# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_[Re(HPAN)(CO)3Cl] _database_code_depnum_ccdc_archive 'CCDC 894024' #TrackingRef 'Crystal.doc' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H11 Cl N3 O4 Re' _chemical_formula_weight 554.95 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' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.2245(15) _cell_length_b 7.2396(6) _cell_length_c 14.8995(13) _cell_angle_alpha 90.00 _cell_angle_beta 112.193(4) _cell_angle_gamma 90.00 _cell_volume 1820.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 25.00 _exptl_crystal_description parallopiped _exptl_crystal_colour violet _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.025 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 6.852 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.140 _exptl_absorpt_correction_T_max 0.180 _exptl_absorpt_process_details (SADABAS,SHELDRICK-1997) _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13661 _diffrn_reflns_av_R_equivalents 0.0225 _diffrn_reflns_av_sigmaI/netI 0.0193 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3166 _reflns_number_gt 2722 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0234P)^2^+1.9841P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3166 _refine_ls_number_parameters 248 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0278 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_ref 0.0561 _refine_ls_wR_factor_gt 0.0538 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C14 C -0.0257(3) 0.7438(5) -0.0737(4) 0.0597(14) Uani 1 1 d . . . H14 H -0.0639 0.8059 -0.0581 0.072 Uiso 1 1 calc R . . C15 C -0.0431(3) 0.6877(7) -0.1656(4) 0.0632(13) Uani 1 1 d . . . H15 H -0.0931 0.7104 -0.2125 0.076 Uiso 1 1 calc R . . H4A H 0.301(3) 0.562(7) 0.201(3) 0.063(17) Uiso 1 1 d . . . C1 C 0.2534(3) 0.1783(6) 0.1617(3) 0.0516(11) Uani 1 1 d . . . C2 C 0.2109(3) 0.1217(6) -0.0307(4) 0.0547(11) Uani 1 1 d . . . C3 C 0.3574(3) 0.0138(7) 0.0945(3) 0.0577(12) Uani 1 1 d . . . C4 C 0.4047(3) 0.2848(7) -0.0594(4) 0.0582(13) Uani 1 1 d . . . H4 H 0.4213 0.1639 -0.0421 0.070 Uiso 1 1 calc R . . C5 C 0.4381(3) 0.3835(8) -0.1133(3) 0.0647(14) Uani 1 1 d . . . H5 H 0.4762 0.3291 -0.1322 0.078 Uiso 1 1 calc R . . C6 C 0.4149(3) 0.5620(9) -0.1389(3) 0.0645(14) Uani 1 1 d . . . H6 H 0.4376 0.6313 -0.1743 0.077 Uiso 1 1 calc R . . C7 C 0.3573(2) 0.6366(7) -0.1110(3) 0.0524(11) Uani 1 1 d . . . H7 H 0.3395 0.7568 -0.1284 0.063 Uiso 1 1 calc R . . C8 C 0.3267(2) 0.5315(6) -0.0574(3) 0.0398(9) Uani 1 1 d . . . C9 C 0.1843(2) 0.5888(5) 0.0484(3) 0.0376(9) Uani 1 1 d . . . C10 C 0.1995(3) 0.6316(6) 0.1436(3) 0.0521(11) Uani 1 1 d . . . C11 C 0.1401(3) 0.7199(6) 0.1674(4) 0.0630(14) Uani 1 1 d . . . H11 H 0.1500 0.7512 0.2314 0.076 Uiso 1 1 calc R . . C12 C 0.0691(3) 0.7590(5) 0.0978(4) 0.0594(14) Uani 1 1 d . . . H12 H 0.0314 0.8203 0.1148 0.071 Uiso 1 1 calc R . . C13 C 0.0502(3) 0.7099(5) 0.0001(4) 0.0463(11) Uani 1 1 d . . . C16 C 0.0135(2) 0.5956(7) -0.1907(3) 0.0560(12) Uani 1 1 d . . . H16 H 0.0007 0.5548 -0.2540 0.067 Uiso 1 1 calc R . . C17 C 0.0877(2) 0.5648(6) -0.1231(3) 0.0438(10) Uani 1 1 d . . . H17 H 0.1250 0.5045 -0.1414 0.053 Uiso 1 1 calc R . . C18 C 0.1091(2) 0.6222(5) -0.0265(3) 0.0361(9) Uani 1 1 d . . . Cl1 Cl 0.41017(6) 0.40871(16) 0.19066(8) 0.0515(3) Uani 1 1 d . . . N1 N 0.34873(18) 0.3571(5) -0.0306(2) 0.0413(8) Uani 1 1 d . . . N2 N 0.26793(17) 0.6104(4) -0.0305(2) 0.0397(7) Uani 1 1 d . . . N3 N 0.24762(17) 0.5077(4) 0.0253(2) 0.0335(7) Uani 1 1 d . . . O1 O 0.22831(19) 0.1423(5) 0.2190(3) 0.0721(10) Uani 1 1 d . . . O2 O 0.1581(2) 0.0507(5) -0.0877(3) 0.0885(12) Uani 1 1 d . . . O3 O 0.3943(2) -0.1180(5) 0.1086(3) 0.0880(12) Uani 1 1 d . . . O4 O 0.2701(2) 0.6033(6) 