####################################################################### # # 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(26NCP)O _database_code_depnum_ccdc_archive 'CCDC 883520' # CHEMICAL DATA _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51 H32 N5 O Re, C H2 Cl2' _chemical_formula_sum 'C52 H34 Cl2 N5 O Re' _chemical_formula_weight 1001.95 _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' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.587(2) _cell_length_b 12.8360(18) _cell_length_c 13.666(2) _cell_angle_alpha 71.295(8) _cell_angle_beta 83.260(10) _cell_angle_gamma 69.705(7) _cell_volume 1961.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7206 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 31.3 _exptl_crystal_description platelet _exptl_crystal_colour violet _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.696 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 3.284 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.753 _exptl_absorpt_correction_T_max 0.906 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoKa _diffrn_radiation_source 'VariMax 50 kV 24mA Rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33834 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.0519 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 28.00 _reflns_number_total 9426 _reflns_number_gt 8692 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.8.2' _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/[?^2^(Fo^2^)+(0.0591P)^2^+7.3797P] 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 9426 _refine_ls_number_parameters 552 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1184 _refine_ls_wR_factor_gt 0.1149 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _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 0.933770(16) 0.334798(17) 0.423624(14) 0.01961(8) Uani 1 1 d . . . Cl1 Cl 1.1905(3) -0.1220(3) 0.8141(2) 0.0899(9) Uani 1 1 d . . . Cl2 Cl 0.9676(3) -0.0438(4) 0.7364(4) 0.1390(17) Uani 1 1 d . . . O1 O 0.8802(3) 0.2261(4) 0.4582(3) 0.0274(8) Uani 1 1 d . . . N1 N 0.8908(3) 0.4125(4) 0.5409(3) 0.0185(8) Uani 1 1 d . . . N2 N 1.0979(3) 0.2689(4) 0.4791(3) 0.0192(8) Uani 1 1 d . . . N3 N 1.0053(4) 0.3376(4) 0.2771(3) 0.0194(8) Uani 1 1 d . . . N4 N 0.6263(4) 0.6032(4) 0.3153(3) 0.0214(9) Uani 1 1 d . . . H4 H 0.5598 0.6520 0.3251 0.026 Uiso 1 1 calc R . . N5 N 0.4262(4) 0.6951(4) 0.2113(3) 0.0227(9) Uani 1 1 d . . . C1 C 0.7909(4) 0.4990(4) 0.5546(4) 0.0197(10) Uani 1 1 d . . . C2 C 0.7933(4) 0.5175(5) 0.6524(4) 0.0225(10) Uani 1 1 d . . . H2 H 0.7365 0.5724 0.6796 0.027 Uiso 1 1 calc R . . C3 C 0.8922(4) 0.4414(4) 0.6987(4) 0.0219(10) Uani 1 1 d . . . H3 H 0.9170 0.4341 0.7644 0.026 Uiso 1 1 calc R . . C4 C 0.9521(4) 0.3746(5) 0.6319(4) 0.0213(10) Uani 1 1 d . . . C5 C 1.0532(4) 0.2839(4) 0.6557(4) 0.0210(10) Uani 1 1 d . . . C6 C 1.1209(4) 0.2324(4) 0.5838(4) 0.0200(10) Uani 1 1 d . . . C7 C 1.2259(5) 0.1397(5) 0.6042(4) 0.0249(11) Uani 1 1 d . . . H7 H 1.2594 0.0969 0.6701 0.030 Uiso 1 1 calc R . . C8 C 1.2696(5) 0.1234(5) 0.5125(4) 0.0248(11) Uani 1 1 d . . . H8 H 1.3401 0.0684 0.5027 0.030 Uiso 1 1 calc R . . C9 C 1.1912(4) 0.2033(4) 0.4339(4) 0.0207(10) Uani 1 1 d . . . C10 C 1.2047(4) 0.2173(5) 0.3286(4) 0.0212(10) Uani 1 1 d . . . C11 C 1.1205(4) 0.2868(4) 0.2554(4) 0.0205(10) Uani 1 1 d . . . C12 C 1.1373(4) 0.3115(5) 0.1476(4) 0.0219(10) Uani 1 1 d . . . H12 H 1.2080 0.2920 0.1128 0.026 Uiso 1 1 calc R . . C13 C 1.0331(5) 0.3686(4) 0.1025(4) 0.0226(10) Uani 1 1 d . . . H13 H 1.0185 0.3930 0.0306 0.027 Uiso 1 1 calc R . . C14 C 0.9507(4) 0.3853(4) 0.1810(4) 0.0212(10) Uani 1 1 d . . . C15 C 0.8337(4) 0.4463(4) 0.1662(4) 0.0197(10) Uani 1 1 d . . . C16 C 0.7734(4) 0.4939(4) 0.2429(4) 0.0207(10) Uani 1 1 d . . . C17 C 0.6598(4) 0.5713(5) 0.2264(4) 0.0215(10) Uani 1 1 d . . . C18 C 0.8071(4) 0.4779(4) 0.3435(4) 0.0216(10) Uani 1 1 d . . . C19 C 0.7122(4) 0.5473(4) 0.3866(4) 0.0213(10) Uani 1 1 d . . . C20 C 0.7007(4) 0.5597(4) 0.4857(4) 0.0210(10) Uani 1 1 d . . . C21 C 1.0912(5) 0.2351(4) 0.7670(4) 0.0227(10) Uani 1 1 d . . . C22 C 1.0214(5) 0.1912(5) 0.8436(4) 0.0291(12) Uani 1 1 d . . . H22 H 0.9518 0.1899 0.8246 0.035 Uiso 1 1 calc R . . C23 C 1.0512(5) 0.1492(5) 0.9471(4) 0.0320(13) Uani 1 1 d . . . H23 H 1.0034 0.1178 0.9983 0.038 Uiso 1 1 calc R . . C24 C 1.1518(6) 0.1536(5) 0.9746(4) 0.0329(13) Uani 1 1 d . . . H24 H 1.1718 0.1269 1.0455 0.040 Uiso 1 1 calc R . . C25 C 1.2234(5) 0.1964(5) 0.9007(5) 0.0322(13) Uani 1 1 d . . . H25 H 1.2928 0.1978 0.9202 0.039 Uiso 1 1 calc R . . C26 C 1.1922(5) 0.2377(5) 0.7963(4) 0.0269(11) Uani 1 1 d . . . H26 H 1.2407 0.2678 0.7450 0.032 Uiso 1 1 calc R . . C27 C 1.3166(4) 0.1514(4) 0.2904(4) 0.0212(10) Uani 1 1 d . . . C28 C 1.3231(5) 0.0722(5) 0.2381(4) 0.0229(10) Uani 1 1 d . . . H28 H 1.2558 0.0612 0.2253 0.028 Uiso 1 1 calc R . . C29 C 1.4277(5) 0.0088(5) 0.2043(4) 0.0271(11) Uani 1 1 d . . . H29 H 1.4310 -0.0453 0.1692 0.033 Uiso 1 1 calc R . . C30 C 1.5252(5) 0.0247(5) 0.2218(4) 0.0259(11) Uani 1 1 d . . . H30 H 1.5961 -0.0179 0.1985 0.031 Uiso 1 1 calc R . . C31 C 1.5200(5) 0.1036(5) 0.2737(4) 0.0282(12) Uani 1 1 d . . . H31 H 1.5874 0.1148 0.2859 0.034 Uiso 1 1 calc R . . C32 C 1.4164(5) 0.1658(5) 0.3079(4) 0.0260(11) Uani 1 1 d . . . H32 H 1.4138 0.2190 0.3437 0.031 Uiso 1 1 calc R . . C33 C 0.7701(4) 0.4655(5) 0.0758(4) 0.0207(10) Uani 1 1 d . . . C34 C 0.6581(5) 0.5490(5) 0.0589(4) 0.0228(10) Uani 1 1 d . . . C35 C 0.5995(5) 0.5630(5) -0.0305(4) 0.0274(11) Uani 1 1 d . . . H35 H 0.5258 0.6188 -0.0441 0.033 Uiso 1 1 calc R . . C36 C 0.6451(5) 0.4999(5) -0.0959(4) 0.0276(12) Uani 1 1 d . . . H36 H 0.6056 0.5153 -0.1568 0.033 Uiso 1 1 calc R . . C37 C 0.7499(5) 0.4119(5) -0.0751(4) 0.0288(12) Uani 1 1 d . . . H37 H 0.7785 0.3630 -0.1183 0.035 Uiso 1 1 calc R . . C38 C 0.8116(5) 0.3960(5) 0.0083(4) 0.0264(11) Uani 1 1 d . . . H38 H 0.8838 0.3372 0.0208 0.032 Uiso 1 1 calc R . . C39 C 0.5912(4) 0.6361(5) 0.5166(4) 0.0228(10) Uani 1 1 d . . . C40 C 0.5317(5) 0.5937(5) 0.6029(4) 0.0252(11) Uani 1 1 d . . . H40 H 0.5625 0.5159 0.6460 0.030 Uiso 1 1 calc R . . C41 C 0.4257(5) 0.6657(5) 0.6269(5) 0.0299(12) Uani 1 1 d . . . H41 H 0.3850 0.6363 0.6863 0.036 Uiso 1 1 calc R . . C42 C 0.3805(5) 0.7785(5) 0.5646(5) 0.0295(12) Uani 1 1 d . . . H42 H 0.3086 0.8265 0.5807 0.035 Uiso 1 1 calc R . . C43 C 0.4404(5) 0.8225(5) 0.4775(4) 0.0283(12) Uani 1 1 d . . . H43 H 0.4096 0.9004 0.4347 0.034 Uiso 1 1 calc R . . C44 C 0.5442(5) 0.7521(5) 0.4541(4) 0.0244(11) Uani 1 1 d . . . H44 H 0.5849 0.7822 0.3950 0.029 Uiso 1 1 calc R . . C45 C 0.6021(4) 0.6072(5) 0.1355(4) 0.0230(10) Uani 1 1 d . . . C46 C 0.4887(5) 0.6977(5) 0.1233(4) 0.0226(10) Uani 1 1 d . . . C47 C 0.4481(5) 0.7851(5) 0.0305(4) 0.0264(11) Uani 1 1 d . . . H47 H 0.4940 0.7897 -0.0302 0.032 Uiso 1 1 calc R . . C48 C 0.3411(5) 0.8637(5) 0.0288(4) 0.0287(12) Uani 1 1 d . . . H48 H 0.3116 0.9224 -0.0337 0.034 Uiso 1 1 calc R . . C49 C 0.2759(5) 0.8576(5) 0.1181(4) 0.0280(12) Uani 1 1 d . . . H49 H 0.2008 0.9101 0.1169 0.034 Uiso 1 1 calc R . . C50 C 0.3219(4) 0.7732(5) 0.2103(4) 0.0237(11) Uani 1 1 d . . . C51 C 0.2631(5) 0.7666(5) 0.3108(4) 0.0300(12) Uani 1 1 d . . . H51A H 0.2962 0.6889 0.3593 0.036 Uiso 1 1 calc R . . H51B H 0.1825 0.7814 0.3019 0.036 Uiso 1 1 calc R . . H51C H 0.2714 0.8252 0.3381 0.036 Uiso 1 1 calc R . . C52 C 1.1027(8) -0.0914(9) 0.7201(8) 0.064(2) Uani 1 1 d . . . H52A H 1.1221 -0.0330 0.6601 0.077 Uiso 1 1 calc R . . H52B H 1.1202 -0.1631 0.6998 0.077 Uiso 1 1 calc R . . _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 0.01945(11) 0.02141(12) 0.01513(11) -0.00678(8) -0.00250(7) -0.00133(8) Cl1 0.0886(19) 0.098(2) 0.0763(17) 0.0076(15) -0.0067(14) -0.0518(17) Cl2 0.0539(16) 0.161(4) 0.225(5) -0.114(4) 0.008(2) -0.015(2) O1 0.0263(19) 0.033(2) 0.0218(19) -0.0106(16) 0.0019(15) -0.0062(17) N1 0.021(2) 0.018(2) 0.0140(19) -0.0084(16) -0.0040(16) 0.0018(16) N2 0.018(2) 0.021(2) 0.0139(19) -0.0047(16) -0.0026(15) 0.0001(16) N3 0.021(2) 0.019(2) 0.0125(19) -0.0024(15) -0.0033(15) -0.0003(16) N4 0.021(2) 0.021(2) 0.018(2) -0.0084(17) -0.0036(16) 0.0017(17) N5 0.021(2) 0.024(2) 0.020(2) -0.0064(17) -0.0014(17) -0.0030(18) C1 0.021(2) 0.021(2) 0.018(2) -0.0084(19) -0.0007(19) -0.005(2) C2 0.024(3) 0.024(3) 0.017(2) -0.009(2) 0.0006(19) -0.002(2) C3 0.025(3) 0.021(2) 0.016(2) -0.0077(19) -0.0025(19) -0.001(2) C4 0.023(2) 0.024(3) 0.015(2) -0.0045(19) -0.0008(19) -0.006(2) C5 0.023(2) 0.022(2) 0.015(2) -0.0045(19) -0.0038(19) -0.004(2) C6 0.020(2) 0.022(2) 0.013(2) -0.0048(19) -0.0037(18) -0.002(2) C7 0.025(3) 0.023(3) 0.019(2) -0.005(2) -0.006(2) 0.002(2) C8 0.023(3) 0.025(3) 0.020(2) -0.006(2) -0.004(2) 0.001(2) C9 0.017(2) 0.021(2) 0.019(2) -0.0072(19) -0.0011(19) 0.0007(19) C10 0.021(2) 0.021(2) 0.021(2) -0.010(2) 0.0006(19) -0.003(2) C11 0.021(2) 0.018(2) 0.020(2) -0.0068(19) -0.0012(19) -0.0022(19) C12 0.022(2) 0.022(2) 0.017(2) -0.0061(19) -0.0002(19) -0.002(2) C13 0.028(3) 0.021(2) 0.014(2) -0.0047(19) -0.0029(19) -0.001(2) C14 0.025(3) 0.020(2) 0.017(2) -0.0059(19) -0.0048(19) -0.004(2) C15 0.025(2) 0.016(2) 0.017(2) -0.0056(18) -0.0027(19) -0.0038(19) C16 0.021(2) 0.022(2) 0.018(2) -0.0069(19) -0.0053(19) -0.004(2) C17 0.026(3) 0.021(2) 0.017(2) -0.0057(19) -0.0005(19) -0.006(2) C18 0.023(2) 0.021(2) 0.017(2) -0.0068(19) -0.0040(19) -0.001(2) C19 0.021(2) 0.020(2) 0.020(2) -0.0062(19) -0.0052(19) -0.001(2) C20 0.022(2) 0.019(2) 0.017(2) -0.0081(19) -0.0014(19) 0.0011(19) C21 0.026(3) 0.020(2) 0.017(2) -0.0079(19) -0.0028(19) 0.001(2) C22 0.029(3) 0.028(3) 0.024(3) -0.007(2) -0.003(2) -0.001(2) C23 0.040(3) 0.025(3) 0.022(3) -0.006(2) -0.001(2) -0.001(2) C24 0.048(4) 0.026(3) 0.018(3) -0.007(2) -0.011(2) 0.001(3) C25 0.037(3) 0.029(3) 0.031(3) -0.011(2) -0.012(2) -0.006(2) C26 0.028(3) 0.024(3) 0.024(3) -0.007(2) -0.003(2) -0.001(2) C27 0.020(2) 0.019(2) 0.018(2) -0.0041(19) -0.0034(19) 0.0018(19) C28 0.024(3) 0.026(3) 0.016(2) -0.006(2) -0.0018(19) -0.005(2) C29 0.030(3) 0.024(3) 0.024(3) -0.012(2) 0.000(2) 0.000(2) C30 0.021(2) 0.027(3) 0.019(2) -0.005(2) 0.000(2) 0.004(2) C31 0.020(3) 0.036(3) 0.027(3) -0.011(2) 0.000(2) -0.005(2) C32 0.023(3) 0.029(3) 0.027(3) -0.013(2) -0.001(2) -0.006(2) C33 0.019(2) 0.027(3) 0.015(2) -0.0064(19) -0.0010(18) -0.006(2) C34 0.026(3) 0.025(3) 0.017(2) -0.007(2) -0.003(2) -0.007(2) C35 0.023(3) 0.034(3) 0.024(3) -0.010(2) -0.002(2) -0.007(2) C36 0.025(3) 0.043(3) 0.016(2) -0.011(2) -0.003(2) -0.009(2) C37 0.032(3) 0.035(3) 0.025(3) -0.016(2) 0.000(2) -0.012(2) C38 0.025(3) 0.028(3) 0.021(3) -0.007(2) -0.003(2) -0.002(2) C39 0.022(2) 0.026(3) 0.021(2) -0.014(2) -0.0020(19) -0.001(2) C40 0.029(3) 0.021(3) 0.026(3) -0.011(2) 0.002(2) -0.005(2) C41 0.027(3) 0.033(3) 0.034(3) -0.016(2) 0.007(2) -0.012(2) C42 0.020(3) 0.033(3) 0.036(3) -0.021(3) -0.005(2) 0.001(2) C43 0.028(3) 0.023(3) 0.027(3) -0.008(2) -0.012(2) 0.004(2) C44 0.028(3) 0.023(3) 0.020(2) -0.009(2) -0.004(2) -0.003(2) C45 0.022(2) 0.026(3) 0.019(2) -0.007(2) -0.0036(19) -0.004(2) C46 0.026(3) 0.023(3) 0.018(2) -0.006(2) -0.003(2) -0.005(2) C47 0.029(3) 0.031(3) 0.017(2) -0.005(2) 0.000(2) -0.009(2) C48 0.028(3) 0.027(3) 0.024(3) -0.004(2) -0.010(2) -0.002(2) C49 0.024(3) 0.025(3) 0.031(3) -0.009(2) -0.006(2) -0.001(2) C50 0.021(2) 0.022(3) 0.028(3) -0.009(2) -0.002(2) -0.005(2) C51 0.028(3) 0.030(3) 0.029(3) -0.008(2) 0.001(2) -0.006(2) C52 0.065(5) 0.072(6) 0.079(6) -0.033(5) 0.000(5) -0.040(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 O1 1.668(4) . ? Re1 C18 2.050(5) . ? Re1 N2 2.074(4) . ? Re1 N1 2.075(4) . ? Re1 N3 2.091(4) . ? Cl1 C52 1.654(9) . ? Cl2 C52 1.610(9) . ? N1 C4 1.398(6) . ? N1 C1 1.399(6) . ? N2 C6 1.387(6) . ? N2 C9 1.396(6) . ? N3 C14 1.407(6) . ? N3 C11 1.408(6) . ? N4 C19 1.376(6) . ? N4 C17 1.379(6) . ? N4 H4 0.8800 . ? N5 C50 1.345(7) . ? N5 C46 1.355(7) . ? C1 C20 1.396(7) . ? C1 C2 1.436(7) . ? C2 C3 1.360(7) . ? C2 H2 0.9500 . ? C3 C4 1.425(7) . ? C3 H3 0.9500 . ? C4 C5 1.381(7) . ? C5 C6 1.399(7) . ? C5 C21 1.512(7) . ? C6 C7 1.422(7) . ? C7 C8 1.357(7) . ? C7 H7 0.9500 . ? C8 C9 1.421(7) . ? C8 H8 0.9500 . ? C9 C10 1.390(7) . ? C10 C11 1.393(7) . ? C10 C27 1.502(7) . ? C11 C12 1.410(7) . ? C12 C13 1.368(7) . ? C12 H12 0.9500 . ? C13 C14 1.416(7) . ? C13 H13 0.9500 . ? C14 C15 1.411(7) . ? C15 C16 1.396(7) . ? C15 C33 1.458(7) . ? C16 C18 1.417(7) . ? C16 C17 1.425(7) . ? C17 C45 1.376(7) . ? C18 C19 1.415(7) . ? C19 C20 1.398(7) . ? C20 C39 1.493(7) . ? C21 C26 1.390(8) . ? C21 C22 1.391(8) . ? C22 C23 1.388(8) . ? C22 H22 0.9500 . ? C23 C24 1.388(9) . ? C23 H23 0.9500 . ? C24 C25 1.381(9) . ? C24 H24 0.9500 . ? C25 C26 1.405(8) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.389(7) . ? C27 C28 1.393(7) . ? C28 C29 1.402(7) . ? C28 H28 0.9500 . ? C29 C30 1.371(8) . ? C29 H29 0.9500 . ? C30 C31 1.392(8) . ? C30 H30 0.9500 . ? C31 C32 1.388(8) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C38 1.419(7) . ? C33 C34 1.435(7) . ? C34 C35 1.431(7) . ? C34 C45 1.454(7) . ? C35 C36 1.343(8) . ? C35 H35 0.9500 . ? C36 C37 1.395(8) . ? C36 H36 0.9500 . ? C37 C38 1.375(7) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.383(8) . ? C39 C44 1.410(7) . ? C40 C41 1.407(8) . ? C40 H40 0.9500 . ? C41 C42 1.377(8) . ? C41 H41 0.9500 . ? C42 C43 1.399(9) . ? C42 H42 0.9500 . ? C43 C44 1.376(8) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.482(7) . ? C46 C47 1.404(7) . ? C47 C48 1.373(8) . ? C47 H47 0.9500 . ? C48 C49 1.385(8) . ? C48 H48 0.9500 . ? C49 C50 1.399(8) . ? C49 H49 0.9500 . ? C50 C51 1.474(8) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Re1 C18 105.2(2) . . ? O1 Re1 N2 108.00(18) . . ? C18 Re1 N2 146.8(2) . . ? O1 Re1 N1 106.16(18) . . ? C18 Re1 N1 84.50(18) . . ? N2 Re1 N1 86.33(16) . . ? O1 Re1 N3 105.63(18) . . ? C18 Re1 N3 84.08(18) . . ? N2 Re1 N3 87.08(16) . . ? N1 Re1 N3 148.04(17) . . ? C4 N1 C1 105.5(4) . . ? C4 N1 Re1 125.0(3) . . ? C1 N1 Re1 129.0(3) . . ? C6 N2 C9 106.3(4) . . ? C6 N2 Re1 122.1(3) . . ? C9 N2 Re1 124.5(3) . . ? C14 N3 C11 105.4(4) . . ? C14 N3 Re1 128.5(3) . . ? C11 N3 Re1 126.1(3) . . ? C19 N4 C17 109.9(4) . . ? C19 N4 H4 125.0 . . ? C17 N4 H4 125.0 . . ? C50 N5 C46 120.5(5) . . ? C20 C1 N1 126.6(4) . . ? C20 C1 C2 123.7(5) . . ? N1 C1 C2 109.7(4) . . ? C3 C2 C1 107.0(4) . . ? C3 C2 H2 126.5 . . ? C1 C2 H2 126.5 . . ? C2 C3 C4 108.2(4) . . ? C2 C3 H3 125.9 . . ? C4 C3 H3 125.9 . . ? C5 C4 N1 125.7(5) . . ? C5 C4 C3 124.8(5) . . ? N1 C4 C3 109.5(4) . . ? C4 C5 C6 124.0(5) . . ? C4 C5 C21 117.9(4) . . ? C6 C5 C21 118.1(4) . . ? N2 C6 C5 124.6(4) . . ? N2 C6 C7 109.1(4) . . ? C5 C6 C7 126.2(5) . . ? C8 C7 C6 107.7(5) . . ? C8 C7 H7 126.1 . . ? C6 C7 H7 126.1 . . ? C7 C8 C9 107.8(5) . . ? C7 C8 H8 126.1 . . ? C9 C8 H8 126.1 . . ? C10 C9 N2 124.7(4) . . ? C10 C9 C8 126.4(5) . . ? N2 C9 C8 108.9(4) . . ? C9 C10 C11 124.5(5) . . ? C9 C10 C27 118.3(4) . . ? C11 C10 C27 117.3(4) . . ? C10 C11 N3 125.6(5) . . ? C10 C11 C12 124.6(5) . . ? N3 C11 C12 109.7(4) . . ? C13 C12 C11 107.4(5) . . ? C13 C12 H12 126.3 . . ? C11 C12 H12 126.3 . . ? C12 C13 C14 108.5(4) . . ? C12 C13 