2 P Re), C2 H3 N' _chemical_formula_sum 'C68 H57 Cl4 N7 O4 P2 Re2' _chemical_formula_weight 1612.35 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' Cl Cl 0.1484 0.1585 '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.0285(4) _cell_length_b 20.8676(7) _cell_length_c 28.0720(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.662(3) _cell_angle_gamma 90.00 _cell_volume 6460.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10013 _cell_measurement_theta_min 3.4389 _cell_measurement_theta_max 29.3337 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.325 _exptl_crystal_size_mid 0.093 _exptl_crystal_size_min 0.052 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.658 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3176 _exptl_absorpt_coefficient_mu 4.013 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ;CrysAlis RED, (2005) ; _exptl_absorpt_correction_T_min 0.53128 _exptl_absorpt_correction_T_max 1.00000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _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 32105 _diffrn_reflns_av_R_equivalents 0.0521 _diffrn_reflns_av_unetI/netI 0.0587 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11339 _reflns_number_gt 9010 _reflns_threshold_expression >2sigma(I) #========================================================================== # # REFINEMENT DATA _computing_data_collection 'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)' _computing_cell_refinement 'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)' _computing_data_reduction 'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;XP in SHELXTL/PC (Sheldrick, 1990b) ORTEP-3 W v. 1.062 (Farrugia 1997) ; _computing_publication_material ;SHELXL-97 (Sheldrick, 1997) and PLATON (Spek, 1990) ; _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^)+(0.0420P)^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 11339 _refine_ls_number_parameters 784 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0893 _refine_ls_wR_factor_gt 0.0823 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.003 _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 0.283006(19) 0.730160(10) 0.463395(7) 0.02931(7) Uani 1 1 d . . . Re2 Re -0.10121(2) 0.660847(11) 0.705818(7) 0.03503(8) Uani 1 1 d . . . N2 N 0.1064(4) 0.72234(19) 0.43623(14) 0.0266(9) Uani 1 1 d . . . N1 N 0.3448(4) 0.7080(2) 0.40978(15) 0.0351(11) Uani 1 1 d . . . N3 N 0.0607(4) 0.7059(2) 0.39350(14) 0.0308(10) Uani 1 1 d . . . H3A H 0.1029 0.6964 0.3689 0.037 Uiso 1 1 calc R . . N4 N -0.0053(4) 0.7415(2) 0.68456(14) 0.0340(11) Uani 1 1 d . . . N5 N -0.1668(4) 0.6424(2) 0.65175(16) 0.0390(11) Uani 1 1 d . . . N6 N -0.0037(5) 0.7774(2) 0.64424(14) 0.0396(12) Uani 1 1 d . . . H6A H -0.0386 0.7668 0.6179 0.047 Uiso 1 1 calc R . . O1 O 0.1688(3) 0.75694(18) 0.51896(11) 0.0366(9) Uani 1 1 d . . . O2 O -0.0196(4) 0.7553(2) 0.54702(12) 0.0468(10) Uani 1 1 d . . . O3 O 0.0032(4) 0.68814(19) 0.76497(12) 0.0402(9) Uani 1 1 d . . . O4 O 0.1124(4) 0.7667(2) 0.79927(13) 0.0592(13) Uani 1 1 d . . . P1 P 0.28093(12) 0.84622(7) 0.45063(5) 0.0297(3) Uani 1 1 d . . . P2 P 0.06936(13) 0.58894(7) 0.69168(5) 0.0336(3) Uani 1 1 d . . . Cl2 Cl 0.25690(15) 0.62488(7) 0.49577(6) 0.0538(4) Uani 1 1 d . . . Cl1 Cl 0.46270(13) 0.73539(7) 0.51024(5) 0.0460(4) Uani 1 1 d . . . Cl3 Cl -0.19871(16) 0.58344(9) 0.75288(7) 0.0659(5) Uani 1 1 d . . . Cl4 Cl -0.25049(15) 0.73710(8) 0.73280(6) 0.0595(4) Uani 1 1 d . . . C1 C 0.3792(5) 0.8699(3) 0.40165(17) 0.0345(13) Uani 1 1 d . . . C2 C 0.4925(5) 0.8425(3) 0.3981(2) 0.0486(16) Uani 1 1 d . . . H2 H 0.5192 0.8129 0.4206 0.058 Uiso 1 1 calc R . . C3 C 0.5657(6) 0.8597(3) 0.3607(3) 0.0596(19) Uani 1 1 d . . . H3 H 0.6416 0.8407 0.3579 0.072 Uiso 1 1 calc R . . C4 C 0.5296(7) 0.9038(4) 0.3279(2) 0.064(2) Uani 1 1 d . . . H4 H 0.5802 0.9144 0.3028 0.077 Uiso 1 1 calc R . . C5 C 0.4207(6) 0.9318(4) 0.3317(2) 0.0605(19) Uani 1 1 d . . . H5 H 0.3965 0.9626 0.3095 0.073 Uiso 1 1 calc R . . C6 C 0.3446(6) 0.9153(3) 0.3683(2) 0.0485(16) Uani 1 1 d . . . H6 H 0.2691 0.9348 0.3706 0.058 Uiso 1 1 calc R . . C7 C 0.1291(5) 0.8727(2) 0.43536(17) 0.0306(12) Uani 1 1 d . . . C8 C 0.0567(5) 0.9025(3) 0.46924(19) 0.0407(14) Uani 1 1 d . . . H8 H 0.0900 0.9136 0.4987 0.049 Uiso 1 1 calc R . . C9 C -0.0636(5) 0.9158(3) 0.4597(2) 0.0513(16) Uani 1 1 d . . . H9 H -0.1108 0.9355 0.4827 0.062 Uiso 1 1 calc R . . C10 C -0.1139(6) 0.8999(3) 0.4163(2) 0.0511(16) Uani 1 1 d . . . H10 H -0.1950 0.9090 0.4099 0.061 Uiso 1 1 calc R . . C11 C -0.0435(5) 0.8704(3) 0.3821(2) 0.0441(15) Uani 1 1 d . . . H11 H -0.0778 0.8594 0.3528 0.053 Uiso 1 1 calc R . . C12 C 0.0766(5) 0.8572(2) 0.39122(19) 0.0337(12) Uani 1 1 d . . . H12 H 0.1233 0.8378 0.3679 0.040 Uiso 1 1 calc R . . C13 C 0.3278(5) 0.8991(3) 0.49931(19) 0.0393(14) Uani 1 1 d . . . C14 C 0.3305(5) 0.9641(3) 0.4900(2) 0.0484(16) Uani 1 1 d . . . H14 H 0.3078 0.9791 0.4601 0.058 Uiso 1 1 calc R . . C15 C 0.3669(6) 1.0073(3) 0.5251(3) 0.062(2) Uani 1 1 d . . . H15 H 0.3668 1.0511 0.5190 0.074 Uiso 1 1 calc R . . C16 C 0.4029(6) 0.9846(4) 0.5687(3) 0.070(2) Uani 1 1 d . . . H16 H 0.4310 1.0131 0.5918 0.084 Uiso 1 1 calc R . . C17 C 0.3982(7) 0.9212(4) 0.5787(2) 0.069(2) Uani 1 1 d . . . H17 H 0.4206 0.9066 0.6088 0.083 Uiso 1 1 calc R . . C18 C 0.3600(6) 0.8775(3) 0.5439(2) 0.0540(17) Uani 1 1 d . . . H18 H 0.3563 0.8340 0.5509 0.065 Uiso 1 1 calc R . . C19 C 0.0520(5) 0.7487(3) 0.51483(18) 0.0331(12) Uani 1 1 d . . . C20 C 0.0145(5) 0.7308(2) 0.46597(17) 0.0293(12) Uani 1 1 d . . . C21 C -0.0957(5) 0.7214(2) 0.44140(17) 0.0294(12) Uani 1 1 d . . . C22 C -0.2210(5) 0.7244(3) 0.4523(2) 0.0441(15) Uani 1 1 d . . . H22 H -0.2468 0.7346 0.4828 0.053 Uiso 1 1 calc R . . C23 C -0.3014(6) 0.7118(3) 0.4168(2) 0.0528(17) Uani 1 1 d . . . H23 H -0.3838 0.7135 0.4235 0.063 Uiso 1 1 calc R . . C24 C -0.2654(6) 0.6964(3) 0.3701(2) 0.0569(18) Uani 1 1 d . . . H24 H -0.3244 0.6875 0.3471 0.068 Uiso 1 1 calc R . . C25 C -0.1476(6) 0.6941(3) 0.3581(2) 0.0475(16) Uani 1 1 d . . . H25 H -0.1237 0.6850 0.3272 0.057 Uiso 1 1 calc R . . C26 C -0.0626(5) 0.7064(2) 0.39494(17) 0.0309(12) Uani 1 1 d . . . C27 C 0.3781(5) 0.6813(3) 0.3672(2) 0.0434(15) Uani 1 1 d . . . C28 C 0.4048(5) 0.6163(3) 0.3674(3) 0.074(2) Uani 1 1 d . . . H28 H 0.3984 0.5924 0.3952 0.089 Uiso 1 1 calc R . . C29 C 0.4410(5) 0.5879(3) 0.3258(3) 0.115(4) Uani 1 1 d R . . H29 H 0.4597 0.5444 0.3257 0.138 Uiso 1 1 calc R . . C30 C 0.4500(8) 0.6222(8) 0.2843(4) 0.124(6) Uani 1 1 d . . . C31 C 0.4264(8) 0.6857(7) 0.2848(3) 0.106(4) Uani 1 1 d . . . H31 H 0.4351 0.7094 0.2569 0.128 Uiso 1 1 calc R . . C32 C 0.3894(6) 0.7163(4) 0.3259(2) 0.065(2) Uani 1 1 d . . . H32 H 0.3725 0.7600 0.3257 0.078 Uiso 1 1 calc R . . C33 C 0.4894(10) 0.5886(8) 0.2380(4) 0.199(8) Uani 1 1 d . . . H33C H 0.4239 0.5627 0.2260 0.299 Uiso 1 1 calc R . . H33B H 0.5586 0.5620 0.2445 0.299 Uiso 1 1 calc R . . H33A H 0.5101 0.6203 0.2147 0.299 Uiso 1 1 calc R . . C34 C 0.0400(5) 0.5403(3) 0.63883(18) 0.0356(13) Uani 1 1 d . . . C35 C -0.0602(6) 0.5012(3) 0.6393(2) 0.0432(15) Uani 1 1 d . . . H35 H -0.1109 0.5014 0.6656 0.052 Uiso 1 1 calc R . . C36 C -0.0862(6) 0.4615(3) 0.6011(2) 0.0531(17) Uani 1 1 d . . . H36 H -0.1544 0.4354 0.6013 0.064 Uiso 1 1 calc R . . C37 C -0.0098(7) 0.4613(3) 0.5628(2) 0.0590(18) Uani 1 1 d . . . H37 H -0.0259 0.4341 0.5372 0.071 Uiso 1 1 calc R . . C38 C 0.0881(7) 0.4999(3) 0.5616(2) 0.0600(19) Uani 1 1 d . . . H38 H 0.1369 0.5003 0.5348 0.072 Uiso 1 1 calc R . . C39 C 0.1165(6) 0.5388(3) 0.5998(2) 0.0477(15) Uani 1 1 d . . . H39 H 0.1863 0.5639 0.5995 0.057 Uiso 1 1 calc R . . C40 C 0.2090(5) 0.6324(3) 0.68194(19) 0.0381(13) Uani 1 1 d . . . C41 C 0.3048(6) 0.6292(3) 0.7142(2) 0.0590(18) Uani 1 1 d . . . H41 H 0.2986 0.6032 0.7409 0.071 Uiso 1 1 calc R . . C42 C 0.4098(7) 0.6644(4) 0.7071(3) 0.083(3) Uani 1 1 d . . . H42 H 0.4735 0.6614 0.7290 0.100 Uiso 1 1 calc R . . C43 C 0.4202(7) 0.7030(4) 0.6685(3) 0.075(2) Uani 1 1 d . . . H43 H 0.4906 0.7265 0.6639 0.090 Uiso 1 1 calc R . . C44 C 0.3256(7) 0.7069(3) 0.6362(3) 0.064(2) Uani 1 1 d . . . H44 H 0.3328 0.7331 0.6096 0.077 Uiso 1 1 calc R . . C45 C 0.2204(5) 0.6725(3) 0.6427(2) 0.0445(15) Uani 1 1 d . . . H45 H 0.1568 0.6762 0.6208 0.053 Uiso 1 1 calc R . . C46 C 0.1082(5) 0.5277(3) 0.73580(18) 0.0378(13) Uani 1 1 d . . . C47 C 0.1563(6) 0.4705(3) 0.7208(2) 0.0533(17) Uani 1 1 d . . . H47 H 0.1703 0.4634 0.6886 0.064 Uiso 1 1 calc R . . C48 C 0.1837(7) 0.4233(3) 0.7543(3) 0.065(2) Uani 1 1 d . . . H48 H 0.2167 0.3846 0.7444 0.078 Uiso 1 1 calc R . . C49 C 0.1629(6) 0.4332(3) 0.8011(3) 0.0616(19) Uani 1 1 d . . . H49 H 0.1816 0.4013 0.8231 0.074 Uiso 1 1 calc R . . C50 C 0.1145(6) 0.4900(3) 0.8161(2) 0.0515(17) Uani 1 1 d . . . H50 H 0.1007 0.4968 0.8484 0.062 Uiso 1 1 calc R . . C51 C 0.0860(5) 0.5372(3) 0.7831(2) 0.0437(15) Uani 1 1 d . . . H51 H 0.0518 0.5756 0.7932 0.052 Uiso 1 1 calc R . . C52 C 0.0598(5) 0.7430(3) 0.76488(18) 0.0413(15) Uani 1 1 d . . . C53 C 0.0546(5) 0.7745(3) 0.71805(18) 0.0342(13) Uani 1 1 d . . . C54 C 0.0968(5) 0.8323(3) 0.6988(2) 0.0419(14) Uani 1 1 d . . . C55 C 0.1614(6) 0.8861(3) 0.7172(3) 0.0604(19) Uani 1 1 d . . . H55 H 0.1877 0.8885 0.7488 0.072 Uiso 1 1 calc R . . C56 C 0.1823(7) 0.9351(3) 0.6844(4) 0.081(3) Uani 1 1 d . . . H56 H 0.2236 0.9715 0.6947 0.097 Uiso 1 1 calc R . . C57 C 0.1444(8) 0.9322(4) 0.6371(4) 0.082(3) Uani 1 1 d . . . H57 H 0.1623 0.9662 0.6169 0.098 Uiso 1 1 calc R . . C58 C 0.0828(7) 0.8817(3) 0.6196(3) 0.0590(19) Uani 1 1 d . . . H58 H 0.0566 0.8803 0.5880 0.071 Uiso 1 1 calc R . . C59 C 0.0598(6) 0.8316(3) 0.6510(2) 0.0413(14) Uani 1 1 d . . . C60 C -0.2223(5) 0.6255(3) 0.6095(2) 0.0388(13) Uani 1 1 d . . . C61 C -0.3424(6) 0.6081(4) 0.6105(2) 0.0622(19) Uani 1 1 d . . . H61 H -0.3834 0.6078 0.6393 0.075 Uiso 1 1 calc R . . C62 C -0.4023(7) 0.5909(4) 0.5689(3) 0.070(2) Uani 1 1 d . . . H62 H -0.4848 0.5815 0.5694 0.083 Uiso 1 1 calc R . . C63 C -0.3397(7) 0.5876(3) 0.5263(2) 0.0587(18) Uani 1 1 d . . . C64 C -0.2207(7) 0.6047(3) 0.5264(2) 0.0515(16) Uani 1 1 d . . . H64 H -0.1786 0.6038 0.4979 0.062 