0.2181(2) 0.0765(12) Uani 1 1 d . . . Re1 Re 0.298584(9) 0.242682(19) 0.067103(12) 0.03947(7) 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 C14 0.046(3) 0.047(3) 0.098(4) 0.020(3) 0.041(3) 0.015(2) C15 0.041(3) 0.072(3) 0.078(4) 0.029(3) 0.024(3) 0.011(2) C1 0.040(2) 0.041(2) 0.065(3) 0.010(2) 0.009(2) 0.0002(19) C2 0.050(3) 0.038(3) 0.064(3) 0.002(2) 0.007(2) 0.002(2) C3 0.049(3) 0.050(3) 0.063(3) -0.004(2) 0.009(2) 0.004(2) C4 0.043(3) 0.067(3) 0.062(3) -0.019(2) 0.016(2) 0.008(2) C5 0.037(2) 0.110(5) 0.048(3) -0.023(3) 0.018(2) 0.002(3) C6 0.043(3) 0.114(5) 0.037(3) 0.001(3) 0.016(2) -0.004(3) C7 0.041(2) 0.074(3) 0.043(2) 0.014(2) 0.016(2) 0.005(2) C8 0.034(2) 0.053(3) 0.031(2) 0.0002(18) 0.0110(17) 0.0033(18) C9 0.042(2) 0.031(2) 0.047(2) -0.0061(17) 0.0252(19) -0.0024(16) C10 0.055(3) 0.051(3) 0.053(3) -0.017(2) 0.024(2) -0.008(2) C11 0.079(4) 0.058(3) 0.068(3) -0.028(2) 0.047(3) -0.010(3) C12 0.068(3) 0.040(3) 0.090(4) -0.013(2) 0.052(3) 0.000(2) C13 0.050(3) 0.030(2) 0.073(3) 0.008(2) 0.039(2) 0.0017(18) C16 0.045(3) 0.070(3) 0.054(3) 0.015(2) 0.021(2) 0.002(2) C17 0.037(2) 0.051(3) 0.048(2) 0.009(2) 0.0222(19) 0.0051(18) C18 0.036(2) 0.0248(19) 0.054(2) 0.0067(17) 0.0233(19) 0.0012(15) Cl1 0.0391(5) 0.0618(7) 0.0465(6) 0.0036(5) 0.0082(5) -0.0088(5) N1 0.0346(17) 0.050(2) 0.0373(18) -0.0076(16) 0.0108(15) 0.0048(15) N2 0.0352(17) 0.0421(19) 0.0435(19) 0.0057(15) 0.0166(15) 0.0031(14) N3 0.0321(16) 0.0320(18) 0.0364(17) -0.0049(14) 0.0128(14) -0.0026(13) O1 0.056(2) 0.088(3) 0.079(2) 0.032(2) 0.0329(19) 0.0023(19) O2 0.077(3) 0.064(2) 0.088(3) -0.010(2) -0.012(2) -0.018(2) O3 0.080(3) 0.057(2) 0.107(3) 0.001(2) 0.012(2) 0.030(2) O4 0.066(2) 0.108(3) 0.052(2) -0.036(2) 0.0176(19) 0.003(2) Re1 0.03395(11) 0.03389(12) 0.04544(12) 0.00119(7) 0.00918(8) 0.00166(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 C14 C15 1.345(7) . ? C14 C13 1.426(7) . ? C15 C16 1.392(6) . ? C1 O1 1.140(5) . ? C1 Re1 1.939(5) . ? C2 O2 1.138(5) . ? C2 Re1 1.920(5) . ? C3 O3 1.140(5) . ? C3 Re1 1.932(5) . ? C4 N1 1.353(5) . ? C4 C5 1.376(7) . ? C5 C6 1.368(7) . ? C6 C7 1.377(6) . ? C7 C8 1.366(5) . ? C8 N1 1.339(5) . ? C8 N2 1.399(4) . ? C9 C10 1.373(5) . ? C9 C18 1.424(5) . ? C9 N3 1.447(4) . ? C10 O4 1.360(6) . ? C10 C11 1.414(6) . ? C11 C12 1.347(8) . ? C12 C13 1.409(7) . ? C13 C18 1.426(5) . ? C16 C17 1.365(6) . ? C17 C18 1.404(5) . ? Cl1 Re1 2.4781(10) . ? N1 Re1 2.155(3) . ? N2 N3 1.271(4) . ? N3 Re1 2.120(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15 C14 C13 121.3(4) . . ? C14 C15 C16 120.2(5) . . ? O1 C1 Re1 178.4(4) . . ? O2 C2 Re1 178.8(4) . . ? O3 C3 Re1 176.8(4) . . ? N1 C4 C5 122.5(5) . . ? C6 C5 C4 119.6(4) . . ? C5 C6 C7 118.5(4) . . ? C8 C7 C6 118.9(5) . . ? N1 C8 C7 123.9(4) . . ? N1 C8 N2 118.4(3) . . ? C7 C8 N2 117.7(4) . . ? C10 C9 C18 122.0(3) . . ? C10 C9 N3 117.9(4) . . ? C18 C9 N3 120.0(3) . . ? O4 C10 C9 124.7(4) . . ? O4 C10 C11 116.2(4) . . ? C9 C10 C11 119.0(4) . . ? C12 C11 C10 120.4(5) . . ? C11 C12 C13 122.0(4) . . ? C12 C13 C14 122.7(4) . . ? C12 C13 C18 118.9(4) . . ? C14 C13 C18 118.3(4) . . ? C17 C16 C15 120.5(5) . . ? C16 C17 C18 121.4(4) . . ? C17 C18 C9 124.4(3) . . ? C17 C18 C13 118.1(4) . . ? C9 C18 C13 117.4(4) . . ? C8 N1 C4 116.6(4) . . ? C8 N1 Re1 114.1(2) . . ? C4 N1 Re1 128.9(3) . . ? N3 N2 C8 113.1(3) . . ? N2 N3 C9 112.0(3) . . ? N2 N3 Re1 121.2(2) . . ? C9 N3 Re1 126.7(2) . . ? C2 Re1 C3 90.32(18) . . ? C2 Re1 C1 88.93(19) . . ? C3 Re1 C1 89.68(19) . . ? C2 Re1 N3 92.47(14) . . ? C3 Re1 N3 170.06(16) . . ? C1 Re1 N3 99.90(15) . . ? C2 Re1 N1 96.14(17) . . ? C3 Re1 N1 97.43(16) . . ? C1 Re1 N1 171.22(15) . . ? N3 Re1 N1 72.79(11) . . ? C2 Re1 Cl1 178.11(13) . . ? C3 Re1 Cl1 91.43(14) . . ? C1 Re1 Cl1 91.78(14) . . ? N3 Re1 Cl1 85.69(8) . . ? N1 Re1 Cl1 82.93(9) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.399 _refine_diff_density_min -1.074 _refine_diff_density_rms 0.100 data_[Re2(PAN)2(CO)6].C6H12 _database_code_depnum_ccdc_archive 'CCDC 894025' #TrackingRef 'Crystal.doc' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H16 Cl0 N3 O4 Re' _chemical_formula_weight 560.