Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _publ_contact_author_email MPERUZZINI@ICCOM.CNR.IT _publ_contact_author_name 'Dr Maurizio Peruzzini' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; ICCOM Istituto di Chimica dei Composti Organo Metallici, CNR Via Madonna del Piano, snc Area di Ricerca del CNR Sesto Fiorentino (Firenze) 50019 ITALY ; _publ_section_title ; Synthesis, Characterisation and Molecular Structure of Re(III) 2-Oxacyclocarbenes Stabilised by a Benzoyldiazenido Ligand ; loop_ _publ_author_name 'Maurizio Peruzzini' 'Pierluigi Barbaro' 'V. Bertolasi' 'I.de los Rios' 'Nicoletta Mantovani' ; A.Marchi ; 'Lorenza Marvelli' 'Roberto Rossi' data_(2) _database_code_depnum_ccdc_archive 'CCDC 225817' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H41 Cl2 N2 O2 P2 Re, C H2 Cl2' _chemical_formula_sum 'C48 H43 Cl4 N2 O2 P2 Re' _chemical_formula_weight 1069.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' 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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.4338(2) _cell_length_b 25.3055(7) _cell_length_c 16.0016(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.177(1) _cell_angle_gamma 90.00 _cell_volume 4557.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 295 _cell_measurement_reflns_used 34650 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 28.00 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2136 _exptl_absorpt_coefficient_mu 3.012 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.674 _exptl_absorpt_correction_T_max 0.715 _exptl_absorpt_process_details ; SORTAV (R.H. Blessing, Acta Crystallogr., 1995, A51, 33) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295 _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '\f scans and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34650 _diffrn_reflns_av_R_equivalents 0.072 _diffrn_reflns_av_sigmaI/netI 0.0676 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 28.00 _reflns_number_total 10669 _reflns_number_gt 7836 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Kappa CCD server software (Nonius, 1997)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material ; SHELXL-97 (Sheldrick, 1997); PARST (Nardelli, 1995) ; _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^)+(0.0239P)^2^+9.7439P] 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 10669 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0803 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.005 _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 0.158872(16) 0.159119(8) 0.243194(12) 0.02974(7) Uani 1 1 d . . . Cl1 Cl -0.04159(10) 0.12030(6) 0.18737(8) 0.0424(3) Uani 1 1 d . . . Cl2 Cl 0.14389(13) 0.20323(6) 0.10739(8) 0.0499(4) Uani 1 1 d . . . P1 P 0.25643(11) 0.08662(6) 0.17522(8) 0.0326(3) Uani 1 1 d . . . P2 P 0.04787(11) 0.23271(6) 0.29632(8) 0.0322(3) Uani 1 1 d . . . O1 O 0.3721(3) 0.07575(17) 0.4263(2) 0.0531(11) Uani 1 1 d . . . O2 O 0.3757(3) 0.18995(17) 0.3575(2) 0.0521(10) Uani 1 1 d . . . N1 N 0.1741(3) 0.12434(17) 0.3392(2) 0.0327(9) Uani 1 1 d . . . N2 N 0.1717(4) 0.09724(19) 0.4035(3) 0.0417(11) Uani 1 1 d . . . C1 C 0.2756(5) 0.0713(2) 0.4457(3) 0.0414(13) Uani 1 1 d . . . C2 C 0.2504(5) 0.0382(2) 0.5169(3) 0.0416(13) Uani 1 1 d . . . C3 C 0.1414(6) 0.0369(3) 0.5422(4) 0.068(2) Uani 1 1 d . . . H3 H 0.0800 0.0580 0.5146 0.081 Uiso 1 1 calc R . . C4 C 0.1220(8) 0.0047(3) 0.6083(5) 0.087(3) Uani 1 1 d . . . H4 H 0.0477 0.0041 0.6245 0.104 Uiso 1 1 calc R . . C5 C 0.2105(8) -0.0260(3) 0.6494(4) 0.081(2) Uani 1 1 d . . . H5 H 0.1983 -0.0467 0.6950 0.098 Uiso 1 1 calc R . . C6 C 0.3191(7) -0.0263(3) 0.6233(5) 0.096(3) Uani 1 1 d . . . H6 H 0.3795 -0.0483 0.6500 0.115 Uiso 1 1 calc R . . C7 C 0.3380(5) 0.0058(3) 0.5578(4) 0.069(2) Uani 1 1 d . . . H7 H 0.4118 0.0056 0.5410 0.082 Uiso 1 1 calc R . . C8 C 0.3108(4) 0.1978(2) 0.2809(3) 0.0403(13) Uani 1 1 d . . . C9 C 0.4830(5) 0.2233(3) 0.3749(5) 0.075(2) Uani 1 1 d . . . H91 H 0.5539 0.2023 0.3744 0.090 Uiso 1 1 calc R . . H92 H 0.4894 0.2405 0.4297 0.090 Uiso 1 1 calc R . . C10 C 0.4670(7) 0.2627(4) 0.3054(5) 0.092(3) Uani 1 1 d . . . H011 H 0.5402 0.2673 0.2836 0.110 Uiso 1 1 calc R . . H102 H 0.4434 0.2965 0.3255 0.110 Uiso 1 1 calc R . . C11 C 0.3698(5) 0.2406(3) 0.2370(4) 0.0573(17) Uani 1 1 d . . . H111 H 0.3131 0.2679 0.2151 0.069 Uiso 1 1 calc R . . H112 H 0.4034 0.2260 0.1904 0.069 Uiso 1 1 calc R . . C12 C 0.1928(4) 0.0593(2) 0.0707(3) 0.0372(12) Uani 1 1 d . . . C13 C 0.0937(5) 0.0792(3) 0.0199(3) 0.0492(15) Uani 1 1 d . . . H13 H 0.0547 0.1083 0.0375 0.059 Uiso 1 1 calc R . . C14 C 0.0511(5) 0.0556(3) -0.0586(4) 0.0637(19) Uani 1 1 d . . . H14 H -0.0158 0.0694 -0.0932 0.076 Uiso 1 1 calc R . . C15 C 0.1061(6) 0.0126(3) -0.0853(4) 0.0629(19) Uani 1 1 d . . . H15 H 0.0768 -0.0029 -0.1375 0.076 Uiso 1 1 calc R . . C16 C 0.2051(6) -0.0075(3) -0.0345(4) 0.0614(18) Uani 1 1 d . . . H16 H 0.2429 -0.0368 -0.0525 0.074 Uiso 1 1 calc R . . C17 C 0.2493(5) 0.0151(2) 0.0430(4) 0.0524(15) Uani 1 1 d . . . H17 H 0.3166 0.0011 0.0769 0.063 Uiso 1 1 calc R . . C18 C 0.4062(4) 0.1057(2) 0.1623(3) 0.0346(12) Uani 1 1 d . . . C19 C 0.4928(4) 0.1141(2) 0.2340(4) 0.0437(13) Uani 1 1 d . . . H19 H 0.4751 0.1083 0.2878 0.052 Uiso 1 1 calc R . . C20 C 0.6054(5) 0.1311(2) 0.2254(4) 0.0522(16) Uani 1 1 d . . . H20 H 0.6633 0.1364 0.2733 0.063 Uiso 1 1 calc R . . C21 C 0.6311(5) 0.1402(3) 0.1458(5) 0.0623(18) Uani 1 1 d . . . H21 H 0.7066 0.1516 0.1401 0.075 Uiso 1 1 calc R . . C22 C 0.5460(5) 0.1326(3) 0.0749(4) 0.0611(18) Uani 1 1 d . . . H22 H 0.5639 0.1391 0.0213 0.073 Uiso 1 1 calc R . . C23 C 0.4337(5) 0.1154(3) 0.0830(4) 0.0486(15) Uani 1 1 d . . . H23 H 0.3763 0.1103 0.0347 0.058 Uiso 1 1 calc R . . C24 C 0.2725(5) 0.0263(2) 0.2391(3) 0.0413(13) Uani 1 1 d . . . C25 C 0.1724(5) 0.0064(2) 0.2651(4) 0.0492(15) Uani 1 1 d . . . H25 H 0.1007 0.0245 0.2515 0.059 Uiso 1 1 calc R . . C26 C 0.1774(7) -0.0403(3) 0.3114(4) 0.0679(19) Uani 1 1 d . . . H26 H 0.1089 -0.0539 0.3270 0.081 Uiso 1 1 calc R . . C27 C 0.2838(7) -0.0663(3) 0.3339(4) 0.0681(19) Uani 1 1 d . . . H27 H 0.2874 -0.0970 0.3661 0.082 Uiso 1 1 calc R . . C28 C 0.3842(6) -0.0473(3) 0.3095(4) 0.0631(18) Uani 1 1 d . . . H28 H 0.4562 -0.0649 0.3248 0.076 Uiso 1 1 calc R . . C29 C 0.3776(5) -0.0010(2) 0.2611(4) 0.0494(15) Uani 1 1 d . . . H29 H 0.4456 0.0117 0.2434 0.059 Uiso 1 1 calc R . . C30 C 0.1444(4) 0.2835(2) 0.3542(3) 0.0347(12) Uani 1 1 d . . . C31 C 0.1493(5) 0.3360(2) 0.3313(4) 0.0467(14) Uani 1 1 d . . . H31 H 0.1013 0.3483 0.2822 0.056 Uiso 1 1 calc R . . C32 C 0.2261(6) 0.3704(3) 0.3819(4) 0.0594(17) Uani 1 1 d . . . H32 H 0.2298 0.4056 0.3656 0.071 Uiso 1 1 calc R . . C33 C 0.2967(5) 0.3533(3) 0.4556(4) 0.0522(16) Uani 1 1 d . . . H33 H 0.3472 0.3767 0.4893 0.063 Uiso 1 1 calc R . . C34 C 0.2913(5) 0.3013(3) 0.4786(4) 0.0506(15) Uani 1 1 d . . . H34 H 0.3385 0.2892 0.5283 0.061 Uiso 1 1 calc R . . C35 C 0.2163(5) 0.2667(2) 0.4283(3) 0.0455(14) Uani 1 1 d . . . H35 H 0.2139 0.2315 0.4444 0.055 Uiso 1 1 calc R . . C36 C -0.0579(4) 0.2674(2) 0.2161(3) 0.0361(12) Uani 1 1 d . . . C37 C -0.1792(5) 0.2604(2) 0.2113(4) 0.0498(15) Uani 1 1 d . . . H37 H -0.2068 0.2377 0.2492 0.060 Uiso 1 1 calc R . . C38 C -0.2597(6) 0.2868(3) 0.1510(5) 0.068(2) Uani 1 1 d . . . H38 H -0.3408 0.2814 0.1478 0.082 Uiso 1 1 calc R . . C39 C -0.2193(7) 0.3208(3) 0.0959(4) 0.075(2) Uani 1 1 d . . . H39 H -0.2738 0.3398 0.0573 0.090 Uiso 1 1 calc R . . C40 C -0.1006(7) 0.3273(3) 0.0967(4) 0.0599(18) Uani 1 1 d . . . H40 H -0.0744 0.3498 0.0579 0.072 Uiso 1 1 calc R . . C41 C -0.0186(5) 0.2999(2) 0.1567(3) 0.0503(15) Uani 1 1 d . . . H41 H 0.0623 0.3034 0.1567 0.060 Uiso 1 1 calc R . . C42 C -0.0411(4) 0.2151(2) 0.3766(3) 0.0373(12) Uani 1 1 d . . . C43 C -0.0740(5) 0.1636(2) 0.3908(3) 0.0420(13) Uani 1 1 d . . . H43 H -0.0504 0.1360 0.3592 0.050 Uiso 1 1 calc R . . C44 C -0.1421(6) 0.1536(3) 0.4524(4) 0.0629(18) Uani 1 1 d . . . H44 H -0.1624 0.1189 0.4630 0.075 Uiso 1 1 calc R . . C45 C -0.1802(7) 0.1939(3) 0.4981(4) 0.078(2) Uani 1 1 d . . . H45 H -0.2269 0.1865 0.5387 0.093 Uiso 1 1 calc R . . C46 C -0.1495(7) 0.2453(3) 0.4842(5) 0.082(2) Uani 1 1 d . . . H46 H -0.1751 0.2729 0.5150 0.098 Uiso 1 1 calc R . . C47 C -0.0797(6) 0.2551(3) 0.4234(4) 0.0638(18) Uani 1 1 d . . . H47 H -0.0583 0.2898 0.4139 0.077 Uiso 1 1 calc R . . C48 C 0.2946(15) 0.0989(8) 0.7970(14) 0.275(13) Uani 1 1 d . . . H481 H 0.3282 0.1216 0.7585 0.330 Uiso 1 1 calc R . . H482 H 0.2526 0.0713 0.7617 0.330 Uiso 1 1 calc R . . Cl3 Cl 0.4039(4) 0.0702(3) 0.8488(3) 0.251(3) Uani 1 1 d . . . Cl4 Cl 0.2003(8) 0.1307(3) 0.8223(7) 0.478(9) 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 0.03020(10) 0.03139(12) 0.02760(10) 0.00078(10) 0.00500(7) -0.00109(9) Cl1 0.0331(6) 0.0526(9) 0.0407(7) -0.0083(6) 0.0041(5) -0.0044(6) Cl2 0.0626(9) 0.0534(10) 0.0367(7) 0.0121(7) 0.0171(6) 0.0032(7) P1 0.0304(6) 0.0357(8) 0.0313(7) -0.0021(6) 0.0044(5) -0.0007(5) P2 0.0371(7) 0.0318(8) 0.0275(7) 0.0016(6) 0.0050(5) -0.0001(6) O1 0.043(2) 0.063(3) 0.053(2) 0.010(2) 0.0063(18) 0.0012(19) O2 0.040(2) 0.055(3) 0.058(3) -0.010(2) -0.0031(18) -0.0061(18) N1 0.034(2) 0.035(3) 0.028(2) -0.0015(19) 0.0025(16) 0.0018(18) N2 0.043(2) 0.046(3) 0.036(3) 0.009(2) 0.0048(19) 0.005(2) C1 0.047(3) 0.040(4) 0.035(3) 0.000(2) 0.001(2) 0.001(3) C2 0.048(3) 0.039(4) 0.034(3) 0.004(2) -0.004(2) -0.001(2) C3 0.073(4) 0.072(5) 0.063(4) 0.027(4) 0.023(3) 0.019(4) C4 0.102(6) 0.083(6) 0.087(6) 0.031(5) 0.049(5) 0.009(5) C5 0.107(6) 0.075(6) 0.057(4) 0.031(4) 0.001(4) -0.019(5) C6 0.078(5) 0.091(7) 0.105(6) 0.061(5) -0.019(5) -0.003(5) C7 0.048(4) 0.079(6) 0.072(5) 0.031(4) -0.007(3) -0.004(3) C8 0.038(3) 0.040(4) 0.045(3) -0.006(3) 0.012(2) 0.002(2) C9 0.038(3) 0.079(6) 0.102(6) -0.036(5) -0.002(3) -0.016(3) C10 0.077(5) 0.092(7) 0.111(7) -0.016(6) 0.028(5) -0.050(5) C11 0.051(3) 0.050(4) 0.074(4) -0.005(3) 0.020(3) -0.020(3) C12 0.040(3) 0.041(3) 0.032(3) -0.005(2) 0.010(2) -0.010(2) C13 0.038(3) 0.069(5) 0.039(3) -0.010(3) 0.003(2) 0.003(3) C14 0.050(4) 0.099(6) 0.038(3) -0.011(4) -0.002(3) -0.013(4) C15 0.072(4) 0.077(6) 0.042(4) -0.020(4) 0.014(3) -0.022(4) C16 0.082(5) 0.050(4) 0.056(4) -0.013(3) 0.022(3) -0.009(3) C17 0.069(4) 0.039(4) 0.047(4) -0.007(3) 0.004(3) 0.003(3) C18 0.030(2) 0.035(3) 0.039(3) 0.000(2) 0.008(2) 0.001(2) C19 0.041(3) 0.044(4) 0.044(3) -0.004(3) 0.001(2) -0.004(2) C20 0.033(3) 0.048(4) 0.069(4) 0.003(3) -0.009(3) -0.003(3) C21 0.039(3) 0.060(5) 0.089(5) 0.015(4) 0.015(3) -0.002(3) C22 0.045(3) 0.082(5) 0.060(4) 0.016(4) 0.019(3) -0.003(3) C23 0.040(3) 0.061(4) 0.046(3) 0.002(3) 0.011(2) -0.003(3) C24 0.060(3) 0.033(3) 0.031(3) -0.004(2) 0.008(2) 0.003(3) C25 0.057(4) 0.041(4) 0.053(4) 0.000(3) 0.018(3) 0.000(3) C26 0.087(5) 0.049(5) 0.073(5) 0.007(4) 0.029(4) -0.011(4) C27 0.101(6) 0.042(4) 0.064(5) 0.013(3) 0.023(4) 0.006(4) C28 0.076(5) 0.045(4) 0.065(4) 0.003(3) 0.001(3) 0.013(3) C29 0.048(3) 0.046(4) 0.054(4) 0.001(3) 0.007(3) -0.004(3) C30 0.039(3) 0.035(3) 0.031(3) -0.001(2) 0.008(2) 0.002(2) C31 0.054(3) 0.033(3) 0.049(3) -0.001(3) -0.003(3) -0.002(3) C32 0.071(4) 0.037(4) 0.067(4) -0.005(3) 0.002(3) -0.007(3) C33 0.048(3) 0.053(5) 0.054(4) -0.016(3) 0.003(3) -0.009(3) C34 0.046(3) 0.057(4) 0.044(3) -0.004(3) -0.003(3) 0.005(3) C35 0.056(3) 0.038(4) 0.039(3) 0.001(3) 0.001(2) -0.003(3) C36 0.046(3) 0.030(3) 0.030(3) -0.001(2) 0.000(2) 0.002(2) C37 0.050(3) 0.051(4) 0.044(3) -0.002(3) -0.003(3) 0.007(3) C38 0.055(4) 0.070(5) 0.070(5) -0.008(4) -0.016(3) 0.021(4) C39 0.103(6) 0.058(5) 0.049(4) -0.004(4) -0.026(4) 0.026(4) C40 0.090(5) 0.041(4) 0.043(4) 0.005(3) -0.005(3) 0.008(3) C41 0.062(4) 0.046(4) 0.042(3) 0.002(3) 0.005(3) 0.003(3) C42 0.043(3) 0.039(3) 0.032(3) -0.002(2) 0.011(2) 0.002(2) C43 0.048(3) 0.039(4) 0.042(3) 0.001(3) 0.016(2) 0.001(3) C44 0.076(4) 0.062(5) 0.058(4) -0.001(4) 0.032(3) -0.018(4) C45 0.094(5) 0.091(7) 0.062(5) -0.013(4) 0.054(4) -0.021(5) C46 0.113(6) 0.072(6) 0.079(5) -0.026(4) 0.067(5) -0.012(5) C47 0.087(5) 0.045(4) 0.071(5) -0.009(3) 0.044(4) -0.005(3) C48 0.148(14) 0.28(3) 0.36(3) 0.20(2) -0.052(16) -0.001(14) Cl3 0.191(4) 0.382(8) 0.206(5) -0.082(5) 0.110(4) -0.071(5) Cl4 0.483(12) 0.276(8) 0.815(19) 0.345(11) 0.499(14) 0.189(8) _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 1.752(4) . ? Re1 C8 1.993(5) . ? Re1 Cl2 2.4220(13) . ? Re1 P2 2.4866(14) . ? Re1 P1 2.4945(13) . ? Re1 Cl1 2.5086(12) . ? P1 C18 1.825(5) . ? P1 C24 1.829(6) . ? P1 C12 1.837(5) . ? P2 C36 1.825(5) . ? P2 C42 1.829(5) . ? P2 C30 1.836(5) . ? O1 C1 1.204(6) . ? O2 C8 1.331(6) . ? O2 C9 1.474(7) . ? N1 N2 1.242(5) . ? N2 C1 1.419(7) . ? C1 C2 1.483(7) . ? C2 C7 1.368(8) . ? C2 C3 1.377(8) . ? C3 C4 1.384(9) . ? C3 H3 0.9300 . ? C4 C5 1.350(10) . ? C4 H4 0.9300 . ? C5 C6 1.378(10) . ? C5 H5 0.9300 . ? C6 C7 1.373(9) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C11 1.512(8) . ? C9 C10 1.480(11) . ? C9 H91 0.9700 . ? C9 H92 0.9700 . ? C10 C11 1.521(9) . ? C10 H011 0.9700 . ? C10 H102 0.9700 . ? C11 H111 0.9700 . ? C11 H112 0.9700 . ? C12 C13 1.368(7) . ? C12 C17 1.401(8) . ? C13 C14 1.398(8) . ? C13 H13 0.9300 . ? C14 C15 1.362(9) . ? C14 H14 0.9300 . ? C15 C16 1.369(9) . ? C15 H15 0.9300 . ? C16 C17 1.379(8) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C23 1.382(7) . ? C18 C19 1.394(7) . ? C19 C20 1.386(7) . ? C19 H19 0.9300 . ? C20 C21 1.376(8) . ? C20 H20 0.9300 . ? C21 C22 1.372(9) . ? C21 H21 0.9300 . ? C22 C23 1.384(7) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C29 1.375(8) . ? C24 C25 1.380(7) . ? C25 C26 1.390(9) . ? C25 H25 0.9300 . ? C26 C27 1.373(9) . ? C26 H26 0.9300 . ? C27 C28 1.364(9) . ? C27 H27 0.9300 . ? C28 C29 1.399(8) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.382(7) . ? C30 C35 1.384(7) . ? C31 C32 1.390(8) . ? C31 H31 0.9300 . ? C32 C33 1.376(8) . ? C32 H32 0.9300 . ? C33 C34 1.372(9) . ? C33 H33 0.9300 . ? C34 C35 1.380(8) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C37 1.387(7) . ? C36 C41 1.390(8) . ? C37 C38 1.381(8) . ? C37 H37 0.9300 . ? C38 C39 1.368(10) . ? C38 H38 0.9300 . ? C39 C40 1.365(10) . ? C39 H39 0.9300 . ? C40 C41 1.402(8) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C47 1.377(8) . ? C42 C43 1.388(7) . ? C43 C44 1.383(7) . ? C43 H43 0.9300 . ? C44 C45 1.370(9) . ? C44 H44 0.9300 . ? C45 C46 1.376(10) . ? C45 H45 0.9300 . ? C46 C47 1.386(8) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C48 Cl4 1.46(2) . ? C48 Cl3 1.552(13) . ? C48 H481 0.9700 . ? C48 H482 0.9700 . ? 