H13 125.8 . . ? C14 C13 H13 125.8 . . ? N3 C14 C15 124.8(5) . . ? N3 C14 C13 108.8(4) . . ? C15 C14 C13 126.3(5) . . ? C16 C15 C14 118.0(4) . . ? C16 C15 C33 116.8(4) . . ? C14 C15 C33 125.1(5) . . ? C15 C16 C18 129.9(5) . . ? C15 C16 C17 121.0(4) . . ? C18 C16 C17 109.1(4) . . ? C45 C17 N4 129.6(5) . . ? C45 C17 C16 124.0(5) . . ? N4 C17 C16 106.3(4) . . ? C19 C18 C16 105.3(4) . . ? C19 C18 Re1 126.4(4) . . ? C16 C18 Re1 123.5(4) . . ? N4 C19 C20 122.7(5) . . ? N4 C19 C18 109.3(4) . . ? C20 C19 C18 128.0(5) . . ? C1 C20 C19 119.5(5) . . ? C1 C20 C39 121.1(4) . . ? C19 C20 C39 119.3(4) . . ? C26 C21 C22 118.5(5) . . ? C26 C21 C5 121.9(5) . . ? C22 C21 C5 119.6(5) . . ? C23 C22 C21 121.5(6) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C24 C23 C22 119.0(6) . . ? C24 C23 H23 120.5 . . ? C22 C23 H23 120.5 . . ? C25 C24 C23 121.1(5) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 119.0(6) . . ? C24 C25 H25 120.5 . . ? C26 C25 H25 120.5 . . ? C21 C26 C25 120.9(6) . . ? C21 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C32 C27 C28 118.3(5) . . ? C32 C27 C10 121.1(5) . . ? C28 C27 C10 120.7(5) . . ? C27 C28 C29 120.8(5) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C30 C29 C28 120.1(5) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C31 119.7(5) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? C32 C31 C30 120.1(5) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C31 C32 C27 121.0(5) . . ? C31 C32 H32 119.5 . . ? C27 C32 H32 119.5 . . ? C38 C33 C34 118.2(5) . . ? C38 C33 C15 121.6(5) . . ? C34 C33 C15 119.9(5) . . ? C35 C34 C33 117.3(5) . . ? C35 C34 C45 121.4(5) . . ? C33 C34 C45 121.0(4) . . ? C36 C35 C34 122.3(5) . . ? C36 C35 H35 118.8 . . ? C34 C35 H35 118.8 . . ? C35 C36 C37 120.6(5) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C38 C37 C36 119.8(5) . . ? C38 C37 H37 120.1 . . ? C36 C37 H37 120.1 . . ? C37 C38 C33 121.6(5) . . ? C37 C38 H38 119.2 . . ? C33 C38 H38 119.2 . . ? C40 C39 C44 119.0(5) . . ? C40 C39 C20 121.2(5) . . ? C44 C39 C20 119.7(5) . . ? C39 C40 C41 120.1(5) . . ? C39 C40 H40 120.0 . . ? C41 C40 H40 120.0 . . ? C42 C41 C40 120.2(5) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C41 C42 C43 120.1(5) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C44 C43 C42 119.6(5) . . ? C44 C43 H43 120.2 . . ? C42 C43 H43 120.2 . . ? C43 C44 C39 120.9(5) . . ? C43 C44 H44 119.5 . . ? C39 C44 H44 119.5 . . ? C17 C45 C34 115.9(5) . . ? C17 C45 C46 119.2(5) . . ? C34 C45 C46 124.9(4) . . ? N5 C46 C47 120.7(5) . . ? N5 C46 C45 114.9(4) . . ? C47 C46 C45 124.3(5) . . ? C48 C47 C46 118.8(5) . . ? C48 C47 H47 120.6 . . ? C46 C47 H47 120.6 . . ? C47 C48 C49 120.1(5) . . ? C47 C48 H48 120.0 . . ? C49 C48 H48 120.0 . . ? C48 C49 C50 119.2(5) . . ? C48 C49 H49 120.4 . . ? C50 C49 H49 120.4 . . ? N5 C50 C49 120.5(5) . . ? N5 C50 C51 116.4(5) . . ? C49 C50 C51 123.1(5) . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? Cl2 C52 Cl1 121.0(6) . . ? Cl2 C52 H52A 107.1 . . ? Cl1 C52 H52A 107.1 . . ? Cl2 C52 H52B 107.1 . . ? Cl1 C52 H52B 107.1 . . ? H52A C52 H52B 106.8 . . ? _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Re1 N1 C4 84.6(4) . . . . ? C18 Re1 N1 C4 -171.1(4) . . . . ? N2 Re1 N1 C4 -23.0(4) . . . . ? N3 Re1 N1 C4 -101.6(5) . . . . ? O1 Re1 N1 C1 -85.3(5) . . . . ? C18 Re1 N1 C1 19.0(4) . . . . ? N2 Re1 N1 C1 167.0(5) . . . . ? N3 Re1 N1 C1 88.5(5) . . . . ? O1 Re1 N2 C6 -68.8(4) . . . . ? C18 Re1 N2 C6 111.2(5) . . . . ? N1 Re1 N2 C6 37.1(4) . . . . ? N3 Re1 N2 C6 -174.2(4) . . . . ? O1 Re1 N2 C9 77.7(4) . . . . ? C18 Re1 N2 C9 -102.3(5) . . . . ? N1 Re1 N2 C9 -176.5(4) . . . . ? N3 Re1 N2 C9 -27.8(4) . . . . ? O1 Re1 N3 C14 79.7(5) . . . . ? C18 Re1 N3 C14 -24.5(4) . . . . ? N2 Re1 N3 C14 -172.5(4) . . . . ? N1 Re1 N3 C14 -94.2(5) . . . . ? O1 Re1 N3 C11 -97.8(4) . . . . ? C18 Re1 N3 C11 158.0(4) . . . . ? N2 Re1 N3 C11 10.1(4) . . . . ? N1 Re1 N3 C11 88.4(5) . . . . ? C4 N1 C1 C20 -177.4(5) . . . . ? Re1 N1 C1 C20 -5.9(8) . . . . ? C4 N1 C1 C2 2.4(6) . . . . ? Re1 N1 C1 C2 173.8(4) . . . . ? C20 C1 C2 C3 178.5(5) . . . . ? N1 C1 C2 C3 -1.3(6) . . . . ? C1 C2 C3 C4 -0.3(6) . . . . ? C1 N1 C4 C5 175.3(5) . . . . ? Re1 N1 C4 C5 3.4(8) . . . . ? C1 N1 C4 C3 -2.6(6) . . . . ? Re1 N1 C4 C3 -174.4(3) . . . . ? C2 C3 C4 C5 -176.1(5) . . . . ? C2 C3 C4 N1 1.8(6) . . . . ? N1 C4 C5 C6 13.9(9) . . . . ? C3 C4 C5 C6 -168.5(5) . . . . ? N1 C4 C5 C21 -164.2(5) . . . . ? C3 C4 C5 C21 13.4(8) . . . . ? C9 N2 C6 C5 173.8(5) . . . . ? Re1 N2 C6 C5 -34.5(7) . . . . ? C9 N2 C6 C7 -3.1(6) . . . . ? Re1 N2 C6 C7 148.5(4) . . . . ? C4 C5 C6 N2 3.0(9) . . . . ? C21 C5 C6 N2 -178.9(5) . . . . ? C4 C5 C6 C7 179.4(5) . . . . ? C21 C5 C6 C7 -2.5(8) . . . . ? N2 C6 C7 C8 3.0(7) . . . . ? C5 C6 C7 C8 -173.9(5) . . . . ? C6 C7 C8 C9 -1.6(7) . . . . ? C6 N2 C9 C10 -176.5(5) . . . . ? Re1 N2 C9 C10 32.7(7) . . . . ? C6 N2 C9 C8 2.1(6) . . . . ? Re1 N2 C9 C8 -148.7(4) . . . . ? C7 C8 C9 C10 178.3(5) . . . . ? C7 C8 C9 N2 -0.3(6) . . . . ? N2 C9 C10 C11 -9.5(9) . . . . ? C8 C9 C10 C11 172.1(5) . . . . ? N2 C9 C10 C27 171.9(5) . . . . ? C8 C9 C10 C27 -6.5(8) . . . . ? C9 C10 C11 N3 -11.1(9) . . . . ? C27 C10 C11 N3 167.6(5) . . . . ? C9 C10 C11 C12 172.6(5) . . . . ? C27 C10 C11 C12 -8.7(8) . . . . ? C14 N3 C11 C10 -171.9(5) . . . . ? Re1 N3 C11 C10 6.0(7) . . . . ? C14 N3 C11 C12 4.9(6) . . . . ? Re1 N3 C11 C12 -177.2(3) . . . . ? C10 C11 C12 C13 172.0(5) . . . . ? N3 C11 C12 C13 -4.8(6) . . . . ? C11 C12 C13 C14 2.8(6) . . . . ? C11 N3 C14 C15 -179.3(5) . . . . ? Re1 N3 C14 C15 2.9(8) . . . . ? C11 N3 C14 C13 -3.1(6) . . . . ? Re1 N3 C14 C13 179.1(3) . . . . ? C12 C13 C14 N3 0.2(6) . . . . ? C12 C13 C14 C15 176.3(5) . . . . ? N3 C14 C15 C16 20.5(8) . . . . ? C13 C14 C15 C16 -155.0(5) . . . . ? N3 C14 C15 C33 -160.5(5) . . . . ? C13 C14 C15 C33 24.0(9) . . . . ? C14 C15 C16 C18 -9.9(9) . . . . ? C33 C15 C16 C18 171.0(5) . . . . ? C14 C15 C16 C17 170.2(5) . . . . ? C33 C15 C16 C17 -8.9(8) . . . . ? C19 N4 C17 C45 -178.8(6) . . . . ? C19 N4 C17 C16 -1.4(6) . . . . ? C15 C16 C17 C45 -1.6(8) . . . . ? C18 C16 C17 C45 178.5(5) . . . . ? C15 C16 C17 N4 -179.1(5) . . . . ? C18 C16 C17 N4 1.0(6) . . . . ? C15 C16 C18 C19 179.9(5) . . . . ? C17 C16 C18 C19 -0.2(6) . . . . ? C15 C16 C18 Re1 -23.5(8) . . . . ? C17 C16 C18 Re1 156.4(4) . . . . ? O1 Re1 C18 C19 79.3(5) . . . . ? N2 Re1 C18 C19 -100.6(5) . . . . ? N1 Re1 C18 C19 -25.9(5) . . . . ? N3 Re1 C18 C19 -176.0(5) . . . . ? O1 Re1 C18 C16 -72.2(5) . . . . ? N2 Re1 C18 C16 107.9(5) . . . . ? N1 Re1 C18 C16 -177.5(5) . . . . ? N3 Re1 C18 C16 32.4(5) . . . . ? C17 N4 C19 C20 -177.6(5) . . . . ? C17 N4 C19 C18 1.4(6) . . . . ? C16 C18 C19 N4 -0.7(6) . . . . ? Re1 C18 C19 N4 -156.3(4) . . . . ? C16 C18 C19 C20 178.2(5) . . . . ? Re1 C18 C19 C20 22.6(8) . . . . ? N1 C1 C20 C19 -8.9(8) . . . . ? C2 C1 C20 C19 171.4(5) . . . . ? N1 C1 C20 C39 170.0(5) . . . . ? C2 C1 C20 C39 -9.7(8) . . . . ? N4 C19 C20 C1 179.1(5) . . . . ? C18 C19 C20 C1 0.3(9) . . . . ? N4 C19 C20 C39 0.2(8) . . . . ? C18 C19 C20 C39 -178.7(5) . . . . ? C4 C5 C21 C26 -119.0(6) . . . . ? C6 C5 C21 C26 62.8(7) . . . . ? C4 C5 C21 C22 57.9(7) . . . . ? C6 C5 C21 C22 -120.3(6) . . . . ? C26 C21 C22 C23 -0.8(8) . . . . ? C5 C21 C22 C23 -177.8(5) . . . . ? C21 C22 C23 C24 1.4(9) . . . . ? C22 C23 C24 C25 -1.6(9) . . . . ? C23 C24 C25 C26 1.1(9) . . . . ? C22 C21 C26 C25 0.3(8) . . . . ? C5 C21 C26 C25 177.2(5) . . . . ? C24 C25 C26 C21 -0.5(9) . . . . ? C9 C10 C27 C32 -58.5(7) . . . . ? C11 C10 C27 C32 122.7(6) . . . . ? C9 C10 C27 C28 120.2(6) . . . . ? C11 C10 C27 C28 -58.6(7) . . . . ? C32 C27 C28 C29 0.1(8) . . . . ? C10 C27 C28 C29 -178.7(5) . . . . ? C27 C28 C29 C30 -0.4(8) . . . . ? C28 C29 C30 C31 0.4(8) . . . . ? C29 C30 C31 C32 0.1(9) . . . . ? C30 C31 C32 C27 -0.5(9) . . . . ? C28 C27 C32 C31 0.4(8) . . . . ? C10 C27 C32 C31 179.1(5) . . . . ? C16 C15 C33 C38 -161.7(5) . . . . ? C14 C15 C33 C38 19.2(8) . . . . ? C16 C15 C33 C34 12.4(7) . . . . ? C14 C15 C33 C34 -166.6(5) . . . . ? C38 C33 C34 C35 -4.9(8) . . . . ? C15 C33 C34 C35 -179.3(5) . . . . ? C38 C33 C34 C45 168.3(5) . . . . ? C15 C33 C34 C45 -6.1(8) . . . . ? C33 C34 C35 C36 1.2(8) . . . . ? C45 C34 C35 C36 -172.0(6) . . . . ? C34 C35 C36 C37 4.2(9) . . . . ? C35 C36 C37 C38 -5.6(9) . . . . ? C36 C37 C38 C33 1.6(9) . . . . ? C34 C33 C38 C37 3.6(8) . . . . ? C15 C33 C38 C37 177.9(5) . . . . ? C1 C20 C39 C40 -55.3(8) . . . . ? C19 C20 C39 C40 123.6(6) . . . . ? C1 C20 C39 C44 128.0(6) . . . . ? C19 C20 C39 C44 -53.1(7) . . . . ? C44 C39 C40 C41 0.4(8) . . . . ? C20 C39 C40 C41 -176.3(5) . . . . ? C39 C40 C41 C42 0.2(9) . . . . ? C40 C41 C42 C43 -0.6(9) . . . . ? C41 C42 C43 C44 0.4(8) . . . . ? C42 C43 C44 C39 0.1(8) . . . . ? C40 C39 C44 C43 -0.5(8) . . . . ? C20 C39 C44 C43 176.2(5) . . . . ? N4 C17 C45 C34 -174.9(5) . . . . ? C16 C17 C45 C34 8.1(8) . . . . ? N4 C17 C45 C46 3.5(9) . . . . ? C16 C17 C45 C46 -173.5(5) . . . . ? C35 C34 C45 C17 168.8(5) . . . . ? C33 C34 C45 C17 -4.1(8) . . . . ? C35 C34 C45 C46 -9.5(9) . . . . ? C33 C34 C45 C46 177.6(5) . . . . ? C50 N5 C46 C47 3.0(8) . . . . ? C50 N5 C46 C45 179.7(5) . . . . ? C17 C45 C46 N5 -33.4(7) . . . . ? C34 C45 C46 N5 144.9(5) . . . . ? C17 C45 C46 C47 143.3(6) . . . . ? C34 C45 C46 C47 -38.5(9) . . . . ? N5 C46 C47 C48 -4.0(8) . . . . ? C45 C46 C47 C48 179.6(5) . . . . ? C46 C47 C48 C49 1.4(9) . . . . ? C47 C48 C49 C50 2.1(9) . . . . ? C46 N5 C50 C49 0.6(8) . . . . ? C46 N5 C50 C51 -177.1(5) . . . . ? C48 C49 C50 N5 -3.2(8) . . . . ? C48 C49 C50 C51 174.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.889 _refine_diff_density_min -1.802 _refine_diff_density_rms 0.175 data_Re(2,21-Me2NCP)(CO)3 _database_code_depnum_ccdc_archive 'CCDC 883521' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C49 H33 N4 O3 Re' _chemical_formula_sum 'C49 H33 N4 O3 Re' _chemical_formula_weight 912.00 _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' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' _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 11.888(6) _cell_length_b 26.464(13) _cell_length_c 12.738(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.467(5) _cell_angle_gamma 90.00 _cell_volume 3862(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 10817 _cell_measurement_theta_min 1.5390 _cell_measurement_theta_max 30.4851 _exptl_crystal_description block _exptl_crystal_colour violet _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1816 _exptl_absorpt_coefficient_mu 3.196 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5674 _exptl_absorpt_correction_T_max 0.8565 _exptl_absorpt_process_details "REQAB''(REQAB; Jacobson, 1998)" _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.710747 _diffrn_radiation_type MoKa _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_radiation_detector CCD _diffrn_measurement_device_type ? _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33609 _diffrn_reflns_av_R_equivalents 0.1315 _diffrn_reflns_av_sigmaI/netI 0.0928 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8624 _reflns_number_gt 7736 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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/[?^2^(Fo^2^)+(0.0546P)^2^+33.4676P] 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 8624 _refine_ls_number_parameters 516 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0825 _refine_ls_R_factor_gt 0.0732 _refine_ls_wR_factor_ref 0.1689 _refine_ls_wR_factor_gt 0.1606 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.121 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _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 0.4377(6) 0.8955(3) 0.3120(6) 0.0384(16) Uani 1 1 d . . . C2 C 0.5193(7) 0.8568(3) 0.3483(7) 0.0414(17) Uani 1 1 d . . . H1 H 0.5526 0.8482 0.4225 0.050 Uiso 1 1 calc R . . N1 N 0.5435(6) 0.8340(3) 0.2637(6) 0.0466(16) Uani 1 1 d . . . C3 C 0.4782(6) 0.8582(3) 0.1685(7) 0.0407(17) Uani 1 1 d . . . C4 C 0.4619(7) 0.8360(3) 0.0642(7) 0.0416(18) Uani 1 1 d . . . C5 C 0.3542(7) 0.8370(3) -0.0162(7) 0.0399(17) Uani 1 1 d . . . C6 C 0.3428(7) 0.8200(3) -0.1258(6) 0.0442(18) Uani 1 1 d . . . H2 H 0.4028 0.8053 -0.1524 0.053 Uiso 1 1 calc R . . C7 C 0.2322(7) 0.8285(3) -0.1838(7) 0.0430(17) Uani 1 1 d . . . H3 H 0.1990 0.8209 -0.2586 0.052 Uiso 1 1 calc R . . C8 C 0.1735(6) 0.8515(3) -0.1096(6) 0.0349(15) Uani 1 1 d . . . C9 C 0.0572(7) 0.8681(3) -0.1465(7) 0.0428(17) Uani 1 1 d . . . C10 C -0.0005(6) 0.8945(3) -0.0820(6) 0.0402(16) Uani 1 1 d . . . C11 C -0.1085(7) 0.9223(4) -0.1210(7) 0.0467(19) Uani 1 1 d . . . H4 H -0.1532 0.9249 -0.1947 0.056 Uiso 1 1 calc R . . C12 C -0.1348(7) 0.9441(4) -0.0336(7) 0.049(2) Uani 1 1 d . . . H5 H -0.2012 0.9643 -0.0343 0.059 Uiso 1 1 calc R . . C13 C -0.0419(7) 0.9305(3) 0.0597(6) 0.0400(16) Uani 1 1 d . . . C14 C -0.0283(6) 0.9466(3) 0.1668(6) 0.0400(17) Uani 1 1 d . . . C15 C 0.0786(6) 0.9443(3) 0.2506(7) 0.0390(16) Uani 1 1 d . . . C16 C 0.0930(7) 0.9704(4) 0.3518(7) 0.0459(19) Uani 1 1 d . . . H6 H 0.0351 0.9896 0.3728 0.055 Uiso 1 1 calc R . . C17 C 0.2033(7) 0.9626(4) 0.4118(7) 0.049(2) Uani 1 1 d . . . H7 H 0.2375 0.9750 0.4833 0.058 Uiso 1 1 calc R . . C18 C 0.2598(6) 0.9319(3) 0.3469(6) 0.0383(16) Uani 1 1 d . . . C19 C 0.3764(6) 0.9171(3) 0.3837(6) 0.0388(16) Uani 1 1 d . . . C20 C 0.4180(6) 0.8984(3) 0.1989(6) 0.0374(16) Uani 1 1 d . . . C21 C 0.3650(7) 0.9435(3) 0.1288(7) 0.0436(18) Uani 1 1 d . . . H8 H 0.3774 0.9742 0.1736 0.065 Uiso 1 1 calc R . . H9 H 0.2811 0.9380 0.0982 0.065 Uiso 1 1 calc R . . H10 H 0.4025 0.9474 0.0694 0.065 Uiso 1 1 calc R . . C22 C 0.6093(10) 0.7867(4) 0.2745(9) 0.066(3) Uani 1 1 d . . . H11 H 0.6292 0.7755 0.3506 0.099 Uiso 1 1 calc R . . H12 H 0.6811 0.7921 0.2521 0.099 Uiso 1 1 calc R . . H13 H 0.5617 0.7608 0.2282 0.099 Uiso 1 1 calc R . . N2 N 0.2475(6) 0.8552(3) -0.0065(6) 0.0406(15) Uani 1 1 d . . . N3 N 0.0380(5) 0.9001(3) 0.0283(5) 0.0350(13) Uani 1 1 d . . . N4 N 0.1806(5) 0.9208(3) 0.2461(5) 0.0378(14) Uani 1 1 d . . . Re1 Re 0.15190(2) 0.847718(12) 0.13503(2) 0.03761(12) Uani 1 1 d . . . C23 C 0.0494(7) 0.8328(3) 0.2235(7) 0.0440(18) Uani 1 1 d . . . O1 O -0.0108(6) 0.8206(3) 0.2750(6) 0.0624(19) Uani 1 1 d . . . C24 C 0.2656(7) 0.8048(3) 0.2321(7) 0.0446(18) Uani 1 1 d . . . O2 O 0.3305(6) 0.7786(3) 0.2875(6) 0.0627(19) Uani 1 1 d . . . C25 C 0.0967(7) 0.7877(4) 0.0578(7) 0.051(2) Uani 1 1 d . . . O3 O 0.0595(6) 0.7501(3) 0.0161(6) 0.0633(18) Uani 1 1 d . . . C26 C 0.5643(6) 0.8112(4) 0.0385(6) 0.0434(18) Uani 1 1 d . . . C27 C 0.6680(7) 0.8369(4) 0.0509(8) 0.051(2) Uani 1 1 d . . . H14 H 0.6722 0.8714 0.0724 0.061 Uiso 1 1 calc R . . C28 C 0.7652(8) 0.8145(6) 0.0334(10) 0.074(3) Uani 1 1 d . . . H15 H 0.8345 0.8335 0.0404 0.088 Uiso 1 1 calc R . . C29 C 0.7621(9) 0.7647(6) 0.0059(10) 0.077(4) Uani 1 1 d . . . H16 H 0.8299 0.7488 -0.0048 0.093 Uiso 1 1 calc R . . C30 C 0.6613(9) 0.7375(5) -0.0066(9) 0.070(3) Uani 1 1 d . . . H17 H 0.6594 0.7027 -0.0253 0.084 Uiso 1 1 calc R . . C31 C 0.5620(8) 0.7607(4) 0.0082(8) 0.057(2) Uani 1 1 d . . . H18 H 0.4918 0.7419 -0.0025 0.068 Uiso 1 1 calc R . . C32 C -0.0064(7) 0.8620(4) -0.2642(7) 0.0457(18) Uani 1 1 d . . . C33 C 0.0292(9) 0.8867(4) -0.3466(8) 0.057(2) Uani 1 1 d . . . H19 H 0.0971 0.9073 -0.3279 0.068 Uiso 1 1 calc R . . C34 C -0.0325(11) 0.8820(5) -0.4556(8) 0.067(3) Uani 1 1 d . . . H20 H -0.0074 0.8990 -0.5110 0.080 Uiso 1 1 calc R . . C35 C -0.1309(11) 0.8520(5) -0.4811(9) 0.072(3) Uani 1 1 d . . . H21 H -0.1731 0.8482 -0.5553 0.087 Uiso 1 1 calc R . . C36 C -0.1693(10) 0.8276(5) -0.4030(10) 0.069(3) Uani 1 1 d . . . H22 H -0.2377 0.8073 -0.4226 0.082 Uiso 1 1 calc R . . C37 C -0.1064(9) 0.8327(4) -0.2929(8) 0.060(2) Uani 1 1 d . . . H23 H -0.1327 0.8158 -0.2380 0.072 Uiso 1 1 calc R . . C38 C -0.1329(6) 0.9658(3) 0.1966(7) 0.0402(17) Uani 1 1 d . . . C39 C -0.1896(8) 1.0106(3) 0.1554(8) 0.050(2) Uani 1 1 d . . . H24 H -0.1604 1.0305 0.1063 0.060 Uiso 1 1 calc R . . C40 C -0.2882(9) 1.0266(4) 0.1852(9) 0.058(2) Uani 1 1 d . . . H25 H -0.3250 1.0575 0.1572 0.070 Uiso 1 1 calc R . . C41 C -0.3328(8) 0.9982(4) 0.2549(9) 0.058(2) Uani 1 1 d . . . H26 H -0.3989 1.0095 0.2769 0.070 Uiso 1 1 calc R . . C42 C -0.2791(8) 0.9521(4) 0.2930(9) 0.060(3) Uani 1 1 d . . . H27 H -0.3112 0.9312 0.3382 0.072 Uiso 1 1 calc R . . C43 C -0.1807(7) 0.9374(4) 0.2652(7) 0.050(2) Uani 1 1 d . . . H28 H -0.1439 0.9066 0.2939 0.061 Uiso 1 1 calc R . . C44 C 0.4369(6) 0.9179(3) 0.4998(6) 0.0401(17) Uani 1 1 d . . . C45 C 0.3931(8) 0.8939(4) 0.5761(8) 0.055(2) Uani 1 1 d . . . H29 H 0.3167 0.8800 0.5553 0.066 Uiso 1 1 calc R . . C46 C 0.4604(10) 0.8896(5) 0.6847(9) 0.074(3) Uani 1 1 d . . . H30 H 0.4306 0.8717 0.7362 0.089 Uiso 1 1 calc R . . C47 C 0.5693(10) 0.9112(5) 0.7162(8) 0.067(3) Uani 1 1 d . . . H31 H 0.6138 0.9087 0.7900 0.080 Uiso 1 1 calc R . . C48 C 0.6143(9) 0.9361(4) 0.6431(8) 0.058(2) Uani 1 1 d . . . H32 H 0.6893 0.9513 0.6654 0.070 Uiso 1 1 calc R . . C49 C 0.5481(7) 0.9387(4) 0.5341(7) 0.049(2) Uani 1 1 d . . . H33 H 0.5800 0.9552 0.4824 0.059 Uiso 1 1 calc R . . _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 0.029(3) 0.051(4) 0.034(4) 0.003(3) 0.006(3) 0.001(3) C2 0.030(3) 0.056(5) 0.036(4) 0.000(3) 0.004(3) 0.007(3) N1 0.035(3) 0.065(5) 0.041(4) -0.002(3) 0.012(3) 0.007(3) C3 0.027(3) 0.054(5) 0.041(4) -0.003(3) 0.008(3) 0.001(3) C4 0.029(3) 0.058(5) 0.038(4) -0.002(4) 0.010(3) 0.005(3) C5 0.030(3) 0.053(5) 0.038(4) 0.000(3) 0.011(3) -0.003(3) C6 0.044(4) 0.057(5) 0.037(4) 0.001(4) 0.019(4) 0.005(4) C7 0.042(4) 0.056(5) 0.031(4) 0.000(3) 0.010(3) -0.003(4) C8 0.029(3) 0.045(4) 0.030(3) 0.001(3) 0.006(3) -0.005(3) C9 0.035(4) 0.054(5) 0.040(4) 0.003(4) 0.010(3) -0.001(3) C10 0.031(3) 0.052(4) 0.034(4) 0.001(3) 0.003(3) -0.001(3) C11 0.036(4) 0.062(5) 0.036(4) 0.000(4) -0.001(3) 0.002(4) C12 0.039(4) 0.062(5) 0.045(5) 0.003(4) 0.009(4) 0.009(4) C13 0.034(4) 0.047(4) 0.038(4) 0.003(3) 0.007(3) 0.005(3) C14 0.030(3) 0.055(5) 0.036(4) -0.002(3) 0.009(3) 0.001(3) C15 0.031(3) 0.045(4) 0.041(4) -0.004(3) 0.010(3) 0.003(3) C16 0.031(4) 0.061(5) 0.044(4) -0.010(4) 0.008(3) 0.007(3) C17 0.033(4) 0.071(6) 0.042(4) -0.012(4) 0.010(3) 0.000(4) C18 0.027(3) 0.046(4) 0.040(4) -0.009(3) 0.006(3) -0.002(3) C19 0.028(3) 0.049(4) 0.036(4) 0.001(3) 0.003(3) 0.003(3) C20 0.029(3) 0.050(4) 0.032(4) 0.001(3) 0.006(3) 0.005(3) C21 0.044(4) 0.048(4) 0.039(4) 0.001(3) 0.011(3) 0.003(3) C22 0.070(6) 0.074(7) 0.055(6) 0.006(5) 0.019(5) 0.020(6) N2 0.034(3) 0.052(4) 0.039(3) 0.004(3) 0.016(3) 0.005(3) N3 0.026(3) 0.047(4) 0.030(3) 0.004(3) 0.003(2) 0.010(2) N4 0.028(3) 0.047(4) 0.038(3) -0.004(3) 0.009(3) 0.001(3) Re1 0.02777(16) 0.0507(2) 0.03381(18) 0.00284(13) 0.00730(12) 0.00113(12) C23 0.032(4) 0.049(4) 0.043(4) -0.004(4) -0.004(3) 0.002(3) O1 0.049(4) 0.092(5) 0.056(4) 0.019(4) 0.032(3) 0.008(4) C24 0.038(4) 0.053(5) 0.046(4) -0.007(4) 0.016(4) -0.004(4) O2 0.046(3) 0.075(5) 0.061(4) 0.034(4) 0.003(3) 0.016(3) C25 0.032(4) 0.078(6) 0.040(4) 0.013(4) 0.008(3) 0.003(4) O3 0.052(4) 0.066(4) 0.070(5) -0.022(4) 0.012(3) -0.019(3) C26 0.026(3) 0.070(6) 0.035(4) -0.007(4) 0.009(3) 0.001(3) C27 0.036(4) 0.065(6) 0.053(5) -0.004(4) 0.016(4) -0.005(4) C28 0.034(4) 0.119(11) 0.073(7) -0.005(7) 0.022(5) -0.004(6) C29 0.040(5) 0.116(10) 0.076(7) -0.025(7) 0.016(5) 0.018(6) C30 0.054(6) 0.078(7) 0.068(7) -0.032(6) -0.001(5) 0.020(5) C31 0.041(4) 0.066(6) 0.061(6) -0.021(5) 0.010(4) -0.005(4) C32 0.041(4) 0.056(5) 0.038(4) -0.002(4) 0.007(3) 0.005(4) C33 0.054(5) 0.072(6) 0.044(5) 0.003(4) 0.012(4) -0.018(5) C34 0.079(7) 0.084(8) 0.034(5) 0.012(5) 0.011(5) 0.007(6) C35 0.077(8) 0.091(8) 0.039(5) 0.010(5) -0.001(5) 0.012(6) C36 0.058(6) 0.072(7) 0.070(7) -0.007(6) 0.005(5) -0.019(5) C37 0.056(5) 0.073(6) 0.048(5) -0.002(5) 0.012(4) -0.021(5) C38 0.028(3) 0.050(4) 0.043(4) -0.004(3) 0.010(3) -0.002(3) C39 0.047(5) 0.049(5) 0.056(5) 0.002(4) 0.017(4) 0.005(4) C40 0.052(5) 0.051(5) 0.073(6) -0.002(5) 0.018(5) 0.016(4) C41 0.036(4) 0.069(6) 0.074(7) -0.016(5) 0.021(4) 0.000(4) C42 0.053(5) 0.070(6) 0.067(6) 0.001(5) 0.036(5) -0.008(5) C43 0.040(4) 0.062(5) 0.051(5) 0.008(4) 0.013(4) 0.006(4) C44 0.025(3) 0.062(5) 0.032(4) -0.004(3) 0.005(3) -0.004(3) C45 0.046(5) 0.076(6) 0.047(5) 0.002(5) 0.017(4) -0.011(4) C46 0.066(7) 0.110(10) 0.052(6) 0.022(6) 0.026(5) 0.000(6) C47 0.068(6) 0.087(8) 0.040(5) 0.002(5) 0.006(5) 0.016(6) C48 0.047(5) 0.076(7) 0.042(5) 0.001(5) -0.004(4) -0.001(5) C49 0.037(4) 0.063(5) 0.044(5) -0.004(4) 0.006(4) -0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; _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 C20 1.399(10) . ? C1 C2 1.401(11) . ? C1 C19 1.430(10) . ? C2 N1 1.332(10) . ? C2 H1 0.9500 . ? N1 C3 1.407(11) . ? N1 C22 1.464(12) . ? C3 C20 1.393(11) . ? C3 C4 1.418(11) . ? C4 C5 1.411(11) . ? C4 C26 1.493(10) . ? C5 N2 1.393(10) . ? C5 C6 1.439(11) . ? C6 C7 1.345(11) . ? C6 H2 0.9500 . ? C7 C8 1.451(11) . ? C7 H3 0.9500 . ? C8 N2 1.375(10) . ? C8 C9 1.408(11) . ? C9 C10 1.390(11) . ? C9 C32 1.497(12) . ? C10 N3 1.365(10) . ? C10 C11 1.448(11) . ? C11 C12 1.362(12) . ? C11 H4 0.9500 . ? C12 C13 1.436(11) . ? C12 H5 0.9500 . ? C13 N3 1.383(9) . ? C13 C14 1.396(11) . ? C14 C15 1.427(11) . ? C14 C38 1.483(10) . ? C15 N4 1.377(9) . ? C15 C16 1.431(11) . ? C16 C17 1.346(11) . ? C16 H6 0.9500 . ? C17 C18 1.446(11) . ? C17 H7 0.9500 . ? C18 C19 1.395(10) . ? C18 N4 1.406(10) . ? C19 C44 1.462(10) . ? C20 C21 1.524(11) . ? C21 H8 0.9800 . ? C21 H9 0.9800 . ? C21 H10 0.9800 . ? C22 H11 0.9800 . ? C22 H12 0.9800 . ? C22 H13 0.9800 . ? N2 Re1 2.382(6) . ? N3 Re1 2.150(6) . ? N4 Re1 2.368(7) . ? Re1 C25 1.891(11) . ? Re1 C23 1.909(9) . ? Re1 C24 1.937(9) . ? C23 O1 1.139(10) . ? C24 O2 1.135(10) . ? C25 O3 1.160(12) . ? C26 C27 1.380(11) . ? C26 C31 1.391(13) . ? C27 C28 1.369(13) . ? C27 H14 0.9500 . ? C28 C29 1.360(18) . ? C28 H15 0.9500 . ? C29 C30 1.371(17) . ? C29 H16 0.9500 . ? C30 C31 1.387(13) . ? C30 H17 0.9500 . ? C31 H18 0.9500 . ? C32 C37 1.384(13) . ? C32 C33 1.395(12) . ? C33 C34 1.392(13) . ? C33 H19 0.9500 . ? C34 C35 1.379(17) . ? C34 H20 0.9500 . ? C35 C36 1.363(16) . ? C35 H21 0.9500 . ? C36 C37 1.409(15) . ? C36 H22 0.9500 . ? C37 H23 0.9500 . ? C38 C43 1.386(12) . ? C38 C39 1.395(12) . ? C39 C40 1.392(12) . ? C39 H24 0.9500 . ? C40 C41 1.374(14) . ? C40 H25 0.9500 . ? C41 C42 1.400(15) . ? C41 H26 0.9500 . ? C42 C43 1.366(12) . ? C42 H27 0.9500 . ? C43 H28 0.9500 . ? C44 C45 1.376(11) . ? C44 C49 1.390(11) . ? C45 C46 1.406(14) . ? C45 H29 0.9500 . ? C46 C47 1.374(16) . ? C46 H30 0.9500 . ? C47 C48 1.362(15) . ? C47 H31 0.9500 . ? C48 C49 1.403(12) . ? C48 H32 0.9500 . ? C49 H33 0.9500 . ? _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 C20 C1 C2 106.9(7) . . ? C20 C1 C19 131.4(7) . . ? C2 C1 C19 120.5(7) . . ? N1 C2 C1 110.1(7) . . ? N1 C2 H1 124.9 . . ? C1 C2 H1 124.9 . . ? C2 N1 C3 107.6(7) . . ? C2 N1 C22 122.4(8) . . ? C3 N1 C22 129.0(8) . . ? C20 C3 N1 108.3(7) . . ? C20 C3 C4 128.7(7) . . ? N1 C3 C4 121.7(7) . . ? C5 C4 C3 122.9(7) . . ? C5 C4 C26 119.0(7) . . ? C3 C4 C26 118.1(7) . . ? N2 C5 C4 127.9(7) . . ? N2 C5 C6 110.0(7) . . ? C4 C5 C6 122.1(7) . . ? C7 C6 C5 107.8(7) . . ? C7 C6 H2 126.1 . . ? C5 C6 H2 126.1 . . ? C6 C7 C8 106.3(7) . . ? C6 C7 H3 126.8 . . ? C8 C7 H3 126.8 . . ? N2 C8 C9 128.2(7) . . ? N2 C8 C7 110.9(6) . . ? C9 C8 C7 120.9(7) . . ? C10 C9 C8 123.7(7) . . ? C10 C9 C32 116.7(7) . . ? C8 C9 C32 119.3(7) . . ? N3 C10 C9 125.5(7) . . ? N3 C10 C11 108.7(7) . . ? C9 C10 C11 125.7(7) . . ? C12 C11 C10 108.1(7) . . ? C12 C11 H4 125.9 . . ? C10 C11 H4 125.9 . . ? C11 C12 C13 106.1(7) . . ? C11 C12 H5 127.0 . . ? C13 C12 H5 127.0 . . ? N3 C13 C14 123.3(7) . . ? N3 C13 C12 110.0(7) . . ? C14 C13 C12 126.6(7) . . ? C13 C14 C15 124.5(7) . . ? C13 C14 C38 117.9(7) . . ? C15 C14 C38 117.6(7) . . ? N4 C15 C14 127.3(7) . . ? N4 C15 C16 111.1(7) . . ? C14 C15 C16 121.5(7) . . ? C17 C16 C15 107.6(7) . . ? C17 C16 H6 126.2 . . ? C15 C16 H6 126.2 . . ? C16 C17 C18 107.0(7) . . ? C16 C17 H7 126.5 . . ? C18 C17 H7 126.5 . . ? C19 C18 N4 127.7(7) . . ? C19 C18 C17 122.5(7) . . ? N4 C18 C17 109.8(6) . . ? C18 C19 C1 121.9(7) . . ? C18 C19 C44 120.8(7) . . ? C1 C19 C44 117.0(6) . . ? C3 C20 C1 106.7(7) . . ? C3 C20 C21 126.7(7) . . ? C1 C20 C21 125.1(7) . . ? C20 C21 H8 109.5 . . ? C20 C21 H9 109.5 . . ? H8 C21 H9 109.5 . . ? C20 C21 H10 109.5 . . ? H8 C21 H10 109.5 . . ? H9 C21 H10 109.5 . . ? N1 C22 H11 109.5 . . ? N1 C22 H12 109.5 . . ? H11 C22 H12 109.5 . . ? N1 C22 H13 109.5 . . ? H11 C22 H13 109.5 . . ? H12 C22 H13 109.5 . . ? C8 N2 C5 104.8(6) . . ? C8 N2 Re1 113.8(5) . . ? C5 N2 Re1 131.9(5) . . ? C10 N3 C13 107.1(6) . . ? C10 N3 Re1 124.2(5) . . ? C13 N3 Re1 123.9(5) . . ? C15 N4 C18 104.5(6) . . ? C15 N4 Re1 113.9(5) . . ? C18 N4 Re1 132.2(5) . . ? C25 Re1 C23 86.9(4) . . ? C25 Re1 C24 85.8(4) . . ? C23 Re1 C24 87.0(3) . . ? C25 Re1 N3 98.0(3) . . ? C23 Re1 N3 96.5(3) . . ? C24 Re1 N3 174.9(3) . . ? C25 Re1 N4 166.4(3) . . ? C23 Re1 N4 80.2(3) . . ? C24 Re1 N4 97.6(3) . . ? N3 Re1 N4 79.4(2) . . ? C25 Re1 N2 81.1(3) . . ? C23 Re1 N2 166.6(3) . . ? C24 Re1 N2 98.0(3) . . ? N3 Re1 N2 79.3(2) . . ? N4 Re1 N2 111.3(2) . . ? O1 C23 Re1 175.6(8) . . ? O2 C24 Re1 178.1(8) . . ? O3 C25 Re1 175.3(8) . . ? C27 C26 C31 117.2(8) . . ? C27 C26 C4 120.9(8) . . ? C31 C26 C4 121.8(8) . . ? C28 C27 C26 122.3(10) . . ? C28 C27 H14 118.8 . . ? C26 C27 H14 118.8 . . ? C29 C28 C27 119.8(10) . . ? C29 C28 H15 120.1 . . ? C27 C28 H15 120.1 . . ? C28 C29 C30 120.0(9) . . ? C28 C29 H16 120.0 . . ? C30 C29 H16 120.0 . . ? C29 C30 C31 120.1(10) . . ? C29 C30 H17 119.9 . . ? C31 C30 H17 119.9 . . ? C30 C31 C26 120.6(9) . . ? C30 C31 H18 119.7 . . ? C26 C31 H18 119.7 . . ? C37 C32 C33 118.4(8) . . ? C37 C32 C9 119.6(8) . . ? C33 C32 C9 121.9(8) . . ? C34 C33 C32 121.6(9) . . ? C34 C33 H19 119.2 . . ? C32 C33 H19 119.2 . . ? C35 C34 C33 118.3(10) . . ? C35 C34 H20 120.9 . . ? C33 C34 H20 120.9 . . ? C36 C35 C34 122.0(10) . . ? C36 C35 H21 119.0 . . ? C34 C35 H21 119.0 . . ? C35 C36 C37 119.3(10) . . ? C35 C36 H22 120.4 . . ? C37 C36 H22 120.4 . . ? C32 C37 C36 120.5(9) . . ? C32 C37 H23 119.8 . . ? C36 C37 H23 119.8 . . ? C43 C38 C39 117.4(7) . . ? C43 C38 C14 119.3(8) . . ? C39 C38 C14 123.3(7) . . ? C40 C39 C38 120.9(9) . . ? C40 C39 H24 119.5 . . ? C38 C39 H24 119.5 . . ? C41 C40 C39 120.5(9) . . ? C41 C40 H25 119.8 . . ? C39 C40 H25 119.8 . . ? C40 C41 C42 118.8(8) . . ? C40 C41 H26 120.6 . . ? C42 C41 H26 120.6 . . ? C43 C42 C41 120.1(9) . . ? C43 C42 H27 119.9 . . ? C41 C42 H27 119.9 . . ? C42 C43 C38 122.1(9) . . ? C42 C43 H28 118.9 . . ? C38 C43 H28 118.9 . . ? C45 C44 C49 117.9(8) . . ? C45 C44 C19 122.1(7) . . ? C49 C44 C19 119.6(7) . . ? C44 C45 C46 120.7(9) . . ? C44 C45 H29 119.7 . . ? C46 C45 H29 119.7 . . ? C47 C46 C45 119.9(9) . . ? C47 C46 H30 120.1 . . ? C45 C46 H30 120.1 . . ? C48 C47 C46 120.9(10) . . ? C48 C47 H31 119.6 . . ? C46 C47 H31 119.6 . . ? C47 C48 C49 118.8(9) . . ? C47 C48 H32 120.6 . . ? C49 C48 H32 120.6 . . ? C44 C49 C48 121.8(9) . . ? C44 C49 H33 119.1 . . ? C48 C49 H33 119.1 . . ? _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C20 C1 C2 N1 -4.4(10) . . . . ? C19 C1 C2 N1 164.4(7) . . . . ? C1 C2 N1 C3 0.8(10) . . . . ? C1 C2 N1 C22 -168.8(8) . . . . ? C2 N1 C3 C20 3.1(9) . . . . ? C22 N1 C3 C20 171.8(9) . . . . ? C2 N1 C3 C4 -164.7(8) . . . . ? C22 N1 C3 C4 4.1(14) . . . . ? C20 C3 C4 C5 -26.7(14) . . . . ? N1 C3 C4 C5 138.4(8) . . . . ? C20 C3 C4 C26 152.5(8) . . . . ? N1 C3 C4 C26 -42.5(12) . . . . ? C3 C4 C5 N2 -5.2(14) . . . . ? C26 C4 C5 N2 175.6(8) . . . . ? C3 C4 C5 C6 172.1(8) . . . . ? C26 C4 C5 C6 -7.1(13) . . . . ? N2 C5 C6 C7 1.4(10) . . . . ? C4 C5 C6 C7 -176.3(8) . . . . ? C5 C6 C7 C8 0.4(10) . . . . ? C6 C7 C8 N2 -2.1(10) . . . . ? C6 C7 C8 C9 176.0(8) . . . . ? N2 C8 C9 C10 3.7(14) . . . . ? C7 C8 C9 C10 -174.0(8) . . . . ? N2 C8 C9 C32 177.6(8) . . . . ? C7 C8 C9 C32 -0.1(12) . . . . ? C8 C9 C10 N3 -12.2(14) . . . . ? C32 C9 C10 N3 173.7(8) . . . . ? C8 C9 C10 C11 164.9(8) . . . . ? C32 C9 C10 C11 -9.1(13) . . . . ? N3 C10 C11 C12 -0.5(10) . . . . ? C9 C10 C11 C12 -178.1(9) . . . . ? C10 C11 C12 C13 0.9(10) . . . . ? C11 C12 C13 N3 -1.0(10) . . . . ? C11 C12 C13 C14 176.3(9) . . . . ? N3 C13 C14 C15 15.5(13) . . . . ? C12 C13 C14 C15 -161.5(9) . . . . ? N3 C13 C14 C38 -162.4(8) . . . . ? C12 C13 C14 C38 20.6(13) . . . . ? C13 C14 C15 N4 -8.8(14) . . . . ? C38 C14 C15 N4 169.0(8) . . . . ? C13 C14 C15 C16 167.3(8) . . . . ? C38 C14 C15 C16 -14.9(12) . . . . ? N4 C15 C16 C17 -1.0(11) . . . . ? C14 C15 C16 C17 -177.7(8) . . . . ? C15 C16 C17 C18 0.9(11) . . . . ? C16 C17 C18 C19 179.1(8) . . . . ? C16 C17 C18 N4 -0.5(10) . . . . ? N4 C18 C19 C1 12.2(13) . . . . ? C17 C18 C19 C1 -167.5(8) . . . . ? N4 C18 C19 C44 -161.0(8) . . . . ? C17 C18 C19 C44 19.4(13) . . . . ? C20 C1 C19 C18 22.4(14) . . . . ? C2 C1 C19 C18 -143.3(8) . . . . ? C20 C1 C19 C44 -164.2(9) . . . . ? C2 C1 C19 C44 30.1(11) . . . . ? N1 C3 C20 C1 -5.7(9) . . . . ? C4 C3 C20 C1 160.9(8) . . . . ? N1 C3 C20 C21 161.3(8) . . . . ? C4 C3 C20 C21 -32.1(14) . . . . ? C2 C1 C20 C3 6.1(9) . . . . ? C19 C1 C20 C3 -161.0(9) . . . . ? C2 C1 C20 C21 -161.2(7) . . . . ? C19 C1 C20 C21 31.8(14) . . . . ? C9 C8 N2 C5 -175.1(8) . . . . ? C7 C8 N2 C5 2.8(9) . . . . ? C9 C8 N2 Re1 34.2(10) . . . . ? C7 C8 N2 Re1 -147.9(5) . . . . ? C4 C5 N2 C8 175.0(8) . . . . ? C6 C5 N2 C8 -2.6(9) . . . . ? C4 C5 N2 Re1 -41.9(13) . . . . ? C6 C5 N2 Re1 140.5(6) . . . . ? C9 C10 N3 C13 177.4(8) . . . . ? C11 C10 N3 C13 -0.1(9) . . . . ? C9 C10 N3 Re1 -26.4(11) . . . . ? C11 C10 N3 Re1 156.0(6) . . . . ? C14 C13 N3 C10 -176.7(8) . . . . ? C12 C13 N3 C10 0.7(9) . . . . ? C14 C13 N3 Re1 27.1(11) . . . . ? C12 C13 N3 Re1 -155.5(6) . . . . ? C14 C15 N4 C18 177.1(8) . . . . ? C16 C15 N4 C18 0.6(9) . . . . ? C14 C15 N4 Re1 -32.0(10) . . . . ? C16 C15 N4 Re1 151.5(6) . . . . ? C19 C18 N4 C15 -179.7(8) . . . . ? C17 C18 N4 C15 -0.1(9) . . . . ? C19 C18 N4 Re1 37.2(12) . . . . ? C17 C18 N4 Re1 -143.2(6) . . . . ? C10 N3 Re1 C25 -33.8(7) . . . . ? C13 N3 Re1 C25 118.4(6) . . . . ? C10 N3 Re1 C23 -121.5(6) . . . . ? C13 N3 Re1 C23 30.7(7) . . . . ? C10 N3 Re1 N4 159.8(6) . . . . ? C13 N3 Re1 N4 -48.0(6) . . . . ? C10 N3 Re1 N2 45.5(6) . . . . ? C13 N3 Re1 N2 -162.3(7) . . . . ? C15 N4 Re1 C25 -32.6(15) . . . . ? C18 N4 Re1 C25 107.9(14) . . . . ? C15 N4 Re1 C23 -50.8(6) . . . . ? C18 N4 Re1 C23 89.7(7) . . . . ? C15 N4 Re1 C24 -136.4(6) . . . . ? C18 N4 Re1 C24 4.1(7) . . . . ? C15 N4 Re1 N3 47.8(5) . . . . ? C18 N4 Re1 N3 -171.7(7) . . . . ? C15 N4 Re1 N2 121.9(5) . . . . ? C18 N4 Re1 N2 -97.6(7) . . . . ? C8 N2 Re1 C25 53.3(6) . . . . ? C5 N2 Re1 C25 -87.2(8) . . . . ? C8 N2 Re1 C23 26.5(16) . . . . ? C5 N2 Re1 C23 -114.1(14) . . . . ? C8 N2 Re1 C24 137.8(6) . . . . ? C5 N2 Re1 C24 -2.8(8) . . . . ? C8 N2 Re1 N3 -46.6(6) . . . . ? C5 N2 Re1 N3 172.8(8) . . . . ? C8 N2 Re1 N4 -120.8(5) . . . . ? C5 N2 Re1 N4 98.6(7) . . . . ? C5 C4 C26 C27 125.5(9) . . . . ? C3 C4 C26 C27 -53.6(12) . . . . ? C5 C4 C26 C31 -58.8(12) . . . . ? C3 C4 C26 C31 122.0(10) . . . . ? C31 C26 C27 C28 0.7(15) . . . . ? C4 C26 C27 C28 176.6(9) . . . . ? C26 C27 C28 C29 -2.0(18) . . . . ? C27 C28 C29 C30 1.4(19) . . . . ? C28 C29 C30 C31 0.5(19) . . . . ? C29 C30 C31 C26 -1.8(18) . . . . ? C27 C26 C31 C30 1.2(15) . . . . ? C4 C26 C31 C30 -174.7(9) . . . . ? C10 C9 C32 C37 -66.6(12) . . . . ? C8 C9 C32 C37 119.0(10) . . . . ? C10 C9 C32 C33 110.7(10) . . . . ? C8 C9 C32 C33 -63.6(12) . . . . ? C37 C32 C33 C34 -0.7(16) . . . . ? C9 C32 C33 C34 -178.1(10) . . . . ? C32 C33 C34 C35 0.0(17) . . . . ? C33 C34 C35 C36 0.6(19) . . . . ? C34 C35 C36 C37 -1(2) . . . . ? C33 C32 C37 C36 0.8(16) . . . . ? C9 C32 C37 C36 178.2(10) . . . . ? C35 C36 C37 C32 -0.2(18) . . . . ? C13 C14 C38 C43 109.9(10) . . . . ? C15 C14 C38 C43 -68.1(11) . . . . ? C13 C14 C38 C39 -67.5(11) . . . . ? C15 C14 C38 C39 114.6(10) . . . . ? C43 C38 C39 C40 1.9(14) . . . . ? C14 C38 C39 C40 179.3(9) . . . . ? C38 C39 C40 C41 -0.9(15) . . . . ? C39 C40 C41 C42 -1.7(16) . . . . ? C40 C41 C42 C43 3.2(16) . . . . ? C41 C42 C43 C38 -2.2(16) . . . . ? C39 C38 C43 C42 -0.4(14) . . . . ? C14 C38 C43 C42 -177.8(9) . . . . ? C18 C19 C44 C45 53.4(13) . . . . ? C1 C19 C44 C45 -120.1(9) . . . . ? C18 C19 C44 C49 -133.8(9) . . . . ? C1 C19 C44 C49 52.7(12) . . . . ? C49 C44 C45 C46 -1.5(15) . . . . ? C19 C44 C45 C46 171.4(10) . . . . ? C44 C45 C46 C47 2.5(18) . . . . ? C45 C46 C47 C48 -1.2(19) . . . . ? C46 C47 C48 C49 -0.8(17) . . . . ? C45 C44 C49 C48 -0.6(14) . . . . ? C19 C44 C49 C48 -173.7(9) . . . . ? C47 C48 C49 C44 1.8(16) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 2.767 _refine_diff_density_min -2.577 _refine_diff_density_rms 0.164 data_Re(26NCP-NHC)(CO)3 _database_code_depnum_ccdc_archive 'CCDC 883522' #============================================================================== _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H34 N5 O3 Re, C6 H5 Cl' _chemical_formula_sum 'C62 H39 Cl N5 O3 Re' _chemical_formula_weight 1123.64 _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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 _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 20.305(6) _cell_length_b 13.757(3) _cell_length_c 17.729(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.049(4) _cell_angle_gamma 90.00 _cell_volume 4735(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13595 _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 31.4 _exptl_crystal_description prism _exptl_crystal_colour violet _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2248 _exptl_absorpt_coefficient_mu 2.679 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.835 _exptl_absorpt_correction_T_max 0.948 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoKa _diffrn_radiation_source 'VariMax 50 kV 24mA Rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'VariMaxTM with Saturn' _diffrn_measurement_method w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 79431 _diffrn_reflns_av_R_equivalents 0.0914 _diffrn_reflns_av_sigmaI/netI 0.0643 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 28.00 _reflns_number_total 11423 _reflns_number_gt 10267 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.8.2' _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/[?^2^(Fo^2^)+(0.0461P)^2^+22.8382P] 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 11423 _refine_ls_number_parameters 652 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0851 _refine_ls_R_factor_gt 0.0749 _refine_ls_wR_factor_ref 0.1475 _refine_ls_wR_factor_gt 0.1419 _refine_ls_goodness_of_fit_ref 1.213 _refine_ls_restrained_S_all 1.216 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _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 0.776954(13) 0.283191(18) 0.061717(14) 0.01763(9) Uani 1 1 d . . . O1 O 0.7613(2) 0.0621(3) 0.0761(3) 0.0255(10) Uani 1 1 d U . . O2 O 0.6525(3) 0.2931(4) 0.1301(3) 0.0317(11) Uani 1 1 d U . . O3 O 0.8696(2) 0.2910(3) 0.2339(3) 0.0264(10) Uani 1 1 d U . . N1 N 0.8637(3) 0.2070(4) -0.0473(3) 0.0189(11) Uani 1 1 d . . . N2 N 0.7128(3) 0.2933(4) -0.0577(3) 0.0171(11) Uani 1 1 d . . . N3 N 0.7805(3) 0.4396(4) 0.0451(3) 0.0173(11) Uani 1 1 d . . . N4 N 1.0327(3) 0.3725(4) 0.0546(3) 0.0203(11) Uani 1 1 d . . . N5 N 1.1608(3) 0.4119(4) 0.2057(3) 0.0217(12) Uani 1 1 d . . . C1 C 0.9254(3) 0.1827(5) -0.0638(4) 0.0222(14) Uani 1 1 d . . . C2 C 0.9164(4) 0.0888(5) -0.1015(4) 0.0250(15) Uani 1 1 d . . . H2 H 0.9506 0.0540 -0.1172 0.030 Uiso 1 1 calc R . . C3 C 0.8519(4) 0.0588(5) -0.1107(4) 0.0250(14) Uani 1 1 d . . . H3 H 0.8342 -0.0030 -0.1307 0.030 Uiso 1 1 calc R . . C4 C 0.8130(3) 0.1337(5) -0.0860(4) 0.0222(14) Uani 1 1 d . . . C5 C 0.7430(3) 0.1405(5) -0.1135(4) 0.0207(13) Uani 1 1 d . . . C6 C 0.6989(3) 0.2214(5) -0.1115(4) 0.0202(13) Uani 1 1 d . . . C7 C 0.6363(4) 0.2404(6) -0.1722(4) 0.0294(16) Uani 1 1 d . . . H7 H 0.6144 0.1992 -0.2152 0.035 Uiso 1 1 calc R . . C8 C 0.6138(4) 0.3310(5) -0.1559(4) 0.0258(15) Uani 1 1 d . . . H8 H 0.5741 0.3647 -0.1864 0.031 Uiso 1 1 calc R . . C9 C 0.6618(3) 0.3635(5) -0.0846(4) 0.0196(13) Uani 1 1 d . . . C10 C 0.6653(3) 0.4571(5) -0.0508(4) 0.0184(13) Uani 1 1 d . . . C11 C 0.7220(3) 0.4942(4) 0.0076(4) 0.0177(12) Uani 1 1 d . . . C12 C 0.7354(3) 0.5934(5) 0.0322(4) 0.0190(13) Uani 1 1 d . . . H12 H 0.7042 0.6462 0.0172 0.023 Uiso 1 1 calc R . . C13 C 0.8011(3) 0.5981(5) 0.0811(4) 0.0184(13) Uani 1 1 d . . . H13 H 0.8246 0.6549 0.1054 0.022 Uiso 1 1 calc R . . C14 C 0.8284(3) 0.5000(4) 0.0891(4) 0.0161(12) Uani 1 1 d . . . C15 C 0.8997(3) 0.4748(5) 0.1274(4) 0.0170(12) Uani 1 1 d . . . C16 C 0.9369(3) 0.4125(5) 0.0920(4) 0.0182(13) Uani 1 1 d . . . C17 C 1.0102(3) 0.4272(4) 0.1094(4) 0.0177(12) Uani 1 1 d . . . C18 C 0.9184(3) 0.3365(4) 0.0319(4) 0.0170(12) Uani 1 1 d . . . C19 C 0.9809(3) 0.3151(4) 0.0116(4) 0.0171(12) Uani 1 1 d . . . C20 C 0.9841(3) 0.2373(5) -0.0380(4) 0.0189(13) Uani 1 1 d . . . C21 C 1.0966(3) 0.3903(5) 0.0335(4) 0.0220(14) Uani 1 1 d . . . H21A H 1.1097 0.4588 0.0428 0.026 Uiso 1 1 calc R . . H21B H 1.0890 0.3748 -0.0224 0.026 Uiso 1 1 calc R . . H21C H 1.1334 0.3491 0.0659 0.026 Uiso 1 1 calc R . . C22 C 0.8592(3) 0.2783(4) 0.0067(3) 0.0142(11) Uani 1 1 d . . . C23 C 0.7051(4) 0.0562(5) -0.1614(4) 0.0248(14) Uani 1 1 d . . . C24 C 0.6584(4) 0.0041(6) -0.1350(4) 0.0348(18) Uani 1 1 d . . . H24 H 0.6510 0.0208 -0.0861 0.042 Uiso 1 1 calc R . . C25 C 0.6217(4) -0.0726(6) -0.1789(5) 0.041(2) Uani 1 1 d . . . H25 H 0.5902 -0.1087 -0.1594 0.049 Uiso 1 1 calc R . . C26 C 0.6309(4) -0.0963(6) -0.2507(5) 0.040(2) Uani 1 1 d . . . H26 H 0.6054 -0.1482 -0.2809 0.048 Uiso 1 1 calc R . . C27 C 0.6771(4) -0.0448(5) -0.2789(4) 0.0329(17) Uani 1 1 d . . . H27 H 0.6841 -0.0620 -0.3278 0.039 Uiso 1 1 calc R . . C28 C 0.7133(4) 0.0326(5) -0.2349(4) 0.0296(16) Uani 1 1 d . . . H28 H 0.7438 0.0696 -0.2551 0.035 Uiso 1 1 calc R . . C29 C 0.6074(3) 0.5246(5) -0.0857(4) 0.0223(14) Uani 1 1 d . . . C30 C 0.5421(4) 0.5069(5) -0.0770(4) 0.0283(15) Uani 1 1 d . . . H30 H 0.5346 0.4508 -0.0494 0.034 Uiso 1 1 calc R . . C31 C 0.4883(4) 0.5714(6) -0.1088(5) 0.0392(19) Uani 1 1 d . . . H31 H 0.4441 0.5590 -0.1029 0.047 Uiso 1 1 calc R . . C32 C 0.4987(4) 0.6529(6) -0.1488(4) 0.0377(19) Uani 1 1 d . . . H32 H 0.4625 0.6985 -0.1680 0.045 Uiso 1 1 calc R . . C33 C 0.5623(5) 0.6681(6) -0.1607(5) 0.040(2) Uani 1 1 d . . . H33 H 0.5686 0.7217 -0.1917 0.048 Uiso 1 1 calc R . . C34 C 0.6166(4) 0.6065(5) -0.1284(4) 0.0310(16) Uani 1 1 d . . . H34 H 0.6605 0.6195 -0.1350 0.037 Uiso 1 1 calc R . . C35 C 0.9384(3) 0.5322(4) 0.1937(4) 0.0192(13) Uani 1 1 d . . . C36 C 0.9042(3) 0.5837(5) 0.2413(4) 0.0216(13) Uani 1 1 d . . . H36 H 0.8554 0.5809 0.2283 0.026 Uiso 1 1 calc R . . C37 C 0.9406(3) 0.6372(5) 0.3055(4) 0.0228(14) Uani 1 1 d . . . H37 H 0.9168 0.6747 0.3342 0.027 Uiso 1 1 calc R . . C38 C 1.0130(4) 0.6365(5) 0.3287(4) 0.0253(15) Uani 1 1 d . . . H38 H 1.0380 0.6708 0.3747 0.030 Uiso 1 1 calc R . . C39 C 1.0479(4) 0.5866(5) 0.2851(4) 0.0233(14) Uani 1 1 d . . . H39 H 1.0968 0.5862 0.3017 0.028 Uiso 1 1 calc R . . C40 C 1.0117(3) 0.5355(4) 0.2156(4) 0.0174(12) Uani 1 1 d . . . C41 C 1.0461(3) 0.2041(5) -0.0597(4) 0.0206(13) Uani 1 1 d . . . C42 C 1.1028(4) 0.1615(6) -0.0053(4) 0.0322(17) Uani 1 1 d . . . H42 H 1.1036 0.1559 0.0483 0.039 Uiso 1 1 calc R . . C43 C 1.1579(4) 0.1272(6) -0.0284(4) 0.0339(18) Uani 1 1 d . . . H43 H 1.1967 0.0997 0.0094 0.041 Uiso 1 1 calc R . . C44 C 1.1564(4) 0.1334(5) -0.1070(4) 0.0274(15) Uani 1 1 d . . . H44 H 1.1939 0.1087 -0.1229 0.033 Uiso 1 1 calc R . . C45 C 1.1009(4) 0.1749(5) -0.1624(4) 0.0236(14) Uani 1 1 d . . . H45 H 1.1004 0.1794 -0.2160 0.028 Uiso 1 1 calc R . . C46 C 1.0459(3) 0.2102(5) -0.1389(4) 0.0222(14) Uani 1 1 d . . . H46 H 1.0077 0.2388 -0.1768 0.027 Uiso 1 1 calc R . . C47 C 1.0482(3) 0.4865(5) 0.1681(4) 0.0187(13) Uani 1 1 d . . . C48 C 1.1253(3) 0.4959(5) 0.1880(4) 0.0196(13) Uani 1 1 d . . . C49 C 1.1569(4) 0.5853(5) 0.1880(4) 0.0251(14) Uani 1 1 d . . . H49 H 1.1301 0.6427 0.1740 0.030 Uiso 1 1 calc R . . C50 C 1.2279(4) 0.5897(5) 0.2086(4) 0.0299(16) Uani 1 1 d . . . H50 H 1.2507 0.6501 0.2089 0.036 Uiso 1 1 calc R . . C51 C 1.2655(4) 0.5037(6) 0.2290(4) 0.0299(16) Uani 1 1 d . . . H51 H 1.3144 0.5049 0.2444 0.036 Uiso 1 1 calc R . . C52 C 1.2302(4) 0.4158(6) 0.2265(4) 0.0268(15) Uani 1 1 d . . . C53 C 1.2666(4) 0.3207(6) 0.2463(5) 0.0341(18) Uani 1 1 d . . . H53A H 1.2502 0.2871 0.2861 0.041 Uiso 1 1 calc R . . H53B H 1.3163 0.3321 0.2670 0.041 Uiso 1 1 calc R . . H53C H 1.2571 0.2806 0.1986 0.041 Uiso 1 1 calc R . . C54 C 0.7710(3) 0.1451(4) 0.0670(3) 0.0116(10) Uani 1 1 d U . . C55 C 0.6981(4) 0.2923(5) 0.1046(4) 0.0240(13) Uani 1 1 d U . . C56 C 0.8367(3) 0.2872(4) 0.1697(4) 0.0191(11) Uani 1 1 d U . . Cl1 Cl 0.55403(13) 0.42796(18) 0.62971(15) 0.0566(6) Uani 1 1 d . . . C57 C 0.5616(4) 0.5459(6) 0.5967(5) 0.0381(19) Uani 1 1 d . . . C58 C 0.5157(5) 0.6161(6) 0.6053(5) 0.044(2) Uani 1 1 d . . . H58 H 0.4805 0.6006 0.6287 0.052 Uiso 1 1 calc R . . C59 C 0.5221(5) 0.7095(6) 0.5790(6) 0.048(2) Uani 1 1 d . . . H59 H 0.4905 0.7582 0.5841 0.058 Uiso 1 1 calc R . . C60 C 0.5739(4) 0.7335(6) 0.5452(5) 0.041(2) Uani 1 1 d . . . H60 H 0.5781 0.7977 0.5274 0.049 Uiso 1 1 calc R . . C61 C 0.6190(4) 0.6612(7) 0.5384(5) 0.041(2) Uani 1 1 d . . . H61 H 0.6545 0.6759 0.5152 0.050 Uiso 1 1 calc R . . C62 C 0.6135(4) 0.5666(6) 0.5652(5) 0.0387(19) Uani 1 1 d . . . H62 H 0.6455 0.5178 0.5614 0.046 Uiso 1 1 calc R . . _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 0.01928(14) 0.01724(14) 0.01764(14) 0.00007(10) 0.00737(10) 0.00162(10) O1 0.030(2) 0.016(2) 0.030(2) 0.0025(17) 0.0084(19) -0.0001(18) O2 0.031(2) 0.032(2) 0.038(3) -0.004(2) 0.019(2) 0.000(2) O3 0.028(2) 0.026(2) 0.023(2) 0.0030(19) 0.0037(18) 0.0010(19) N1 0.020(3) 0.020(3) 0.019(3) -0.002(2) 0.011(2) 0.001(2) N2 0.020(3) 0.018(3) 0.012(2) 0.000(2) 0.003(2) 0.004(2) N3 0.017(3) 0.015(3) 0.020(3) 0.001(2) 0.006(2) -0.001(2) N4 0.019(3) 0.024(3) 0.021(3) 0.005(2) 0.011(2) 0.002(2) N5 0.019(3) 0.023(3) 0.025(3) 0.005(2) 0.009(2) 0.006(2) C1 0.027(3) 0.025(3) 0.022(3) 0.002(3) 0.019(3) 0.007(3) C2 0.034(4) 0.026(4) 0.019(3) 0.001(3) 0.014(3) 0.006(3) C3 0.032(4) 0.021(3) 0.024(4) -0.002(3) 0.011(3) 0.003(3) C4 0.029(3) 0.023(3) 0.018(3) -0.004(3) 0.013(3) 0.000(3) C5 0.027(3) 0.022(3) 0.014(3) -0.004(2) 0.008(3) -0.002(3) C6 0.020(3) 0.018(3) 0.024(3) -0.003(3) 0.009(3) -0.001(3) C7 0.020(3) 0.041(4) 0.021(4) 0.001(3) -0.003(3) 0.002(3) C8 0.029(4) 0.019(3) 0.025(4) 0.000(3) 0.000(3) -0.003(3) C9 0.022(3) 0.020(3) 0.018(3) 0.002(2) 0.007(3) 0.002(3) C10 0.020(3) 0.020(3) 0.018(3) 0.007(2) 0.009(3) 0.001(2) C11 0.021(3) 0.015(3) 0.016(3) 0.001(2) 0.005(3) 0.006(2) C12 0.021(3) 0.016(3) 0.021(3) 0.005(2) 0.008(3) 0.007(2) C13 0.016(3) 0.017(3) 0.027(3) -0.004(3) 0.013(3) -0.001(2) C14 0.017(3) 0.016(3) 0.018(3) -0.002(2) 0.009(2) 0.004(2) C15 0.015(3) 0.020(3) 0.017(3) 0.000(2) 0.006(2) -0.003(2) C16 0.020(3) 0.019(3) 0.020(3) 0.005(2) 0.011(3) 0.002(2) C17 0.020(3) 0.018(3) 0.019(3) 0.003(2) 0.010(3) 0.005(2) C18 0.020(3) 0.016(3) 0.017(3) 0.004(2) 0.008(2) 0.005(2) C19 0.019(3) 0.017(3) 0.015(3) 0.002(2) 0.006(2) 0.000(2) C20 0.025(3) 0.019(3) 0.018(3) 0.005(2) 0.013(3) 0.003(3) C21 0.018(3) 0.030(4) 0.021(3) -0.002(3) 0.009(3) -0.003(3) C22 0.016(3) 0.014(3) 0.014(3) 0.000(2) 0.007(2) 0.001(2) C23 0.030(4) 0.024(4) 0.022(3) -0.003(3) 0.010(3) -0.001(3) C24 0.038(4) 0.042(5) 0.027(4) -0.009(3) 0.013(3) -0.008(4) C25 0.043(5) 0.034(5) 0.051(5) -0.011(4) 0.022(4) -0.018(4) C26 0.037(4) 0.031(4) 0.051(5) -0.014(4) 0.011(4) -0.005(4) C27 0.043(4) 0.027(4) 0.027(4) -0.007(3) 0.006(3) 0.009(3) C28 0.037(4) 0.030(4) 0.023(4) -0.009(3) 0.012(3) -0.004(3) C29 0.023(3) 0.023(3) 0.020(3) -0.002(3) 0.005(3) 0.005(3) C30 0.025(4) 0.023(4) 0.035(4) -0.001(3) 0.005(3) 0.000(3) C31 0.024(4) 0.039(5) 0.050(5) -0.003(4) 0.004(4) 0.004(3) C32 0.034(4) 0.041(5) 0.030(4) 0.002(3) -0.003(3) 0.018(4) C33 0.056(5) 0.031(4) 0.035(4) 0.011(3) 0.015(4) 0.013(4) C34 0.038(4) 0.032(4) 0.026(4) 0.009(3) 0.014(3) 0.009(3) C35 0.026(3) 0.015(3) 0.019(3) 0.002(2) 0.011(3) 0.002(3) C36 0.025(3) 0.021(3) 0.022(3) 0.002(3) 0.011(3) -0.001(3) C37 0.029(3) 0.022(3) 0.023(3) -0.004(3) 0.016(3) -0.008(3) C38 0.031(4) 0.028(4) 0.020(3) -0.007(3) 0.012(3) -0.007(3) C39 0.024(3) 0.024(3) 0.023(3) -0.004(3) 0.008(3) -0.005(3) C40 0.019(3) 0.016(3) 0.019(3) 0.000(2) 0.009(3) 0.000(2) C41 0.020(3) 0.023(3) 0.022(3) 0.002(3) 0.012(3) 0.001(3) C42 0.037(4) 0.042(4) 0.025(4) 0.011(3) 0.020(3) 0.020(4) C43 0.032(4) 0.042(5) 0.030(4) 0.007(3) 0.011(3) 0.020(3) C44 0.035(4) 0.020(3) 0.032(4) 0.003(3) 0.017(3) 0.008(3) C45 0.034(4) 0.019(3) 0.024(3) -0.004(3) 0.018(3) -0.003(3) C46 0.024(3) 0.026(3) 0.020(3) -0.002(3) 0.012(3) -0.005(3) C47 0.024(3) 0.018(3) 0.016(3) 0.002(2) 0.008(3) -0.003(3) C48 0.017(3) 0.030(4) 0.014(3) -0.004(3) 0.008(2) -0.004(3) C49 0.031(4) 0.023(3) 0.024(4) 0.003(3) 0.012(3) 0.000(3) C50 0.031(4) 0.030(4) 0.032(4) 0.002(3) 0.013(3) -0.010(3) C51 0.020(3) 0.048(5) 0.023(4) -0.002(3) 0.007(3) -0.002(3) C52 0.023(3) 0.040(4) 0.019(3) 0.007(3) 0.008(3) 0.006(3) C53 0.030(4) 0.044(5) 0.033(4) 0.010(3) 0.015(3) 0.015(3) C54 0.0136(17) 0.0099(16) 0.0117(17) -0.0033(14) 