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.328(5) _cell_length_b 9.625(5) _cell_length_c 11.929(5) _cell_angle_alpha 83.557(5) _cell_angle_beta 68.824(5) _cell_angle_gamma 78.410(5) _cell_volume 977.4(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.83 _cell_measurement_theta_max 25.00 _exptl_crystal_description parallopiped _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.905 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 6.249 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.167 _exptl_absorpt_correction_T_max 0.210 _exptl_absorpt_process_details (SADABAS,SHELDRICK-1997) _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9400 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3436 _reflns_number_gt 3353 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0218P)^2^+0.5988P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3436 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0239 _refine_ls_R_factor_gt 0.0229 _refine_ls_wR_factor_ref 0.0541 _refine_ls_wR_factor_gt 0.0537 _refine_ls_goodness_of_fit_ref 1.185 _refine_ls_restrained_S_all 1.185 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2743(5) 0.1605(5) 0.1142(4) 0.0489(10) Uani 1 1 d . . . C2 C 0.2883(5) -0.0050(5) -0.0540(4) 0.0444(10) Uani 1 1 d . . . C3 C 0.3030(5) -0.1250(5) 0.1499(4) 0.0510(11) Uani 1 1 d . . . C4 C -0.1082(5) -0.0178(4) 0.3531(4) 0.0397(9) Uani 1 1 d . . . C5 C -0.1777(5) 0.0103(5) 0.4789(4) 0.0468(10) Uani 1 1 d . . . H5 H -0.1405 0.0744 0.5097 0.056 Uiso 1 1 calc R . . C6 C -0.2946(5) -0.0531(5) 0.5533(4) 0.0496(11) Uani 1 1 d . . . H6 H -0.3332 -0.0344 0.6347 0.060 Uiso 1 1 calc R . . C7 C -0.3615(5) -0.1483(5) 0.5118(4) 0.0449(10) Uani 1 1 d . . . C8 C -0.4855(6) -0.2137(5) 0.5894(4) 0.0570(12) Uani 1 1 d . . . H8 H -0.5233 -0.1980 0.6713 0.068 Uiso 1 1 calc R . . C9 C -0.5507(6) -0.2996(5) 0.5458(5) 0.0629(13) Uani 1 1 d . . . H9 H -0.6313 -0.3435 0.5984 0.076 Uiso 1 1 calc R . . C10 C -0.4981(5) -0.3221(5) 0.4243(4) 0.0555(11) Uani 1 1 d . . . H10 H -0.5452 -0.3792 0.3953 0.067 Uiso 1 1 calc R . . C11 C -0.3767(5) -0.2608(4) 0.3458(4) 0.0460(10) Uani 1 1 d . . . H11 H -0.3433 -0.2756 0.2639 0.055 Uiso 1 1 calc R . . C12 C -0.3028(5) -0.1761(4) 0.3880(3) 0.0397(9) Uani 1 1 d . . . C13 C -0.1682(4) -0.1151(4) 0.3079(3) 0.0372(8) Uani 1 1 d . . . C14 C 0.0690(5) -0.2291(4) 0.0186(3) 0.0380(9) Uani 1 1 d . . . C15 C 0.1658(6) -0.3527(5) 0.0334(4) 0.0573(12) Uani 1 1 d . . . H15 H 0.1927 -0.3691 0.1022 0.069 Uiso 1 1 calc R . . C16 C 0.2224(6) -0.4515(5) -0.0532(4) 0.0643(13) Uani 1 1 d . . . H16 H 0.2874 -0.5357 -0.0445 0.077 Uiso 1 1 calc R . . C17 C 0.1798(6) -0.4219(5) -0.1534(4) 0.0597(13) Uani 1 1 d . . . H17 H 0.2161 -0.4860 -0.2144 0.072 Uiso 1 1 calc R . . C18 C -0.0843(6) 0.2981(5) 0.1623(4) 0.0536(11) Uani 1 1 d . . . H18 H -0.0572 0.2802 0.2309 0.064 Uiso 1 1 calc R . . N1 N -0.1049(4) -0.1718(3) 0.1987(3) 0.0378(7) Uani 1 1 d . . . N2 N 0.0120(4) -0.1287(3) 0.1126(3) 0.0367(7) Uani 1 1 d . . . N3 N -0.0257(4) 0.1986(3) 0.0779(3) 0.0377(7) Uani 1 1 d . . . O1 O 0.3447(4) 0.2443(4) 0.1166(4) 0.0751(10) Uani 1 1 d . . . O2 O 0.3739(4) -0.0260(4) -0.1510(3) 0.0620(9) Uani 1 1 d . . . O3 O 0.3932(5) -0.2126(4) 0.1724(4) 0.0781(11) Uani 1 1 d . . . O4 O 0.0073(3) 0.0442(3) 0.2900(2) 0.0456(7) Uani 1 1 d . . . Re1 Re 0.155357(17) 0.019781(16) 0.109139(13) 0.03846(7) Uani 