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 C8 92.0(2) . . ? N1 Re1 Cl2 176.77(14) . . ? C8 Re1 Cl2 87.97(17) . . ? N1 Re1 P2 93.11(13) . . ? C8 Re1 P2 89.92(15) . . ? Cl2 Re1 P2 90.12(5) . . ? N1 Re1 P1 91.71(14) . . ? C8 Re1 P1 93.47(15) . . ? Cl2 Re1 P1 85.06(5) . . ? P2 Re1 P1 174.00(4) . . ? N1 Re1 Cl1 93.35(13) . . ? C8 Re1 Cl1 173.26(17) . . ? Cl2 Re1 Cl1 86.89(5) . . ? P2 Re1 Cl1 85.73(4) . . ? P1 Re1 Cl1 90.43(4) . . ? C18 P1 C24 106.3(2) . . ? C18 P1 C12 103.0(2) . . ? C24 P1 C12 100.3(2) . . ? C18 P1 Re1 110.84(18) . . ? C24 P1 Re1 112.26(17) . . ? C12 P1 Re1 122.55(18) . . ? C36 P2 C42 103.3(2) . . ? C36 P2 C30 106.4(2) . . ? C42 P2 C30 100.1(2) . . ? C36 P2 Re1 115.76(17) . . ? C42 P2 Re1 116.04(18) . . ? C30 P2 Re1 113.54(16) . . ? C8 O2 C9 113.5(5) . . ? N2 N1 Re1 172.4(4) . . ? N1 N2 C1 120.7(4) . . ? O1 C1 N2 124.2(5) . . ? O1 C1 C2 124.2(5) . . ? N2 C1 C2 111.5(5) . . ? C7 C2 C3 118.0(6) . . ? C7 C2 C1 118.7(5) . . ? C3 C2 C1 123.2(5) . . ? C2 C3 C4 120.9(6) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 120.2(7) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 119.6(7) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C7 C6 C5 120.0(7) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C2 C7 C6 121.2(7) . . ? C2 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? O2 C8 C11 108.2(5) . . ? O2 C8 Re1 121.3(4) . . ? C11 C8 Re1 130.4(4) . . ? O2 C9 C10 104.8(5) . . ? O2 C9 H91 110.8 . . ? C10 C9 H91 110.8 . . ? O2 C9 H92 110.8 . . ? C10 C9 H92 110.8 . . ? H91 C9 H92 108.9 . . ? C9 C10 C11 105.7(6) . . ? C9 C10 H011 110.6 . . ? C11 C10 H011 110.6 . . ? C9 C10 H102 110.6 . . ? C11 C10 H102 110.6 . . ? H011 C10 H102 108.7 . . ? C8 C11 C10 104.9(5) . . ? C8 C11 H111 110.8 . . ? C10 C11 H111 110.8 . . ? C8 C11 H112 110.8 . . ? C10 C11 H112 110.8 . . ? H111 C11 H112 108.8 . . ? C13 C12 C17 119.0(5) . . ? C13 C12 P1 123.8(4) . . ? C17 C12 P1 117.2(4) . . ? C12 C13 C14 119.8(6) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C15 C14 C13 121.1(6) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C16 119.3(6) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C15 C16 C17 120.8(6) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C16 C17 C12 120.0(6) . . ? C16 C17 H17 120.0 . . ? C12 C17 H17 120.0 . . ? C23 C18 C19 119.0(5) . . ? C23 C18 P1 121.4(4) . . ? C19 C18 P1 119.5(4) . . ? C20 C19 C18 120.2(5) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C21 C20 C19 119.8(5) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C22 C21 C20 120.5(6) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 120.0(6) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C18 C23 C22 120.5(5) . . ? C18 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C29 C24 C25 118.3(5) . . ? C29 C24 P1 123.9(4) . . ? C25 C24 P1 117.7(4) . . ? C24 C25 C26 120.7(6) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C27 C26 C25 119.9(6) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C28 C27 C26 120.5(7) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C29 119.2(6) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C24 C29 C28 121.3(6) . . ? C24 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? C31 C30 C35 118.5(5) . . ? C31 C30 P2 126.1(4) . . ? C35 C30 P2 115.5(4) . . ? C30 C31 C32 119.9(5) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C33 C32 C31 121.1(6) . . ? C33 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C34 C33 C32 119.0(5) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? C33 C34 C35 120.3(5) . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C34 C35 C30 121.2(6) . . ? C34 C35 H35 119.4 . . ? C30 C35 H35 119.4 . . ? C37 C36 C41 118.6(5) . . ? C37 C36 P2 120.6(4) . . ? C41 C36 P2 120.8(4) . . ? C38 C37 C36 120.9(6) . . ? C38 C37 H37 119.6 . . ? C36 C37 H37 119.6 . . ? C39 C38 C37 119.6(7) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? C40 C39 C38 121.2(6) . . ? C40 C39 H39 119.4 . . ? C38 C39 H39 119.4 . . ? C39 C40 C41 119.3(6) . . ? C39 C40 H40 120.4 . . ? C41 C40 H40 120.4 . . ? C36 C41 C40 120.3(6) . . ? C36 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C47 C42 C43 118.7(5) . . ? C47 C42 P2 118.4(4) . . ? C43 C42 P2 122.9(4) . . ? C44 C43 C42 119.5(5) . . ? C44 C43 H43 120.3 . . ? C42 C43 H43 120.3 . . ? C45 C44 C43 121.0(6) . . ? C45 C44 H44 119.5 . . ? C43 C44 H44 119.5 . . ? C44 C45 C46 120.3(6) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? C45 C46 C47 118.5(6) . . ? C45 C46 H46 120.8 . . ? C47 C46 H46 120.8 . . ? C42 C47 C46 122.0(6) . . ? C42 C47 H47 119.0 . . ? C46 C47 H47 119.0 . . ? Cl4 C48 Cl3 132.4(18) . . ? Cl4 C48 H481 104.1 . . ? Cl3 C48 H481 104.1 . . ? Cl4 C48 H482 104.1 . . ? Cl3 C48 H482 104.1 . . ? H481 C48 H482 105.5 . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 1.437 _refine_diff_density_min -1.108 _refine_diff_density_rms 0.113 ###===END data_(3a) _database_code_depnum_ccdc_archive 'CCDC 225818' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H43 Cl2 N2 O2 P2 Re' _chemical_formula_sum 'C48 H43 Cl2 N2 O2 P2 Re' _chemical_formula_weight 998.88 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 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.0911(2) _cell_length_b 15.0661(2) _cell_length_c 19.1572(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.089(1) _cell_angle_gamma 90.00 _cell_volume 4361.7(1) _cell_formula_units_Z 4 _cell_measurement_temperature 295 _cell_measurement_reflns_used 45504 _cell_measurement_theta_min 3.50 _cell_measurement_theta_max 28.00 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 3.023 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.448 _exptl_absorpt_correction_T_max 0.669 _exptl_absorpt_process_details ; SORTAV (R.H. Blessing, Acta Crystallogr.. 1995. A51, 33) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295 _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '\f scans and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45584 _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.50 _diffrn_reflns_theta_max 28.00 _reflns_number_total 10503 _reflns_number_gt 8175 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Kappa CCD server software (Nonius, 1997)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1987)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1987)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP II (Johnson, 1976)' _computing_publication_material ; SHELXL-97 (Sheldrick, 1997), PARST (Nardelli, 1995) ; _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^)+(0.0295P)^2^+5.0565P] 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 10503 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0857 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.119 _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 0.231650(10) 0.190776(9) -0.100041(8) 0.03011(6) Uani 1 1 d . . . Cl1 Cl 0.38554(7) 0.25254(7) -0.05932(6) 0.0470(3) Uani 1 1 d . . . Cl2 Cl 0.18317(7) 0.31860(6) -0.18173(6) 0.0443(2) Uani 1 1 d . . . P1 P 0.20944(8) 0.27680(7) 0.00373(6) 0.0410(3) Uani 1 1 d . . . P2 P 0.26282(7) 0.10518(7) -0.19911(6) 0.0339(2) Uani 1 1 d . . . O1 O 0.1675(2) 0.0228(2) 0.0348(2) 0.0677(10) Uani 1 1 d . . . O2 O 0.0854(2) 0.0664(2) -0.12896(19) 0.0579(9) Uani 1 1 d . . . N1 N 0.2633(2) 0.0990(2) -0.04063(17) 0.0329(7) Uani 1 1 d . . . N2 N 0.2934(2) 0.0365(2) 0.00335(18) 0.0373(8) Uani 1 1 d . . . C1 C 0.2413(3) -0.0014(3) 0.0407(2) 0.0431(10) Uani 1 1 d . . . C2 C 0.2883(3) -0.0730(3) 0.0924(2) 0.0445(10) Uani 1 1 d . . . C3 C 0.3644(3) -0.1125(3) 0.0894(3) 0.0593(13) Uani 1 1 d . . . H3 H 0.3898 -0.0917 0.0556 0.071 Uiso 1 1 calc R . . C4 C 0.4036(4) -0.1826(4) 0.1358(4) 0.0801(18) Uani 1 1 d . . . H4 H 0.4539 -0.2100 0.1325 0.096 Uiso 1 1 calc R . . C5 C 0.3668(5) -0.2107(4) 0.1866(4) 0.097(2) Uani 1 1 d . . . H5 H 0.3922 -0.2578 0.2180 0.116 Uiso 1 1 calc R . . C6 C 0.2931(5) -0.1703(5) 0.1918(4) 0.109(3) Uani 1 1 d . . . H6 H 0.2698 -0.1891 0.2276 0.131 Uiso 1 1 calc R . . C7 C 0.2530(4) -0.1019(4) 0.1446(3) 0.0765(18) Uani 1 1 d . . . H7 H 0.2023 -0.0753 0.1479 0.092 Uiso 1 1 calc R . . C8 C 0.1071(3) 0.1484(3) -0.1412(2) 0.0372(9) Uani 1 1 d . . . C9 C -0.0153(6) 0.0547(7) -0.1522(6) 0.048(2) Uani 0.60 1 d P . . H9 H -0.0319 0.0657 -0.1133 0.060 Uiso 0.60 1 d P . . C9' C 0.0000(11) 0.0374(12) -0.1834(10) 0.064(4) Uani 0.40 1 d P . . H9' H 0.0093 0.0231 -0.2167 0.070 Uiso 0.40 1 d P . . C10 C -0.0479(3) 0.1247(4) -0.2076(3) 0.0633(14) Uani 1 1 d . . . H101 H -0.1019 0.1476 -0.2024 0.070 Uiso 1 1 d . . . H102 H -0.0611 0.1043 -0.2582 0.070 Uiso 1 1 d . . . C11 C 0.0235(3) 0.1953(3) -0.1882(3) 0.0476(11) Uani 1 1 d . . . H111 H 0.0303 0.2195 -0.2329 0.057 Uiso 1 1 calc R . . H112 H 0.0090 0.2432 -0.1606 0.057 Uiso 1 1 calc R . . C12 C -0.0273(19) -0.0435(15) -0.1757(16) 0.106(8) Uani 0.60 1 d P . . H121 H -0.0941 -0.0475 -0.1826 0.090 Uiso 0.60 1 d P . . H122 H 0.0000 -0.0709 -0.1263 0.090 Uiso 0.60 1 d P . . H123 H -0.0134 -0.0557 -0.2105 0.090 Uiso 0.60 1 d P . . C12' C -0.035(2) -0.0282(15) -0.150(2) 0.084(9) Uani 0.40 1 d P . . H124 H 0.0185 -0.0790 -0.1611 0.100 Uiso 0.40 1 d P . . H125 H -0.0823 -0.0551 -0.1946 0.100 Uiso 0.40 1 d P . . H126 H -0.0301 -0.0393 -0.1099 0.100 Uiso 0.40 1 d P . . C13 C 0.2625(3) 0.2214(3) 0.0932(2) 0.0433(10) Uani 1 1 d . . . C14 C 0.3508(3) 0.1986(3) 0.1118(2) 0.0503(11) Uani 1 1 d . . . H14 H 0.3805 0.2124 0.0792 0.060 Uiso 1 1 calc R . . C15 C 0.3958(4) 0.1557(4) 0.1775(3) 0.0606(13) Uani 1 1 d . . . H15 H 0.4549 0.1403 0.1887 0.073 Uiso 1 1 calc R . . C16 C 0.3534(4) 0.1359(4) 0.2263(3) 0.0662(15) Uani 1 1 d . . . H16 H 0.3834 0.1070 0.2707 0.079 Uiso 1 1 calc R . . C17 C 0.2651(4) 0.1591(4) 0.2091(3) 0.0693(15) Uani 1 1 d . . . H17 H 0.2360 0.1458 0.2422 0.083 Uiso 1 1 calc R . . C18 C 0.2206(4) 0.2016(3) 0.1434(3) 0.0573(13) Uani 1 1 d . . . H18 H 0.1616 0.2172 0.1325 0.069 Uiso 1 1 calc R . . C19 C 0.0924(3) 0.2852(3) -0.0067(3) 0.0516(12) Uani 1 1 d . . . C20 C 0.0454(3) 0.2088(4) -0.0032(3) 0.0572(13) Uani 1 1 d . . . H20 H 0.0749 0.1547 0.0083 0.069 Uiso 1 1 calc R . . C21 C -0.0444(4) 0.2122(4) -0.0165(3) 0.0707(16) Uani 1 1 d . . . H21 H -0.0747 0.1610 -0.0126 0.085 Uiso 1 1 calc R . . C22 C -0.0891(4) 0.2917(5) -0.0356(4) 0.087(2) Uani 1 1 d . . . H22 H -0.1499 0.2940 -0.0457 0.104 Uiso 1 1 calc R . . C23 C -0.0438(4) 0.3665(5) -0.0394(4) 0.091(2) Uani 1 1 d . . . H23 H -0.0742 0.4200 -0.0515 0.109 Uiso 1 1 calc R . . C24 C 0.0465(4) 0.3653(4) -0.0258(3) 0.0696(16) Uani 1 1 d . . . H24 H 0.0761 0.4171 -0.0293 0.083 Uiso 1 1 calc R . . C25 C 0.2490(3) 0.3918(3) 0.0246(3) 0.0495(11) Uani 1 1 d . . . C26 C 0.2547(4) 0.4284(4) 0.0923(3) 0.0781(18) Uani 1 1 d . . . H26 H 0.2420 0.3940 0.1277 0.094 Uiso 1 1 calc R . . C27 C 0.2794(5) 0.5167(4) 0.1073(4) 0.091(2) Uani 1 1 d . . . H27 H 0.2829 0.5412 0.1528 0.109 Uiso 1 1 calc R . . C28 C 0.2984(4) 0.5675(4) 0.0565(4) 0.0799(19) Uani 1 1 d . . . H28 H 0.3146 0.6266 0.0669 0.096 Uiso 1 1 calc R . . C29 C 0.2938(4) 0.5318(3) -0.0095(4) 0.0736(16) Uani 1 1 d . . . H29 H 0.3069 0.5668 -0.0444 0.088 Uiso 1 1 calc R . . C30 C 0.2699(3) 0.4441(3) -0.0261(3) 0.0575(13) Uani 1 1 d . . . H30 H 0.2679 0.4203 -0.0715 0.069 Uiso 1 1 calc R . . C31 C 0.1663(3) 0.0740(3) -0.2792(2) 0.0356(9) Uani 1 1 d . . . C32 C 0.1129(3) 0.1433(3) -0.3173(2) 