Uiso 1 1 calc R . . C65 C -0.1597(6) 0.6234(3) 0.5678(2) 0.0488(16) Uani 1 1 d . . . H65 H -0.0780 0.6343 0.5671 0.059 Uiso 1 1 calc R . . C66 C -0.4033(8) 0.5681(4) 0.4805(3) 0.087(3) Uani 1 1 d . . . H66C H -0.3629 0.5872 0.4539 0.131 Uiso 1 1 calc R . . H66B H -0.4860 0.5824 0.4810 0.131 Uiso 1 1 calc R . . H66A H -0.4013 0.5223 0.4774 0.131 Uiso 1 1 calc R . . N99 N -0.2288(11) 0.9062(5) 0.5745(4) 0.142(4) Uani 1 1 d . . . C98 C -0.2662(10) 0.8571(6) 0.5828(3) 0.091(3) Uani 1 1 d . . . C99 C -0.3132(9) 0.7959(5) 0.5950(4) 0.104(3) Uani 1 1 d . . . H99C H -0.2635 0.7631 0.5813 0.156 Uiso 1 1 calc R . . H99B H -0.3946 0.7920 0.5828 0.156 Uiso 1 1 calc R . . H99A H -0.3131 0.7913 0.6290 0.156 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 0.02842(12) 0.03652(14) 0.02296(12) -0.00009(9) -0.00154(8) -0.00251(10) Re2 0.03613(14) 0.03890(14) 0.03010(13) 0.00140(9) 0.00277(9) -0.00146(10) N2 0.028(2) 0.029(2) 0.023(2) -0.0025(17) -0.0026(18) -0.0008(19) N1 0.031(2) 0.042(3) 0.032(2) -0.008(2) 0.0022(19) -0.005(2) N3 0.034(3) 0.040(3) 0.018(2) -0.0103(18) -0.0007(18) -0.004(2) N4 0.045(3) 0.034(3) 0.023(2) -0.0026(19) 0.001(2) 0.000(2) N5 0.036(3) 0.039(3) 0.043(3) 0.001(2) -0.001(2) 0.004(2) N6 0.064(3) 0.039(3) 0.016(2) 0.0023(19) 0.000(2) 0.002(3) O1 0.035(2) 0.055(2) 0.0195(18) -0.0048(16) -0.0036(15) -0.0047(19) O2 0.048(2) 0.070(3) 0.022(2) -0.0054(19) 0.0104(18) -0.008(2) O3 0.045(2) 0.053(3) 0.0220(19) 0.0046(17) 0.0031(16) -0.003(2) O4 0.055(3) 0.098(4) 0.024(2) -0.016(2) -0.0041(19) -0.008(2) P1 0.0276(7) 0.0367(8) 0.0248(7) -0.0032(6) 0.0015(5) -0.0010(6) P2 0.0365(8) 0.0374(8) 0.0270(7) 0.0015(6) 0.0024(6) -0.0020(7) Cl2 0.0608(10) 0.0454(9) 0.0550(10) 0.0136(7) -0.0094(8) -0.0104(8) Cl1 0.0363(8) 0.0602(10) 0.0412(8) -0.0015(7) -0.0119(6) 0.0009(7) Cl3 0.0514(10) 0.0693(11) 0.0776(12) 0.0258(9) 0.0239(9) -0.0058(9) Cl4 0.0494(10) 0.0650(11) 0.0642(11) -0.0123(8) 0.0078(8) 0.0123(8) C1 0.033(3) 0.045(3) 0.025(3) -0.007(2) 0.004(2) -0.013(3) C2 0.037(4) 0.049(4) 0.061(4) -0.003(3) 0.011(3) -0.005(3) C3 0.034(4) 0.067(5) 0.078(5) -0.021(4) 0.022(4) -0.014(3) C4 0.067(5) 0.084(5) 0.042(4) -0.009(4) 0.026(4) -0.034(4) C5 0.052(4) 0.086(5) 0.043(4) 0.014(4) 0.007(3) -0.023(4) C6 0.039(3) 0.064(4) 0.043(4) 0.011(3) 0.002(3) -0.007(3) C7 0.033(3) 0.032(3) 0.027(3) 0.002(2) 0.005(2) -0.002(2) C8 0.037(3) 0.052(4) 0.033(3) -0.005(3) 0.000(2) 0.003(3) C9 0.036(4) 0.058(4) 0.060(4) -0.005(3) 0.012(3) 0.013(3) C10 0.035(3) 0.057(4) 0.061(4) 0.008(3) -0.001(3) 0.006(3) C11 0.038(3) 0.054(4) 0.041(3) 0.012(3) -0.007(3) -0.005(3) C12 0.033(3) 0.034(3) 0.034(3) 0.002(2) 0.005(2) -0.001(3) C13 0.028(3) 0.053(4) 0.036(3) -0.014(3) 0.000(2) -0.009(3) C14 0.043(4) 0.051(4) 0.051(4) -0.013(3) 0.006(3) -0.001(3) C15 0.054(4) 0.057(4) 0.075(5) -0.030(4) 0.011(4) -0.017(4) C16 0.048(4) 0.090(6) 0.073(5) -0.049(5) 0.002(4) -0.009(4) C17 0.062(5) 0.101(7) 0.045(4) -0.032(4) -0.009(3) 0.007(5) C18 0.051(4) 0.072(5) 0.039(4) -0.018(3) -0.006(3) 0.004(4) C19 0.035(3) 0.039(3) 0.025(3) 0.001(2) 0.000(2) -0.005(3) C20 0.034(3) 0.035(3) 0.019(3) 0.001(2) 0.005(2) -0.003(2) C21 0.031(3) 0.031(3) 0.027(3) 0.005(2) -0.001(2) -0.003(2) C22 0.031(3) 0.059(4) 0.042(3) 0.007(3) 0.000(3) 0.005(3) C23 0.031(3) 0.065(4) 0.062(4) 0.007(3) -0.007(3) 0.005(3) C24 0.037(4) 0.079(5) 0.054(4) -0.005(4) -0.018(3) -0.007(4) C25 0.045(4) 0.068(4) 0.029(3) -0.005(3) -0.010(3) -0.006(3) C26 0.029(3) 0.035(3) 0.028(3) 0.003(2) -0.003(2) -0.005(2) C27 0.021(3) 0.066(4) 0.043(4) -0.015(3) -0.001(2) -0.003(3) C28 0.067(5) 0.074(5) 0.081(5) -0.031(4) -0.004(4) 0.017(4) C29 0.091(7) 0.110(8) 0.143(10) -0.082(8) -0.023(7) 0.039(6) C30 0.045(5) 0.236(16) 0.092(7) -0.106(10) -0.004(5) 0.006(7) C31 0.071(6) 0.214(13) 0.035(4) -0.024(6) 0.007(4) -0.020(8) C32 0.062(5) 0.101(6) 0.032(4) -0.011(4) 0.001(3) -0.006(4) C33 0.079(7) 0.37(2) 0.148(10) -0.186(13) -0.004(7) 0.044(10) C34 0.042(3) 0.033(3) 0.032(3) 0.002(2) -0.003(2) -0.002(3) C35 0.051(4) 0.034(3) 0.045(4) 0.002(3) 0.003(3) -0.004(3) C36 0.057(4) 0.037(4) 0.065(4) -0.006(3) -0.010(3) -0.011(3) C37 0.077(5) 0.048(4) 0.051(4) -0.018(3) -0.009(4) -0.007(4) C38 0.076(5) 0.067(5) 0.036(4) -0.014(3) 0.008(3) -0.009(4) C39 0.049(4) 0.056(4) 0.038(3) -0.005(3) 0.006(3) -0.006(3) C40 0.036(3) 0.043(3) 0.035(3) -0.001(3) 0.008(3) -0.001(3) C41 0.053(4) 0.074(5) 0.050(4) 0.016(3) -0.003(3) -0.013(4) C42 0.050(5) 0.112(7) 0.088(6) 0.017(5) -0.010(4) -0.034(5) C43 0.048(5) 0.093(6) 0.083(6) 0.010(5) 0.009(4) -0.027(4) C44 0.075(5) 0.060(4) 0.059(5) 0.010(4) 0.023(4) -0.014(4) C45 0.041(4) 0.048(4) 0.045(4) 0.002(3) 0.006(3) 0.000(3) C46 0.041(3) 0.042(3) 0.031(3) 0.001(3) 0.000(2) -0.006(3) C47 0.069(5) 0.049(4) 0.042(4) 0.000(3) -0.006(3) 0.014(4) C48 0.077(5) 0.037(4) 0.081(5) 0.006(4) -0.018(4) 0.003(4) C49 0.063(5) 0.057(5) 0.064(5) 0.027(4) -0.020(4) -0.011(4) C50 0.053(4) 0.067(5) 0.034(3) 0.021(3) -0.008(3) -0.011(4) C51 0.052(4) 0.036(3) 0.043(4) 0.008(3) 0.003(3) -0.001(3) C52 0.038(3) 0.066(4) 0.020(3) -0.008(3) 0.002(2) 0.011(3) C53 0.033(3) 0.045(3) 0.025(3) -0.004(2) 0.001(2) -0.002(3) C54 0.034(3) 0.046(4) 0.046(4) -0.011(3) 0.004(3) 0.000(3) C55 0.046(4) 0.052(4) 0.084(5) -0.027(4) 0.006(4) 0.000(3) C56 0.067(5) 0.038(4) 0.138(8) -0.015(5) 0.025(5) -0.012(4) C57 0.077(6) 0.057(5) 0.113(8) 0.022(5) 0.040(5) 0.007(5) C58 0.076(5) 0.035(4) 0.067(5) 0.017(3) 0.025(4) 0.003(4) C59 0.048(4) 0.031(3) 0.045(4) 0.001(3) 0.011(3) 0.003(3) C60 0.040(3) 0.029(3) 0.046(4) -0.003(3) -0.010(3) 0.000(3) C61 0.047(4) 0.081(5) 0.058(4) -0.009(4) -0.001(3) -0.001(4) C62 0.051(4) 0.089(6) 0.069(5) -0.005(4) -0.015(4) -0.015(4) C63 0.071(5) 0.051(4) 0.054(4) -0.003(3) -0.020(4) -0.006(4) C64 0.070(5) 0.045(4) 0.039(4) 0.004(3) -0.006(3) 0.000(3) C65 0.053(4) 0.044(4) 0.050(4) 0.002(3) -0.010(3) -0.007(3) C66 0.106(7) 0.091(6) 0.064(5) -0.007(4) -0.041(5) -0.019(5) N99 0.192(12) 0.111(8) 0.123(8) 0.030(7) -0.014(7) 0.008(8) C98 0.102(8) 0.099(8) 0.073(6) 0.006(6) -0.014(5) 0.021(7) C99 0.089(7) 0.105(8) 0.118(8) -0.003(6) -0.032(6) -0.012(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 N1 1.722(4) . ? Re1 N2 2.089(4) . ? Re1 O1 2.092(3) . ? Re1 Cl1 2.3683(14) . ? Re1 Cl2 2.3961(15) . ? Re1 P1 2.4484(14) . ? Re2 N5 1.717(5) . ? Re2 N4 2.079(4) . ? Re2 O3 2.089(4) . ? Re2 Cl3 2.3545(15) . ? Re2 Cl4 2.4177(16) . ? Re2 P2 2.4423(15) . ? N2 C20 1.333(6) . ? N2 N3 1.341(5) . ? N1 C27 1.374(7) . ? N3 C26 1.361(6) . ? N3 H3A 0.8600 . ? N4 C53 1.333(7) . ? N4 N6 1.357(6) . ? N5 C60 1.375(7) . ? N6 C59 1.342(7) . ? N6 H6A 0.8600 . ? O1 C19 1.303(6) . ? O2 C19 1.215(6) . ? O3 C52 1.304(7) . ? O4 C52 1.225(7) . ? P1 C7 1.810(5) . ? P1 C13 1.826(5) . ? P1 C1 1.829(5) . ? P2 C40 1.811(6) . ? P2 C34 1.824(5) . ? P2 C46 1.828(6) . ? C1 C2 1.379(8) . ? C1 C6 1.382(8) . ? C2 C3 1.378(8) . ? C2 H2 0.9300 . ? C3 C4 1.359(10) . ? C3 H3 0.9300 . ? C4 C5 1.341(10) . ? C4 H4 0.9300 . ? C5 C6 1.379(8) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.395(7) . ? C7 C12 1.400(7) . ? C8 C9 1.378(8) . ? C8 H8 0.9300 . ? C9 C10 1.373(8) . ? C9 H9 0.9300 . ? C10 C11 1.387(8) . ? C10 H10 0.9300 . ? C11 C12 1.375(8) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C18 1.373(8) . ? C13 C14 1.382(8) . ? C14 C15 1.391(8) . ? C14 H14 0.9300 . ? C15 C16 1.366(10) . ? C15 H15 0.9300 . ? C16 C17 1.354(11) . ? C16 H16 0.9300 . ? C17 C18 1.397(9) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.476(7) . ? C20 C21 1.404(7) . ? C21 C26 1.394(7) . ? C21 C22 1.420(7) . ? C22 C23 1.351(8) . ? C22 H22 0.9300 . ? C23 C24 1.411(9) . ? C23 H23 0.9300 . ? C24 C25 1.346(8) . ? C24 H24 0.9300 . ? C25 C26 1.411(7) . ? C25 H25 0.9300 . ? C27 C32 1.375(9) . ? C27 C28 1.390(9) . ? C28 C29 1.3724 . ? C28 H28 0.9300 . ? C29 C30 1.373(15) . ? C29 H29 0.9300 . ? C30 C31 1.351(16) . ? C30 C33 1.543(11) . ? C31 C32 1.386(11) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 H33C 0.9600 . ? C33 H33B 0.9600 . ? C33 H33A 0.9600 . ? C34 C35 1.374(8) . ? C34 C39 1.390(8) . ? C35 C36 1.383(8) . ? C35 H35 0.9300 . ? C36 C37 1.375(9) . ? C36 H36 0.9300 . ? C37 C38 1.347(10) . ? C37 H37 0.9300 . ? C38 C39 1.379(8) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C41 1.384(8) . ? C40 C45 1.391(8) . ? C41 C42 1.387(9) . ? C41 H41 0.9300 . ? C42 C43 1.356(10) . ? C42 H42 0.9300 . ? C43 C44 1.376(10) . ? C43 H43 0.9300 . ? C44 C45 1.378(9) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 C51 1.368(7) . ? C46 C47 1.373(8) . ? C47 C48 1.393(9) . ? C47 H47 0.9300 . ? C48 C49 1.352(9) . ? C48 H48 0.9300 . ? C49 C50 1.368(9) . ? C49 H49 0.9300 . ? C50 C51 1.387(8) . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? C52 C53 1.470(7) . ? C53 C54 1.404(8) . ? C54 C59 1.399(8) . ? C54 C55 1.424(9) . ? C55 C56 1.398(11) . ? C55 H55 0.9300 . ? C56 C57 1.389(11) . ? C56 H56 0.9300 . ? C57 C58 1.343(11) . ? C57 H57 0.9300 . ? C58 C59 1.392(8) . ? C58 H58 0.9300 . ? C60 C65 1.366(8) . ? C60 C61 1.374(8) . ? C61 C62 1.384(9) . ? C61 H61 0.9300 . ? C62 C63 1.389(10) . ? C62 H62 0.9300 . ? C63 C64 1.360(9) . ? C63 C66 1.514(9) . ? C64 C65 1.392(8) . ? C64 H64 0.9300 . ? C65 H65 0.9300 . ? C66 H66C 0.9600 . ? C66 H66B 0.9600 . ? C66 H66A 0.9600 . ? N99 C98 1.128(12) . ? C98 C99 1.422(14) . ? C99 H99C 0.9600 . ? C99 H99B 0.9600 . ? C99 H99A 0.9600 . ? 