1 1 d . . . C38 C 0.0486(12) 0.4686(11) 0.3770(7) 0.133(3) Uani 1 1 d . . . H10A H 0.0134 0.5070 0.3108 0.159 Uiso 1 1 calc R . . H10B H 0.1372 0.3936 0.3461 0.159 Uiso 1 1 calc R . . C39 C 0.1025(11) 0.5824(12) 0.4172(8) 0.151(4) Uani 1 1 d . . . H10C H 0.2148 0.5715 0.3774 0.181 Uiso 1 1 calc R . . H10D H 0.0575 0.6725 0.3879 0.181 Uiso 1 1 calc R . . C37 C -0.0714(14) 0.4084(12) 0.4644(9) 0.171(5) Uani 1 1 d . . . H10E H -0.1670 0.4489 0.4492 0.205 Uiso 1 1 calc R . . H10F H -0.0507 0.3081 0.4490 0.205 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 C1 0.050(3) 0.052(3) 0.050(3) -0.003(2) -0.021(2) -0.010(2) C2 0.044(2) 0.046(2) 0.043(2) -0.0006(19) -0.019(2) -0.0012(19) C3 0.052(3) 0.056(3) 0.048(3) 0.001(2) -0.022(2) -0.008(2) C4 0.043(2) 0.041(2) 0.0312(19) -0.0014(16) -0.0132(17) 0.0016(17) C5 0.059(3) 0.051(3) 0.031(2) -0.0156(18) -0.016(2) -0.002(2) C6 0.053(3) 0.063(3) 0.027(2) -0.0091(19) -0.0092(19) -0.001(2) C7 0.045(2) 0.047(2) 0.035(2) -0.0022(18) -0.0099(18) 0.0020(19) C8 0.057(3) 0.060(3) 0.036(2) -0.001(2) 0.001(2) -0.002(2) C9 0.053(3) 0.061(3) 0.057(3) 0.002(2) 0.001(2) -0.012(2) C10 0.049(3) 0.048(3) 0.064(3) -0.009(2) -0.011(2) -0.009(2) C11 0.048(2) 0.046(2) 0.038(2) -0.0098(18) -0.0093(19) -0.0011(19) C12 0.041(2) 0.039(2) 0.033(2) -0.0067(17) -0.0100(17) 0.0020(17) C13 0.041(2) 0.041(2) 0.0272(18) -0.0040(16) -0.0124(16) 0.0017(17) C14 0.040(2) 0.039(2) 0.0303(19) -0.0104(16) -0.0065(16) -0.0034(17) C15 0.071(3) 0.052(3) 0.044(2) -0.008(2) -0.022(2) 0.007(2) C16 0.076(3) 0.046(3) 0.056(3) -0.011(2) -0.016(3) 0.015(2) C17 0.078(3) 0.049(3) 0.041(2) -0.016(2) -0.008(2) -0.001(2) C18 0.070(3) 0.050(3) 0.037(2) -0.0135(19) -0.015(2) -0.002(2) N1 0.0386(18) 0.0440(18) 0.0307(17) -0.0070(14) -0.0139(14) -0.0002(14) N2 0.0438(18) 0.0390(18) 0.0259(16) -0.0057(13) -0.0109(14) -0.0039(14) N3 0.0431(18) 0.0384(18) 0.0292(16) -0.0093(13) -0.0085(14) -0.0053(14) O1 0.073(2) 0.070(2) 0.093(3) -0.003(2) -0.034(2) -0.029(2) O2 0.0539(19) 0.077(2) 0.0383(17) -0.0049(15) -0.0044(15) 0.0060(17) O3 0.074(2) 0.078(3) 0.090(3) 0.017(2) -0.048(2) -0.004(2) O4 0.0524(17) 0.0559(18) 0.0303(14) -0.0083(13) -0.0119(13) -0.0147(14) Re1 0.04125(11) 0.04405(11) 0.03043(10) -0.00465(7) -0.01259(7) -0.00628(7) C38 0.158(8) 0.168(9) 0.071(5) -0.036(5) -0.016(5) -0.054(7) C39 0.166(8) 0.242(12) 0.096(6) 0.056(7) -0.064(6) -0.150(9) C37 0.252(13) 0.195(10) 0.115(7) -0.015(7) -0.054(8) -0.163(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.147(5) . ? C1 Re1 1.934(5) . ? C2 O2 1.157(6) . ? C2 Re1 1.904(5) . ? C3 O3 1.148(6) . ? C3 Re1 1.907(5) . ? C4 O4 1.287(5) . ? C4 C13 1.422(6) . ? C4 C5 1.437(5) . ? C5 C6 1.339(6) . ? C6 C7 1.424(6) . ? C7 C8 1.407(6) . ? C7 C12 1.414(6) . ? C8 C9 1.360(7) . ? C9 C10 1.380(7) . ? C10 C11 1.373(6) . ? C11 C12 1.400(6) . ? C12 C13 1.462(6) . ? C13 N1 1.348(5) . ? C14 N3 1.337(5) 2 ? C14 C15 1.378(6) . ? C14 N2 1.442(5) . ? C15 C16 1.369(6) . ? C16 C17 1.375(7) . ? C17 C18 1.355(7) 2 ? C18 C17 1.355(7) 2 ? C18 N3 1.356(5) . ? N1 N2 1.301(4) . ? N2 Re1 2.133(3) . ? N3 C14 1.337(5) 2 ? N3 Re1 2.258(3) . ? O4 Re1 2.109(3) . ? C38 C37 1.399(11) . ? C38 C39 1.481(11) . ? C39 C37 1.346(11) 2_566 ? C37 C39 1.346(11) 2_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 Re1 179.6(4) . . ? O2 C2 Re1 176.4(4) . . ? O3 C3 Re1 178.8(4) . . ? O4 C4 C13 124.7(4) . . ? O4 C4 C5 117.3(4) . . ? C13 C4 C5 118.0(4) . . ? C6 C5 C4 122.0(4) . . ? C5 C6 C7 122.1(4) . . ? C8 C7 C12 118.9(4) . . ? C8 C7 C6 122.3(4) . . ? C12 C7 C6 118.8(4) . . ? C9 C8 C7 120.7(4) . . ? C8 C9 C10 120.5(4) . . ? C11 C10 C9 120.5(5) . . ? C10 C11 C12 120.5(4) . . ? C11 C12 C7 118.7(4) . . ? C11 C12 C13 122.0(4) . . ? C7 C12 C13 119.3(4) . . ? N1 C13 C4 126.9(4) . . ? N1 