0.0464(11) Uani 1 1 d . . . H32 H 0.1263 0.2013 -0.3006 0.056 Uiso 1 1 calc R . . C33 C 0.0399(3) 0.1266(3) -0.3799(2) 0.0548(12) Uani 1 1 d . . . H33 H 0.0047 0.1733 -0.4055 0.066 Uiso 1 1 calc R . . C34 C 0.0199(3) 0.0412(3) -0.4040(3) 0.0588(13) Uani 1 1 d . . . H34 H -0.0302 0.0299 -0.4453 0.071 Uiso 1 1 calc R . . C35 C 0.0729(3) -0.0278(3) -0.3680(3) 0.0585(13) Uani 1 1 d . . . H35 H 0.0590 -0.0856 -0.3850 0.070 Uiso 1 1 calc R . . C36 C 0.1465(3) -0.0113(3) -0.3066(2) 0.0486(11) Uani 1 1 d . . . H36 H 0.1834 -0.0580 -0.2833 0.058 Uiso 1 1 calc R . . C37 C 0.3191(3) 0.0038(3) -0.1562(2) 0.0417(10) Uani 1 1 d . . . C38 C 0.2739(3) -0.0671(3) -0.1420(2) 0.0527(12) Uani 1 1 d . . . H38 H 0.2124 -0.0656 -0.1579 0.063 Uiso 1 1 calc R . . C39 C 0.3188(4) -0.1411(3) -0.1041(3) 0.0692(16) Uani 1 1 d . . . H39 H 0.2876 -0.1903 -0.0973 0.083 Uiso 1 1 calc R . . C40 C 0.4100(5) -0.1408(4) -0.0767(3) 0.081(2) Uani 1 1 d . . . H40 H 0.4404 -0.1899 -0.0509 0.098 Uiso 1 1 calc R . . C41 C 0.4557(4) -0.0690(4) -0.0871(3) 0.0735(17) Uani 1 1 d . . . H41 H 0.5172 -0.0686 -0.0671 0.088 Uiso 1 1 calc R . . C42 C 0.4115(3) 0.0031(4) -0.1272(3) 0.0612(14) Uani 1 1 d . . . H42 H 0.4433 0.0513 -0.1351 0.073 Uiso 1 1 calc R . . C43 C 0.3325(3) 0.1493(3) -0.2485(2) 0.0484(11) Uani 1 1 d . . . C44 C 0.3583(4) 0.0925(5) -0.2946(3) 0.0831(19) Uani 1 1 d . . . H44 H 0.3440 0.0325 -0.2967 0.100 Uiso 1 1 calc R . . C45 C 0.4057(5) 0.1260(6) -0.3375(4) 0.112(3) Uani 1 1 d . . . H45 H 0.4226 0.0885 -0.3688 0.135 Uiso 1 1 calc R . . C46 C 0.4276(5) 0.2153(6) -0.3337(4) 0.096(2) Uani 1 1 d . . . H46 H 0.4587 0.2377 -0.3627 0.116 Uiso 1 1 calc R . . C47 C 0.4035(4) 0.2703(5) -0.2874(4) 0.0761(17) Uani 1 1 d . . . H47 H 0.4189 0.3300 -0.2844 0.091 Uiso 1 1 calc R . . C48 C 0.3563(3) 0.2371(3) -0.2449(3) 0.0557(12) Uani 1 1 d . . . H48 H 0.3403 0.2751 -0.2134 0.067 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 0.03169(9) 0.02884(8) 0.02520(8) -0.00010(6) 0.00386(6) 0.00151(6) Cl1 0.0380(6) 0.0483(6) 0.0447(6) 0.0016(5) 0.0013(5) -0.0067(4) Cl2 0.0494(6) 0.0342(5) 0.0408(6) 0.0063(4) 0.0045(5) 0.0027(4) P1 0.0455(7) 0.0400(5) 0.0330(6) -0.0052(5) 0.0078(5) 0.0067(5) P2 0.0326(6) 0.0371(5) 0.0276(5) -0.0027(4) 0.0048(4) 0.0008(4) O1 0.052(2) 0.078(2) 0.080(3) 0.032(2) 0.032(2) 0.0200(18) O2 0.0411(19) 0.0452(17) 0.074(2) 0.0125(16) 0.0019(17) -0.0100(14) N1 0.0326(18) 0.0318(16) 0.0312(17) -0.0033(13) 0.0072(15) -0.0002(13) N2 0.041(2) 0.0358(17) 0.0326(18) 0.0088(14) 0.0089(16) 0.0067(14) C1 0.044(3) 0.041(2) 0.044(3) 0.0086(19) 0.015(2) 0.0040(19) C2 0.043(3) 0.044(2) 0.043(2) 0.0084(19) 0.009(2) -0.0035(19) C3 0.053(3) 0.058(3) 0.060(3) 0.023(2) 0.011(3) 0.006(2) C4 0.066(4) 0.072(4) 0.096(5) 0.037(3) 0.019(4) 0.017(3) C5 0.075(5) 0.084(4) 0.112(6) 0.065(4) 0.008(4) 0.007(3) C6 0.087(5) 0.141(6) 0.106(6) 0.087(5) 0.041(4) 0.019(5) C7 0.065(4) 0.095(4) 0.076(4) 0.045(3) 0.033(3) 0.014(3) C8 0.036(2) 0.040(2) 0.031(2) 0.0003(17) 0.0060(18) 0.0007(17) C9 0.025(4) 0.070(6) 0.051(6) -0.005(5) 0.018(4) -0.007(4) C9' 0.045(9) 0.080(11) 0.070(12) -0.002(9) 0.023(8) -0.019(8) C10 0.037(3) 0.077(4) 0.067(4) 0.002(3) 0.005(3) -0.004(2) C11 0.036(2) 0.055(3) 0.044(3) 0.005(2) 0.004(2) 0.006(2) C12 0.061(11) 0.084(11) 0.170(19) -0.064(10) 0.037(10) -0.020(8) C12' 0.055(11) 0.038(10) 0.16(3) 0.013(14) 0.041(17) -0.008(9) C13 0.054(3) 0.043(2) 0.028(2) -0.0052(17) 0.007(2) 0.005(2) C14 0.056(3) 0.057(3) 0.033(2) -0.003(2) 0.009(2) -0.001(2) C15 0.059(3) 0.073(3) 0.037(3) -0.006(2) 0.000(2) 0.008(3) C16 0.083(4) 0.069(3) 0.033(3) 0.000(2) 0.002(3) 0.005(3) C17 0.092(5) 0.075(4) 0.045(3) 0.001(3) 0.029(3) -0.008(3) C18 0.063(3) 0.070(3) 0.038(3) -0.001(2) 0.017(2) 0.007(3) C19 0.051(3) 0.062(3) 0.039(3) -0.012(2) 0.013(2) 0.012(2) C20 0.049(3) 0.075(3) 0.048(3) -0.008(2) 0.017(2) 0.010(2) C21 0.050(3) 0.106(4) 0.061(4) -0.012(3) 0.024(3) 0.006(3) C22 0.048(4) 0.134(6) 0.073(4) -0.020(4) 0.015(3) 0.025(4) C23 0.065(4) 0.103(5) 0.092(5) -0.019(4) 0.013(4) 0.039(4) C24 0.060(4) 0.070(3) 0.068(4) -0.014(3) 0.008(3) 0.024(3) C25 0.050(3) 0.040(2) 0.046(3) -0.011(2) 0.001(2) 0.008(2) C26 0.109(5) 0.058(3) 0.061(4) -0.021(3) 0.021(3) 0.006(3) C27 0.115(6) 0.068(4) 0.074(4) -0.041(3) 0.012(4) 0.006(4) C28 0.068(4) 0.040(3) 0.111(5) -0.025(3) 0.005(4) 0.005(3) C29 0.071(4) 0.047(3) 0.089(4) -0.011(3) 0.009(3) -0.002(3) C30 0.064(3) 0.043(3) 0.054(3) -0.009(2) 0.006(3) -0.001(2) C31 0.033(2) 0.041(2) 0.027(2) -0.0049(16) 0.0044(17) -0.0016(17) C32 0.050(3) 0.042(2) 0.036(2) -0.0012(18) 0.000(2) 0.006(2) C33 0.052(3) 0.063(3) 0.036(2) 0.001(2) -0.002(2) 0.013(2) C34 0.048(3) 0.077(3) 0.035(3) -0.014(2) -0.006(2) -0.008(2) C35 0.070(4) 0.045(3) 0.046(3) -0.014(2) 0.001(3) -0.010(2) C36 0.055(3) 0.041(2) 0.039(2) -0.0091(19) 0.003(2) 0.004(2) C37 0.043(3) 0.046(2) 0.030(2) -0.0076(17) 0.0043(19) 0.0107(19) C38 0.059(3) 0.046(3) 0.041(3) -0.001(2) 0.001(2) 0.008(2) C39 0.093(5) 0.043(3) 0.052(3) -0.005(2) 0.001(3) 0.007(3) C40 0.094(5) 0.069(4) 0.058(4) -0.007(3) -0.004(3) 0.038(4) C41 0.052(3) 0.089(4) 0.064(4) -0.015(3) -0.001(3) 0.036(3) C42 0.045(3) 0.070(3) 0.059(3) -0.011(3) 0.005(3) 0.014(2) C43 0.038(3) 0.072(3) 0.032(2) -0.006(2) 0.008(2) -0.007(2) C44 0.088(5) 0.105(5) 0.070(4) -0.040(3) 0.045(4) -0.036(4) C45 0.113(6) 0.175(8) 0.076(5) -0.049(5) 0.068(5) -0.045(6) C46 0.078(5) 0.161(7) 0.056(4) 0.015(4) 0.029(4) -0.031(5) C47 0.061(4) 0.092(4) 0.077(4) 0.035(4) 0.025(3) 0.004(3) C48 0.051(3) 0.062(3) 0.056(3) 0.021(2) 0.020(3) 0.010(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 1.751(3) . ? Re1 C8 1.990(4) . ? Re1 Cl2 2.4346(10) . ? Re1 P2 2.4840(10) . ? Re1 P1 2.4995(11) . ? Re1 Cl1 2.5058(11) . ? P1 C19 1.829(5) . ? P1 C13 1.832(4) . ? P1 C25 1.842(4) . ? P2 C37 1.822(4) . ? P2 C43 1.824(5) . ? P2 C31 1.830(4) . ? O1 C1 1.209(5) . ? O2 C8 1.326(5) . ? O2 C9' 1.477(17) . ? O2 C9 1.536(10) . ? N1 N2 1.246(4) . ? N2 C1 1.399(5) . ? C1 C2 1.484(6) . ? C2 C7 1.379(7) . ? C2 C3 1.381(7) . ? C3 C4 1.385(7) . ? C3 H3 0.9300 . ? C4 C5 1.370(9) . ? C4 H4 0.9300 . ? C5 C6 1.367(10) . ? C5 H5 0.9300 . ? C6 C7 1.377(8) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C11 1.514(6) . ? C9 C9' 0.767(15) . ? C9 C12' 1.29(3) . ? C9 C10 1.460(12) . ? C9 C12 1.54(2) . ? C9 H9 0.887(9) . ? C9 H9' 1.500(9) . ? C9' C12 1.32(3) . ? C9' C12' 1.40(3) . ? C9' C10 1.514(19) . ? C9' H9' 0.736(18) . ? C9' H123 1.485(19) . ? C10 C11 1.515(6) . ? C10 H101 0.971(5) . ? C10 H102 0.967(6) . ? C11 H111 0.9700 . ? C11 H112 0.9700 . ? C12 C12' 0.59(4) . ? C12 H9' 1.51(3) . ? C12 H121 1.04(3) . ? C12 H122 0.99(3) . ? C12 H123 0.79(2) . ? C12 H124 0.88(3) . ? C12 H125 0.85(3) . ? C12 H126 1.28(3) . ? C12' H9 1.57(3) . ? C12' H121 0.99(4) . ? C12' H122 0.87(3) . ? C12' H123 1.38(3) . ? C12' H124 1.22(3) . ? C12' H125 1.01(4) . ? C12' H126 0.76(3) . ? C13 C18 1.384(6) . ? C13 C14 1.384(6) . ? C14 C15 1.379(7) . ? C14 H14 0.9300 . ? C15 C16 1.366(7) . ? C15 H15 0.9300 . ? C16 C17 1.387(8) . ? C16 H16 0.9300 . ? C17 C18 1.374(7) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.392(7) . ? C19 C24 1.396(7) . ? C20 C21 1.379(7) . ? C20 H20 0.9300 . ? C21 C22 1.381(8) . ? C21 H21 0.9300 . ? C22 C23 1.358(9) . ? C22 H22 0.9300 . ? C23 C24 1.385(8) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C30 1.378(7) . ? C25 C26 1.383(7) . ? C26 C27 1.390(8) . ? C26 H26 0.9300 . ? C27 C28 1.353(9) . ? C27 H27 0.9300 . ? C28 C29 1.352(8) . ? C28 H28 0.9300 . ? C29 C30 1.383(7) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C36 1.385(5) . ? C31 C32 1.389(6) . ? C32 C33 1.383(6) . ? C32 H32 0.9300 . ? C33 C34 1.367(7) . ? C33 H33 0.9300 . ? C34 C35 1.372(7) . ? C34 H34 0.9300 . ? C35 C36 1.375(6) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.371(6) . ? C37 C42 1.398(6) . ? C38 C39 1.390(6) . ? C38 H38 0.9300 . ? C39 C40 1.377(8) . ? C39 H39 0.9300 . ? C40 C41 1.361(9) . ? C40 H40 0.9300 . ? C41 C42 1.378(7) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C48 1.372(7) . ? C43 C44 1.392(7) . ? C44 C45 1.394(8) . ? C44 H44 0.9300 . ? C45 C46 1.386(10) . ? C45 H45 0.9300 . ? C46 C47 1.363(9) . ? C46 H46 0.9300 . ? C47 C48 1.384(7) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Re1 C8 91.87(15) . . ? N1 Re1 Cl2 178.12(11) . . ? C8 Re1 Cl2 86.71(12) . . ? N1 Re1 P2 89.82(10) . . ? C8 Re1 P2 88.31(12) . . ? Cl2 Re1 P2 91.36(4) . . ? N1 Re1 P1 88.94(10) . . ? C8 Re1 P1 94.71(12) . . ? Cl2 Re1 P1 89.96(4) . . ? P2 Re1 P1 176.77(4) . . ? N1 Re1 Cl1 93.15(11) . . ? C8 Re1 Cl1 174.56(12) . . ? Cl2 Re1 Cl1 88.32(4) . . ? P2 Re1 Cl1 89.62(4) . . ? P1 Re1 Cl1 87.47(4) . . ? C19 P1 C13 105.4(2) . . ? C19 P1 C25 103.0(2) . . ? C13 P1 C25 102.1(2) . . ? C19 P1 Re1 111.84(15) . . ? C13 P1 Re1 111.05(14) . . ? C25 P1 Re1 121.80(17) . . ? C37 P2 C43 104.0(2) . . ? C37 P2 C31 108.11(19) . . ? C43 P2 C31 98.91(19) . . ? C37 P2 Re1 106.86(13) . . ? C43 P2 Re1 121.92(16) . . ? C31 P2 Re1 115.93(13) . . ? C8 O2 C9' 112.9(8) . . ? C8 O2 C9 111.8(5) . . ? C9' O2 C9 29.4(6) . . ? N2 N1 Re1 174.4(3) . . ? N1 N2 C1 119.5(3) . . ? O1 C1 N2 124.8(4) . . ? O1 C1 C2 122.7(4) . . ? N2 C1 C2 112.4(4) . . ? C7 C2 C3 119.2(4) . . ? C7 C2 C1 118.1(4) . . ? C3 C2 C1 122.8(4) . . ? C2 C3 C4 121.1(5) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 118.6(6) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? C6 C5 C4 120.8(5) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 120.5(6) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C6 C7 C2 119.7(6) . . ? C6 C7 H7 120.1 . . ? C2 C7 H7 120.1 . . ? O2 C8 C11 107.8(3) . . ? O2 C8 Re1 121.3(3) . . ? C11 C8 Re1 130.9(3) . . ? C9' C9 C12' 81(2) . . ? C9' C9 C10 79.0(19) . . ? C12' C9 C10 133.7(19) . . ? C9' C9 O2 71.0(16) . . ? C12' C9 O2 110.3(17) . . ? C10 C9 O2 102.0(6) . . ? C9' C9 C12 59.1(19) . . ? C12' C9 C12 22(2) . . ? C10 C9 C12 120.2(14) . . ? O2 C9 C12 102.0(12) . . ? C9' C9 H9 171(2) . . ? C12' C9 H9 90.3(16) . . ? C10 C9 H9 109.8(9) . . ? O2 C9 H9 109.0(8) . . ? C12 C9 H9 112.4(13) . . ? C9' C9 H9' 3.6(16) . . ? C12' C9 H9' 81.8(15) . . ? C10 C9 H9' 76.1(5) . . ? O2 C9 H9' 74.0(4) . . ? C12 C9 H9' 59.7(11) . . ? H9 C9 H9' 172.1(11) . . ? C9 C9' C12 91(2) . . ? C9 C9' C12' 66.1(19) . . ? C12 C9' C12' 25.1(17) . . ? C9 C9' O2 79.6(18) . . ? C12 C9' O2 117.3(19) . . ? C12' C9' O2 108(2) . . ? C9 C9' C10 71.2(19) . . ? C12 C9' C10 133.0(17) . . ? C12' C9' C10 120.8(17) . . ? O2 C9' C10 102.2(11) . . ? C9 C9' H9' 173(3) . . ? C12 C9' H9' 90(2) . . ? C12' C9' H9' 115(2) . . ? O2 C9' H9' 106.4(15) . . ? C10 C9' H9' 102.8(17) . . ? C9 C9' H123 123(2) . . ? C12 C9' H123 32.2(11) . . ? C12' C9' H123 57.2(15) . . ? O2 C9' H123 121.0(13) . . ? C10 C9' H123 135.7(13) . . ? H9' C9' H123 58.0(12) . . ? C9 C10 C9' 29.8(6) . . ? C9 C10 C11 106.0(5) . . ? C9' C10 C11 105.7(7) . . ? C9 C10 H101 107.0(6) . . ? C9' C10 H101 131.1(8) . . ? C11 C10 H101 110.7(5) . . ? C9 C10 H102 113.6(6) . . ? C9' C10 H102 86.8(8) . . ? C11 C10 H102 110.8(5) . . ? H101 C10 H102 108.7(5) . . ? C8 C11 C10 105.2(4) . . ? C8 C11 H111 110.7 . . ? C10 C11 H111 110.7 . . ? C8 C11 H112 110.7 . . ? C10 C11 H112 110.7 . . ? H111 C11 H112 108.8 . . ? C12' C12 C9' 85(4) . . ? C12' C12 C9 55(4) . . ? C9' C12 C9 29.9(8) . . ? C12' C12 H9' 114(5) . . ? C9' C12 H9' 29.1(11) . . ? C9 C12 H9' 58.8(10) . . ? C12' C12 H121 68(5) . . ? C9' C12 H121 114(2) . . ? C9 C12 H121 96.5(14) . . ? H9' C12 H121 123(3) . . ? C12' C12 H122 61(5) . . ? C9' C12 H122 116(2) . . ? C9 C12 H122 98.8(17) . . ? H9' C12 H122 131(2) . . ? H121 C12 H122 101(2) . . ? C12' C12 H123 170(7) . . ? C9' C12 H123 85(3) . . ? C9 C12 H123 115(3) . . ? H9' C12 H123 56.3(17) . . ? H121 C12 H123 117(3) . . ? H122 C12 H123 123(3) . . ? C12' C12 H124 111(7) . . ? C9' C12 H124 109(3) . . ? C9 C12 H124 119(2) . . ? H9' C12 H124 98(2) . . ? H121 C12 H124 137(3) . . ? H122 C12 H124 52.3(17) . . ? H123 C12 H124 71.2(16) . . ? C12' C12 H125 87(6) . . ? C9' C12 H125 119(3) . . ? C9 C12 H125 109.2(19) . . ? H9' C12 H125 117(3) . . ? H121 C12 H125 19.0(6) . . ? H122 C12 H125 112(3) . . ? H123 C12 H125 98(3) . . ? H124 C12 H125 130(3) . . ? C12' C12 H126 22(4) . . ? C9' C12 H126 101.0(15) . . ? C9 C12 H126 73.0(10) . . ? H9' C12 H126 129.2(16) . . ? H121 C12 H126 75.2(15) . . ? H122 C12 H126 39.6(10) . . ? H123 C12 H126 163(3) . . ? H124 C12 H126 92(3) . . ? H125 C12 H126 93(2) . . ? C12 C12' C9 103(5) . . ? C12 C12' C9' 70(5) . . ? C9 C12' C9' 32.8(10) . . ? C12 C12' H9 137(5) . . ? C9 C12' H9 34.4(8) . . ? C9' C12' H9 67.2(14) . . ? C12 C12' H121 78(6) . . ? C9 C12' H121 117(3) . . ? C9' C12' H121 112(3) . . ? H9 C12' H121 115(2) . . ? C12 C12' H122 82(5) . . ? C9 C12' H122 128(4) . . ? C9' C12' H122 118(3) . . ? H9 C12' H122 121(3) . . ? H121 C12' H122 115(3) . . ? C12 C12' H123 6(4) . . ? C9 C12' H123 97.3(19) . . ? C9' C12' H123 64.6(15) . . ? H9 C12' H123 131.7(18) . . ? H121 C12' H123 81(2) . . ? H122 C12' H123 