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 N1 Re1 N2 92.10(18) . . ? N1 Re1 O1 166.12(18) . . ? N2 Re1 O1 74.13(14) . . ? N1 Re1 Cl1 99.24(15) . . ? N2 Re1 Cl1 167.59(11) . . ? O1 Re1 Cl1 94.63(10) . . ? N1 Re1 Cl2 97.83(15) . . ? N2 Re1 Cl2 87.21(12) . . ? O1 Re1 Cl2 83.46(11) . . ? Cl1 Re1 Cl2 86.27(5) . . ? N1 Re1 P1 98.07(15) . . ? N2 Re1 P1 90.96(11) . . ? O1 Re1 P1 80.81(11) . . ? Cl1 Re1 P1 92.41(5) . . ? Cl2 Re1 P1 164.05(5) . . ? N5 Re2 N4 97.93(19) . . ? N5 Re2 O3 170.49(18) . . ? N4 Re2 O3 74.33(16) . . ? N5 Re2 Cl3 98.74(16) . . ? N4 Re2 Cl3 162.48(12) . . ? O3 Re2 Cl3 89.55(11) . . ? N5 Re2 Cl4 98.22(15) . . ? N4 Re2 Cl4 84.68(13) . . ? O3 Re2 Cl4 86.70(11) . . ? Cl3 Re2 Cl4 87.63(6) . . ? N5 Re2 P2 92.06(15) . . ? N4 Re2 P2 93.20(13) . . ? O3 Re2 P2 83.01(11) . . ? Cl3 Re2 P2 91.56(6) . . ? Cl4 Re2 P2 169.68(5) . . ? C20 N2 N3 108.3(4) . . ? C20 N2 Re1 118.3(3) . . ? N3 N2 Re1 133.3(3) . . ? C27 N1 Re1 169.2(4) . . ? N2 N3 C26 109.7(4) . . ? N2 N3 H3A 125.2 . . ? C26 N3 H3A 125.2 . . ? C53 N4 N6 107.0(4) . . ? C53 N4 Re2 117.7(3) . . ? N6 N4 Re2 134.2(4) . . ? C60 N5 Re2 177.4(4) . . ? C59 N6 N4 111.0(5) . . ? C59 N6 H6A 124.5 . . ? N4 N6 H6A 124.5 . . ? C19 O1 Re1 120.1(3) . . ? C52 O3 Re2 119.8(3) . . ? C7 P1 C13 104.2(3) . . ? C7 P1 C1 107.1(2) . . ? C13 P1 C1 103.6(2) . . ? C7 P1 Re1 110.12(17) . . ? C13 P1 Re1 119.1(2) . . ? C1 P1 Re1 111.87(19) . . ? C40 P2 C34 107.4(3) . . ? C40 P2 C46 105.0(3) . . ? C34 P2 C46 101.5(3) . . ? C40 P2 Re2 112.04(19) . . ? C34 P2 Re2 110.17(19) . . ? C46 P2 Re2 119.65(19) . . ? C2 C1 C6 118.5(5) . . ? C2 C1 P1 119.3(5) . . ? C6 C1 P1 122.2(4) . . ? C3 C2 C1 119.2(6) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C4 C3 C2 121.5(7) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C5 C4 C3 119.8(6) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.2(7) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 120.7(6) . . ? C5 C6 H6 119.6 . . ? C1 C6 H6 119.6 . . ? C8 C7 C12 118.2(5) . . ? C8 C7 P1 120.7(4) . . ? C12 C7 P1 120.7(4) . . ? C9 C8 C7 121.0(5) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C10 C9 C8 120.1(6) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 119.9(6) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C12 C11 C10 120.4(6) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C7 120.4(5) . . ? C11 C12 H12 119.8 . . ? C7 C12 H12 119.8 . . ? C18 C13 C14 119.2(5) . . ? C18 C13 P1 123.5(5) . . ? C14 C13 P1 117.3(4) . . ? C13 C14 C15 120.6(6) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C16 C15 C14 119.2(7) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C17 C16 C15 120.8(7) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 120.4(7) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C13 C18 C17 119.6(7) . . ? C13 C18 H18 120.2 . . ? C17 C18 H18 120.2 . . ? O2 C19 O1 124.7(5) . . ? O2 C19 C20 122.8(5) . . ? O1 C19 C20 112.5(4) . . ? N2 C20 C21 109.5(4) . . ? N2 C20 C19 114.1(5) . . ? C21 C20 C19 136.4(5) . . ? C26 C21 C20 104.9(4) . . ? C26 C21 C22 118.5(5) . . ? C20 C21 C22 136.6(5) . . ? C23 C22 C21 117.7(6) . . ? C23 C22 H22 121.1 . . ? C21 C22 H22 121.1 . . ? C22 C23 C24 122.6(6) . . ? C22 C23 H23 118.7 . . ? C24 C23 H23 118.7 . . ? C25 C24 C23 121.6(6) . . ? C25 C24 H24 119.2 . . ? C23 C24 H24 119.2 . . ? C24 C25 C26 116.4(5) . . ? C24 C25 H25 121.8 . . ? C26 C25 H25 121.8 . . ? N3 C26 C21 107.5(4) . . ? N3 C26 C25 129.3(5) . . ? C21 C26 C25 123.2(5) . . ? N1 C27 C32 123.1(6) . . ? N1 C27 C28 116.8(6) . . ? C32 C27 C28 120.1(6) . . ? C29 C28 C27 118.8(4) . . ? C29 C28 H28 120.6 . . ? C27 C28 H28 120.6 . . ? C28 C29 C30 121.5(6) . . ? C28 C29 H29 119.3 . . ? C30 C29 H29 119.3 . . ? C31 C30 C29 119.2(8) . . ? C31 C30 C33 120.7(13) . . ? C29 C30 C33 120.1(13) . . ? C30 C31 C32 121.3(10) . . ? C30 C31 H31 119.4 . . ? C32 C31 H31 119.4 . . ? C27 C32 C31 119.2(9) . . ? C27 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C30 C33 H33C 109.5 . . ? C30 C33 H33B 109.5 . . ? H33C C33 H33B 109.5 . . ? C30 C33 H33A 109.5 . . ? H33C C33 H33A 109.5 . . ? H33B C33 H33A 109.5 . . ? C35 C34 C39 119.4(5) . . ? C35 C34 P2 117.2(4) . . ? C39 C34 P2 123.3(5) . . ? C34 C35 C36 120.4(6) . . ? C34 C35 H35 119.8 . . ? C36 C35 H35 119.8 . . ? C37 C36 C35 119.1(6) . . ? C37 C36 H36 120.5 . . ? C35 C36 H36 120.5 . . ? C38 C37 C36 121.0(6) . . ? C38 C37 H37 119.5 . . ? C36 C37 H37 119.5 . . ? C37 C38 C39 120.6(6) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C38 C39 C34 119.4(6) . . ? C38 C39 H39 120.3 . . ? C34 C39 H39 120.3 . . ? C41 C40 C45 118.1(6) . . ? C41 C40 P2 121.4(4) . . ? C45 C40 P2 120.4(5) . . ? C40 C41 C42 120.8(6) . . ? C40 C41 H41 119.6 . . ? C42 C41 H41 119.6 . . ? C43 C42 C41 120.5(7) . . ? C43 C42 H42 119.8 . . ? C41 C42 H42 119.8 . . ? C42 C43 C44 119.4(7) . . ? C42 C43 H43 120.3 . . ? C44 C43 H43 120.3 . . ? C43 C44 C45 121.0(7) . . ? C43 C44 H44 119.5 . . ? C45 C44 H44 119.5 . . ? C44 C45 C40 120.1(6) . . ? C44 C45 H45 120.0 . . ? C40 C45 H45 120.0 . . ? C51 C46 C47 119.9(5) . . ? C51 C46 P2 120.9(4) . . ? C47 C46 P2 119.2(4) . . ? C46 C47 C48 119.2(6) . . ? C46 C47 H47 120.4 . . ? C48 C47 H47 120.4 . . ? C49 C48 C47 120.7(7) . . ? C49 C48 H48 119.7 . . ? C47 C48 H48 119.7 . . ? C48 C49 C50 120.3(6) . . ? C48 C49 H49 119.9 . . ? C50 C49 H49 119.9 . . ? C49 C50 C51 119.7(6) . . ? C49 C50 H50 120.2 . . ? C51 C50 H50 120.2 . . ? C46 C51 C50 120.3(6) . . ? C46 C51 H51 119.9 . . ? C50 C51 H51 119.9 . . ? O4 C52 O3 125.1(5) . . ? O4 C52 C53 122.5(6) . . ? O3 C52 C53 112.3(5) . . ? N4 C53 C54 109.6(5) . . ? N4 C53 C52 114.5(5) . . ? C54 C53 C52 135.9(5) . . ? C59 C54 C53 105.4(5) . . ? C59 C54 C55 119.8(6) . . ? C53 C54 C55 134.8(6) . . ? C56 C55 C54 115.0(7) . . ? C56 C55 H55 122.5 . . ? C54 C55 H55 122.5 . . ? C57 C56 C55 123.3(7) . . ? C57 C56 H56 118.4 . . ? C55 C56 H56 118.4 . . ? C58 C57 C56 121.9(7) . . ? C58 C57 H57 119.1 . . ? C56 C57 H57 119.1 . . ? C57 C58 C59 117.1(7) . . ? C57 C58 H58 121.5 . . ? C59 C58 H58 121.5 . . ? N6 C59 C58 130.0(6) . . ? N6 C59 C54 106.9(5) . . ? C58 C59 C54 123.0(6) . . ? C65 C60 C61 120.5(6) . . ? C65 C60 N5 121.5(5) . . ? C61 C60 N5 117.9(5) . . ? C60 C61 C62 120.1(6) . . ? C60 C61 H61 120.0 . . ? C62 C61 H61 120.0 . . ? C61 C62 C63 120.1(7) . . ? C61 C62 H62 119.9 . . ? C63 C62 H62 119.9 . . ? C64 C63 C62 118.3(6) . . ? C64 C63 C66 120.7(7) . . ? C62 C63 C66 120.9(7) . . ? C63 C64 C65 122.2(6) . . ? C63 C64 H64 118.9 . . ? C65 C64 H64 118.9 . . ? C60 C65 C64 118.7(6) . . ? C60 C65 H65 120.7 . . ? C64 C65 H65 120.7 . . ? C63 C66 H66C 109.5 . . ? C63 C66 H66B 109.5 . . ? H66C C66 H66B 109.5 . . ? C63 C66 H66A 109.5 . . ? H66C C66 H66A 109.5 . . ? H66B C66 H66A 109.5 . . ? N99 C98 C99 178.0(12) . . ? C98 C99 H99C 109.5 . . ? C98 C99 H99B 109.5 . . ? H99C C99 H99B 109.5 . . ? C98 C99 H99A 109.5 . . ? H99C C99 H99A 109.5 . . ? H99B C99 H99A 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3A O4 0.86 2.10 2.772(5) 134.0 4_575 N6 H6A O2 0.86 2.02 2.771(5) 146.0 . C4 H4 Cl3 0.93 2.83 3.692(7) 155.2 4_675 C18 H18 Cl1 0.93 2.64 3.315(7) 130.5 . C51 H51 O3 0.93 2.53 3.317(7) 142.0 . C56 H56 Cl3 0.93 2.78 3.565(8) 143.2 2_556 C99 H99B Cl1 0.96 2.82 3.637(9) 143.5 1_455 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.337 _refine_diff_density_min -1.181 _refine_diff_density_rms 0.131 _database_code_depnum_ccdc_archive 'CCDC 973298' data_added_by_encifer _publ_section_references ;CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET) Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. Flack. H. D. (1983). Acta Cryst. A39, 876--881. Sheldrick, G. M. (1990a). Acta Cryst. A46, 467--473. Sheldrick, G. M. (1990b). SHELXTL/PC Software. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany Spek, A. L. (1990). Acta Cryst. A46, C-34. UNIL IC & KUMA (2000). CrysAlis CCD. Version 1.163. Kuma Diffraction Instruments GmbH, Wroc\/law, Poland. UNIL IC & KUMA (2000). CrysAlis RED. Version 1.163. Kuma Diffraction Instruments GmbH, Wroc\/law, Poland. ; data_ren250 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C33 H27 Br2 N3 O2 P Re), C H4 O' _chemical_formula_sum 'C67 H58 Br4 N6 O5 P2 Re2' _chemical_formula_weight 1781.17 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' Br Br -0.2901 2.4595 '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.1469(3) _cell_length_b 21.1457(6) _cell_length_c 28.1190(7) _cell_angle_alpha 90.00 _cell_angle_beta 91.056(2) _cell_angle_gamma 90.00 _cell_volume 6626.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 18575 _cell_measurement_theta_min 3.3914 _cell_measurement_theta_max 29.2937 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.11512 _exptl_crystal_size_mid 0.07928 _exptl_crystal_size_min 0.01911 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.785 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3448 _exptl_absorpt_coefficient_mu 6.163 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ;CrysAlis RED, (2005) ; _exptl_absorpt_correction_T_min 0.38128 _exptl_absorpt_correction_T_max 1.00000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _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 48598 _diffrn_reflns_av_R_equivalents 0.1008 _diffrn_reflns_av_unetI/netI 0.0963 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 25.05 _reflns_number_total 11720 _reflns_number_gt 7948 _reflns_threshold_expression >2sigma(I) #========================================================================== # # REFINEMENT DATA _computing_data_collection 'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)' _computing_cell_refinement 'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)' _computing_data_reduction 'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;XP in SHELXTL/PC (Sheldrick, 1990b) ORTEP-3 W v. 1.062 (Farrugia 1997) ; _computing_publication_material ;SHELXL-97 (Sheldrick, 1997) and PLATON (Spek, 1990) ; _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^)+(0.0569P)^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 11720 _refine_ls_number_parameters 779 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0947 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1330 _refine_ls_wR_factor_gt 0.1194 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _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 0.40077(3) 0.662266(17) 0.703122(13) 0.03457(12) Uani 1 1 d . . . Re2 Re 0.78312(3) 0.734592(17) 0.462450(12) 0.03117(12) Uani 1 1 d . . . N2 N 0.4996(7) 0.7424(3) 0.6836(2) 0.0326(17) Uani 1 1 d . . . N1 N 0.3366(6) 0.6455(3) 0.6496(3) 0.0354(18) Uani 1 1 d . . . N3 N 0.5020(7) 0.7779(3) 0.6431(3) 0.0396(19) Uani 1 1 d . . . H3 H 0.4684 0.7680 0.6163 0.048 Uiso 1 1 calc R . . N4 N 0.6074(6) 0.7260(3) 0.4358(2) 0.0293(17) Uani 1 1 d . . . N5 N 0.8430(6) 0.7138(4) 0.4096(2) 0.0363(19) Uani 1 1 d . . . N6 N 0.5628(6) 0.7087(3) 0.3934(2) 0.0313(17) Uani 1 1 d . . . H6 H 0.6045 0.6986 0.3691 0.038 Uiso 1 1 calc R . . O1 O 0.5016(6) 0.6879(3) 0.76332(19) 