C13 C12 113.2(3) . . ? C4 C13 C12 119.6(3) . . ? N3 C14 C15 123.2(4) 2 . ? N3 C14 N2 118.9(3) 2 . ? C15 C14 N2 117.9(4) . . ? C16 C15 C14 120.0(4) . . ? C15 C16 C17 117.7(4) . . ? C18 C17 C16 119.3(4) 2 . ? C17 C18 N3 124.4(4) 2 . ? N2 N1 C13 123.0(3) . . ? N1 N2 C14 108.1(3) . . ? N1 N2 Re1 131.5(2) . . ? C14 N2 Re1 118.3(2) . . ? C14 N3 C18 115.4(4) 2 . ? C14 N3 Re1 129.0(2) 2 . ? C18 N3 Re1 115.1(3) . . ? C4 O4 Re1 130.1(3) . . ? C2 Re1 C3 86.52(19) . . ? C2 Re1 C1 87.37(19) . . ? C3 Re1 C1 89.6(2) . . ? C2 Re1 O4 179.14(14) . . ? C3 Re1 O4 93.16(16) . . ? C1 Re1 O4 93.42(16) . . ? C2 Re1 N2 95.93(16) . . ? C3 Re1 N2 92.13(17) . . ? C1 Re1 N2 176.35(15) . . ? O4 Re1 N2 83.29(11) . . ? C2 Re1 N3 98.22(15) . . ? C3 Re1 N3 174.74(15) . . ? C1 Re1 N3 88.33(16) . . ? O4 Re1 N3 82.14(12) . . ? N2 Re1 N3 89.66(13) . . ? C37 C38 C39 116.1(7) . . ? C37 C39 C38 118.7(7) 2_566 . ? C39 C37 C38 122.0(7) 2_566 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.507 _refine_diff_density_min -0.712 _refine_diff_density_rms 0.107 data_[Re(PAN)(CO)(P?P)].CH2Cl2 _database_code_depnum_ccdc_archive 'CCDC 894026' #TrackingRef 'Crystal.doc' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H36 Cl2 N3 O2 P2 Re' _chemical_formula_weight 945.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.429(2) _cell_length_b 28.788(6) _cell_length_c 12.820(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.00(3) _cell_angle_gamma 90.00 _cell_volume 3910.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.41 _cell_measurement_theta_max 25.00 _exptl_crystal_description parallopiped _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1880 _exptl_absorpt_coefficient_mu 3.367 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.379 _exptl_absorpt_correction_T_max 0.431 _exptl_absorpt_process_details (SADABAS,SHELDRICK-1997) _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18706 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0659 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6667 _reflns_number_gt 5780 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0383P)^2^+33.0079P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6667 _refine_ls_number_parameters 473 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1003 _refine_ls_R_factor_gt 0.0858 _refine_ls_wR_factor_ref 0.1631 _refine_ls_wR_factor_gt 0.1579 _refine_ls_goodness_of_fit_ref 1.346 _refine_ls_restrained_S_all 1.346 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8112(12) 0.7797(4) 0.7916(9) 0.034(3) Uani 1 1 d . . . C2 C 0.9341(12) 0.8820(5) 0.8421(10) 0.041(3) Uani 1 1 d . . . H2 H 0.9690 0.8551 0.8258 0.050 Uiso 1 1 calc R . . C3 C 0.9997(14) 0.9213(6) 0.8551(12) 0.058(4) Uani 1 1 d . . . H3 H 1.0793 0.9212 0.8512 0.070 Uiso 1 1 calc R . . C4 C 0.9472(16) 0.9622(6) 0.8744(13) 0.069(5) Uani 1 1 d . . . H4 H 0.9884 0.9904 0.8787 0.083 Uiso 1 1 calc R . . C5 C 0.8365(16) 0.9603(5) 0.8867(13) 0.064(4) Uani 1 1 d . . . H5 H 0.8023 0.9877 0.9012 0.076 Uiso 1 1 calc R . . C6 C 0.7692(13) 0.9187(4) 0.8786(10) 0.040(3) Uani 1 1 d . . . C7 C 0.5667(11) 0.8540(4) 0.9580(9) 0.030(3) Uani 1 1 d . . . C8 C 0.5946(12) 0.8079(4) 0.9825(9) 0.034(3) Uani 1 1 d . . . C9 C 0.5424(14) 0.7829(4) 1.0476(10) 0.048(4) Uani 1 1 d . . . H9 H 0.5590 0.7514 1.0619 0.057 Uiso 1 1 calc R . . C10 C 0.4659(13) 0.8064(5) 1.0897(13) 0.056(4) Uani 1 1 d . . . H10 H 0.4346 0.7901 1.1363 0.068 Uiso 1 1 calc R . . C11 C 0.4315(13) 0.8527(5) 1.0680(11) 0.045(3) Uani 1 1 d . . . C12 C 0.3467(15) 0.8743(6) 1.1077(11) 0.059(4) Uani 1 1 d . . . H12 H 0.3132 0.8579 1.1524 0.071 Uiso 1 1 calc R . . C13 C 0.3131(15) 0.9199(6) 1.0803(14) 0.067(5) Uani 1 1 d . . . H13 H 0.2547 0.9338 1.1050 0.080 Uiso 1 1 calc R . . C14 C 0.3644(16) 0.9450(6) 