85(2) . . ? C12 C12' H124 42(5) . . ? C9 C12' H124 114(2) . . ? C9' C12' H124 86.8(19) . . ? H9 C12' H124 136(3) . . ? H121 C12' H124 107(2) . . ? H122 C12' H124 42.4(13) . . ? H123 C12' H124 43.3(10) . . ? C12 C12' H125 57(5) . . ? C9 C12' H125 119(3) . . ? C9' C12' H125 101(3) . . ? H9 C12' H125 129(3) . . ? H121 C12' H125 20.8(8) . . ? H122 C12' H125 108(2) . . ? H123 C12' H125 60.3(17) . . ? H124 C12' H125 88(2) . . ? C12 C12' H126 140(7) . . ? C9 C12' H126 108(3) . . ? C9' C12' H126 134(4) . . ? H9 C12' H126 77(2) . . ? H121 C12' H126 109(3) . . ? H122 C12' H126 59(2) . . ? H123 C12' H126 144(3) . . ? H124 C12' H126 102(3) . . ? H125 C12' H126 123(3) . . ? C18 C13 C14 118.0(4) . . ? C18 C13 P1 124.5(4) . . ? C14 C13 P1 117.5(3) . . ? C15 C14 C13 121.4(5) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C16 C15 C14 119.9(5) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 119.6(5) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C18 C17 C16 120.3(5) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C13 120.8(5) . . ? C17 C18 H18 119.6 . . ? C13 C18 H18 119.6 . . ? C20 C19 C24 118.7(5) . . ? C20 C19 P1 119.6(4) . . ? C24 C19 P1 121.4(4) . . ? C21 C20 C19 120.8(5) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C22 120.0(6) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 119.6(6) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 C24 121.8(6) . . ? C22 C23 H23 119.1 . . ? C24 C23 H23 119.1 . . ? C23 C24 C19 119.2(6) . . ? C23 C24 H24 120.4 . . ? C19 C24 H24 120.4 . . ? C30 C25 C26 118.7(5) . . ? C30 C25 P1 122.3(3) . . ? C26 C25 P1 119.0(4) . . ? C25 C26 C27 119.8(6) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C28 C27 C26 120.8(6) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C29 C28 C27 119.6(5) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C28 C29 C30 121.1(6) . . ? C28 C29 H29 119.5 . . ? C30 C29 H29 119.5 . . ? C25 C30 C29 120.0(5) . . ? C25 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C36 C31 C32 118.6(4) . . ? C36 C31 P2 125.1(3) . . ? C32 C31 P2 116.2(3) . . ? C33 C32 C31 120.4(4) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C34 C33 C32 119.7(4) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 120.6(4) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? C34 C35 C36 119.9(4) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C35 C36 C31 120.7(4) . . ? C35 C36 H36 119.7 . . ? C31 C36 H36 119.7 . . ? C38 C37 C42 118.7(4) . . ? C38 C37 P2 121.8(3) . . ? C42 C37 P2 118.8(4) . . ? C37 C38 C39 120.8(5) . . ? C37 C38 H38 119.6 . . ? C39 C38 H38 119.6 . . ? C40 C39 C38 119.4(6) . . ? C40 C39 H39 120.3 . . ? C38 C39 H39 120.3 . . ? C41 C40 C39 120.3(5) . . ? C41 C40 H40 119.8 . . ? C39 C40 H40 119.8 . . ? C40 C41 C42 120.4(6) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C41 C42 C37 120.1(6) . . ? C41 C42 H42 119.9 . . ? C37 C42 H42 119.9 . . ? C48 C43 C44 119.1(5) . . ? C48 C43 P2 122.4(4) . . ? C44 C43 P2 118.4(4) . . ? C43 C44 C45 119.6(6) . . ? C43 C44 H44 120.2 . . ? C45 C44 H44 120.2 . . ? C46 C45 C44 120.1(6) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C47 C46 C45 120.0(6) . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C46 C47 C48 120.0(6) . . ? C46 C47 H47 120.0 . . ? C48 C47 H47 120.0 . . ? C43 C48 C47 121.2(5) . . ? C43 C48 H48 119.4 . . ? C47 C48 H48 119.4 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.583 _refine_diff_density_min -1.163 _refine_diff_density_rms 0.101 ###===END data_(3b) _database_code_depnum_ccdc_archive 'CCDC 225819' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H43 Cl2 N2 O2 P2 Re, C2 H6 O' _chemical_formula_sum 'C50 H49 Cl2 N2 O3 P2 Re' _chemical_formula_weight 1044.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 18.5316(3) _cell_length_b 11.9170(2) _cell_length_c 20.5233(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.718(1) _cell_angle_gamma 90.00 _cell_volume 4530.3(1) _cell_formula_units_Z 4 _cell_measurement_temperature 295 _cell_measurement_reflns_used 35232 _cell_measurement_theta_min 3.60 _cell_measurement_theta_max 28.00 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 2.915 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.641 _exptl_absorpt_correction_T_max 0.885 _exptl_absorpt_process_details ; SORTAV (R.H. Blessing, Acta Crystallogr., 1995, A51, 33) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295 _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '\f scans and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35232 _diffrn_reflns_av_R_equivalents 0.047 _diffrn_reflns_av_sigmaI/netI 0.0539 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.60 _diffrn_reflns_theta_max 28.00 _reflns_number_total 10891 _reflns_number_gt 8375 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Kappa CCd server software (Nonius, 1997)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP II (Johnson, 1976)' _computing_publication_material ; SHELXL-97 (Sheldrick, 1997), PARST (Nardelli, 1995) ; _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^)+(0.0456P)^2^+9.2398P] 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 SHELXL _refine_ls_extinction_coef 0.00076(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10891 _refine_ls_number_parameters 529 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1235 _refine_ls_wR_factor_gt 0.1080 _refine_ls_goodness_of_fit_ref 1.151 _refine_ls_restrained_S_all 1.151 _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 0.785824(11) 0.851391(17) 0.878547(10) 0.03648(9) Uani 1 1 d . . . P1 P 0.80480(8) 0.64480(11) 0.88689(6) 0.0355(3) Uani 1 1 d . . . P2 P 0.76885(8) 1.05831(12) 0.86875(7) 0.0416(3) Uani 1 1 d . . . Cl1 Cl 0.78175(11) 0.83449(14) 0.75674(7) 0.0620(4) Uani 1 1 d . . . Cl2 Cl 0.91647(8) 0.86625(13) 0.87284(8) 0.0543(4) Uani 1 1 d . . . O1 O 0.6197(3) 0.7093(6) 0.9690(3) 0.0875(17) Uani 1 1 d . . . O2 O 0.7398(3) 0.8808(4) 1.0130(2) 0.0651(12) Uani 1 1 d . . . N1 N 0.6922(3) 0.8322(4) 0.8829(2) 0.0410(11) Uani 1 1 d . . . N2 N 0.6265(3) 0.8186(4) 0.8759(3) 0.0514(12) Uani 1 1 d . . . C1 C 0.5894(3) 0.7541(6) 0.9220(3) 0.0575(16) Uani 1 1 d . . . C2 C 0.5106(3) 0.7445(6) 0.9076(3) 0.0577(16) Uani 1 1 d . . . C3 C 0.4702(4) 0.6750(8) 0.9467(4) 0.083(2) Uani 1 1 d . . . H3 H 0.4922 0.6363 0.9813 0.099 Uiso 1 1 calc R . . C4 C 0.3960(5) 0.6639(10) 0.9337(5) 0.106(3) Uani 1 1 d . . . H4 H 0.3685 0.6185 0.9602 0.127 Uiso 1 1 calc R . . C5 C 0.3640(5) 0.7189(9) 0.8826(5) 0.096(3) Uani 1 1 d . . . H5 H 0.3145 0.7118 0.8744 0.116 Uiso 1 1 calc R . . C6 C 0.4031(5) 0.7824(9) 0.8448(5) 0.097(3) Uani 1 1 d . . . H6 H 0.3807 0.8189 0.8096 0.116 Uiso 1 1 calc R . . C7 C 0.4775(4) 0.7965(7) 0.8560(4) 0.077(2) Uani 1 1 d . . . H7 H 0.5040 0.8411 0.8283 0.093 Uiso 1 1 calc R . . C8 C 0.7971(3) 0.8744(4) 0.9751(3) 0.0429(13) Uani 1 1 d . . . C9 C 0.7600(5) 0.8990(8) 1.0825(4) 0.081(2) Uani 1 1 d . . . H9 H 0.7586 0.8246 1.1029 0.097 Uiso 1 1 calc R . . C10 C 0.8369(5) 0.9297(9) 1.0815(4) 0.093(3) Uani 1 1 d . . . H101 H 0.8637 0.8943 1.1172 0.112 Uiso 1 1 calc R . . H102 H 0.8429 1.0104 1.0848 0.112 Uiso 1 1 calc R . . C11 C 0.8619(4) 0.8878(6) 1.0175(3) 0.0529(15) Uani 1 1 d . . . H111 H 0.8948 0.9411 0.9986 0.063 Uiso 1 1 calc R . . H112 H 0.8866 0.8166 1.0230 0.063 Uiso 1 1 calc R . . C12 C 0.7055(6) 0.9621(12) 1.1123(5) 0.137(5) Uani 1 1 d . . . H121 H 0.6590 0.9347 1.0981 0.164 Uiso 1 1 calc R . . H122 H 0.7100 1.0396 1.1004 0.164 Uiso 1 1 calc R . . H123 H 0.7106 0.9549 1.1588 0.164 Uiso 1 1 calc R . . C13 C 0.8317(3) 0.6102(4) 0.9705(3) 0.0402(12) Uani 1 1 d . . . C14 C 0.9057(3) 0.5967(5) 0.9871(3) 0.0454(13) Uani 1 1 d . . . H14 H 0.9398 0.5952 0.9548 0.054 Uiso 1 1 calc R . . C15 C 0.9268(4) 0.5857(5) 1.0519(3) 0.0558(16) Uani 1 1 d . . . H15 H 0.9756 0.5788 1.0629 0.067 Uiso 1 1 calc R . . C16 C 0.8778(4) 0.5848(5) 1.1000(3) 0.0591(17) Uani 1 1 d . . . H16 H 0.8931 0.5761 1.1433 0.071 Uiso 1 1 calc R . . C17 C 0.8053(4) 0.5970(6) 1.0839(3) 0.0616(17) Uani 1 1 d . . . H17 H 0.7717 0.5940 1.1167 0.074 Uiso 1 1 calc R . . C18 C 0.7821(3) 0.6133(5) 1.0212(3) 0.0430(13) Uani 1 1 d . . . H18 H 0.7335 0.6266 1.0117 0.052 Uiso 1 1 calc R . . C19 C 0.7234(3) 0.5630(4) 0.8669(3) 0.0388(12) Uani 1 1 d . . . C20 C 0.6991(3) 0.4754(5) 0.9039(3) 0.0546(15) Uani 1 1 d . . . H20 H 0.7233 0.4564 0.9427 0.065 Uiso 1 1 calc R . . C21 C 0.6376(4) 0.4146(6) 0.8829(4) 0.0658(19) Uani 1 1 d . . . H21 H 0.6222 0.3540 0.9074 0.079 Uiso 1 1 calc R . . C22 C 0.6004(4) 0.4434(6) 0.8273(4) 0.0671(19) Uani 1 1 d . . . H22 H 0.5586 0.4050 0.8147 0.081 Uiso 1 1 calc R . . C23 C 0.6251(4) 0.5294(6) 0.7903(4) 0.070(2) Uani 1 1 d . . . H23 H 0.6008 0.5470 0.7513 0.084 Uiso 1 1 calc R . . C24 C 0.6858(3) 0.5914(6) 0.8092(3) 0.0546(16) Uani 1 1 d . . . H24 H 0.7012 0.6509 0.7838 0.066 Uiso 1 1 calc R . . C25 C 0.8717(3) 0.5711(5) 0.8387(3) 0.0431(13) Uani 1 1 d . . . C26 C 0.8864(3) 0.4588(5) 0.8540(3) 0.0484(14) Uani 1 1 d . . . H26 H 0.8631 0.4241 0.8881 0.058 Uiso 1 1 calc R . . C27 C 0.9360(4) 0.3992(6) 0.8180(3) 0.0599(17) Uani 1 1 d . . . H27 H 0.9461 0.3248 0.8285 0.072 Uiso 1 1 calc R . . C28 C 0.9696(4) 0.4484(7) 0.7679(4) 0.071(2) Uani 1 1 d . . . H28 H 1.0029 0.4079 0.7444 0.086 Uiso 1 1 calc R . . C29 C 0.9547(4) 0.5583(8) 0.7517(4) 0.076(2) Uani 1 1 d . . . H29 H 0.9777 0.5914 0.7168 0.092 Uiso 1 1 calc R . . C30 C 0.9056(4) 0.6202(6) 0.7870(3) 0.0633(18) Uani 1 1 d . . . H30 H 0.8957 0.6944 0.7758 0.076 Uiso 1 1 calc R . . C31 C 0.6724(3) 1.0835(5) 0.8757(4) 0.0539(16) Uani 1 1 d . . . C32 C 0.6394(4) 1.0748(6) 0.9345(4) 0.074(2) Uani 1 1 d . . . H32 H 0.6664 1.0596 0.9724 0.089 Uiso 1 1 calc R . . C33 C 0.5639(6) 1.0892(7) 0.9366(7) 0.107(4) Uani 1 1 d . . . H33 H 0.5411 1.0840 0.9763 0.128 Uiso 1 1 calc R . . C34 C 0.5239(5) 1.1108(9) 0.8808(10) 0.129(6) Uani 1 1 d . . . H34 H 0.4744 1.1226 0.8827 0.155 Uiso 1 1 calc R . . C35 C 0.5564(5) 1.1148(9) 0.8237(7) 0.113(4) Uani 1 1 d . . . H35 H 0.5284 1.1259 0.7859 0.136 Uiso 1 1 calc R . . C36 C 0.6292(4) 1.1031(7) 0.8189(5) 0.082(2) Uani 1 1 d . . . H36 H 0.6504 1.1081 0.7785 0.099 Uiso 1 1 calc R . . C37 C 0.8148(3) 1.1437(5) 0.9320(3) 0.0447(13) Uani 1 1 d . . . C38 C 0.8885(4) 1.1341(6) 0.9368(4) 0.0653(19) Uani 1 1 d . . . H38 H 0.9123 1.0846 0.9097 0.078 Uiso 1 1 calc R . . C39 C 0.9283(4) 1.1991(7) 0.9824(4) 0.074(2) Uani 1 1 d . . . H39 H 0.9782 1.1914 0.9862 0.089 Uiso 1 1 calc R . . C40 C 0.8936(4) 1.2732(6) 1.0211(3) 0.0643(19) Uani 1 1 d . . . H40 H 0.9198 1.3160 1.0514 0.077 Uiso 1 1 calc R . . C41 C 0.8215(4) 1.2848(6) 1.0157(3) 0.0656(19) Uani 1 1 d . . . H41 H 0.7982 1.3363 1.0418 0.079 Uiso 1 1 calc R . . C42 C 0.7816(4) 1.2200(5) 0.9712(3) 0.0575(16) Uani 1 1 d . . . H42 H 0.7317 1.2287 0.9680 0.069 Uiso 1 1 calc R . . C43 C 0.7952(3) 1.1368(5) 0.7965(3) 0.0464(14) Uani 1 1 d . . . C44 C 0.7672(4) 1.2442(5) 0.7861(3) 0.0535(15) Uani 1 1 d . . . H44 H 0.7331 1.2726 0.8141 0.064 Uiso 1 1 calc R . . C45 C 0.7896(4) 1.3090(6) 0.7345(4) 0.0663(19) Uani 1 1 d . . . H45 H 0.7708 1.3806 0.7279 0.080 Uiso 1 1 calc R . . C46 C 0.8391(5) 1.2673(6) 0.6938(3) 0.068(2) Uani 1 1 d . . . H46 H 0.8530 1.3099 0.6584 0.082 Uiso 1 1 calc R . . C47 C 0.8695(5) 1.1622(6) 0.7040(4) 0.072(2) Uani 1 1 d . . . H47 H 0.9051 1.1361 0.6769 0.087 Uiso 1 1 calc R . . C48 C 0.8465(4) 1.0964(5) 0.7551(3) 0.0583(17) Uani 1 1 d . . . H48 H 0.8655 1.0249 0.7614 0.070 Uiso 1 1 calc R . . O1A O 0.5837(9) 0.8229(14) 0.7165(9) 0.263(7) Uiso 1 1 d . . . H1A H 0.5815 0.8421 0.7547 0.315 Uiso 1 1 calc R . . C1A C 0.6014(11) 0.9160(19) 0.6782(11) 0.221(8) Uiso 1 1 d . . . H11A H 0.6487 0.9461 0.6900 0.265 Uiso 1 1 calc R . . H12A H 0.5654 0.9749 0.6800 0.265 Uiso 1 1 calc R . . C2A C 0.6004(10) 0.8606(13) 0.6165(9) 0.184(7) Uiso 1 1 d . . . H21A H 0.5514 0.8511 0.6011 0.221 Uiso 1 1 calc R . . H22A H 0.6231 0.7885 0.6211 0.221 Uiso 1 1 calc R . . H23A H 0.6262 0.9050 0.5859 0.221 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 0.03674(13) 0.03978(13) 0.03272(13) 0.00102(9) -0.00229(8) -0.00034(10) P1 0.0353(7) 0.0406(7) 0.0304(7) 0.0008(5) -0.0016(5) 0.0009(6) P2 0.0411(8) 0.0389(7) 0.0446(8) -0.0001(6) -0.0015(6) 0.0010(6) Cl1 0.0881(13) 0.0630(10) 0.0344(7) 0.0054(7) -0.0063(7) -0.0072(8) Cl2 0.0418(8) 0.0633(10) 0.0580(9) -0.0026(7) 0.0061(7) -0.0051(7) O1 0.056(3) 0.132(5) 0.074(4) 0.037(3) -0.005(3) -0.006(3) O2 0.062(3) 0.084(3) 0.049(3) -0.012(2) 0.001(2) -0.002(2) N1 0.051(3) 0.047(3) 0.025(2) 0.0052(18) 0.006(2) 0.004(2) N2 0.039(3) 0.053(3) 0.062(3) 0.003(2) -0.001(2) 0.001(2) C1 0.041(4) 0.071(4) 0.060(4) -0.002(3) 0.002(3) 0.000(3) C2 0.044(4) 0.070(4) 0.059(4) -0.004(3) 0.003(3) -0.004(3) C3 0.055(5) 0.121(7) 0.072(5) 0.011(5) 0.005(4) -0.013(4) C4 0.073(6) 0.147(10) 0.098(7) 0.015(7) 0.016(5) -0.034(6) C5 0.052(5) 0.135(9) 0.102(7) 0.015(6) 0.000(5) -0.008(5) C6 0.056(5) 0.120(8) 0.115(8) 0.025(6) -0.012(5) 0.002(5) C7 0.055(5) 0.084(5) 0.092(6) 