0.0425(16) Uani 1 1 d . . . O2 O 0.6143(6) 0.7632(4) 0.7985(2) 0.056(2) Uani 1 1 d . . . O3 O 0.6723(5) 0.7607(3) 0.51784(19) 0.0361(15) Uani 1 1 d . . . O4 O 0.4846(6) 0.7580(3) 0.5464(2) 0.0480(17) Uani 1 1 d . . . P1 P 0.5683(2) 0.59015(11) 0.69029(8) 0.0340(6) Uani 1 1 d . . . P2 P 0.7789(2) 0.84921(11) 0.44976(8) 0.0325(6) Uani 1 1 d . . . Br2 Br 0.24414(10) 0.74311(5) 0.73006(4) 0.0568(3) Uani 1 1 d . . . Br1 Br 0.29097(11) 0.58143(6) 0.75010(5) 0.0681(4) Uani 1 1 d . . . Br4 Br 0.75954(10) 0.62405(5) 0.49659(4) 0.0556(3) Uani 1 1 d . . . Br3 Br 0.97400(9) 0.74058(5) 0.51109(4) 0.0498(3) Uani 1 1 d . . . C1 C 0.5407(8) 0.5420(4) 0.6380(3) 0.037(2) Uani 1 1 d . . . C2 C 0.4386(9) 0.5030(4) 0.6386(3) 0.046(2) Uani 1 1 d . . . H2 H 0.3868 0.5044 0.6642 0.055 Uiso 1 1 calc R . . C3 C 0.4164(10) 0.4627(5) 0.6008(4) 0.058(3) Uani 1 1 d . . . H3A H 0.3507 0.4357 0.6016 0.069 Uiso 1 1 calc R . . C4 C 0.4887(11) 0.4619(5) 0.5624(4) 0.061(3) Uani 1 1 d . . . H4 H 0.4705 0.4361 0.5365 0.074 Uiso 1 1 calc R . . C5 C 0.5871(11) 0.4989(5) 0.5624(4) 0.061(3) Uani 1 1 d . . . H5 H 0.6379 0.4972 0.5366 0.073 Uiso 1 1 calc R . . C6 C 0.6148(10) 0.5394(5) 0.5997(3) 0.050(3) Uani 1 1 d . . . H6A H 0.6831 0.5645 0.5987 0.061 Uiso 1 1 calc R . . C7 C 0.6046(9) 0.5301(4) 0.7340(3) 0.039(2) Uani 1 1 d . . . C8 C 0.6535(9) 0.4738(5) 0.7201(4) 0.051(3) Uani 1 1 d . . . H8 H 0.6694 0.4671 0.6881 0.061 Uiso 1 1 calc R . . C9 C 0.6798(12) 0.4265(6) 0.7528(5) 0.070(3) Uani 1 1 d . . . H9 H 0.7135 0.3887 0.7427 0.084 Uiso 1 1 calc R . . C10 C 0.6565(11) 0.4354(6) 0.7991(5) 0.067(4) Uani 1 1 d . . . H10 H 0.6731 0.4033 0.8209 0.081 Uiso 1 1 calc R . . C11 C 0.6083(10) 0.4916(5) 0.8147(4) 0.055(3) Uani 1 1 d . . . H11 H 0.5926 0.4973 0.8468 0.066 Uiso 1 1 calc R . . C12 C 0.5833(9) 0.5397(5) 0.7825(4) 0.049(3) Uani 1 1 d . . . H12 H 0.5526 0.5780 0.7929 0.059 Uiso 1 1 calc R . . C13 C 0.7076(8) 0.6321(4) 0.6809(3) 0.034(2) Uani 1 1 d . . . C14 C 0.8008(10) 0.6285(6) 0.7128(4) 0.060(3) Uani 1 1 d . . . H14 H 0.7941 0.6034 0.7398 0.073 Uiso 1 1 calc R . . C15 C 0.9066(11) 0.6625(6) 0.7052(5) 0.073(4) Uani 1 1 d . . . H15 H 0.9710 0.6585 0.7265 0.088 Uiso 1 1 calc R . . C16 C 0.9155(10) 0.7006(7) 0.6673(5) 0.083(4) Uani 1 1 d . . . H16 H 0.9856 0.7235 0.6626 0.100 Uiso 1 1 calc R . . C17 C 0.8218(11) 0.7059(5) 0.6356(4) 0.059(3) Uani 1 1 d . . . H17 H 0.8286 0.7328 0.6097 0.071 Uiso 1 1 calc R . . C18 C 0.7194(9) 0.6726(5) 0.6412(3) 0.047(3) Uani 1 1 d . . . H18 H 0.6570 0.6764 0.6189 0.056 Uiso 1 1 calc R . . C19 C 0.5613(9) 0.7417(5) 0.7639(3) 0.040(2) Uani 1 1 d . . . C20 C 0.5575(8) 0.7740(4) 0.7179(3) 0.035(2) Uani 1 1 d . . . C21 C 0.5997(8) 0.8316(4) 0.7005(4) 0.040(2) Uani 1 1 d . . . C22 C 0.6625(10) 0.8828(5) 0.7186(5) 0.065(3) Uani 1 1 d . . . H22 H 0.6858 0.8847 0.7505 0.078 Uiso 1 1 calc R . . C23 C 0.6890(12) 0.9308(6) 0.6875(7) 0.091(5) Uani 1 1 d . . . H23 H 0.7340 0.9649 0.6985 0.109 Uiso 1 1 calc R . . C24 C 0.6511(13) 0.9299(6) 0.6404(7) 0.092(5) Uani 1 1 d . . . H24 H 0.6701 0.9642 0.6212 0.110 Uiso 1 1 calc R . . C25 C 0.5878(11) 0.8819(5) 0.6211(4) 0.065(3) Uani 1 1 d . . . H25 H 0.5605 0.8823 0.5896 0.078 Uiso 1 1 calc R . . C26 C 0.5663(9) 0.8314(4) 0.6520(4) 0.043(2) Uani 1 1 d . . . C27 C 0.2814(8) 0.6272(4) 0.6066(3) 0.033(2) Uani 1 1 d . . . C28 C 0.1632(9) 0.6089(5) 0.6074(4) 0.059(3) Uani 1 1 d . . . H28 H 0.1216 0.6082 0.6358 0.070 Uiso 1 1 calc R . . C29 C 0.1073(12) 0.5916(6) 0.5650(5) 0.077(4) Uani 1 1 d . . . H29 H 0.0260 0.5818 0.5650 0.092 Uiso 1 1 calc R . . C30 C 0.1661(11) 0.5884(5) 0.5236(4) 0.056(3) Uani 1 1 d . . . C31 C 0.2835(10) 0.6067(4) 0.5238(4) 0.049(3) Uani 1 1 d . . . H31 H 0.3254 0.6059 0.4955 0.059 Uiso 1 1 calc R . . C32 C 0.3415(9) 0.6264(4) 0.5649(3) 0.041(2) Uani 1 1 d . . . H32 H 0.4214 0.6390 0.5642 0.049 Uiso 1 1 calc R . . C33 C 0.1026(12) 0.5685(7) 0.4777(4) 0.090(5) Uani 1 1 d . . . H33A H 0.1169 0.5244 0.4721 0.135 Uiso 1 1 calc R . . H33B H 0.1328 0.5928 0.4517 0.135 Uiso 1 1 calc R . . H33C H 0.0180 0.5757 0.4804 0.135 Uiso 1 1 calc R . . C34 C 0.8727(8) 0.8735(4) 0.4007(3) 0.037(2) Uani 1 1 d . . . C35 C 0.9852(9) 0.8452(4) 0.3969(4) 0.044(3) Uani 1 1 d . . . H35 H 1.0112 0.8148 0.4187 0.053 Uiso 1 1 calc R . . C36 C 1.0561(10) 0.8633(6) 0.3602(4) 0.061(3) Uani 1 1 d . . . H36 H 1.1316 0.8451 0.3575 0.073 Uiso 1 1 calc R . . C37 C 1.0200(11) 0.9075(6) 0.3269(4) 0.061(3) Uani 1 1 d . . . H37 H 1.0691 0.9179 0.3017 0.073 Uiso 1 1 calc R . . C38 C 0.9116(11) 0.9354(6) 0.3317(4) 0.066(3) Uani 1 1 d . . . H38 H 0.8869 0.9658 0.3097 0.079 Uiso 1 1 calc R . . C39 C 0.8366(9) 0.9197(5) 0.3687(4) 0.053(3) Uani 1 1 d . . . H39 H 0.7631 0.9399 0.3720 0.063 Uiso 1 1 calc R . . C40 C 0.8226(8) 0.9016(4) 0.4988(3) 0.038(2) Uani 1 1 d . . . C41 C 0.8293(9) 0.9667(5) 0.4884(4) 0.053(3) Uani 1 1 d . . . H41 H 0.8090 0.9814 0.4582 0.063 Uiso 1 1 calc R . . C42 C 0.8663(10) 1.0086(6) 0.5235(5) 0.066(3) Uani 1 1 d . . . H42 H 0.8680 1.0517 0.5169 0.079 Uiso 1 1 calc R . . C43 C 0.9002(11) 0.9878(7) 0.5673(5) 0.072(4) Uani 1 1 d . . . H43 H 0.9299 1.0163 0.5898 0.086 Uiso 1 1 calc R . . C44 C 0.8907(11) 0.9248(7) 0.5784(4) 0.078(4) Uani 1 1 d . . . H44 H 0.9101 0.9113 0.6091 0.094 Uiso 1 1 calc R . . C45 C 0.8515(9) 0.8799(6) 0.5437(3) 0.055(3) Uani 1 1 d . . . H45 H 0.8456 0.8372 0.5512 0.066 Uiso 1 1 calc R . . C46 C 0.6268(8) 0.8745(4) 0.4343(3) 0.034(2) Uani 1 1 d . . . C47 C 0.5566(9) 0.9034(5) 0.4680(3) 0.045(2) Uani 1 1 d . . . H47 H 0.5895 0.9137 0.4976 0.054 Uiso 1 1 calc R . . C48 C 0.4371(10) 0.9170(5) 0.4576(4) 0.063(3) Uani 1 1 d . . . H48 H 0.3904 0.9375 0.4799 0.075 Uiso 1 1 calc R . . C49 C 0.3878(9) 0.9000(5) 0.4142(4) 0.056(3) Uani 1 1 d . . . H49 H 0.3070 0.9078 0.4078 0.067 Uiso 1 1 calc R . . C50 C 0.4558(9) 0.8724(5) 0.3812(4) 0.054(3) Uani 1 1 d . . . H50 H 0.4220 0.8623 0.3517 0.065 Uiso 1 1 calc R . . C51 C 0.5754(8) 0.8588(4) 0.3904(3) 0.037(2) Uani 1 1 d . . . H51 H 0.6212 0.8392 0.3674 0.044 Uiso 1 1 calc R . . C52 C 0.5553(10) 0.7520(4) 0.5143(3) 0.038(2) Uani 1 1 d . . . C53 C 0.5167(8) 0.7336(4) 0.4652(3) 0.035(2) Uani 1 1 d . . . C54 C 0.4056(8) 0.7242(4) 0.4412(3) 0.031(2) Uani 1 1 d . . . C55 C 0.2837(8) 0.7281(4) 0.4522(3) 0.040(2) Uani 1 1 d . . . H55 H 0.2583 0.7388 0.4825 0.047 Uiso 1 1 calc R . . C56 C 0.2028(8) 0.7150(5) 0.4154(4) 0.047(3) Uani 1 1 d . . . H56 H 0.1212 0.7156 0.4216 0.057 Uiso 1 1 calc R . . C57 C 0.2394(10) 0.7010(6) 0.3694(4) 0.062(3) Uani 1 1 d . . . H57 H 0.1812 0.6939 0.3459 0.075 Uiso 1 1 calc R . . C58 C 0.3574(9) 0.6973(5) 0.3578(3) 0.048(3) Uani 1 1 d . . . H58 H 0.3815 0.6872 0.3272 0.057 Uiso 1 1 calc R . . C59 C 0.4400(8) 0.7097(4) 0.3947(3) 0.032(2) Uani 1 1 d . . . C60 C 0.8787(8) 0.6853(5) 0.3662(3) 0.043(2) Uani 1 1 d . . . C61 C 0.9035(12) 0.6218(6) 0.3673(5) 0.076(4) Uani 1 1 d . . . H61 H 0.8948 0.5978 0.3948 0.092 Uiso 1 1 calc R . . C62 C 0.9423(13) 0.5951(7) 0.3253(7) 0.099(5) Uani 1 1 d . . . H62 H 0.9614 0.5523 0.3251 0.119 Uiso 1 1 calc R . . C63 C 0.9538(12) 0.6285(12) 0.2840(6) 0.111(7) Uani 1 1 d . . . C64 C 0.9269(12) 0.6901(9) 0.2854(4) 0.091(5) Uani 1 1 d . . . H64 H 0.9349 0.7138 0.2577 0.110 Uiso 1 1 calc R . . C65 C 0.8877(10) 0.7203(6) 0.3259(4) 0.063(3) Uani 1 1 d . . . H65 H 0.8682 0.7630 0.3255 0.076 Uiso 1 1 calc R . . C66 C 0.9940(15) 0.5954(10) 0.2391(6) 0.164(10) Uani 1 1 d . . . H66A H 1.0257 0.6260 0.2174 0.245 Uiso 1 1 calc R . . H66B H 0.9267 0.5743 0.2243 0.245 Uiso 1 1 calc R . . H66C H 1.0550 0.5649 0.2470 0.245 Uiso 1 1 calc R . . O99 O 0.2077(18) 0.8218(15) 0.5907(7) 0.312(17) Uani 1 1 d . . . H99 H 0.1560 0.8273 0.6107 0.468 Uiso 1 1 calc R . . C99 C 0.279(2) 0.8964(12) 0.5775(6) 0.164(11) Uani 1 1 d . . . H99A H 0.2403 0.9297 0.5946 0.246 Uiso 1 1 calc R . . H99B H 0.2728 0.9046 0.5440 0.246 Uiso 1 1 calc R . . H99C H 0.3623 0.8945 0.5870 0.246 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 0.0347(2) 0.0364(2) 0.0327(2) 0.00144(16) 0.00259(17) -0.00258(17) Re2 0.0279(2) 0.0386(2) 0.0269(2) -0.00043(15) -0.00087(15) -0.00381(16) N2 0.041(5) 0.034(4) 0.023(4) -0.006(3) -0.002(3) 0.000(3) N1 0.034(4) 0.030(4) 0.043(5) 0.003(3) 0.010(4) 0.012(3) N3 0.050(5) 0.041(5) 0.028(4) 0.003(3) -0.005(4) -0.001(4) N4 0.035(4) 0.038(4) 0.015(4) -0.002(3) -0.005(3) -0.009(3) N5 0.025(4) 0.054(5) 0.029(4) -0.005(3) 0.005(3) -0.021(4) N6 0.033(4) 0.039(4) 0.022(4) -0.007(3) 0.005(3) -0.003(3) O1 0.045(4) 0.057(4) 0.025(3) 0.010(3) 0.005(3) 0.003(3) O2 0.049(5) 0.088(6) 0.032(4) -0.015(4) -0.007(3) -0.004(4) O3 0.026(4) 0.055(4) 0.027(3) -0.006(3) -0.004(3) -0.009(3) O4 0.051(4) 0.069(5) 0.025(4) -0.005(3) 0.007(3) -0.008(4) P1 0.0369(15) 0.0351(14) 0.0302(13) 0.0015(10) 0.0025(11) -0.0023(11) P2 0.0279(13) 0.0388(14) 0.0307(13) -0.0022(10) 0.0024(10) -0.0034(10) Br2 0.0487(7) 0.0588(7) 0.0629(7) -0.0099(5) 0.0032(6) 0.0113(5) Br1 0.0535(7) 0.0671(8) 0.0846(9) 0.0257(6) 0.0245(6) -0.0068(6) Br4 0.0602(7) 0.0477(7) 0.0588(7) 0.0116(5) -0.0069(6) -0.0103(5) Br3 0.0351(6) 0.0679(7) 0.0460(6) -0.0012(5) -0.0094(5) -0.0018(5) C1 0.042(6) 0.031(5) 0.039(5) -0.005(4) 0.011(5) 0.002(4) C2 0.053(7) 0.046(6) 0.039(6) 0.002(5) 0.007(5) -0.005(5) C3 0.064(8) 0.048(7) 0.062(7) -0.001(6) -0.003(6) -0.023(6) C4 0.077(9) 0.058(8) 0.049(7) -0.018(5) -0.004(6) -0.018(6) C5 0.079(9) 0.064(8) 0.040(6) -0.019(5) 0.011(6) 0.000(7) C6 0.059(7) 0.042(6) 0.050(7) -0.004(5) 0.008(6) 0.000(5) C7 0.047(6) 0.035(6) 0.035(5) 0.004(4) -0.007(5) 0.000(5) C8 0.064(7) 0.045(6) 0.044(6) 0.003(5) 0.007(5) 0.011(5) C9 0.084(10) 0.051(8) 0.075(9) 0.004(6) -0.007(7) 0.008(6) C10 0.064(8) 0.054(8) 0.083(9) 0.041(7) -0.022(7) -0.023(6) C11 0.055(7) 0.061(8) 0.050(7) 0.019(6) -0.008(5) -0.018(6) C12 0.051(7) 0.044(6) 0.054(7) 0.001(5) 0.005(5) -0.005(5) C13 0.030(5) 0.036(5) 0.035(5) -0.004(4) 0.001(4) -0.001(4) C14 0.050(7) 0.077(8) 0.054(7) 0.009(6) -0.005(6) -0.012(6) C15 0.051(8) 0.085(10) 0.083(10) 0.012(7) -0.018(7) -0.021(7) C16 0.034(7) 0.107(11) 0.109(11) 0.021(9) 0.002(7) -0.046(7) C17 0.071(9) 0.050(7) 0.058(7) 0.006(5) 0.030(7) -0.012(6) C18 0.041(6) 0.056(7) 0.043(6) -0.008(5) 