1.0173(15) 0.071(5) Uani 1 1 d . . . H14 H 0.3421 0.9760 1.0017 0.085 Uiso 1 1 calc R . . C15 C 0.4470(13) 0.9254(5) 0.9772(11) 0.048(3) Uani 1 1 d . . . H15 H 0.4795 0.9430 0.9335 0.058 Uiso 1 1 calc R . . C16 C 0.4839(12) 0.8789(5) 1.0010(10) 0.039(3) Uani 1 1 d . . . C17 C 0.3853(11) 0.7736(4) 0.7466(10) 0.036(3) Uani 1 1 d . . . C18 C 0.3307(13) 0.8155(5) 0.7479(12) 0.051(4) Uani 1 1 d . . . H18 H 0.3621 0.8415 0.7237 0.061 Uiso 1 1 calc R . . C19 C 0.2313(15) 0.8217(7) 0.7832(15) 0.074(5) Uani 1 1 d . . . H19 H 0.1966 0.8509 0.7836 0.089 Uiso 1 1 calc R . . C20 C 0.1863(15) 0.7827(8) 0.8176(14) 0.072(5) Uani 1 1 d . . . H20 H 0.1191 0.7858 0.8414 0.087 Uiso 1 1 calc R . . C21 C 0.2362(15) 0.7394(7) 0.8183(13) 0.066(5) Uani 1 1 d . . . H21 H 0.2034 0.7136 0.8416 0.080 Uiso 1 1 calc R . . C22 C 0.3360(13) 0.7351(5) 0.7837(11) 0.051(4) Uani 1 1 d . . . H22 H 0.3716 0.7060 0.7850 0.061 Uiso 1 1 calc R . . C23 C 0.5599(11) 0.7077(4) 0.7201(10) 0.030(3) Uani 1 1 d . . . C24 C 0.6469(14) 0.6914(5) 0.8186(12) 0.053(4) Uani 1 1 d . . . H24 H 0.6924 0.7121 0.8749 0.063 Uiso 1 1 calc R . . C25 C 0.6678(13) 0.6429(5) 0.8352(12) 0.048(4) Uani 1 1 d . . . H25 H 0.7232 0.6314 0.9036 0.058 Uiso 1 1 calc R . . C26 C 0.6042(15) 0.6132(5) 0.7475(13) 0.056(4) Uani 1 1 d . . . H26 H 0.6198 0.5814 0.7560 0.067 Uiso 1 1 calc R . . C27 C 0.5210(16) 0.6295(5) 0.6511(13) 0.061(4) Uani 1 1 d . . . H27 H 0.4795 0.6090 0.5930 0.073 Uiso 1 1 calc R . . C28 C 0.4955(14) 0.6765(5) 0.6361(11) 0.057(4) Uani 1 1 d . . . H28 H 0.4347 0.6871 0.5693 0.069 Uiso 1 1 calc R . . C29 C 0.4639(11) 0.7836(5) 0.5587(9) 0.038(3) Uani 1 1 d . . . H29A H 0.4262 0.7561 0.5155 0.046 Uiso 1 1 calc R . . H29B H 0.3996 0.8075 0.5416 0.046 Uiso 1 1 calc R . . C30 C 0.5710(13) 0.8002(5) 0.5272(10) 0.043(3) Uani 1 1 d . . . H30A H 0.5392 0.8108 0.4497 0.052 Uiso 1 1 calc R . . H30B H 0.6302 0.7751 0.5347 0.052 Uiso 1 1 calc R . . C31 C 0.7805(12) 0.8670(4) 0.5825(10) 0.038(3) Uani 1 1 d . . . C32 C 0.8530(13) 0.8357(5) 0.5572(11) 0.046(3) Uiso 1 1 d . . . H32 H 0.8332 0.8043 0.5540 0.056 Uiso 1 1 calc R . . C33 C 0.9581(18) 0.8504(7) 0.5356(15) 0.079(5) Uani 1 1 d . . . H33 H 1.0107 0.8286 0.5222 0.095 Uiso 1 1 calc R . . C34 C 0.9841(17) 0.8964(7) 0.5342(14) 0.072(5) Uani 1 1 d . . . H34 H 1.0519 0.9059 0.5161 0.087 Uiso 1 1 calc R . . C35 C 0.9097(17) 0.9294(6) 0.5597(14) 0.073(5) Uani 1 1 d . . . H35 H 0.9277 0.9610 0.5605 0.088 Uiso 1 1 calc R . . C36 C 0.8065(14) 0.9135(5) 0.5842(13) 0.057(4) Uani 1 1 d . . . H36 H 0.7554 0.9348 0.6018 0.068 Uiso 1 1 calc R . . C37 C 0.5329(13) 0.8945(5) 0.5632(11) 0.046(3) Uani 1 1 d . . . C38 C 0.4985(14) 0.9092(5) 0.4521(12) 0.056(4) Uani 1 1 d . . . H38 H 0.5360 0.8955 0.4067 0.067 Uiso 1 1 calc R . . C39 C 0.4107(17) 0.9433(6) 0.4088(16) 0.080(6) Uani 1 1 d . . . H39 H 0.3893 0.9531 0.3348 0.096 Uiso 1 1 calc R . . C40 C 0.3545(19) 0.9629(6) 0.475(2) 0.093(7) Uani 1 1 d . . . H40 H 0.2938 0.9859 0.4453 0.112 Uiso 1 1 calc R . . C41 C 0.3859(16) 0.9494(6) 0.5840(18) 0.077(5) Uani 1 1 d . . . H41 H 0.3462 0.9627 0.6282 0.093 Uiso 1 1 calc R . . C42 C 0.4780(14) 0.9153(5) 0.6288(14) 0.060(4) Uani 1 1 d . . . H42 H 0.5020 0.9068 0.7039 0.072 Uiso 1 1 calc R . . C43 C 1.247(3) 1.0671(13) 0.792(2) 0.203(19) Uani 1 1 d . . . H43A H 1.1970 1.0900 0.8124 0.244 Uiso 1 1 calc R . . H43B H 1.3155 1.0584 0.8618 0.244 Uiso 1 1 calc R . . N1 N 0.8181(9) 0.8785(4) 0.8511(8) 0.036(2) Uani 1 1 d . . . N2 N 0.6711(11) 0.9154(3) 0.9081(9) 0.042(3) Uani 1 1 d . . . N3 N 0.6295(9) 0.8714(3) 0.8927(7) 0.028(2) Uani 1 1 d . . . O1 O 0.8890(9) 0.7542(3) 0.7897(8) 0.053(3) Uani 1 1 d . . . O2 O 0.6732(8) 0.7871(3) 0.9419(6) 0.0346(19) Uani 1 1 d . . . P1 P 0.5233(3) 0.77008(11) 0.7097(2) 