0.0042(14) 0.0028(14) C55 0.029(3) 0.019(3) 0.027(3) -0.002(2) 0.012(2) 0.001(2) C56 0.022(3) 0.017(3) 0.020(3) 0.004(2) 0.009(2) 0.002(2) Cl1 0.0582(15) 0.0460(13) 0.0588(15) 0.0126(11) 0.0066(12) -0.0030(11) C57 0.045(5) 0.035(4) 0.032(4) 0.000(3) 0.008(4) 0.001(4) C58 0.041(5) 0.045(5) 0.049(5) -0.004(4) 0.021(4) -0.001(4) C59 0.043(5) 0.039(5) 0.063(6) -0.002(4) 0.015(5) 0.010(4) C60 0.043(5) 0.041(5) 0.037(5) 0.001(4) 0.007(4) 0.001(4) C61 0.043(5) 0.053(5) 0.033(4) -0.002(4) 0.019(4) -0.003(4) C62 0.031(4) 0.044(5) 0.042(5) -0.006(4) 0.014(4) 0.006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; _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 C54 1.908(6) . ? Re1 C56 1.944(6) . ? Re1 C55 1.967(7) . ? Re1 N2 2.141(5) . ? Re1 C22 2.168(6) . ? Re1 N3 2.176(5) . ? O1 C54 1.177(7) . ? O2 C55 1.145(8) . ? O3 C56 1.139(8) . ? N1 C22 1.392(7) . ? N1 C1 1.409(8) . ? N1 C4 1.460(8) . ? N2 C6 1.346(8) . ? N2 C9 1.393(8) . ? N3 C14 1.342(8) . ? N3 C11 1.397(8) . ? N4 C19 1.358(8) . ? N4 C17 1.407(8) . ? N4 C21 1.471(8) . ? N5 C52 1.348(8) . ? N5 C48 1.349(8) . ? C1 C20 1.368(9) . ? C1 C2 1.442(9) . ? C2 C3 1.335(10) . ? C2 H2 0.9500 . ? C3 C4 1.444(9) . ? C3 H3 0.9500 . ? C4 C5 1.365(9) . ? C5 C6 1.435(9) . ? C5 C23 1.508(9) . ? C6 C7 1.429(9) . ? C7 C8 1.385(10) . ? C7 H7 0.9500 . ? C8 C9 1.422(9) . ? C8 H8 0.9500 . ? C9 C10 1.414(9) . ? C10 C11 1.399(9) . ? C10 C29 1.484(9) . ? C11 C12 1.434(9) . ? C12 C13 1.363(9) . ? C12 H12 0.9500 . ? C13 C14 1.449(8) . ? C13 H13 0.9500 . ? C14 C15 1.450(8) . ? C15 C16 1.405(8) . ? C15 C35 1.444(9) . ? C16 C17 1.443(8) . ? C16 C18 1.461(9) . ? C17 C47 1.369(9) . ? C18 C22 1.404(8) . ? C18 C19 1.446(8) . ? C19 C20 1.399(9) . ? C20 C41 1.491(8) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C23 C24 1.377(10) . ? C23 C28 1.399(9) . ? C24 C25 1.391(10) . ? C24 H24 0.9500 . ? C25 C26 1.379(11) . ? C25 H25 0.9500 . ? C26 C27 1.379(11) . ? C26 H26 0.9500 . ? C27 C28 1.395(10) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.399(9) . ? C29 C34 1.400(10) . ? C30 C31 1.392(10) . ? C30 H30 0.9500 . ? C31 C32 1.375(12) . ? C31 H31 0.9500 . ? C32 C33 1.386(12) . ? C32 H32 0.9500 . ? C33 C34 1.375(10) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C40 1.424(9) . ? C35 C36 1.428(9) . ? C36 C37 1.376(9) . ? C36 H36 0.9500 . ? C37 C38 1.407(9) . ? C37 H37 0.9500 . ? C38 C39 1.375(9) . ? C38 H38 0.9500 . ? C39 C40 1.422(9) . ? C39 H39 0.9500 . ? C40 C47 1.441(8) . ? C41 C42 1.397(9) . ? C41 C46 1.405(9) . ? C42 C43 1.382(9) . ? C42 H42 0.9500 . ? C43 C44 1.386(10) . ? C43 H43 0.9500 . ? C44 C45 1.383(10) . ? C44 H44 0.9500 . ? C45 C46 1.389(9) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.508(9) . ? C48 C49 1.388(9) . ? C49 C50 1.380(10) . ? C49 H49 0.9500 . ? C50 C51 1.397(10) . ? C50 H50 0.9500 . ? C51 C52 1.401(10) . ? C51 H51 0.9500 . ? C52 C53 1.492(10) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? Cl1 C57 1.747(8) . ? C57 C62 1.359(11) . ? C57 C58 1.381(11) . ? C58 C59 1.387(12) . ? C58 H58 0.9500 . ? C59 C60 1.394(13) . ? C59 H59 0.9500 . ? C60 C61 1.381(12) . ? C60 H60 0.9500 . ? C61 C62 1.400(12) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? _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 C54 Re1 C56 90.6(2) . . ? C54 Re1 C55 88.5(3) . . ? C56 Re1 C55 87.8(3) . . ? C54 Re1 N2 94.8(2) . . ? C56 Re1 N2 174.6(2) . . ? C55 Re1 N2 92.9(2) . . ? C54 Re1 C22 93.4(2) . . ? C56 Re1 C22 95.9(2) . . ? C55 Re1 C22 175.8(3) . . ? N2 Re1 C22 83.3(2) . . ? C54 Re1 N3 175.2(2) . . ? C56 Re1 N3 94.0(2) . . ? C55 Re1 N3 93.0(2) . . ? N2 Re1 N3 80.56(19) . . ? C22 Re1 N3 84.8(2) . . ? C22 N1 C1 123.5(5) . . ? C22 N1 C4 129.1(5) . . ? C1 N1 C4 106.6(5) . . ? C6 N2 C9 106.6(5) . . ? C6 N2 Re1 126.4(4) . . ? C9 N2 Re1 124.0(4) . . ? C14 N3 C11 108.2(5) . . ? C14 N3 Re1 125.5(4) . . ? C11 N3 Re1 122.7(4) . . ? C19 N4 C17 110.1(5) . . ? C19 N4 C21 123.3(5) . . ? C17 N4 C21 125.2(5) . . ? C52 N5 C48 118.2(6) . . ? C20 C1 N1 122.8(6) . . ? C20 C1 C2 128.8(6) . . ? N1 C1 C2 108.0(6) . . ? C3 C2 C1 108.7(6) . . ? C3 C2 H2 125.7 . . ? C1 C2 H2 125.7 . . ? C2 C3 C4 110.3(6) . . ? C2 C3 H3 124.9 . . ? C4 C3 H3 124.9 . . ? C5 C4 C3 123.1(6) . . ? C5 C4 N1 129.7(6) . . ? C3 C4 N1 105.2(5) . . ? C4 C5 C6 129.5(6) . . ? C4 C5 C23 117.1(6) . . ? C6 C5 C23 113.1(6) . . ? N2 C6 C7 110.7(6) . . ? N2 C6 C5 125.9(6) . . ? C7 C6 C5 123.2(6) . . ? C8 C7 C6 106.4(6) . . ? C8 C7 H7 126.8 . . ? C6 C7 H7 126.8 . . ? C7 C8 C9 106.6(6) . . ? C7 C8 H8 126.7 . . ? C9 C8 H8 126.7 . . ? N2 C9 C10 123.0(6) . . ? N2 C9 C8 109.5(5) . . ? C10 C9 C8 126.9(6) . . ? C11 C10 C9 125.1(6) . . ? C11 C10 C29 117.4(6) . . ? C9 C10 C29 117.2(6) . . ? N3 C11 C10 123.7(5) . . ? N3 C11 C12 108.0(5) . . ? C10 C11 C12 127.9(6) . . ? C13 C12 C11 107.6(5) . . ? C13 C12 H12 126.2 . . ? C11 C12 H12 126.2 . . ? C12 C13 C14 107.0(5) . . ? C12 C13 H13 126.5 . . ? C14 C13 H13 126.5 . . ? N3 C14 C13 109.2(5) . . ? N3 C14 C15 125.3(5) . . ? C13 C14 C15 124.6(6) . . ? C16 C15 C35 117.5(6) . . ? C16 C15 C14 122.0(5) . . ? C35 C15 C14 118.8(5) . . ? C15 C16 C17 118.3(6) . . ? C15 C16 C18 134.9(6) . . ? C17 C16 C18 106.5(5) . . ? C47 C17 N4 128.2(6) . . ? C47 C17 C16 124.2(6) . . ? N4 C17 C16 107.6(5) . . ? C22 C18 C19 122.4(5) . . ? C22 C18 C16 130.7(5) . . ? C19 C18 C16 105.8(5) . . ? N4 C19 C20 128.8(6) . . ? N4 C19 C18 109.5(5) . . ? C20 C19 C18 121.2(6) . . ? C1 C20 C19 115.6(6) . . ? C1 C20 C41 117.7(6) . . ? C19 C20 C41 126.5(6) . . ? N4 C21 H21A 109.5 . . ? N4 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N4 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 C22 C18 113.4(5) . . ? N1 C22 Re1 123.1(4) . . ? C18 C22 Re1 122.7(4) . . ? C24 C23 C28 118.5(7) . . ? C24 C23 C5 119.8(6) . . ? C28 C23 C5 121.6(6) . . ? C23 C24 C25 120.9(7) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C26 C25 C24 120.0(7) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C27 C26 C25 120.3(7) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C28 119.5(7) . . ? C26 C27 H27 120.3 . . ? C28 C27 H27 120.3 . . ? C27 C28 C23 120.7(7) . . ? C27 C28 H28 119.6 . . ? C23 C28 H28 119.6 . . ? C30 C29 C34 118.7(6) . . ? C30 C29 C10 120.4(6) . . ? C34 C29 C10 120.9(6) . . ? C31 C30 C29 120.0(7) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C32 C31 C30 120.5(7) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C31 C32 C33 119.5(7) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? C34 C33 C32 120.8(7) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C33 C34 C29 120.3(7) . . ? C33 C34 H34 119.9 . . ? C29 C34 H34 119.9 . . ? C40 C35 C36 118.3(6) . . ? C40 C35 C15 121.0(6) . . ? C36 C35 C15 120.6(6) . . ? C37 C36 C35 121.2(6) . . ? C37 C36 H36 119.4 . . ? C35 C36 H36 119.4 . . ? C36 C37 C38 120.0(6) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C39 C38 C37 120.4(6) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C38 C39 C40 120.9(6) . . ? C38 C39 H39 119.5 . . ? C40 C39 H39 119.5 . . ? C39 C40 C35 119.0(6) . . ? C39 C40 C47 120.9(6) . . ? C35 C40 C47 120.1(6) . . ? C42 C41 C46 118.4(6) . . ? C42 C41 C20 122.5(6) . . ? C46 C41 C20 119.0(6) . . ? C43 C42 C41 120.9(6) . . ? C43 C42 H42 119.5 . . ? C41 C42 H42 119.5 . . ? C42 C43 C44 119.7(7) . . ? C42 C43 H43 120.2 . . ? C44 C43 H43 120.2 . . ? C45 C44 C43 120.8(6) . . ? C45 C44 H44 119.6 . . ? C43 C44 H44 119.6 . . ? C44 C45 C46 119.4(6) . . ? C44 C45 H45 120.3 . . ? C46 C45 H45 120.3 . . ? C45 C46 C41 120.8(6) . . ? C45 C46 H46 119.6 . . ? C41 C46 H46 119.6 . . ? C17 C47 C40 116.8(6) . . ? C17 C47 C48 123.0(6) . . ? C40 C47 C48 120.1(5) . . ? N5 C48 C49 123.0(6) . . ? N5 C48 C47 115.3(6) . . ? C49 C48 C47 121.7(6) . . ? C50 C49 C48 119.1(7) . . ? C50 C49 H49 120.5 . . ? C48 C49 H49 120.5 . . ? C49 C50 C51 118.7(7) . . ? C49 C50 H50 120.6 . . ? C51 C50 H50 120.6 . . ? C50 C51 C52 119.1(6) . . ? C50 C51 H51 120.4 . . ? C52 C51 H51 120.4 . . ? N5 C52 C51 121.8(6) . . ? N5 C52 C53 115.8(7) . . ? C51 C52 C53 122.4(6) . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O1 C54 Re1 171.0(5) . . ? O2 C55 Re1 176.8(6) . . ? O3 C56 Re1 177.2(6) . . ? C62 C57 C58 121.9(8) . . ? C62 C57 Cl1 119.2(7) . . ? C58 C57 Cl1 118.9(7) . . ? C57 C58 C59 118.6(8) . . ? C57 C58 H58 120.7 . . ? C59 C58 H58 120.7 . . ? C58 C59 C60 121.4(8) . . ? C58 C59 H59 119.3 . . ? C60 C59 H59 119.3 . . ? C61 C60 C59 118.0(8) . . ? C61 C60 H60 121.0 . . ? C59 C60 H60 121.0 . . ? C60 C61 C62 121.3(8) . . ? C60 C61 H61 119.4 . . ? C62 C61 H61 119.4 . . ? C57 C62 C61 118.9(8) . . ? C57 C62 H62 120.6 . . ? C61 C62 H62 120.6 . . ? _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C54 Re1 N2 C6 -20.6(5) . . . . ? C55 Re1 N2 C6 -109.3(5) . . . . ? C22 Re1 N2 C6 72.3(5) . . . . ? N3 Re1 N2 C6 158.2(5) . . . . ? C54 Re1 N2 C9 137.4(5) . . . . ? C55 Re1 N2 C9 48.6(5) . . . . ? C22 Re1 N2 C9 -129.7(5) . . . . ? N3 Re1 N2 C9 -43.9(5) . . . . ? C56 Re1 N3 C14 19.1(5) . . . . ? C55 Re1 N3 C14 107.1(5) . . . . ? N2 Re1 N3 C14 -160.5(5) . . . . ? C22 Re1 N3 C14 -76.5(5) . . . . ? C56 Re1 N3 C11 -136.9(5) . . . . ? C55 Re1 N3 C11 -48.9(5) . . . . ? N2 Re1 N3 C11 43.5(5) . . . . ? C22 Re1 N3 C11 127.5(5) . . . . ? C22 N1 C1 C20 -10.9(10) . . . . ? C4 N1 C1 C20 178.5(6) . . . . ? C22 N1 C1 C2 162.1(6) . . . . ? C4 N1 C1 C2 -8.4(7) . . . . ? C20 C1 C2 C3 174.9(7) . . . . ? N1 C1 C2 C3 2.4(8) . . . . ? C1 C2 C3 C4 4.8(8) . . . . ? C2 C3 C4 C5 155.4(7) . . . . ? C2 C3 C4 N1 -9.8(7) . . . . ? C22 N1 C4 C5 37.3(11) . . . . ? C1 N1 C4 C5 -152.9(7) . . . . ? C22 N1 C4 C3 -158.9(6) . . . . ? C1 N1 C4 C3 10.9(7) . . . . ? C3 C4 C5 C6 -162.1(7) . . . . ? N1 C4 C5 C6 -0.9(12) . . . . ? C3 C4 C5 C23 10.1(10) . . . . ? N1 C4 C5 C23 171.4(6) . . . . ? C9 N2 C6 C7 -3.4(7) . . . . ? Re1 N2 C6 C7 157.6(5) . . . . ? C9 N2 C6 C5 170.9(6) . . . . ? Re1 N2 C6 C5 -28.1(9) . . . . ? C4 C5 C6 N2 -27.3(11) . . . . ? C23 C5 C6 N2 160.2(6) . . . . ? C4 C5 C6 C7 146.4(7) . . . . ? C23 C5 C6 C7 -26.1(9) . . . . ? N2 C6 C7 C8 3.4(8) . . . . ? C5 C6 C7 C8 -171.2(6) . . . . ? C6 C7 C8 C9 -1.8(8) . . . . ? C6 N2 C9 C10 -169.1(6) . . . . ? Re1 N2 C9 C10 29.3(8) . . . . ? C6 N2 C9 C8 2.2(7) . . . . ? Re1 N2 C9 C8 -159.4(4) . . . . ? C7 C8 C9 N2 -0.2(8) . . . . ? C7 C8 C9 C10 170.8(6) . . . . ? N2 C9 C10 C11 6.4(10) . . . . ? C8 C9 C10 C11 -163.4(7) . . . . ? N2 C9 C10 C29 179.8(6) . . . . ? C8 C9 C10 C29 10.0(10) . . . . ? C14 N3 C11 C10 171.3(6) . . . . ? Re1 N3 C11 C10 -29.0(8) . . . . ? C14 N3 C11 C12 -1.3(7) . . . . ? Re1 N3 C11 C12 158.3(4) . . . . ? C9 C10 C11 N3 -5.9(10) . . . . ? C29 C10 C11 N3 -179.3(6) . . . . ? C9 C10 C11 C12 165.3(6) . . . . ? C29 C10 C11 C12 -8.2(10) . . . . ? N3 C11 C12 C13 2.0(7) . . . . ? C10 C11 C12 C13 -170.3(6) . . . . ? C11 C12 C13 C14 -1.8(7) . . . . ? C11 N3 C14 C13 0.3(7) . . . . ? Re1 N3 C14 C13 -158.6(4) . . . . ? C11 N3 C14 C15 -169.9(6) . . . . ? Re1 N3 C14 C15 31.2(8) . . . . ? C12 C13 C14 N3 1.0(7) . . . . ? C12 C13 C14 C15 171.3(6) . . . . ? N3 C14 C15 C16 37.2(9) . . . . ? C13 C14 C15 C16 -131.6(7) . . . . ? N3 C14 C15 C35 -158.0(6) . . . . ? C13 C14 C15 C35 33.3(9) . . . . ? C35 C15 C16 C17 -15.8(8) . . . . ? C14 C15 C16 C17 149.2(6) . . . . ? C35 C15 C16 C18 171.7(6) . . . . ? C14 C15 C16 C18 -23.3(11) . . . . ? C19 N4 C17 C47 173.3(6) . . . . ? C21 N4 C17 C47 -19.9(10) . . . . ? C19 N4 C17 C16 -8.1(7) . . . . ? C21 N4 C17 C16 158.6(6) . . . . ? C15 C16 C17 C47 11.8(9) . . . . ? C18 C16 C17 C47 -173.7(6) . . . . ? C15 C16 C17 N4 -166.8(5) . . . . ? C18 C16 C17 N4 7.7(7) . . . . ? C15 C16 C18 C22 -23.5(12) . . . . ? C17 C16 C18 C22 163.4(6) . . . . ? C15 C16 C18 C19 168.6(7) . . . . ? C17 C16 C18 C19 -4.5(6) . . . . ? C17 N4 C19 C20 -166.9(6) . . . . ? C21 N4 C19 C20 26.0(10) . . . . ? C17 N4 C19 C18 5.3(7) . . . . ? C21 N4 C19 C18 -161.8(5) . . . . ? C22 C18 C19 N4 -169.5(6) . . . . ? C16 C18 C19 N4 -0.3(7) . . . . ? C22 C18 C19 C20 3.4(9) . . . . ? C16 C18 C19 C20 172.6(6) . . . . ? N1 C1 C20 C19 5.1(9) . . . . ? C2 C1 C20 C19 -166.4(6) . . . . ? N1 C1 C20 C41 -179.7(6) . . . . ? C2 C1 C20 C41 8.8(10) . . . . ? N4 C19 C20 C1 169.8(6) . . . . ? C18 C19 C20 C1 -1.5(9) . . . . ? N4 C19 C20 C41 -4.9(11) . . . . ? C18 C19 C20 C41 -176.3(6) . . . . ? C1 N1 C22 C18 11.6(8) . . . . ? C4 N1 C22 C18 179.9(6) . . . . ? C1 N1 C22 Re1 -158.4(5) . . . . ? C4 N1 C22 Re1 9.9(9) . . . . ? C19 C18 C22 N1 -8.0(8) . . . . ? C16 C18 C22 N1 -174.2(6) . . . . ? C19 C18 C22 Re1 162.1(4) . . . . ? C16 C18 C22 Re1 -4.2(9) . . . . ? C54 Re1 C22 N1 35.3(5) . . . . ? C56 Re1 C22 N1 126.3(5) . . . . ? N2 Re1 C22 N1 -59.2(5) . . . . ? N3 Re1 C22 N1 -140.2(5) . . . . ? C54 Re1 C22 C18 -133.8(5) . . . . ? C56 Re1 C22 C18 -42.8(5) . . . . ? N2 Re1 C22 C18 131.8(5) . . . . ? N3 Re1 C22 C18 50.7(5) . . . . ? C4 C5 C23 C24 118.4(8) . . . . ? C6 C5 C23 C24 -68.1(9) . . . . ? C4 C5 C23 C28 -65.4(9) . . . . ? C6 C5 C23 C28 108.1(8) . . . . ? C28 C23 C24 C25 2.2(12) . . . . ? C5 C23 C24 C25 178.6(7) . . . . ? C23 C24 C25 C26 -1.2(13) . . . . ? C24 C25 C26 C27 0.7(13) . . . . ? C25 C26 C27 C28 -1.3(12) . . . . ? C26 C27 C28 C23 2.4(12) . . . . ? C24 C23 C28 C27 -2.8(11) . . . . ? C5 C23 C28 C27 -179.1(7) . . . . ? C11 C10 C29 C30 -117.1(7) . . . . ? C9 C10 C29 C30 69.0(8) . . . . ? C11 C10 C29 C34 63.4(8) . . . . ? C9 C10 C29 C34 -110.5(7) . . . . ? C34 C29 C30 C31 -1.6(11) . . . . ? C10 C29 C30 C31 178.9(7) . . . . ? C29 C30 C31 C32 -0.2(12) . . . . ? C30 C31 C32 C33 3.3(12) . . . . ? C31 C32 C33 C34 -4.7(13) . . . . ? C32 C33 C34 C29 2.9(12) . . . . ? C30 C29 C34 C33 0.2(11) . . . . ? C10 C29 C34 C33 179.7(7) . . . . ? C16 C15 C35 C40 8.4(9) . . . . ? C14 C15 C35 C40 -157.1(6) . . . . ? C16 C15 C35 C36 -168.8(6) . . . . ? C14 C15 C35 C36 25.7(9) . . . . ? C40 C35 C36 C37 1.6(9) . . . . ? C15 C35 C36 C37 178.8(6) . . . . ? C35 C36 C37 C38 -4.5(10) . . . . ? C36 C37 C38 C39 3.4(10) . . . . ? C37 C38 C39 C40 0.6(10) . . . . ? C38 C39 C40 C35 -3.4(10) . . . . ? C38 C39 C40 C47 177.5(6) . . . . ? C36 C35 C40 C39 2.3(9) . . . . ? C15 C35 C40 C39 -174.9(6) . . . . ? C36 C35 C40 C47 -178.5(6) . . . . ? C15 C35 C40 C47 4.2(9) . . . . ? C1 C20 C41 C42 -106.5(8) . . . . ? C19 C20 C41 C42 68.1(9) . . . . ? C1 C20 C41 C46 69.4(8) . . . . ? C19 C20 C41 C46 -116.0(7) . . . . ? C46 C41 C42 C43 0.9(11) . . . . ? C20 C41 C42 C43 176.8(7) . . . . ? C41 C42 C43 C44 -1.4(12) . . . . ? C42 C43 C44 C45 1.2(12) . . . . ? C43 C44 C45 C46 -0.5(11) . . . . ? C44 C45 C46 C41 0.1(10) . . . . ? C42 C41 C46 C45 -0.2(10) . . . . ? C20 C41 C46 C45 -176.3(6) . . . . ? N4 C17 C47 C40 179.1(6) . . . . ? C16 C17 C47 C40 0.8(9) . . . . ? N4 C17 C47 C48 -5.4(10) . . . . ? C16 C17 C47 C48 176.3(6) . . . . ? C39 C40 C47 C17 170.4(6) . . . . ? C35 C40 C47 C17 -8.7(9) . . . . ? C39 C40 C47 C48 -5.2(9) . . . . ? C35 C40 C47 C48 175.7(6) . . . . ? C52 N5 C48 C49 2.0(9) . . . . ? C52 N5 C48 C47 -177.8(6) . . . . ? C17 C47 C48 N5 -56.1(8) . . . . ? C40 C47 C48 N5 119.2(6) . . . . ? C17 C47 C48 C49 124.0(7) . . . . ? C40 C47 C48 C49 -60.6(8) . . . . ? N5 C48 C49 C50 -1.5(10) . . . . ? C47 C48 C49 C50 178.3(6) . . . . ? C48 C49 C50 C51 -0.2(10) . . . . ? C49 C50 C51 C52 1.2(10) . . . . ? C48 N5 C52 C51 -0.9(10) . . . . ? C48 N5 C52 C53 179.4(6) . . . . ? C50 C51 C52 N5 -0.7(10) . . . . ? C50 C51 C52 C53 179.0(7) . . . . ? C62 C57 C58 C59 1.7(13) . . . . ? Cl1 C57 C58 C59 180.0(7) . . . . ? C57 C58 C59 C60 -0.7(14) . . . . ? C58 C59 C60 C61 0.1(14) . . . . ? C59 C60 C61 C62 -0.6(13) . . . . ? C58 C57 C62 C61 -2.1(13) . . . . ? Cl1 C57 C62 C61 179.6(6) . . . . ? C60 C61 C62 C57 1.5(13) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.723 _refine_diff_density_min -1.819 _refine_diff_density_rms 0.169 data_Re(NCPO-NHC)(CO)3 _database_code_depnum_ccdc_archive 'CCDC 883523' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2 (C49 H29 N4 O4 Re)' _chemical_formula_sum 'C98 H58 N8 O8 Re2' _chemical_formula_weight 1847.92 _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' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' _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 24.059(11) _cell_length_b 12.964(6) _cell_length_c 28.542(14) _cell_angle_alpha 90.00 _cell_angle_beta 93.437(5) _cell_angle_gamma 90.00 _cell_volume 8886(7) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 13502 _cell_measurement_theta_min 1.4295 _cell_measurement_theta_max 30.4847 _exptl_crystal_description block _exptl_crystal_colour violet _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3664 _exptl_absorpt_coefficient_mu 2.781 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6805 _exptl_absorpt_correction_T_max 0.8969 _exptl_absorpt_process_details "REQAB''(REQAB; Jacobson, 1998)" _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.710747 _diffrn_radiation_type MoKa _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator Confocal _diffrn_radiation_detector CCD _diffrn_measurement_device_type ? _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 88219 _diffrn_reflns_av_R_equivalents 0.0895 _diffrn_reflns_av_sigmaI/netI 0.0856 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 0.85 _diffrn_reflns_theta_max 27.50 _reflns_number_total 20404 _reflns_number_gt 12974 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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/[?