0.007(5) -0.013(5) C19 0.037(6) 0.052(7) 0.030(5) -0.006(5) -0.004(4) 0.003(5) C20 0.025(5) 0.054(6) 0.028(5) -0.008(4) 0.005(4) 0.005(4) C21 0.025(5) 0.043(6) 0.053(6) -0.005(5) 0.017(5) -0.006(4) C22 0.050(7) 0.044(7) 0.101(10) -0.025(7) 0.008(7) -0.011(6) C23 0.065(9) 0.039(8) 0.169(16) -0.053(10) 0.021(10) -0.005(7) C24 0.092(11) 0.037(8) 0.149(15) 0.010(9) 0.051(11) -0.014(7) C25 0.082(9) 0.047(7) 0.067(8) 0.014(6) 0.036(7) 0.020(7) C26 0.042(6) 0.025(5) 0.061(7) 0.004(5) 0.010(5) 0.001(4) C27 0.033(5) 0.027(5) 0.038(5) -0.002(4) -0.006(4) 0.000(4) C28 0.032(6) 0.074(8) 0.070(8) 0.006(6) 0.005(6) 0.003(5) C29 0.057(8) 0.073(9) 0.099(11) -0.010(7) -0.036(8) -0.006(7) C30 0.069(9) 0.048(7) 0.052(7) -0.006(5) -0.001(6) 0.007(6) C31 0.057(7) 0.040(6) 0.050(6) -0.010(5) -0.001(6) -0.006(5) C32 0.042(6) 0.034(6) 0.047(6) 0.001(4) -0.001(5) -0.005(4) C33 0.090(11) 0.114(12) 0.064(8) -0.030(8) -0.033(8) 0.000(9) C34 0.032(6) 0.043(6) 0.037(5) -0.007(4) -0.004(4) -0.007(4) C35 0.036(6) 0.041(6) 0.055(7) -0.005(5) 0.009(5) -0.018(5) C36 0.040(7) 0.063(8) 0.081(9) -0.011(7) 0.019(6) -0.007(6) C37 0.055(8) 0.086(9) 0.042(7) -0.011(6) 0.016(6) -0.027(7) C38 0.057(8) 0.099(10) 0.043(7) 0.012(6) 0.016(6) -0.020(7) C39 0.043(6) 0.064(7) 0.051(7) 0.002(5) -0.003(5) 0.009(5) C40 0.034(5) 0.046(6) 0.034(5) -0.022(4) 0.010(4) -0.010(4) C41 0.053(7) 0.057(7) 0.048(6) -0.018(5) 0.000(5) -0.015(5) C42 0.047(7) 0.065(8) 0.087(9) -0.020(7) 0.017(7) -0.016(6) C43 0.056(8) 0.081(10) 0.080(10) -0.044(8) 0.009(7) -0.027(7) C44 0.069(9) 0.118(13) 0.047(7) -0.034(7) 0.002(6) -0.014(8) C45 0.053(7) 0.070(8) 0.041(6) -0.015(5) -0.006(5) 0.008(6) C46 0.025(5) 0.043(6) 0.034(5) 0.004(4) 0.000(4) -0.003(4) C47 0.049(7) 0.050(6) 0.037(6) -0.003(5) 0.003(5) 0.007(5) C48 0.046(7) 0.073(8) 0.069(8) -0.006(6) 0.012(6) 0.018(6) C49 0.026(6) 0.062(7) 0.080(9) 0.007(6) 0.000(6) -0.003(5) C50 0.044(7) 0.070(8) 0.047(6) 0.006(6) 0.000(5) -0.010(6) C51 0.029(5) 0.044(6) 0.037(5) 0.001(4) 0.002(4) 0.004(4) C52 0.061(7) 0.032(5) 0.021(5) 0.006(4) -0.003(5) -0.005(5) C53 0.034(5) 0.040(6) 0.032(5) 0.000(4) 0.005(4) -0.004(4) C54 0.027(5) 0.040(5) 0.024(5) 0.005(4) 0.001(4) -0.003(4) C55 0.037(6) 0.039(6) 0.043(6) 0.005(4) 0.008(5) 0.003(4) C56 0.021(5) 0.054(7) 0.066(7) 0.002(5) -0.005(5) -0.006(4) C57 0.050(8) 0.077(9) 0.060(8) 0.004(6) -0.015(6) -0.009(6) C58 0.057(7) 0.066(7) 0.019(5) -0.009(4) -0.004(5) -0.005(6) C59 0.031(5) 0.034(5) 0.031(5) -0.001(4) 0.000(4) -0.014(4) C60 0.027(5) 0.061(7) 0.041(6) -0.015(5) 0.000(4) -0.005(5) C61 0.094(10) 0.054(8) 0.081(9) -0.023(7) -0.012(8) 0.019(7) C62 0.088(11) 0.083(11) 0.125(14) -0.063(11) -0.011(10) 0.042(9) C63 0.044(8) 0.20(2) 0.088(12) -0.080(14) 0.006(8) 0.018(11) C64 0.061(9) 0.165(17) 0.048(8) -0.037(9) 0.009(7) -0.010(10) C65 0.067(8) 0.082(9) 0.041(7) -0.013(6) 0.018(6) -0.011(7) C66 0.102(14) 0.28(3) 0.112(14) -0.124(16) 0.019(11) 0.030(15) O99 0.17(2) 0.63(5) 0.130(15) -0.16(2) -0.082(14) 0.18(2) C99 0.14(2) 0.30(3) 0.052(10) -0.045(15) -0.049(12) 0.10(2) _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 N1 1.692(7) . ? Re1 O1 2.086(6) . ? Re1 N2 2.100(7) . ? Re1 P1 2.443(2) . ? Re1 Br1 2.4949(11) . ? Re1 Br2 2.5677(11) . ? Re2 N5 1.698(7) . ? Re2 O3 2.081(6) . ? Re2 N4 2.092(7) . ? Re2 P2 2.450(2) . ? Re2 Br3 2.5113(10) . ? Re2 Br4 2.5425(11) . ? N2 C20 1.330(10) . ? N2 N3 1.366(9) . ? N1 C27 1.401(10) . ? N3 C26 1.360(11) . ? N3 H3 0.8600 . ? N4 C53 1.328(11) . ? N4 N6 1.334(8) . ? N5 C60 1.424(11) . ? N6 C59 1.370(11) . ? N6 H6 0.8600 . ? O1 C19 1.318(11) . ? O2 C19 1.219(10) . ? O3 C52 1.318(12) . ? O4 C52 1.217(11) . ? P1 C7 1.808(9) . ? P1 C1 1.810(9) . ? P1 C13 1.811(9) . ? P2 C34 1.819(10) . ? P2 C46 1.823(9) . ? P2 C40 1.828(8) . ? C1 C6 1.370(13) . ? C1 C2 1.406(13) . ? C2 C3 1.382(13) . ? C2 H2 0.9300 . ? C3 C4 1.360(14) . ? C3 H3A 0.9300 . ? C4 C5 1.347(15) . ? C4 H4 0.9300 . ? C5 C6 1.383(13) . ? C5 H5 0.9300 . ? C6 H6A 0.9300 . ? C7 C8 1.370(13) . ? C7 C12 1.402(13) . ? C8 C9 1.385(14) . ? C8 H8 0.9300 . ? C9 C10 1.347(16) . ? C9 H9 0.9300 . ? C10 C11 1.380(16) . ? C10 H10 0.9300 . ? C11 C12 1.387(14) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.363(13) . ? C13 C18 1.417(13) . ? C14 C15 1.401(15) . ? C14 H14 0.9300 . ? C15 C16 1.341(16) . ? C15 H15 0.9300 . ? C16 C17 1.365(16) . ? C16 H16 0.9300 . ? C17 C18 1.352(14) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.463(13) . ? C20 C21 1.398(13) . ? C21 C22 1.380(13) . ? C21 C26 1.408(13) . ? C22 C23 1.375(19) . ? C22 H22 0.9300 . ? C23 C24 1.382(19) . ? C23 H23 0.9300 . ? C24 C25 1.345(18) . ? C24 H24 0.9300 . ? C25 C26 1.401(14) . ? C25 H25 0.9300 . ? C27 C32 1.361(12) . ? C27 C28 1.374(13) . ? C28 C29 1.385(14) . ? C28 H28 0.9300 . ? C29 C30 1.348(16) . ? C29 H29 0.9300 . ? C30 C31 1.365(15) . ? C30 C33 1.520(14) . ? C31 C32 1.379(12) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C39 1.383(13) . ? C34 C35 1.396(13) . ? C35 C36 1.366(14) . ? C35 H35 0.9300 . ? C36 C37 1.376(15) . ? C36 H36 0.9300 . ? C37 C38 1.354(16) . ? C37 H37 0.9300 . ? C38 C39 1.387(14) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C45 1.375(13) . ? C40 C41 1.410(14) . ? C41 C42 1.384(14) . ? C41 H41 0.9300 . ? C42 C43 1.355(16) . ? C42 H42 0.9300 . ? C43 C44 1.373(18) . ? C43 H43 0.9300 . ? C44 C45 1.425(15) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 C47 1.381(12) . ? C46 C51 1.391(11) . ? C47 C48 1.390(14) . ? C47 H47 0.9300 . ? C48 C49 1.375(14) . ? C48 H48 0.9300 . ? C49 C50 1.343(15) . ? C49 H49 0.9300 . ? C50 C51 1.384(13) . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? C52 C53 1.489(12) . ? C53 C54 1.414(12) . ? C54 C55 1.402(12) . ? C54 C59 1.403(11) . ? C55 C56 1.388(12) . ? C55 H55 0.9300 . ? C56 C57 1.393(14) . ? C56 H56 0.9300 . ? C57 C58 1.364(14) . ? C57 H57 0.9300 . ? C58 C59 1.400(12) . ? C58 H58 0.9300 . ? C60 C65 1.359(14) . ? C60 C61 1.372(15) . ? C61 C62 1.385(18) . ? C61 H61 0.9300 . ? C62 C63 1.37(2) . ? C62 H62 0.9300 . ? C63 C64 1.34(2) . ? C63 C66 1.521(18) . ? C64 C65 1.384(16) . ? C64 H64 0.9300 . ? C65 H65 0.9300 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? O99 C99 1.81(3) . ? O99 H99 0.8200 . ? C99 H99A 0.9600 . ? C99 H99B 0.9600 . ? C99 H99C 0.9600 . ? 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 N1 Re1 O1 171.4(3) . . ? N1 Re1 N2 98.8(3) . . ? O1 Re1 N2 74.0(2) . . ? N1 Re1 P1 92.8(2) . . ? O1 Re1 P1 83.10(19) . . ? N2 Re1 P1 93.4(2) . . ? N1 Re1 Br1 97.1(2) . . ? O1 Re1 Br1 90.60(18) . . ? N2 Re1 Br1 162.98(18) . . ? P1 Re1 Br1 91.97(6) . . ? N1 Re1 Br2 97.1(2) . . ? O1 Re1 Br2 86.97(18) . . ? N2 Re1 Br2 84.4(2) . . ? P1 Re1 Br2 170.05(6) . . ? Br1 Re1 Br2 87.54(4) . . ? N5 Re2 O3 166.5(3) . . ? N5 Re2 N4 92.5(3) . . ? O3 Re2 N4 74.1(2) . . ? N5 Re2 P2 97.8(3) . . ? O3 Re2 P2 80.57(18) . . ? N4 Re2 P2 91.07(19) . . ? N5 Re2 Br3 98.5(2) . . ? O3 Re2 Br3 95.04(15) . . ? N4 Re2 Br3 167.87(18) . . ? P2 Re2 Br3 92.48(6) . . ? N5 Re2 Br4 97.9(3) . . ? O3 Re2 Br4 83.96(17) . . ? N4 Re2 Br4 87.28(18) . . ? P2 Re2 Br4 164.29(6) . . ? Br3 Re2 Br4 86.17(4) . . ? C20 N2 N3 108.2(7) . . ? C20 N2 Re1 117.8(6) . . ? N3 N2 Re1 132.8(5) . . ? C27 N1 Re1 175.8(6) . . ? C26 N3 N2 108.8(7) . . ? C26 N3 H3 125.6 . . ? N2 N3 H3 125.6 . . ? C53 N4 N6 108.3(7) . . ? C53 N4 Re2 119.0(5) . . ? N6 N4 Re2 132.5(6) . . ? C60 N5 Re2 168.5(6) . . ? N4 N6 C59 109.2(7) . . ? N4 N6 H6 125.4 . . ? C59 N6 H6 125.4 . . ? C19 O1 Re1 119.9(5) . . ? C52 O3 Re2 120.4(5) . . ? C7 P1 C1 101.0(4) . . ? C7 P1 C13 105.1(4) . . ? C1 P1 C13 106.9(4) . . ? C7 P1 Re1 120.0(3) . . ? C1 P1 Re1 110.6(3) . . ? C13 P1 Re1 112.0(3) . . ? C34 P2 C46 106.4(4) . . ? C34 P2 C40 104.6(4) . . ? C46 P2 C40 103.7(4) . . ? C34 P2 Re2 112.3(3) . . ? C46 P2 Re2 109.9(3) . . ? C40 P2 Re2 119.0(3) . . ? C6 C1 C2 119.1(9) . . ? C6 C1 P1 124.5(8) . . ? C2 C1 P1 116.4(7) . . ? C3 C2 C1 119.0(10) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C4 C3 C2 121.2(10) . . ? C4 C3 H3A 119.4 . . ? C2 C3 H3A 119.4 . . ? C5 C4 C3 119.2(10) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 121.9(11) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C1 C6 C5 119.5(10) . . ? C1 C6 H6A 120.3 . . ? C5 C6 H6A 120.3 . . ? C8 C7 C12 118.6(9) . . ? C8 C7 P1 120.1(7) . . ? C12 C7 P1 121.3(7) . . ? C7 C8 C9 121.2(10) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C10 C9 C8 120.0(11) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 120.7(10) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C10 C11 C12 119.9(11) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C11 C12 C7 119.6(10) . . ? C11 C12 H12 120.2 . . ? C7 C12 H12 120.2 . . ? C14 C13 C18 118.2(9) . . ? C14 C13 P1 121.5(7) . . ? C18 C13 P1 120.2(7) . . ? C13 C14 C15 120.3(10) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C16 C15 C14 120.4(11) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 120.0(10) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C18 C17 C16 121.4(10) . . ? C18 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C17 C18 C13 119.7(10) . . ? C17 C18 H18 120.1 . . ? C13 C18 H18 120.1 . . ? O2 C19 O1 124.7(9) . . ? O2 C19 C20 122.5(9) . . ? O1 C19 C20 112.7(7) . . ? N2 C20 C21 110.3(8) . . ? N2 C20 C19 114.3(8) . . ? C21 C20 C19 135.4(9) . . ? C22 C21 C20 136.5(11) . . ? C22 C21 C26 118.9(10) . . ? C20 C21 C26 104.6(8) . . ? C23 C22 C21 117.2(12) . . ? C23 C22 H22 121.4 . . ? C21 C22 H22 121.4 . . ? C22 C23 C24 122.3(12) . . ? C22 C23 H23 118.8 . . ? C24 C23 H23 118.8 . . ? C25 C24 C23 123.0(13) . . ? C25 C24 H24 118.5 . . ? C23 C24 H24 118.5 . . ? C24 C25 C26 114.8(12) . . ? C24 C25 H25 122.6 . . ? C26 C25 H25 122.6 . . ? N3 C26 C25 128.0(10) . . ? N3 C26 C21 108.1(8) . . ? C25 C26 C21 123.6(10) . . ? C32 C27 C28 119.9(9) . . ? C32 C27 N1 122.1(8) . . ? C28 C27 N1 118.0(9) . . ? C27 C28 C29 118.4(11) . . ? C27 C28 H28 120.8 . . ? C29 C28 H28 120.8 . . ? C30 C29 C28 122.6(12) . . ? C30 C29 H29 118.7 . . ? C28 C29 H29 118.7 . . ? C29 C30 C31 117.7(11) . . ? C29 C30 C33 121.4(12) . . ? C31 C30 C33 120.9(11) . . ? C30 C31 C32 121.6(10) . . ? C30 C31 H31 119.2 . . ? C32 C31 H31 119.2 . . ? C27 C32 C31 119.7(9) . . ? C27 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C39 C34 C35 120.2(9) . . ? C39 C34 P2 121.9(8) . . ? C35 C34 P2 117.9(7) . . ? C36 C35 C34 118.1(10) . . ? C36 C35 H35 120.9 . . ? C34 C35 H35 120.9 . . ? C35 C36 C37 122.5(11) . . ? C35 C36 H36 118.7 . . ? C37 C36 H36 118.7 . . ? C38 C37 C36 118.6(11) . . ? C38 C37 H37 120.7 . . ? C36 C37 H37 120.7 . . ? C37 C38 C39 121.4(11) . . ? C37 C38 H38 119.3 . . ? C39 C38 H38 119.3 . . ? C34 C39 C38 119.1(10) . . ? C34 C39 H39 120.5 . . ? C38 C39 H39 120.5 . . ? C45 C40 C41 120.2(8) . . ? C45 C40 P2 123.1(8) . . ? C41 C40 P2 116.7(7) . . ? C42 C41 C40 119.7(10) . . ? C42 C41 H41 120.2 . . ? C40 C41 H41 120.2 . . ? C43 C42 C41 120.9(12) . . ? C43 C42 H42 119.5 . . ? C41 C42 H42 119.5 . . ? C42 C43 C44 120.1(11) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C43 C44 C45 121.0(12) . . ? C43 C44 H44 119.5 . . ? C45 C44 H44 119.5 . . ? C40 C45 C44 118.1(11) . . ? C40 C45 H45 121.0 . . ? C44 C45 H45 121.0 . . ? C47 C46 C51 119.0(8) . . ? C47 C46 P2 120.1(7) . . ? C51 C46 P2 120.5(7) . . ? C46 C47 C48 120.0(9) . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C49 C48 C47 119.9(10) . . ? C49 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? C50 C49 C48 120.3(10) . . ? C50 C49 H49 119.8 . . ? C48 C49 H49 119.8 . . ? C49 C50 C51 121.0(10) . . ? C49 C50 H50 119.5 . . ? C51 C50 H50 119.5 . . ? C50 C51 C46 119.8(9) . . ? C50 C51 H51 120.1 . . ? C46 C51 H51 120.1 . . ? O4 C52 O3 125.6(8) . . ? O4 C52 C53 122.3(9) . . ? O3 C52 C53 112.0(9) . . ? N4 C53 C54 110.8(7) . . ? N4 C53 C52 113.4(8) . . ? C54 C53 C52 135.7(9) . . ? C55 C54 C59 120.1(8) . . ? C55 C54 C53 136.9(8) . . ? C59 C54 C53 103.0(7) . . ? C56 C55 C54 116.3(9) . . ? C56 C55 H55 121.9 . . ? C54 C55 H55 121.9 . . ? C55 C56 C57 122.5(9) . . ? C55 C56 H56 118.7 . . ? C57 C56 H56 118.7 . . ? C58 C57 C56 122.3(9) . . ? C58 C57 H57 118.8 . . ? C56 C57 H57 118.8 . . ? C57 C58 C59 115.8(9) . . ? C57 C58 H58 122.1 . . ? C59 C58 H58 122.1 . . ? N6 C59 C58 128.4(8) . . ? N6 C59 C54 108.6(7) . . ? C58 C59 C54 123.0(8) . . ? C65 C60 C61 122.2(10) . . ? C65 C60 N5 120.7(10) . . ? C61 C60 N5 117.0(10) . . ? C60 C61 C62 116.4(13) . . ? C60 C61 H61 121.8 . . ? C62 C61 H61 121.8 . . ? C63 C62 C61 123.4(14) . . ? C63 C62 H62 118.3 . . ? C61 C62 H62 118.3 . . ? C64 C63 C62 117.1(14) . . ? C64 C63 C66 123(2) . . ? C62 C63 C66 120(2) . . ? C63 C64 C65 123.1(16) . . ? C63 C64 H64 118.5 . . ? C65 C64 H64 118.5 . . ? C60 C65 C64 117.8(13) . . ? C60 C65 H65 121.1 . . ? C64 C65 H65 121.1 . . ? C63 C66 H66A 109.5 . . ? C63 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C63 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C99 O99 H99 109.5 . . ? O99 C99 H99A 109.5 . . ? O99 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? O99 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3 O4 0.86 1.99 2.753(9) 147.6 . N6 H6 O2 0.86 2.15 2.802(9) 132.7 4_575 C12 H12 O1 0.93 2.53 3.304(12) 141.1 . C23 H23 Br1 0.93 2.87 3.642(12) 141.0 2_656 C37 H37 Br1 0.93 2.89 3.753(11) 154.8 4_675 C45 H45 Br3 0.93 2.75 3.382(11) 126.1 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.874 _refine_diff_density_min -1.200 _refine_diff_density_rms 0.176 _database_code_depnum_ccdc_archive 'CCDC 973299' data_added_by_encifer _publ_section_references ;CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET) Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. Flack. H. D. (1983). Acta Cryst. A39, 876--881. Sheldrick, G. M. (1990a). Acta Cryst. A46, 467--473. Sheldrick, G. M. (1990b). SHELXTL/PC Software. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany Spek, A. L. (1990). Acta Cryst. A46, C-34. UNIL IC & KUMA (2000). CrysAlis CCD. Version 1.163. Kuma Diffraction Instruments GmbH, Wroc\/law, Poland. UNIL IC & KUMA (2000). CrysAlis RED. Version 1.163. Kuma Diffraction Instruments GmbH, Wroc\/law, Poland. ; data_ren406 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C33 H27 Br2 N3 O2 P Re), C2 H3 N' _chemical_formula_sum 'C68 H57 Br4 N7 O4 P2 Re2' _chemical_formula_weight 1790.19 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' Br Br -0.2901 2.4595 '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.1434(3) _cell_length_b 21.1471(6) _cell_length_c 28.1174(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.062(2) _cell_angle_gamma 90.00 _cell_volume 6624.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12882 _cell_measurement_theta_min 3.8780 _cell_measurement_theta_max 28.9190 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.25975 _exptl_crystal_size_mid 0.05336 _exptl_crystal_size_min 0.02643 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.795 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3464 _exptl_absorpt_coefficient_mu 6.165 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ;CrysAlis RED, (2005) ; _exptl_absorpt_correction_T_min 0.29354 _exptl_absorpt_correction_T_max 1.00000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _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 39796 _diffrn_reflns_av_R_equivalents 0.0633 _diffrn_reflns_av_unetI/netI 0.0659 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11642 _reflns_number_gt 8962 _reflns_threshold_expression >2sigma(I) #========================================================================== # # REFINEMENT DATA _computing_data_collection 'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)' _computing_cell_refinement 'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)' _computing_data_reduction 'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ;XP in SHELXTL/PC (Sheldrick, 1990b) ORTEP-3 W v. 1.062 (Farrugia 1997) ; _computing_publication_material ;SHELXL-97 (Sheldrick, 1997) and PLATON (Spek, 1990) ; _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^)+(0.0345P)^2^+1.2787P] 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 11642 _refine_ls_number_parameters 787 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.0888 _refine_ls_wR_factor_gt 0.0830 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 0.78344(2) 0.734675(12) 0.462441(7) 0.02989(8) Uani 1 1 d . . . Re2 Re 0.40106(2) 0.662415(12) 0.702947(8) 0.03380(8) Uani 1 1 d . . . Br1 Br 0.75988(7) 0.62409(3) 0.49665(2) 0.0538(2) Uani 1 1 d . . . Br2 Br 0.97444(6) 0.74093(3) 0.51100(2) 0.04811(18) Uani 1 1 d . . . Br3 Br 0.29140(7) 0.58133(4) 0.74979(3) 0.0669(2) Uani 1 1 d . . . Br4 Br 0.24437(7) 0.74327(4) 0.72993(3) 0.0550(2) Uani 1 1 d . . . P1 P 0.77850(14) 0.84926(8) 0.44977(5) 0.0315(4) Uani 1 1 d . . . P2 P 0.56861(15) 0.59032(8) 0.69017(5) 0.0330(4) Uani 1 1 d . . . O1 O 0.6716(4) 0.76018(19) 0.51802(12) 0.0359(10) Uani 1 1 d . . . O2 O 0.4838(4) 0.7576(2) 0.54623(13) 0.0445(11) Uani 1 1 d . . . O3 O 0.5024(4) 0.6881(2) 0.76335(12) 0.0414(11) Uani 1 1 d . . . O4 O 0.6132(4) 0.7635(2) 0.79876(13) 0.0572(14) Uani 1 1 d . . . N1 N 0.6082(4) 0.7256(2) 0.43595(15) 0.0287(11) Uani 1 1 d . . . N2 N 0.8440(4) 0.7138(2) 0.40915(15) 0.0341(12) Uani 1 1 d . . . N3 N 0.5620(4) 0.7089(2) 0.39334(14) 0.0316(12) Uani 1 1 d . . . H3A H 0.6039 0.6997 0.3689 0.038 Uiso 1 1 calc R . . N4 N 0.5000(5) 0.7424(2) 0.68361(14) 0.0327(12) Uani 1 1 d . . . N5 N 0.3383(4) 0.6458(2) 0.64894(17) 0.0381(13) Uani 1 1 d . . . N6 N 0.5018(5) 0.7778(2) 0.64387(16) 0.0382(13) Uani 1 1 d . . . H6A H 0.4678 0.7677 0.6172 0.046 Uiso 1 1 calc R . . C1 C 0.6269(5) 0.8748(3) 0.43440(19) 0.0322(14) Uani 1 1 d . . . C2 C 0.5750(6) 0.8587(3) 0.3905(2) 0.0389(15) Uani 1 1 d . . . H2 H 0.6213 0.8394 0.3674 0.047 Uiso 1 1 calc R . . C3 C 0.4564(6) 0.8713(3) 0.3812(2) 0.0460(17) Uani 1 1 d . . . H3 H 0.4224 0.8604 0.3519 0.055 Uiso 1 1 calc R . . C4 C 0.3868(6) 0.9001(3) 0.4152(3) 0.0548(19) Uani 1 1 d . . . H4 H 0.3061 0.9083 0.4089 0.066 Uiso 1 1 calc R . . C5 C 0.4371(7) 0.9166(4) 0.4582(3) 0.058(2) Uani 1 1 d . . . H5 H 0.3906 0.9365 0.4809 0.069 Uiso 1 1 calc R . . C6 C 0.5562(6) 0.9038(3) 0.4681(2) 0.0424(16) Uani 1 1 d . . . H6 H 0.5894 0.9148 0.4976 0.051 Uiso 1 1 calc R . . C7 C 0.8241(5) 0.9019(3) 0.4983(2) 0.0394(16) Uani 1 1 d . . . C8 C 0.8523(6) 0.8811(4) 0.5433(2) 0.0540(19) Uani 1 1 d . . . H8 H 0.8456 0.8384 0.5509 0.065 Uiso 1 1 calc R . . C9 C 0.8913(7) 0.9245(5) 0.5779(3) 0.072(3) Uani 1 1 d . . . H9 H 0.9123 0.9104 0.6083 0.087 Uiso 1 1 calc R . . C10 C 0.8985(7) 0.9870(5) 0.5676(3) 0.073(3) Uani 1 1 d . . . H10 H 0.9256 1.0153 0.5906 0.088 Uiso 1 1 calc R . . C11 C 0.8666(7) 1.0081(4) 0.5238(3) 0.064(2) Uani 1 1 d . . . H11 H 0.8697 1.0512 0.5173 0.077 Uiso 1 1 calc R . . C12 C 0.8293(6) 0.9663(4) 0.4886(2) 0.0523(19) Uani 1 1 d . . . H12 H 0.8077 0.9813 0.4585 0.063 Uiso 1 1 calc R . . C13 C 0.8742(6) 0.8734(3) 0.4010(2) 0.0365(15) Uani 1 1 d . . . C14 C 0.8373(6) 0.9194(3) 0.3687(2) 0.0482(18) Uani 1 1 d . . . H14 H 0.7628 0.9386 0.3718 0.058 Uiso 1 1 calc R . . C15 C 0.9110(7) 0.9367(4) 0.3318(2) 0.062(2) Uani 1 1 d . . . H15 H 0.8868 0.9679 0.3104 0.074 Uiso 1 1 calc R . . C16 C 1.0192(8) 0.9075(4) 0.3270(3) 0.064(2) Uani 1 1 d . . . H16 H 1.0675 0.9180 0.3016 0.077 Uiso 1 1 calc R . . C17 C 1.0578(7) 0.8632(4) 0.3592(3) 0.062(2) Uani 1 1 d . . . H17 H 1.1330 0.8446 0.3562 0.074 Uiso 1 1 calc R . . C18 C 0.9847(6) 0.8461(3) 0.3963(2) 0.0442(17) Uani 1 1 d . . . H18 H 1.0108 0.8158 0.4181 0.053 Uiso 1 1 calc R . . C19 C 0.5550(6) 0.7514(3) 0.51388(19) 0.0351(15) Uani 1 1 d . . . C20 C 0.5172(5) 0.7338(3) 0.46527(18) 0.0302(14) Uani 1 1 d . . . C21 C 0.4073(5) 0.7238(3) 0.44109(19) 0.0303(14) Uani 1 1 d . . . C22 C 0.2845(6) 0.7274(3) 0.4516(2) 0.0418(16) Uani 1 1 d . . . H22 H 0.2594 0.7381 0.4819 0.050 Uiso 1 1 calc R . . C23 C 0.2027(6) 0.7147(3) 0.4157(2) 0.0536(19) Uani 1 1 d . . . H23 H 0.1213 0.7157 0.4223 0.064 Uiso 1 1 calc R . . C24 C 0.2389(6) 0.7003(4) 0.3694(2) 0.059(2) Uani 1 1 d . . . H24 H 0.1805 0.6930 0.3460 0.071 Uiso 1 1 calc R . . C25 C 0.3562(6) 0.6968(3) 0.3576(2) 0.0462(18) Uani 1 1 d . . . H25 H 0.3797 0.6870 0.3269 0.055 Uiso 1 1 calc R . . C26 C 0.4398(5) 0.7086(3) 0.39413(19) 0.0322(14) Uani 1 1 d . . . C27 C 0.8789(6) 0.6863(3) 0.3668(2) 0.0431(17) Uani 1 1 d . . . C28 C 0.9069(8) 0.6228(4) 0.3669(3) 0.073(2) Uani 