0.018(5) -0.016(4) -0.004(4) C8 0.042(3) 0.042(3) 0.045(3) 0.000(2) -0.001(3) -0.001(2) C9 0.099(7) 0.097(6) 0.046(4) -0.015(4) 0.012(4) -0.003(5) C10 0.097(7) 0.132(8) 0.049(4) -0.021(5) -0.014(4) -0.016(6) C11 0.056(4) 0.057(3) 0.045(3) -0.004(3) -0.005(3) -0.004(3) C12 0.138(10) 0.186(13) 0.088(7) -0.057(8) 0.021(7) -0.010(9) C13 0.045(3) 0.037(3) 0.038(3) 0.000(2) -0.006(2) 0.001(2) C14 0.042(3) 0.042(3) 0.052(4) -0.004(3) -0.004(3) 0.003(2) C15 0.058(4) 0.048(3) 0.060(4) -0.004(3) -0.021(3) 0.009(3) C16 0.078(5) 0.059(4) 0.040(3) 0.004(3) -0.017(3) 0.002(3) C17 0.070(5) 0.069(4) 0.047(4) 0.001(3) 0.007(3) -0.006(4) C18 0.034(3) 0.059(3) 0.036(3) 0.013(2) -0.003(2) 0.002(2) C19 0.035(3) 0.040(3) 0.042(3) -0.005(2) 0.001(2) -0.002(2) C20 0.050(4) 0.053(4) 0.060(4) -0.001(3) -0.003(3) -0.002(3) C21 0.062(4) 0.051(4) 0.084(5) 0.000(3) 0.003(4) -0.023(3) C22 0.047(4) 0.072(5) 0.081(5) -0.020(4) -0.006(4) -0.013(3) C23 0.060(4) 0.070(5) 0.078(5) -0.006(4) -0.028(4) -0.004(4) C24 0.052(4) 0.058(4) 0.053(4) -0.003(3) -0.011(3) -0.007(3) C25 0.039(3) 0.058(3) 0.033(3) -0.006(2) -0.002(2) 0.000(3) C26 0.049(4) 0.051(3) 0.045(3) -0.010(3) 0.001(3) 0.004(3) C27 0.052(4) 0.064(4) 0.064(4) -0.020(3) -0.010(3) 0.016(3) C28 0.050(4) 0.094(6) 0.071(5) -0.026(4) 0.005(4) 0.016(4) C29 0.067(5) 0.104(6) 0.059(4) -0.013(4) 0.020(4) 0.002(4) C30 0.062(4) 0.076(4) 0.052(4) -0.007(3) 0.016(3) 0.001(4) C31 0.047(4) 0.037(3) 0.078(5) -0.004(3) -0.001(3) 0.000(3) C32 0.060(5) 0.057(4) 0.107(6) -0.002(4) 0.024(4) 0.003(3) C33 0.081(7) 0.070(6) 0.173(11) -0.019(6) 0.065(7) -0.007(5) C34 0.039(5) 0.083(7) 0.264(19) -0.017(9) -0.014(8) 0.004(5) C35 0.045(5) 0.111(8) 0.182(13) 0.003(8) -0.015(6) -0.001(5) C36 0.053(5) 0.080(5) 0.111(7) -0.012(5) -0.021(4) -0.008(4) C37 0.052(3) 0.040(3) 0.042(3) 0.004(2) -0.003(3) -0.006(3) C38 0.049(4) 0.064(4) 0.082(5) -0.020(4) 0.002(4) -0.005(3) C39 0.054(4) 0.072(5) 0.096(6) -0.014(4) -0.013(4) -0.016(4) C40 0.079(5) 0.054(4) 0.059(4) -0.006(3) -0.005(4) -0.021(4) C41 0.085(6) 0.059(4) 0.053(4) -0.012(3) -0.001(4) 0.003(4) C42 0.059(4) 0.052(4) 0.060(4) -0.011(3) -0.006(3) 0.002(3) C43 0.054(4) 0.042(3) 0.043(3) 0.004(2) -0.010(3) -0.002(3) C44 0.064(4) 0.046(3) 0.049(4) 0.003(3) -0.010(3) 0.006(3) C45 0.082(5) 0.050(4) 0.066(5) 0.013(3) -0.021(4) 0.000(4) C46 0.109(6) 0.051(4) 0.044(4) 0.008(3) -0.011(4) -0.017(4) C47 0.103(6) 0.061(4) 0.054(4) 0.001(3) 0.016(4) -0.001(4) C48 0.073(5) 0.045(3) 0.058(4) 0.005(3) 0.010(3) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 N1 1.755(5) . ? Re1 C8 2.005(6) . ? Re1 Cl2 2.4338(15) . ? Re1 P1 2.4921(14) . ? Re1 P2 2.4932(15) . ? Re1 Cl1 2.5069(15) . ? P1 C13 1.820(6) . ? P1 C19 1.832(5) . ? P1 C25 1.833(6) . ? P2 C31 1.822(7) . ? P2 C43 1.832(6) . ? P2 C37 1.838(6) . ? O1 C1 1.224(8) . ? O2 C8 1.338(7) . ? O2 C9 1.479(9) . ? N1 N2 1.233(7) . ? N2 C1 1.414(8) . ? C1 C2 1.486(9) . ? C2 C7 1.358(10) . ? C2 C3 1.388(10) . ? C3 C4 1.398(12) . ? C3 H3 0.9300 . ? C4 C5 1.358(13) . ? C4 H4 0.9300 . ? C5 C6 1.318(12) . ? C5 H5 0.9300 . ? C6 C7 1.401(11) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C11 1.470(8) . ? C9 C12 1.413(13) . ? C9 C10 1.472(12) . ? C9 H9 0.9800 . ? C10 C11 1.492(10) . ? C10 H101 0.9700 . ? C10 H102 0.9700 . ? C11 H111 0.9700 . ? C11 H112 0.9700 . ? C12 H121 0.9600 . ? C12 H122 0.9600 . ? C12 H123 0.9600 . ? C13 C18 1.410(8) . ? C13 C14 1.412(8) . ? C14 C15 1.381(8) . ? C14 H14 0.9300 . ? C15 C16 1.360(9) . ? C15 H15 0.9300 . ? C16 C17 1.382(10) . ? C16 H16 0.9300 . ? C17 C18 1.359(8) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.374(8) . ? C19 C24 1.398(8) . ? C20 C21 1.407(9) . ? C20 H20 0.9300 . ? C21 C22 1.360(10) . ? C21 H21 0.9300 . ? C22 C23 1.363(10) . ? C22 H22 0.9300 . ? C23 C24 1.392(9) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C30 1.380(9) . ? C25 C26 1.400(8) . ? C26 C27 1.391(8) . ? C26 H26 0.9300 . ? C27 C28 1.351(10) . ? C27 H27 0.9300 . ? C28 C29 1.378(11) . ? C28 H28 0.9300 . ? C29 C30 1.392(10) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.372(10) . ? C31 C36 1.414(11) . ? C32 C33 1.413(12) . ? C32 H32 0.9300 . ? C33 C34 1.369(17) . ? C33 H33 0.9300 . ? C34 C35 1.335(18) . ? C34 H34 0.9300 . ? C35 C36 1.363(12) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C42 1.372(8) . ? C37 C38 1.372(9) . ? C38 C39 1.406(10) . ? C38 H38 0.9300 . ? C39 C40 1.362(10) . ? C39 H39 0.9300 . ? C40 C41 1.344(10) . ? C40 H40 0.9300 . ? C41 C42 1.391(9) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C48 1.381(9) . ? C43 C44 1.396(8) . ? C44 C45 1.384(9) . ? C44 H44 0.9300 . ? C45 C46 1.354(11) . ? C45 H45 0.9300 . ? C46 C47 1.387(10) . ? C46 H46 0.9300 . ? C47 C48 1.386(9) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? O1A C1A 1.40(2) . ? O1A H1A 0.8200 . ? C1A C2A 1.43(2) . ? C1A H11A 0.9700 . ? C1A H12A 0.9700 . ? C2A H21A 0.9600 . ? C2A H22A 0.9600 . ? C2A H23A 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 C8 92.3(2) . . ? N1 Re1 Cl2 176.69(15) . . ? C8 Re1 Cl2 87.90(17) . . ? N1 Re1 P1 90.32(15) . . ? C8 Re1 P1 93.25(16) . . ? Cl2 Re1 P1 86.37(5) . . ? N1 Re1 P2 90.59(15) . . ? C8 Re1 P2 87.35(16) . . ? Cl2 Re1 P2 92.72(5) . . ? P1 Re1 P2 178.89(5) . . ? N1 Re1 Cl1 92.32(14) . . ? C8 Re1 Cl1 174.64(17) . . ? Cl2 Re1 Cl1 87.60(6) . . ? P1 Re1 Cl1 89.38(5) . . ? P2 Re1 Cl1 89.95(5) . . ? C13 P1 C19 106.9(3) . . ? C13 P1 C25 103.3(3) . . ? C19 P1 C25 100.9(2) . . ? C13 P1 Re1 108.82(18) . . ? C19 P1 Re1 113.39(18) . . ? C25 P1 Re1 122.2(2) . . ? C31 P2 C43 105.4(3) . . ? C31 P2 C37 106.7(3) . . ? C43 P2 C37 99.2(3) . . ? C31 P2 Re1 106.17(19) . . ? C43 P2 Re1 122.3(2) . . ? C37 P2 Re1 115.83(19) . . ? C8 O2 C9 112.8(5) . . ? N2 N1 Re1 170.3(4) . . ? N1 N2 C1 119.4(5) . . ? O1 C1 N2 122.9(6) . . ? O1 C1 C2 123.3(6) . . ? N2 C1 C2 113.8(6) . . ? C7 C2 C3 119.0(7) . . ? C7 C2 C1 122.6(7) . . ? C3 C2 C1 118.4(7) . . ? C2 C3 C4 119.4(8) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 120.4(9) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C6 C5 C4 119.8(9) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C7 121.9(9) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C2 C7 C6 119.5(8) . . ? C2 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? O2 C8 C11 107.3(5) . . ? O2 C8 Re1 121.5(4) . . ? C11 C8 Re1 131.2(4) . . ? C12 C9 C10 125.3(9) . . ? C12 C9 O2 109.4(8) . . ? C10 C9 O2 103.8(6) . . ? C12 C9 H9 105.6 . . ? C10 C9 H9 105.6 . . ? O2 C9 H9 105.6 . . ? C9 C10 C11 104.8(6) . . ? C9 C10 H101 110.8 . . ? C11 C10 H101 110.8 . . ? C9 C10 H102 110.8 . . ? C11 C10 H102 110.8 . . ? H101 C10 H102 108.9 . . ? C8 C11 C10 106.7(6) . . ? C8 C11 H111 110.4 . . ? C10 C11 H111 110.4 . . ? C8 C11 H112 110.4 . . ? C10 C11 H112 110.4 . . ? H111 C11 H112 108.6 . . ? C9 C12 H121 109.5 . . ? C9 C12 H122 109.5 . . ? H121 C12 H122 109.5 . . ? C9 C12 H123 109.5 . . ? H121 C12 H123 109.5 . . ? H122 C12 H123 109.5 . . ? C18 C13 C14 118.4(5) . . ? C18 C13 P1 121.6(4) . . ? C14 C13 P1 119.3(4) . . ? C15 C14 C13 119.2(6) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C16 C15 C14 121.6(6) . . ? C16 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? C15 C16 C17 119.4(6) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C18 C17 C16 121.2(6) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C13 120.1(6) . . ? C17 C18 H18 120.0 . . ? C13 C18 H18 120.0 . . ? C20 C19 C24 119.3(5) . . ? C20 C19 P1 124.2(5) . . ? C24 C19 P1 116.5(4) . . ? C19 C20 C21 119.8(6) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C22 C21 C20 120.9(7) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C23 119.1(6) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C22 C23 C24 121.8(7) . . ? C22 C23 H23 119.1 . . ? C24 C23 H23 119.1 . . ? C23 C24 C19 119.1(6) . . ? C23 C24 H24 120.5 . . ? C19 C24 H24 120.5 . . ? C30 C25 C26 119.2(6) . . ? C30 C25 P1 122.9(5) . . ? C26 C25 P1 117.9(4) . . ? C27 C26 C25 119.8(6) . . ? C27 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C28 C27 C26 120.6(7) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 120.2(7) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C28 C29 C30 120.5(7) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C25 C30 C29 119.7(7) . . ? C25 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C32 C31 C36 118.8(7) . . ? C32 C31 P2 121.4(6) . . ? C36 C31 P2 119.6(6) . . ? C31 C32 C33 119.1(9) . . ? C31 C32 H32 120.4 . . ? C33 C32 H32 120.4 . . ? C34 C33 C32 120.6(10) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C35 C34 C33 119.6(10) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C34 C35 C36 122.3(12) . . ? C34 C35 H35 118.8 . . ? C36 C35 H35 118.8 . . ? C35 C36 C31 119.6(10) . . ? C35 C36 H36 120.2 . . ? C31 C36 H36 120.2 . . ? C42 C37 C38 118.4(6) . . ? C42 C37 P2 125.1(5) . . ? C38 C37 P2 116.3(5) . . ? C37 C38 C39 120.2(7) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C40 C39 C38 119.9(7) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C41 C40 C39 120.3(7) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C40 C41 C42 120.3(7) . . ? C40 C41 H41 119.8 . . ? C42 C41 H41 119.8 . . ? C37 C42 C41 120.9(7) . . ? C37 C42 H42 119.5 . . ? C41 C42 H42 119.5 . . ? C48 C43 C44 119.0(6) . . ? C48 C43 P2 121.7(4) . . ? C44 C43 P2 119.1(5) . . ? C45 C44 C43 120.7(7) . . ? C45 C44 H44 119.7 . . ? C43 C44 H44 119.7 . . ? C46 C45 C44 119.5(6) . . ? C46 C45 H45 120.3 . . ? C44 C45 H45 120.3 . . ? C45 C46 C47 121.2(7) . . ? C45 C46 H46 119.4 . . ? C47 C46 H46 119.4 . . ? C48 C47 C46 119.5(7) . . ? C48 C47 H47 120.3 . . ? C46 C47 H47 120.3 . . ? C43 C48 C47 120.1(6) . . ? C43 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? C1A O1A H1A 109.5 . . ? O1A C1A C2A 97.7(17) . . ? O1A C1A H11A 112.2 . . ? C2A C1A H11A 112.2 . . ? O1A C1A H12A 112.2 . . ? C2A C1A H12A 112.2 . . ? H11A C1A H12A 109.8 . . ? C1A C2A H21A 109.5 . . ? C1A C2A H22A 109.5 . . ? H21A C2A H22A 109.5 . . ? C1A C2A H23A 109.5 . . ? H21A C2A H23A 109.5 . . ? H22A C2A H23A 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.441 _refine_diff_density_min -1.449 _refine_diff_density_rms 0.118 ###===END data_(4) _database_code_depnum_ccdc_archive 'CCDC 225820' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H43 Cl2 N2 O2 P2 Re, C H2 Cl2' _chemical_formula_sum 'C49 H45 Cl4 N2 O2 P2 Re' _chemical_formula_weight 1083.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.5556(2) _cell_length_b 25.2193(6) _cell_length_c 16.0769(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.176(1) _cell_angle_gamma 90.00 _cell_volume 4596.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 295 _cell_measurement_reflns_used 31970 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 28.00 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_absorpt_coefficient_mu 2.987 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.605 _exptl_absorpt_correction_T_max 0.678 _exptl_absorpt_process_details ; SORTAV (R.H. Blessing, Acta Crystallogr., 1995, A51, 33) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295 _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '\f scans and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31970 _diffrn_reflns_av_R_equivalents 0.067 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 28.00 _reflns_number_total 10977 _reflns_number_gt 9096 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Kappa CCD server software (Nonius, 1997)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP II (Johnson, 1976)' _computing_publication_material ; SHELXL-97 (Sheldrick, 1997), PARST (Nardelli, 1995) ; _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^)+(0.0000P)^2^+18.8030P] 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 10977 _refine_ls_number_parameters 539 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.0981 _refine_ls_wR_factor_gt 0.0900 _refine_ls_goodness_of_fit_ref 1.158 _refine_ls_restrained_S_all 1.158 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.147287(17) 0.163430(8) 0.248026(11) 0.02906(6) Uani 1 1 d . . . Cl1 Cl -0.05010(11) 0.12131(6) 0.19306(8) 0.0421(3) Uani 1 1 d . . . Cl2 Cl 0.12096(13) 0.20874(6) 0.11259(8) 0.0493(4) Uani 1 1 d . . . P1 P 0.24314(11) 0.09185(6) 0.17854(8) 0.0323(3) Uani 1 1 d . . . P2 P 0.03533(11) 0.23455(5) 0.30453(8) 0.0308(3) Uani 1 1 d . . . O1 O 0.3673(4) 0.07861(18) 0.4270(3) 0.0541(11) Uani 1 1 d . . . O2 O 0.3618(3) 0.19280(17) 0.3625(2) 0.0507(10) Uani 1 1 d . . . N1 N 0.1681(4) 0.12710(17) 0.3439(2) 0.0326(9) Uani 1 1 d . . . N2 N 0.1685(4) 0.09907(19) 0.4060(3) 0.0398(10) Uani 1 1 d . . . C1 C 0.2724(5) 0.0738(2) 0.4471(3) 0.0384(12) Uani 1 1 d . . . C2 C 0.2519(5) 0.0391(2) 0.5174(3) 0.0403(12) Uani 1 1 d . . . C3 C 0.1442(6) 0.0360(3) 0.5415(4) 0.0591(17) Uani 1 1 d . . . H3 H 0.0813 0.0563 0.5137 0.071 Uiso 1 1 calc R . . C4 C 0.1289(8) 0.0024(3) 0.6078(5) 0.076(2) Uani 1 1 d . . . H4 H 0.0557 0.0002 0.6234 0.091 Uiso 1 1 calc R . . C5 C 0.2215(8) -0.0272(3) 0.6497(5) 0.078(2) Uani 