^2^(Fo^2^)+(0.0900P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20404 _refine_ls_number_parameters 1047 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.1106 _refine_ls_R_factor_gt 0.0693 _refine_ls_wR_factor_ref 0.1962 _refine_ls_wR_factor_gt 0.1678 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _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 -0.3663(3) 0.5754(6) 0.0389(3) 0.0573(19) Uani 1 1 d . . . C2 C -0.3876(3) 0.4769(6) 0.0159(3) 0.0515(17) Uani 1 1 d . . . C3 C -0.3638(3) 0.4753(5) -0.0298(3) 0.0532(18) Uani 1 1 d . . . C4 C -0.3580(3) 0.3959(6) -0.0617(3) 0.0541(19) Uani 1 1 d . . . N1 N -0.3344(3) 0.4260(5) -0.1044(2) 0.0630(18) Uani 1 1 d . . . C5 C -0.3245(4) 0.3670(7) -0.1466(3) 0.071(2) Uani 1 1 d . . . C6 C -0.2883(4) 0.4291(9) -0.1719(4) 0.091(3) Uani 1 1 d . . . H1 H -0.2718 0.4083 -0.1999 0.110 Uiso 1 1 calc R . . C7 C -0.2803(5) 0.5210(9) -0.1513(4) 0.093(3) Uani 1 1 d . . . H2 H -0.2589 0.5759 -0.1629 0.111 Uiso 1 1 calc R . . C8 C -0.3084(4) 0.5233(7) -0.1098(3) 0.067(2) Uani 1 1 d . . . C9 C -0.3089(3) 0.5998(6) -0.0747(3) 0.060(2) Uani 1 1 d . . . C10 C -0.3363(3) 0.5736(6) -0.0352(3) 0.0527(18) Uani 1 1 d . . . N2 N -0.3378(3) 0.6296(5) 0.0051(2) 0.0607(17) Uani 1 1 d . . . C11 C -0.3543(4) 0.2852(8) -0.1673(3) 0.078(3) Uani 1 1 d . . . C12 C -0.3993(4) 0.2262(7) -0.1525(3) 0.066(2) Uani 1 1 d . . . C13 C -0.4376(4) 0.1726(8) -0.1833(3) 0.084(3) Uani 1 1 d . . . H3 H -0.4351 0.1646 -0.2162 0.101 Uiso 1 1 calc R . . C14 C -0.4782(4) 0.1349(8) -0.1576(3) 0.081(3) Uani 1 1 d . . . H4 H -0.5095 0.0954 -0.1688 0.098 Uiso 1 1 calc R . . C15 C -0.4649(4) 0.1662(7) -0.1100(3) 0.068(2) Uani 1 1 d . . . N3 N -0.4150(3) 0.2183(5) -0.1074(2) 0.0600(17) Uani 1 1 d . . . C16 C -0.4988(3) 0.1563(6) -0.0715(3) 0.058(2) Uani 1 1 d . . . C17 C -0.4916(3) 0.2136(6) -0.0306(3) 0.0561(19) Uani 1 1 d . . . C18 C -0.5313(3) 0.2283(7) 0.0036(3) 0.064(2) Uani 1 1 d . . . H5 H -0.5656 0.1926 0.0053 0.076 Uiso 1 1 calc R . . C19 C -0.5114(4) 0.3022(7) 0.0329(3) 0.064(2) Uani 1 1 d . . . H6 H -0.5289 0.3286 0.0594 0.077 Uiso 1 1 calc R . . C20 C -0.4595(3) 0.3334(6) 0.0169(3) 0.0520(18) Uani 1 1 d . . . N4 N -0.4465(3) 0.2775(5) -0.0203(2) 0.0509(15) Uani 1 1 d . . . C21 C -0.4269(3) 0.4198(6) 0.0366(3) 0.0500(17) Uani 1 1 d . . . O1 O -0.3709(3) 0.6072(5) 0.0778(2) 0.0754(17) Uani 1 1 d . . . C22 C -0.3057(5) 0.7212(8) 0.0183(4) 0.086(3) Uani 1 1 d . . . H7 H -0.2675 0.7129 0.0088 0.130 Uiso 1 1 calc R . . H8 H -0.3052 0.7307 0.0524 0.130 Uiso 1 1 calc R . . H9 H -0.3227 0.7816 0.0025 0.130 Uiso 1 1 calc R . . C23 C -0.2820(4) 0.7000(7) -0.0847(3) 0.063(2) Uani 1 1 d . . . C24 C -0.3151(5) 0.7854(8) -0.0916(4) 0.090(3) Uani 1 1 d . . . H10 H -0.3541 0.7792 -0.0891 0.108 Uiso 1 1 calc R . . C25 C -0.2922(5) 0.8831(10) -0.1022(5) 0.107(4) Uani 1 1 d . . . H11 H -0.3153 0.9417 -0.1080 0.128 Uiso 1 1 calc R . . C26 C -0.2345(6) 0.8894(10) -0.1038(4) 0.105(4) Uani 1 1 d . . . H12 H -0.2178 0.9546 -0.1087 0.125 Uiso 1 1 calc R . . C27 C -0.2006(5) 0.8025(9) -0.0984(5) 0.097(4) Uani 1 1 d . . . H13 H -0.1616 0.8070 -0.1017 0.117 Uiso 1 1 calc R . . C28 C -0.2257(4) 0.7081(8) -0.0879(4) 0.084(3) Uani 1 1 d . . . H14 H -0.2030 0.6486 -0.0828 0.100 Uiso 1 1 calc R . . C29 C -0.3375(5) 0.2574(9) -0.2156(4) 0.087(3) Uani 1 1 d DU . . C30 C -0.3513(7) 0.3184(13) -0.2530(5) 0.137(6) Uani 1 1 d . . . H15 H -0.3720 0.3794 -0.2481 0.165 Uiso 1 1 calc R . . C31 C -0.3360(9) 0.2954(16) -0.2996(6) 0.151(6) Uani 1 1 d U . . H16 H -0.3452 0.3375 -0.3262 0.181 Uiso 1 1 calc R . . C32 C -0.3069(7) 0.2067(16) -0.3010(6) 0.132(6) Uani 1 1 d U . . H17 H -0.2941 0.1896 -0.3309 0.159 Uiso 1 1 calc R . . C33 C -0.2934(6) 0.1393(16) -0.2670(6) 0.145(6) Uani 1 1 d U . . H18 H -0.2740 0.0770 -0.2723 0.174 Uiso 1 1 calc R . . C34 C -0.3103(5) 0.1684(12) -0.2228(5) 0.119(5) Uani 1 1 d DU . . H19 H -0.3023 0.1238 -0.1968 0.143 Uiso 1 1 calc R . . C35 C -0.5499(4) 0.0894(7) -0.0796(3) 0.068(2) Uani 1 1 d . . . C36 C -0.5441(4) -0.0165(8) -0.0768(4) 0.080(3) Uani 1 1 d . . . H20 H -0.5083 -0.0461 -0.0704 0.096 Uiso 1 1 calc R . . C37 C -0.5907(5) -0.0799(8) -0.0834(4) 0.092(3) Uani 1 1 d U . . H21 H -0.5874 -0.1525 -0.0797 0.110 Uiso 1 1 calc R . . C38 C -0.6411(4) -0.0362(10) -0.0951(4) 0.091(3) Uani 1 1 d U . . H22 H -0.6730 -0.0785 -0.1007 0.110 Uiso 1 1 calc R . . C39 C -0.6456(4) 0.0669(10) -0.0986(4) 0.093(3) Uani 1 1 d . . . H23 H -0.6811 0.0963 -0.1064 0.111 Uiso 1 1 calc R . . C40 C -0.6010(4) 0.1303(8) -0.0913(4) 0.080(3) Uani 1 1 d . . . H24 H -0.6054 0.2028 -0.0944 0.096 Uiso 1 1 calc R . . C41 C -0.4445(3) 0.4519(6) 0.0849(3) 0.0545(19) Uani 1 1 d . . . C42 C -0.4211(4) 0.4007(7) 0.1237(3) 0.073(3) Uani 1 1 d . . . H25 H -0.3944 0.3476 0.1203 0.087 Uiso 1 1 calc R . . C43 C -0.4370(5) 0.4281(11) 0.1672(4) 0.109(4) Uani 1 1 d . . . H26 H -0.4197 0.3956 0.1942 0.131 Uiso 1 1 calc R . . C44 C -0.4771(6) 0.5010(11) 0.1729(4) 0.110(4) Uani 1 1 d . . . H27 H -0.4874 0.5191 0.2035 0.133 Uiso 1 1 calc R . . C45 C -0.5021(4) 0.5472(8) 0.1348(4) 0.087(3) Uani 1 1 d . . . H28 H -0.5306 0.5967 0.1385 0.105 Uiso 1 1 calc R . . C46 C -0.4860(4) 0.5220(7) 0.0896(3) 0.073(2) Uani 1 1 d . . . H29 H -0.5039 0.5536 0.0627 0.087 Uiso 1 1 calc R . . Re1 Re -0.365447(13) 0.23572(2) -0.043912(12) 0.05595(11) Uani 1 1 d . . . C47 C -0.3735(4) 0.0905(8) -0.0296(3) 0.068(2) Uani 1 1 d . . . O2 O -0.3777(3) 0.0010(5) -0.0245(2) 0.087(2) Uani 1 1 d . . . C48 C -0.3273(4) 0.2555(6) 0.0158(4) 0.061(2) Uani 1 1 d . . . O3 O -0.3057(3) 0.2664(5) 0.0526(3) 0.086(2) Uani 1 1 d . . . C49 C -0.2968(4) 0.1975(7) -0.0688(4) 0.072(2) Uani 1 1 d . . . O4 O -0.2540(3) 0.1734(6) -0.0829(3) 0.106(3) Uani 1 1 d . . . C50 C 0.0437(4) 0.1721(7) -0.0856(3) 0.064(2) Uani 1 1 d . . . C51 C 0.0348(4) 0.1731(6) -0.0357(3) 0.060(2) Uani 1 1 d . . . C52 C -0.0173(3) 0.2288(5) -0.0301(3) 0.0509(18) Uani 1 1 d . . . C53 C -0.0361(3) 0.2824(5) 0.0081(3) 0.0534(19) Uani 1 1 d . . . N5 N -0.0910(3) 0.3240(5) -0.0015(2) 0.0547(16) Uani 1 1 d . . . C54 C -0.1247(3) 0.3841(6) 0.0293(3) 0.057(2) Uani 1 1 d . . . C55 C -0.1714(4) 0.4251(7) -0.0001(3) 0.070(2) Uani 1 1 d . . . H30 H -0.2003 0.4685 0.0098 0.084 Uiso 1 1 calc R . . C56 C -0.1654(3) 0.3884(6) -0.0454(3) 0.060(2) Uani 1 1 d . . . H31 H -0.1904 0.4019 -0.0717 0.072 Uiso 1 1 calc R . . C57 C -0.1172(3) 0.3289(6) -0.0464(3) 0.057(2) Uani 1 1 d . . . C58 C -0.0934(4) 0.2886(6) -0.0858(3) 0.061(2) Uani 1 1 d . . . C59 C -0.0417(4) 0.2423(6) -0.0759(3) 0.057(2) Uani 1 1 d . . . N6 N -0.0047(3) 0.2094(6) -0.1095(3) 0.074(2) Uani 1 1 d . . . C60 C 0.0679(3) 0.1155(6) -0.0043(3) 0.058(2) Uani 1 1 d . . . C61 C 0.0614(3) 0.0969(6) 0.0437(3) 0.059(2) Uani 1 1 d . . . C62 C 0.0847(3) 0.0094(6) 0.0702(3) 0.062(2) Uani 1 1 d . . . H32 H 0.1082 -0.0426 0.0588 0.075 Uiso 1 1 calc R . . C63 C 0.0664(4) 0.0160(7) 0.1140(3) 0.068(2) Uani 1 1 d . . . H33 H 0.0743 -0.0317 0.1388 0.082 Uiso 1 1 calc R . . C64 C 0.0332(3) 0.1071(6) 0.1165(3) 0.061(2) Uani 1 1 d . . . N7 N 0.0291(3) 0.1551(5) 0.0714(2) 0.0518(15) Uani 1 1 d . . . C65 C 0.0008(3) 0.1374(6) 0.1521(3) 0.059(2) Uani 1 1 d . . . C66 C -0.0411(4) 0.2129(6) 0.1479(3) 0.064(2) Uani 1 1 d . . . C67 C -0.0837(4) 0.2356(7) 0.1795(3) 0.067(2) Uani 1 1 d . . . H34 H -0.0872 0.2056 0.2096 0.081 Uiso 1 1 calc R . . C68 C -0.1177(4) 0.3068(7) 0.1590(3) 0.071(2) Uani 1 1 d . . . H35 H -0.1491 0.3376 0.1720 0.086 Uiso 1 1 calc R . . C69 C -0.0969(3) 0.3276(6) 0.1132(3) 0.0566(19) Uani 1 1 d . . . N8 N -0.0507(3) 0.2728(5) 0.1077(2) 0.0560(16) Uani 1 1 d . . . C70 C -0.1256(3) 0.3900(6) 0.0780(3) 0.057(2) Uani 1 1 d . . . C71 C -0.0086(7) 0.2321(12) -0.1599(5) 0.142(6) Uani 1 1 d . . . H36 H -0.0471 0.2226 -0.1723 0.213 Uiso 1 1 calc R . . H37 H 0.0159 0.1854 -0.1760 0.213 Uiso 1 1 calc R . . H38 H 0.0028 0.3036 -0.1649 0.213 Uiso 1 1 calc R . . O5 O 0.0822(4) 0.1487(9) -0.1098(4) 0.148(4) Uani 1 1 d . . . C72 C -0.1206(4) 0.2983(7) -0.1328(3) 0.068(2) Uani 1 1 d D . . C73 C -0.1199(6) 0.3901(10) -0.1574(4) 0.113(5) Uani 1 1 d D . . H39 H -0.1037 0.4491 -0.1422 0.136 Uiso 1 1 calc R . . C74 C -0.1415(6) 0.3998(13) -0.2027(4) 0.128(5) Uani 1 1 d U . . H40 H -0.1387 0.4637 -0.2187 0.153 Uiso 1 1 calc R . . C75 C -0.1669(5) 0.3180(14) -0.2248(4) 0.111(5) Uani 1 1 d U . . H41 H -0.1820 0.3235 -0.2562 0.133 Uiso 1 1 calc R . . C76 C -0.1698(5) 0.2282(12) -0.2005(5) 0.108(4) Uani 1 1 d . . . H42 H -0.1879 0.1708 -0.2154 0.129 Uiso 1 1 calc R . . C77 C -0.1474(4) 0.2165(8) -0.1541(4) 0.081(3) Uani 1 1 d D . . H43 H -0.1508 0.1530 -0.1380 0.097 Uiso 1 1 calc R . . C78 C 0.1158(3) 0.0580(7) -0.0235(3) 0.064(2) Uani 1 1 d . . . C79 C 0.1087(4) -0.0403(7) -0.0433(4) 0.073(3) Uani 1 1 d . . . H44 H 0.0722 -0.0683 -0.0476 0.088 Uiso 1 1 calc R . . C80 C 0.1534(4) -0.0971(8) -0.0566(4) 0.089(3) Uani 1 1 d . . . H45 H 0.1476 -0.1629 -0.0708 0.107 Uiso 1 1 calc R . . C81 C 0.2077(4) -0.0574(8) -0.0493(4) 0.089(3) Uani 1 1 d . . . H46 H 0.2388 -0.0968 -0.0577 0.107 Uiso 1 1 calc R . . C82 C 0.2149(4) 0.0366(10) -0.0303(4) 0.102(4) Uani 1 1 d . . . H47 H 0.2515 0.0639 -0.0257 0.122 Uiso 1 1 calc R . . C83 C 0.1696(4) 0.0952(8) -0.0171(4) 0.086(3) Uani 1 1 d . . . H48 H 0.1758 0.1614 -0.0035 0.103 Uiso 1 1 calc R . . C84 C 0.0074(4) 0.0829(7) 0.1979(4) 0.072(2) Uani 1 1 d U . . C85 C 0.0506(7) 0.1050(14) 0.2284(6) 0.171(8) Uani 1 1 d U . . H49 H 0.0761 0.1563 0.2194 0.205 Uiso 1 1 calc R . . C86 C 0.0606(9) 0.0593(16) 0.2712(7) 0.172(7) Uani 1 1 d U . . H50 H 0.0926 0.0767 0.2907 0.206 Uiso 1 1 calc R . . C87 C 0.0238(8) -0.0114(13) 0.2848(6) 0.136(6) Uani 1 1 d . . . H51 H 0.0276 -0.0402 0.3154 0.164 Uiso 1 1 calc R . . C88 C -0.0184(8) -0.0407(12) 0.2547(6) 0.138(5) Uani 1 1 d U . . H52 H -0.0423 -0.0947 0.2636 0.165 Uiso 1 1 calc R . . C89 C -0.0286(6) 0.0071(10) 0.2093(5) 0.125(5) Uani 1 1 d . . . H53 H -0.0589 -0.0133 0.1884 0.150 Uiso 1 1 calc R . . C90 C -0.1655(4) 0.4682(7) 0.0963(3) 0.062(2) Uani 1 1 d . . . C91 C -0.2195(4) 0.4433(8) 0.1072(4) 0.082(3) Uani 1 1 d . . . H54 H -0.2324 0.3744 0.1036 0.098 Uiso 1 1 calc R . . C92 C -0.2547(4) 0.5193(10) 0.1235(4) 0.088(3) Uani 1 1 d . . . H55 H -0.2916 0.5022 0.1308 0.105 Uiso 1 1 calc R . . C93 C -0.2364(5) 0.6159(9) 0.1287(4) 0.099(4) Uani 1 1 d . . . H56 H -0.2605 0.6672 0.1399 0.118 Uiso 1 1 calc R . . C94 C -0.1833(5) 0.6424(9) 0.1180(4) 0.097(3) Uani 1 1 d . . . H57 H -0.1710 0.7118 0.1215 0.117 Uiso 1 1 calc R . . C95 C -0.1477(4) 0.5684(7) 0.1022(3) 0.074(3) Uani 1 1 d . . . H58 H -0.1108 0.5867 0.0954 0.089 Uiso 1 1 calc R . . Re2 Re 0.017266(14) 0.31953(2) 0.067539(12) 0.05588(12) Uani 1 1 d . . . C96 C 0.0667(4) 0.3421(6) 0.1223(3) 0.062(2) Uani 1 1 d . . . O6 O 0.0977(3) 0.3531(6) 0.1544(3) 0.094(2) Uani 1 1 d . . . C97 C -0.0021(3) 0.4644(7) 0.0669(3) 0.064(2) Uani 1 1 d . . . O7 O -0.0117(3) 0.5501(4) 0.0670(3) 0.083(2) Uani 1 1 d . . . C98 C 0.0785(4) 0.3481(6) 0.0307(3) 0.064(2) Uani 1 1 d . . . O8 O 0.1170(3) 0.3655(5) 0.0082(3) 0.088(2) Uani 1 1 d . . . _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 0.062(5) 0.046(4) 0.064(5) -0.001(4) 0.002(4) 0.005(4) C2 0.051(4) 0.050(4) 0.053(4) 0.006(3) -0.004(3) 0.002(3) C3 0.057(5) 0.032(4) 0.071(5) 0.006(3) 0.006(4) -0.003(3) C4 0.041(4) 0.039(4) 0.080(5) 0.008(4) -0.007(4) -0.010(3) N1 0.072(5) 0.050(4) 0.070(4) -0.012(3) 0.023(3) -0.014(3) C5 0.079(6) 0.058(5) 0.077(6) -0.017(4) 0.028(5) -0.019(4) C6 0.099(8) 0.103(9) 0.075(6) -0.018(6) 0.034(6) -0.039(6) C7 0.104(8) 0.095(8) 0.083(7) 0.000(6) 0.028(6) -0.039(6) C8 0.065(5) 0.056(5) 0.080(6) -0.011(4) 0.017(4) -0.014(4) C9 0.062(5) 0.046(4) 0.075(5) -0.007(4) 0.019(4) -0.010(4) C10 0.057(5) 0.043(4) 0.057(4) -0.001(3) 0.001(4) -0.002(3) N2 0.064(4) 0.047(4) 0.071(4) -0.003(3) 0.005(3) -0.006(3) C11 0.097(7) 0.081(7) 0.059(5) -0.016(5) 0.025(5) -0.008(5) C12 0.067(6) 0.063(5) 0.071(6) -0.014(4) 0.019(4) -0.016(4) C13 0.088(7) 0.105(8) 0.062(6) -0.018(5) 0.025(5) -0.028(6) C14 0.085(7) 0.087(7) 0.072(6) -0.030(5) 0.006(5) -0.031(6) C15 0.063(5) 0.063(6) 0.080(6) -0.020(4) 0.011(4) -0.012(4) N3 0.049(4) 0.061(4) 0.072(4) -0.006(3) 0.021(3) -0.013(3) C16 0.055(5) 0.053(5) 0.067(5) -0.002(4) 0.013(4) -0.007(4) C17 0.050(5) 0.048(4) 0.070(5) -0.003(4) 0.010(4) -0.003(3) C18 0.042(4) 0.067(6) 0.082(6) -0.005(5) 0.008(4) 0.003(4) C19 0.066(5) 0.062(5) 0.066(5) -0.013(4) 0.018(4) -0.011(4) C20 0.058(5) 0.049(4) 0.050(4) 0.004(3) 0.010(3) 0.003(3) N4 0.050(4) 0.043(3) 0.061(4) -0.005(3) 0.009(3) -0.004(3) C21 0.042(4) 0.051(4) 0.057(4) -0.002(3) -0.002(3) 0.006(3) O1 0.097(5) 0.067(4) 0.063(4) -0.016(3) 0.012(3) -0.008(3) C22 0.108(8) 0.066(6) 0.087(7) -0.017(5) 0.019(6) -0.025(6) C23 0.062(5) 0.055(5) 0.075(6) -0.002(4) 0.012(4) -0.003(4) C24 0.097(8) 0.069(7) 0.106(8) 0.009(6) 0.025(6) -0.006(6) C25 0.102(9) 0.084(8) 0.138(11) 0.016(7) 0.036(8) 0.003(7) C26 0.127(11) 0.075(8) 0.113(9) 0.000(7) 0.019(8) -0.031(7) C27 0.076(7) 0.073(7) 0.146(11) -0.011(7) 0.028(7) -0.018(6) C28 