1 1 d . . . H28 H 0.9009 0.5994 0.3947 0.088 Uiso 1 1 calc R . . C29 C 0.9437(9) 0.5942(5) 0.3259(4) 0.106(4) Uani 1 1 d . . . H29 H 0.9628 0.5514 0.3260 0.128 Uiso 1 1 calc R . . C30 C 0.9527(9) 0.6289(7) 0.2842(4) 0.103(4) Uani 1 1 d . . . C31 C 0.9262(8) 0.6904(6) 0.2849(3) 0.088(3) Uani 1 1 d . . . H31 H 0.9339 0.7137 0.2570 0.106 Uiso 1 1 calc R . . C32 C 0.8878(7) 0.7207(4) 0.3254(2) 0.061(2) Uani 1 1 d . . . H32 H 0.8684 0.7635 0.3247 0.074 Uiso 1 1 calc R . . C33 C 0.9937(10) 0.5957(7) 0.2386(4) 0.187(8) Uani 1 1 d . . . H33A H 0.9650 0.5529 0.2383 0.281 Uiso 1 1 calc R . . H33B H 1.0798 0.5957 0.2378 0.281 Uiso 1 1 calc R . . H33C H 0.9619 0.6178 0.2113 0.281 Uiso 1 1 calc R . . C34 C 0.6053(6) 0.5301(3) 0.73477(19) 0.0372(15) Uani 1 1 d . . . C35 C 0.6550(7) 0.4737(3) 0.7206(2) 0.0543(19) Uani 1 1 d . . . H35 H 0.6722 0.4674 0.6887 0.065 Uiso 1 1 calc R . . C36 C 0.6796(8) 0.4265(4) 0.7530(3) 0.068(2) Uani 1 1 d . . . H36 H 0.7123 0.3883 0.7431 0.082 Uiso 1 1 calc R . . C37 C 0.6557(7) 0.4363(4) 0.7995(3) 0.066(2) Uani 1 1 d . . . H37 H 0.6720 0.4043 0.8214 0.079 Uiso 1 1 calc R . . C38 C 0.6080(6) 0.4921(4) 0.8149(2) 0.0491(18) Uani 1 1 d . . . H38 H 0.5926 0.4985 0.8469 0.059 Uiso 1 1 calc R . . C39 C 0.5833(6) 0.5388(3) 0.7818(2) 0.0449(17) Uani 1 1 d . . . H39 H 0.5509 0.5770 0.7918 0.054 Uiso 1 1 calc R . . C40 C 0.5400(6) 0.5415(3) 0.6380(2) 0.0363(15) Uani 1 1 d . . . C41 C 0.4388(7) 0.5033(3) 0.6382(2) 0.0475(18) Uani 1 1 d . . . H41 H 0.3875 0.5045 0.6639 0.057 Uiso 1 1 calc R . . C42 C 0.4146(7) 0.4638(3) 0.6007(3) 0.057(2) Uani 1 1 d . . . H42 H 0.3464 0.4385 0.6009 0.069 Uiso 1 1 calc R . . C43 C 0.4902(8) 0.4614(3) 0.5628(3) 0.060(2) Uani 1 1 d . . . H43 H 0.4743 0.4339 0.5377 0.072 Uiso 1 1 calc R . . C44 C 0.5882(8) 0.4994(4) 0.5620(2) 0.061(2) Uani 1 1 d . . . H44 H 0.6379 0.4985 0.5358 0.074 Uiso 1 1 calc R . . C45 C 0.6150(6) 0.5393(3) 0.5997(2) 0.0466(17) Uani 1 1 d . . . H45 H 0.6834 0.5645 0.5991 0.056 Uiso 1 1 calc R . . C46 C 0.7089(6) 0.6324(3) 0.6806(2) 0.0348(15) Uani 1 1 d . . . C47 C 0.8027(7) 0.6285(4) 0.7122(2) 0.060(2) Uani 1 1 d . . . H47 H 0.7972 0.6025 0.7388 0.072 Uiso 1 1 calc R . . C48 C 0.9061(8) 0.6631(5) 0.7049(3) 0.083(3) Uani 1 1 d . . . H48 H 0.9694 0.6606 0.7269 0.099 Uiso 1 1 calc R . . C49 C 0.9163(7) 0.7006(4) 0.6662(3) 0.071(2) Uani 1 1 d . . . H49 H 0.9868 0.7231 0.6614 0.085 Uiso 1 1 calc R . . C50 C 0.8234(7) 0.7053(3) 0.6344(3) 0.058(2) Uani 1 1 d . . . H50 H 0.8302 0.7311 0.6078 0.070 Uiso 1 1 calc R . . C51 C 0.7193(6) 0.6719(3) 0.6414(2) 0.0439(17) Uani 1 1 d . . . H51 H 0.6556 0.6758 0.6198 0.053 Uiso 1 1 calc R . . C52 C 0.5610(6) 0.7414(3) 0.76434(19) 0.0390(16) Uani 1 1 d . . . C53 C 0.5585(6) 0.7737(3) 0.71728(19) 0.0356(15) Uani 1 1 d . . . C54 C 0.6013(6) 0.8310(3) 0.6996(2) 0.0408(16) Uani 1 1 d . . . C55 C 0.6660(7) 0.8826(4) 0.7193(3) 0.061(2) Uani 1 1 d . . . H55 H 0.6926 0.8834 0.7508 0.073 Uiso 1 1 calc R . . C56 C 0.6864(8) 0.9316(4) 0.6881(4) 0.083(3) Uani 1 1 d . . . H56 H 0.7270 0.9672 0.6994 0.100 Uiso 1 1 calc R . . C57 C 0.6495(9) 0.9304(4) 0.6407(4) 0.085(3) Uani 1 1 d . . . H57 H 0.6676 0.9647 0.6214 0.102 Uiso 1 1 calc R . . C58 C 0.5886(8) 0.8816(4) 0.6218(3) 0.066(2) Uani 1 1 d . . . H58 H 0.5636 0.8814 0.5900 0.080 Uiso 1 1 calc R . . C59 C 0.5648(6) 0.8315(3) 0.6519(2) 0.0416(17) Uani 1 1 d . . . C60 C 0.2816(6) 0.6272(3) 0.6063(2) 0.0414(16) Uani 1 1 d . . . C61 C 0.1624(7) 0.6091(4) 0.6076(3) 0.062(2) Uani 1 1 d . . . H61 H 0.1213 0.6097 0.6361 0.074 Uiso 1 1 calc R . . C62 C 0.1059(7) 0.5902(4) 0.5663(3) 0.071(2) Uani 1 1 d . . . H62 H 0.0255 0.5784 0.5668 0.085 Uiso 1 1 calc R . . C63 C 0.1656(8) 0.5883(4) 0.5243(3) 0.059(2) Uani 1 1 d . . . C64 C 0.2836(7) 0.6063(3) 0.5237(2) 0.0530(19) Uani 1 1 d . . . H64 H 0.3248 0.6053 0.4952 0.064 Uiso 1 1 calc R . . C65 C 0.3419(7) 0.6257(3) 0.5647(2) 0.0488(18) Uani 1 1 d . . . H65 H 0.4221 0.6378 0.5640 0.059 Uiso 1 1 calc R . . C66 C 0.1021(9) 0.5673(5) 0.4785(3) 0.093(3) Uani 1 1 d . . . H66A H 0.1071 0.5221 0.4757 0.140 Uiso 1 1 calc R . . H66B H 0.1400 0.5866 0.4518 0.140 Uiso 1 1 calc R . . H66C H 0.0194 0.5798 0.4791 0.140 Uiso 1 1 calc R . . N99 N 0.2830(13) 0.9108(6) 0.5763(4) 0.153(5) Uani 1 1 d . . . C99 C 0.1983(11) 0.8031(6) 0.5960(4) 0.128(4) Uani 1 1 d . . . H99A H 0.2400 0.7705 0.5793 0.192 Uiso 1 1 calc R . . H99B H 0.1146 0.8019 0.5873 0.192 Uiso 1 1 calc R . . H99C H 0.2076 0.7965 0.6296 0.192 Uiso 1 1 calc R . . C98 C 0.2461(13) 0.8626(7) 0.5839(4) 0.104(4) 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 Re1 0.02748(15) 0.04073(17) 0.02142(12) -0.00030(10) -0.00055(10) -0.00379(11) Re2 0.03426(16) 0.03961(17) 0.02760(13) 0.00117(10) 0.00253(11) -0.00244(12) Br1 0.0594(5) 0.0486(5) 0.0532(4) 0.0133(3) -0.0062(4) -0.0112(4) Br2 0.0333(4) 0.0714(5) 0.0392(3) -0.0021(3) -0.0091(3) -0.0012(3) Br3 0.0525(5) 0.0699(6) 0.0792(5) 0.0247(4) 0.0257(4) -0.0066(4) Br4 0.0457(5) 0.0628(5) 0.0567(4) -0.0118(4) 0.0036(4) 0.0095(4) P1 0.0276(9) 0.0416(10) 0.0253(7) -0.0040(7) 0.0022(7) -0.0056(7) P2 0.0361(10) 0.0367(10) 0.0264(7) 0.0018(7) 0.0037(7) -0.0033(8) O1 0.033(3) 0.052(3) 0.023(2) -0.0005(18) -0.0004(18) -0.008(2) O2 0.040(3) 0.070(3) 0.024(2) -0.005(2) 0.011(2) -0.007(2) O3 0.042(3) 0.062(3) 0.020(2) 0.007(2) 0.0024(18) 0.002(2) O4 0.054(3) 0.096(4) 0.021(2) -0.011(2) -0.004(2) -0.012(3) N1 0.026(3) 0.036(3) 0.024(2) 0.001(2) -0.002(2) -0.006(2) N2 0.028(3) 0.050(3) 0.025(2) 0.006(2) 0.002(2) -0.003(2) N3 0.031(3) 0.046(3) 0.017(2) -0.009(2) 0.000(2) -0.002(2) N4 0.041(3) 0.040(3) 0.017(2) 0.004(2) -0.002(2) 0.001(2) N5 0.028(3) 0.043(3) 0.043(3) -0.003(2) -0.002(2) 0.004(2) N6 0.052(4) 0.040(3) 0.023(2) 0.005(2) 0.002(2) 0.002(3) C1 0.031(4) 0.035(4) 0.032(3) 0.001(3) 0.008(3) -0.005(3) C2 0.035(4) 0.047(4) 0.035(3) 0.001(3) 0.007(3) -0.004(3) C3 0.042(4) 0.057(5) 0.039(4) 0.012(3) -0.006(3) -0.009(4) C4 0.030(4) 0.065(5) 0.069(5) 0.006(4) -0.003(4) 0.000(4) C5 0.042(5) 0.072(6) 0.060(5) -0.013(4) 0.015(4) 0.014(4) C6 0.037(4) 0.055(4) 0.035(3) -0.007(3) 0.009(3) 0.000(3) C7 0.028(4) 0.052(5) 0.038(3) -0.011(3) 0.003(3) -0.003(3) C8 0.046(5) 0.077(6) 0.038(4) -0.017(4) -0.005(3) 0.004(4) C9 0.067(6) 0.112(8) 0.038(4) -0.031(5) -0.007(4) 0.008(5) C10 0.048(5) 0.091(7) 0.080(6) -0.052(5) -0.001(4) -0.017(5) C11 0.046(5) 0.064(6) 0.082(6) -0.022(5) 0.010(4) -0.016(4) C12 0.048(5) 0.059(5) 0.050(4) -0.018(4) 0.007(3) -0.008(4) C13 0.033(4) 0.043(4) 0.034(3) -0.007(3) 0.009(3) -0.011(3) C14 0.039(4) 0.071(5) 0.035(3) 0.009(3) 0.007(3) -0.005(4) C15 0.053(5) 0.093(6) 0.040(4) 0.014(4) 0.006(4) -0.026(5) C16 0.067(6) 0.082(6) 0.044(4) -0.014(4) 0.027(4) -0.035(5) C17 0.036(4) 0.069(6) 0.081(6) -0.020(5) 0.024(4) -0.014(4) C18 0.036(4) 0.028(4) 0.068(5) -0.012(3) 0.011(4) -0.008(3) C19 0.045(4) 0.042(4) 0.019(3) 0.000(3) 0.002(3) -0.006(3) C20 0.030(4) 0.039(4) 0.022(3) 0.000(3) 0.002(3) -0.001(3) C21 0.029(4) 0.034(4) 0.027(3) 0.003(2) -0.001(3) -0.006(3) C22 0.039(4) 0.044(4) 0.042(4) 0.005(3) 0.006(3) -0.002(3) C23 0.031(4) 0.073(5) 0.056(4) 0.006(4) -0.002(3) 0.001(4) C24 0.035(5) 0.088(6) 0.054(4) 0.005(4) -0.019(4) -0.011(4) C25 0.042(4) 0.070(5) 0.026(3) -0.003(3) -0.009(3) -0.011(4) C26 0.030(4) 0.040(4) 0.026(3) 0.003(3) -0.001(3) -0.004(3) C27 0.027(4) 0.062(5) 0.040(4) -0.018(3) 0.003(3) -0.009(3) C28 0.076(6) 0.068(6) 0.076(6) -0.021(5) 0.004(5) 0.016(5) C29 0.089(8) 0.101(9) 0.129(9) -0.065(8) -0.008(7) 0.034(6) C30 0.059(7) 0.175(13) 0.076(7) -0.076(8) 0.004(5) 0.002(7) C31 0.064(6) 0.162(11) 0.040(5) -0.027(6) 0.008(4) -0.019(7) C32 0.057(5) 0.096(6) 0.031(4) -0.011(4) 0.002(3) -0.010(4) C33 0.098(10) 0.33(2) 0.132(10) -0.168(12) 0.028(8) 0.012(11) C34 0.039(4) 0.043(4) 0.030(3) 0.006(3) -0.001(3) -0.003(3) C35 0.072(5) 0.048(5) 0.042(4) 0.001(3) -0.006(4) 0.013(4) C36 0.080(6) 0.046(5) 0.078(6) 0.000(4) -0.017(5) 0.010(4) C37 0.068(6) 0.052(5) 0.077(6) 0.029(4) -0.023(5) -0.010(4) C38 0.051(5) 0.062(5) 0.034(3) 0.014(3) -0.006(3) -0.012(4) C39 0.045(4) 0.054(5) 0.035(3) 0.004(3) 0.005(3) -0.005(3) C40 0.045(4) 0.032(4) 0.032(3) 0.002(3) 0.001(3) -0.005(3) C41 0.056(5) 0.046(4) 0.041(4) -0.002(3) 0.013(3) -0.009(4) C42 0.052(5) 0.056(5) 0.064(5) -0.011(4) -0.004(4) -0.014(4) C43 0.079(6) 0.051(5) 0.050(4) -0.014(4) -0.004(4) -0.011(4) C44 0.080(6) 0.062(5) 0.042(4) -0.015(4) 0.016(4) -0.014(5) C45 0.042(4) 0.060(5) 0.038(4) -0.007(3) 0.004(3) -0.013(3) C46 0.035(4) 0.038(4) 0.032(3) -0.004(3) 0.004(3) -0.005(3) C47 0.047(5) 0.083(6) 0.049(4) 0.007(4) -0.005(4) -0.016(4) C48 0.052(6) 0.117(9) 0.079(6) 0.008(5) -0.016(5) -0.028(5) C49 0.050(5) 0.085(7) 0.079(6) 0.008(5) 0.015(5) -0.027(5) C50 0.064(6) 0.052(5) 0.059(5) 0.004(4) 0.024(4) -0.016(4) C51 0.046(4) 0.047(4) 0.039(4) -0.002(3) 0.001(3) -0.003(3) C52 0.038(4) 0.060(5) 0.020(3) -0.010(3) 0.008(3) 0.001(3) C53 0.040(4) 0.045(4) 0.022(3) -0.011(3) 0.003(3) 0.003(3) C54 0.034(4) 0.037(4) 0.053(4) -0.013(3) 0.017(3) -0.003(3) C55 0.049(5) 0.048(5) 0.087(6) -0.018(4) 0.008(4) -0.003(4) C56 0.063(6) 0.030(5) 0.158(10) -0.026(6) 0.026(7) -0.007(4) C57 0.082(7) 0.042(6) 0.132(9) 0.012(6) 0.049(7) -0.002(5) C58 0.087(7) 0.040(5) 0.074(5) 0.011(4) 0.037(5) 0.012(5) C59 0.054(5) 0.029(4) 0.041(4) 0.005(3) 0.017(3) -0.001(3) C60 0.047(4) 0.038(4) 0.039(4) -0.001(3) -0.010(3) 0.002(3) C61 0.049(5) 0.077(6) 0.059(5) -0.012(4) 0.000(4) -0.007(4) C62 0.040(5) 0.100(7) 0.072(6) -0.012(5) -0.016(4) -0.003(4) C63 0.061(6) 0.064(5) 0.052(4) 0.000(4) -0.022(4) 0.004(4) C64 0.074(6) 0.053(5) 0.032(3) 0.000(3) -0.006(4) 0.001(4) C65 0.053(5) 0.046(4) 0.048(4) 0.004(3) -0.005(4) -0.001(4) C66 0.096(8) 0.119(8) 0.065(5) -0.024(5) -0.037(5) 0.007(6) N99 0.217(14) 0.127(10) 0.115(8) 0.024(8) -0.028(8) 0.007(10) C99 0.125(11) 0.132(11) 0.125(9) -0.017(8) -0.052(8) -0.024(9) C98 0.141(12) 0.097(9) 0.072(7) -0.004(7) -0.030(7) 0.022(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 N2 1.713(4) . ? Re1 N1 2.086(5) . ? Re1 O1 2.087(4) . ? Re1 P1 2.4496(17) . ? Re1 Br2 2.5108(7) . ? Re1 Br1 2.5442(7) . ? Re2 N5 1.697(5) . ? Re2 O3 2.094(4) . ? Re2 N4 2.097(5) . ? Re2 P2 