1 1 d . . . H5 H 0.2123 -0.0493 0.6943 0.094 Uiso 1 1 calc R . . C6 C 0.3272(8) -0.0236(3) 0.6247(5) 0.090(3) Uani 1 1 d . . . H6 H 0.3905 -0.0436 0.6528 0.108 Uiso 1 1 calc R . . C7 C 0.3431(6) 0.0089(3) 0.5592(4) 0.066(2) Uani 1 1 d . . . H7 H 0.4162 0.0104 0.5433 0.079 Uiso 1 1 calc R . . C8 C 0.2986(5) 0.2043(2) 0.2867(3) 0.0383(12) Uani 1 1 d . . . C9 C 0.4751(6) 0.2175(3) 0.4020(4) 0.0649(19) Uani 1 1 d . . . H9A H 0.4666 0.2323 0.4560 0.074 Uiso 1 1 d . . . H9B H 0.5344 0.1899 0.4128 0.074 Uiso 1 1 d . . . C10 C 0.5284(14) 0.2519(7) 0.3472(9) 0.076(4) Uiso 0.60 1 d P . . H101 H 0.5715 0.2384 0.3167 0.090 Uiso 0.60 1 d P . . H102 H 0.5676 0.2821 0.3850 0.090 Uiso 0.60 1 d P . . C11 C 0.4316(11) 0.2860(5) 0.2939(8) 0.059(3) Uiso 0.60 1 d P . . H111 H 0.4758 0.3043 0.2548 0.070 Uiso 0.60 1 d P . . H112 H 0.3960 0.3080 0.3232 0.070 Uiso 0.60 1 d P . . C10' C 0.4927(19) 0.2718(9) 0.3601(13) 0.070(5) Uiso 0.40 1 d P . . H103 H 0.4384 0.2993 0.3779 0.080 Uiso 0.40 1 d P . . H104 H 0.5726 0.2864 0.3823 0.080 Uiso 0.40 1 d P . . C11' C 0.466(2) 0.2668(11) 0.2689(16) 0.092(7) Uiso 0.40 1 d P . . H113 H 0.5270 0.2433 0.2517 0.100 Uiso 0.40 1 d P . . H114 H 0.4794 0.3019 0.2416 0.100 Uiso 0.40 1 d P . . C12 C 0.3451(6) 0.2469(3) 0.2382(4) 0.0539(16) Uani 1 1 d . . . H12A H 0.3746 0.2306 0.1919 0.065 Uiso 1 1 d . . . H12B H 0.2804 0.2699 0.2139 0.065 Uiso 1 1 d . . . C13 C -0.0516(4) 0.2144(2) 0.3836(3) 0.0358(11) Uani 1 1 d . . . C14 C -0.0796(5) 0.1627(2) 0.3967(4) 0.0452(13) Uani 1 1 d . . . H14 H -0.0546 0.1357 0.3648 0.054 Uiso 1 1 calc R . . C15 C -0.1459(6) 0.1505(3) 0.4580(4) 0.0582(17) Uani 1 1 d . . . H15 H -0.1639 0.1154 0.4675 0.070 Uiso 1 1 calc R . . C16 C -0.1848(7) 0.1902(3) 0.5046(4) 0.071(2) Uani 1 1 d . . . H16 H -0.2296 0.1818 0.5450 0.085 Uiso 1 1 calc R . . C17 C -0.1579(7) 0.2415(3) 0.4915(5) 0.072(2) Uani 1 1 d . . . H17 H -0.1845 0.2682 0.5229 0.087 Uiso 1 1 calc R . . C18 C -0.0915(6) 0.2543(3) 0.4320(4) 0.0564(16) Uani 1 1 d . . . H18 H -0.0730 0.2896 0.4238 0.068 Uiso 1 1 calc R . . C19 C 0.1297(4) 0.2853(2) 0.3655(3) 0.0346(11) Uani 1 1 d . . . C20 C 0.2019(5) 0.2678(2) 0.4399(3) 0.0439(13) Uani 1 1 d . . . H20 H 0.2008 0.2322 0.4547 0.053 Uiso 1 1 calc R . . C21 C 0.2756(5) 0.3025(3) 0.4923(4) 0.0491(15) Uani 1 1 d . . . H21 H 0.3220 0.2904 0.5425 0.059 Uiso 1 1 calc R . . C22 C 0.2798(5) 0.3547(3) 0.4697(4) 0.0551(16) Uani 1 1 d . . . H22 H 0.3300 0.3780 0.5041 0.066 Uiso 1 1 calc R . . C23 C 0.2100(6) 0.3724(3) 0.3964(4) 0.0596(17) Uani 1 1 d . . . H23 H 0.2129 0.4080 0.3814 0.071 Uiso 1 1 calc R . . C24 C 0.1352(6) 0.3381(2) 0.3442(4) 0.0509(15) Uani 1 1 d . . . H24 H 0.0883 0.3508 0.2945 0.061 Uiso 1 1 calc R . . C25 C -0.0717(5) 0.2696(2) 0.2256(3) 0.0373(12) Uani 1 1 d . . . C26 C -0.0359(6) 0.3041(2) 0.1679(3) 0.0472(14) Uani 1 1 d . . . H26 H 0.0441 0.3093 0.1693 0.057 Uiso 1 1 calc R . . C27 C -0.1183(7) 0.3309(3) 0.1082(4) 0.0616(19) Uani 1 1 d . . . H27 H -0.0935 0.3540 0.0701 0.074 Uiso 1 1 calc R . . C28 C -0.2366(7) 0.3232(3) 0.1057(4) 0.065(2) Uani 1 1 d . . . H28 H -0.2920 0.3423 0.0675 0.078 Uiso 1 1 calc R . . C29 C -0.2726(6) 0.2877(3) 0.1591(4) 0.065(2) Uani 1 1 d . . . H29 H -0.3527 0.2811 0.1549 0.078 Uiso 1 1 calc R . . C30 C -0.1908(5) 0.2613(3) 0.2202(4) 0.0496(15) Uani 1 1 d . . . H30 H -0.2167 0.2380 0.2575 0.060 Uiso 1 1 calc R . . C31 C 0.2588(5) 0.0305(2) 0.2399(3) 0.0365(11) Uani 1 1 d . . . C32 C 0.3636(5) 0.0025(2) 0.2581(3) 0.0392(12) Uani 1 1 d . . . H32 H 0.4301 0.0157 0.2407 0.047 Uiso 1 1 calc R . . C33 C 0.3704(6) -0.0454(3) 0.3024(4) 0.0608(18) Uani 1 1 d . . . H33 H 0.4414 -0.0638 0.3149 0.073 Uiso 1 1 calc R . . C34 C 0.2721(8) -0.0652(3) 0.3274(5) 0.071(2) Uani 1 1 d . . . H34 H 0.2759 -0.0972 0.3565 0.085 Uiso 1 1 calc R . . C35 C 0.1684(7) -0.0375(3) 0.3094(5) 0.0643(19) Uani 1 1 d . . . H35 H 0.1017 -0.0510 0.3264 0.077 Uiso 1 1 calc R . . C36 C 0.1613(5) 0.0100(2) 0.2664(4) 0.0470(14) Uani 1 1 d . . . H36 H 0.0903 0.0284 0.2552 0.056 Uiso 1 1 calc R . . C37 C 0.1780(5) 0.0657(2) 0.0733(3) 0.0390(12) Uani 1 1 d . . . C38 C 0.2317(6) 0.0214(3) 0.0448(4) 0.0559(16) Uani 1 1 d . . . H38 H 0.2983 0.0067 0.0789 0.067 Uiso 1 1 calc R . . C39 C 0.1868(7) -0.0011(3) -0.0334(4) 0.067(2) Uani 1 1 d . . . H39 H 0.2225 -0.0309 -0.0516 0.081 Uiso 1 1 calc R . . C40 C 0.0895(7) 0.0209(3) -0.0839(4) 0.070(2) Uani 1 1 d . . . H40 H 0.0586 0.0059 -0.1363 0.083 Uiso 1 1 calc R . . C41 C 0.0382(6) 0.0643(4) -0.0577(4) 0.073(2) Uani 1 1 d . . . H41 H -0.0271 0.0792 -0.0928 0.088 Uiso 1 1 calc R . . C42 C 0.0815(5) 0.0872(3) 0.0213(4) 0.0575(18) Uani 1 1 d . . . H42 H 0.0450 0.1171 0.0384 0.069 Uiso 1 1 calc R . . C43 C 0.3927(4) 0.1098(2) 0.1674(3) 0.0369(11) Uani 1 1 d . . . C44 C 0.4781(5) 0.1171(2) 0.2403(4) 0.0424(13) Uani 1 1 d . . . H44 H 0.4600 0.1119 0.2936 0.051 Uiso 1 1 calc R . . C45 C 0.5918(5) 0.1324(3) 0.2324(4) 0.0489(15) Uani 1 1 d . . . H45 H 0.6492 0.1371 0.2811 0.059 Uiso 1 1 calc R . . C46 C 0.6203(6) 0.1408(3) 0.1552(5) 0.0622(18) Uani 1 1 d . . . H46 H 0.6967 0.1502 0.1508 0.075 Uiso 1 1 calc R . . C47 C 0.5336(6) 0.1350(3) 0.0835(5) 0.0648(19) Uani 1 1 d . . . H47 H 0.5517 0.1412 0.0304 0.078 Uiso 1 1 calc R . . C48 C 0.4201(5) 0.1202(3) 0.0892(4) 0.0503(15) Uani 1 1 d . . . H48 H 0.3623 0.1173 0.0403 0.060 Uiso 1 1 calc R . . C49 C 0.3211(17) 0.0827(8) 0.8041(16) 0.272(14) Uani 1 1 d D . . H49A H 0.3609 0.1010 0.7646 0.326 Uiso 1 1 calc R . . H49B H 0.2657 0.0584 0.7708 0.326 Uiso 1 1 calc R . . Cl3 Cl 0.2467(8) 0.1250(3) 0.8406(5) 0.324(4) Uani 1 1 d D . . Cl4 Cl 0.4199(6) 0.0468(4) 0.8647(5) 0.314(5) Uani 1 1 d 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 0.02728(10) 0.03217(11) 0.02647(9) 0.00171(8) 0.00211(6) -0.00126(9) Cl1 0.0307(6) 0.0540(9) 0.0391(7) -0.0062(6) 0.0004(5) -0.0050(6) Cl2 0.0540(9) 0.0588(10) 0.0353(7) 0.0136(6) 0.0086(6) 0.0022(7) P1 0.0294(6) 0.0362(7) 0.0301(6) -0.0014(5) 0.0027(5) -0.0025(5) P2 0.0322(7) 0.0300(7) 0.0290(6) 0.0023(5) 0.0029(5) -0.0003(5) O1 0.042(2) 0.064(3) 0.055(2) 0.012(2) 0.0057(19) 0.002(2) O2 0.040(2) 0.060(3) 0.048(2) -0.001(2) -0.0046(17) -0.010(2) N1 0.030(2) 0.034(2) 0.034(2) -0.0017(18) 0.0064(17) -0.0017(18) N2 0.037(2) 0.046(3) 0.034(2) 0.008(2) 0.0017(18) 0.005(2) C1 0.041(3) 0.039(3) 0.032(3) 0.002(2) 0.000(2) -0.002(2) C2 0.045(3) 0.040(3) 0.033(3) 0.002(2) 0.000(2) -0.004(2) C3 0.057(4) 0.064(5) 0.058(4) 0.021(3) 0.015(3) 0.007(3) C4 0.086(6) 0.075(6) 0.073(5) 0.022(4) 0.034(4) 0.000(4) C5 0.098(6) 0.070(5) 0.058(4) 0.033(4) -0.003(4) -0.017(5) C6 0.076(6) 0.081(6) 0.098(6) 0.053(5) -0.018(5) -0.008(5) C7 0.049(4) 0.066(5) 0.075(5) 0.034(4) -0.009(3) 0.000(3) C8 0.033(3) 0.038(3) 0.045(3) -0.002(2) 0.010(2) -0.003(2) C9 0.041(4) 0.075(5) 0.069(4) -0.014(4) -0.012(3) -0.008(3) C12 0.047(4) 0.057(4) 0.058(4) 0.008(3) 0.011(3) -0.012(3) C13 0.034(3) 0.041(3) 0.032(2) 0.000(2) 0.006(2) -0.002(2) C14 0.050(3) 0.043(3) 0.047(3) 0.000(3) 0.019(3) -0.002(3) C15 0.064(4) 0.055(4) 0.061(4) 0.006(3) 0.026(3) -0.014(3) C16 0.088(6) 0.080(6) 0.057(4) -0.007(4) 0.045(4) -0.016(4) C17 0.090(6) 0.072(5) 0.068(5) -0.019(4) 0.047(4) -0.009(4) C18 0.069(4) 0.048(4) 0.057(4) -0.004(3) 0.026(3) -0.003(3) C19 0.036(3) 0.034(3) 0.033(2) -0.003(2) 0.005(2) 0.000(2) C20 0.045(3) 0.041(3) 0.041(3) 0.001(2) -0.001(2) -0.003(3) C21 0.045(3) 0.059(4) 0.039(3) -0.009(3) -0.001(2) -0.004(3) C22 0.043(3) 0.059(4) 0.060(4) -0.020(3) 0.002(3) -0.010(3) C23 0.066(4) 0.039(4) 0.067(4) -0.002(3) -0.004(3) -0.012(3) C24 0.059(4) 0.039(3) 0.049(3) 0.002(3) -0.006(3) 0.000(3) C25 0.040(3) 0.034(3) 0.034(3) 0.000(2) -0.003(2) 0.006(2) C26 0.056(4) 0.042(3) 0.041(3) 0.006(2) 0.005(3) 0.003(3) C27 0.092(6) 0.044(4) 0.041(3) 0.009(3) -0.006(3) 0.013(4) C28 0.071(5) 0.059(5) 0.053(4) 0.006(3) -0.018(3) 0.022(4) C29 0.045(4) 0.074(5) 0.065(4) -0.005(4) -0.014(3) 0.013(3) C30 0.043(3) 0.058(4) 0.045(3) 0.002(3) 0.000(2) 0.005(3) C31 0.038(3) 0.034(3) 0.036(3) -0.001(2) 0.003(2) 0.001(2) C32 0.037(3) 0.036(3) 0.045(3) -0.002(2) 0.009(2) -0.005(2) C33 0.064(4) 0.050(4) 0.068(4) 0.006(3) 0.010(3) 0.018(3) C34 0.103(6) 0.043(4) 0.072(5) 0.012(3) 0.029(4) 0.006(4) C35 0.077(5) 0.048(4) 0.077(5) 0.008(3) 0.038(4) -0.010(4) C36 0.046(3) 0.045(3) 0.051(3) 0.000(3) 0.011(3) -0.006(3) C37 0.039(3) 0.044(3) 0.034(3) -0.004(2) 0.007(2) -0.010(2) C38 0.075(5) 0.045(4) 0.043(3) -0.004(3) 0.002(3) 0.000(3) C39 0.104(6) 0.051(4) 0.049(4) -0.014(3) 0.020(4) -0.016(4) C40 0.073(5) 0.095(6) 0.041(3) -0.018(4) 0.011(3) -0.031(5) C41 0.049(4) 0.126(8) 0.041(3) -0.013(4) -0.002(3) -0.004(4) C42 0.042(3) 0.090(5) 0.038(3) -0.012(3) 0.001(2) 0.005(3) C43 0.033(3) 0.033(3) 0.042(3) 0.000(2) 0.003(2) 0.002(2) C44 0.033(3) 0.046(3) 0.047(3) -0.002(3) 0.003(2) -0.002(2) C45 0.023(3) 0.061(4) 0.060(4) -0.001(3) 0.002(2) 0.003(3) C46 0.035(3) 0.072(5) 0.080(5) 0.014(4) 0.013(3) -0.008(3) C47 0.051(4) 0.082(6) 0.064(4) 0.015(4) 0.018(3) -0.008(4) C48 0.044(3) 0.062(4) 0.044(3) 0.006(3) 0.006(2) -0.008(3) C49 0.164(17) 0.25(2) 0.45(4) -0.02(2) 0.18(2) 0.077(17) Cl3 0.450(12) 0.209(7) 0.351(9) 0.119(6) 0.172(9) -0.018(7) Cl4 0.188(5) 0.431(12) 0.373(9) -0.149(9) 0.183(6) -0.058(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 1.769(4) . ? Re1 C8 2.021(5) . ? Re1 Cl2 2.4254(13) . ? Re1 P2 2.4842(13) . ? Re1 P1 2.4926(14) . ? Re1 Cl1 2.5161(13) . ? P1 C31 1.826(5) . ? P1 C43 1.829(5) . ? P1 C37 1.835(5) . ? P2 C25 1.820(5) . ? P2 C19 1.837(5) . ? P2 C13 1.837(5) . ? O1 C1 1.208(6) . ? O2 C8 1.325(6) . ? O2 C9 1.478(7) . ? N1 N2 1.222(6) . ? N2 C1 1.406(7) . ? C1 C2 1.484(7) . ? C2 C7 1.366(8) . ? C2 C3 1.375(8) . ? C3 C4 1.398(9) . ? C3 H3 0.9300 . ? C4 C5 1.370(11) . ? C4 H4 0.9300 . ? C5 C6 1.361(11) . ? C5 H5 0.9300 . ? C6 C7 1.375(10) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C12 1.489(8) . ? C9 C10 1.454(17) . ? C9 C10' 1.55(2) . ? C9 H9A 0.967(7) . ? C9 H9B 0.968(7) . ? C10 C10' 0.71(2) . ? C10 C11' 1.38(3) . ? C10 C11 1.53(2) . ? C10 H101 0.836(16) . ? C10 H102 1.025(16) . ? C10 H104 1.108(16) . ? C10 H113 1.547(15) . ? C11 C11' 0.78(3) . ? C11 C10' 1.21(2) . ? C11 C12 1.556(14) . ? C11 H111 0.997(12) . ? C11 H112 0.880(13) . ? C11 H103 1.379(13) . ? C11 H114 1.165(12) . ? C10' C11' 1.44(3) . ? C10' H101 1.51(2) . ? C10' H102 0.92(2) . ? C10' H112 1.48(2) . ? C10' H103 1.01(2) . ? C10' H104 1.00(2) . ? C11' C12 1.47(3) . ? C11' H101 1.50(3) . ? C11' H111 0.99(3) . ? C11' H113 1.00(3) . ? C11' H114 1.01(3) . ? C12 H12A 0.970(7) . ? C12 H12B 0.967(7) . ? C13 C14 1.371(8) . ? C13 C18 1.403(8) . ? C14 C15 1.394(8) . ? C14 H14 0.9300 . ? C15 C16 1.376(10) . ? C15 H15 0.9300 . ? C16 C17 1.356(10) . ? C16 H16 0.9300 . ? C17 C18 1.376(9) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C24 1.380(8) . ? C19 C20 1.391(7) . ? C20 C21 1.387(8) . ? C20 H20 0.9300 . ? C21 C22 1.368(9) . ? C21 H21 0.9300 . ? C22 C23 1.368(9) . ? C22 H22 0.9300 . ? C23 C24 1.386(8) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C30 1.379(8) . ? C25 C26 1.392(8) . ? C26 C27 1.390(8) . ? C26 H26 0.9300 . ? C27 C28 1.374(10) . ? C27 H27 0.9300 . ? C28 C29 1.361(10) . ? C28 H28 0.9300 . ? C29 C30 1.393(8) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C36 1.380(8) . ? C31 C32 1.383(7) . ? C32 C33 1.396(8) . ? C32 H32 0.9300 . ? C33 C34 1.371(10) . ? C33 H33 0.9300 . ? C34 C35 1.369(10) . ? C34 H34 0.9300 . ? C35 C36 1.377(9) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C42 1.369(8) . ? C37 C38 1.400(8) . ? C38 C39 1.386(8) . ? C38 H38 0.9300 . ? C39 C40 1.371(11) . ? C39 H39 0.9300 . ? C40 C41 1.350(11) . ? C40 H40 0.9300 . ? C41 C42 1.397(8) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C48 1.380(8) . ? C43 C44 1.391(7) . ? C44 C45 1.398(7) . ? C44 H44 0.9300 . ? C45 C46 1.362(9) . ? C45 H45 0.9300 . ? C46 C47 1.381(9) . ? C46 H46 0.9300 . ? C47 C48 1.383(8) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 Cl3 1.554(14) . ? C49 Cl4 1.625(17) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? 