# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # 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_Compound_1a #=================================================================== #=================================================================== # 5. CHEMICAL DATA #=================================================================== _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety 'C15 H17 N5 O3 Re, C4 H8 O, F6 P' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C19 H25 F6 N5 O4 P Re' _chemical_formula_weight 718.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=================================================================== # 6. CRYSTAL DATA #=================================================================== _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_Hall 'P 2c -2n' _symmetry_space_group_name_H-M 'P n a 21' _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,1/2+z 3 1/2-x,1/2+y,1/2+z 4 1/2+x,1/2-y,z _cell_length_a 17.6769(7) _cell_length_b 13.3006(5) _cell_length_c 10.9901(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2583.92(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used 9833 _cell_measurement_theta_min 1.92 _cell_measurement_theta_max 25.34 _exptl_crystal_description fragment _exptl_crystal_colour colorless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.847 _exptl_crystal_density_method none _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 4.842 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3761 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_process_details 'SADABS, Bruker, 2008b' _exptl_special_details ; Diffractometer operator E. Herdtweck scanspeed 10 s per frame dx 40 2274 frames measured in 9 data sets phi-scan with delta_phi = 1.00 omega-scans with delta_omega = 1.00 ; #=================================================================== # 7. EXPERIMENTAL DATA #=================================================================== _diffrn_ambient_temperature 173(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'rotating anode FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' \k-geometry diffractometer ' _diffrn_measurement_device_type ' Bruker APEX-II CCD ' _diffrn_measurement_method ' phi- and omega-rotation ' _diffrn_detector ' CCD plate ' _diffrn_detector_area_resol_mean 16 # 8 for binned mode _diffrn_standards_decay_% 0 # number of measured reflections (redundant set) _diffrn_reflns_number 95541 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_sigmaI/netI 0.0163 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.34 _reflns_number_total 4700 _reflns_number_gt 4521 # number of observed reflections (> n sig(I)) _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX II Control Software (Bruker, 2008a)' _computing_cell_refinement 'SAINT (Bruker, 2008b)' _computing_data_reduction 'SAINT (Bruker, 2008b)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2010)' _computing_publication_material 'PLATON (Spek, 2010)' #=================================================================== # 8. REFINEMENT DATA #=================================================================== _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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 sigma _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0167P)^2^+5.5662P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.240(8) _chemical_absolute_configuration ad _refine_ls_number_reflns 4700 _refine_ls_number_parameters 329 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0229 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0530 _refine_ls_wR_factor_gt 0.0515 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.142 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.987 _refine_diff_density_min -0.914 _refine_diff_density_rms 0.082 #=================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=================================================================== loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Re1 Re Uani 0.33890(1) 0.48913(1) 0.08513(4) 1.000 0.0279(1) . . O1 O Uani 0.4046(3) 0.6126(3) 0.2999(4) 1.000 0.0637(17) . . O2 O Uani 0.2636(3) 0.6847(3) -0.0054(5) 1.000 0.0583(16) . . O3 O Uani 0.4790(3) 0.5664(3) -0.0492(5) 1.000 0.0687(18) . . N1 N Uani 0.2225(2) 0.3936(3) -0.1123(4) 1.000 0.0327(12) . . N2 N Uani 0.3359(2) 0.3393(3) -0.1401(4) 1.000 0.0363(14) . . N3 N Uani 0.4182(2) 0.2643(3) 0.0910(8) 1.000 0.0522(16) . . N4 N Uani 0.3851(3) 0.3122(4) 0.2685(5) 1.000 0.0527(19) . . N5 N Uani 0.2403(2) 0.4413(3) 0.1833(4) 1.000 0.0353(12) . . C1 C Uani 0.3801(3) 0.5648(4) 0.2228(5) 1.000 0.0397(17) . . C2 C Uani 0.2896(3) 0.6104(4) 0.0287(5) 1.000 0.0353(16) . . C3 C Uani 0.4277(3) 0.5340(4) -0.0001(5) 1.000 0.0400(17) . . C4 C Uani 0.1905(3) 0.4154(5) 0.2415(5) 1.000 0.0400(19) . . C5 C Uani 0.1282(4) 0.3820(6) 0.3213(7) 1.000 0.066(3) . . C6 C Uani 0.2937(3) 0.4025(3) -0.0678(4) 1.000 0.0283(12) . . C7 C Uani 0.2209(3) 0.3272(4) -0.2109(5) 1.000 0.0430(17) . . C8 C Uani 0.2912(3) 0.2935(4) -0.2276(5) 1.000 0.0440(17) . . C9 C Uani 0.4168(3) 0.3247(5) -0.1300(6) 1.000 0.047(2) . . C10 C Uani 0.4402(4) 0.2472(6) -0.0350(8) 1.000 0.072(3) . . C11 C Uani 0.3871(3) 0.3438(4) 0.1498(5) 1.000 0.0380(16) . . C12 C Uani 0.4324(4) 0.1855(5) 0.1743(11) 1.000 0.087(4) . . C13 C Uani 0.4141(4) 0.2168(6) 0.2822(9) 1.000 0.073(3) . . C14 C Uani 0.1549(3) 0.4449(5) -0.0695(6) 1.000 0.0433(19) . . C15 C Uani 0.3574(4) 0.3645(6) 0.3786(6) 1.000 0.059(3) . . O4 O Uani 0.1453(3) 0.2114(4) 0.1058(8) 1.000 0.093(2) . . C16 C Uani 0.2193(4) 0.1771(5) 0.0886(13) 1.000 0.094(3) . . C17 C Uani 0.2230(5) 0.0735(7) 0.1088(15) 1.000 0.123(5) . . C18 C Uani 0.1495(5) 0.0435(7) 0.1661(10) 1.000 0.092(4) . . C19 C Uani 0.1000(5) 0.1263(7) 0.1338(9) 1.000 0.098(4) . . P1 P Uani 0.00519(7) 0.38135(10) 0.61666(12) 1.000 0.0367(4) . . F1 F Uani -0.0266(5) 0.4713(7) 0.6821(11) 1.000 0.197(5) . . F2 F Uani -0.0123(3) 0.4315(6) 0.4911(5) 1.000 0.100(2) . . F3 F Uani -0.0758(2) 0.3314(4) 0.6168(4) 1.000 0.0940(18) . . F4 F Uani 0.0860(2) 0.4350(3) 0.6162(4) 1.000 0.0774(18) . . F5 F Uani 0.0247(3) 0.3293(5) 0.7392(5) 1.000 0.129(3) . . F6 F Uani 0.0403(3) 0.2927(3) 0.5398(6) 1.000 0.126(3) . . H51 H Uiso 0.09070 0.43590 0.32860 1.000 0.0990 calc R H52 H Uiso 0.14830 0.36570 0.40200 1.000 0.0990 calc R H53 H Uiso 0.10420 0.32220 0.28630 1.000 0.0990 calc R H71 H Uiso 0.17770 0.30930 -0.25750 1.000 0.0520 calc R H81 H Uiso 0.30750 0.24700 -0.28780 1.000 0.0530 calc R H91 H Uiso 0.44060 0.38990 -0.10940 1.000 0.0560 calc R H92 H Uiso 0.43670 0.30340 -0.21020 1.000 0.0560 calc R H101 H Uiso 0.41930 0.18140 -0.06020 1.000 0.0860 calc R H102 H Uiso 0.49600 0.24120 -0.03750 1.000 0.0860 calc R H121 H Uiso 0.45190 0.12090 0.15470 1.000 0.1040 calc R H131 H Uiso 0.41980 0.18090 0.35630 1.000 0.0870 calc R H141 H Uiso 0.12220 0.46070 -0.13890 1.000 0.0650 calc R H142 H Uiso 0.16930 0.50730 -0.02810 1.000 0.0650 calc R H143 H Uiso 0.12760 0.40130 -0.01260 1.000 0.0650 calc R H151 H Uiso 0.38880 0.34560 0.44850 1.000 0.0880 calc R H152 H Uiso 0.30480 0.34520 0.39420 1.000 0.0880 calc R H153 H Uiso 0.36030 0.43740 0.36620 1.000 0.0880 calc R H161 H Uiso 0.23590 0.19230 0.00450 1.000 0.1120 calc R H162 H Uiso 0.25380 0.21220 0.14540 1.000 0.1120 calc R H171 H Uiso 0.26570 0.05720 0.16370 1.000 0.1470 calc R H172 H Uiso 0.23040 0.03730 0.03100 1.000 0.1470 calc R H181 H Uiso 0.13070 -0.02090 0.13220 1.000 0.1100 calc R H182 H Uiso 0.15450 0.03700 0.25550 1.000 0.1100 calc R H191 H Uiso 0.06870 0.10780 0.06250 1.000 0.1180 calc R H192 H Uiso 0.06580 0.14200 0.20250 1.000 0.1180 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0242(1) 0.0267(1) 0.0329(1) 0.0002(2) 0.0006(2) 0.0004(1) O1 0.077(3) 0.054(3) 0.060(3) -0.008(2) -0.021(2) -0.017(2) O2 0.062(3) 0.039(2) 0.074(3) 0.009(2) 0.002(2) 0.014(2) O3 0.051(2) 0.057(3) 0.098(4) -0.012(3) 0.032(3) -0.017(2) N1 0.027(2) 0.038(2) 0.033(2) -0.0040(19) -0.0010(17) 0.0027(19) N2 0.027(2) 0.037(2) 0.045(3) -0.008(2) 0.0022(19) 0.0028(18) N3 0.035(2) 0.0337(19) 0.088(4) 0.011(4) -0.022(4) 0.0063(15) N4 0.039(3) 0.049(3) 0.070(4) 0.032(3) -0.026(3) -0.013(3) N5 0.035(2) 0.039(2) 0.032(2) -0.0044(18) -0.0014(19) 0.0023(19) C1 0.044(3) 0.033(3) 0.042(3) -0.001(2) -0.007(3) -0.007(2) C2 0.036(3) 0.034(3) 0.036(2) 0.000(2) 0.006(2) 0.006(2) C3 0.034(3) 0.032(3) 0.054(3) -0.001(2) 0.002(3) -0.001(2) C4 0.035(3) 0.050(4) 0.035(3) 0.006(3) -0.002(3) 0.005(3) C5 0.048(4) 0.088(5) 0.062(4) 0.020(4) 0.022(3) 0.001(4) C6 0.027(2) 0.030(2) 0.028(2) 0.0012(19) 0.0046(19) 0.0016(18) C7 0.041(3) 0.046(3) 0.042(3) -0.009(2) -0.012(2) 0.001(2) C8 0.046(3) 0.047(3) 0.039(3) -0.016(2) 0.003(2) 0.001(3) C9 0.030(3) 0.052(4) 0.059(4) -0.017(3) 0.005(3) 0.008(3) C10 0.054(4) 0.057(4) 0.105(6) -0.040(5) -0.024(4) 0.028(4) C11 0.024(2) 0.033(3) 0.057(3) 0.004(2) -0.009(2) -0.001(2) C12 0.068(5) 0.027(3) 0.166(10) 0.021(5) -0.045(6) 0.007(3) C13 0.060(5) 0.056(4) 0.102(7) 0.029(5) -0.029(4) -0.002(3) C14 0.028(3) 0.054(4) 0.048(3) -0.006(3) 0.000(2) 0.007(3) C15 0.048(4) 0.081(5) 0.047(4) 0.020(3) -0.012(3) -0.016(3) O4 0.076(3) 0.059(3) 0.144(6) 0.018(4) 0.018(4) 0.004(2) C16 0.065(4) 0.069(4) 0.147(8) 0.014(9) 0.037(7) -0.009(3) C17 0.068(5) 0.096(6) 0.204(14) 0.070(9) 0.028(8) 0.023(4) C18 0.096(6) 0.078(6) 0.102(7) 0.032(5) 0.002(5) 0.002(5) C19 0.071(5) 0.105(7) 0.118(8) 0.032(6) 0.004(5) -0.005(5) P1 0.0321(6) 0.0416(6) 0.0365(9) 0.0018(5) -0.0013(5) -0.0069(5) F1 0.152(7) 0.132(6) 0.306(12) -0.138(7) 0.106(7) -0.035(5) F2 0.061(3) 0.150(6) 0.088(3) 0.051(4) -0.013(3) -0.015(3) F3 0.063(2) 0.137(4) 0.082(3) 0.039(3) -0.013(2) -0.059(2) F4 0.0512(19) 0.092(3) 0.089(4) 0.030(2) -0.017(2) -0.0322(18) F5 0.091(4) 0.197(7) 0.099(4) 0.081(4) -0.038(3) -0.080(4) F6 0.145(5) 0.046(2) 0.186(8) -0.013(3) 0.074(5) 0.011(3) #================================================================== # 10. MOLECULAR GEOMETRY #=================================================================== _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 N5 2.146(4) . . yes Re1 C1 1.958(5) . . yes Re1 C2 1.935(5) . . yes Re1 C3 1.923(5) . . yes Re1 C6 2.189(4) . . yes Re1 C11 2.229(5) . . yes P1 F4 1.597(4) . . yes P1 F5 1.553(6) . . yes P1 F6 1.578(5) . . yes P1 F3 1.578(4) . . yes P1 F1 1.505(10) . . yes P1 F2 1.564(6) . . yes O1 C1 1.144(7) . . yes O2 C2 1.153(7) . . yes O3 C3 1.140(7) . . yes O4 C19 1.420(11) . . yes O4 C16 1.398(9) . . yes N1 C14 1.454(7) . . yes N1 C6 1.356(6) . . yes N1 C7 1.398(7) . . yes N2 C8 1.386(7) . . yes N2 C6 1.376(6) . . yes N2 C9 1.447(6) . . yes N3 C12 1.414(11) . . yes N3 C10 1.456(12) . . yes N3 C11 1.356(8) . . yes N4 C11 1.371(8) . . yes N4 C15 1.479(9) . . yes N4 C13 1.377(10) . . yes N5 C4 1.141(7) . . yes C4 C5 1.476(9) . . no C7 C8 1.334(8) . . no C9 C10 1.524(11) . . no C12 C13 1.298(15) . . no C5 H51 0.9800 . . no C5 H52 0.9800 . . no C5 H53 0.9800 . . no C7 H71 0.9500 . . no C8 H81 0.9500 . . no C9 H91 0.9900 . . no C9 H92 0.9900 . . no C10 H101 0.9900 . . no C10 H102 0.9900 . . no C12 H121 0.9500 . . no C13 H131 0.9500 . . no C14 H143 0.9800 . . no C14 H142 0.9800 . . no C14 H141 0.9800 . . no C15 H153 0.9800 . . no C15 H151 0.9800 . . no C15 H152 0.9800 . . no C16 C17 1.397(12) . . no C17 C18 1.498(14) . . no C18 C19 1.451(13) . . no C16 H161 0.9900 . . no C16 H162 0.9900 . . no C17 H172 0.9900 . . no C17 H171 0.9900 . . no C18 H181 0.9900 . . no C18 H182 0.9900 . . no C19 H192 0.9900 . . no C19 H191 0.9900 . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Re1 C1 93.78(19) . . . yes N5 Re1 C2 92.43(19) . . . yes N5 Re1 C3 178.8(2) . . . yes N5 Re1 C6 86.19(17) . . . yes N5 Re1 C11 83.86(17) . . . yes C1 Re1 C2 89.2(2) . . . yes C1 Re1 C3 85.0(2) . . . yes C1 Re1 C6 179.1(2) . . . yes C1 Re1 C11 93.3(2) . . . yes C2 Re1 C3 87.3(2) . . . yes C2 Re1 C6 91.6(2) . . . yes C2 Re1 C11 175.7(2) . . . yes C3 Re1 C6 95.0(2) . . . yes C3 Re1 C11 96.5(2) . . . yes C6 Re1 C11 85.86(18) . . . yes F1 P1 F6 175.6(5) . . . yes F2 P1 F3 90.1(3) . . . yes F2 P1 F4 89.1(3) . . . yes F2 P1 F5 178.0(3) . . . yes F2 P1 F6 85.7(3) . . . yes F3 P1 F4 178.4(2) . . . yes F3 P1 F5 90.7(3) . . . yes F3 P1 F6 92.5(3) . . . yes F4 P1 F5 90.2(3) . . . yes F4 P1 F6 88.9(2) . . . yes F5 P1 F6 92.5(3) . . . yes F1 P1 F4 88.9(4) . . . yes F1 P1 F2 90.5(5) . . . yes F1 P1 F3 89.7(4) . . . yes F1 P1 F5 91.3(5) . . . yes C16 O4 C19 107.3(6) . . . yes C6 N1 C7 110.7(4) . . . yes C6 N1 C14 127.3(4) . . . yes C7 N1 C14 122.0(4) . . . yes C8 N2 C9 123.9(4) . . . yes C6 N2 C9 125.0(4) . . . yes C6 N2 C8 111.1(4) . . . yes C11 N3 C12 110.0(8) . . . yes C10 N3 C12 116.9(6) . . . yes C10 N3 C11 133.1(6) . . . yes C13 N4 C15 117.9(6) . . . yes C11 N4 C15 130.0(5) . . . yes C11 N4 C13 112.2(6) . . . yes Re1 N5 C4 175.9(4) . . . yes Re1 C1 O1 177.0(5) . . . yes Re1 C2 O2 176.7(5) . . . yes Re1 C3 O3 175.9(5) . . . yes N5 C4 C5 177.6(6) . . . yes Re1 C6 N2 124.5(4) . . . yes N1 C6 N2 104.0(4) . . . yes Re1 C6 N1 131.5(3) . . . yes N1 C7 C8 107.5(5) . . . yes N2 C8 C7 106.7(5) . . . yes N2 C9 C10 114.3(5) . . . yes N3 C10 C9 118.2(6) . . . yes Re1 C11 N3 132.8(5) . . . yes N3 C11 N4 103.0(5) . . . yes Re1 C11 N4 124.0(4) . . . yes N3 C12 C13 108.0(7) . . . yes N4 C13 C12 106.8(8) . . . yes H51 C5 H52 109.00 . . . no C4 C5 H51 109.00 . . . no C4 C5 H52 110.00 . . . no C4 C5 H53 110.00 . . . no H51 C5 H53 109.00 . . . no H52 C5 H53 109.00 . . . no C8 C7 H71 126.00 . . . no N1 C7 H71 126.00 . . . no C7 C8 H81 127.00 . . . no N2 C8 H81 127.00 . . . no C10 C9 H92 109.00 . . . no H91 C9 H92 108.00 . . . no N2 C9 H92 109.00 . . . no C10 C9 H91 109.00 . . . no N2 C9 H91 109.00 . . . no N3 C10 H102 108.00 . . . no C9 C10 H101 108.00 . . . no C9 C10 H102 108.00 . . . no H101 C10 H102 107.00 . . . no N3 C10 H101 108.00 . . . no N3 C12 H121 126.00 . . . no C13 C12 H121 126.00 . . . no C12 C13 H131 127.00 . . . no N4 C13 H131 127.00 . . . no N1 C14 H142 110.00 . . . no N1 C14 H143 109.00 . . . no N1 C14 H141 109.00 . . . no H141 C14 H143 109.00 . . . no H142 C14 H143 109.00 . . . no H141 C14 H142 109.00 . . . no N4 C15 H151 109.00 . . . no N4 C15 H152 110.00 . . . no N4 C15 H153 110.00 . . . no H151 C15 H152 109.00 . . . no H151 C15 H153 109.00 . . . no H152 C15 H153 109.00 . . . no O4 C16 C17 110.1(7) . . . yes C16 C17 C18 106.8(8) . . . no C17 C18 C19 102.6(8) . . . no O4 C19 C18 108.5(7) . . . yes H161 C16 H162 108.00 . . . no O4 C16 H161 110.00 . . . no O4 C16 H162 110.00 . . . no C17 C16 H161 110.00 . . . no C17 C16 H162 110.00 . . . no C16 C17 H171 110.00 . . . no C16 C17 H172 110.00 . . . no C18 C17 H171 110.00 . . . no C18 C17 H172 110.00 . . . no H171 C17 H172 109.00 . . . no C17 C18 H181 111.00 . . . no C17 C18 H182 111.00 . . . no C19 C18 H181 111.00 . . . no C19 C18 H182 111.00 . . . no H181 C18 H182 109.00 . . . no O4 C19 H191 110.00 . . . no O4 C19 H192 110.00 . . . no C18 C19 H191 110.00 . . . no C18 C19 H192 110.00 . . . no H191 C19 H192 108.00 . . . no _iucr_refine_instructions_details ; ; # End of Crystallographic Information File _database_code_depnum_ccdc_archive 'CCDC 933791' ####################################################################### # # 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_Compound_1b #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_moiety 'C16 H19 N5 O3 Re, F6 P' _chemical_formula_sum 'C16 H19 F6 N5 O3 P Re' _chemical_formula_weight 660.54 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 11.6963(4) _cell_length_b 12.6367(4) _cell_length_c 15.3154(5) _cell_angle_alpha 98.234(2) _cell_angle_beta 98.282(2) _cell_angle_gamma 90.816(2) _cell_volume 2215.55(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100 _cell_measurement_reflns_used 9586 _cell_measurement_theta_min 2.3561 _cell_measurement_theta_max 25.3530 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.130 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.040 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.980 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 5.635 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS, Bruker, 2008b' _exptl_absorpt_correction_T_min 0.537 _exptl_absorpt_correction_T_max 0.794 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; Diffractometer operator A. Poethig scanspeed 10 s per frame dx 40 5676 frames measured in 11 data sets phi-scan with delta_phi = 0.5 omega-scans with delta_omega = 0.5 ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' \k-geometry diffractometer ' _diffrn_measurement_device_type ' Bruker APEX-II CCD ' _diffrn_measurement_method ' phi- and omega-rotation ' _diffrn_detector ' CCD plate ' _diffrn_detector_area_resol_mean 16 # number of measured reflections (redundant set) _diffrn_reflns_number 91463 _diffrn_reflns_av_R_equivalents 0.0306 _diffrn_reflns_av_sigmaI/netI 0.0167 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 25.39 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 8099 # number of observed reflections (> n sig(I)) _reflns_number_gt 7397 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX II Control Software (Bruker, 2008a)' _computing_cell_refinement 'SAINT (Bruker, 2008b)' _computing_data_reduction 'SAINT (Bruker, 2008b)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997), SHELXLE (Huebschle, 2011)' _computing_molecular_graphics 'PLATON (Spek, 2011)' _computing_publication_material 'PLATON (Spek, 2011), enCIFer (Allen, 2004)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0175P)^2^+8.0068P] 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_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 8099 _refine_ls_number_parameters 583 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0243 _refine_ls_R_factor_gt 0.0206 _refine_ls_wR_factor_ref 0.0481 _refine_ls_wR_factor_gt 0.0464 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.724 _refine_diff_density_min -0.939 _refine_diff_density_rms 0.100 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re Uani 0.20069(1) 0.11507(1) -0.07038(1) 1.000 0.0118(1) d . . . O1 O Uani 0.1126(2) 0.1134(2) -0.27182(18) 1.000 0.0264(9) d . . . O2 O Uani 0.3816(2) -0.0477(2) -0.11771(18) 1.000 0.0251(9) d . . . O3 O Uani 0.0170(2) -0.0701(2) -0.10146(18) 1.000 0.0247(9) d . . . N1 N Uani 0.2784(2) 0.3413(2) -0.1208(2) 1.000 0.0146(9) d . . . N2 N Uani 0.4215(2) 0.2837(2) -0.0402(2) 1.000 0.0149(9) d . . . N3 N Uani 0.3062(3) 0.1754(2) 0.1403(2) 1.000 0.0186(10) d . . . N4 N Uani 0.2592(3) 0.0087(2) 0.1097(2) 1.000 0.0171(9) d . . . N5 N Uani 0.0856(2) 0.2269(2) -0.0123(2) 1.000 0.0146(9) d . . . C1 C Uani 0.1444(3) 0.1191(3) -0.1962(3) 1.000 0.0166(10) d . . . C2 C Uani 0.3130(3) 0.0147(3) -0.1026(2) 1.000 0.0166(11) d . . . C3 C Uani 0.0868(3) -0.0024(3) -0.0842(2) 1.000 0.0170(11) d . . . C4 C Uani 0.3091(3) 0.2584(3) -0.0748(2) 1.000 0.0130(10) d . . . C5 C Uani 0.3696(3) 0.4144(3) -0.1142(3) 1.000 0.0190(11) d . . . C6 C Uani 0.4594(3) 0.3784(3) -0.0635(3) 1.000 0.0191(11) d . . . C7 C Uani 0.4885(3) 0.2331(3) 0.0299(3) 1.000 0.0216(11) d . . . C8 C Uani 0.4699(3) 0.2897(3) 0.1210(3) 1.000 0.0245(11) d . . . C9 C Uani 0.3438(3) 0.2853(3) 0.1349(3) 1.000 0.0219(11) d . . . C10 C Uani 0.2622(3) 0.0997(3) 0.0714(2) 1.000 0.0159(11) d . . . C11 C Uani 0.2990(3) 0.0289(3) 0.1998(3) 1.000 0.0223(12) d . . . C12 C Uani 0.3291(3) 0.1332(3) 0.2192(3) 1.000 0.0232(12) d . . . C13 C Uani 0.1665(3) 0.3580(3) -0.1724(3) 1.000 0.0234(11) d . . . C14 C Uani 0.2177(4) -0.0986(3) 0.0672(3) 1.000 0.0252(11) d . . . C15 C Uani 0.0300(3) 0.2812(3) 0.0292(2) 1.000 0.0168(11) d . . . C16 C Uani -0.0420(3) 0.3476(3) 0.0833(3) 1.000 0.0251(12) d . . . Re2 Re Uani 0.23297(1) 0.12078(1) 0.49057(1) 1.000 0.0121(1) d . . . O4 O Uani 0.0680(2) 0.0704(2) 0.31102(19) 1.000 0.0335(10) d . . . O5 O Uani 0.4005(2) -0.0334(2) 0.40759(18) 1.000 0.0232(8) d . . . O6 O Uani 0.0995(2) -0.0761(2) 0.5302(2) 1.000 0.0288(9) d . . . N6 N Uani 0.2443(2) 0.3309(2) 0.3941(2) 1.000 0.0182(9) d . . . N7 N Uani 0.4161(2) 0.2858(2) 0.43800(19) 1.000 0.0133(8) d . . . N8 N Uani 0.4117(3) 0.2342(2) 0.6650(2) 1.000 0.0162(9) d . . . N9 N Uani 0.3777(2) 0.0700(2) 0.67501(19) 1.000 0.0151(9) d . . . N10 N Uani 0.1172(3) 0.2277(2) 0.5534(2) 1.000 0.0170(9) d . . . C17 C Uani 0.1277(3) 0.0931(3) 0.3776(3) 1.000 0.0205(11) d . . . C18 C Uani 0.3382(3) 0.0253(3) 0.4389(2) 1.000 0.0150(10) d . . . C19 C Uani 0.1517(3) -0.0018(3) 0.5208(3) 1.000 0.0192(11) d . . . C20 C Uani 0.3032(3) 0.2595(3) 0.4403(2) 1.000 0.0152(10) d . . . C21 C Uani 0.3181(3) 0.3999(3) 0.3651(2) 1.000 0.0192(11) d . . . C22 C Uani 0.4262(3) 0.3724(3) 0.3926(2) 1.000 0.0165(11) d . . . C23 C Uani 0.5156(3) 0.2519(3) 0.4960(2) 1.000 0.0170(11) d . . . C24 C Uani 0.5352(3) 0.3293(3) 0.5829(3) 1.000 0.0207(11) d . . . C25 C Uani 0.4306(3) 0.3356(3) 0.6323(3) 1.000 0.0203(11) d . . . C26 C Uani 0.3500(3) 0.1451(3) 0.6201(2) 1.000 0.0134(10) d . . . C27 C Uani 0.4542(3) 0.1119(3) 0.7500(2) 1.000 0.0181(11) d . . . C28 C Uani 0.4763(3) 0.2139(3) 0.7437(2) 1.000 0.0183(11) d . . . C29 C Uani 0.1189(3) 0.3434(4) 0.3786(4) 1.000 0.0395(16) d . . . C30 C Uani 0.3415(3) -0.0432(3) 0.6592(3) 1.000 0.0216(11) d . . . C31 C Uani 0.0462(3) 0.2746(3) 0.5830(3) 1.000 0.0189(11) d . . . C32 C Uani -0.0475(4) 0.3330(3) 0.6197(3) 1.000 0.0322(14) d . . . P1 P Uani 0.22114(8) 0.58784(8) 0.15272(7) 1.000 0.0192(3) d . . . F1 F Uani 0.2426(2) 0.6852(2) 0.23315(18) 1.000 0.0444(9) d . . . F2 F Uani 0.1997(2) 0.49175(18) 0.07184(17) 1.000 0.0355(8) d . . . F3 F Uani 0.09666(19) 0.6318(2) 0.12133(16) 1.000 0.0325(8) d . . . F4 F Uani 0.27742(19) 0.65918(18) 0.09026(18) 1.000 0.0327(8) d . . . F5 F Uani 0.34600(19) 0.54438(18) 0.18487(17) 1.000 0.0318(8) d . . . F6 F Uani 0.1643(2) 0.5169(2) 0.21486(17) 1.000 0.0403(9) d . . . P2 P Uani 0.77063(10) 0.38902(11) 0.34330(10) 1.000 0.0429(4) d . . . F7 F Uani 0.8336(4) 0.3462(5) 0.2649(3) 1.000 0.127(3) d . . . F8 F Uani 0.7072(3) 0.4384(3) 0.4271(2) 1.000 0.0576(11) d . . . F9 F Uani 0.8580(4) 0.3385(6) 0.4070(4) 1.000 0.164(4) d . . . F10 F Uani 0.6849(4) 0.2853(3) 0.3275(3) 1.000 0.0784(15) d . . . F11 F Uani 0.6737(4) 0.4367(3) 0.2792(3) 1.000 0.0857(17) d . . . F12 F Uani 0.8404(6) 0.4965(5) 0.3533(4) 1.000 0.169(3) d . . . H5 H Uiso 0.36870 0.47800 -0.14060 1.000 0.0230 c R . . H6 H Uiso 0.53430 0.41150 -0.04690 1.000 0.0230 c R . . H7A H Uiso 0.57160 0.23690 0.02420 1.000 0.0260 c R . . H7B H Uiso 0.46380 0.15670 0.02350 1.000 0.0260 c R . . H8A H Uiso 0.49680 0.36540 0.12750 1.000 0.0290 c R . . H8B H Uiso 0.51710 0.25600 0.16780 1.000 0.0290 c R . . H9A H Uiso 0.33410 0.33240 0.19070 1.000 0.0260 c R . . H9B H Uiso 0.29510 0.31180 0.08480 1.000 0.0260 c R . . H11 H Uiso 0.30410 -0.02160 0.24050 1.000 0.0270 c R . . H12 H Uiso 0.36020 0.17080 0.27610 1.000 0.0280 c R . . H13A H Uiso 0.16540 0.32550 -0.23460 1.000 0.0350 c R . . H13B H Uiso 0.15430 0.43490 -0.16970 1.000 0.0350 c R . . H13C H Uiso 0.10490 0.32470 -0.14740 1.000 0.0350 c R . . H14A H Uiso 0.13330 -0.10390 0.06270 1.000 0.0380 c R . . H14B H Uiso 0.25220 -0.15160 0.10300 1.000 0.0380 c R . . H14C H Uiso 0.23980 -0.11240 0.00730 1.000 0.0380 c R . . H16A H Uiso -0.06040 0.31010 0.13160 1.000 0.0300 c R . . H16B H Uiso -0.11380 0.36200 0.04600 1.000 0.0300 c R . . H16C H Uiso -0.00030 0.41530 0.10880 1.000 0.0300 c R . . H21 H Uiso 0.29640 0.45620 0.33190 1.000 0.0230 c R . . H22 H Uiso 0.49590 0.40550 0.38300 1.000 0.0200 c R . . H23A H Uiso 0.58530 0.25160 0.46610 1.000 0.0200 c R . . H23B H Uiso 0.50070 0.17850 0.50820 1.000 0.0200 c R . . H24A H Uiso 0.55430 0.40150 0.57000 1.000 0.0250 c R . . H24B H Uiso 0.60230 0.30650 0.62220 1.000 0.0250 c R . . H25A H Uiso 0.44350 0.39450 0.68310 1.000 0.0240 c R . . H25B H Uiso 0.36110 0.35110 0.59150 1.000 0.0240 c R . . H27 H Uiso 0.48520 0.07460 0.79720 1.000 0.0220 c R . . H28 H Uiso 0.52650 0.26320 0.78500 1.000 0.0220 c R . . H29A H Uiso 0.09870 0.40630 0.41800 1.000 0.0590 c R . . H29B H Uiso 0.07950 0.27950 0.39120 1.000 0.0590 c R . . H29C H Uiso 0.09460 0.35280 0.31630 1.000 0.0590 c R . . H30A H Uiso 0.26280 -0.05080 0.67300 1.000 0.0330 c R . . H30B H Uiso 0.39430 -0.08250 0.69750 1.000 0.0330 c R . . H30C H Uiso 0.34310 -0.07210 0.59650 1.000 0.0330 c R . . H32A H Uiso -0.01760 0.40320 0.65110 1.000 0.0480 c R . . H32B H Uiso -0.07850 0.29240 0.66140 1.000 0.0480 c R . . H32C H Uiso -0.10900 0.34260 0.57110 1.000 0.0480 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0129(1) 0.0106(1) 0.0124(1) 0.0036(1) 0.0021(1) -0.0001(1) O1 0.0348(16) 0.0267(15) 0.0167(16) 0.0053(11) -0.0011(12) -0.0042(12) O2 0.0317(15) 0.0219(14) 0.0252(16) 0.0086(11) 0.0100(12) 0.0104(12) O3 0.0287(15) 0.0217(14) 0.0236(16) 0.0058(11) 0.0021(12) -0.0102(12) N1 0.0147(15) 0.0130(14) 0.0172(16) 0.0040(12) 0.0039(12) 0.0004(11) N2 0.0134(15) 0.0128(14) 0.0180(16) 0.0002(11) 0.0027(12) -0.0006(11) N3 0.0254(17) 0.0170(16) 0.0142(17) 0.0036(12) 0.0037(13) 0.0056(13) N4 0.0193(16) 0.0158(15) 0.0179(17) 0.0069(12) 0.0042(12) 0.0032(12) N5 0.0131(15) 0.0146(15) 0.0174(16) 0.0073(12) 0.0015(12) -0.0001(12) C1 0.0142(17) 0.0132(17) 0.023(2) 0.0038(14) 0.0043(15) -0.0029(14) C2 0.0203(19) 0.0142(18) 0.0163(19) 0.0060(14) 0.0022(14) -0.0008(15) C3 0.0207(19) 0.0194(19) 0.0134(19) 0.0062(14) 0.0070(14) 0.0026(16) C4 0.0141(17) 0.0134(17) 0.0112(18) -0.0006(13) 0.0035(13) 0.0009(13) C5 0.023(2) 0.0120(17) 0.024(2) 0.0027(14) 0.0100(16) -0.0020(14) C6 0.0172(18) 0.0142(18) 0.026(2) -0.0022(15) 0.0095(15) -0.0051(14) C7 0.0138(18) 0.0203(19) 0.029(2) 0.0054(16) -0.0046(15) 0.0028(14) C8 0.029(2) 0.0193(19) 0.021(2) 0.0020(15) -0.0087(16) -0.0038(16) C9 0.033(2) 0.0145(18) 0.017(2) 0.0009(14) 0.0006(16) 0.0025(15) C10 0.0176(18) 0.0153(18) 0.0165(19) 0.0057(14) 0.0043(14) 0.0034(14) C11 0.027(2) 0.028(2) 0.015(2) 0.0104(15) 0.0051(15) 0.0092(16) C12 0.030(2) 0.028(2) 0.012(2) 0.0039(15) 0.0029(15) 0.0058(17) C13 0.022(2) 0.0201(19) 0.029(2) 0.0126(16) -0.0023(16) 0.0028(15) C14 0.034(2) 0.0162(19) 0.027(2) 0.0100(16) 0.0036(17) -0.0001(16) C15 0.0140(18) 0.0179(18) 0.019(2) 0.0074(15) -0.0004(15) -0.0024(15) C16 0.021(2) 0.029(2) 0.025(2) -0.0008(17) 0.0072(16) 0.0035(16) Re2 0.0109(1) 0.0127(1) 0.0129(1) 0.0023(1) 0.0020(1) -0.0006(1) O4 0.0271(16) 0.0468(19) 0.0227(17) 0.0033(13) -0.0069(13) -0.0106(13) O5 0.0256(14) 0.0243(14) 0.0204(15) 0.0016(11) 0.0065(11) 0.0075(12) O6 0.0203(14) 0.0236(15) 0.0434(19) 0.0136(13) 0.0003(12) -0.0073(12) N6 0.0150(15) 0.0200(16) 0.0212(18) 0.0090(13) 0.0017(12) 0.0018(12) N7 0.0131(14) 0.0122(14) 0.0151(16) 0.0036(11) 0.0026(11) -0.0010(11) N8 0.0207(16) 0.0152(15) 0.0122(16) -0.0002(11) 0.0031(12) 0.0008(12) N9 0.0159(15) 0.0166(15) 0.0133(16) 0.0029(11) 0.0032(12) 0.0021(12) N10 0.0165(16) 0.0165(15) 0.0189(17) 0.0049(12) 0.0031(13) 0.0001(13) C17 0.0142(18) 0.024(2) 0.024(2) 0.0043(16) 0.0051(16) -0.0031(15) C18 0.0165(18) 0.0151(17) 0.0130(18) 0.0029(14) -0.0001(14) -0.0015(14) C19 0.0149(18) 0.022(2) 0.021(2) 0.0040(15) 0.0026(15) 0.0011(15) C20 0.0177(18) 0.0155(17) 0.0124(18) 0.0029(13) 0.0012(14) 0.0009(14) C21 0.026(2) 0.0134(17) 0.019(2) 0.0066(14) 0.0020(15) -0.0003(15) C22 0.0207(19) 0.0133(17) 0.0162(19) 0.0032(14) 0.0040(14) -0.0019(14) C23 0.0119(17) 0.0169(18) 0.023(2) 0.0078(14) 0.0004(14) 0.0015(14) C24 0.0200(19) 0.0166(18) 0.024(2) 0.0066(15) -0.0047(15) -0.0064(15) C25 0.029(2) 0.0115(17) 0.018(2) -0.0004(14) -0.0019(15) -0.0008(15) C26 0.0118(17) 0.0158(17) 0.0130(18) 0.0013(13) 0.0041(13) 0.0026(13) C27 0.0163(18) 0.027(2) 0.0117(19) 0.0044(14) 0.0027(14) 0.0029(15) C28 0.0183(18) 0.0226(19) 0.0127(19) 0.0008(14) 0.0001(14) 0.0002(15) C29 0.015(2) 0.050(3) 0.061(3) 0.037(2) 0.002(2) 0.0063(19) C30 0.026(2) 0.0162(18) 0.023(2) 0.0060(15) 0.0015(16) 0.0005(15) C31 0.0189(19) 0.0183(18) 0.019(2) 0.0028(15) 0.0009(15) -0.0013(15) C32 0.023(2) 0.036(2) 0.037(3) -0.0022(19) 0.0087(18) 0.0097(18) P1 0.0134(5) 0.0229(5) 0.0229(5) 0.0093(4) 0.0025(4) 0.0023(4) F1 0.0401(15) 0.0474(16) 0.0388(17) -0.0110(12) -0.0001(12) 0.0048(12) F2 0.0428(15) 0.0253(13) 0.0355(15) 0.0000(10) 0.0007(11) 0.0012(11) F3 0.0186(12) 0.0482(15) 0.0341(15) 0.0169(11) 0.0032(10) 0.0123(10) F4 0.0270(13) 0.0265(12) 0.0528(17) 0.0225(11) 0.0161(11) 0.0061(10) F5 0.0179(11) 0.0321(13) 0.0482(16) 0.0189(11) 0.0005(10) 0.0055(10) F6 0.0260(13) 0.0641(18) 0.0374(16) 0.0334(13) 0.0015(11) -0.0067(12) P2 0.0217(6) 0.0564(8) 0.0603(9) 0.0367(7) 0.0105(5) 0.0041(5) F7 0.112(4) 0.205(6) 0.089(4) 0.044(4) 0.073(3) 0.056(4) F8 0.0499(18) 0.067(2) 0.053(2) -0.0001(15) 0.0080(15) -0.0083(15) F9 0.097(4) 0.319(9) 0.103(4) 0.109(5) 0.022(3) 0.119(5) F10 0.114(3) 0.0413(18) 0.090(3) 0.0077(18) 0.052(2) -0.0084(19) F11 0.094(3) 0.085(3) 0.074(3) 0.023(2) -0.015(2) 0.031(2) F12 0.197(6) 0.168(5) 0.138(5) 0.001(4) 0.048(4) -0.148(5) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 N5 2.154(3) . . yes Re1 C1 1.953(4) . . yes Re1 C2 1.906(4) . . yes Re1 C3 1.948(4) . . yes Re1 C4 2.211(4) . . yes Re1 C10 2.224(3) . . yes Re2 C26 2.221(3) . . yes Re2 C18 1.910(4) . . yes Re2 N10 2.154(3) . . yes Re2 C17 1.958(4) . . yes Re2 C19 1.951(4) . . yes Re2 C20 2.207(4) . . yes P1 F1 1.601(3) . . yes P1 F6 1.600(3) . . yes P1 F3 1.599(3) . . yes P1 F4 1.604(3) . . yes P1 F2 1.595(3) . . yes P1 F5 1.603(2) . . yes P2 F10 1.607(4) . . yes P2 F11 1.575(5) . . yes P2 F9 1.521(6) . . yes P2 F8 1.626(4) . . yes P2 F7 1.535(5) . . yes P2 F12 1.551(7) . . yes O1 C1 1.156(5) . . yes O2 C2 1.157(4) . . yes O3 C3 1.150(4) . . yes O4 C17 1.147(5) . . yes O5 C18 1.151(4) . . yes O6 C19 1.150(5) . . yes N1 C4 1.368(4) . . yes N1 C5 1.384(4) . . yes N1 C13 1.463(5) . . yes N2 C6 1.382(5) . . yes N2 C7 1.464(5) . . yes N2 C4 1.360(4) . . yes N3 C10 1.354(4) . . yes N3 C12 1.383(5) . . yes N3 C9 1.468(5) . . yes N4 C10 1.366(5) . . yes N4 C11 1.377(5) . . yes N4 C14 1.461(5) . . yes N5 C15 1.142(4) . . yes N6 C29 1.466(4) . . yes N6 C21 1.379(4) . . yes N6 C20 1.360(4) . . yes N7 C22 1.390(4) . . yes N7 C20 1.364(4) . . yes N7 C23 1.467(4) . . yes N8 C26 1.369(5) . . yes N8 C25 1.466(5) . . yes N8 C28 1.386(4) . . yes N9 C26 1.368(4) . . yes N9 C30 1.462(5) . . yes N9 C27 1.384(4) . . yes N10 C31 1.137(5) . . yes C5 C6 1.339(6) . . no C7 C8 1.520(6) . . no C8 C9 1.522(5) . . no C11 C12 1.339(5) . . no C15 C16 1.457(5) . . no C5 H5 0.9500 . . no C6 H6 0.9500 . . no C7 H7A 0.9900 . . no C7 H7B 0.9900 . . no C8 H8A 0.9900 . . no C8 H8B 0.9900 . . no C9 H9A 0.9900 . . no C9 H9B 0.9900 . . no C11 H11 0.9500 . . no C12 H12 0.9500 . . no C13 H13C 0.9800 . . no C13 H13B 0.9800 . . no C13 H13A 0.9800 . . no C14 H14C 0.9800 . . no C14 H14A 0.9800 . . no C14 H14B 0.9800 . . no C16 H16B 0.9800 . . no C16 H16C 0.9800 . . no C16 H16A 0.9800 . . no C21 C22 1.341(5) . . no C23 C24 1.521(5) . . no C24 C25 1.526(5) . . no C27 C28 1.331(5) . . no C31 C32 1.464(6) . . no C21 H21 0.9500 . . no C22 H22 0.9500 . . no C23 H23B 0.9900 . . no C23 H23A 0.9900 . . no C24 H24A 0.9900 . . no C24 H24B 0.9900 . . no C25 H25A 0.9900 . . no C25 H25B 0.9900 . . no C27 H27 0.9500 . . no C28 H28 0.9500 . . no C29 H29A 0.9800 . . no C29 H29B 0.9800 . . no C29 H29C 0.9800 . . no C30 H30A 0.9800 . . no C30 H30C 0.9800 . . no C30 H30B 0.9800 . . no C32 H32B 0.9800 . . no C32 H32C 0.9800 . . no C32 H32A 0.9800 . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Re1 C1 98.86(13) . . . yes N5 Re1 C2 170.83(12) . . . yes N5 Re1 C3 91.81(12) . . . yes N5 Re1 C4 85.07(11) . . . yes N5 Re1 C10 82.99(12) . . . yes C1 Re1 C2 90.31(14) . . . yes C1 Re1 C3 83.99(14) . . . yes C1 Re1 C4 86.69(14) . . . yes C1 Re1 C10 176.47(15) . . . yes C2 Re1 C3 89.34(15) . . . yes C2 Re1 C4 95.32(15) . . . yes C2 Re1 C10 87.87(13) . . . yes C3 Re1 C4 169.60(13) . . . yes C3 Re1 C10 92.96(13) . . . yes C4 Re1 C10 96.50(12) . . . yes C17 Re2 C20 87.26(14) . . . yes C17 Re2 C26 177.44(15) . . . yes C18 Re2 C19 89.12(16) . . . yes C18 Re2 C20 92.93(14) . . . yes C18 Re2 C26 90.76(13) . . . yes C19 Re2 C20 171.49(15) . . . yes C19 Re2 C26 92.97(16) . . . yes C20 Re2 C26 95.26(13) . . . yes N10 Re2 C17 93.22(14) . . . yes N10 Re2 C18 178.01(12) . . . yes N10 Re2 C19 90.35(14) . . . yes N10 Re2 C20 87.87(12) . . . yes N10 Re2 C26 87.35(12) . . . yes C17 Re2 C18 88.64(15) . . . yes C17 Re2 C19 84.54(17) . . . yes F1 P1 F3 89.74(13) . . . yes F1 P1 F4 89.81(14) . . . yes F1 P1 F5 89.84(13) . . . yes F1 P1 F6 90.19(14) . . . yes F2 P1 F3 89.99(13) . . . yes F2 P1 F4 89.64(14) . . . yes F2 P1 F5 90.44(13) . . . yes F2 P1 F6 90.36(14) . . . yes F1 P1 F2 179.38(15) . . . yes F3 P1 F4 90.03(13) . . . yes F3 P1 F5 179.57(15) . . . yes F3 P1 F6 89.66(13) . . . yes F4 P1 F5 90.06(13) . . . yes F4 P1 F6 179.68(14) . . . yes F5 P1 F6 90.26(13) . . . yes F9 P2 F10 91.8(3) . . . yes F7 P2 F9 90.5(3) . . . yes F7 P2 F10 92.9(3) . . . yes F7 P2 F11 91.5(3) . . . yes F7 P2 F12 88.9(3) . . . yes F8 P2 F9 89.4(3) . . . yes F8 P2 F10 89.3(2) . . . yes F8 P2 F11 88.8(2) . . . yes F8 P2 F12 88.9(3) . . . yes F9 P2 F11 176.2(3) . . . yes F9 P2 F12 95.1(4) . . . yes F10 P2 F11 84.9(2) . . . yes F10 P2 F12 172.9(3) . . . yes F11 P2 F12 88.2(3) . . . yes F7 P2 F8 177.8(3) . . . yes C4 N1 C13 128.1(3) . . . yes C4 N1 C5 111.5(3) . . . yes C5 N1 C13 120.4(3) . . . yes C6 N2 C7 121.4(3) . . . yes C4 N2 C6 112.2(3) . . . yes C4 N2 C7 124.9(3) . . . yes C9 N3 C10 126.9(3) . . . yes C9 N3 C12 121.0(3) . . . yes C10 N3 C12 111.6(3) . . . yes C11 N4 C14 120.7(3) . . . yes C10 N4 C11 111.2(3) . . . yes C10 N4 C14 128.1(3) . . . yes Re1 N5 C15 170.6(3) . . . yes C20 N6 C29 127.5(3) . . . yes C20 N6 C21 111.7(3) . . . yes C21 N6 C29 120.7(3) . . . yes C22 N7 C23 120.9(3) . . . yes C20 N7 C22 111.5(3) . . . yes C20 N7 C23 125.4(3) . . . yes C25 N8 C26 127.7(3) . . . yes C25 N8 C28 119.5(3) . . . yes C26 N8 C28 111.9(3) . . . yes C27 N9 C30 120.9(3) . . . yes C26 N9 C27 111.5(3) . . . yes C26 N9 C30 127.6(3) . . . yes Re2 N10 C31 171.7(3) . . . yes Re1 C1 O1 174.9(3) . . . yes Re1 C2 O2 176.4(3) . . . yes Re1 C3 O3 172.9(3) . . . yes Re1 C4 N2 130.5(3) . . . yes N1 C4 N2 102.9(3) . . . yes Re1 C4 N1 126.5(2) . . . yes N1 C5 C6 107.0(3) . . . yes N2 C6 C5 106.4(3) . . . yes N2 C7 C8 109.8(3) . . . yes C7 C8 C9 112.5(3) . . . no N3 C9 C8 110.7(3) . . . yes N3 C10 N4 103.6(3) . . . yes Re1 C10 N4 126.5(2) . . . yes Re1 C10 N3 129.8(3) . . . yes N4 C11 C12 107.0(4) . . . yes N3 C12 C11 106.6(4) . . . yes N5 C15 C16 178.2(4) . . . yes C6 C5 H5 126.00 . . . no N1 C5 H5 127.00 . . . no N2 C6 H6 127.00 . . . no C5 C6 H6 127.00 . . . no C8 C7 H7B 110.00 . . . no C8 C7 H7A 110.00 . . . no N2 C7 H7B 110.00 . . . no N2 C7 H7A 110.00 . . . no H7A C7 H7B 108.00 . . . no C7 C8 H8A 109.00 . . . no C9 C8 H8B 109.00 . . . no H8A C8 H8B 108.00 . . . no C7 C8 H8B 109.00 . . . no C9 C8 H8A 109.00 . . . no N3 C9 H9B 110.00 . . . no H9A C9 H9B 108.00 . . . no C8 C9 H9A 109.00 . . . no N3 C9 H9A 110.00 . . . no C8 C9 H9B 110.00 . . . no C12 C11 H11 127.00 . . . no N4 C11 H11 126.00 . . . no C11 C12 H12 127.00 . . . no N3 C12 H12 127.00 . . . no H13A C13 H13C 109.00 . . . no N1 C13 H13B 109.00 . . . no H13B C13 H13C 109.00 . . . no N1 C13 H13A 109.00 . . . no N1 C13 H13C 109.00 . . . no H13A C13 H13B 110.00 . . . no H14A C14 H14C 109.00 . . . no N4 C14 H14B 110.00 . . . no N4 C14 H14A 110.00 . . . no H14A C14 H14B 109.00 . . . no N4 C14 H14C 109.00 . . . no H14B C14 H14C 109.00 . . . no H16A C16 H16C 109.00 . . . no C15 C16 H16A 109.00 . . . no C15 C16 H16B 110.00 . . . no H16B C16 H16C 110.00 . . . no H16A C16 H16B 109.00 . . . no C15 C16 H16C 109.00 . . . no Re2 C17 O4 175.8(3) . . . yes Re2 C18 O5 179.1(3) . . . yes Re2 C19 O6 173.5(4) . . . yes Re2 C20 N6 128.1(2) . . . yes Re2 C20 N7 128.0(2) . . . yes N6 C20 N7 103.4(3) . . . yes N6 C21 C22 107.1(3) . . . yes N7 C22 C21 106.3(3) . . . yes N7 C23 C24 108.8(3) . . . yes C23 C24 C25 113.1(3) . . . no N8 C25 C24 110.2(3) . . . yes Re2 C26 N8 130.7(3) . . . yes Re2 C26 N9 126.6(2) . . . yes N8 C26 N9 102.8(3) . . . yes N9 C27 C28 107.4(3) . . . yes N8 C28 C27 106.5(3) . . . yes N10 C31 C32 178.5(4) . . . yes C22 C21 H21 126.00 . . . no N6 C21 H21 126.00 . . . no N7 C22 H22 127.00 . . . no C21 C22 H22 127.00 . . . no H23A C23 H23B 108.00 . . . no C24 C23 H23B 110.00 . . . no N7 C23 H23A 110.00 . . . no N7 C23 H23B 110.00 . . . no C24 C23 H23A 110.00 . . . no C23 C24 H24A 109.00 . . . no C25 C24 H24B 109.00 . . . no C23 C24 H24B 109.00 . . . no C25 C24 H24A 109.00 . . . no H24A C24 H24B 108.00 . . . no C24 C25 H25A 110.00 . . . no N8 C25 H25A 110.00 . . . no N8 C25 H25B 110.00 . . . no C24 C25 H25B 110.00 . . . no H25A C25 H25B 108.00 . . . no N9 C27 H27 126.00 . . . no C28 C27 H27 126.00 . . . no C27 C28 H28 127.00 . . . no N8 C28 H28 127.00 . . . no N6 C29 H29B 110.00 . . . no N6 C29 H29A 109.00 . . . no H29A C29 H29C 109.00 . . . no N6 C29 H29C 109.00 . . . no H29A C29 H29B 109.00 . . . no H29B C29 H29C 109.00 . . . no N9 C30 H30C 109.00 . . . no N9 C30 H30A 109.00 . . . no N9 C30 H30B 109.00 . . . no H30B C30 H30C 110.00 . . . no H30A C30 H30B 109.00 . . . no H30A C30 H30C 109.00 . . . no H32B C32 H32C 109.00 . . . no C31 C32 H32A 109.00 . . . no C31 C32 H32B 109.00 . . . no C31 C32 H32C 109.00 . . . no H32A C32 H32B 110.00 . . . no H32A C32 H32C 109.00 . . . no loop_ _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 N5 Re1 C4 N1 -61.3(3) . . . . no N5 Re1 C4 N2 124.1(3) . . . . no C1 Re1 C4 N1 37.9(3) . . . . no C1 Re1 C4 N2 -136.7(3) . . . . no C2 Re1 C4 N1 127.9(3) . . . . no C2 Re1 C4 N2 -46.7(3) . . . . no C10 Re1 C4 N1 -143.7(3) . . . . no C10 Re1 C4 N2 41.7(3) . . . . no N5 Re1 C10 N3 -57.9(3) . . . . no N5 Re1 C10 N4 119.2(3) . . . . no C2 Re1 C10 N3 121.4(4) . . . . no C2 Re1 C10 N4 -61.5(3) . . . . no C3 Re1 C10 N3 -149.4(3) . . . . no C3 Re1 C10 N4 27.7(3) . . . . no C4 Re1 C10 N3 26.3(4) . . . . no C4 Re1 C10 N4 -156.6(3) . . . . no C20 Re2 C26 N8 20.6(3) . . . . no N10 Re2 C20 N6 -52.4(3) . . . . no N10 Re2 C20 N7 136.9(3) . . . . no C17 Re2 C20 N6 40.9(3) . . . . no C17 Re2 C20 N7 -129.8(3) . . . . no C18 Re2 C20 N6 129.4(3) . . . . no C18 Re2 C20 N7 -41.3(3) . . . . no C26 Re2 C20 N6 -139.6(3) . . . . no C26 Re2 C20 N7 49.8(3) . . . . no N10 Re2 C26 N8 -67.1(3) . . . . no N10 Re2 C26 N9 113.2(3) . . . . no C18 Re2 C26 N8 113.6(3) . . . . no C18 Re2 C26 N9 -66.2(3) . . . . no C19 Re2 C26 N8 -157.3(3) . . . . no C19 Re2 C26 N9 23.0(3) . . . . no C20 Re2 C26 N9 -159.2(3) . . . . no C5 N1 C4 Re1 -175.7(3) . . . . no C5 N1 C4 N2 0.1(4) . . . . no C13 N1 C4 Re1 4.2(5) . . . . no C13 N1 C4 N2 179.9(3) . . . . no C4 N1 C5 C6 -0.1(4) . . . . no C13 N1 C5 C6 180.0(3) . . . . no C6 N2 C4 Re1 175.6(3) . . . . no C6 N2 C4 N1 0.1(4) . . . . no C7 N2 C4 Re1 -18.0(5) . . . . no C7 N2 C4 N1 166.5(3) . . . . no C4 N2 C6 C5 -0.1(4) . . . . no C7 N2 C6 C5 -167.1(3) . . . . no C4 N2 C7 C8 -86.5(4) . . . . no C6 N2 C7 C8 78.8(4) . . . . no C10 N3 C9 C8 -87.9(5) . . . . no C12 N3 C9 C8 82.3(5) . . . . no C9 N3 C10 N4 170.5(3) . . . . no C12 N3 C10 Re1 177.2(3) . . . . no C12 N3 C10 N4 -0.5(4) . . . . no C9 N3 C12 C11 -171.6(3) . . . . no C10 N3 C12 C11 0.0(4) . . . . no C9 N3 C10 Re1 -11.9(6) . . . . no C11 N4 C10 N3 0.8(4) . . . . no C14 N4 C10 Re1 1.2(6) . . . . no C11 N4 C10 Re1 -177.0(3) . . . . no C10 N4 C11 C12 -0.8(4) . . . . no C14 N4 C11 C12 -179.1(4) . . . . no C14 N4 C10 N3 179.0(4) . . . . no C29 N6 C20 Re2 10.6(5) . . . . no C20 N6 C21 C22 0.3(4) . . . . no C29 N6 C21 C22 176.8(4) . . . . no C29 N6 C20 N7 -177.0(4) . . . . no C21 N6 C20 Re2 -173.2(2) . . . . no C21 N6 C20 N7 -0.7(4) . . . . no C23 N7 C22 C21 -164.6(3) . . . . no C20 N7 C23 C24 -85.1(4) . . . . no C22 N7 C23 C24 76.3(4) . . . . no C23 N7 C20 Re2 -23.7(5) . . . . no C22 N7 C20 Re2 173.4(2) . . . . no C22 N7 C20 N6 0.9(4) . . . . no C23 N7 C20 N6 163.8(3) . . . . no C20 N7 C22 C21 -0.8(4) . . . . no C26 N8 C25 C24 -86.4(5) . . . . no C28 N8 C26 Re2 -178.8(3) . . . . no C28 N8 C26 N9 1.0(4) . . . . no C25 N8 C28 C27 -170.9(3) . . . . no C26 N8 C28 C27 -1.1(4) . . . . no C28 N8 C25 C24 81.6(4) . . . . no C25 N8 C26 Re2 -10.1(6) . . . . no C25 N8 C26 N9 169.7(3) . . . . no C26 N9 C27 C28 -0.1(4) . . . . no C30 N9 C27 C28 176.3(3) . . . . no C27 N9 C26 N8 -0.5(4) . . . . no C30 N9 C26 Re2 3.2(5) . . . . no C27 N9 C26 Re2 179.3(2) . . . . no C30 N9 C26 N8 -176.7(3) . . . . no N1 C5 C6 N2 0.2(5) . . . . no N2 C7 C8 C9 60.2(4) . . . . no C7 C8 C9 N3 68.0(4) . . . . no N4 C11 C12 N3 0.5(4) . . . . no N6 C21 C22 N7 0.3(4) . . . . no N7 C23 C24 C25 58.7(4) . . . . no C23 C24 C25 N8 67.7(4) . . . . no N9 C27 C28 N8 0.7(4) . . . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C5 H5 F11 0.9500 2.5100 3.347(6) 148.00 2_665 yes C6 H6 F4 0.9500 2.5300 3.197(4) 127.00 2_665 yes C9 H9B N2 0.9900 2.5700 2.950(5) 103.00 . yes C13 H13C N5 0.9800 2.5900 3.382(5) 138.00 . yes C13 H13C F3 0.9800 2.5000 3.283(4) 136.00 2_565 yes C14 H14B F4 0.9800 2.4000 3.206(5) 140.00 1_545 yes C16 H16A F7 0.9800 2.5300 3.322(6) 138.00 1_455 yes C16 H16C F6 0.9800 2.5300 3.417(5) 150.00 . yes C21 H21 F6 0.9500 2.4100 3.252(4) 147.00 . yes C22 H22 F8 0.9500 2.4800 3.328(5) 149.00 . yes C23 H23B O5 0.9900 2.5800 3.405(4) 140.00 2_656 yes C25 H25B N7 0.9900 2.5500 2.932(5) 103.00 . yes C27 H27 O2 0.9500 2.5600 3.242(4) 129.00 1_556 yes C32 H32A F12 0.9800 2.4300 3.160(8) 131.00 2_666 yes C32 H32C F9 0.9800 2.4800 3.297(8) 141.00 1_455 yes # Loop Mechanism for Extra Tables(s) #loop_ #_publ_manuscript_incl_extra_item #'_geom_extra_tableA_col_1' #'_geom_extra_tableA_col_2' #'_geom_extra_tableA_col_3' #'_geom_extra_table_head_A' #'_geom_table_footnote_A' #'_geom_extra_tableB_col_1' #'_geom_extra_tableB_col_2' #'_geom_extra_tableB_col_3' #'_geom_extra_table_head_B' #'_geom_table_footnote_B' # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 # ? ? ? # #loop_ #_geom_extra_tableB_col_1 #_geom_extra_tableB_col_2 #_geom_extra_tableB_col_3 # ? ? ? # #_geom_table_footnote_A #; # ? #; # #_geom_table_footnote_B #; # ? #; # #_geom_table_footnote_A #; # ? #; # #_geom_table_footnote_B #; # ? #; _iucr_refine_instructions_details ; ; #===END _database_code_depnum_ccdc_archive 'CCDC 933792' ####################################################################### # # 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_Compound_3b #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_moiety '2(C32 H35 N5 O3 Re), 2(F6 P), C2 H3 N' _chemical_formula_sum 'C66 H73 F12 N11 O6 P2 Re2' _chemical_formula_weight 1778.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 1/2+x,1/2-y,1/2+z _cell_length_a 9.8542(1) _cell_length_b 24.3821(3) _cell_length_c 29.5971(4) _cell_angle_alpha 90 _cell_angle_beta 96.311(1) _cell_angle_gamma 90 _cell_volume 7068.08(15) _cell_formula_units_Z 4 _cell_measurement_temperature 123 _cell_measurement_reflns_used 9934 _cell_measurement_theta_min 2.2409 _cell_measurement_theta_max 25.3989 _exptl_crystal_description fragment _exptl_crystal_colour yellow _exptl_crystal_size_max 0.550 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_min 0.080 _exptl_crystal_density_diffrn 1.671 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 3528 _exptl_absorpt_coefficient_mu 3.557 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS, Bruker, 2008b' _exptl_absorpt_correction_T_min 0.245 _exptl_absorpt_correction_T_max 0.764 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; Diffractometer operator A. Poethig scanspeed 10 s per frame dx 60 mm 5248 frames measured in 11 data sets phi-scans with delta_phi = 0.5 omega-scans with delta_omega = 0.5 ; _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' \k-geometry diffractometer ' _diffrn_measurement_device_type ' Bruker APEX-II CCD ' _diffrn_measurement_method ' phi- and omega-rotation ' _diffrn_detector ' CCD plate ' _diffrn_detector_area_resol_mean 16 # number of measured reflections (redundant set) _diffrn_reflns_number 189575 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 25.53 _diffrn_reflns_theta_full 25.53 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 13124 # number of observed reflections (> n sig(I)) _reflns_number_gt 11348 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX II Control Software (Bruker, 2008a)' _computing_cell_refinement 'SAINT (Bruker, 2008b)' _computing_data_reduction 'SAINT (Bruker, 2008b)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997), SHELXLE (Huebschle, 2011)' _computing_molecular_graphics 'PLATON (Spek, 2011)' _computing_publication_material 'PLATON (Spek, 2011), enCIFer (Allen, 2004)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0175P)^2^+8.6376P] 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_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 13124 _refine_ls_number_parameters 962 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0219 _refine_ls_wR_factor_ref 0.0461 _refine_ls_wR_factor_gt 0.0435 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.049 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.938 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.080 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re Uani 0.61223(1) 0.38480(1) 0.37492(1) 1.000 0.0149(1) d . . . O1 O Uani 0.8006(2) 0.30542(9) 0.43417(8) 1.000 0.0310(8) d . . . O2 O Uani 0.4225(2) 0.38555(9) 0.45062(8) 1.000 0.0321(8) d . . . O3 O Uani 0.5189(2) 0.26600(8) 0.35274(7) 1.000 0.0277(7) d . . . N1 N Uani 0.8017(2) 0.47049(10) 0.43667(8) 1.000 0.0179(8) d . . . N2 N Uani 0.6785(2) 0.51721(9) 0.38699(8) 1.000 0.0180(7) d . . . N3 N Uani 0.3574(2) 0.46071(10) 0.33596(8) 1.000 0.0193(8) d . . . N4 N Uani 0.4109(2) 0.40913(10) 0.28247(8) 1.000 0.0189(8) d . . . N5 N Uani 0.7514(2) 0.39070(10) 0.32464(8) 1.000 0.0198(8) d . . . C1 C Uani 0.7409(3) 0.33925(12) 0.41406(10) 1.000 0.0211(9) d . . . C2 C Uani 0.4929(3) 0.38483(11) 0.42187(10) 1.000 0.0203(9) d . . . C3 C Uani 0.5474(3) 0.31145(12) 0.35765(10) 1.000 0.0203(9) d . . . C4 C Uani 0.7056(3) 0.46420(11) 0.40003(10) 1.000 0.0167(9) d . . . C5 C Uani 0.8303(3) 0.52515(12) 0.44619(11) 1.000 0.0239(10) d . . . C6 C Uani 0.7527(3) 0.55427(12) 0.41521(11) 1.000 0.0238(10) d . . . C7 C Uani 0.5870(3) 0.53700(12) 0.34818(10) 1.000 0.0203(9) d . . . C8 C Uani 0.4454(3) 0.55008(12) 0.36170(10) 1.000 0.0216(9) d . . . C9 C Uani 0.3704(3) 0.49870(12) 0.37471(10) 1.000 0.0214(9) d . . . C10 C Uani 0.4525(3) 0.42274(11) 0.32690(10) 1.000 0.0173(9) d . . . C11 C Uani 0.2948(3) 0.43779(12) 0.26568(11) 1.000 0.0242(10) d . . . C12 C Uani 0.2618(3) 0.47018(12) 0.29904(11) 1.000 0.0235(9) d . . . C13 C Uani 0.8768(3) 0.42866(12) 0.46340(10) 1.000 0.0190(9) d . . . C14 C Uani 0.9957(3) 0.40737(12) 0.44836(10) 1.000 0.0204(9) d . . . C15 C Uani 1.0674(3) 0.36820(13) 0.47582(11) 1.000 0.0258(10) d . . . C16 C Uani 1.0247(3) 0.35136(13) 0.51666(11) 1.000 0.0277(10) d . . . C17 C Uani 0.9101(3) 0.37535(13) 0.53126(10) 1.000 0.0284(10) d . . . C18 C Uani 0.8341(3) 0.41451(12) 0.50527(10) 1.000 0.0222(9) d . . . C19 C Uani 1.0449(3) 0.42448(14) 0.40422(11) 1.000 0.0289(10) d . . . C20 C Uani 1.1020(4) 0.30773(14) 0.54471(12) 1.000 0.0454(14) d . . . C21 C Uani 0.7116(3) 0.44172(14) 0.52212(11) 1.000 0.0339(11) d . . . C22 C Uani 0.4709(3) 0.36927(12) 0.25456(10) 1.000 0.0205(9) d . . . C23 C Uani 0.4187(3) 0.31579(12) 0.25300(10) 1.000 0.0231(10) d . . . C24 C Uani 0.4751(3) 0.27846(13) 0.22481(10) 1.000 0.0242(10) d . . . C25 C Uani 0.5771(3) 0.29342(13) 0.19815(10) 1.000 0.0255(10) d . . . C26 C Uani 0.6197(3) 0.34796(13) 0.19893(10) 1.000 0.0253(10) d . . . C27 C Uani 0.5669(3) 0.38685(12) 0.22648(10) 1.000 0.0218(9) d . . . C28 C Uani 0.2995(3) 0.30056(13) 0.27848(11) 1.000 0.0284(10) d . . . C29 C Uani 0.6370(4) 0.25212(14) 0.16792(11) 1.000 0.0345(11) d . . . C30 C Uani 0.6067(4) 0.44637(13) 0.22370(11) 1.000 0.0308(11) d . . . C31 C Uani 0.8335(3) 0.39516(13) 0.30071(11) 1.000 0.0249(10) d . . . C32 C Uani 0.9391(4) 0.40247(17) 0.27052(13) 1.000 0.0454(14) d . . . Re2 Re Uani 0.12264(1) 0.17662(1) 0.40694(1) 1.000 0.0160(1) d . . . O4 O Uani 0.0329(2) 0.28387(9) 0.35690(8) 1.000 0.0308(8) d . . . O5 O Uani -0.0709(2) 0.20441(9) 0.47860(8) 1.000 0.0288(7) d . . . O6 O Uani 0.3119(2) 0.26958(9) 0.44710(8) 1.000 0.0322(8) d . . . N6 N Uani -0.0853(2) 0.12864(9) 0.32326(8) 1.000 0.0177(7) d . . . N7 N Uani -0.1259(2) 0.09034(10) 0.38548(8) 1.000 0.0193(8) d . . . N8 N Uani 0.2067(2) 0.05075(10) 0.44150(8) 1.000 0.0195(8) d . . . N9 N Uani 0.3240(2) 0.10963(10) 0.48239(8) 1.000 0.0212(8) d . . . N10 N Uani 0.2634(2) 0.15623(10) 0.35979(8) 1.000 0.0196(8) d . . . C33 C Uani 0.0590(3) 0.24185(13) 0.37317(10) 1.000 0.0203(9) d . . . C34 C Uani 0.0011(3) 0.19341(11) 0.45158(10) 1.000 0.0205(9) d . . . C35 C Uani 0.2506(3) 0.23122(13) 0.43525(10) 1.000 0.0218(9) d . . . C36 C Uani -0.0387(3) 0.12676(11) 0.36868(10) 1.000 0.0185(9) d . . . C37 C Uani -0.1964(3) 0.09411(12) 0.31291(11) 1.000 0.0234(10) d . . . C38 C Uani -0.2213(3) 0.07002(13) 0.35191(11) 1.000 0.0249(10) d . . . C39 C Uani -0.1049(3) 0.06423(12) 0.43023(10) 1.000 0.0228(10) d . . . C40 C Uani -0.0249(3) 0.01121(12) 0.42629(11) 1.000 0.0244(10) d . . . C41 C Uani 0.1121(3) 0.02133(12) 0.40843(10) 1.000 0.0223(9) d . . . C42 C Uani 0.2238(3) 0.10606(11) 0.44638(10) 1.000 0.0178(9) d . . . C43 C Uani 0.3638(3) 0.05851(13) 0.49917(11) 1.000 0.0268(10) d . . . C44 C Uani 0.2906(3) 0.02161(13) 0.47355(10) 1.000 0.0249(10) d . . . C45 C Uani -0.0348(3) 0.16153(12) 0.28819(10) 1.000 0.0178(9) d . . . C46 C Uani 0.0648(3) 0.13940(12) 0.26339(10) 1.000 0.0200(9) d . . . C47 C Uani 0.1070(3) 0.17112(13) 0.22831(10) 1.000 0.0249(10) d . . . C48 C Uani 0.0496(3) 0.22183(13) 0.21678(10) 1.000 0.0259(10) d . . . C49 C Uani -0.0525(3) 0.24108(13) 0.24117(11) 1.000 0.0256(10) d . . . C50 C Uani -0.0985(3) 0.21155(12) 0.27683(10) 1.000 0.0217(9) d . . . C51 C Uani 0.1190(3) 0.08214(12) 0.27215(11) 1.000 0.0267(10) d . . . C52 C Uani 0.0968(4) 0.25503(15) 0.17833(11) 1.000 0.0382(11) d . . . C53 C Uani -0.2171(3) 0.23134(13) 0.30000(12) 1.000 0.0287(11) d . . . C54 C Uani 0.3904(3) 0.15832(12) 