0.0314(7) Uani 1 1 d . . . P2 P 0.6492(3) 0.84792(11) 0.6217(3) 0.0343(7) Uani 1 1 d . . . Re1 Re 0.69520(5) 0.822658(16) 0.81037(4) 0.02873(16) Uani 1 1 d . . . Cl1 Cl 1.1530(8) 1.0182(3) 0.7450(7) 0.158(3) Uani 1 1 d . . . Cl2 Cl 1.3022(14) 1.0898(7) 0.7271(7) 0.384(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.031(7) 0.039(7) 0.023(6) 0.003(5) -0.001(5) 0.000(6) C2 0.041(8) 0.040(7) 0.045(7) -0.003(6) 0.018(6) -0.003(6) C3 0.039(9) 0.082(12) 0.056(9) -0.018(8) 0.021(7) -0.031(8) C4 0.071(12) 0.072(12) 0.079(11) -0.030(9) 0.045(10) -0.046(10) C5 0.083(13) 0.047(9) 0.072(10) -0.017(8) 0.043(10) -0.021(9) C6 0.048(9) 0.037(7) 0.038(7) -0.004(6) 0.019(6) 0.000(6) C7 0.030(7) 0.033(7) 0.027(6) 0.004(5) 0.009(5) 0.012(5) C8 0.035(8) 0.039(7) 0.027(6) -0.004(5) 0.013(6) -0.006(6) C9 0.070(10) 0.028(7) 0.038(7) -0.003(6) 0.013(7) -0.001(7) C10 0.040(9) 0.065(10) 0.064(10) -0.031(8) 0.020(8) -0.008(7) C11 0.043(9) 0.053(9) 0.041(7) 0.006(6) 0.018(7) 0.004(7) C12 0.071(11) 0.077(12) 0.045(8) 0.001(8) 0.039(8) -0.014(9) C13 0.054(11) 0.072(12) 0.089(12) -0.008(10) 0.044(10) 0.006(9) C14 0.069(12) 0.059(10) 0.104(14) 0.013(9) 0.056(11) 0.017(9) C15 0.048(9) 0.048(8) 0.052(8) 0.006(7) 0.023(7) 0.005(7) C16 0.037(8) 0.051(8) 0.031(6) -0.005(6) 0.016(6) -0.004(6) C17 0.027(7) 0.042(7) 0.032(6) -0.002(5) 0.004(6) -0.008(6) C18 0.034(8) 0.059(10) 0.061(9) -0.005(7) 0.020(7) 0.014(7) C19 0.046(10) 0.080(12) 0.091(13) -0.031(11) 0.019(9) 0.017(10) C20 0.032(10) 0.113(16) 0.073(11) -0.019(11) 0.022(8) -0.008(10) C21 0.059(11) 0.090(13) 0.057(10) 0.007(9) 0.030(9) -0.008(10) C22 0.036(8) 0.062(10) 0.056(9) -0.006(7) 0.018(7) -0.008(7) C23 0.029(7) 0.024(6) 0.038(6) -0.005(5) 0.013(6) -0.001(5) C24 0.057(10) 0.036(8) 0.060(9) -0.002(6) 0.016(8) -0.008(7) C25 0.046(9) 0.040(8) 0.053(9) 0.008(6) 0.014(7) 0.017(7) C26 0.078(12) 0.024(7) 0.068(10) -0.002(7) 0.030(9) 0.008(7) C27 0.082(12) 0.034(8) 0.057(9) -0.010(7) 0.013(9) 0.000(8) C28 0.066(10) 0.051(9) 0.041(7) -0.006(7) 0.004(7) 0.002(8) C29 0.028(7) 0.042(7) 0.035(7) 0.003(6) -0.001(6) -0.007(6) C30 0.048(9) 0.049(8) 0.036(7) -0.002(6) 0.019(6) -0.005(7) C31 0.042(8) 0.037(7) 0.033(7) 0.001(5) 0.011(6) -0.001(6) C33 0.075(13) 0.088(14) 0.080(12) 0.010(11) 0.038(11) 0.029(11) C34 0.066(12) 0.092(14) 0.080(12) 0.019(10) 0.050(10) 0.004(11) C35 0.072(13) 0.064(11) 0.079(12) 0.017(9) 0.023(10) -0.012(10) C36 0.043(9) 0.045(9) 0.079(11) 0.006(8) 0.019(8) -0.001(7) C37 0.037(8) 0.043(8) 0.053(8) 0.007(6) 0.012(7) 0.000(6) C38 0.041(9) 0.052(9) 0.060(9) 0.022(7) 0.002(7) -0.005(7) C39 0.057(12) 0.061(11) 0.083(13) 0.035(10) -0.017(10) -0.010(9) C40 0.065(13) 0.033(9) 0.16(2) 0.015(12) 0.012(14) 0.003(9) C41 0.063(12) 0.051(10) 0.112(16) 0.006(10) 0.026(11) 0.020(9) C42 0.046(10) 0.039(8) 0.080(11) 0.003(8) 0.007(8) 0.015(7) C43 0.18(3) 0.35(5) 0.11(2) -0.09(3) 0.08(2) -0.17(3) N1 0.029(6) 0.044(6) 0.037(6) -0.013(5) 0.014(5) -0.013(5) N2 0.060(8) 0.025(5) 0.056(7) -0.009(5) 0.038(6) -0.006(5) N3 0.043(6) 0.015(4) 0.032(5) -0.005(4) 0.022(5) 0.002(4) O1 0.048(6) 0.055(6) 0.061(6) 0.002(5) 0.027(5) 0.028(5) O2 0.041(5) 0.032(4) 0.028(4) 0.002(3) 0.011(4) 0.006(4) P1 0.0264(18) 0.0340(17) 0.0311(16) -0.0017(13) 0.0076(14) 0.0012(14) P2 0.034(2) 0.0333(17) 0.0353(17) -0.0001(13) 0.0126(15) -0.0021(15) Re1 0.0262(3) 0.0294(2) 0.0292(2) -0.0043(2) 0.00872(19) 0.0009(2) Cl1 0.167(7) 0.141(6) 0.150(6) 0.021(5) 0.042(5) -0.062(5) Cl2 0.352(17) 0.66(3) 0.095(6) -0.001(11) 0.027(8) -0.38(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 C1 O1 1.160(14) . ? C1 Re1 1.893(13) . ? C2 C3 1.333(18) . ? C2 N1 1.376(15) . ? C3 C4 1.39(2) . ? C4 C5 1.33(2) . ? C5 C6 1.407(18) . ? C6 N2 1.314(16) . ? C6 N1 1.386(15) . ? C7 C8 1.374(16) . ? C7 N3 