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 C8 91.9(2) . . ? N1 Re1 Cl2 176.80(14) . . ? C8 Re1 Cl2 89.25(16) . . ? N1 Re1 P2 92.74(14) . . ? C8 Re1 P2 89.99(16) . . ? Cl2 Re1 P2 90.26(5) . . ? N1 Re1 P1 91.04(14) . . ? C8 Re1 P1 94.26(16) . . ? Cl2 Re1 P1 85.88(5) . . ? P2 Re1 P1 174.21(4) . . ? N1 Re1 Cl1 92.76(13) . . ? C8 Re1 Cl1 174.10(16) . . ? Cl2 Re1 Cl1 86.34(5) . . ? P2 Re1 Cl1 86.12(4) . . ? P1 Re1 Cl1 89.33(4) . . ? C31 P1 C43 105.5(2) . . ? C31 P1 C37 100.0(2) . . ? C43 P1 C37 103.0(2) . . ? C31 P1 Re1 112.21(17) . . ? C43 P1 Re1 112.01(18) . . ? C37 P1 Re1 122.29(19) . . ? C25 P2 C19 106.6(2) . . ? C25 P2 C13 103.2(2) . . ? C19 P2 C13 99.9(2) . . ? C25 P2 Re1 115.28(17) . . ? C19 P2 Re1 113.63(17) . . ? C13 P2 Re1 116.53(19) . . ? C8 O2 C9 126.0(5) . . ? N2 N1 Re1 171.7(4) . . ? N1 N2 C1 121.0(5) . . ? O1 C1 N2 124.4(5) . . ? O1 C1 C2 123.4(5) . . ? N2 C1 C2 112.2(5) . . ? C7 C2 C3 118.9(6) . . ? C7 C2 C1 118.7(6) . . ? C3 C2 C1 122.4(5) . . ? C2 C3 C4 120.3(6) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 120.2(7) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C6 C5 C4 118.6(7) . . ? C6 C5 H5 120.7 . . ? C4 C5 H5 120.7 . . ? C5 C6 C7 121.8(7) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C2 C7 C6 120.3(7) . . ? C2 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? O2 C8 C12 116.6(5) . . ? O2 C8 Re1 117.5(4) . . ? C12 C8 Re1 125.9(4) . . ? C10 C9 O2 115.8(8) . . ? C10 C9 C10' 26.9(9) . . ? O2 C9 C10' 111.4(9) . . ? C10 C9 H9A 116.3(9) . . ? O2 C9 H9A 108.2(6) . . ? C10' C9 H9A 95.4(10) . . ? C10 C9 H9B 99.7(9) . . ? O2 C9 H9B 108.1(6) . . ? C10' C9 H9B 124.3(11) . . ? H9A C9 H9B 107.9(7) . . ? C10' C10 C11' 81(3) . . ? C10' C10 C9 85(3) . . ? C11' C10 C9 120.4(16) . . ? C10' C10 C11 50(2) . . ? C11' C10 C11 30.5(11) . . ? C9 C10 C11 108.8(11) . . ? C10' C10 H101 156(3) . . ? C11' C10 H101 81.0(17) . . ? C9 C10 H101 118.9(16) . . ? C11 C10 H101 110.7(14) . . ? C10' C10 H102 61(2) . . ? C11' C10 H102 115.6(18) . . ? C9 C10 H102 106.0(12) . . ? C11 C10 H102 96.0(13) . . ? H101 C10 H102 114.0(16) . . ? C10' C10 H104 62(2) . . ? C11' C10 H104 111.0(17) . . ? C9 C10 H104 111.6(12) . . ? C11 C10 H104 93.3(12) . . ? H101 C10 H104 110.5(15) . . ? H102 C10 H104 5.67(11) . . ? C10' C10 H113 120(3) . . ? C11' C10 H113 39.6(12) . . ? C9 C10 H113 126.4(11) . . ? C11 C10 H113 70.0(8) . . ? H101 C10 H113 41.8(7) . . ? H102 C10 H113 127.6(13) . . ? H104 C10 H113 122.0(12) . . ? C11' C11 C10' 90(3) . . ? C11' C11 C10 64(2) . . ? C10' C11 C10 26.6(11) . . ? C11' C11 C12 69(2) . . ? C10' C11 C12 121.2(15) . . ? C10 C11 C12 106.5(10) . . ? C11' C11 H111 66(2) . . ? C10' C11 H111 114.1(15) . . ? C10 C11 H111 101.8(11) . . ? C12 C11 H111 106.4(10) . . ? C11' C11 H112 178(3) . . ? C10' C11 H112 88.3(15) . . ? C10 C11 H112 114.9(13) . . ? C12 C11 H112 113.2(11) . . ? H111 C11 H112 113.0(13) . . ? C11' C11 H103 136(3) . . ? C10' C11 H103 45.5(12) . . ? C10 C11 H103 72.1(9) . . ? C12 C11 H103 128.8(9) . . ? H111 C11 H103 124.3(11) . . ? H112 C11 H103 42.8(6) . . ? C11' C11 H114 59(2) . . ? C10' C11 H114 117.3(15) . . ? C10 C11 H114 101.5(10) . . ? C12 C11 H114 98.3(9) . . ? H111 C11 H114 8.72(15) . . ? H112 C11 H114 120.3(13) . . ? H103 C11 H114 132.7(10) . . ? C10 C10' C11 103(3) . . ? C10 C10' C11' 70(2) . . ? C11 C10' C11' 32.8(12) . . ? C10 C10' C9 69(2) . . ? C11 C10' C9 122.5(18) . . ? C11' C10' C9 110.0(18) . . ? C10 C10' H101 13.3(18) . . ? C11 C10' H101 93.4(15) . . ? C11' C10' H101 60.8(14) . . ? C9 C10' H101 81.4(12) . . ? C10 C10' H102 77(3) . . ? C11 C10' H102 130(2) . . ? C11' C10' H102 118(2) . . ? C9 C10' H102 104.6(18) . . ? H101 C10' H102 76.0(15) . . ? C10 C10' H112 140(3) . . ? C11 C10' H112 36.6(10) . . ? C11' C10' H112 69.4(15) . . ? C9 C10' H112 124.6(15) . . ? H101 C10' H112 129.6(14) . . ? H102 C10' H112 125(2) . . ? C10 C10' H103 178(4) . . ? C11 C10' H103 76.0(17) . . ? C11' C10' H103 109(2) . . ? C9 C10' H103 110.0(17) . . ? H101 C10' H103 167(2) . . ? H102 C10' H103 105(2) . . ? H112 C10' H103 39.4(8) . . ? C10 C10' H104 79(3) . . ? C11 C10' H104 123(2) . . ? C11' C10' H104 114(2) . . ? C9 C10' H104 111.2(18) . . ? H101 C10' H104 76.7(14) . . ? H102 C10' H104 6.60(18) . . ? H112 C10' H104 119.4(19) . . ? H103 C10' H104 103(2) . . ? C11 C11' C10 86(3) . . ? C11 C11' C10' 57(2) . . ? C10 C11' C10' 28.9(11) . . ? C11 C11' C12 81(2) . . ? C10 C11' C12 120.6(19) . . ? C10' C11' C12 112.0(19) . . ? C11 C11' H101 118(3) . . ? C10 C11' H101 33.5(9) . . ? C10' C11' H101 61.7(14) . . ? C12 C11' H101 129.4(19) . . ? C11 C11' H111 68(2) . . ? C10 C11' H111 114(2) . . ? C10' C11' H111 98(2) . . ? C12 C11' H111 113(2) . . ? H101 C11' H111 117(2) . . ? C11 C11' H113 164(4) . . ? C10 C11' H113 79.3(18) . . ? C10' C11' H113 108(2) . . ? C12 C11' H113 112(2) . . ? H101 C11' H113 46.1(11) . . ? H111 C11' H113 112(2) . . ? C11 C11' H114 80(3) . . ? C10 C11' H114 122(2) . . ? C10' C11' H114 110(2) . . ? C12 C11' H114 112(2) . . ? H101 C11' H114 117(2) . . ? H111 C11' H114 13.3(3) . . ? H113 C11' H114 103(2) . . ? C8 C12 C11' 119.0(11) . . ? C8 C12 C11 114.4(6) . . ? C11' C12 C11 29.7(10) . . ? C8 C12 H12A 108.2(6) . . ? C11' C12 H12A 87.3(11) . . ? C11 C12 H12A 115.4(7) . . ? C8 C12 H12B 108.3(5) . . ? C11' C12 H12B 122.6(12) . . ? C11 C12 H12B 102.3(7) . . ? H12A C12 H12B 107.6(6) . . ? C14 C13 C18 119.0(5) . . ? C14 C13 P2 123.1(4) . . ? C18 C13 P2 117.9(4) . . ? C13 C14 C15 119.7(6) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 120.5(6) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C17 C16 C15 120.0(6) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C16 C17 C18 120.5(7) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C17 C18 C13 120.3(6) . . ? C17 C18 H18 119.9 . . ? C13 C18 H18 119.9 . . ? C24 C19 C20 118.1(5) . . ? C24 C19 P2 126.3(4) . . ? C20 C19 P2 115.6(4) . . ? C21 C20 C19 121.1(6) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C22 C21 C20 119.7(6) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C23 C22 C21 119.9(6) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 120.8(6) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C19 C24 C23 120.4(5) . . ? C19 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C30 C25 C26 118.4(5) . . ? C30 C25 P2 120.3(4) . . ? C26 C25 P2 121.3(4) . . ? C27 C26 C25 120.8(6) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C28 C27 C26 119.8(6) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C29 C28 C27 119.9(6) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 120.7(7) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C25 C30 C29 120.3(6) . . ? C25 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C36 C31 C32 118.5(5) . . ? C36 C31 P1 118.9(4) . . ? C32 C31 P1 122.5(4) . . ? C31 C32 C33 120.7(6) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C34 C33 C32 119.8(6) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C35 C34 C33 119.6(7) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C34 C35 C36 120.9(7) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C35 C36 C31 120.6(6) . . ? C35 C36 H36 119.7 . . ? C31 C36 H36 119.7 . . ? C42 C37 C38 118.5(5) . . ? C42 C37 P1 124.1(5) . . ? C38 C37 P1 117.4(4) . . ? C39 C38 C37 120.9(6) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C40 C39 C38 119.4(7) . . ? C40 C39 H39 120.3 . . ? C38 C39 H39 120.3 . . ? C41 C40 C39 120.2(6) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C40 C41 C42 121.2(7) . . ? C40 C41 H41 119.4 . . ? C42 C41 H41 119.4 . . ? C37 C42 C41 119.8(7) . . ? C37 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? C48 C43 C44 119.5(5) . . ? C48 C43 P1 121.7(4) . . ? C44 C43 P1 118.7(4) . . ? C43 C44 C45 119.1(5) . . ? C43 C44 H44 120.5 . . ? C45 C44 H44 120.5 . . ? C46 C45 C44 121.6(6) . . ? C46 C45 H45 119.2 . . ? C44 C45 H45 119.2 . . ? C45 C46 C47 118.7(6) . . ? C45 C46 H46 120.7 . . ? C47 C46 H46 120.7 . . ? C46 C47 C48 121.1(6) . . ? C46 C47 H47 119.4 . . ? C48 C47 H47 119.4 . . ? C43 C48 C47 120.0(6) . . ? C43 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? Cl3 C49 Cl4 122.1(17) . . ? Cl3 C49 H49A 106.8 . . ? Cl4 C49 H49A 106.8 . . ? Cl3 C49 H49B 106.8 . . ? Cl4 C49 H49B 106.8 . . ? H49A C49 H49B 106.7 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.545 _refine_diff_density_min -1.172 _refine_diff_density_rms 0.110 ###===END data_(6) _database_code_depnum_ccdc_archive 'CCDC 225821' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H40 Cl2 N3 O P2 Re, C H2 Cl2' _chemical_formula_sum 'C47 H42 Cl4 N3 O P2 Re' _chemical_formula_weight 1054.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' 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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P bcn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 33.3037(1) _cell_length_b 11.0025(3) _cell_length_c 24.7218(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9058.7(3) _cell_formula_units_Z 8 _cell_measurement_temperature 295 _cell_measurement_reflns_used 59233 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 28.00 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4208 _exptl_absorpt_coefficient_mu 3.028 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.574 _exptl_absorpt_correction_T_max 0.817 _exptl_absorpt_process_details ; SORTAV (R.H. Blessing, Acta Crystallogr., 1995, A51, 33) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295 _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '\f scans and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59233 _diffrn_reflns_av_R_equivalents 0.087 _diffrn_reflns_av_sigmaI/netI 0.0480 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 28.00 _reflns_number_total 10554 _reflns_number_gt 7866 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Kappa CCD server software (Nonius, 1997)' _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP II (Johnson, 1976)' _computing_publication_material ; SHELXL-97 (Sheldrick, 1997), PARST (Nardelli, 1995) ; _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^)+(0.0368P)^2^+25.2532P] 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 10554 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0847 _refine_ls_R_factor_gt 0.0491 _refine_ls_wR_factor_ref 0.1146 _refine_ls_wR_factor_gt 0.0922 _refine_ls_goodness_of_fit_ref 1.169 _refine_ls_restrained_S_all 1.169 _refine_ls_shift/su_max 0.004 _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 0.880096(6) 0.929107(17) 0.933762(8) 0.02801(7) Uani 1 1 d . . . Cl1 Cl 0.87268(5) 1.14640(12) 0.92091(6) 0.0424(3) Uani 1 1 d . . . Cl2 Cl 0.92623(4) 0.95334(12) 1.00839(6) 0.0414(3) Uani 1 1 d . . . P1 P 0.93845(4) 0.93844(12) 0.87295(5) 0.0316(3) Uani 1 1 d . . . P2 P 0.82557(4) 0.93156(12) 1.00089(5) 0.0296(3) Uani 1 1 d . . . O1 O 0.86086(15) 0.6746(4) 0.83516(19) 0.0613(13) Uani 1 1 d . . . N1 N 0.84809(14) 0.8864(4) 0.88138(17) 0.0325(10) Uani 1 1 d . . . N2 N 0.82420(15) 0.8512(4) 0.84506(19) 0.0412(12) Uani 1 1 d . . . N3 N 0.88795(14) 0.7305(4) 0.94622(18) 0.0366(11) Uani 1 1 d . . . H3A H 0.8634 0.7015 0.9545 0.044 Uiso 1 1 calc R . . H3B H 0.8942 0.6997 0.9136 0.044 Uiso 1 1 calc R . . C1 C 0.83148(19) 0.7367(5) 0.8237(2) 0.0411(14) Uani 1 1 d . . . C2 C 0.79984(19) 0.6933(5) 0.7863(2) 0.0417(14) Uani 1 1 d . . . C3 C 0.8059(2) 0.5859(6) 0.7581(3) 0.0570(18) Uani 1 1 d . . . H3 H 0.8304 0.5456 0.7603 0.068 Uiso 1 1 calc R . . C4 C 0.7752(3) 0.5390(7) 0.7266(3) 0.072(2) Uani 1 1 d . . . H4 H 0.7792 0.4661 0.7083 0.086 Uiso 1 1 calc R . . C5 C 0.7395(3) 0.5967(8) 0.7218(3) 0.081(3) Uani 1 1 d . . . H5 H 0.7193 0.5646 0.7001 0.097 Uiso 1 1 calc R . . C6 C 0.7334(3) 0.7025(9) 0.7493(4) 0.096(3) Uani 1 1 d . . . H6 H 0.7088 0.7422 0.7467 0.116 Uiso 1 1 calc R . . C7 C 0.7639(2) 0.7520(7) 0.7813(3) 0.071(2) Uani 1 1 d . . . H7 H 0.7598 0.8251 0.7993 0.086 Uiso 1 1 calc R . . C8 C 0.91610(19) 0.6727(5) 0.9850(2) 0.0432(14) Uani 1 1 d . . . H81 H 0.9091 0.6952 1.0218 0.052 Uiso 1 1 calc R . . H82 H 0.9433 0.6996 0.9780 0.052 Uiso 1 1 calc R . . C9 C 0.9132(2) 0.5385(6) 0.9782(3) 0.0515(17) Uani 1 1 d . . . C10 C 0.9089(3) 0.4354(6) 0.9698(3) 0.074(2) Uani 1 1 d . . . H10 H 0.9055 0.3529 0.9630 0.089 Uiso 1 1 calc R . . C11 C 0.92453(18) 0.9266(5) 0.8016(2) 0.0399(13) Uani 1 1 d . . . C12 C 0.9441(2) 0.8553(6) 0.7643(3) 0.0552(17) Uani 1 1 d . . . H12 H 0.9655 0.8070 0.7753 0.066 Uiso 1 1 calc R . . C13 C 0.9323(3) 0.8545(8) 0.7105(3) 0.074(2) Uani 1 1 d . . . H13 H 0.9453 0.8041 0.6858 0.088 Uiso 1 1 calc R . . C14 C 0.9021(3) 0.9264(8) 0.6939(3) 0.081(3) Uani 1 1 d . . . H14 H 0.8944 0.9259 0.6578 0.097 Uiso 1 1 calc R . . C15 C 0.8826(3) 1.0001(8) 0.7296(3) 0.076(2) Uani 1 1 d . . . H15 H 0.8620 1.0503 0.7174 0.092 Uiso 1 1 calc R . . C16 C 0.8931(2) 1.0011(6) 0.7842(3) 0.0541(17) Uani 1 1 d . . . H16 H 0.8794 1.0505 0.8085 0.065 Uiso 1 1 calc R . . C17 C 0.97420(17) 0.8156(4) 0.8855(2) 0.0336(12) Uani 1 1 d . . . C18 C 1.00745(18) 0.8362(6) 0.9181(2) 0.0428(14) Uani 1 1 d . . . H18 H 1.0129 0.9142 0.9306 0.051 Uiso 1 1 calc R . . C19 C 1.0325(2) 0.7406(6) 0.9320(3) 0.0526(16) Uani 1 1 d . . . H19 H 1.0547 0.7551 0.9539 0.063 Uiso 1 1 calc R . . C20 C 1.0249(2) 0.6236(6) 0.9139(3) 0.063(2) Uani 1 1 d . . . H20 H 1.0418 0.5599 0.9235 0.075 Uiso 1 1 calc R . . C21 C 0.9921(2) 0.6031(6) 0.8816(3) 0.0593(19) Uani 1 1 d . . . H21 H 0.9871 0.5252 0.8686 0.071 Uiso 1 1 calc R . . C22 C 0.96616(18) 0.6976(5) 0.8680(2) 0.0434(14) Uani 1 1 d . . . H22 H 0.9434 0.6820 0.8473 0.052 Uiso 1 1 calc R . . C23 C 0.97102(17) 1.0731(5) 0.8735(2) 0.0371(12) Uani 1 1 d . . . C24 C 0.97344(18) 1.1516(5) 0.9166(3) 0.0443(14) Uani 1 1 d . . . H24 H 0.9573 1.1388 0.9468 0.053 Uiso 1 1 calc R . . C25 C 0.9996(2) 1.2493(6) 0.9157(3) 0.0528(17) Uani 1 1 d . . . H25 H 1.0005 1.3020 0.9451 0.063 Uiso 1 1 calc R . . C26 C 1.0237(2) 1.2692(6) 0.8727(3) 0.064(2) Uani 1 