0.50163(10) 1.000 0.0221(9) d . . . C55 C Uani 0.5091(3) 0.17672(14) 0.48474(11) 1.000 0.0280(10) d . . . C56 C Uani 0.5707(3) 0.22362(14) 0.50438(12) 1.000 0.0332(11) d . . . C57 C Uani 0.5172(4) 0.25124(13) 0.53934(12) 1.000 0.0335(11) d . . . C58 C Uani 0.4038(3) 0.22946(13) 0.55669(11) 1.000 0.0288(10) d . . . C59 C Uani 0.3380(3) 0.18258(12) 0.53873(10) 1.000 0.0224(9) d . . . C60 C Uani 0.5675(3) 0.14862(16) 0.44591(12) 1.000 0.0404(14) d . . . C61 C Uani 0.5792(4) 0.30481(15) 0.55690(14) 1.000 0.0502(16) d . . . C62 C Uani 0.2167(3) 0.15882(13) 0.55854(11) 1.000 0.0286(11) d . . . C63 C Uani 0.3482(3) 0.14653(12) 0.33791(11) 1.000 0.0222(10) d . . . C64 C Uani 0.4572(3) 0.13399(15) 0.31058(13) 1.000 0.0372(11) d . . . P1 P Uani -0.01764(9) 0.59419(4) 0.31682(3) 1.000 0.0333(3) d . . . F1A F Uani -0.1078(12) 0.6212(5) 0.3522(4) 0.760(11) 0.057(3) d P A 2 F2A F Uani 0.0773(10) 0.5725(3) 0.2815(3) 0.760(11) 0.117(3) d P A 2 F3A F Uani -0.0928(8) 0.6329(3) 0.27844(13) 0.760(11) 0.068(2) d P A 2 F4A F Uani 0.0858(5) 0.6435(3) 0.3275(3) 0.760(11) 0.109(3) d P A 2 F5A F Uani 0.0624(7) 0.5594(2) 0.35506(16) 0.760(11) 0.077(2) d P A 2 F6A F Uani -0.1218(6) 0.5483(3) 0.3058(3) 0.760(11) 0.107(3) d P A 2 F1 F Uani -0.065(4) 0.6200(14) 0.3578(10) 0.240(11) 0.042(7) d P A 1 F2 F Uani 0.0225(16) 0.5551(5) 0.2753(5) 0.240(11) 0.030(4) d P A 1 F3 F Uani 0.037(4) 0.6445(5) 0.2989(10) 0.240(11) 0.147(12) d P A 1 F4 F Uani -0.1622(17) 0.6038(12) 0.2901(7) 0.240(11) 0.099(8) d P A 1 F5 F Uani -0.073(3) 0.5351(6) 0.3328(6) 0.240(11) 0.091(11) d P A 1 F6 F Uani 0.1219(19) 0.5778(13) 0.3426(11) 0.240(11) 0.164(15) d P A 1 P2 P Uani 0.02800(9) 0.45373(4) 0.14411(3) 1.000 0.0347(3) d . . . F8 F Uani 0.0547(3) 0.42322(12) 0.09894(7) 1.000 0.0769(10) d . . . F9 F Uani 0.0421(3) 0.39836(10) 0.17193(9) 1.000 0.0777(10) d . . . F10 F Uani 0.0022(3) 0.48513(9) 0.18946(7) 1.000 0.0594(9) d . . . F11 F Uani 0.0203(3) 0.51078(12) 0.11845(9) 1.000 0.0872(13) d . . . F12 F Uani -0.1298(2) 0.44688(13) 0.13318(12) 1.000 0.0941(13) d . . . F13 F Uani 0.1874(2) 0.46102(15) 0.15574(10) 1.000 0.0937(13) d . . . N11 N Uani 0.8517(3) 0.10448(12) 0.53997(11) 1.000 0.0437(11) d . . . C65 C Uani 0.8252(3) 0.13324(14) 0.56794(12) 1.000 0.0305(11) d . . . C66 C Uani 0.7915(4) 0.16947(16) 0.60409(13) 1.000 0.0464(12) d . . . H5 H Uiso 0.89300 0.53910 0.47010 1.000 0.0290 c R . . H6 H Uiso 0.74900 0.59310 0.41290 1.000 0.0290 c R . . H7A H Uiso 0.57890 0.50870 0.32400 1.000 0.0240 c R . . H7B H Uiso 0.62630 0.57040 0.33570 1.000 0.0240 c R . . H8A H Uiso 0.45460 0.57580 0.38770 1.000 0.0260 c R . . H8B H Uiso 0.39080 0.56850 0.33600 1.000 0.0260 c R . . H9A H Uiso 0.42190 0.48100 0.40140 1.000 0.0260 c R . . H9B H Uiso 0.27880 0.50870 0.38280 1.000 0.0260 c R . . H11 H Uiso 0.24770 0.43490 0.23600 1.000 0.0290 c R . . H12 H Uiso 0.18710 0.49500 0.29770 1.000 0.0280 c R . . H15 H Uiso 1.14780 0.35260 0.46620 1.000 0.0310 c R . . H17 H Uiso 0.88250 0.36480 0.55980 1.000 0.0340 c R . . H19A H Uiso 1.14340 0.41810 0.40560 1.000 0.0430 c R . . H19B H Uiso 1.02570 0.46350 0.39900 1.000 0.0430 c R . . H19C H Uiso 0.99760 0.40300 0.37930 1.000 0.0430 c R . . H20A H Uiso 1.19250 0.30300 0.53440 1.000 0.0680 c R . . H20B H Uiso 1.05180 0.27300 0.54120 1.000 0.0680 c R . . H20C H Uiso 1.11220 0.31870 0.57680 1.000 0.0680 c R . . H21A H Uiso 0.69460 0.42550 0.55130 1.000 0.0510 c R . . H21B H Uiso 0.63150 0.43620 0.49990 1.000 0.0510 c R . . H21C H Uiso 0.72920 0.48110 0.52610 1.000 0.0510 c R . . H24 H Uiso 0.44320 0.24170 0.22370 1.000 0.0290 c R . . H26 H Uiso 0.68690 0.35880 0.18000 1.000 0.0300 c R . . H28A H Uiso 0.29670 0.26070 0.28220 1.000 0.0420 c R . . H28B H Uiso 0.21440 0.31310 0.26130 1.000 0.0420 c R . . H28C H Uiso 0.31020 0.31810 0.30850 1.000 0.0420 c R . . H29A H Uiso 0.70780 0.26980 0.15220 1.000 0.0520 c R . . H29B H Uiso 0.56480 0.23810 0.14550 1.000 0.0520 c R . . H29C H Uiso 0.67710 0.22170 0.18650 1.000 0.0520 c R . . H30A H Uiso 0.68520 0.44970 0.20620 1.000 0.0460 c R . . H30B H Uiso 0.63110 0.46080 0.25440 1.000 0.0460 c R . . H30C H Uiso 0.52980 0.46730 0.20860 1.000 0.0460 c R . . H32A H Uiso 0.90840 0.38660 0.24070 1.000 0.0680 c R . . H32B H Uiso 1.02290 0.38400 0.28340 1.000 0.0680 c R . . H32C H Uiso 0.95720 0.44170 0.26710 1.000 0.0680 c R . . H37 H Uiso -0.24540 0.08860 0.28380 1.000 0.0280 c R . . H38 H Uiso -0.29090 0.04400 0.35570 1.000 0.0300 c R . . H39A H Uiso -0.19420 0.05610 0.44120 1.000 0.0270 c R . . H39B H Uiso -0.05370 0.08920 0.45230 1.000 0.0270 c R . . H40A H Uiso -0.00930 -0.00640 0.45650 1.000 0.0290 c R . . H40B H Uiso -0.07950 -0.01430 0.40560 1.000 0.0290 c R . . H41A H Uiso 0.15290 -0.01430 0.40120 1.000 0.0270 c R . . H41B H Uiso 0.09750 0.04290 0.38000 1.000 0.0270 c R . . H43 H Uiso 0.43050 0.05110 0.52410 1.000 0.0320 c R . . H44 H Uiso 0.29510 -0.01710 0.47670 1.000 0.0300 c R . . H47 H Uiso 0.17730 0.15760 0.21180 1.000 0.0300 c R . . H49 H Uiso -0.09260 0.27570 0.23330 1.000 0.0310 c R . . H51A H Uiso 0.20440 0.07780 0.25840 1.000 0.0400 c R . . H51B H Uiso 0.05180 0.05550 0.25870 1.000 0.0400 c R . . H51C H Uiso 0.13600 0.07590 0.30500 1.000 0.0400 c R . . H52A H Uiso 0.11490 0.29280 0.18850 1.000 0.0580 c R . . H52B H Uiso 0.02560 0.25490 0.15250 1.000 0.0580 c R . . H52C H Uiso 0.18050 0.23890 0.16910 1.000 0.0580 c R . . H53A H Uiso -0.22350 0.27140 0.29750 1.000 0.0430 c R . . H53B H Uiso -0.20390 0.22080 0.33220 1.000 0.0430 c R . . H53C H Uiso -0.30150 0.21470 0.28550 1.000 0.0430 c R . . H56 H Uiso 0.65170 0.23710 0.49360 1.000 0.0400 c R . . H58 H Uiso 0.36990 0.24720 0.58170 1.000 0.0350 c R . . H60A H Uiso 0.54350 0.10960 0.44570 1.000 0.0600 c R . . H60B H Uiso 0.66710 0.15250 0.44960 1.000 0.0600 c R . . H60C H Uiso 0.53010 0.16540 0.41710 1.000 0.0600 c R . . H61A H Uiso 0.67890 0.30140 0.56110 1.000 0.0760 c R . . H61B H Uiso 0.54610 0.31370 0.58610 1.000 0.0760 c R . . H61C H Uiso 0.55300 0.33400 0.53490 1.000 0.0760 c R . . H62A H Uiso 0.14590 0.14930 0.53390 1.000 0.0430 c R . . H62B H Uiso 0.18070 0.18590 0.57860 1.000 0.0430 c R . . H62C H Uiso 0.24460 0.12580 0.57600 1.000 0.0430 c R . . H64A H Uiso 0.43580 0.14960 0.28010 1.000 0.0560 c R . . H64B H Uiso 0.46690 0.09410 0.30820 1.000 0.0560 c R . . H64C H Uiso 0.54290 0.14970 0.32490 1.000 0.0560 c R . . H66A H Uiso 0.83000 0.20590 0.59980 1.000 0.0700 c R . . H66B H Uiso 0.82980 0.15460 0.63350 1.000 0.0700 c R . . H66C H Uiso 0.69210 0.17230 0.60330 1.000 0.0700 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0163(1) 0.0132(1) 0.0152(1) -0.0017(1) 0.0024(1) -0.0023(1) O1 0.0343(13) 0.0196(12) 0.0362(14) 0.0040(10) -0.0097(11) -0.0020(10) O2 0.0370(13) 0.0308(13) 0.0322(13) -0.0024(11) 0.0205(11) -0.0062(11) O3 0.0325(13) 0.0158(12) 0.0344(13) -0.0037(10) 0.0016(10) -0.0055(10) N1 0.0190(13) 0.0171(13) 0.0178(13) -0.0028(10) 0.0028(10) -0.0048(10) N2 0.0196(13) 0.0143(12) 0.0204(13) 0.0005(10) 0.0036(11) -0.0036(10) N3 0.0186(13) 0.0179(13) 0.0217(14) -0.0047(10) 0.0039(11) -0.0002(10) N4 0.0202(13) 0.0191(13) 0.0171(13) -0.0031(10) 0.0011(10) 0.0028(10) N5 0.0190(13) 0.0182(13) 0.0217(14) -0.0041(11) -0.0001(11) -0.0025(10) C1 0.0235(16) 0.0194(16) 0.0205(17) -0.0048(13) 0.0024(13) -0.0074(13) C2 0.0257(16) 0.0112(14) 0.0233(17) -0.0033(12) -0.0001(14) -0.0046(12) C3 0.0181(15) 0.0226(17) 0.0203(16) -0.0030(13) 0.0033(13) -0.0004(12) C4 0.0177(15) 0.0158(15) 0.0176(15) -0.0007(12) 0.0062(12) -0.0029(12) C5 0.0244(16) 0.0189(16) 0.0276(18) -0.0078(13) -0.0003(14) -0.0078(13) C6 0.0263(17) 0.0155(15) 0.0297(18) -0.0041(13) 0.0030(14) -0.0065(13) C7 0.0256(16) 0.0159(15) 0.0196(16) 0.0009(12) 0.0033(13) -0.0028(12) C8 0.0276(17) 0.0159(15) 0.0212(16) -0.0028(12) 0.0021(13) 0.0016(13) C9 0.0241(16) 0.0187(15) 0.0225(17) -0.0075(13) 0.0076(13) 0.0014(13) C10 0.0183(15) 0.0132(14) 0.0208(16) -0.0019(12) 0.0044(12) -0.0023(12) C11 0.0224(16) 0.0237(17) 0.0242(17) -0.0005(13) -0.0071(13) 0.0030(13) C12 0.0163(15) 0.0220(16) 0.0313(18) -0.0030(14) -0.0007(13) 0.0036(13) C13 0.0242(16) 0.0161(15) 0.0157(15) -0.0022(12) -0.0019(13) -0.0056(12) C14 0.0214(15) 0.0176(15) 0.0218(16) -0.0051(13) 0.0006(13) -0.0056(12) C15 0.0255(17) 0.0235(17) 0.0262(18) -0.0066(14) -0.0068(14) -0.0013(13) C16 0.041(2) 0.0187(16) 0.0210(17) -0.0024(13) -0.0074(15) -0.0060(15) C17 0.046(2) 0.0246(17) 0.0140(16) -0.0013(13) 0.0010(15) -0.0115(15) C18 0.0272(17) 0.0213(16) 0.0183(16) -0.0047(13) 0.0030(13) -0.0115(13) C19 0.0245(17) 0.0363(19) 0.0265(18) 0.0012(15) 0.0050(14) -0.0033(14) C20 0.071(3) 0.029(2) 0.031(2) 0.0019(16) -0.018(2) 0.0030(19) C21 0.042(2) 0.038(2) 0.0240(18) -0.0097(15) 0.0143(16) -0.0083(17) C22 0.0233(16) 0.0198(16) 0.0168(16) -0.0039(12) -0.0048(13) 0.0058(13) C23 0.0254(17) 0.0226(17) 0.0194(16) -0.0043(13) -0.0055(13) 0.0013(13) C24 0.0269(17) 0.0203(16) 0.0232(17) -0.0064(13) -0.0067(14) 0.0015(13) C25 0.0328(18) 0.0260(17) 0.0159(16) -0.0046(13) -0.0047(14) 0.0084(14) C26 0.0340(18) 0.0276(17) 0.0145(16) 0.0005(13) 0.0030(14) 0.0057(14) C27 0.0284(17) 0.0228(16) 0.0134(15) 0.0013(12) -0.0013(13) 0.0045(13) C28 0.0233(17) 0.0257(17) 0.035(2) -0.0077(15) -0.0023(15) -0.0036(14) C29 0.049(2) 0.0298(19) 0.0249(19) -0.0091(15) 0.0045(16) 0.0083(16) C30 0.044(2) 0.0225(17) 0.0274(19) 0.0017(14) 0.0102(16) 0.0030(15) C31 0.0223(16) 0.0300(19) 0.0227(17) -0.0057(14) 0.0043(14) -0.0049(14) C32 0.037(2) 0.063(3) 0.040(2) -0.007(2) 0.0209(18) -0.0122(19) Re2 0.0170(1) 0.0142(1) 0.0166(1) -0.0003(1) 0.0011(1) -0.0006(1) O4 0.0405(14) 0.0201(12) 0.0306(13) 0.0046(10) -0.0019(11) 0.0019(10) O5 0.0338(13) 0.0247(12) 0.0306(13) -0.0001(10) 0.0163(11) 0.0035(10) O6 0.0329(13) 0.0213(12) 0.0394(14) -0.0023(10) -0.0091(11) -0.0074(10) N6 0.0169(12) 0.0172(13) 0.0187(13) -0.0006(10) 0.0003(10) -0.0013(10) N7 0.0191(13) 0.0185(13) 0.0206(14) 0.0024(11) 0.0039(11) -0.0024(10) N8 0.0230(13) 0.0175(13) 0.0177(13) -0.0005(10) 0.0016(11) 0.0023(10) N9 0.0227(13) 0.0206(13) 0.0192(14) -0.0021(11) -0.0024(11) 0.0010(11) N10 0.0198(13) 0.0191(13) 0.0193(14) 0.0000(11) -0.0006(11) -0.0036(11) C33 0.0185(15) 0.0252(17) 0.0169(16) -0.0034(13) 0.0000(12) -0.0034(13) C34 0.0262(17) 0.0121(14) 0.0215(17) 0.0026(12) -0.0046(14) -0.0017(12) C35 0.0209(16) 0.0244(17) 0.0196(16) 0.0014(13) -0.0006(13) 0.0036(14) C36 0.0201(15) 0.0150(15) 0.0205(16) 0.0003(12) 0.0027(13) 0.0027(12) C37 0.0194(16) 0.0217(16) 0.0282(18) -0.0009(14) -0.0016(13) -0.0041(13) C38 0.0192(16) 0.0235(17) 0.0318(19) 0.0016(14) 0.0025(14) -0.0035(13) C39 0.0244(16) 0.0232(17) 0.0219(17) 0.0044(13) 0.0071(13) -0.0030(13) C40 0.0298(17) 0.0193(16) 0.0231(17) 0.0035(13) -0.0012(14) -0.0037(13) C41 0.0290(17) 0.0139(15) 0.0233(17) -0.0024(13) -0.0003(14) 0.0002(13) C42 0.0206(15) 0.0179(15) 0.0152(15) -0.0006(12) 0.0029(12) 0.0006(12) C43 0.0290(18) 0.0248(17) 0.0255(18) 0.0044(14) -0.0015(14) 0.0094(14) C44 0.0310(18) 0.0183(16) 0.0240(17) 0.0020(13) -0.0027(14) 0.0048(13) C45 0.0153(15) 0.0213(16) 0.0160(15) -0.0016(12) -0.0017(12) -0.0040(12) C46 0.0219(16) 0.0186(15) 0.0187(16) -0.0058(12) -0.0016(13) -0.0051(12) C47 0.0297(17) 0.0293(18) 0.0167(16) -0.0079(13) 0.0065(14) -0.0082(14) C48 0.0310(18) 0.0283(18) 0.0164(16) 0.0000(13) -0.0058(14) -0.0115(14) C49 0.0271(17) 0.0219(16) 0.0255(18) 0.0042(14) -0.0079(14) -0.0019(14) C50 0.0195(16) 0.0237(17) 0.0206(16) 0.0024(13) -0.0037(13) -0.0013(13) C51 0.0283(17) 0.0242(17) 0.0285(18) -0.0038(14) 0.0068(15) -0.0014(14) C52 0.050(2) 0.043(2) 0.0207(18) 0.0077(16) 0.0000(17) -0.0105(18) C53 0.0224(17) 0.0260(18) 0.037(2) 0.0052(15) 0.0008(15) 0.0053(14) C54 0.0211(16) 0.0212(16) 0.0219(17) 0.0006(13) -0.0064(13) 0.0009(13) C55 0.0205(16) 0.0333(19) 0.0292(18) 0.0047(15) -0.0012(14) 0.0026(14) C56 0.0216(17) 0.040(2) 0.036(2) 0.0076(17) -0.0058(15) -0.0087(15) C57 0.036(2) 0.0245(18) 0.036(2) 0.0042(15) -0.0137(17) -0.0051(15) C58 0.0364(19) 0.0253(18) 0.0222(17) -0.0021(14) -0.0076(15) 0.0026(15) C59 0.0240(16) 0.0225(16) 0.0189(16) 0.0016(13) -0.0055(13) 0.0016(13) C60 0.0259(19) 0.057(3) 0.039(2) -0.0009(19) 0.0063(16) 0.0021(17) C61 0.059(3) 0.034(2) 0.053(3) 0.0004(19) -0.015(2) -0.0180(19) C62 0.0334(19) 0.0288(18) 0.0235(18) -0.0031(14) 0.0023(15) -0.0015(15) C63 0.0217(16) 0.0228(17) 0.0217(17) -0.0023(13) 0.0010(14) -0.0009(13) C64 0.0280(19) 0.046(2) 0.040(2) -0.0043(17) 0.0145(17) -0.0001(16) P1 0.0313(5) 0.0430(5) 0.0278(5) 0.0121(4) 0.0137(4) 0.0148(4) F1A 0.087(7) 0.042(3) 0.052(5) 0.013(3) 0.050(5) 0.018(4) F2A 0.152(7) 0.111(6) 0.108(5) 0.085(4) 0.111(5) 0.111(5) F3A 0.077(4) 0.097(4) 0.0285(19) -0.001(2) 0.003(2) 0.065(3) F4A 0.036(2) 0.100(4) 0.187(7) 0.063(4) 0.001(3) -0.020(2) F5A 0.099(5) 0.083(4) 0.050(2) 0.045(3) 0.016(3) 0.057(3) F6A 0.097(4) 0.061(4) 0.163(7) -0.054(4) 0.018(5) -0.017(3) F1 0.081(18) 0.029(7) 0.015(6) -0.008(5) 0.000(9) 0.024(9) F2 0.063(8) 0.016(5) 0.015(5) -0.006(4) 0.028(5) -0.004(5) F3 0.30(3) 0.013(6) 0.17(2) 0.029(10) 0.22(2) 0.026(13) F4 0.040(8) 0.18(2) 0.068(12) -0.074(13) -0.035(7) 0.062(11) F5 0.21(3) 0.032(7) 0.047(9) -0.008(7) 0.081(13) -0.018(10) F6 0.043(10) 0.21(3) 0.22(3) -0.17(2) -0.065(13) 0.057(12) P2 0.0316(5) 0.0501(6) 0.0230(5) 0.0022(4) 0.0061(4) 0.0129(4) F8 0.093(2) 0.109(2) 0.0270(13) -0.0110(13) -0.0007(13) 0.0692(17) F9 0.123(2) 0.0499(16) 0.0691(18) 0.0131(13) 0.0507(17) 0.0334(15) F10 0.0980(19) 0.0500(14) 0.0343(13) -0.0055(11) 0.0263(13) 0.0032(13) F11 0.136(3) 0.076(2) 0.0571(17) 0.0317(15) 0.0448(18) 0.0366(18) F12 0.0369(14) 0.104(2) 0.138(3) -0.064(2) -0.0053(16) 0.0081(15) F13 0.0381(15) 0.170(3) 0.073(2) 0.013(2) 0.0057(14) -0.0021(17) N11 0.067(2) 0.0267(17) 0.0408(19) 0.0047(14) 0.0210(17) 0.0011(15) C65 0.0331(19) 0.0244(18) 0.034(2) 0.0055(16) 0.0040(16) -0.0040(15) C66 0.048(2) 0.044(2) 0.046(2) -0.0178(19) 0.000(2) -0.0012(19) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 N5 2.136(2) . . yes Re1 C1 1.965(3) . . yes Re1 C2 1.917(3) . . yes Re1 C3 1.948(3) . . yes Re1 C4 2.235(3) . . yes Re1 C10 2.205(3) . . yes Re2 C36 2.212(3) . . yes Re2 C42 2.250(3) . . yes Re2 C33 1.945(3) . . yes Re2 C34 1.922(3) . . yes Re2 N10 2.132(2) . . yes Re2 C35 1.958(3) . . yes P1 F1 1.49(3) . . yes P1 F2 1.638(14) . . yes P1 F5A 1.558(5) . . yes P1 F6A 1.529(7) . . yes P1 F5 1.629(18) . . yes P1 F3 1.46(2) . . yes P1 F4 1.569(18) . . yes P1 F4A 1.585(7) . . yes P1 F6 1.55(2) . . yes P1 F3A 1.595(6) . . yes P1 F1A 1.589(12) . . yes P1 F2A 1.569(9) . . yes P2 F10 1.590(2) . . yes P2 F8 1.577(3) . . yes P2 F9 1.580(3) . . yes P2 F13 1.581(2) . . yes P2 F11 1.583(3) . . yes P2 F12 1.562(2) . . yes O1 C1 1.142(4) . . yes O2 C2 1.156(4) . . yes O3 C3 1.149(4) . . yes O4 C33 1.149(4) . . yes O5 C34 1.157(4) . . yes O6 C35 1.147(4) . . yes N1 C5 1.385(4) . . yes N1 C4 1.368(4) . . yes N1 C13 1.444(4) . . yes N2 C4 1.367(3) . . yes N2 C7 1.462(4) . . yes N2 C6 1.384(4) . . yes N3 C9 1.469(4) . . yes N3 C10 1.365(4) . . yes N3 C12 1.382(4) . . yes N4 C22 1.444(4) . . yes N4 C10 1.374(4) . . yes N4 C11 1.385(4) . . yes N5 C31 1.138(4) . . yes N6 C45 1.443(4) . . yes N6 C36 1.373(4) . . yes N6 C37 1.388(4) . . yes N7 C39 1.464(4) . . yes N7 C38 1.382(4) . . yes N7 C36 1.367(4) . . yes N8 C44 1.384(4) . . yes N8 C41 1.463(4) . . yes N8 C42 1.365(4) . . yes N9 C43 1.383(4) . . yes N9 C54 1.442(4) . . yes N9 C42 1.374(4) . . yes N10 C63 1.137(4) . . yes N11 C65 1.137(5) . . yes C5 C6 1.333(4) . . no C7 C8 1.527(4) . . no C8 C9 1.525(4) . . no C11 C12 1.332(4) . . no C13 C18 1.395(4) . . no C13 C14 1.398(4) . . no C14 C19 1.502(4) . . no C14 C15 1.395(4) . . no C15 C16 1.385(5) . . no C16 C20 1.504(5) . . no C16 C17 1.383(4) . . no C17 C18 1.392(4) . . no C18 C21 1.509(4) . . no C22 C23 1.401(4) . . no C22 C27 1.394(4) . . no C23 C24 1.391(4) . . no C23 C28 1.510(4) . . no C24 C25 1.393(4) . . no C25 C29 1.510(5) . . no C25 C26 1.394(4) . . no C26 C27 1.389(4) . . no C27 C30 1.508(4) . . no C31 C32 1.455(5) . . no C5 H5 0.9500 . . no C6 H6 0.9500 . . no C7 H7A 0.9900 . . no C7 H7B 0.9900 . . no C8 H8B 0.9900 . . no C8 H8A 0.9900 . . no C9 H9B 0.9900 . . no C9 H9A 0.9900 . . no C11 H11 0.9500 . . no C12 H12 0.9500 . . no C15 H15 0.9500 . . no C17 H17 0.9500 . . no C19 H19A 0.9800 . . no C19 H19B 0.9800 . . no C19 H19C 0.9800 . . no C20 H20A 0.9800 . . no C20 H20B 0.9800 . . no C20 H20C 0.9800 . . no C21 H21B 0.9800 . . no C21 H21A 0.9800 . . no C21 H21C 0.9800 . . no C24 H24 0.9500 . . no C26 H26 0.9500 . . no C28 H28C 0.9800 . . no C28 H28A 0.9800 . . no C28 H28B 0.9800 . . no C29 H29C 0.9800 . . no C29 H29B 0.9800 . . no C29 H29A 0.9800 . . no C30 H30C 0.9800 . . no C30 H30B 0.9800 . . no C30 H30A 0.9800 . . no C32 H32C 0.9800 . . no C32 H32A 0.9800 . . no C32 H32B 0.9800 . . no C37 C38 1.342(4) . . no C39 C40 1.525(4) . . no C40 C41 1.523(4) . . no C43 C44 1.336(4) . . no C45 C50 1.396(4) . . no C45 C46 1.397(4) . . no C46 C47 1.394(4) . . no C46 C51 1.507(4) . . no C47 C48 1.387(4) . . no C48 C49 1.383(4) . . no C48 C52 1.511(5) . . no C49 C50 1.394(4) . . no C50 C53 1.498(4) . . no C54 C59 1.395(4) . . no C54 C55 1.396(4) . . no C55 C60 1.506(5) . . no C55 C56 1.392(5) . . no C56 C57 1.386(5) . . no C57 C58 1.386(5) . . no C57 C61 1.510(5) . . no C58 C59 1.391(4) . . no C59 C62 1.504(4) . . no C63 C64 1.447(4) . . no C37 H37 0.9500 . . no C38 H38 0.9500 . . no C39 H39A 0.9900 . . no C39 H39B 0.9900 . . no C40 H40B 0.9900 . . no C40 H40A 0.9900 . . no C41 H41A 0.9900 . . no C41 H41B 0.9900 . . no C43 H43 0.9500 . . no C44 H44 0.9500 . . no C47 H47 0.9500 . . no C49 H49 0.9500 . . no C51 H51C 0.9800 . . no C51 H51A 0.9800 . . no C51 H51B 0.9800 . . no C52 H52A 0.9800 . . no C52 H52B 0.9800 . . no C52 H52C 0.9800 . . no C53 H53A 0.9800 . . no C53 H53C 0.9800 . . no C53 H53B 0.9800 . . no C56 H56 0.9500 . . no C58 H58 0.9500 . . no C60 H60B 0.9800 . . no C60 H60C 0.9800 . . no C60 H60A 0.9800 . . no C61 H61A 0.9800 . . no C61 H61B 0.9800 . . no C61 H61C 0.9800 . . no C62 H62A 0.9800 . . no C62 H62B 0.9800 . . no C62 H62C 0.9800 . . no C64 H64B 0.9800 . . no C64 H64C 0.9800 . . no C64 H64A 0.9800 . . no C65 C66 1.454(5) . . no C66 H66A 0.9800 . . no C66 H66B 0.9800 . . no C66 H66C 0.9800 . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Re1 C1 91.53(11) . . . yes N5 Re1 C2 175.55(10) . . . yes N5 Re1 C3 95.52(11) . . . yes N5 Re1 C4 84.32(10) . . . yes N5 Re1 C10 89.44(10) . . . yes C1 Re1 C2 88.87(12) . . . yes C1 Re1 C3 78.91(12) . . . yes C1 Re1 C4 94.48(11) . . . yes C1 Re1 C10 170.38(11) . . . yes C2 Re1 C3 88.91(12) . . . yes C2 Re1 C4 91.23(11) . . . yes C2 Re1 C10 90.90(12) . . . yes C3 Re1 C4 173.38(11) . . . yes C3 Re1 C10 91.48(11) . . . yes C4 Re1 C10 95.14(10) . . . yes C34 Re2 C42 94.61(11) . . . yes C35 Re2 C36 170.36(11) . . . yes C35 Re2 C42 94.02(12) . . . yes C36 Re2 C42 95.62(10) . . . yes N10 Re2 C33 92.89(11) . . . yes N10 Re2 C34 177.41(11) . . . yes N10 Re2 C35 90.22(11) . . . yes N10 Re2 C36 91.11(10) . . . yes N10 Re2 C42 83.00(10) . . . yes C33 Re2 C34 89.37(12) . . . yes C33 Re2 C35 79.63(13) . . . yes C33 Re2 C36 90.76(11) . . . yes C33 Re2 C42 172.47(12) . . . yes C34 Re2 C35 88.95(12) . . . yes C34 Re2 C36 90.11(12) . . . yes F3A P1 F4A 86.1(4) . . . yes F3A P1 F5A 176.4(4) . . . yes F3A P1 F6A 91.9(4) . . . yes F4A P1 F5A 90.3(4) . . . yes F4 P1 F6 173.7(16) . . . yes F5 P1 F6 86.4(15) . . . yes F5A P1 F6A 91.8(4) . . . yes F1A P1 F2A 175.0(5) . . . yes F1A P1 F3A 88.5(5) . . . yes F1A P1 F4A 87.0(5) . . . yes F1A P1 F5A 91.3(5) . . . yes F1A P1 F6A 91.9(5) . . . yes F2A P1 F3A 89.4(4) . . . yes F2A P1 F4A 88.3(4) . . . yes F2A P1 F5A 90.5(4) . . . yes F2A P1 F6A 92.7(4) . . . yes F3 P1 F4 92.4(17) . . . yes F3 P1 F5 174.6(14) . . . yes F3 P1 F6 93.0(18) . . . yes F4 P1 F5 87.9(14) . . . yes F4A P1 F6A 177.7(3) . . . yes F2 P1 F4 89.4(10) . . . yes F1 P1 F2 169.2(14) . . . yes F1 P1 F3 95.9(17) . . . yes F1 P1 F4 89.9(16) . . . yes F1 P1 F5 89.6(15) . . . yes F1 P1 F6 92.8(18) . . . yes F2 P1 F3 95.0(12) . . . yes F2 P1 F5 79.6(8) . . . yes F2 P1 F6 86.8(13) . . . yes F8 P2 F9 91.46(15) . . . yes F10 P2 F13 90.53(16) . . . yes F11 P2 F12 90.03(17) . . . yes F11 P2 F13 89.99(17) . . . yes F12 P2 F13 179.30(19) . . . yes F9 P2 F10 89.12(13) . . . yes F9 P2 F11 176.59(16) . . . yes F9 P2 F12 92.59(17) . . . yes F8 P2 F10 179.27(16) . . . yes F8 P2 F11 90.66(15) . . . yes F8 P2 F12 91.67(17) . . . yes F8 P2 F13 89.04(16) . . . yes F9 P2 F13 87.38(17) . . . yes F10 P2 F11 88.75(14) . . . yes F10 P2 F12 88.76(17) . . . yes C5 N1 C13 119.2(2) . . . yes C4 N1 C13 128.6(2) . . . yes C4 N1 C5 112.2(2) . . . yes C4 N2 C7 128.2(2) . . . yes C4 N2 C6 111.9(2) . . . yes C6 N2 C7 119.9(2) . . . yes C10 N3 C12 112.4(2) . . . yes C9 N3 C10 125.3(2) . . . yes C9 N3 C12 120.4(2) . . . yes C11 N4 C22 120.6(2) . . . yes C10 N4 C22 127.8(2) . . . yes C10 N4 C11 111.7(2) . . . yes Re1 N5 C31 174.3(2) . . . yes C37 N6 C45 120.3(2) . . . yes C36 N6 C37 111.5(2) . . . yes C36 N6 C45 128.2(2) . . . yes C38 N7 C39 120.8(2) . . . yes C36 N7 C39 125.4(2) . . . yes C36 N7 C38 112.1(2) . . . yes C42 N8 C44 112.2(2) . . . yes C41 N8 C42 128.1(2) . . . yes C41 N8 C44 119.7(2) . . . yes C42 N9 C54 127.9(2) . . . yes C42 N9 C43 111.9(2) . . . yes C43 N9 C54 120.1(2) . . . yes Re2 N10 C63 173.4(2) . . . yes Re1 C1 O1 167.9(3) . . . yes Re1 C2 O2 178.7(2) . . . yes Re1 C3 O3 170.9(3) . . . yes Re1 C4 N1 125.77(19) . . . yes N1 C4 N2 102.4(2) . . . yes Re1 C4 N2 131.7(2) . . . yes N1 C5 C6 106.5(3) . . . yes N2 C6 C5 107.0(3) . . . yes N2 C7 C8 111.4(2) . . . yes C7 C8 C9 112.1(2) . . . no N3 C9 C8 108.9(2) . . . yes Re1 C10 N3 128.0(2) . . . yes Re1 C10 N4 129.2(2) . . . yes N3 C10 N4 102.3(2) . . . yes N4 C11 C12 107.0(3) . . . yes N3 C12 C11 106.6(3) . . . yes N1 C13 C14 119.0(3) . . . yes N1 C13 C18 118.4(3) . . . yes C14 C13 C18 122.4(3) . . . no C13 C14 C15 117.2(3) . . . no C15 C14 C19 120.4(3) . . . no C13 C14 C19 122.4(3) . . . no C14 C15 C16 121.9(3) . . . no C15 C16 C17 119.0(3) . . . no C17 C16 C20 120.6(3) . . . no C15 C16 C20 120.5(3) . . . no C16 C17 C18 121.7(3) . . . no C13 C18 C17 117.7(3) . . . no C13 C18 C21 121.0(3) . . . no C17 C18 C21 121.3(3) . . . no N4 C22 C23 118.3(3) . . . yes N4 C22 C27 118.8(3) . . . yes C23 C22 C27 122.5(3) . . . no C22 C23 C24 117.4(3) . . . no C24 C23 C28 121.5(3) . . . no C22 C23 C28 121.0(3) . . . no C23 C24 C25 122.0(3) . . . no C24 C25 C26 118.4(3) . . . no C24 C25 C29 121.0(3) . . . no C26 C25 C29 120.6(3) . . . no C25 C26 C27 122.0(3) . . . no C22 C27 C26 117.6(3) . . . no C22 C27 C30 121.8(3) . . . no C26 C27 C30 120.6(3) . . . no N5 C31 C32 178.4(3) . . . yes N1 C5 H5 127.00 . . . no C6 C5 H5 127.00 . . . no C5 C6 H6 127.00 . . . no N2 C6 H6 126.00 . . . no H7A C7 H7B 108.00 . . . no C8 C7 H7A 109.00 . . . no C8 C7 H7B 109.00 . . . no N2 C7 H7B 109.00 . . . no N2 C7 H7A 109.00 . . . no C9 C8 H8A 109.00 . . . no C7 C8 H8B 109.00 . . . no C7 C8 H8A 109.00 . . . no C9 C8 H8B 109.00 . . . no H8A C8 H8B 108.00 . . . no N3 C9 H9A 110.00 . . . no C8 C9 H9B 110.00 . . . no H9A C9 H9B 108.00 . . . no C8 C9 H9A 110.00 . . . no N3 C9 H9B 110.00 . . . no C12 C11 H11 127.00 . . . no N4 C11 H11 126.00 . . . no N3 C12 H12 127.00 . . . no C11 C12 H12 127.00 . . . no C14 C15 H15 119.00 . . . no C16 C15 H15 119.00 . . . no C18 C17 H17 119.00 . . . no C16 C17 H17 119.00 . . . no C14 C19 H19C 110.00 . . . no C14 C19 H19B 109.00 . . . no C14 C19 H19A 109.00 . . . no H19A C19 H19B 110.00 . . . no H19A C19 H19C 109.00 . . . no H19B C19 H19C 109.00 . . . no H20B C20 H20C 110.00 . . . no C16 C20 H20B 109.00 . . . no C16 C20 H20C 109.00 . . . no C16 C20 H20A 110.00 . . . no H20A C20 H20C 109.00 . . . no H20A C20 H20B 109.00 . . . no C18 C21 H21C 109.00 . . . no H21A C21 H21C 110.00 . . . no H21B C21 H21C 110.00 . . . no C18 C21 H21A 110.00 . . . no C18 C21 H21B 109.00 . . . no H21A C21 H21B 109.00 . . . no C25 C24 H24 119.00 . . . no C23 C24 H24 119.00 . . . no C27 C26 H26 119.00 . . . no C25 C26 H26 119.00 . . . no C23 C28 H28A 109.00 . . . no H28A C28 H28B 110.00 . . . no H28A C28 H28C 109.00 . . . no C23 C28 H28C 109.00 . . . no H28B C28 H28C 110.00 . . . no C23 C28 H28B 109.00 . . . no C25 C29 H29C 109.00 . . . no C25 C29 H29B 109.00 . . . no H29B C29 H29C 110.00 . . . no H29A C29 H29C 110.00 . . . no C25 C29 H29A 109.00 . . . no H29A C29 H29B 110.00 . . . no C27 C30 H30A 109.00 . . . no C27 C30 H30B 110.00 . . . no C27 C30 H30C 109.00 . . . no H30A C30 H30C 109.00 . . . no H30B C30 H30C 110.00 . . . no H30A C30 H30B 109.00 . . . no C31 C32 H32A 109.00 . . . no H32A C32 H32C 109.00 . . . no H32B C32 H32C 109.00 . . . no C31 C32 H32B 109.00 . . . no C31 C32 H32C 109.00 . . . no H32A C32 H32B 109.00 . . . no Re2 C33 O4 171.5(3) . . . yes Re2 C34 O5 178.8(2) . . . yes Re2 C35 O6 168.0(3) . . . yes N6 C36 N7 102.8(2) . . . yes Re2 C36 N7 128.0(2) . . . yes Re2 C36 N6 128.85(19) . . . yes N6 C37 C38 106.9(3) . . . yes N7 C38 C37 106.7(3) . . . yes N7 C39 C40 108.8(2) . . . yes C39 C40 C41 112.0(2) . . . no N8 C41 C40 111.8(2) . . . yes Re2 C42 N9 126.43(19) . . . yes N8 C42 N9 102.4(2) . . . yes Re2 C42 N8 131.2(2) . . . yes N9 C43 C44 106.8(3) . . . yes N8 C44 C43 106.7(3) . . . yes N6 C45 C46 118.8(3) . . . yes C46 C45 C50 122.3(3) . . . no N6 C45 C50 118.5(3) . . . yes C45 C46 C51 121.6(3) . . . no C47 C46 C51 120.9(3) . . . no C45 C46 C47 117.5(3) . . . no C46 C47 C48 122.1(3) . . . no C49 C48 C52 120.9(3) . . . no C47 C48 C49 118.3(3) . . . no C47 C48 C52 120.8(3) . . . no C48 C49 C50 122.4(3) . . . no C45 C50 C49 117.3(3) . . . no C45 C50 C53 121.6(3) . . . no C49 C50 C53 121.0(3) . . . no C55 C54 C59 122.9(3) . . . no N9 C54 C55 119.0(3) . . . yes N9 C54 C59 117.9(3) . . . yes C54 C55 C60 122.2(3) . . . no C54 C55 C56 117.3(3) . . . no C56 C55 C60 120.5(3) . . . no C55 C56 C57 121.8(3) . . . no C58 C57 C61 121.1(3) . . . no C56 C57 C61 120.3(3) . . . no C56 C57 C58 118.6(3) . . . no C57 C58 C59 122.3(3) . . . no C54 C59 C62 121.5(3) . . . no C54 C59 C58 116.9(3) . . . no C58 C59 C62 121.7(3) . . . no N10 C63 C64 179.3(3) . . . yes C38 C37 H37 127.00 . . . no N6 C37 H37 127.00 . . . no N7 C38 H38 127.00 . . . no C37 C38 H38 127.00 . . . no H39A C39 H39B 108.00 . . . no N7 C39 H39A 110.00 . . . no N7 C39 H39B 110.00 . . . no C40 C39 H39A 110.00 . . . no C40 C39 H39B 110.00 . . . no C39 C40 H40A 109.00 . . . no C39 C40 H40B 109.00 . . . no C41 C40 H40A 109.00 . . . no C41 C40 H40B 109.00 . . . no H40A C40 H40B 108.00 . . . no N8 C41 H41B 109.00 . . . no C40 C41 H41A 109.00 . . . no N8 C41 H41A 109.00 . . . no C40 C41 H41B 109.00 . . . no H41A C41 H41B 108.00 . . . no N9 C43 H43 127.00 . . . no C44 C43 H43 127.00 . . . no N8 C44 H44 127.00 . . . no C43 C44 H44 127.00 . . . no C46 C47 H47 119.00 . . . no C48 C47 H47 119.00 . . . no C48 C49 H49 119.00 . . . no C50 C49 H49 119.00 . . . no H51A C51 H51C 110.00 . . . no H51B C51 H51C 110.00 . . . no C46 C51 H51A 109.00 . . . no C46 C51 H51B 109.00 . . . no C46 C51 H51C 109.00 . . . no H51A C51 H51B 109.00 . . . no H52B C52 H52C 110.00 . . . no C48 C52 H52C 109.00 . . . no C48 C52 H52A 109.00 . . . no C48 C52 H52B 109.00 . . . no H52A C52 H52B 109.00 . . . no H52A C52 H52C 109.00 . . . no C50 C53 H53B 109.00 . . . no C50 C53 H53A 109.00 . . . no C50 C53 H53C 109.00 . . . no H53A C53 H53B 110.00 . . . no H53A C53 H53C 110.00 . . . no H53B C53 H53C 109.00 . . . no C57 C56 H56 119.00 . . . no C55 C56 H56 119.00 . . . no C57 C58 H58 119.00 . . . no C59 C58 H58 119.00 . . . no H60A C60 H60C 109.00 . . . no C55 C60 H60B 109.00 . . . no H60B C60 H60C 109.00 . . . no C55 C60 H60A 110.00 . . . no C55 C60 H60C 110.00 . . . no H60A C60 H60B 109.00 . . . no C57 C61 H61C 109.00 . . . no C57 C61 H61B 109.00 . . . no C57 C61 H61A 109.00 . . . no H61B C61 H61C 110.00 . . . no H61A C61 H61B 109.00 . . . no H61A C61 H61C 109.00 . . . no H62A C62 H62B 110.00 . . . no C59 C62 H62A 109.00 . . . no C59 C62 H62B 109.00 . . . no C59 C62 H62C 109.00 . . . no H62A C62 H62C 109.00 . . . no H62B C62 H62C 109.00 . . . no H64B C64 H64C 109.00 . . . no C63 C64 H64A 110.00 . . . no C63 C64 H64B 110.00 . . . no C63 C64 H64C 109.00 . . . no H64A C64 H64B 109.00 . . . no H64A C64 H64C 110.00 . . . no N11 C65 C66 179.3(4) . . . yes C65 C66 H66A 109.00 . . . no C65 C66 H66B 109.00 . . . no C65 C66 H66C 110.00 . . . no H66A C66 H66B 110.00 . . . no H66A C66 H66C 109.00 . . . no H66B C66 H66C 110.00 . . . no loop_ _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 N5 Re1 C4 N1 -101.5(2) . . . . no N5 Re1 C4 N2 84.3(3) . . . . no C1 Re1 C4 N1 -10.4(3) . . . . no C1 Re1 C4 N2 175.4(3) . . . . no C2 Re1 C4 N1 78.6(3) . . . . no C2 Re1 C4 N2 -95.7(3) . . . . no C10 Re1 C4 N1 169.6(2) . . . . no C10 Re1 C4 N2 -4.6(3) . . . . no N5 Re1 C10 N3 -140.0(2) . . . . no N5 Re1 C10 N4 50.1(3) . . . . no C2 Re1 C10 N3 35.5(3) . . . . no C2 Re1 C10 N4 -134.4(3) . . . . no C3 Re1 C10 N3 124.5(3) . . . . no C3 Re1 C10 N4 -45.4(3) . . . . no C4 Re1 C10 N3 -55.8(3) . . . . no C4 Re1 C10 N4 134.3(3) . . . . no C42 Re2 C36 N6 -135.6(2) . . . . no C42 Re2 C36 N7 51.7(3) . . . . no N10 Re2 C42 N8 -79.4(3) . . . . no N10 Re2 C42 N9 99.5(2) . . . . no C34 Re2 C42 N8 101.6(3) . . . . no C34 Re2 C42 N9 -79.6(3) . . . . no C35 Re2 C42 N8 -169.1(3) . . . . no C35 Re2 C42 N9 9.7(3) . . . . no C36 Re2 C42 N8 11.1(3) . . . . no N10 Re2 C36 N6 -52.5(2) . . . . no N10 Re2 C36 N7 134.8(2) . . . . no C33 Re2 C36 N6 40.4(3) . . . . no C33 Re2 C36 N7 -132.3(3) . . . . no C34 Re2 C36 N6 129.8(3) . . . . no C34 Re2 C36 N7 -42.9(3) . . . . no C36 Re2 C42 N9 -170.1(2) . . . . no C5 N1 C4 Re1 -174.5(2) . . . . no C5 N1 C4 N2 1.1(3) . . . . no C13 N1 C4 N2 -175.6(2) . . . . no C4 N1 C5 C6 -0.5(3) . . . . no C13 N1 C5 C6 176.6(3) . . . . no C4 N1 C13 C14 84.6(4) . . . . no C4 N1 C13 C18 -100.9(3) . . . . no C5 N1 C13 C14 -92.0(3) . . . . no C13 N1 C4 Re1 8.8(4) . . . . no C5 N1 C13 C18 82.5(3) . . . . no C7 N2 C6 C5 -177.6(2) . . . . no C6 N2 C4 Re1 173.8(2) . . . . no C6 N2 C4 N1 -1.4(3) . . . . no C7 N2 C4 Re1 -7.5(4) . . . . no C7 N2 C4 N1 177.3(2) . . . . no C4 N2 C6 C5 1.2(3) . . . . no C4 N2 C7 C8 94.2(3) . . . . no C6 N2 C7 C8 -87.2(3) . . . . no C10 N3 C12 C11 0.3(3) . . . . no C10 N3 C9 C8 86.9(3) . . . . no C12 N3 C9 C8 -76.3(3) . . . . no C9 N3 C10 Re1 23.7(4) . . . . no C9 N3 C10 N4 -164.4(2) . . . . no C12 N3 C10 Re1 -172.0(2) . . . . no C12 N3 C10 N4 0.0(3) . . . . no C9 N3 C12 C11 165.5(2) . . . . no C11 N4 C10 N3 -0.2(3) . . . . no C22 N4 C10 Re1 -6.3(4) . . . . no C22 N4 C10 N3 -178.2(2) . . . . no C10 N4 C11 C12 0.4(3) . . . . no C22 N4 C11 C12 178.5(3) . . . . no C10 N4 C22 C23 93.0(3) . . . . no C10 N4 C22 C27 -94.2(4) . . . . no C11 N4 C22 C23 -84.8(3) . . . . no C11 N4 C22 C27 88.0(3) . . . . no C11 N4 C10 Re1 171.6(2) . . . . no C37 N6 C45 C50 83.4(3) . . . . no C45 N6 C36 Re2 4.2(4) . . . . no C36 N6 C37 C38 0.1(3) . . . . no C45 N6 C37 C38 -178.8(2) . . . . no C45 N6 C36 N7 178.3(2) . . . . no C37 N6 C36 Re2 -174.6(2) . . . . no C37 N6 C36 N7 -0.5(3) . . . . no C37 N6 C45 C46 -89.2(3) . . . . no C36 N6 C45 C46 92.1(4) . . . . no C36 N6 C45 C50 -95.2(3) . . . . no C39 N7 C36 Re2 -19.8(4) . . . . no C39 N7 C36 N6 166.0(2) . . . . no C36 N7 C38 C37 -0.7(3) . . . . no C39 N7 C38 C37 -166.8(3) . . . . no C38 N7 C36 N6 0.7(3) . . . . no C38 N7 C36 Re2 174.9(2) . . . . no C36 N7 C39 C40 -88.9(3) . . . . no C38 N7 C39 C40 75.2(3) . . . . no C44 N8 C41 C40 88.6(3) . . . . no C44 N8 C42 Re2 -179.9(2) . . . . no C41 N8 C42 Re2 -1.3(4) . . . . no C41 N8 C42 N9 179.7(2) . . . . no C42 N8 C41 C40 -89.9(3) . . . . no C42 N8 C44 C43 -0.6(3) . . . . no C44 N8 C42 N9 1.1(3) . . . . no C41 N8 C44 C43 -179.3(2) . . . . no C43 N9 C42 N8 -1.2(3) . . . . no C54 N9 C42 Re2 -2.9(4) . . . . no C54 N9 C42 N8 176.2(2) . . . . no C42 N9 C43 C44 0.9(3) . . . . no C43 N9 C42 Re2 179.7(2) . . . . no C43 N9 C54 C55 86.9(3) . . . . no C43 N9 C54 C59 -88.4(3) . . . . no C42 N9 C54 C55 -90.3(4) . . . . no C42 N9 C54 C59 94.3(4) . . . . no C54 N9 C43 C44 -176.8(2) . . . . no N1 C5 C6 N2 -0.4(3) . . . . no N2 C7 C8 C9 -67.3(3) . . . . no C7 C8 C9 N3 -58.8(3) . . . . no N4 C11 C12 N3 -0.4(3) . . . . no N1 C13 C18 C17 -178.0(3) . . . . no N1 C13 C18 C21 0.6(4) . . . . no C14 C13 C18 C17 -3.7(4) . . . . no C14 C13 C18 C21 175.0(3) . . . . no N1 C13 C14 C15 178.2(3) . . . . no N1 C13 C14 C19 -3.0(4) . . . . no C18 C13 C14 C15 3.9(4) . . . . no C18 C13 C14 C19 -177.3(3) . . . . no C13 C14 C15 C16 -0.9(5) . . . . no C19 C14 C15 C16 -179.8(3) . . . . no C14 C15 C16 C17 -2.1(5) . . . . no C14 C15 C16 C20 178.1(3) . . . . no C20 C16 C17 C18 -177.9(3) . . . . no C15 C16 C17 C18 2.3(5) . . . . no C16 C17 C18 C13 0.5(5) . . . . no C16 C17 C18 C21 -178.1(3) . . . . no N4 C22 C27 C30 -1.6(4) . . . . no C23 C22 C27 C30 170.9(3) . . . . no N4 C22 C23 C28 2.1(4) . . . . no C23 C22 C27 C26 -5.5(4) . . . . no N4 C22 C23 C24 178.1(3) . . . . no N4 C22 C27 C26 -178.0(3) . . . . no C27 C22 C23 C24 5.5(4) . . . . no C27 C22 C23 C28 -170.4(3) . . . . no C22 C23 C24 C25 -1.6(4) . . . . no C28 C23 C24 C25 174.4(3) . . . . no C23 C24 C25 C29 179.8(3) . . . . no C23 C24 C25 C26 -2.2(4) . . . . no C24 C25 C26 C27 2.2(4) . . . . no C29 C25 C26 C27 -179.8(3) . . . . no C25 C26 C27 C30 -175.0(3) . . . . no C25 C26 C27 C22 1.5(4) . . . . no N6 C37 C38 N7 0.4(3) . . . . no N7 C39 C40 C41 58.2(3) . . . . no C39 C40 C41 N8 69.0(3) . . . . no N9 C43 C44 N8 -0.2(3) . . . . no N6 C45 C46 C47 177.1(3) . . . . no N6 C45 C46 C51 0.6(4) . . . . no C50 C45 C46 C47 4.7(4) . . . . no C50 C45 C46 C51 -171.7(3) . . . . no N6 C45 C50 C49 -176.6(3) . . . . no N6 C45 C50 C53 -0.2(4) . . . . no C46 C45 C50 C49 -4.2(4) . . . . no C46 C45 C50 C53 172.2(3) . . . . no C45 C46 C47 C48 -2.6(4) . . . . no C51 C46 C47 C48 173.9(3) . . . . no C46 C47 C48 C49 0.1(5) . . . . no C46 C47 C48 C52 -179.5(3) . . . . no C47 C48 C49 C50 0.4(5) . . . . no C52 C48 C49 C50 -180.0(3) . . . . no C48 C49 C50 C45 1.6(5) . . . . no C48 C49 C50 C53 -174.8(3) . . . . no N9 C54 C55 C56 -179.6(3) . . . . no N9 C54 C55 C60 2.3(5) . . . . no C59 C54 C55 C56 -4.5(5) . . . . no C59 C54 C55 C60 177.4(3) . . . . no N9 C54 C59 C58 180.0(3) . . . . no N9 C54 C59 C62 0.4(4) . . . . no C55 C54 C59 C58 4.8(5) . . . . no C55 C54 C59 C62 -174.7(3) . . . . no C54 C55 C56 C57 0.0(5) . . . . no C60 C55 C56 C57 178.2(3) . . . . no C55 C56 C57 C58 3.7(5) . . . . no C55 C56 C57 C61 -174.4(3) . . . . no C56 C57 C58 C59 -3.4(5) . . . . no C61 C57 C58 C59 174.7(3) . . . . no C57 C58 C59 C54 -0.8(5) . . . . no C57 C58 C59 C62 178.8(3) . . . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C6 H6 F1A 0.9500 2.5000 2.932(12) 108.00 1_655 yes C7 H7A N3 0.9900 2.5400 2.921(4) 103.00 . yes C9 H9B F5A 0.9900 2.5200 3.369(7) 143.00 . yes C11 H11 F13 0.9500 2.4700 3.357(4) 156.00 . yes C12 H12 F2A 0.9500 2.2000 3.097(9) 156.00 . yes C37 H37 F3A 0.9500 2.5400 3.359(6) 144.00 2_445 yes C38 H38 F12 0.9500 2.5300 3.392(4) 152.00 2_445 yes C41 H41A F13 0.9900 2.5000 3.240(4) 131.00 2_545 yes C41 H41B N7 0.9900 2.5100 2.906(4) 104.00 . yes C43 H43 F8 0.9500 2.4900 3.352(4) 151.00 4_555 yes C44 H44 N11 0.9500 2.5900 3.385(4) 141.00 3_656 yes C60 H60A N9 0.9800 2.5200 2.898(4) 102.00 . yes C64 H64A F3A 0.9800 2.4800 3.083(6) 119.00 2_545 yes # Loop Mechanism for Extra Tables(s) #loop_ #_publ_manuscript_incl_extra_item #'_geom_extra_tableA_col_1' #'_geom_extra_tableA_col_2' #'_geom_extra_tableA_col_3' #'_geom_extra_table_head_A' #'_geom_table_footnote_A' #'_geom_extra_tableB_col_1' #'_geom_extra_tableB_col_2' #'_geom_extra_tableB_col_3' #'_geom_extra_table_head_B' #'_geom_table_footnote_B' # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 # ? ? ? # #loop_ #_geom_extra_tableB_col_1 #_geom_extra_tableB_col_2 #_geom_extra_tableB_col_3 # ? ? ? # #_geom_table_footnote_A #; # ? #; # #_geom_table_footnote_B #; # ? #; # #_geom_table_footnote_A #; # ? #; # #_geom_table_footnote_B #; # ? #; _iucr_refine_instructions_details ; ; # start Validation Reply Form _vrf_PLAT214_I ; PROBLEM: Atom F2 (Anion/Solvent) ADP max/min Ratio 7.6 prola RESPONSE: The PF6- anion is heavily disordered and could not be modeled adequately by split-position refinement (which is applied) or application of restraints (which had been tried intensively but due to non-improvement were not applied for the final refinement).Therefore these alerts still remain. ; # end Validation Reply Form #===END _database_code_depnum_ccdc_archive 'CCDC 933793' ####################################################################### # # 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_Compound_3c #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_moiety 'C33 H37 N5 O3 Re, F6 P' _chemical_formula_sum 'C33 H37 F6 N5 O3 P Re' _chemical_formula_weight 882.86 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,y,1/2-z 3 -x,-y,-z 4 x,-y,1/2+z 5 1/2+x,1/2+y,z 6 1/2-x,1/2+y,1/2-z 7 1/2-x,1/2-y,-z 8 1/2+x,1/2-y,1/2+z _cell_length_a 33.2454(9) _cell_length_b 8.9066(2) _cell_length_c 27.3469(8) _cell_angle_alpha 90 _cell_angle_beta 101.758(1) _cell_angle_gamma 90 _cell_volume 7927.6(4) _cell_formula_units_Z 8 _cell_measurement_temperature 123 _cell_measurement_reflns_used 9242 _cell_measurement_theta_min 2.4506 _cell_measurement_theta_max 25.4486 _cell_special_details ; ; _exptl_crystal_description fragment _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.550 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.400 _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 3504 _exptl_absorpt_coefficient_mu 3.170 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS, Bruker, 2008b' _exptl_absorpt_correction_T_min 0.275 _exptl_absorpt_correction_T_max 0.364 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; Diffractometer operator A. Poethig scanspeed 5 s per frame dx 50 1967 frames measured in 5 data sets phi-scan with delta_phi = 0.5 omega-scans with delta_omega = 0.5 ; _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed-tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' \k-geometry diffractometer ' _diffrn_measurement_device_type ' Bruker APEX-II CCD ' _diffrn_measurement_method ' phi- and omega-rotation ' _diffrn_detector ' CCD plate ' _diffrn_detector_area_resol_mean 16 # number of measured reflections (redundant set) _diffrn_reflns_number 48269 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0251 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.45 _diffrn_reflns_theta_full 25.46 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 7320 # number of observed reflections (> n sig(I)) _reflns_number_gt 6969 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX II Control Software (Bruker, 2008a)' _computing_cell_refinement 'SAINT (Bruker, 2008b)' _computing_data_reduction 'SAINT (Bruker, 2008b)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2011)' _computing_publication_material 'PLATON (Spek, 2011), enCIFer (Allen, 2004)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R-factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0029P)^2^+93.1056P] 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_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 7320 _refine_ls_number_parameters 449 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0468 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.0841 _refine_ls_wR_factor_gt 0.0829 _refine_ls_goodness_of_fit_ref 1.289 _refine_ls_restrained_S_all 1.289 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.884 _refine_diff_density_min -1.872 _refine_diff_density_rms 0.114 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re Uani 0.17542(1) 0.55371(2) 0.03784(1) 1.000 0.0182(1) d . . . O1 O Uani 0.20550(14) 0.3497(5) 0.12800(15) 1.000 0.0372(14) d . . . O2 O Uani 0.22911(12) 0.3824(5) -0.02291(15) 1.000 0.0308(12) d . . . O3 O Uani 0.25964(11) 0.7099(5) 0.05949(15) 1.000 0.0302(12) d . . . N1 N Uani 0.16304(13) 0.8019(5) 0.12088(17) 1.000 0.0231(12) d . . . N2 N Uani 0.10944(14) 0.7943(5) 0.06247(18) 1.000 0.0263(14) d . . . N3 N Uani 0.08975(14) 0.3867(5) 0.04669(19) 1.000 0.0279(14) d . . . N4 N Uani 0.10782(13) 0.3129(5) -0.01970(17) 1.000 0.0232(14) d . . . N5 N Uani 0.15437(13) 0.6773(5) -0.03024(17) 1.000 0.0218(14) d . . . C1 C Uani 0.19411(16) 0.4287(6) 0.0943(2) 1.000 0.0242(17) d . . . C2 C Uani 0.20642(16) 0.4321(6) -0.0013(2) 1.000 0.0218(17) d . . . C3 C Uani 0.22720(16) 0.6623(6) 0.05255(19) 1.000 0.0197(17) d . . . C4 C Uani 0.14653(16) 0.7264(6) 0.0779(2) 1.000 0.0225(17) d . . . C5 C Uani 0.13649(18) 0.9112(6) 0.1311(2) 1.000 0.0311(17) d . . . C6 C Uani 0.10310(18) 0.9058(6) 0.0951(2) 1.000 0.0318(19) d . . . C7 C Uani 0.07732(16) 0.7439(7) 0.0211(2) 1.000 0.0325(19) d . . . C8 C Uani 0.04088(18) 0.6701(8) 0.0383(3) 1.000 0.044(2) d . . . C9 C Uani 0.05014(19) 0.5761(8) 0.0858(3) 1.000 0.045(2) d . . . C10 C Uani 0.08634(18) 0.4648(7) 0.0925(2) 1.000 0.035(2) d . . . C11 C Uani 0.11941(15) 0.4103(5) 0.0196(2) 1.000 0.0200(16) d . . . C12 C Uani 0.06141(17) 0.2811(7) 0.0253(2) 1.000 0.0314(19) d . . . C13 C Uani 0.07250(16) 0.2348(7) -0.0161(2) 1.000 0.0303(19) d . . . C14 C Uani 0.20164(16) 0.7690(6) 0.15523(19) 1.000 0.0202(17) d . . . C15 C Uani 0.20188(19) 0.6597(7) 0.1917(2) 1.000 0.0289(17) d . . . C16 C Uani 0.2394(2) 0.6302(7) 0.2236(2) 1.000 0.0347(19) d . . . C17 C Uani 0.27463(19) 0.7069(7) 0.2206(2) 1.000 0.0311(19) d . . . C18 C Uani 0.27238(17) 0.8192(6) 0.1851(2) 1.000 0.0257(17) d . . . C19 C Uani 0.23586(17) 0.8546(6) 0.15237(19) 1.000 0.0242(17) d . . . C20 C Uani 0.1636(2) 0.5792(7) 0.1984(2) 1.000 0.040(2) d . . . C21 C Uani 0.3141(2) 0.6709(8) 0.2566(2) 1.000 0.047(2) d . . . C22 C Uani 0.23406(19) 0.9824(6) 0.1163(2) 1.000 0.0310(17) d . . . C23 C Uani 0.12837(16) 0.2840(6) -0.0605(2) 1.000 0.0213(17) d . . . C24 C Uani 0.11485(16) 0.3583(6) -0.1058(2) 1.000 0.0247(17) d . . . C25 C Uani 0.13546(18) 0.3275(7) -0.1438(2) 1.000 0.0310(17) d . . . C26 C Uani 0.16746(18) 0.2238(6) -0.1383(2) 1.000 0.0288(17) d . . . C27 C Uani 0.17793(17) 0.1477(6) -0.0934(2) 1.000 0.0283(17) d . . . C28 C Uani 0.15864(16) 0.1737(6) -0.0538(2) 1.000 0.0251(17) d . . . C29 C Uani 0.07740(17) 0.4587(7) -0.1139(2) 1.000 0.0342(19) d . . . C30 C Uani 0.1894(2) 0.1945(8) -0.1802(2) 1.000 0.045(2) d . . . C31 C Uani 0.16942(17) 0.0868(6) -0.0060(2) 1.000 0.0292(17) d . . . C32 C Uani 0.14694(16) 0.7288(6) -0.0689(2) 1.000 0.0234(17) d . . . C33 C Uani 0.13783(19) 0.7914(7) -0.1193(2) 1.000 0.034(2) d . . . P1 P Uani 0.01132(5) 0.0939(2) 0.38482(7) 1.000 0.0376(6) d . . . F1 F Uani 0.00422(19) -0.0690(6) 0.3636(2) 1.000 0.089(2) d . . . F2 F Uani 0.00119(11) 0.0358(4) 0.43634(14) 1.000 0.0411(12) d . . . F3 F Uani 0.01790(14) 0.2587(5) 0.40841(18) 1.000 0.0625(16) d . . . F4 F Uani 0.05862(13) 0.0578(6) 0.40626(19) 1.000 0.073(2) d . . . F5 F Uani -0.03574(12) 0.1328(6) 0.36582(17) 1.000 0.0645(16) d . . . F6 F Uani 0.02160(17) 0.1543(7) 0.33452(19) 1.000 0.086(2) d . . . H5 H Uiso 0.14130 0.97800 0.15880 1.000 0.0370 c R . . H6 H Uiso 0.07930 0.96690 0.09230 1.000 0.0380 c R . . H7A H Uiso 0.08930 0.67110 0.00070 1.000 0.0390 c R . . H7B H Uiso 0.06720 0.83100 -0.00030 1.000 0.0390 c R . . H8A H Uiso 0.02150 0.75040 0.04310 1.000 0.0530 c R . . H8B H Uiso 0.02650 0.60510 0.01080 1.000 0.0530 c R . . H9A H Uiso 0.02510 0.51830 0.08780 1.000 0.0540 c R . . H9B H Uiso 0.05530 0.64590 0.11460 1.000 0.0540 c R . . H10A H Uiso 0.11220 0.52020 0.10520 1.000 0.0420 c R . . H10B H Uiso 0.08300 0.38960 0.11810 1.000 0.0420 c R . . H12 H Uiso 0.03830 0.24770 0.03780 1.000 0.0380 c R . . H13 H Uiso 0.05880 0.16200 -0.03890 1.000 0.0360 c R . . H16 H Uiso 0.24060 0.55440 0.24830 1.000 0.0420 c R . . H18 H Uiso 0.29650 0.87360 0.18300 1.000 0.0310 c R . . H20A H Uiso 0.15980 0.48890 0.17750 1.000 0.0600 c R . . H20B H Uiso 0.13980 0.64570 0.18860 1.000 0.0600 c R . . H20C H Uiso 0.16630 0.55060 0.23350 1.000 0.0600 c R . . H21A H Uiso 0.31290 0.71090 0.28960 1.000 0.0700 c R . . H21B H Uiso 0.33720 0.71650 0.24470 1.000 0.0700 c R . . H21C H Uiso 0.31780 0.56180 0.25870 1.000 0.0700 c R . . H22A H Uiso 0.21760 0.95290 0.08380 1.000 0.0460 c R . . H22B H Uiso 0.26190 1.00810 0.11260 1.000 0.0460 c R . . H22C H Uiso 0.22140 1.06980 0.12900 1.000 0.0460 c R . . H25 H Uiso 0.12750 0.37880 -0.17480 1.000 0.0370 c R . . H27 H Uiso 0.19920 0.07470 -0.08960 1.000 0.0340 c R . . H29A H Uiso 0.07570 0.51590 -0.14480 1.000 0.0510 c R . . H29B H Uiso 0.07950 0.52810 -0.08570 1.000 0.0510 c R . . H29C H Uiso 0.05270 0.39700 -0.11640 1.000 0.0510 c R . . H30A H Uiso 0.20890 0.27590 -0.18180 1.000 0.0680 c R . . H30B H Uiso 0.16930 0.18930 -0.21180 1.000 0.0680 c R . . H30C H Uiso 0.20420 0.09900 -0.17440 1.000 0.0680 c R . . H31A H Uiso 0.18950 0.00880 -0.00930 1.000 0.0440 c R . . H31B H Uiso 0.14460 0.03990 0.00110 1.000 0.0440 c R . . H31C H Uiso 0.18120 0.15480 0.02130 1.000 0.0440 c R . . H33A H Uiso 0.16320 0.82870 -0.12790 1.000 0.0520 c R . . H33B H Uiso 0.11820 0.87420 -0.12070 1.000 0.0520 c R . . H33C H Uiso 0.12590 0.71320 -0.14310 1.000 0.0520 c R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0145(1) 0.0177(1) 0.0221(1) -0.0011(1) 0.0028(1) -0.0012(1) O1 0.055(3) 0.026(2) 0.029(2) 0.0098(19) 0.005(2) 0.009(2) O2 0.025(2) 0.032(2) 0.039(2) -0.0072(19) 0.0149(18) -0.0007(17) O3 0.018(2) 0.037(2) 0.036(2) -0.0072(19) 0.0062(17) -0.0086(18) N1 0.022(2) 0.019(2) 0.027(2) -0.0049(19) 0.0020(19) 0.0015(18) N2 0.022(2) 0.021(2) 0.035(3) -0.002(2) 0.004(2) 0.0033(19) N3 0.018(2) 0.025(2) 0.042(3) -0.004(2) 0.009(2) -0.0041(19) N4 0.014(2) 0.020(2) 0.034(3) -0.003(2) 0.0015(19) -0.0019(18) N5 0.015(2) 0.020(2) 0.029(3) -0.001(2) 0.0015(18) -0.0005(18) C1 0.024(3) 0.018(3) 0.032(3) -0.013(3) 0.009(2) 0.000(2) C2 0.020(3) 0.018(3) 0.025(3) 0.003(2) -0.001(2) -0.006(2) C3 0.020(3) 0.020(3) 0.018(3) -0.001(2) 0.001(2) 0.002(2) C4 0.019(3) 0.024(3) 0.023(3) 0.002(2) 0.001(2) -0.004(2) C5 0.036(3) 0.019(3) 0.039(3) -0.010(2) 0.009(3) 0.003(2) C6 0.025(3) 0.022(3) 0.049(4) -0.008(3) 0.009(3) 0.007(2) C7 0.014(3) 0.034(3) 0.046(4) -0.009(3) -0.002(2) 0.006(2) C8 0.019(3) 0.041(4) 0.071(5) -0.022(4) 0.007(3) 0.003(3) C9 0.031(3) 0.041(4) 0.070(5) -0.021(4) 0.026(3) -0.008(3) C10 0.027(3) 0.034(4) 0.048(4) -0.008(3) 0.018(3) -0.008(3) C11 0.014(2) 0.016(3) 0.029(3) 0.002(2) 0.002(2) 0.0022(19) C12 0.018(3) 0.028(3) 0.049(4) 0.001(3) 0.009(3) -0.003(2) C13 0.017(3) 0.026(3) 0.046(4) -0.006(3) 0.002(3) -0.005(2) C14 0.028(3) 0.017(3) 0.015(3) -0.008(2) 0.003(2) 0.004(2) C15 0.041(3) 0.026(3) 0.022(3) -0.005(2) 0.012(2) -0.002(3) C16 0.061(4) 0.027(3) 0.015(3) 0.001(2) 0.005(3) 0.008(3) C17 0.040(4) 0.034(3) 0.016(3) -0.005(2) -0.002(2) 0.009(3) C18 0.029(3) 0.024(3) 0.024(3) -0.008(2) 0.005(2) 0.003(2) C19 0.032(3) 0.022(3) 0.019(3) -0.007(2) 0.006(2) 0.003(2) C20 0.054(4) 0.039(4) 0.031(3) 0.001(3) 0.017(3) -0.010(3) C21 0.056(4) 0.049(4) 0.028(3) -0.005(3) -0.010(3) 0.014(4) C22 0.039(3) 0.023(3) 0.029(3) 0.000(2) 0.002(3) -0.001(2) C23 0.018(3) 0.014(3) 0.031(3) -0.006(2) 0.003(2) -0.003(2) C24 0.021(3) 0.018(3) 0.031(3) -0.005(2) -0.004(2) 0.001(2) C25 0.035(3) 0.029(3) 0.026(3) -0.004(3) -0.001(3) -0.001(3) C26 0.032(3) 0.026(3) 0.028(3) -0.009(2) 0.005(2) -0.005(2) C27 0.023(3) 0.022(3) 0.038(3) -0.005(3) 0.002(2) 0.000(2) C28 0.021(3) 0.020(3) 0.032(3) -0.002(2) 0.000(2) -0.005(2) C29 0.026(3) 0.029(3) 0.043(4) 0.000(3) -0.004(3) 0.008(3) C30 0.050(4) 0.050(4) 0.037(4) -0.010(3) 0.011(3) 0.002(3) C31 0.025(3) 0.021(3) 0.040(3) 0.004(2) 0.003(2) 0.001(2) C32 0.019(3) 0.025(3) 0.025(3) 0.002(2) 0.002(2) -0.003(2) C33 0.037(4) 0.037(4) 0.028(3) 0.003(3) 0.004(3) -0.002(3) P1 0.0314(9) 0.0396(10) 0.0430(10) 0.0051(8) 0.0102(7) -0.0052(7) F1 0.120(5) 0.067(3) 0.084(4) -0.040(3) 0.032(3) -0.019(3) F2 0.041(2) 0.038(2) 0.046(2) 0.0114(18) 0.0126(17) 0.0019(17) F3 0.067(3) 0.035(2) 0.082(3) 0.005(2) 0.007(2) -0.014(2) F4 0.035(2) 0.089(4) 0.099(4) 0.034(3) 0.024(2) 0.009(2) F5 0.037(2) 0.088(3) 0.066(3) 0.032(3) 0.005(2) 0.002(2) F6 0.085(4) 0.120(5) 0.062(3) 0.029(3) 0.034(3) -0.004(3) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 N5 2.153(5) . . yes Re1 C1 1.902(5) . . yes Re1 C2 1.957(5) . . yes Re1 C3 1.944(5) . . yes Re1 C4 2.217(5) . . yes Re1 C11 2.229(5) . . yes P1 F2 1.600(4) . . yes P1 F3 1.600(5) . . yes P1 F4 1.595(5) . . yes P1 F5 1.583(5) . . yes P1 F6 1.578(6) . . yes P1 F1 1.563(6) . . yes O1 C1 1.160(7) . . yes O2 C2 1.138(7) . . yes O3 C3 1.138(7) . . yes N1 C14 1.457(7) . . yes N1 C5 1.380(7) . . yes N1 C4 1.368(7) . . yes N2 C4 1.361(7) . . yes N2 C6 1.380(7) . . yes N2 C7 1.459(7) . . yes N3 C10 1.457(7) . . yes N3 C11 1.365(7) . . yes N3 C12 1.375(8) . . yes N4 C13 1.386(7) . . yes N4 C11 1.374(7) . . yes N4 C23 1.445(7) . . yes N5 C32 1.133(7) . . yes C5 C6 1.326(8) . . no C7 C8 1.534(9) . . no C8 C9 1.523(11) . . no C9 C10 1.541(9) . . no C12 C13 1.326(8) . . no C14 C15 1.393(8) . . no C14 C19 1.385(8) . . no C15 C16 1.394(9) . . no C15 C20 1.504(9) . . no C16 C17 1.373(9) . . no C17 C18 1.385(8) . . no C17 C21 1.506(9) . . no C18 C19 1.390(8) . . no C19 C22 1.499(7) . . no C23 C24 1.396(8) . . no C23 C28 1.392(8) . . no C24 C25 1.384(8) . . no C24 C29 1.512(8) . . no C25 C26 1.394(8) . . no C26 C30 1.501(8) . . no C26 C27 1.384(8) . . no C27 C28 1.386(8) . . no C28 C31 1.498(8) . . no C32 C33 1.460(8) . . no C5 H5 0.9500 . . no C6 H6 0.9500 . . no C7 H7A 0.9900 . . no C7 H7B 0.9900 . . no C8 H8B 0.9900 . . no C8 H8A 0.9900 . . no C9 H9A 0.9900 . . no C9 H9B 0.9900 . . no C10 H10A 0.9900 . . no C10 H10B 0.9900 . . no C12 H12 0.9500 . . no C13 H13 0.9500 . . no C16 H16 0.9500 . . no C18 H18 0.9500 . . no C20 H20A 0.9800 . . no C20 H20B 0.9800 . . no C20 H20C 0.9800 . . no C21 H21A 0.9800 . . no C21 H21B 0.9800 . . no C21 H21C 0.9800 . . no C22 H22B 0.9800 . . no C22 H22A 0.9800 . . no C22 H22C 0.9800 . . no C25 H25 0.9500 . . no C27 H27 0.9500 . . no C29 H29C 0.9800 . . no C29 H29A 0.9800 . . no C29 H29B 0.9800 . . no C30 H30B 0.9800 . . no C30 H30A 0.9800 . . no C30 H30C 0.9800 . . no C31 H31B 0.9800 . . no C31 H31A 0.9800 . . no C31 H31C 0.9800 . . no C33 H33C 0.9800 . . no C33 H33A 0.9800 . . no C33 H33B 0.9800 . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Re1 C1 174.8(2) . . . yes N5 Re1 C2 85.7(2) . . . yes N5 Re1 C3 92.44(19) . . . yes N5 Re1 C4 88.59(18) . . . yes N5 Re1 C11 89.43(18) . . . yes C1 Re1 C2 89.9(2) . . . yes C1 Re1 C3 89.7(2) . . . yes C1 Re1 C4 96.2(2) . . . yes C1 Re1 C11 88.1(2) . . . yes C2 Re1 C3 81.1(2) . . . yes C2 Re1 C4 169.5(2) . . . yes C2 Re1 C11 94.0(2) . . . yes C3 Re1 C4 90.4(2) . . . yes C3 Re1 C11 174.6(2) . . . yes C4 Re1 C11 94.70(19) . . . yes F2 P1 F3 88.7(2) . . . yes F2 P1 F4 88.8(2) . . . yes F2 P1 F5 89.3(2) . . . yes F2 P1 F6 178.9(3) . . . yes F3 P1 F4 89.6(3) . . . yes F3 P1 F5 88.6(3) . . . yes F3 P1 F6 90.2(3) . . . yes F4 P1 F5 177.5(3) . . . yes F4 P1 F6 91.0(3) . . . yes F5 P1 F6 90.8(3) . . . yes F1 P1 F2 89.1(3) . . . yes F1 P1 F3 177.8(3) . . . yes F1 P1 F4 90.7(3) . . . yes F1 P1 F5 91.0(3) . . . yes F1 P1 F6 92.1(3) . . . yes C4 N1 C5 111.1(4) . . . yes C4 N1 C14 127.0(4) . . . yes C5 N1 C14 121.8(4) . . . yes C4 N2 C6 111.6(5) . . . yes C4 N2 C7 125.3(5) . . . yes C6 N2 C7 122.6(5) . . . yes C10 N3 C11 125.8(5) . . . yes C10 N3 C12 121.7(5) . . . yes C11 N3 C12 112.5(5) . . . yes C11 N4 C13 111.6(4) . . . yes C11 N4 C23 128.0(4) . . . yes C13 N4 C23 120.4(4) . . . yes Re1 N5 C32 170.0(4) . . . yes Re1 C1 O1 178.4(5) . . . yes Re1 C2 O2 167.9(5) . . . yes Re1 C3 O3 171.5(5) . . . yes Re1 C4 N1 128.8(4) . . . yes Re1 C4 N2 127.7(4) . . . yes N1 C4 N2 103.2(4) . . . yes N1 C5 C6 107.3(5) . . . yes N2 C6 C5 106.9(5) . . . yes N2 C7 C8 113.1(5) . . . yes C7 C8 C9 117.5(5) . . . no C8 C9 C10 118.2(6) . . . no N3 C10 C9 113.6(5) . . . yes N3 C11 N4 102.1(4) . . . yes Re1 C11 N4 128.7(4) . . . yes Re1 C11 N3 129.0(4) . . . yes N3 C12 C13 106.9(5) . . . yes N4 C13 C12 107.0(5) . . . yes N1 C14 C15 118.6(5) . . . yes N1 C14 C19 118.6(5) . . . yes C15 C14 C19 122.7(5) . . . no C14 C15 C16 117.0(6) . . . no C14 C15 C20 122.6(5) . . . no C16 C15 C20 120.4(5) . . . no C15 C16 C17 122.3(5) . . . no C16 C17 C18 118.5(5) . . . no C16 C17 C21 119.7(5) . . . no C18 C17 C21 121.8(6) . . . no C17 C18 C19 122.0(5) . . . no C14 C19 C18 117.3(5) . . . no C14 C19 C22 122.1(5) . . . no C18 C19 C22 120.6(5) . . . no N4 C23 C28 117.8(5) . . . yes N4 C23 C24 118.9(5) . . . yes C24 C23 C28 123.0(5) . . . no C25 C24 C29 121.8(5) . . . no C23 C24 C25 117.0(5) . . . no C23 C24 C29 121.1(5) . . . no C24 C25 C26 122.3(5) . . . no C25 C26 C30 120.8(5) . . . no C25 C26 C27 118.0(5) . . . no C27 C26 C30 121.3(5) . . . no C26 C27 C28 122.6(5) . . . no C27 C28 C31 121.9(5) . . . no C23 C28 C27 116.9(5) . . . no C23 C28 C31 121.2(5) . . . no N5 C32 C33 178.4(6) . . . yes N1 C5 H5 126.00 . . . no C6 C5 H5 126.00 . . . no N2 C6 H6 126.00 . . . no C5 C6 H6 127.00 . . . no N2 C7 H7A 109.00 . . . no N2 C7 H7B 109.00 . . . no C8 C7 H7A 109.00 . . . no C8 C7 H7B 109.00 . . . no H7A C7 H7B 108.00 . . . no C7 C8 H8A 108.00 . . . no C7 C8 H8B 108.00 . . . no C9 C8 H8A 108.00 . . . no C9 C8 H8B 108.00 . . . no H8A C8 H8B 107.00 . . . no C8 C9 H9A 108.00 . . . no C10 C9 H9A 108.00 . . . no C10 C9 H9B 108.00 . . . no C8 C9 H9B 108.00 . . . no H9A C9 H9B 107.00 . . . no N3 C10 H10B 109.00 . . . no C9 C10 H10A 109.00 . . . no N3 C10 H10A 109.00 . . . no H10A C10 H10B 108.00 . . . no C9 C10 H10B 109.00 . . . no N3 C12 H12 127.00 . . . no C13 C12 H12 127.00 . . . no C12 C13 H13 126.00 . . . no N4 C13 H13 127.00 . . . no C15 C16 H16 119.00 . . . no C17 C16 H16 119.00 . . . no C19 C18 H18 119.00 . . . no C17 C18 H18 119.00 . . . no C15 C20 H20A 109.00 . . . no C15 C20 H20B 110.00 . . . no C15 C20 H20C 109.00 . . . no H20A C20 H20B 110.00 . . . no H20A C20 H20C 109.00 . . . no H20B C20 H20C 109.00 . . . no C17 C21 H21A 109.00 . . . no C17 C21 H21B 109.00 . . . no C17 C21 H21C 109.00 . . . no H21A C21 H21B 110.00 . . . no H21A C21 H21C 110.00 . . . no H21B C21 H21C 109.00 . . . no C19 C22 H22A 109.00 . . . no C19 C22 H22B 110.00 . . . no C19 C22 H22C 109.00 . . . no H22B C22 H22C 110.00 . . . no H22A C22 H22B 110.00 . . . no H22A C22 H22C 109.00 . . . no C24 C25 H25 119.00 . . . no C26 C25 H25 119.00 . . . no C28 C27 H27 119.00 . . . no C26 C27 H27 119.00 . . . no C24 C29 H29C 109.00 . . . no C24 C29 H29A 110.00 . . . no C24 C29 H29B 109.00 . . . no H29B C29 H29C 109.00 . . . no H29A C29 H29B 109.00 . . . no H29A C29 H29C 109.00 . . . no C26 C30 H30C 109.00 . . . no C26 C30 H30A 110.00 . . . no C26 C30 H30B 109.00 . . . no H30A C30 H30B 110.00 . . . no H30A C30 H30C 110.00 . . . no H30B C30 H30C 109.00 . . . no C28 C31 H31A 109.00 . . . no C28 C31 H31B 109.00 . . . no C28 C31 H31C 109.00 . . . no H31A C31 H31B 109.00 . . . no H31A C31 H31C 110.00 . . . no H31B C31 H31C 110.00 . . . no C32 C33 H33A 109.00 . . . no C32 C33 H33B 109.00 . . . no C32 C33 H33C 109.00 . . . no H33A C33 H33B 110.00 . . . no H33A C33 H33C 109.00 . . . no H33B C33 H33C 109.00 . . . no loop_ _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 N5 Re1 C4 N1 -130.9(5) . . . . no C1 Re1 C4 N1 51.3(5) . . . . no C3 Re1 C4 N1 -38.5(5) . . . . no C11 Re1 C4 N1 139.8(5) . . . . no N5 Re1 C4 N2 41.3(5) . . . . no C1 Re1 C4 N2 -136.6(5) . . . . no C3 Re1 C4 N2 133.7(5) . . . . no C11 Re1 C4 N2 -48.0(5) . . . . no C2 Re1 C11 N3 152.4(5) . . . . no C4 Re1 C11 N3 -33.4(5) . . . . no N5 Re1 C11 N4 64.4(4) . . . . no C1 Re1 C11 N4 -111.0(5) . . . . no C2 Re1 C11 N4 -21.2(5) . . . . no N5 Re1 C11 N3 -121.9(5) . . . . no C1 Re1 C11 N3 62.7(5) . . . . no C4 Re1 C11 N4 152.9(4) . . . . no C5 N1 C4 Re1 174.1(4) . . . . no C14 N1 C4 Re1 -10.9(8) . . . . no C14 N1 C4 N2 175.5(5) . . . . no C4 N1 C14 C15 -84.0(7) . . . . no C5 N1 C4 N2 0.4(6) . . . . no C5 N1 C14 C19 -85.2(6) . . . . no C14 N1 C5 C6 -175.1(5) . . . . no C4 N1 C5 C6 0.2(6) . . . . no C4 N1 C14 C19 100.2(6) . . . . no C5 N1 C14 C15 90.5(6) . . . . no C7 N2 C4 N1 -172.3(5) . . . . no C6 N2 C4 Re1 -174.6(4) . . . . no C6 N2 C7 C8 -64.3(7) . . . . no C6 N2 C4 N1 -0.9(6) . . . . no C4 N2 C7 C8 106.2(6) . . . . no C4 N2 C6 C5 1.1(6) . . . . no C7 N2 C4 Re1 13.9(8) . . . . no C7 N2 C6 C5 172.8(5) . . . . no C12 N3 C11 N4 -0.2(6) . . . . no C11 N3 C12 C13 0.1(7) . . . . no C11 N3 C10 C9 108.5(6) . . . . no C12 N3 C10 C9 -69.6(7) . . . . no C10 N3 C12 C13 178.3(5) . . . . no C12 N3 C11 Re1 -175.1(4) . . . . no C10 N3 C11 N4 -178.3(5) . . . . no C10 N3 C11 Re1 6.7(8) . . . . no C13 N4 C11 Re1 175.2(4) . . . . no C13 N4 C23 C24 84.8(6) . . . . no C23 N4 C11 Re1 -3.0(8) . . . . no C11 N4 C23 C24 -97.2(6) . . . . no C11 N4 C23 C28 88.0(7) . . . . no C11 N4 C13 C12 -0.2(6) . . . . no C13 N4 C11 N3 0.2(6) . . . . no C23 N4 C11 N3 -178.0(5) . . . . no C23 N4 C13 C12 178.2(5) . . . . no C13 N4 C23 C28 -90.0(6) . . . . no N1 C5 C6 N2 -0.7(6) . . . . no N2 C7 C8 C9 -35.7(8) . . . . no C7 C8 C9 C10 -45.0(9) . . . . no C8 C9 C10 N3 -39.6(8) . . . . no N3 C12 C13 N4 0.1(6) . . . . no N1 C14 C15 C16 179.4(5) . . . . no N1 C14 C19 C22 2.0(8) . . . . no C15 C14 C19 C18 5.4(8) . . . . no C15 C14 C19 C22 -173.6(5) . . . . no C19 C14 C15 C20 172.9(5) . . . . no N1 C14 C15 C20 -2.7(8) . . . . no C19 C14 C15 C16 -5.0(8) . . . . no N1 C14 C19 C18 -179.1(5) . . . . no C14 C15 C16 C17 1.6(9) . . . . no C20 C15 C16 C17 -176.3(6) . . . . no C15 C16 C17 C18 1.2(9) . . . . no C15 C16 C17 C21 179.3(6) . . . . no C21 C17 C18 C19 -178.9(5) . . . . no C16 C17 C18 C19 -0.8(9) . . . . no C17 C18 C19 C14 -2.4(8) . . . . no C17 C18 C19 C22 176.6(5) . . . . no N4 C23 C24 C25 179.9(5) . . . . no N4 C23 C24 C29 -4.6(8) . . . . no C28 C23 C24 C25 -5.6(8) . . . . no C28 C23 C24 C29 170.0(5) . . . . no N4 C23 C28 C27 179.9(5) . . . . no N4 C23 C28 C31 0.4(8) . . . . no C24 C23 C28 C27 5.3(8) . . . . no C24 C23 C28 C31 -174.2(5) . . . . no C23 C24 C25 C26 2.0(9) . . . . no C29 C24 C25 C26 -173.5(5) . . . . no C24 C25 C26 C27 1.5(9) . . . . no C24 C25 C26 C30 -179.4(6) . . . . no C25 C26 C27 C28 -1.7(9) . . . . no C30 C26 C27 C28 179.1(5) . . . . no C26 C27 C28 C23 -1.5(8) . . . . no C26 C27 C28 C31 178.0(5) . . . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C6 H6 F5 0.9500 2.5000 3.350(7) 148.00 2_565 yes C7 H7A N5 0.9900 2.4800 3.217(7) 131.00 . yes C12 H12 F2 0.9500 2.4800 3.331(7) 149.00 2_555 yes C13 H13 F4 0.9500 2.4700 3.334(8) 152.00 4_554 yes C20 H20A O1 0.9800 2.5500 3.304(8) 133.00 . yes C20 H20B N1 0.9800 2.5600 2.901(7) 100.00 . yes C22 H22C O1 0.9800 2.5500 3.439(7) 151.00 1_565 yes C33 H33B F4 0.9800 2.3300 3.159(8) 142.00 4_564 yes # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _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 0.000 0.548 0.250 343 83 ' ' 2 0.500 1.048 0.250 343 83 ' ' 3 0.000 0.449 0.750 343 83 ' ' 4 0.500 -0.051 0.750 343 83 ' ' _platon_squeeze_details ; The unit cell contains 8 diethylether molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; #===END _database_code_depnum_ccdc_archive 'CCDC 933794' ####################################################################### # # 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_Compound_5a #=================================================================== #=================================================================== # 5. CHEMICAL DATA #=================================================================== _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety 'C31 H33 N5 O3 Re, C16 Al F36 O4, C5 H12' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C52 H45 Al F36 N5 O7 Re' _chemical_formula_weight 1749.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=================================================================== # 6. CRYSTAL DATA #=================================================================== _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 x,1/2-y,1/2+z _cell_length_a 15.4858(4) _cell_length_b 28.1684(8) _cell_length_c 15.2405(4) _cell_angle_alpha 90 _cell_angle_beta 103.6769(10) _cell_angle_gamma 90 _cell_volume 6459.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 9873 _cell_measurement_theta_min 1.35 _cell_measurement_theta_max 25.37 _exptl_crystal_description fragment _exptl_crystal_colour colorless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.799 _exptl_crystal_density_method none _exptl_crystal_F_000 3440 _exptl_absorpt_coefficient_mu 2.052 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5442 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_process_details 'SADABS, Bruker, 2008b' _exptl_special_details ; Diffractometer operator E. Herdtweck scanspeed 10 s per frame dx 60 3579 frames measured in 9 data sets phi-scan with delta_phi = 0.50 omega-scans with delta_omega = 0.50 ; #=================================================================== # 7. EXPERIMENTAL DATA #=================================================================== _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'rotating anode FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' \k-geometry diffractometer ' _diffrn_measurement_device_type ' Bruker APEX-II CCD ' _diffrn_measurement_method ' phi- and omega-rotation ' _diffrn_detector ' CCD plate ' _diffrn_detector_area_resol_mean 16 # 8 for binned mode _diffrn_standards_decay_% 0 # number of measured reflections (redundant set) _diffrn_reflns_number 105811 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_sigmaI/netI 0.0127 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 25.37 _reflns_number_total 11853 _reflns_number_gt 11086 # number of observed reflections (> n sig(I)) _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX II Control Software (Bruker, 2008a)' _computing_cell_refinement 'SAINT (Bruker, 2008b)' _computing_data_reduction 'SAINT (Bruker, 2008b)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2010)' _computing_publication_material 'PLATON (Spek, 2010)' #=================================================================== # 8. REFINEMENT DATA #=================================================================== _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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 sigma _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0275P)^2^+22.3170P] 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_number_reflns 11853 _refine_ls_number_parameters 928 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0337 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0743 _refine_ls_wR_factor_gt 0.0721 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.377 _refine_diff_density_min -1.052 _refine_diff_density_rms 0.084 #=================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=================================================================== loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Re1 Re Uani 0.65698(1) 0.19890(1) 0.12448(1) 1.000 0.0183(1) . . O1 O Uani 0.81441(18) 0.16428(10) 0.05093(19) 1.000 0.0388(9) . . O2 O Uani 0.66597(17) 0.28665(9) 0.00609(16) 1.000 0.0316(8) . . O3 O Uani 0.5337(2) 0.18191(10) -0.06381(18) 1.000 0.0443(9) . . N1 N Uani 0.78327(19) 0.27077(10) 0.26511(18) 1.000 0.0255(8) . . N2 N Uani 0.77439(18) 0.20578(10) 0.33426(18) 1.000 0.0245(8) . . N3 N Uani 0.62376(18) 0.11802(10) 0.26452(18) 1.000 0.0227(8) . . N4 N Uani 0.60649(18) 0.08713(10) 0.13386(18) 1.000 0.0238(8) . . N5 N Uani 0.54919(18) 0.22413(10) 0.17954(19) 1.000 0.0244(8) . . C1 C Uani 0.7557(2) 0.17612(12) 0.0800(2) 1.000 0.0252(10) . . C2 C Uani 0.6661(2) 0.25707(12) 0.0588(2) 1.000 0.0237(9) . . C3 C Uani 0.5774(2) 0.18420(12) 0.0085(2) 1.000 0.0288(11) . . C4 C Uani 0.7457(2) 0.22663(12) 0.2515(2) 1.000 0.0212(9) . . C5 C Uani 0.8330(3) 0.27656(15) 0.3532(2) 1.000 0.0367(11) . . C6 C Uani 0.8271(3) 0.23583(14) 0.3960(2) 1.000 0.0346(11) . . C7 C Uani 0.7535(2) 0.15807(12) 0.3594(2) 1.000 0.0272(10) . . C8 C Uani 0.6538(2) 0.14895(12) 0.3426(2) 1.000 0.0244(10) . . C9 C Uani 0.6294(2) 0.12910(11) 0.1790(2) 1.000 0.0212(9) . . C10 C Uani 0.6004(2) 0.07111(12) 0.2727(2) 1.000 0.0306(11) . . C11 C Uani 0.5890(3) 0.05193(13) 0.1906(2) 1.000 0.0315(11) . . C12 C Uani 0.7784(2) 0.30944(12) 0.2018(2) 1.000 0.0252(10) . . C13 C Uani 0.7122(2) 0.34363(12) 0.1959(2) 1.000 0.0290(10) . . C14 C Uani 0.7139(3) 0.38230(13) 0.1392(3) 1.000 0.0329(11) . . C15 C Uani 0.7805(3) 0.38811(12) 0.0929(2) 1.000 0.0313(11) . . C16 C Uani 0.8461(2) 0.35350(13) 0.1025(2) 1.000 0.0285(10) . . C17 C Uani 0.8466(2) 0.31353(12) 0.1562(2) 1.000 0.0256(10) . . C18 C Uani 0.6423(3) 0.33987(15) 0.2502(3) 1.000 0.0416(14) . . C19 C Uani 0.7833(3) 0.43168(14) 0.0362(3) 1.000 0.0448(14) . . C20 C Uani 0.9186(2) 0.27647(14) 0.1661(3) 1.000 0.0343(11) . . C21 C Uani 0.6017(2) 0.07629(11) 0.0404(2) 1.000 0.0243(10) . . C22 C Uani 0.5188(2) 0.07734(12) -0.0205(2) 1.000 0.0300(11) . . C23 C Uani 0.5154(3) 0.06346(13) -0.1092(3) 1.000 0.0352(11) . . C24 C Uani 0.5902(3) 0.04776(13) -0.1359(3) 1.000 0.0368(13) . . C25 C Uani 0.6706(3) 0.04628(13) -0.0725(3) 1.000 0.0351(11) . . C26 C Uani 0.6783(2) 0.05996(12) 0.0169(2) 1.000 0.0279(10) . . C27 C Uani 0.4361(3) 0.09174(16) 0.0084(3) 1.000 0.0431(14) . . C28 C Uani 0.5837(4) 0.03089(16) -0.2317(3) 1.000 0.0536(16) . . C29 C Uani 0.7655(3) 0.05441(14) 0.0861(3) 1.000 0.0378(12) . . C30 C Uani 0.4938(2) 0.23804(13) 0.2103(2) 1.000 0.0275(10) . . C31 C Uani 0.4249(3) 0.25670(16) 0.2518(3) 1.000 0.0412(12) . . Al1 Al Uani 0.20266(6) 0.13800(4) 0.47416(7) 1.000 0.0220(3) . . F1 F Uani 0.4319(2) 0.15583(13) 0.57362(19) 1.000 0.0736(13) . . F2 F Uani 0.4168(2) 0.19324(11) 0.4489(2) 1.000 0.0658(11) . . F3 F Uani 0.52418(17) 0.14272(14) 0.4905(2) 1.000 0.0784(13) . . F4 F Uani 0.43487(17) 0.13229(11) 0.31142(18) 1.000 0.0577(10) . . F5 F Uani 0.30009(17) 0.15239(10) 0.30937(18) 1.000 0.0541(9) . . F6 F Uani 0.3313(2) 0.07964(11) 0.29145(19) 1.000 0.0633(10) . . F7 F Uani 0.45866(18) 0.05996(13) 0.5544(2) 1.000 0.0727(13) . . F8 F Uani 0.49034(19) 0.05481(12) 0.4242(2) 1.000 0.0727(11) . . F9 F Uani 0.3675(2) 0.02674(10) 0.4432(2) 1.000 0.0665(11) . . F10 F Uani 0.0650(2) 0.15076(11) 0.20840(18) 1.000 0.0664(11) . . F11 F Uani -0.05182(19) 0.15908(10) 0.2611(2) 1.000 0.0682(10) . . F12 F Uani -0.0365(2) 0.09774(11) 0.17940(19) 1.000 0.0670(10) . . F13 F Uani 0.0373(2) 0.02067(10) 0.2777(2) 1.000 0.0688(10) . . F14 F Uani 0.1403(2) 0.06311(12) 0.2422(2) 1.000 0.0730(11) . . F15 F Uani 0.15623(18) 0.03832(9) 0.3777(2) 1.000 0.0642(10) . . F16 F Uani 0.0133(2) 0.05390(11) 0.4443(2) 1.000 0.0683(11) . . F17 F Uani -0.09293(17) 0.07280(11) 0.3291(2) 1.000 0.0649(10) . . F18 F Uani -0.03594(18) 0.12557(12) 0.4286(2) 1.000 0.0667(11) . . F19 F Uani 0.2422(4) 0.02214(14) 0.7238(3) 1.000 0.124(2) . . F20 F Uani 0.2997(4) 0.04254(17) 0.6240(5) 1.000 