2.4421(17) . ? Re2 Br3 2.4957(8) . ? Re2 Br4 2.5685(8) . ? P1 C1 1.818(6) . ? P1 C13 1.825(6) . ? P1 C7 1.826(6) . ? P2 C40 1.817(6) . ? P2 C46 1.823(6) . ? P2 C34 1.828(6) . ? O1 C19 1.316(7) . ? O2 C19 1.225(7) . ? O3 C52 1.303(7) . ? O4 C52 1.213(7) . ? N1 C20 1.330(7) . ? N1 N3 1.342(6) . ? N2 C27 1.388(7) . ? N3 C26 1.363(7) . ? N3 H3A 0.8600 . ? N4 C53 1.317(7) . ? N4 N6 1.344(6) . ? N5 C60 1.400(7) . ? N6 C59 1.352(8) . ? N6 H6A 0.8600 . ? C1 C6 1.388(8) . ? C1 C2 1.396(8) . ? C2 C3 1.368(9) . ? C2 H2 0.9300 . ? C3 C4 1.385(9) . ? C3 H3 0.9300 . ? C4 C5 1.368(9) . ? C4 H4 0.9300 . ? C5 C6 1.378(9) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.372(9) . ? C7 C12 1.390(9) . ? C8 C9 1.401(10) . ? C8 H8 0.9300 . ? C9 C10 1.355(12) . ? C9 H9 0.9300 . ? C10 C11 1.350(11) . ? C10 H10 0.9300 . ? C11 C12 1.387(9) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C18 1.370(9) . ? C13 C14 1.389(9) . ? C14 C15 1.383(9) . ? C14 H14 0.9300 . ? C15 C16 1.364(11) . ? C15 H15 0.9300 . ? C16 C17 1.367(11) . ? C16 H16 0.9300 . ? C17 C18 1.382(9) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.470(7) . ? C20 C21 1.406(8) . ? C21 C22 1.408(9) . ? C21 C26 1.413(7) . ? C22 C23 1.373(9) . ? C22 H22 0.9300 . ? C23 C24 1.404(9) . ? C23 H23 0.9300 . ? C24 C25 1.356(9) . ? C24 H24 0.9300 . ? C25 C26 1.396(8) . ? C25 H25 0.9300 . ? C27 C28 1.378(10) . ? C27 C32 1.378(9) . ? C28 C29 1.371(12) . ? C28 H28 0.9300 . ? C29 C30 1.387(15) . ? C29 H29 0.9300 . ? C30 C31 1.335(15) . ? C30 C33 1.538(11) . ? C31 C32 1.382(11) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C39 1.362(8) . ? C34 C35 1.377(9) . ? C35 C36 1.375(10) . ? C35 H35 0.9300 . ? C36 C37 1.355(10) . ? C36 H36 0.9300 . ? C37 C38 1.369(10) . ? C37 H37 0.9300 . ? C38 C39 1.382(9) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C45 1.378(8) . ? C40 C41 1.387(9) . ? C41 C42 1.368(9) . ? C41 H41 0.9300 . ? C42 C43 1.372(9) . ? C42 H42 0.9300 . ? C43 C44 1.355(10) . ? C43 H43 0.9300 . ? C44 C45 1.383(9) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 C47 1.362(9) . ? C46 C51 1.390(8) . ? C47 C48 1.385(10) . ? C47 H47 0.9300 . ? C48 C49 1.353(11) . ? C48 H48 0.9300 . ? C49 C50 1.360(10) . ? C49 H49 0.9300 . ? C50 C51 1.374(9) . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? C52 C53 1.488(8) . ? C53 C54 1.397(9) . ? C54 C59 1.393(9) . ? C54 C55 1.415(9) . ? C55 C56 1.381(12) . ? C55 H55 0.9300 . ? C56 C57 1.388(13) . ? C56 H56 0.9300 . ? C57 C58 1.339(12) . ? C57 H57 0.9300 . ? C58 C59 1.387(9) . ? C58 H58 0.9300 . ? C60 C65 1.361(9) . ? C60 C61 1.383(10) . ? C61 C62 1.372(9) . ? C61 H61 0.9300 . ? C62 C63 1.366(10) . ? C62 H62 0.9300 . ? C63 C64 1.369(10) . ? C63 C66 1.524(9) . ? C64 C65 1.376(9) . ? C64 H64 0.9300 . ? C65 H65 0.9300 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? N99 C98 1.121(14) . ? C99 C98 1.410(15) . ? C99 H99A 0.9600 . ? C99 H99B 0.9600 . ? C99 H99C 0.9600 . ? 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 N2 Re1 N1 92.6(2) . . ? N2 Re1 O1 166.42(19) . . ? N1 Re1 O1 73.94(16) . . ? N2 Re1 P1 97.83(17) . . ? N1 Re1 P1 91.18(13) . . ? O1 Re1 P1 80.86(12) . . ? N2 Re1 Br2 98.35(16) . . ? N1 Re1 Br2 167.85(12) . . ? O1 Re1 Br2 95.22(11) . . ? P1 Re1 Br2 92.49(4) . . ? N2 Re1 Br1 97.97(16) . . ? N1 Re1 Br1 87.03(12) . . ? O1 Re1 Br1 83.52(11) . . ? P1 Re1 Br1 164.16(4) . . ? Br2 Re1 Br1 86.28(2) . . ? N5 Re2 O3 170.7(2) . . ? N5 Re2 N4 98.4(2) . . ? O3 Re2 N4 73.90(17) . . ? N5 Re2 P2 92.44(17) . . ? O3 Re2 P2 83.05(12) . . ? N4 Re2 P2 93.36(14) . . ? N5 Re2 Br3 97.57(17) . . ? O3 Re2 Br3 90.69(12) . . ? N4 Re2 Br3 163.00(12) . . ? P2 Re2 Br3 91.83(4) . . ? N5 Re2 Br4 97.54(17) . . ? O3 Re2 Br4 86.96(12) . . ? N4 Re2 Br4 84.43(14) . . ? P2 Re2 Br4 169.99(4) . . ? Br3 Re2 Br4 87.66(3) . . ? C1 P1 C13 107.0(3) . . ? C1 P1 C7 104.0(3) . . ? C13 P1 C7 103.4(3) . . ? C1 P1 Re1 110.3(2) . . ? C13 P1 Re1 112.0(2) . . ? C7 P1 Re1 119.3(2) . . ? C40 P2 C46 107.2(3) . . ? C40 P2 C34 101.0(3) . . ? C46 P2 C34 105.0(3) . . ? C40 P2 Re2 110.5(2) . . ? C46 P2 Re2 112.2(2) . . ? C34 P2 Re2 119.7(2) . . ? C19 O1 Re1 120.0(3) . . ? C52 O3 Re2 120.3(3) . . ? C20 N1 N3 107.7(4) . . ? C20 N1 Re1 119.1(3) . . ? N3 N1 Re1 133.1(4) . . ? C27 N2 Re1 168.6(5) . . ? N1 N3 C26 110.7(4) . . ? N1 N3 H3A 124.6 . . ? C26 N3 H3A 124.6 . . ? C53 N4 N6 107.7(5) . . ? C53 N4 Re2 118.3(4) . . ? N6 N4 Re2 132.8(4) . . ? C60 N5 Re2 174.7(5) . . ? N4 N6 C59 110.0(5) . . ? N4 N6 H6A 125.0 . . ? C59 N6 H6A 125.0 . . ? C6 C1 C2 118.8(6) . . ? C6 C1 P1 120.4(4) . . ? C2 C1 P1 120.4(5) . . ? C3 C2 C1 120.3(6) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 C4 120.4(6) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 119.8(7) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.5(6) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 120.3(6) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C8 C7 C12 119.2(6) . . ? C8 C7 P1 123.3(6) . . ? C12 C7 P1 117.5(5) . . ? C7 C8 C9 119.5(8) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? C10 C9 C8 120.6(8) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C11 C10 C9 120.2(7) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 120.7(8) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C11 C12 C7 119.8(7) . . ? C11 C12 H12 120.1 . . ? C7 C12 H12 120.1 . . ? C18 C13 C14 119.2(6) . . ? C18 C13 P1 119.6(5) . . ? C14 C13 P1 121.2(5) . . ? C15 C14 C13 120.2(7) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C16 C15 C14 119.6(7) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C17 120.8(7) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C16 C17 C18 119.7(7) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C13 C18 C17 120.4(7) . . ? C13 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? O2 C19 O1 124.8(5) . . ? O2 C19 C20 122.7(6) . . ? O1 C19 C20 112.5(5) . . ? N1 C20 C21 110.4(5) . . ? N1 C20 C19 113.6(5) . . ? C21 C20 C19 136.0(6) . . ? C20 C21 C22 137.1(5) . . ? C20 C21 C26 104.5(5) . . ? C22 C21 C26 118.4(5) . . ? C23 C22 C21 118.0(6) . . ? C23 C22 H22 121.0 . . ? C21 C22 H22 121.0 . . ? C22 C23 C24 121.7(7) . . ? C22 C23 H23 119.1 . . ? C24 C23 H23 119.1 . . ? C25 C24 C23 122.2(6) . . ? C25 C24 H24 118.9 . . ? C23 C24 H24 118.9 . . ? C24 C25 C26 116.3(6) . . ? C24 C25 H25 121.8 . . ? C26 C25 H25 121.8 . . ? N3 C26 C25 130.0(5) . . ? N3 C26 C21 106.7(5) . . ? C25 C26 C21 123.3(6) . . ? C28 C27 C32 119.8(7) . . ? C28 C27 N2 118.2(6) . . ? C32 C27 N2 121.9(7) . . ? C29 C28 C27 119.9(9) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 120.3(10) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C31 C30 C29 119.0(9) . . ? C31 C30 C33 121.7(13) . . ? C29 C30 C33 119.3(13) . . ? C30 C31 C32 122.4(10) . . ? C30 C31 H31 118.8 . . ? C32 C31 H31 118.8 . . ? C27 C32 C31 118.6(9) . . ? C27 C32 H32 120.7 . . ? C31 C32 H32 120.7 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C39 C34 C35 118.6(6) . . ? C39 C34 P2 121.9(5) . . ? C35 C34 P2 119.4(5) . . ? C36 C35 C34 120.9(7) . . ? C36 C35 H35 119.5 . . ? C34 C35 H35 119.5 . . ? C37 C36 C35 119.2(7) . . ? C37 C36 H36 120.4 . . ? C35 C36 H36 120.4 . . ? C36 C37 C38 121.4(7) . . ? C36 C37 H37 119.3 . . ? C38 C37 H37 119.3 . . ? C37 C38 C39 118.5(7) . . ? C37 C38 H38 120.7 . . ? C39 C38 H38 120.7 . . ? C34 C39 C38 121.3(7) . . ? C34 C39 H39 119.3 . . ? C38 C39 H39 119.3 . . ? C45 C40 C41 119.3(6) . . ? C45 C40 P2 123.5(5) . . ? C41 C40 P2 117.2(5) . . ? C42 C41 C40 120.1(6) . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C41 C42 C43 120.4(7) . . ? C41 C42 H42 119.8 . . ? C43 C42 H42 119.8 . . ? C44 C43 C42 119.9(7) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C43 C44 C45 120.7(7) . . ? C43 C44 H44 119.6 . . ? C45 C44 H44 119.6 . . ? C40 C45 C44 119.6(6) . . ? C40 C45 H45 120.2 . . ? C44 C45 H45 120.2 . . ? C47 C46 C51 118.7(6) . . ? C47 C46 P2 121.6(5) . . ? C51 C46 P2 119.7(5) . . ? C46 C47 C48 120.1(7) . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C49 C48 C47 120.9(8) . . ? C49 C48 H48 119.6 . . ? C47 C48 H48 119.6 . . ? C48 C49 C50 119.8(7) . . ? C48 C49 H49 120.1 . . ? C50 C49 H49 120.1 . . ? C49 C50 C51 120.2(7) . . ? C49 C50 H50 119.9 . . ? C51 C50 H50 119.9 . . ? C50 C51 C46 120.4(7) . . ? C50 C51 H51 119.8 . . ? C46 C51 H51 119.8 . . ? O4 C52 O3 125.6(6) . . ? O4 C52 C53 122.3(6) . . ? O3 C52 C53 112.1(5) . . ? N4 C53 C54 110.3(5) . . ? N4 C53 C52 114.2(6) . . ? C54 C53 C52 135.5(6) . . ? C59 C54 C53 104.7(5) . . ? C59 C54 C55 120.6(7) . . ? C53 C54 C55 134.7(7) . . ? C56 C55 C54 114.8(8) . . ? C56 C55 H55 122.6 . . ? C54 C55 H55 122.6 . . ? C55 C56 C57 123.2(8) . . ? C55 C56 H56 118.4 . . ? C57 C56 H56 118.4 . . ? C58 C57 C56 122.3(8) . . ? C58 C57 H57 118.8 . . ? C56 C57 H57 118.8 . . ? C57 C58 C59 116.6(8) . . ? C57 C58 H58 121.7 . . ? C59 C58 H58 121.7 . . ? N6 C59 C58 130.1(7) . . ? N6 C59 C54 107.2(5) . . ? C58 C59 C54 122.6(7) . . ? C65 C60 C61 120.4(6) . . ? C65 C60 N5 121.4(6) . . ? C61 C60 N5 118.2(6) . . ? C62 C61 C60 119.0(7) . . ? C62 C61 H61 120.5 . . ? C60 C61 H61 120.5 . . ? C63 C62 C61 121.1(8) . . ? C63 C62 H62 119.4 . . ? C61 C62 H62 119.4 . . ? C62 C63 C64 119.1(7) . . ? C62 C63 C66 120.8(8) . . ? C64 C63 C66 120.1(7) . . ? C63 C64 C65 120.8(7) . . ? C63 C64 H64 119.6 . . ? C65 C64 H64 119.6 . . ? C60 C65 C64 119.6(7) . . ? C60 C65 H65 120.2 . . ? C64 C65 H65 120.2 . . ? C63 C66 H66A 109.5 . . ? C63 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C63 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C98 C99 H99A 109.5 . . ? C98 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? C98 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? N99 C98 C99 176.9(15) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3A O4 0.86 2.12 2.792(6) 134.1 4_575 N6 H6A O2 0.86 2.02 2.781(6) 147.4 . C8 H8 Br2 0.93 2.76 3.392(7) 125.9 . C16 H16 Br3 0.93 2.91 3.770(7) 154.0 4_675 C39 H39 O3 0.93 2.54 3.321(8) 142.2 . C56 H56 Br3 0.93 2.81 3.622(8) 145.8 2_656 C99 H99B Br2 0.96 2.93 3.666(10) 134.5 1_455 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.320 _refine_diff_density_min -1.568 _refine_diff_density_rms 0.131 _database_code_depnum_ccdc_archive 'CCDC 973300'