1 d . . . H26 H 1.0412 1.3350 0.8725 0.077 Uiso 1 1 calc R . . C27 C 1.0222(3) 1.1923(7) 0.8295(4) 0.085(3) Uani 1 1 d . . . H27 H 1.0390 1.2050 0.8000 0.102 Uiso 1 1 calc R . . C28 C 0.9956(2) 1.0948(6) 0.8295(3) 0.067(2) Uani 1 1 d . . . H28 H 0.9944 1.0437 0.7996 0.080 Uiso 1 1 calc R . . C29 C 0.82843(17) 0.8012(5) 1.0470(2) 0.0355(12) Uani 1 1 d . . . C30 C 0.8474(2) 0.8156(5) 1.0964(2) 0.0495(16) Uani 1 1 d . . . H30 H 0.8549 0.8927 1.1078 0.059 Uiso 1 1 calc R . . C31 C 0.8551(2) 0.7162(6) 1.1288(3) 0.0621(19) Uani 1 1 d . . . H31 H 0.8684 0.7268 1.1615 0.074 Uiso 1 1 calc R . . C32 C 0.8434(2) 0.6017(6) 1.1131(3) 0.065(2) Uani 1 1 d . . . H32 H 0.8480 0.5356 1.1357 0.078 Uiso 1 1 calc R . . C33 C 0.8250(2) 0.5852(6) 1.0643(3) 0.0570(18) Uani 1 1 d . . . H33 H 0.8178 0.5075 1.0532 0.068 Uiso 1 1 calc R . . C34 C 0.81699(18) 0.6842(5) 1.0314(2) 0.0421(14) Uani 1 1 d . . . H34 H 0.8039 0.6726 0.9986 0.050 Uiso 1 1 calc R . . C35 C 0.77637(17) 0.9295(5) 0.9691(2) 0.0350(12) Uani 1 1 d . . . C36 C 0.7450(2) 0.8534(6) 0.9843(3) 0.0523(16) Uani 1 1 d . . . H36 H 0.7485 0.7980 1.0123 0.063 Uiso 1 1 calc R . . C37 C 0.7084(2) 0.8604(7) 0.9575(3) 0.066(2) Uani 1 1 d . . . H37 H 0.6875 0.8090 0.9676 0.079 Uiso 1 1 calc R . . C38 C 0.7028(2) 0.9418(8) 0.9168(3) 0.072(2) Uani 1 1 d . . . H38 H 0.6783 0.9454 0.8989 0.086 Uiso 1 1 calc R . . C39 C 0.7336(2) 1.0195(8) 0.9019(3) 0.072(2) Uani 1 1 d . . . H39 H 0.7296 1.0763 0.8745 0.086 Uiso 1 1 calc R . . C40 C 0.7702(2) 1.0124(6) 0.9276(2) 0.0512(16) Uani 1 1 d . . . H40 H 0.7910 1.0636 0.9171 0.061 Uiso 1 1 calc R . . C41 C 0.82068(18) 1.0600(5) 1.0475(2) 0.0347(12) Uani 1 1 d . . . C42 C 0.85093(19) 1.1449(5) 1.0542(2) 0.0427(14) Uani 1 1 d . . . H42 H 0.8746 1.1379 1.0345 0.051 Uiso 1 1 calc R . . C43 C 0.8461(2) 1.2403(6) 1.0901(3) 0.0606(19) Uani 1 1 d . . . H43 H 0.8664 1.2978 1.0940 0.073 Uiso 1 1 calc R . . C44 C 0.8116(3) 1.2504(6) 1.1199(3) 0.064(2) Uani 1 1 d . . . H44 H 0.8086 1.3141 1.1443 0.077 Uiso 1 1 calc R . . C45 C 0.7815(2) 1.1667(6) 1.1139(3) 0.062(2) Uani 1 1 d . . . H45 H 0.7580 1.1742 1.1339 0.075 Uiso 1 1 calc R . . C46 C 0.7859(2) 1.0714(5) 1.0782(2) 0.0482(16) Uani 1 1 d . . . H46 H 0.7654 1.0143 1.0747 0.058 Uiso 1 1 calc R . . C47 C 0.9129(6) 0.3976(17) 0.8065(7) 0.215(10) Uani 1 1 d . . . H471 H 0.9325 0.3439 0.8229 0.258 Uiso 1 1 calc R . . H472 H 0.9044 0.4563 0.8334 0.258 Uiso 1 1 calc R . . Cl3 Cl 0.8755(2) 0.3216(4) 0.7862(2) 0.266(3) Uani 1 1 d . . . Cl4 Cl 0.9349(3) 0.4747(8) 0.7497(4) 0.361(6) 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 0.02699(12) 0.02402(11) 0.03301(11) -0.00150(8) -0.00116(9) 0.00041(9) Cl1 0.0424(9) 0.0252(6) 0.0595(9) 0.0018(6) 0.0063(6) 0.0012(6) Cl2 0.0370(8) 0.0437(8) 0.0434(8) -0.0039(6) -0.0104(6) -0.0029(6) P1 0.0302(8) 0.0306(7) 0.0341(7) -0.0029(6) 0.0010(6) 0.0012(6) P2 0.0289(8) 0.0274(6) 0.0326(7) -0.0011(6) 0.0002(5) -0.0018(6) O1 0.063(3) 0.052(3) 0.069(3) -0.020(2) -0.025(3) 0.015(3) N1 0.035(3) 0.028(2) 0.034(2) 0.0035(18) 0.000(2) 0.007(2) N2 0.042(3) 0.040(3) 0.042(3) -0.002(2) -0.011(2) -0.001(2) N3 0.037(3) 0.025(2) 0.047(3) 0.0000(19) -0.005(2) 0.005(2) C1 0.045(4) 0.039(3) 0.039(3) -0.002(2) -0.001(3) -0.001(3) C2 0.049(4) 0.039(3) 0.037(3) 0.003(2) -0.006(3) -0.009(3) C3 0.064(5) 0.057(4) 0.050(4) -0.014(3) -0.003(3) -0.013(4) C4 0.090(7) 0.065(5) 0.061(5) -0.017(4) -0.004(4) -0.031(5) C5 0.076(7) 0.084(6) 0.081(6) -0.010(5) -0.022(5) -0.034(5) C6 0.061(6) 0.098(7) 0.130(8) -0.016(6) -0.048(5) 0.000(5) C7 0.071(6) 0.054(4) 0.089(6) -0.010(4) -0.032(4) -0.003(4) C8 0.047(4) 0.037(3) 0.046(3) 0.004(3) -0.010(3) 0.005(3) C9 0.051(4) 0.039(3) 0.064(4) 0.007(3) -0.016(3) 0.009(3) C10 0.092(7) 0.035(4) 0.095(6) 0.007(4) -0.030(5) 0.006(4) C11 0.041(3) 0.045(3) 0.034(3) -0.002(3) 0.000(2) -0.007(3) C12 0.053(5) 0.067(4) 0.045(4) -0.011(3) 0.001(3) 0.005(4) C13 0.089(7) 0.086(6) 0.045(4) -0.010(4) 0.004(4) 0.003(5) C14 0.098(7) 0.104(7) 0.042(4) -0.012(4) -0.019(4) -0.003(6) C15 0.079(6) 0.088(6) 0.061(5) 0.020(5) -0.015(4) 0.014(5) C16 0.052(4) 0.058(4) 0.052(4) 0.006(3) 0.002(3) 0.012(4) C17 0.031(3) 0.030(3) 0.040(3) -0.002(2) 0.002(2) 0.004(2) C18 0.041(4) 0.045(3) 0.043(3) -0.007(3) 0.001(3) -0.006(3) C19 0.041(4) 0.061(4) 0.057(4) 0.001(3) -0.014(3) 0.011(3) C20 0.066(5) 0.052(4) 0.070(5) -0.003(4) -0.014(4) 0.021(4) C21 0.070(5) 0.036(3) 0.072(5) -0.008(3) -0.013(4) 0.014(3) C22 0.037(4) 0.039(3) 0.055(4) -0.011(3) -0.002(3) 0.003(3) C23 0.034(3) 0.032(3) 0.046(3) 0.001(2) 0.002(2) 0.000(3) C24 0.036(4) 0.044(3) 0.053(4) -0.002(3) 0.003(3) -0.008(3) C25 0.047(4) 0.044(3) 0.067(4) -0.007(3) -0.004(3) -0.004(3) C26 0.056(5) 0.046(4) 0.090(6) 0.000(4) 0.007(4) -0.019(3) C27 0.093(7) 0.058(5) 0.103(7) -0.007(5) 0.051(5) -0.028(5) C28 0.080(6) 0.053(4) 0.067(5) -0.016(3) 0.033(4) -0.024(4) C29 0.036(3) 0.034(3) 0.037(3) 0.003(2) 0.003(2) 0.000(3) C30 0.068(5) 0.039(3) 0.041(4) 0.002(3) -0.005(3) -0.002(3) C31 0.083(6) 0.058(4) 0.046(4) 0.008(3) -0.013(4) 0.005(4) C32 0.075(6) 0.053(4) 0.068(5) 0.022(4) 0.004(4) 0.006(4) C33 0.050(4) 0.040(4) 0.080(5) 0.015(3) 0.005(4) -0.005(3) C34 0.036(4) 0.035(3) 0.056(4) 0.000(3) 0.002(3) -0.007(3) C35 0.029(3) 0.038(3) 0.039(3) -0.003(2) -0.001(2) -0.001(3) C36 0.044(4) 0.044(3) 0.069(4) 0.006(3) -0.004(3) -0.004(3) C37 0.035(4) 0.068(5) 0.095(6) -0.002(4) -0.006(4) -0.017(4) C38 0.040(4) 0.104(6) 0.073(5) -0.010(5) -0.019(4) 0.009(5) C39 0.048(5) 0.105(6) 0.062(5) 0.029(4) -0.011(4) 0.011(5) C40 0.039(4) 0.065(4) 0.049(4) 0.020(3) 0.000(3) 0.005(3) C41 0.039(3) 0.028(3) 0.036(3) -0.002(2) 0.000(2) 0.006(3) C42 0.041(4) 0.042(3) 0.046(3) -0.008(3) 0.002(3) 0.000(3) C43 0.063(5) 0.052(4) 0.067(5) -0.021(3) -0.002(4) -0.005(4) C44 0.090(6) 0.046(4) 0.057(4) -0.019(3) 0.008(4) 0.006(4) C45 0.069(5) 0.060(4) 0.058(4) -0.010(3) 0.032(4) 0.008(4) C46 0.048(4) 0.043(3) 0.054(4) -0.006(3) 0.013(3) -0.002(3) C47 0.175(17) 0.26(2) 0.215(18) -0.126(17) -0.115(15) 0.014(15) Cl3 0.475(11) 0.115(3) 0.210(5) 0.002(3) -0.100(6) 0.010(4) Cl4 0.356(11) 0.270(8) 0.456(13) -0.186(9) 0.146(10) -0.041(7) _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 1.742(4) . ? Re1 N3 2.222(4) . ? Re1 Cl2 2.4156(14) . ? Re1 Cl1 2.4244(13) . ? Re1 P1 2.4590(14) . ? Re1 P2 2.4602(14) . ? P1 C17 1.828(5) . ? P1 C11 1.828(6) . ? P1 C23 1.836(6) . ? P2 C35 1.817(6) . ? P2 C41 1.830(5) . ? P2 C29 1.834(5) . ? O1 C1 1.227(7) . ? N1 N2 1.261(6) . ? N2 C1 1.388(7) . ? N3 C8 1.485(7) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? C1 C2 1.481(8) . ? C2 C7 1.364(9) . ? C2 C3 1.387(8) . ? C3 C4 1.384(10) . ? C3 H3 0.9300 . ? C4 C5 1.355(12) . ? C4 H4 0.9300 . ? C5 C6 1.362(12) . ? C5 H5 0.9300 . ? C6 C7 1.398(10) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.489(8) . ? C8 H81 0.9700 . ? C8 H82 0.9700 . ? C9 C10 1.163(9) . ? C10 H10 0.9300 . ? C11 C12 1.374(8) . ? C11 C16 1.399(9) . ? C12 C13 1.389(9) . ? C12 H12 0.9300 . ? C13 C14 1.344(11) . ? C13 H13 0.9300 . ? C14 C15 1.362(11) . ? C14 H14 0.9300 . ? C15 C16 1.394(10) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.389(8) . ? C17 C22 1.394(7) . ? C18 C19 1.386(8) . ? C18 H18 0.9300 . ? C19 C20 1.387(9) . ? C19 H19 0.9300 . ? C20 C21 1.372(10) . ? C20 H20 0.9300 . ? C21 C22 1.393(8) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.374(8) . ? C23 C28 1.383(8) . ? C24 C25 1.383(8) . ? C24 H24 0.9300 . ? C25 C26 1.351(9) . ? C25 H25 0.9300 . ? C26 C27 1.363(10) . ? C26 H26 0.9300 . ? C27 C28 1.390(10) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.383(8) . ? C29 C34 1.398(8) . ? C30 C31 1.380(8) . ? C30 H30 0.9300 . ? C31 C32 1.374(10) . ? C31 H31 0.9300 . ? C32 C33 1.367(10) . ? C32 H32 0.9300 . ? C33 C34 1.385(8) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C40 1.389(8) . ? C35 C36 1.391(8) . ? C36 C37 1.390(9) . ? C36 H36 0.9300 . ? C37 C38 1.361(11) . ? C37 H37 0.9300 . ? C38 C39 1.385(11) . ? C38 H38 0.9300 . ? C39 C40 1.377(9) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C41 C42 1.385(8) . ? C41 C46 1.392(8) . ? C42 C43 1.384(8) . ? C42 H42 0.9300 . ? C43 C44 1.369(10) . ? C43 H43 0.9300 . ? C44 C45 1.370(10) . ? C44 H44 0.9300 . ? C45 C46 1.378(8) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 Cl3 1.581(15) . ? C47 Cl4 1.80(2) . ? C47 H471 0.9700 . ? C47 H472 0.9700 . ? 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 N3 84.83(18) . . ? N1 Re1 Cl2 170.69(14) . . ? N3 Re1 Cl2 85.86(12) . . ? N1 Re1 Cl1 96.09(14) . . ? N3 Re1 Cl1 178.98(13) . . ? Cl2 Re1 Cl1 93.21(5) . . ? N1 Re1 P1 92.31(15) . . ? N3 Re1 P1 91.87(13) . . ? Cl2 Re1 P1 87.69(5) . . ? Cl1 Re1 P1 87.66(5) . . ? N1 Re1 P2 93.03(15) . . ? N3 Re1 P2 90.24(13) . . ? Cl2 Re1 P2 87.31(5) . . ? Cl1 Re1 P2 90.14(5) . . ? P1 Re1 P2 174.41(5) . . ? C17 P1 C11 106.0(3) . . ? C17 P1 C23 102.2(3) . . ? C11 P1 C23 102.4(3) . . ? C17 P1 Re1 112.38(18) . . ? C11 P1 Re1 112.7(2) . . ? C23 P1 Re1 119.75(19) . . ? C35 P2 C41 101.6(3) . . ? C35 P2 C29 107.8(3) . . ? C41 P2 C29 102.5(2) . . ? C35 P2 Re1 111.96(18) . . ? C41 P2 Re1 119.91(19) . . ? C29 P2 Re1 111.86(19) . . ? N2 N1 Re1 177.0(4) . . ? N1 N2 C1 116.1(5) . . ? C8 N3 Re1 125.8(3) . . ? C8 N3 H3A 105.9 . . ? Re1 N3 H3A 105.9 . . ? C8 N3 H3B 105.9 . . ? Re1 N3 H3B 105.9 . . ? H3A N3 H3B 106.2 . . ? O1 C1 N2 123.9(5) . . ? O1 C1 C2 122.1(5) . . ? N2 C1 C2 114.0(5) . . ? C7 C2 C3 119.0(6) . . ? C7 C2 C1 121.8(6) . . ? C3 C2 C1 119.0(6) . . ? C4 C3 C2 119.5(7) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C5 C4 C3 121.5(7) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C4 C5 C6 119.1(8) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C5 C6 C7 120.5(9) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C2 C7 C6 120.3(7) . . ? C2 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? N3 C8 C9 108.1(5) . . ? N3 C8 H81 110.1 . . ? C9 C8 H81 110.1 . . ? N3 C8 H82 110.1 . . ? C9 C8 H82 110.1 . . ? H81 C8 H82 108.4 . . ? C10 C9 C8 174.8(7) . . ? C9 C10 H10 180.0 . . ? C12 C11 C16 118.9(6) . . ? C12 C11 P1 124.6(5) . . ? C16 C11 P1 116.5(5) . . ? C11 C12 C13 120.8(7) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C14 C13 C12 120.0(7) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 120.7(7) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C14 C15 C16 120.8(8) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C15 C16 C11 118.8(7) . . ? C15 C16 H16 120.6 . . ? C11 C16 H16 120.6 . . ? C18 C17 C22 119.0(5) . . ? C18 C17 P1 119.8(4) . . ? C22 C17 P1 120.7(4) . . ? C19 C18 C17 120.0(6) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 120.9(6) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C21 C20 C19 119.1(6) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C20 C21 C22 120.7(6) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C21 C22 C17 120.2(6) . . ? C21 C22 H22 119.9 . . ? C17 C22 H22 119.9 . . ? C24 C23 C28 117.8(6) . . ? C24 C23 P1 123.2(4) . . ? C28 C23 P1 118.9(5) . . ? C23 C24 C25 120.9(6) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C26 C25 C24 120.8(6) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C25 C26 C27 119.6(7) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C26 C27 C28 120.2(7) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C23 C28 C27 120.6(7) . . ? C23 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C30 C29 C34 118.2(5) . . ? C30 C29 P2 118.9(4) . . ? C34 C29 P2 122.3(4) . . ? C31 C30 C29 120.5(6) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C32 C31 C30 120.6(6) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C33 C32 C31 119.9(6) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C32 C33 C34 120.1(6) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C33 C34 C29 120.7(6) . . ? C33 C34 H34 119.7 . . ? C29 C34 H34 119.7 . . ? C40 C35 C36 118.9(6) . . ? C40 C35 P2 116.4(5) . . ? C36 C35 P2 124.7(5) . . ? C37 C36 C35 119.9(6) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C38 C37 C36 120.5(7) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C37 C38 C39 120.2(7) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C40 C39 C38 119.8(7) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C39 C40 C35 120.7(6) . . ? C39 C40 H40 119.7 . . ? C35 C40 H40 119.7 . . ? C42 C41 C46 118.7(5) . . ? C42 C41 P2 122.1(4) . . ? C46 C41 P2 119.2(5) . . ? C43 C42 C41 120.3(6) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C44 C43 C42 120.3(7) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C43 C44 C45 120.1(6) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C44 C45 C46 120.3(6) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C45 C46 C41 120.4(6) . . ? C45 C46 H46 119.8 . . ? C41 C46 H46 119.8 . . ? Cl3 C47 Cl4 108.9(9) . . ? Cl3 C47 H471 109.9 . . ? Cl4 C47 H471 109.9 . . ? Cl3 C47 H472 109.9 . . ? Cl4 C47 H472 109.9 . . ? H471 C47 H472 108.3 . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 1.469 _refine_diff_density_min -0.951 _refine_diff_density_rms 0.116