1.386(14) . ? C7 C16 1.451(16) . ? C8 O2 1.335(13) . ? C8 C9 1.395(17) . ? C9 C10 1.366(18) . ? C10 C11 1.39(2) . ? C11 C12 1.397(19) . ? C11 C16 1.431(17) . ? C12 C13 1.38(2) . ? C13 C14 1.37(2) . ? C14 C15 1.355(19) . ? C15 C16 1.401(18) . ? C17 C18 1.362(17) . ? C17 C22 1.405(18) . ? C17 P1 1.811(13) . ? C18 C19 1.38(2) . ? C19 C20 1.38(2) . ? C20 C21 1.37(2) . ? C21 C22 1.375(19) . ? C23 C24 1.365(18) . ? C23 C28 1.384(17) . ? C23 P1 1.838(11) . ? C24 C25 1.419(18) . ? C25 C26 1.383(19) . ? C26 C27 1.33(2) . ? C27 C28 1.381(19) . ? C29 C30 1.503(17) . ? C29 P1 1.837(12) . ? C30 P2 1.829(13) . ? C31 C32 1.344(18) . ? C31 C36 1.371(18) . ? C31 P2 1.836(13) . ? C32 C33 1.39(2) . ? C33 C34 1.36(2) . ? C34 C35 1.39(2) . ? C35 C36 1.41(2) . ? C37 C42 1.36(2) . ? C37 C38 1.394(18) . ? C37 P2 1.839(14) . ? C38 C39 1.37(2) . ? C39 C40 1.36(3) . ? C40 C41 1.36(3) . ? C41 C42 1.40(2) . ? C43 Cl2 1.38(3) . ? C43 Cl1 1.74(3) . ? N1 Re1 2.069(9) . ? N2 N3 1.342(12) . ? N3 Re1 2.060(8) . ? O2 Re1 2.066(7) . ? P1 Re1 2.433(3) . ? P2 Re1 2.388(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 Re1 174.1(10) . . ? C3 C2 N1 124.4(13) . . ? C2 C3 C4 118.9(14) . . ? C5 C4 C3 118.6(15) . . ? C4 C5 C6 122.9(15) . . ? N2 C6 N1 118.9(11) . . ? N2 C6 C5 122.8(12) . . ? N1 C6 C5 117.9(12) . . ? C8 C7 N3 111.1(10) . . ? C8 C7 C16 121.3(11) . . ? N3 C7 C16 127.6(10) . . ? O2 C8 C7 118.4(10) . . ? O2 C8 C9 120.3(11) . . ? C7 C8 C9 121.4(11) . . ? C10 C9 C8 117.5(13) . . ? C9 C10 C11 124.8(15) . . ? C10 C11 C12 122.4(13) . . ? C10 C11 C16 118.4(13) . . ? C12 C11 C16 119.2(13) . . ? C13 C12 C11 119.8(13) . . ? C14 C13 C12 120.9(14) . . ? C15 C14 C13 121.1(15) . . ? C14 C15 C16 120.7(14) . . ? C15 C16 C11 118.3(12) . . ? C15 C16 C7 125.1(11) . . ? C11 C16 C7 116.5(12) . . ? C18 C17 C22 116.8(13) . . ? C18 C17 P1 120.0(10) . . ? C22 C17 P1 123.0(10) . . ? C17 C18 C19 123.6(16) . . ? C20 C19 C18 116.9(16) . . ? C21 C20 C19 122.7(16) . . ? C20 C21 C22 118.3(16) . . ? C21 C22 C17 121.6(15) . . ? C24 C23 C28 119.2(12) . . ? C24 C23 P1 118.0(9) . . ? C28 C23 P1 122.6(10) . . ? C23 C24 C25 120.0(13) . . ? C26 C25 C24 118.6(13) . . ? C27 C26 C25 120.8(13) . . ? C26 C27 C28 121.0(14) . . ? C27 C28 C23 120.3(13) . . ? C30 C29 P1 109.5(8) . . ? C29 C30 P2 107.8(9) . . ? C32 C31 C36 120.6(13) . . ? C32 C31 P2 120.5(10) . . ? C36 C31 P2 118.8(11) . . ? C31 C32 C33 120.0(14) . . ? C34 C33 C32 120.4(16) . . ? C33 C34 C35 120.4(16) . . ? C34 C35 C36 117.9(16) . . ? C31 C36 C35 120.6(15) . . ? C42 C37 C38 118.6(14) . . ? C42 C37 P2 119.9(11) . . ? C38 C37 P2 121.5(11) . . ? C39 C38 C37 121.1(17) . . ? C40 C39 C38 119.4(18) . . ? C41 C40 C39 121.0(18) . . ? C40 C41 C42 119.4(19) . . ? C37 C42 C41 120.5(16) . . ? Cl2 C43 Cl1 122.2(18) . . ? C2 N1 C6 117.0(11) . . ? C2 N1 Re1 128.3(8) . . ? C6 N1 Re1 114.3(8) . . ? C6 N2 N3 108.5(10) . . ? N2 N3 C7 119.2(9) . . ? N2 N3 Re1 122.8(7) . . ? C7 N3 Re1 115.7(7) . . ? C8 O2 Re1 113.7(7) . . ? C17 P1 C29 104.5(6) . . ? C17 P1 C23 103.4(6) . . ? C29 P1 C23 105.5(6) . . ? C17 P1 Re1 115.8(4) . . ? C29 P1 Re1 109.5(4) . . ? C23 P1 Re1 116.9(4) . . ? C30 P2 C31 106.9(6) . . ? C30 P2 C37 100.3(6) . . ? C31 P2 C37 102.1(6) . . ? C30 P2 Re1 108.0(4) . . ? C31 P2 Re1 118.5(4) . . ? C37 P2 Re1 119.1(5) . . ? C1 Re1 N3 156.6(4) . . ? C1 Re1 O2 94.9(4) . . ? N3 Re1 O2 74.9(3) . . ? C1 Re1 N1 95.6(5) . . ? N3 Re1 N1 71.6(4) . . ? O2 Re1 N1 117.2(3) . . ? C1 Re1 P2 88.2(3) . . ? N3 Re1 P2 109.1(3) . . ? O2 Re1 P2 158.3(2) . . ? N1 Re1 P2 83.7(3) . . ? C1 Re1 P1 89.5(4) . . ? N3 Re1 P1 108.6(3) . . ? O2 Re1 P1 78.7(2) . . ? N1 Re1 P1 162.7(3) . . ? P2 Re1 P1 79.90(11) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.576 _refine_diff_density_min -3.074 _refine_diff_density_rms 0.164