0.084(7) 0.057(6) 0.112(8) -0.002(5) 0.018(6) -0.018(5) C29 0.103(8) 0.094(8) 0.066(6) -0.022(6) 0.026(6) -0.028(6) C30 0.178(15) 0.148(14) 0.089(9) -0.018(9) 0.044(10) -0.069(11) C31 0.195(14) 0.167(13) 0.089(9) 0.005(9) -0.004(10) -0.029(12) C32 0.110(10) 0.167(13) 0.125(11) -0.054(10) 0.048(9) -0.051(10) C33 0.116(10) 0.188(14) 0.131(11) -0.081(11) 0.016(9) -0.005(10) C34 0.087(8) 0.170(13) 0.104(9) -0.070(9) 0.034(7) -0.018(8) C35 0.058(5) 0.069(6) 0.077(6) -0.018(5) 0.016(4) -0.015(4) C36 0.081(7) 0.069(7) 0.092(7) 0.006(5) 0.019(5) -0.007(5) C37 0.112(9) 0.060(6) 0.104(8) -0.005(6) 0.015(7) -0.031(6) C38 0.061(6) 0.110(9) 0.105(8) -0.040(7) 0.022(5) -0.040(6) C39 0.052(6) 0.104(9) 0.123(9) -0.038(7) 0.010(5) -0.013(5) C40 0.053(5) 0.074(6) 0.112(8) -0.010(6) 0.004(5) -0.003(5) C41 0.064(5) 0.052(5) 0.048(4) -0.005(3) 0.012(4) 0.004(4) C42 0.082(6) 0.078(6) 0.059(5) 0.014(4) 0.014(4) 0.024(5) C43 0.127(10) 0.138(11) 0.065(6) 0.017(7) 0.025(6) 0.039(9) C44 0.132(11) 0.140(12) 0.060(6) -0.022(7) 0.012(7) 0.030(9) C45 0.086(7) 0.085(7) 0.094(8) -0.023(6) 0.019(6) 0.021(6) C46 0.069(6) 0.076(6) 0.072(6) -0.006(5) -0.005(4) 0.025(5) Re1 0.0531(2) 0.04438(19) 0.0716(2) -0.00584(14) 0.01423(16) -0.00174(13) C47 0.063(5) 0.063(6) 0.079(6) -0.027(5) 0.007(4) 0.015(4) O2 0.116(6) 0.048(4) 0.100(5) -0.005(3) 0.023(4) 0.005(4) C48 0.053(5) 0.055(5) 0.076(6) -0.010(4) 0.009(4) -0.005(4) O3 0.086(5) 0.067(4) 0.102(6) -0.009(4) -0.010(4) -0.007(3) C49 0.069(6) 0.050(5) 0.098(7) 0.006(5) 0.015(5) -0.005(4) O4 0.080(5) 0.089(5) 0.153(7) 0.006(5) 0.051(5) 0.016(4) C50 0.054(5) 0.059(5) 0.082(6) -0.012(4) 0.025(5) -0.004(4) C51 0.062(5) 0.048(5) 0.073(5) -0.009(4) 0.023(4) -0.009(4) C52 0.064(5) 0.033(4) 0.057(4) 0.005(3) 0.016(4) -0.002(3) C53 0.049(4) 0.027(3) 0.086(6) -0.003(3) 0.021(4) -0.011(3) N5 0.061(4) 0.041(4) 0.063(4) -0.006(3) 0.010(3) -0.009(3) C54 0.053(5) 0.044(4) 0.075(5) -0.012(4) 0.013(4) -0.003(3) C55 0.087(7) 0.053(5) 0.070(6) 0.011(4) 0.000(5) -0.010(5) C56 0.055(5) 0.062(5) 0.064(5) -0.012(4) 0.005(4) -0.007(4) C57 0.061(5) 0.052(5) 0.059(5) 0.001(4) 0.004(4) -0.011(4) C58 0.073(6) 0.047(4) 0.064(5) -0.009(4) 0.019(4) -0.013(4) C59 0.065(5) 0.043(4) 0.067(5) -0.006(4) 0.019(4) -0.013(4) N6 0.084(6) 0.071(5) 0.071(5) -0.012(4) 0.031(4) -0.018(4) C60 0.056(5) 0.038(4) 0.083(6) -0.001(4) 0.023(4) -0.007(3) C61 0.050(4) 0.049(5) 0.079(6) -0.001(4) 0.012(4) -0.006(3) C62 0.053(5) 0.044(5) 0.088(6) 0.002(4) -0.002(4) -0.003(3) C63 0.071(6) 0.052(5) 0.083(6) 0.008(4) 0.011(5) 0.002(4) C64 0.059(5) 0.052(5) 0.071(5) 0.006(4) 0.006(4) -0.007(4) N7 0.059(4) 0.041(3) 0.058(4) 0.002(3) 0.018(3) -0.003(3) C65 0.061(5) 0.045(4) 0.073(5) 0.013(4) 0.011(4) -0.003(4) C66 0.074(6) 0.047(5) 0.072(6) 0.008(4) 0.014(4) -0.009(4) C67 0.078(6) 0.068(6) 0.058(5) 0.012(4) 0.024(4) 0.011(4) C68 0.072(6) 0.062(6) 0.082(6) 0.003(5) 0.029(5) 0.004(4) C69 0.057(5) 0.051(5) 0.062(5) 0.001(4) 0.009(4) -0.004(4) N8 0.059(4) 0.047(4) 0.063(4) -0.001(3) 0.014(3) 0.004(3) C70 0.054(5) 0.045(4) 0.074(5) -0.009(4) 0.013(4) -0.007(3) C71 0.173(15) 0.165(15) 0.090(10) 0.001(9) 0.029(10) 0.002(11) O5 0.135(8) 0.187(10) 0.126(8) 0.012(7) 0.039(7) 0.016(7) C72 0.077(6) 0.068(6) 0.061(5) -0.018(4) 0.018(4) -0.017(5) C73 0.143(11) 0.129(11) 0.066(7) 0.004(7) -0.012(7) -0.061(9) C74 0.161(13) 0.146(13) 0.074(8) 0.020(8) -0.002(8) -0.046(10) C75 0.098(9) 0.190(15) 0.047(6) -0.003(7) 0.013(6) 0.015(9) C76 0.074(8) 0.145(12) 0.103(10) -0.050(9) -0.006(7) 0.019(8) C77 0.064(6) 0.082(7) 0.097(8) -0.014(6) -0.004(5) 0.012(5) C78 0.058(5) 0.054(5) 0.081(6) 0.000(4) 0.014(4) -0.001(4) C79 0.066(6) 0.046(5) 0.108(7) -0.006(5) 0.010(5) -0.003(4) C80 0.087(7) 0.061(6) 0.124(9) -0.007(6) 0.039(7) 0.003(5) C81 0.068(6) 0.065(6) 0.137(10) -0.018(6) 0.027(6) 0.012(5) C82 0.054(6) 0.111(10) 0.144(11) -0.026(8) 0.033(6) -0.008(6) C83 0.060(6) 0.080(7) 0.121(8) -0.029(6) 0.029(6) -0.016(5) C84 0.082(6) 0.052(5) 0.083(6) 0.008(5) 0.016(5) 0.004(4) C85 0.187(17) 0.165(16) 0.152(14) 0.074(12) -0.064(12) -0.084(13) C86 0.182(10) 0.175(10) 0.155(10) 0.022(8) -0.018(8) -0.020(9) C87 0.173(17) 0.125(13) 0.111(11) 0.028(10) 0.015(11) 0.052(12) C88 0.170(13) 0.115(10) 0.133(11) 0.051(9) 0.041(10) 0.004(10) C89 0.153(13) 0.095(10) 0.126(11) 0.047(8) 0.009(9) -0.008(9) C90 0.063(5) 0.059(5) 0.063(5) 0.001(4) 0.002(4) 0.006(4) C91 0.066(6) 0.064(6) 0.117(8) 0.012(6) 0.018(6) 0.003(5) C92 0.057(6) 0.104(9) 0.103(8) -0.005(7) 0.010(5) 0.032(6) C93 0.114(10) 0.079(8) 0.107(9) -0.013(6) 0.036(7) 0.028(7) C94 0.120(10) 0.066(7) 0.109(9) -0.008(6) 0.034(7) 0.011(6) C95 0.089(7) 0.054(5) 0.080(6) -0.013(5) 0.012(5) 0.007(5) Re2 0.0600(2) 0.04044(18) 0.0685(2) -0.00009(14) 0.01457(16) -0.00753(13) C96 0.058(5) 0.051(5) 0.077(6) -0.010(4) 0.004(4) -0.005(4) O6 0.097(5) 0.089(5) 0.092(5) -0.008(4) -0.015(4) -0.010(4) C97 0.051(5) 0.068(6) 0.074(6) 0.007(4) 0.002(4) -0.009(4) O7 0.085(5) 0.031(3) 0.135(6) 0.005(3) 0.014(4) -0.005(3) C98 0.063(5) 0.048(5) 0.080(6) -0.001(4) -0.003(4) -0.005(4) O8 0.070(4) 0.085(5) 0.114(5) 0.000(4) 0.041(4) -0.021(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; _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 1.195(9) . ? C1 N2 1.405(10) . ? C1 C2 1.511(11) . ? C2 C21 1.364(10) . ? C2 C3 1.455(10) . ? C3 C4 1.388(11) . ? C3 C10 1.449(10) . ? C4 N1 1.429(10) . ? C4 Re1 2.148(7) . ? N1 C8 1.421(10) . ? N1 C5 1.458(10) . ? C5 C11 1.392(13) . ? C5 C6 1.417(12) . ? C6 C7 1.337(14) . ? C6 H1 0.9500 . ? C7 C8 1.398(12) . ? C7 H2 0.9500 . ? C8 C9 1.411(11) . ? C9 C10 1.380(10) . ? C9 C23 1.487(11) . ? C10 N2 1.364(10) . ? N2 C22 1.453(11) . ? C11 C12 1.411(12) . ? C11 C29 1.504(12) . ? C12 N3 1.369(10) . ? C12 C13 1.417(13) . ? C13 C14 1.347(12) . ? C13 H3 0.9500 . ? C14 C15 1.436(12) . ? C14 H4 0.9500 . ? C15 N3 1.376(10) . ? C15 C16 1.413(11) . ? N3 Re1 2.120(7) . ? C16 C17 1.387(11) . ? C16 C35 1.512(11) . ? C17 N4 1.383(10) . ? C17 C18 1.418(11) . ? C18 C19 1.342(12) . ? C18 H5 0.9500 . ? C19 C20 1.415(11) . ? C19 H6 0.9500 . ? C20 N4 1.338(9) . ? C20 C21 1.461(11) . ? N4 Re1 2.170(6) . ? C21 C41 1.522(10) . ? C22 H7 0.9800 . ? C22 H8 0.9800 . ? C22 H9 0.9800 . ? C23 C28 1.368(13) . ? C23 C24 1.371(14) . ? C24 C25 1.420(15) . ? C24 H10 0.9500 . ? C25 C26 1.394(16) . ? C25 H11 0.9500 . ? C26 C27 1.393(16) . ? C26 H12 0.9500 . ? C27 C28 1.405(14) . ? C27 H13 0.9500 . ? C28 H14 0.9500 . ? C29 C34 1.347(15) . ? C29 C30 1.354(18) . ? C30 C31 1.43(2) . ? C30 H15 0.9500 . ? C31 C32 1.35(2) . ? C31 H16 0.9500 . ? C32 C33 1.33(2) . ? C32 H17 0.9500 . ? C33 C34 1.402(17) . ? C33 H18 0.9500 . ? C34 H19 0.9500 . ? C35 C40 1.360(13) . ? C35 C36 1.383(13) . ? C36 C37 1.395(14) . ? C36 H20 0.9500 . ? C37 C38 1.360(16) . ? C37 H21 0.9500 . ? C38 C39 1.344(16) . ? C38 H22 0.9500 . ? C39 C40 1.358(13) . ? C39 H23 0.9500 . ? C40 H24 0.9500 . ? C41 C46 1.364(11) . ? C41 C42 1.383(11) . ? C42 C43 1.369(13) . ? C42 H25 0.9500 . ? C43 C44 1.368(15) . ? C43 H26 0.9500 . ? C44 C45 1.351(15) . ? C44 H27 0.9500 . ? C45 C46 1.405(13) . ? C45 H28 0.9500 . ? C46 H29 0.9500 . ? Re1 C49 1.902(10) . ? Re1 C48 1.905(10) . ? Re1 C47 1.939(11) . ? C47 O2 1.174(11) . ? C48 O3 1.150(11) . ? C49 O4 1.170(10) . ? C50 O5 1.225(11) . ? C50 N6 1.401(12) . ? C50 C51 1.454(12) . ? C51 C60 1.381(12) . ? C51 C52 1.463(11) . ? C52 C53 1.392(10) . ? C52 C59 1.411(12) . ? C53 N5 1.437(10) . ? C53 Re2 2.121(9) . ? N5 C57 1.395(10) . ? N5 C54 1.458(9) . ? C54 C70 1.394(11) . ? C54 C55 1.460(12) . ? C55 C56 1.394(12) . ? C55 H30 0.9500 . ? C56 C57 1.395(11) . ? C56 H31 0.9500 . ? C57 C58 1.392(11) . ? C58 C59 1.396(12) . ? C58 C72 1.462(13) . ? C59 N6 1.413(10) . ? N6 C71 1.464(15) . ? C60 C61 1.410(11) . ? C60 C78 1.505(11) . ? C61 N7 1.367(9) . ? C61 C62 1.457(11) . ? C62 C63 1.352(12) . ? C62 H32 0.9500 . ? C63 C64 1.431(11) . ? C63 H33 0.9500 . ? C64 C65 1.374(11) . ? C64 N7 1.429(10) . ? N7 Re2 2.153(6) . ? C65 C66 1.405(12) . ? C65 C84 1.487(12) . ? C66 N8 1.392(11) . ? C66 C67 1.435(11) . ? C67 C68 1.344(12) . ? C67 H34 0.9500 . ? C68 C69 1.453(11) . ? C68 H35 0.9500 . ? C69 N8 1.337(10) . ? C69 C70 1.434(12) . ? N8 Re2 2.141(6) . ? C70 C90 1.511(11) . ? C71 H36 0.9800 . ? C71 H37 0.9800 . ? C71 H38 0.9800 . ? C72 C77 1.365(11) . ? C72 C73 1.383(12) . ? C73 C74 1.370(15) . ? C73 H39 0.9500 . ? C74 C75 1.360(18) . ? C74 H40 0.9500 . ? C75 C76 1.360(18) . ? C75 H41 0.9500 . ? C76 C77 1.407(16) . ? C76 H42 0.9500 . ? C77 H43 0.9500 . ? C78 C83 1.382(12) . ? C78 C79 1.401(12) . ? C79 C80 1.375(12) . ? C79 H44 0.9500 . ? C80 C81 1.408(14) . ? C80 H45 0.9500 . ? C81 C82 1.341(14) . ? C81 H46 0.9500 . ? C82 C83 1.399(13) . ? C82 H47 0.9500 . ? C83 H48 0.9500 . ? C84 C85 1.346(17) . ? C84 C89 1.361(15) . ? C85 C86 1.37(2) . ? C85 H49 0.9500 . ? C86 C87 1.35(2) . ? C86 H50 0.9500 . ? C87 C88 1.35(2) . ? C87 H51 0.9500 . ? C88 C89 1.444(18) . ? C88 H52 0.9500 . ? C89 H53 0.9500 . ? C90 C95 1.374(12) . ? C90 C91 1.391(12) . ? C91 C92 1.397(13) . ? C91 H54 0.9500 . ? C92 C93 1.332(15) . ? C92 H55 0.9500 . ? C93 C94 1.377(16) . ? C93 H56 0.9500 . ? C94 C95 1.378(13) . ? C94 H57 0.9500 . ? C95 H58 0.9500 . ? Re2 C98 1.896(9) . ? Re2 C96 1.928(10) . ? Re2 C97 1.935(10) . ? C96 O6 1.156(10) . ? C97 O7 1.135(10) . ? C98 O8 1.181(10) . ? _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 N2 122.7(8) . . ? O1 C1 C2 130.4(8) . . ? N2 C1 C2 106.9(7) . . ? C21 C2 C3 134.6(7) . . ? C21 C2 C1 119.7(7) . . ? C3 C2 C1 105.1(6) . . ? C4 C3 C10 121.2(7) . . ? C4 C3 C2 131.3(7) . . ? C10 C3 C2 106.9(7) . . ? C3 C4 N1 114.7(6) . . ? C3 C4 Re1 123.3(6) . . ? N1 C4 Re1 120.6(6) . . ? C8 N1 C4 122.3(7) . . ? C8 N1 C5 106.4(6) . . ? C4 N1 C5 130.8(7) . . ? C11 C5 C6 122.3(8) . . ? C11 C5 N1 130.2(7) . . ? C6 C5 N1 105.0(7) . . ? C7 C6 C5 111.0(9) . . ? C7 C6 H1 124.5 . . ? C5 C6 H1 124.5 . . ? C6 C7 C8 109.2(9) . . ? C6 C7 H2 125.4 . . ? C8 C7 H2 125.4 . . ? C7 C8 C9 129.9(8) . . ? C7 C8 N1 108.1(8) . . ? C9 C8 N1 121.7(7) . . ? C10 C9 C8 115.6(7) . . ? C10 C9 C23 127.4(7) . . ? C8 C9 C23 117.0(7) . . ? N2 C10 C9 126.6(7) . . ? N2 C10 C3 110.0(7) . . ? C9 C10 C3 123.2(7) . . ? C10 N2 C1 110.6(6) . . ? C10 N2 C22 127.7(7) . . ? C1 N2 C22 120.4(7) . . ? C5 C11 C12 132.2(8) . . ? C5 C11 C29 114.3(8) . . ? C12 C11 C29 113.4(8) . . ? N3 C12 C11 125.6(8) . . ? N3 C12 C13 110.0(7) . . ? C11 C12 C13 124.3(8) . . ? C14 C13 C12 107.8(8) . . ? C14 C13 H3 126.1 . . ? C12 C13 H3 126.1 . . ? C13 C14 C15 106.5(8) . . ? C13 C14 H4 126.7 . . ? C15 C14 H4 126.7 . . ? N3 C15 C16 122.9(8) . . ? N3 C15 C14 109.6(8) . . ? C16 C15 C14 127.2(8) . . ? C12 N3 C15 105.8(7) . . ? C12 N3 Re1 128.6(6) . . ? C15 N3 Re1 122.9(6) . . ? C17 C16 C15 124.0(7) . . ? C17 C16 C35 119.6(7) . . ? C15 C16 C35 115.8(7) . . ? N4 C17 C16 123.7(7) . . ? N4 C17 C18 109.1(7) . . ? C16 C17 C18 126.6(8) . . ? C19 C18 C17 107.1(7) . . ? C19 C18 H5 126.4 . . ? C17 C18 H5 126.4 . . ? C18 C19 C20 107.0(7) . . ? C18 C19 H6 126.5 . . ? C20 C19 H6 126.5 . . ? N4 C20 C19 110.8(7) . . ? N4 C20 C21 125.1(7) . . ? C19 C20 C21 124.0(7) . . ? C20 N4 C17 105.9(6) . . ? C20 N4 Re1 129.7(5) . . ? C17 N4 Re1 119.6(5) . . ? C2 C21 C20 128.3(7) . . ? C2 C21 C41 118.8(7) . . ? C20 C21 C41 112.7(6) . . ? N2 C22 H7 109.5 . . ? N2 C22 H8 109.5 . . ? H7 C22 H8 109.5 . . ? N2 C22 H9 109.5 . . ? H7 C22 H9 109.5 . . ? H8 C22 H9 109.5 . . ? C28 C23 C24 119.9(9) . . ? C28 C23 C9 121.6(8) . . ? C24 C23 C9 118.5(9) . . ? C23 C24 C25 121.4(11) . . ? C23 C24 H10 119.3 . . ? C25 C24 H10 119.3 . . ? C26 C25 C24 117.3(11) . . ? C26 C25 H11 121.3 . . ? C24 C25 H11 121.3 . . ? C27 C26 C25 121.7(11) . . ? C27 C26 H12 119.1 . . ? C25 C26 H12 119.1 . . ? C26 C27 C28 118.2(11) . . ? C26 C27 H13 120.9 . . ? C28 C27 H13 120.9 . . ? C23 C28 C27 121.3(10) . . ? C23 C28 H14 119.3 . . ? C27 C28 H14 119.3 . . ? C34 C29 C30 118.6(12) . . ? C34 C29 C11 120.3(11) . . ? C30 C29 C11 121.1(12) . . ? C29 C30 C31 123.1(17) . . ? C29 C30 H15 118.4 . . ? C31 C30 H15 118.4 . . ? C32 C31 C30 111.6(16) . . ? C32 C31 H16 124.2 . . ? C30 C31 H16 124.2 . . ? C33 C32 C31 130.0(16) . . ? C33 C32 H17 115.0 . . ? C31 C32 H17 115.0 . . ? C32 C33 C34 114.1(17) . . ? C32 C33 H18 122.9 . . ? C34 C33 H18 122.9 . . ? C29 C34 C33 122.5(16) . . ? C29 C34 H19 118.8 . . ? C33 C34 H19 118.8 . . ? C40 C35 C36 119.2(9) . . ? C40 C35 C16 122.0(9) . . ? C36 C35 C16 118.8(9) . . ? C35 C36 C37 119.9(10) . . ? C35 C36 H20 120.0 . . ? C37 C36 H20 120.0 . . ? C38 C37 C36 119.0(10) . . ? C38 C37 H21 120.5 . . ? C36 C37 H21 120.5 . . ? C39 C38 C37 120.0(9) . . ? C39 C38 H22 120.0 . . ? C37 C38 H22 120.0 . . ? C38 C39 C40 122.0(11) . . ? C38 C39 H23 119.0 . . ? C40 C39 H23 119.0 . . ? C39 C40 C35 119.7(10) . . ? C39 C40 H24 120.1 . . ? C35 C40 H24 120.1 . . ? C46 C41 C42 120.3(8) . . ? C46 C41 C21 121.2(7) . . ? C42 C41 C21 118.1(7) . . ? C43 C42 C41 118.7(9) . . ? C43 C42 H25 120.6 . . ? C41 C42 H25 120.6 . . ? C44 C43 C42 121.6(11) . . ? C44 C43 H26 119.2 . . ? C42 C43 H26 119.2 . . ? C45 C44 C43 119.6(10) . . ? C45 C44 H27 120.2 . . ? C43 C44 H27 120.2 . . ? C44 C45 C46 120.1(9) . . ? C44 C45 H28 119.9 . . ? C46 C45 H28 119.9 . . ? C41 C46 C45 119.3(9) . . ? C41 C46 H29 120.3 . . ? C45 C46 H29 120.3 . . ? C49 Re1 C48 89.3(4) . . ? C49 Re1 C47 85.8(4) . . ? C48 Re1 C47 89.5(4) . . ? C49 Re1 N3 96.3(4) . . ? C48 Re1 N3 174.5(3) . . ? C47 Re1 N3 91.0(3) . . ? C49 Re1 C4 94.4(3) . . ? C48 Re1 C4 92.2(3) . . ? C47 Re1 C4 178.2(3) . . ? N3 Re1 C4 87.2(3) . . ? C49 Re1 N4 176.0(4) . . ? C48 Re1 N4 94.7(3) . . ? C47 Re1 N4 94.2(3) . . ? N3 Re1 N4 79.7(2) . . ? C4 Re1 N4 85.5(3) . . ? O2 C47 Re1 174.8(8) . . ? O3 C48 Re1 177.9(8) . . ? O4 C49 Re1 178.2(10) . . ? O5 C50 N6 116.5(10) . . ? O5 C50 C51 135.6(10) . . ? N6 C50 C51 107.9(7) . . ? C60 C51 C50 121.2(8) . . ? C60 C51 C52 131.3(7) . . ? C50 C51 C52 106.8(8) . . ? C53 C52 C59 121.7(7) . . ? C53 C52 C51 130.8(8) . . ? C59 C52 C51 105.8(7) . . ? C52 C53 N5 112.1(7) . . ? C52 C53 Re2 122.0(6) . . ? N5 C53 Re2 125.0(5) . . ? C57 N5 C53 123.5(7) . . ? C57 N5 C54 107.0(7) . . ? C53 N5 C54 128.6(7) . . ? C70 C54 N5 132.3(8) . . ? C70 C54 C55 119.7(7) . . ? N5 C54 C55 106.6(7) . . ? C56 C55 C54 106.7(8) . . ? C56 C55 H30 126.6 . . ? C54 C55 H30 126.6 . . ? C55 C56 C57 110.0(8) . . ? C55 C56 H31 125.0 . . ? C57 C56 H31 125.0 . . ? C58 C57 C56 127.3(8) . . ? C58 C57 N5 122.6(8) . . ? C56 C57 N5 109.6(7) . . ? C57 C58 C59 113.7(8) . . ? C57 C58 C72 121.7(8) . . ? C59 C58 C72 124.5(7) . . ? C58 C59 C52 123.9(7) . . ? C58 C59 N6 125.6(8) . . ? C52 C59 N6 110.4(8) . . ? C50 N6 C59 108.2(8) . . ? C50 N6 C71 123.3(9) . . ? C59 N6 C71 127.0(10) . . ? C51 C60 C61 129.1(7) . . ? C51 C60 C78 117.1(8) . . ? C61 C60 C78 113.7(8) . . ? N7 C61 C60 124.5(8) . . ? N7 C61 C62 110.1(7) . . ? C60 C61 C62 125.2(8) . . ? C63 C62 C61 107.1(8) . . ? C63 C62 H32 126.4 . . ? C61 C62 H32 126.4 . . ? C62 C63 C64 108.2(8) . . ? C62 C63 H33 125.9 . . ? C64 C63 H33 125.9 . . ? C65 C64 N7 122.0(7) . . ? C65 C64 C63 128.1(8) . . ? N7 C64 C63 108.8(7) . . ? C61 N7 C64 105.6(7) . . ? C61 N7 Re2 126.5(5) . . ? C64 N7 Re2 118.6(5) . . ? C64 C65 C66 124.9(8) . . ? C64 C65 C84 118.6(8) . . ? C66 C65 C84 116.3(8) . . ? N8 C66 C65 122.8(8) . . ? N8 C66 C67 108.3(8) . . ? C65 C66 C67 128.6(8) . . ? C68 C67 C66 107.8(8) . . ? C68 C67 H34 126.1 . . ? C66 C67 H34 126.1 . . ? C67 C68 C69 106.6(7) . . ? C67 C68 H35 126.7 . . ? C69 C68 H35 126.7 . . ? N8 C69 C70 125.9(7) . . ? N8 C69 C68 109.9(7) . . ? C70 C69 C68 124.0(8) . . ? C69 N8 C66 107.4(7) . . ? C69 N8 Re2 125.4(5) . . ? C66 N8 Re2 120.3(5) . . ? C54 C70 C69 129.3(7) . . ? C54 C70 C90 115.4(7) . . ? C69 C70 C90 115.2(7) . . ? N6 C71 H36 109.5 . . ? N6 C71 H37 109.5 . . ? H36 C71 H37 109.5 . . ? N6 C71 H38 109.5 . . ? H36 C71 H38 109.5 . . ? H37 C71 H38 109.5 . . ? C77 C72 C73 117.5(10) . . ? C77 C72 C58 121.0(9) . . ? C73 C72 C58 121.5(8) . . ? C74 C73 C72 122.9(12) . . ? C74 C73 H39 118.6 . . ? C72 C73 H39 118.6 . . ? C75 C74 C73 120.1(13) . . ? C75 C74 H40 119.9 . . ? C73 C74 H40 119.9 . . ? C74 C75 C76 117.7(12) . . ? C74 C75 H41 121.1 . . ? C76 C75 H41 121.1 . . ? C75 C76 C77 122.9(13) . . ? C75 C76 H42 118.5 . . ? C77 C76 H42 118.5 . . ? C72 C77 C76 118.7(11) . . ? C72 C77 H43 120.6 . . ? C76 C77 H43 120.6 . . ? C83 C78 C79 117.5(8) . . ? C83 C78 C60 120.7(8) . . ? C79 C78 C60 121.3(8) . . ? C80 C79 C78 121.3(9) . . ? C80 C79 H44 119.4 . . ? C78 C79 H44 119.4 . . ? C79 C80 C81 119.8(10) . . ? C79 C80 H45 120.1 . . ? C81 C80 H45 120.1 . . ? C82 C81 C80 119.4(9) . . ? C82 C81 H46 120.3 . . ? C80 C81 H46 120.3 . . ? C81 C82 C83 121.1(10) . . ? C81 C82 H47 119.4 . . ? C83 C82 H47 119.4 . . ? C78 C83 C82 120.9(9) . . ? C78 C83 H48 119.5 . . ? C82 C83 H48 119.5 . . ? C85 C84 C89 118.6(12) . . ? C85 C84 C65 120.3(10) . . ? C89 C84 C65 121.1(10) . . ? C84 C85 C86 124.9(16) . . ? C84 C85 H49 117.5 . . ? C86 C85 H49 117.5 . . ? C87 C86 C85 118.0(18) . . ? C87 C86 H50 121.0 . . ? C85 C86 H50 121.0 . . ? C88 C87 C86 119.5(17) . . ? C88 C87 H51 120.3 . . ? C86 C87 H51 120.3 . . ? C87 C88 C89 122.3(15) . . ? C87 C88 H52 118.9 . . ? C89 C88 H52 118.9 . . ? C84 C89 C88 116.5(14) . . ? C84 C89 H53 121.8 . . ? C88 C89 H53 121.8 . . ? C95 C90 C91 118.6(8) . . ? C95 C90 C70 118.5(8) . . ? C91 C90 C70 122.9(8) . . ? C90 C91 C92 120.2(10) . . ? C90 C91 H54 119.9 . . ? C92 C91 H54 119.9 . . ? C93 C92 C91 119.8(10) . . ? C93 C92 H55 120.1 . . ? C91 C92 H55 120.1 . . ? C92 C93 C94 121.0(10) . . ? C92 C93 H56 119.5 . . ? C94 C93 H56 119.5 . . ? C93 C94 C95 120.1(11) . . ? C93 C94 H57 120.0 . . ? C95 C94 H57 120.0 . . ? C90 C95 C94 120.3(10) . . ? C90 C95 H58 119.9 . . ? C94 C95 H58 119.9 . . ? C98 Re2 C96 87.6(4) . . ? C98 Re2 C97 90.0(4) . . ? C96 Re2 C97 89.8(4) . . ? C98 Re2 C53 93.1(3) . . ? C96 Re2 C53 175.6(3) . . ? C97 Re2 C53 94.5(3) . . ? C98 Re2 N8 174.8(3) . . ? C96 Re2 N8 93.6(3) . . ? C97 Re2 N8 95.1(3) . . ? C53 Re2 N8 85.4(3) . . ? C98 Re2 N7 96.7(3) . . ? C96 Re2 N7 92.1(3) . . ? C97 Re2 N7 173.1(3) . . ? C53 Re2 N7 83.6(3) . . ? N8 Re2 N7 78.2(2) . . ? O6 C96 Re2 177.4(8) . . ? O7 C97 Re2 177.8(8) . . ? O8 C98 Re2 179.2(9) . . ? _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C21 14.3(13) . . . . ? N2 C1 C2 C21 -165.7(7) . . . . ? O1 C1 C2 C3 -173.7(9) . . . . ? N2 C1 C2 C3 6.3(8) . . . . ? C21 C2 C3 C4 -26.2(15) . . . . ? C1 C2 C3 C4 163.6(8) . . . . ? C21 C2 C3 C10 163.4(8) . . . . ? C1 C2 C3 C10 -6.8(8) . . . . ? C10 C3 C4 N1 -13.5(11) . . . . ? C2 C3 C4 N1 177.3(8) . . . . ? C10 C3 C4 Re1 153.0(6) . . . . ? C2 C3 C4 Re1 -16.3(12) . . . . ? C3 C4 N1 C8 12.4(11) . . . . ? Re1 C4 N1 C8 -154.4(6) . . . . ? C3 C4 N1 C5 -176.4(9) . . . . ? Re1 C4 N1 C5 16.8(12) . . . . ? C8 N1 C5 C11 -155.6(11) . . . . ? C4 N1 C5 C11 32.2(17) . . . . ? C8 N1 C5 C6 6.2(11) . . . . ? C4 N1 C5 C6 -166.1(9) . . . . ? C11 C5 C6 C7 157.8(11) . . . . ? N1 C5 C6 C7 -5.8(13) . . . . ? C5 C6 C7 C8 3.0(15) . . . . ? C6 C7 C8 C9 174.6(11) . . . . ? C6 C7 C8 N1 1.1(13) . . . . ? C4 N1 C8 C7 168.4(8) . . . . ? C5 N1 C8 C7 -4.6(11) . . . . ? C4 N1 C8 C9 -5.7(13) . . . . ? C5 N1 C8 C9 -178.8(9) . . . . ? C7 C8 C9 C10 -173.1(11) . . . . ? N1 C8 C9 C10 -0.4(13) . . . . ? C7 C8 C9 C23 9.1(16) . . . . ? N1 C8 C9 C23 -178.1(8) . . . . ? C8 C9 C10 N2 173.1(8) . . . . ? C23 C9 C10 N2 -9.4(15) . . . . ? C8 C9 C10 C3 -0.9(13) . . . . ? C23 C9 C10 C3 176.6(8) . . . . ? C4 C3 C10 N2 -166.4(7) . . . . ? C2 C3 C10 N2 5.1(9) . . . . ? C4 C3 C10 C9 8.4(13) . . . . ? C2 C3 C10 C9 180.0(8) . . . . ? C9 C10 N2 C1 -175.6(8) . . . . ? C3 C10 N2 C1 -1.0(9) . . . . ? C9 C10 N2 C22 -8.8(14) . . . . ? C3 C10 N2 C22 165.8(9) . . . . ? O1 C1 N2 C10 176.7(8) . . . . ? C2 C1 N2 C10 -3.3(9) . . . . ? O1 C1 N2 C22 8.7(13) . . . . ? C2 C1 N2 C22 -171.3(8) . . . . ? C6 C5 C11 C12 -166.5(12) . . . . ? N1 C5 C11 C12 -8(2) . . . . ? C6 C5 C11 C29 10.0(16) . . . . ? N1 C5 C11 C29 169.1(10) . . . . ? C5 C11 C12 N3 -19.0(19) . . . . ? C29 C11 C12 N3 164.4(10) . . . . ? C5 C11 C12 C13 155.8(12) . . . . ? C29 C11 C12 C13 -20.8(16) . . . . ? N3 C12 C13 C14 2.4(13) . . . . ? C11 C12 C13 C14 -173.1(10) . . . . ? C12 C13 C14 C15 0.2(13) . . . . ? C13 C14 C15 N3 -2.7(12) . . . . ? C13 C14 C15 C16 171.2(10) . . . . ? C11 C12 N3 C15 171.4(10) . . . . ? C13 C12 N3 C15 -4.0(11) . . . . ? C11 C12 N3 Re1 -26.7(14) . . . . ? C13 C12 N3 Re1 157.9(7) . . . . ? C16 C15 N3 C12 -170.2(9) . . . . ? C14 C15 N3 C12 4.1(11) . . . . ? C16 C15 N3 Re1 26.7(12) . . . . ? C14 C15 N3 Re1 -159.1(7) . . . . ? N3 C15 C16 C17 13.4(15) . . . . ? C14 C15 C16 C17 -159.9(10) . . . . ? N3 C15 C16 C35 -175.4(8) . . . . ? C14 C15 C16 C35 11.4(15) . . . . ? C15 C16 C17 N4 -8.5(14) . . . . ? C35 C16 C17 N4 -179.4(8) . . . . ? C15 C16 C17 C18 162.0(9) . . . . ? C35 C16 C17 C18 -8.9(14) . . . . ? N4 C17 C18 C19 2.1(10) . . . . ? C16 C17 C18 C19 -169.5(9) . . . . ? C17 C18 C19 C20 0.1(10) . . . . ? C18 C19 C20 N4 -2.3(10) . . . . ? C18 C19 C20 C21 173.6(8) . . . . ? C19 C20 N4 C17 3.5(9) . . . . ? C21 C20 N4 C17 -172.4(7) . . . . ? C19 C20 N4 Re1 -151.2(6) . . . . ? C21 C20 N4 Re1 33.0(11) . . . . ? C16 C17 N4 C20 168.5(8) . . . . ? C18 C17 N4 C20 -3.4(9) . . . . ? C16 C17 N4 Re1 -33.8(11) . . . . ? C18 C17 N4 Re1 154.3(6) . . . . ? C3 C2 C21 C20 -0.5(14) . . . . ? C1 C2 C21 C20 168.6(7) . . . . ? C3 C2 C21 C41 -174.6(8) . . . . ? C1 C2 C21 C41 -5.5(11) . . . . ? N4 C20 C21 C2 18.7(13) . . . . ? C19 C20 C21 C2 -156.6(8) . . . . ? N4 C20 C21 C41 -166.9(7) . . . . ? C19 C20 C21 C41 17.8(11) . . . . ? C10 C9 C23 C28 114.3(11) . . . . ? C8 C9 C23 C28 -68.3(13) . . . . ? C10 C9 C23 C24 -66.6(14) . . . . ? C8 C9 C23 C24 110.9(10) . . . . ? C28 C23 C24 C25 0.4(17) . . . . ? C9 C23 C24 C25 -178.8(10) . . . . ? C23 C24 C25 C26 -2.2(19) . . . . ? C24 C25 C26 C27 4(2) . . . . ? C25 C26 C27 C28 -4(2) . . . . ? C24 C23 C28 C27 -0.5(17) . . . . ? C9 C23 C28 C27 178.6(10) . . . . ? C26 C27 C28 C23 2.5(18) . . . . ? C5 C11 C29 C34 109.8(13) . . . . ? C12 C11 C29 C34 -73.0(15) . . . . ? C5 C11 C29 C30 -73.1(15) . . . . ? C12 C11 C29 C30 104.1(13) . . . . ? C34 C29 C30 C31 -3(2) . . . . ? C11 C29 C30 C31 179.7(13) . . . . ? C29 C30 C31 C32 0(2) . . . . ? C30 C31 C32 C33 3(3) . . . . ? C31 C32 C33 C34 -3(3) . . . . ? C30 C29 C34 C33 3(2) . . . . ? C11 C29 C34 C33 -179.6(12) . . . . ? C32 C33 C34 C29 0(2) . . . . ? C17 C16 C35 C40 74.4(12) . . . . ? C15 C16 C35 C40 -97.3(11) . . . . ? C17 C16 C35 C36 -108.3(10) . . . . ? C15 C16 C35 C36 80.1(11) . . . . ? C40 C35 C36 C37 -3.6(15) . . . . ? C16 C35 C36 C37 179.0(9) . . . . ? C35 C36 C37 C38 3.6(16) . . . . ? C36 C37 C38 C39 -2.2(17) . . . . ? C37 C38 C39 C40 0.8(18) . . . . ? C38 C39 C40 C35 -0.7(18) . . . . ? C36 C35 C40 C39 2.2(15) . . . . ? C16 C35 C40 C39 179.5(9) . . . . ? C2 C21 C41 C46 87.1(10) . . . . ? C20 C21 C41 C46 -87.9(10) . . . . ? C2 C21 C41 C42 -99.0(10) . . . . ? C20 C21 C41 C42 86.0(9) . . . . ? C46 C41 C42 C43 -5.4(15) . . . . ? C21 C41 C42 C43 -179.3(10) . . . . ? C41 C42 C43 C44 3.0(19) . . . . ? C42 C43 C44 C45 0(2) . . . . ? C43 C44 C45 C46 -1(2) . . . . ? C42 C41 C46 C45 4.4(15) . . . . ? C21 C41 C46 C45 178.1(9) . . . . ? C44 C45 C46 C41 -0.9(17) . . . . ? C12 N3 Re1 C49 -26.4(8) . . . . ? C15 N3 Re1 C49 132.7(7) . . . . ? C12 N3 Re1 C47 -112.3(8) . . . . ? C15 N3 Re1 C47 46.9(7) . . . . ? C12 N3 Re1 C4 67.7(8) . . . . ? C15 N3 Re1 C4 -133.2(7) . . . . ? C12 N3 Re1 N4 153.6(8) . . . . ? C15 N3 Re1 N4 -47.2(6) . . . . ? C3 C4 Re1 C49 -128.6(7) . . . . ? N1 C4 Re1 C49 37.0(7) . . . . ? C3 C4 Re1 C48 -39.2(7) . . . . ? N1 C4 Re1 C48 126.5(6) . . . . ? C3 C4 Re1 N3 135.3(6) . . . . ? N1 C4 Re1 N3 -59.1(6) . . . . ? C3 C4 Re1 N4 55.4(6) . . . . ? N1 C4 Re1 N4 -139.0(6) . . . . ? C20 N4 Re1 C48 21.5(7) . . . . ? C17 N4 Re1 C48 -130.2(6) . . . . ? C20 N4 Re1 C47 111.4(7) . . . . ? C17 N4 Re1 C47 -40.3(6) . . . . ? C20 N4 Re1 N3 -158.3(7) . . . . ? C17 N4 Re1 N3 50.0(6) . . . . ? C20 N4 Re1 C4 -70.4(7) . . . . ? C17 N4 Re1 C4 137.9(6) . . . . ? O5 C50 C51 C60 -19.4(17) . . . . ? N6 C50 C51 C60 161.9(7) . . . . ? O5 C50 C51 C52 169.3(12) . . . . ? N6 C50 C51 C52 -9.4(9) . . . . ? C60 C51 C52 C53 34.7(14) . . . . ? C50 C51 C52 C53 -155.2(8) . . . . ? C60 C51 C52 C59 -160.1(8) . . . . ? C50 C51 C52 C59 10.0(8) . . . . ? C59 C52 C53 N5 18.2(10) . . . . ? C51 C52 C53 N5 -178.7(7) . . . . ? C59 C52 C53 Re2 -151.3(6) . . . . ? C51 C52 C53 Re2 11.8(11) . . . . ? C52 C53 N5 C57 -12.5(9) . . . . ? Re2 C53 N5 C57 156.6(6) . . . . ? C52 C53 N5 C54 179.8(7) . . . . ? Re2 C53 N5 C54 -11.1(10) . . . . ? C57 N5 C54 C70 165.3(8) . . . . ? C53 N5 C54 C70 -25.4(13) . . . . ? C57 N5 C54 C55 -0.8(8) . . . . ? C53 N5 C54 C55 168.5(7) . . . . ? C70 C54 C55 C56 -166.9(7) . . . . ? N5 C54 C55 C56 1.3(9) . . . . ? C54 C55 C56 C57 -1.3(9) . . . . ? C55 C56 C57 C58 -172.1(8) . . . . ? C55 C56 C57 N5 0.9(9) . . . . ? C53 N5 C57 C58 3.4(11) . . . . ? C54 N5 C57 C58 173.4(7) . . . . ? C53 N5 C57 C56 -170.0(6) . . . . ? C54 N5 C57 C56 0.0(8) . . . . ? C56 C57 C58 C59 173.0(8) . . . . ? N5 C57 C58 C59 0.8(11) . . . . ? C56 C57 C58 C72 -5.2(13) . . . . ? N5 C57 C58 C72 -177.4(7) . . . . ? C57 C58 C59 C52 5.2(11) . . . . ? C72 C58 C59 C52 -176.6(7) . . . . ? C57 C58 C59 N6 -169.9(7) . . . . ? C72 C58 C59 N6 8.3(13) . . . . ? C53 C52 C59 C58 -16.0(11) . . . . ? C51 C52 C59 C58 177.2(7) . . . . ? C53 C52 C59 N6 159.7(7) . . . . ? C51 C52 C59 N6 -7.1(8) . . . . ? O5 C50 N6 C59 -173.9(9) . . . . ? C51 C50 N6 C59 5.2(9) . . . . ? O5 C50 N6 C71 -7.2(15) . . . . ? C51 C50 N6 C71 171.8(10) . . . . ? C58 C59 N6 C50 176.9(7) . . . . ? C52 C59 N6 C50 1.3(9) . . . . ? C58 C59 N6 C71 10.9(15) . . . . ? C52 C59 N6 C71 -164.7(10) . . . . ? C50 C51 C60 C61 -171.4(8) . . . . ? C52 C51 C60 C61 -2.5(15) . . . . ? C50 C51 C60 C78 4.2(11) . . . . ? C52 C51 C60 C78 173.1(8) . . . . ? C51 C60 C61 N7 -18.5(13) . . . . ? C78 C60 C61 N7 165.7(7) . . . . ? C51 C60 C61 C62 156.7(8) . . . . ? C78 C60 C61 C62 -19.1(11) . . . . ? N7 C61 C62 C63 -0.5(9) . . . . ? C60 C61 C62 C63 -176.4(8) . . . . ? C61 C62 C63 C64 -1.5(10) . . . . ? C62 C63 C64 C65 170.9(9) . . . . ? C62 C63 C64 N7 2.9(10) . . . . ? C60 C61 N7 C64 178.1(7) . . . . ? C62 C61 N7 C64 2.3(9) . . . . ? C60 C61 N7 Re2 -36.3(11) . . . . ? C62 C61 N7 Re2 147.8(5) . . . . ? C65 C64 N7 C61 -172.1(8) . . . . ? C63 C64 N7 C61 -3.2(9) . . . . ? C65 C64 N7 Re2 39.1(10) . . . . ? C63 C64 N7 Re2 -152.0(5) . . . . ? N7 C64 C65 C66 3.4(13) . . . . ? C63 C64 C65 C66 -163.3(9) . . . . ? N7 C64 C65 C84 179.5(8) . . . . ? C63 C64 C65 C84 12.9(14) . . . . ? C64 C65 C66 N8 -6.2(14) . . . . ? C84 C65 C66 N8 177.5(8) . . . . ? C64 C65 C66 C67 166.9(9) . . . . ? C84 C65 C66 C67 -9.4(14) . . . . ? N8 C66 C67 C68 -0.1(11) . . . . ? C65 C66 C67 C68 -174.0(9) . . . . ? C66 C67 C68 C69 1.3(11) . . . . ? C67 C68 C69 N8 -2.3(11) . . . . ? C67 C68 C69 C70 172.1(8) . . . . ? C70 C69 N8 C66 -172.0(8) . . . . ? C68 C69 N8 C66 2.2(9) . . . . ? C70 C69 N8 Re2 37.4(11) . . . . ? C68 C69 N8 Re2 -148.4(6) . . . . ? C65 C66 N8 C69 173.0(8) . . . . ? C67 C66 N8 C69 -1.4(10) . . . . ? C65 C66 N8 Re2 -34.6(11) . . . . ? C67 C66 N8 Re2 151.1(6) . . . . ? N5 C54 C70 C69 -8.5(14) . . . . ? C55 C54 C70 C69 156.0(8) . . . . ? N5 C54 C70 C90 176.4(8) . . . . ? C55 C54 C70 C90 -19.0(11) . . . . ? N8 C69 C70 C54 22.7(14) . . . . ? C68 C69 C70 C54 -150.8(9) . . . . ? N8 C69 C70 C90 -162.2(8) . . . . ? C68 C69 C70 C90 24.3(12) . . . . ? C57 C58 C72 C77 -103.8(10) . . . . ? C59 C58 C72 C77 78.2(11) . . . . ? C57 C58 C72 C73 76.5(12) . . . . ? C59 C58 C72 C73 -101.5(12) . . . . ? C77 C72 C73 C74 -4.4(19) . . . . ? C58 C72 C73 C74 175.3(12) . . . . ? C72 C73 C74 C75 3(2) . . . . ? C73 C74 C75 C76 0(2) . . . . ? C74 C75 C76 C77 -0.8(19) . . . . ? C73 C72 C77 C76 3.5(15) . . . . ? C58 C72 C77 C76 -176.2(9) . . . . ? C75 C76 C77 C72 -1.1(17) . . . . ? C51 C60 C78 C83 102.4(11) . . . . ? C61 C60 C78 C83 -81.3(11) . . . . ? C51 C60 C78 C79 -85.6(10) . . . . ? C61 C60 C78 C79 90.7(11) . . . . ? C83 C78 C79 C80 -1.2(15) . . . . ? C60 C78 C79 C80 -173.5(10) . . . . ? C78 C79 C80 C81 1.7(17) . . . . ? C79 C80 C81 C82 -1.5(18) . . . . ? C80 C81 C82 C83 1(2) . . . . ? C79 C78 C83 C82 0.6(16) . . . . ? C60 C78 C83 C82 172.9(10) . . . . ? C81 C82 C83 C78 -0.4(19) . . . . ? C64 C65 C84 C85 78.1(15) . . . . ? C66 C65 C84 C85 -105.4(14) . . . . ? C64 C65 C84 C89 -99.1(12) . . . . ? C66 C65 C84 C89 77.3(13) . . . . ? C89 C84 C85 C86 -2(3) . . . . ? C65 C84 C85 C86 -179.7(18) . . . . ? C84 C85 C86 C87 -2(3) . . . . ? C85 C86 C87 C88 6(3) . . . . ? C86 C87 C88 C89 -5(3) . . . . ? C85 C84 C89 C88 3(2) . . . . ? C65 C84 C89 C88 -180.0(11) . . . . ? C87 C88 C89 C84 1(2) . . . . ? C54 C70 C90 C95 -86.2(10) . . . . ? C69 C70 C90 C95 98.0(9) . . . . ? C54 C70 C90 C91 93.6(10) . . . . ? C69 C70 C90 C91 -82.2(11) . . . . ? C95 C90 C91 C92 0.5(15) . . . . ? C70 C90 C91 C92 -179.3(9) . . . . ? C90 C91 C92 C93 -0.2(17) . . . . ? C91 C92 C93 C94 0.4(19) . . . . ? C92 C93 C94 C95 -0.9(19) . . . . ? C91 C90 C95 C94 -1.0(15) . . . . ? C70 C90 C95 C94 178.8(9) . . . . ? C93 C94 C95 C90 1.2(17) . . . . ? C52 C53 Re2 C98 38.2(6) . . . . ? N5 C53 Re2 C98 -129.9(6) . . . . ? C52 C53 Re2 C97 128.4(6) . . . . ? N5 C53 Re2 C97 -39.6(6) . . . . ? C52 C53 Re2 N8 -136.8(6) . . . . ? N5 C53 Re2 N8 55.1(6) . . . . ? C52 C53 Re2 N7 -58.2(6) . . . . ? N5 C53 Re2 N7 133.7(6) . . . . ? C69 N8 Re2 C96 109.0(7) . . . . ? C66 N8 Re2 C96 -38.1(7) . . . . ? C69 N8 Re2 C97 19.0(7) . . . . ? C66 N8 Re2 C97 -128.2(7) . . . . ? C69 N8 Re2 C53 -75.2(7) . . . . ? C66 N8 Re2 C53 137.6(6) . . . . ? C69 N8 Re2 N7 -159.6(7) . . . . ? C66 N8 Re2 N7 53.2(6) . . . . ? C61 N7 Re2 C98 -15.6(7) . . . . ? C64 N7 Re2 C98 126.1(6) . . . . ? C61 N7 Re2 C96 -103.4(7) . . . . ? C64 N7 Re2 C96 38.3(6) . . . . ? C61 N7 Re2 C53 76.8(7) . . . . ? C64 N7 Re2 C53 -141.5(6) . . . . ? C61 N7 Re2 N8 163.4(7) . . . . ? C64 N7 Re2 N8 -54.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.801 _refine_diff_density_min -1.523 _refine_diff_density_rms 0.142 _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 -0.066 0.250 922 312 ' ' 2 0.500 -0.262 0.750 922 311 ' ' _platon_squeeze_details ; ; #============================================================================== # End of CIF #==============================================================================