0.170(3) . . F21 F Uani 0.1680(6) 0.01911(15) 0.5880(4) 1.000 0.209(4) . . F22 F Uani 0.0717(4) 0.13620(16) 0.6848(4) 1.000 0.138(2) . . F23 F Uani 0.1147(2) 0.0729(2) 0.7631(3) 1.000 0.1220(19) . . F24 F Uani 0.0423(3) 0.0696(2) 0.6322(3) 1.000 0.130(2) . . F25 F Uani 0.2785(3) 0.10918(17) 0.7972(2) 1.000 0.112(2) . . F26 F Uani 0.3333(3) 0.1257(3) 0.6858(3) 1.000 0.198(4) . . F27 F Uani 0.2338(4) 0.16773(14) 0.7194(4) 1.000 0.154(2) . . F28 F Uani 0.0924(2) 0.21723(12) 0.5581(3) 1.000 0.0873(14) . . F29 F Uani 0.0926(3) 0.29221(12) 0.5315(3) 1.000 0.0979(15) . . F30 F Uani 0.2058(3) 0.26085(13) 0.6294(2) 1.000 0.0850(13) . . F31 F Uani 0.3407(2) 0.26555(10) 0.5498(2) 1.000 0.0673(10) . . F32 F Uani 0.3023(2) 0.27685(11) 0.4059(2) 1.000 0.0658(11) . . F33 F Uani 0.2514(2) 0.32234(10) 0.4971(3) 1.000 0.0844(15) . . F34 F Uani 0.1611(2) 0.23082(10) 0.31642(17) 1.000 0.0615(10) . . F35 F Uani 0.04960(17) 0.23038(10) 0.3803(2) 1.000 0.0703(12) . . F36 F Uani 0.1153(2) 0.29664(9) 0.3608(2) 1.000 0.0703(11) . . O4 O Uani 0.29986(16) 0.10978(9) 0.46643(18) 1.000 0.0330(8) . . O5 O Uani 0.11702(16) 0.13031(9) 0.37980(17) 1.000 0.0305(7) . . O6 O Uani 0.17009(16) 0.11389(9) 0.56542(16) 1.000 0.0294(8) . . O7 O Uani 0.22617(16) 0.19816(8) 0.48431(17) 1.000 0.0293(8) . . C32 C Uani 0.3771(2) 0.11104(15) 0.4401(3) 1.000 0.0337(11) . . C33 C Uani 0.4382(3) 0.1514(2) 0.4888(3) 1.000 0.0544(18) . . C34 C Uani 0.3609(3) 0.11895(17) 0.3366(3) 1.000 0.0432(14) . . C35 C Uani 0.4232(3) 0.06215(19) 0.4652(3) 1.000 0.0523(16) . . C36 C Uani 0.0545(2) 0.10107(13) 0.3307(3) 1.000 0.0311(11) . . C37 C Uani 0.0075(3) 0.12751(17) 0.2432(3) 1.000 0.0501(16) . . C38 C Uani 0.0967(3) 0.05493(16) 0.3070(3) 1.000 0.0490(14) . . C39 C Uani -0.0169(3) 0.08811(18) 0.3845(3) 1.000 0.0503(16) . . C40 C Uani 0.1903(2) 0.09455(13) 0.6491(2) 1.000 0.0293(11) . . C41 C Uani 0.2287(5) 0.0445(2) 0.6475(4) 1.000 0.078(3) . . C42 C Uani 0.1034(3) 0.0919(2) 0.6830(3) 1.000 0.0619(19) . . C43 C Uani 0.2573(4) 0.1257(2) 0.7159(4) 1.000 0.067(2) . . C44 C Uani 0.1932(3) 0.24302(13) 0.4749(3) 1.000 0.0339(11) . . C45 C Uani 0.1457(4) 0.25406(18) 0.5507(4) 1.000 0.066(2) . . C46 C Uani 0.2741(3) 0.27790(16) 0.4817(4) 1.000 0.0542(16) . . C47 C Uani 0.1292(3) 0.25058(16) 0.3815(3) 1.000 0.0521(16) . . C48 C Uani -0.1170(7) 0.4188(4) 0.3446(7) 1.000 0.150(5) . . C49 C Uani -0.0487(8) 0.4277(8) 0.4103(9) 1.000 0.280(14) . . C50 C Uani 0.0332(8) 0.4228(5) 0.4532(7) 1.000 0.166(7) . . C51 C Uani 0.1025(9) 0.4261(8) 0.5070(11) 1.000 0.280(15) . . C52 C Uani 0.1883(7) 0.4327(4) 0.5331(8) 1.000 0.143(6) . . H51 H Uiso 0.86500 0.30410 0.37810 1.000 0.0440 calc R H61 H Uiso 0.85400 0.22880 0.45730 1.000 0.0420 calc R H71 H Uiso 0.78110 0.15300 0.42420 1.000 0.0330 calc R H72 H Uiso 0.77970 0.13480 0.32450 1.000 0.0330 calc R H81 H Uiso 0.64050 0.13390 0.39660 1.000 0.0290 calc R H82 H Uiso 0.62150 0.17950 0.33190 1.000 0.0290 calc R H101 H Uiso 0.59380 0.05560 0.32610 1.000 0.0360 calc R H111 H Uiso 0.57210 0.02010 0.17420 1.000 0.0380 calc R H141 H Uiso 0.66800 0.40540 0.13200 1.000 0.0400 calc R H161 H Uiso 0.89210 0.35730 0.07130 1.000 0.0340 calc R H181 H Uiso 0.58770 0.35560 0.21750 1.000 0.0620 calc R H182 H Uiso 0.66410 0.35530 0.30900 1.000 0.0620 calc R H183 H Uiso 0.63000 0.30630 0.25930 1.000 0.0620 calc R H191 H Uiso 0.83650 0.45030 0.06280 1.000 0.0670 calc R H192 H Uiso 0.73020 0.45100 0.03410 1.000 0.0670 calc R H193 H Uiso 0.78490 0.42210 -0.02520 1.000 0.0670 calc R H201 H Uiso 0.96300 0.28680 0.13370 1.000 0.0520 calc R H202 H Uiso 0.89240 0.24630 0.14080 1.000 0.0520 calc R H203 H Uiso 0.94720 0.27220 0.23020 1.000 0.0520 calc R H231 H Uiso 0.46010 0.06480 -0.15250 1.000 0.0430 calc R H251 H Uiso 0.72200 0.03560 -0.09050 1.000 0.0420 calc R H271 H Uiso 0.44870 0.11970 0.04760 1.000 0.0650 calc R H272 H Uiso 0.41660 0.06550 0.04150 1.000 0.0650 calc R H273 H Uiso 0.38900 0.09940 -0.04500 1.000 0.0650 calc R H281 H Uiso 0.53360 0.04670 -0.27260 1.000 0.0810 calc R H282 H Uiso 0.57440 -0.00350 -0.23480 1.000 0.0810 calc R H283 H Uiso 0.63890 0.03860 -0.24940 1.000 0.0810 calc R H291 H Uiso 0.81480 0.05730 0.05630 1.000 0.0560 calc R H292 H Uiso 0.76760 0.02310 0.11460 1.000 0.0560 calc R H293 H Uiso 0.77060 0.07920 0.13220 1.000 0.0560 calc R H311 H Uiso 0.38010 0.23210 0.25170 1.000 0.0620 calc R H312 H Uiso 0.39660 0.28430 0.21740 1.000 0.0620 calc R H313 H Uiso 0.45170 0.26630 0.31410 1.000 0.0620 calc R H481 H Uiso -0.09800 0.40080 0.29750 1.000 0.2250 calc R H482 H Uiso -0.14430 0.44870 0.31940 1.000 0.2250 calc R H483 H Uiso -0.16040 0.40010 0.36750 1.000 0.2250 calc R H491 H Uiso -0.04970 0.46280 0.40550 1.000 0.3350 calc R H492 H Uiso -0.07660 0.42130 0.46120 1.000 0.3350 calc R H501 H Uiso 0.03120 0.38770 0.45490 1.000 0.1990 calc R H502 H Uiso 0.05790 0.42940 0.40020 1.000 0.1990 calc R H511 H Uiso 0.09960 0.39570 0.53890 1.000 0.3360 calc R H512 H Uiso 0.08420 0.45000 0.54670 1.000 0.3360 calc R H521 H Uiso 0.21420 0.40880 0.57830 1.000 0.2140 calc R H522 H Uiso 0.20020 0.46450 0.55950 1.000 0.2140 calc R H523 H Uiso 0.21490 0.42990 0.48100 1.000 0.2140 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0197(1) 0.0181(1) 0.0164(1) -0.0001(1) 0.0027(1) 0.0006(1) O1 0.0414(16) 0.0398(15) 0.0421(16) 0.0023(12) 0.0235(13) 0.0081(12) O2 0.0410(15) 0.0256(13) 0.0251(13) 0.0062(11) 0.0017(11) -0.0016(11) O3 0.0591(19) 0.0355(15) 0.0271(15) -0.0008(12) -0.0121(13) -0.0029(14) N1 0.0279(15) 0.0289(15) 0.0193(14) -0.0014(11) 0.0048(11) -0.0071(12) N2 0.0225(14) 0.0304(15) 0.0193(14) 0.0002(11) 0.0025(11) -0.0025(12) N3 0.0257(14) 0.0215(14) 0.0224(14) -0.0013(11) 0.0088(11) -0.0011(11) N4 0.0266(14) 0.0222(14) 0.0232(14) -0.0024(11) 0.0072(11) -0.0034(11) N5 0.0224(14) 0.0236(14) 0.0250(14) 0.0010(11) 0.0013(12) 0.0005(11) C1 0.0308(18) 0.0234(17) 0.0212(16) 0.0017(13) 0.0055(14) 0.0014(14) C2 0.0239(16) 0.0236(17) 0.0215(16) -0.0035(14) 0.0014(13) 0.0008(13) C3 0.0350(19) 0.0216(17) 0.0278(19) 0.0013(14) 0.0032(16) -0.0014(14) C4 0.0196(15) 0.0250(17) 0.0198(15) 0.0000(13) 0.0062(12) 0.0000(13) C5 0.042(2) 0.044(2) 0.0206(17) -0.0034(16) 0.0007(15) -0.0179(18) C6 0.036(2) 0.045(2) 0.0193(17) -0.0016(16) -0.0003(15) -0.0115(17) C7 0.0293(18) 0.0288(18) 0.0215(16) 0.0039(14) 0.0022(14) 0.0015(14) C8 0.0297(18) 0.0256(17) 0.0193(16) 0.0001(13) 0.0086(13) -0.0005(14) C9 0.0202(15) 0.0223(16) 0.0213(16) 0.0000(13) 0.0052(12) 0.0024(12) C10 0.040(2) 0.0246(18) 0.0312(19) 0.0017(14) 0.0164(16) -0.0045(15) C11 0.041(2) 0.0227(17) 0.034(2) -0.0017(15) 0.0150(16) -0.0069(15) C12 0.0295(18) 0.0244(17) 0.0208(16) -0.0024(13) 0.0043(14) -0.0079(14) C13 0.0324(19) 0.0243(17) 0.0312(18) -0.0085(14) 0.0091(15) -0.0063(14) C14 0.039(2) 0.0217(17) 0.037(2) -0.0066(15) 0.0071(17) 0.0003(15) C15 0.045(2) 0.0224(17) 0.0248(18) -0.0050(14) 0.0051(16) -0.0100(15) C16 0.0314(18) 0.0310(19) 0.0229(17) -0.0036(14) 0.0059(14) -0.0117(15) C17 0.0243(17) 0.0292(18) 0.0214(16) -0.0040(14) 0.0016(13) -0.0079(14) C18 0.046(2) 0.033(2) 0.053(3) -0.0069(18) 0.026(2) -0.0021(18) C19 0.070(3) 0.026(2) 0.039(2) -0.0007(17) 0.014(2) -0.0082(19) C20 0.0243(18) 0.042(2) 0.036(2) 0.0056(17) 0.0058(15) -0.0005(16) C21 0.0320(18) 0.0185(16) 0.0230(16) -0.0030(13) 0.0078(14) -0.0043(13) C22 0.0333(19) 0.0228(17) 0.0318(19) -0.0027(14) 0.0036(15) -0.0054(14) C23 0.044(2) 0.0260(19) 0.0294(19) -0.0018(15) -0.0039(17) -0.0084(16) C24 0.063(3) 0.0216(18) 0.0268(19) -0.0032(14) 0.0124(18) -0.0109(17) C25 0.050(2) 0.0242(18) 0.036(2) -0.0033(15) 0.0201(18) -0.0020(16) C26 0.0347(19) 0.0209(17) 0.0297(18) -0.0009(14) 0.0107(15) -0.0008(14) C27 0.028(2) 0.048(2) 0.051(3) -0.005(2) 0.0046(18) -0.0043(18) C28 0.093(4) 0.040(2) 0.030(2) -0.0081(18) 0.019(2) -0.022(2) C29 0.035(2) 0.037(2) 0.042(2) -0.0003(17) 0.0103(17) 0.0071(17) C30 0.0243(17) 0.0287(18) 0.0274(18) -0.0007(14) 0.0019(14) 0.0010(14) C31 0.031(2) 0.051(2) 0.044(2) -0.0082(19) 0.0136(17) 0.0080(18) Al1 0.0168(4) 0.0241(5) 0.0248(5) 0.0034(4) 0.0044(4) 0.0007(4) F1 0.0566(18) 0.116(3) 0.0481(16) -0.0205(17) 0.0125(14) -0.0350(18) F2 0.0573(18) 0.0598(18) 0.088(2) -0.0042(16) 0.0325(16) -0.0211(14) F3 0.0226(13) 0.134(3) 0.078(2) 0.007(2) 0.0107(13) -0.0156(16) F4 0.0447(14) 0.085(2) 0.0511(15) 0.0233(14) 0.0270(12) 0.0187(14) F5 0.0413(14) 0.0704(18) 0.0506(15) 0.0207(13) 0.0109(12) 0.0222(13) F6 0.0670(19) 0.076(2) 0.0460(15) -0.0122(14) 0.0114(14) 0.0106(16) F7 0.0461(16) 0.119(3) 0.0558(17) 0.0435(18) 0.0179(13) 0.0346(17) F8 0.0549(17) 0.097(2) 0.081(2) 0.0374(18) 0.0455(16) 0.0467(17) F9 0.0675(19) 0.0455(16) 0.097(2) 0.0106(15) 0.0404(18) 0.0194(15) F10 0.074(2) 0.078(2) 0.0388(14) 0.0169(14) -0.0034(13) -0.0271(16) F11 0.0492(16) 0.0534(17) 0.084(2) 0.0075(15) -0.0199(15) 0.0161(13) F12 0.0647(18) 0.072(2) 0.0463(15) -0.0011(14) -0.0228(14) -0.0147(15) F13 0.0611(18) 0.0396(15) 0.096(2) -0.0214(15) -0.0005(16) -0.0091(13) F14 0.0590(18) 0.088(2) 0.078(2) -0.0310(18) 0.0282(16) 0.0020(16) F15 0.0514(16) 0.0354(14) 0.091(2) 0.0029(14) -0.0126(15) 0.0130(12) F16 0.0633(18) 0.077(2) 0.0609(18) 0.0222(16) 0.0075(14) -0.0291(16) F17 0.0294(13) 0.074(2) 0.087(2) -0.0072(16) 0.0055(13) -0.0167(13) F18 0.0414(15) 0.087(2) 0.078(2) -0.0203(17) 0.0267(14) -0.0052(14) F19 0.215(5) 0.085(3) 0.083(3) 0.060(2) 0.059(3) 0.086(3) F20 0.181(5) 0.104(3) 0.297(7) 0.117(4) 0.201(6) 0.102(4) F21 0.373(11) 0.045(2) 0.131(4) -0.033(3) -0.093(5) 0.052(4) F22 0.168(4) 0.108(3) 0.186(5) 0.064(3) 0.139(4) 0.087(3) F23 0.063(2) 0.235(5) 0.078(2) 0.096(3) 0.0364(19) 0.027(3) F24 0.068(2) 0.242(6) 0.089(3) -0.052(3) 0.038(2) -0.086(3) F25 0.148(4) 0.138(4) 0.0307(16) 0.0134(19) -0.0168(19) -0.052(3) F26 0.069(3) 0.444(12) 0.081(3) -0.028(5) 0.020(2) -0.128(5) F27 0.177(5) 0.054(2) 0.165(5) -0.022(3) -0.092(4) -0.005(3) F28 0.088(2) 0.064(2) 0.140(3) 0.040(2) 0.087(2) 0.0275(18) F29 0.134(3) 0.0545(19) 0.133(3) 0.021(2) 0.087(3) 0.046(2) F30 0.134(3) 0.082(2) 0.0435(17) -0.0051(16) 0.0298(19) 0.021(2) F31 0.0616(18) 0.0570(17) 0.0662(18) 0.0004(14) -0.0187(15) -0.0178(14) F32 0.0646(18) 0.0634(19) 0.075(2) 0.0241(16) 0.0279(16) -0.0124(15) F33 0.098(3) 0.0299(15) 0.111(3) -0.0058(16) -0.004(2) -0.0106(15) F34 0.085(2) 0.0571(17) 0.0360(14) 0.0063(12) 0.0013(14) 0.0063(15) F35 0.0338(14) 0.0463(16) 0.115(3) 0.0082(16) -0.0141(15) 0.0037(12) F36 0.088(2) 0.0364(15) 0.073(2) 0.0185(13) -0.0081(17) 0.0114(14) O4 0.0196(12) 0.0368(14) 0.0446(15) 0.0020(12) 0.0114(11) 0.0026(10) O5 0.0233(12) 0.0314(13) 0.0327(13) 0.0026(11) -0.0014(10) -0.0008(10) O6 0.0280(13) 0.0317(13) 0.0294(13) 0.0091(10) 0.0086(10) 0.0041(10) O7 0.0278(13) 0.0237(12) 0.0351(14) 0.0054(10) 0.0051(11) -0.0001(10) C32 0.0201(17) 0.048(2) 0.034(2) 0.0048(17) 0.0085(15) 0.0043(16) C33 0.029(2) 0.085(4) 0.051(3) 0.001(3) 0.0133(19) -0.015(2) C34 0.032(2) 0.058(3) 0.041(2) 0.007(2) 0.0113(18) 0.0143(19) C35 0.038(2) 0.072(3) 0.054(3) 0.022(2) 0.025(2) 0.028(2) C36 0.0235(17) 0.0301(19) 0.035(2) 0.0016(15) -0.0023(15) -0.0016(14) C37 0.045(2) 0.050(3) 0.046(3) 0.006(2) -0.008(2) -0.009(2) C38 0.041(2) 0.041(2) 0.060(3) -0.010(2) 0.002(2) -0.0019(19) C39 0.031(2) 0.058(3) 0.059(3) 0.000(2) 0.005(2) -0.009(2) C40 0.0301(18) 0.0312(19) 0.0268(18) 0.0084(15) 0.0073(14) 0.0043(15) C41 0.120(5) 0.062(4) 0.065(4) 0.029(3) 0.046(4) 0.049(4) C42 0.046(3) 0.091(4) 0.050(3) 0.021(3) 0.014(2) 0.001(3) C43 0.079(4) 0.072(4) 0.044(3) 0.004(3) 0.001(3) -0.010(3) C44 0.038(2) 0.0270(19) 0.036(2) 0.0049(15) 0.0073(16) 0.0005(16) C45 0.085(4) 0.042(3) 0.082(4) 0.011(3) 0.043(3) 0.016(3) C46 0.059(3) 0.034(2) 0.062(3) 0.000(2) -0.001(2) -0.005(2) C47 0.054(3) 0.036(2) 0.059(3) 0.011(2) -0.001(2) 0.004(2) C48 0.139(9) 0.156(9) 0.152(9) -0.078(8) 0.031(7) -0.056(7) C49 0.089(8) 0.61(4) 0.121(10) -0.011(16) -0.014(7) -0.057(14) C50 0.138(9) 0.270(16) 0.088(7) -0.018(8) 0.024(6) 0.066(10) C51 0.119(11) 0.51(4) 0.172(14) 0.058(18) -0.041(10) -0.014(16) C52 0.134(9) 0.117(8) 0.197(12) -0.032(7) 0.080(9) -0.021(7) #================================================================== # 10. MOLECULAR GEOMETRY #=================================================================== loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 N5 2.158(3) . . yes Re1 C1 1.923(3) . . yes Re1 C2 1.943(3) . . yes Re1 C3 1.945(3) . . yes Re1 C4 2.233(3) . . yes Re1 C9 2.215(3) . . yes Al1 O6 1.727(3) . . yes Al1 O4 1.731(3) . . yes Al1 O5 1.724(3) . . yes Al1 O7 1.733(3) . . yes F1 C33 1.325(5) . . yes F2 C33 1.332(6) . . yes F3 C33 1.348(6) . . yes F4 C34 1.345(5) . . yes F5 C34 1.327(5) . . yes F6 C34 1.327(6) . . yes F7 C35 1.342(5) . . yes F8 C35 1.350(6) . . yes F9 C35 1.309(6) . . yes F10 C37 1.314(6) . . yes F11 C37 1.352(6) . . yes F12 C37 1.342(5) . . yes F13 C38 1.335(5) . . yes F14 C38 1.342(6) . . yes F15 C38 1.327(5) . . yes F16 C39 1.333(6) . . yes F17 C39 1.347(5) . . yes F18 C39 1.321(6) . . yes F19 C41 1.295(7) . . yes F20 C41 1.236(10) . . yes F21 C41 1.347(9) . . yes F22 C42 1.344(7) . . yes F23 C42 1.306(7) . . yes F24 C42 1.242(7) . . yes F25 C43 1.291(7) . . yes F26 C43 1.361(8) . . yes F27 C43 1.243(7) . . yes F28 C45 1.347(7) . . yes F29 C45 1.343(7) . . yes F30 C45 1.347(7) . . yes F31 C46 1.325(6) . . yes F32 C46 1.328(6) . . yes F33 C46 1.336(5) . . yes F34 C47 1.330(5) . . yes F35 C47 1.354(5) . . yes F36 C47 1.341(5) . . yes O1 C1 1.151(4) . . yes O2 C2 1.157(4) . . yes O3 C3 1.151(4) . . yes O4 C32 1.349(4) . . yes O5 C36 1.354(5) . . yes O6 C40 1.354(4) . . yes O7 C44 1.358(4) . . yes N1 C12 1.445(4) . . yes N1 C4 1.368(4) . . yes N1 C5 1.390(4) . . yes N2 C6 1.380(5) . . yes N2 C4 1.367(4) . . yes N2 C7 1.455(4) . . yes N3 C10 1.383(4) . . yes N3 C8 1.459(4) . . yes N3 C9 1.363(4) . . yes N4 C9 1.372(4) . . yes N4 C11 1.384(5) . . yes N4 C21 1.441(4) . . yes N5 C30 1.140(4) . . yes C5 C6 1.334(5) . . no C7 C8 1.526(4) . . no C10 C11 1.336(4) . . no C12 C13 1.394(5) . . no C12 C17 1.400(4) . . no C13 C18 1.514(6) . . no C13 C14 1.395(5) . . no C14 C15 1.390(6) . . no C15 C16 1.391(5) . . no C15 C19 1.508(5) . . no C16 C17 1.391(5) . . no C17 C20 1.509(5) . . no C21 C26 1.396(4) . . no C21 C22 1.395(4) . . no C22 C23 1.396(5) . . no C22 C27 1.505(6) . . no C23 C24 1.388(7) . . no C24 C25 1.384(7) . . no C24 C28 1.516(6) . . no C25 C26 1.394(5) . . no C26 C29 1.512(6) . . no C30 C31 1.461(6) . . no C5 H51 0.9500 . . no C6 H61 0.9500 . . no C7 H72 0.9900 . . no C7 H71 0.9900 . . no C8 H81 0.9900 . . no C8 H82 0.9900 . . no C10 H101 0.9500 . . no C11 H111 0.9500 . . no C14 H141 0.9500 . . no C16 H161 0.9500 . . no C18 H183 0.9800 . . no C18 H181 0.9800 . . no C18 H182 0.9800 . . no C19 H191 0.9800 . . no C19 H193 0.9800 . . no C19 H192 0.9800 . . no C20 H202 0.9800 . . no C20 H201 0.9800 . . no C20 H203 0.9800 . . no C23 H231 0.9500 . . no C25 H251 0.9500 . . no C27 H273 0.9800 . . no C27 H271 0.9800 . . no C27 H272 0.9800 . . no C28 H281 0.9800 . . no C28 H283 0.9800 . . no C28 H282 0.9800 . . no C29 H291 0.9800 . . no C29 H293 0.9800 . . no C29 H292 0.9800 . . no C31 H313 0.9800 . . no C31 H312 0.9800 . . no C31 H311 0.9800 . . no C32 C33 1.551(7) . . no C32 C34 1.554(6) . . no C32 C35 1.557(7) . . no C36 C37 1.550(6) . . no C36 C38 1.536(6) . . no C36 C39 1.567(6) . . no C40 C41 1.533(7) . . no C40 C42 1.553(6) . . no C40 C43 1.544(7) . . no C44 C45 1.541(8) . . no C44 C46 1.576(6) . . no C44 C47 1.545(6) . . no C48 C49 1.297(17) . . no C49 C50 1.290(18) . . no C50 C51 1.190(19) . . no C51 C52 1.307(19) . . no C48 H481 0.9800 . . no C48 H482 0.9800 . . no C48 H483 0.9800 . . no C49 H491 0.9900 . . no C49 H492 0.9900 . . no C50 H501 0.9900 . . no C50 H502 0.9900 . . no C51 H511 0.9900 . . no C51 H512 0.9900 . . no C52 H521 0.9800 . . no C52 H522 0.9800 . . no C52 H523 0.9800 . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Re1 C1 177.83(12) . . . yes N5 Re1 C2 94.57(12) . . . yes N5 Re1 C3 92.37(12) . . . yes N5 Re1 C4 85.51(11) . . . yes N5 Re1 C9 84.89(11) . . . yes C1 Re1 C2 86.51(14) . . . yes C1 Re1 C3 89.67(13) . . . yes C1 Re1 C4 92.57(12) . . . yes C1 Re1 C9 94.35(13) . . . yes C2 Re1 C3 79.57(13) . . . yes C2 Re1 C4 92.69(12) . . . yes C2 Re1 C9 170.39(12) . . . yes C3 Re1 C4 171.80(13) . . . yes C3 Re1 C9 90.86(13) . . . yes C4 Re1 C9 96.83(11) . . . yes O4 Al1 O7 106.71(13) . . . yes O5 Al1 O6 107.99(13) . . . yes O5 Al1 O7 107.54(13) . . . yes O6 Al1 O7 114.08(13) . . . yes O4 Al1 O6 107.37(13) . . . yes O4 Al1 O5 113.29(14) . . . yes Al1 O4 C32 148.7(3) . . . yes Al1 O5 C36 147.8(3) . . . yes Al1 O6 C40 150.5(2) . . . yes Al1 O7 C44 146.6(3) . . . yes C4 N1 C5 111.8(3) . . . yes C4 N1 C12 129.1(3) . . . yes C5 N1 C12 119.1(3) . . . yes C6 N2 C7 121.3(3) . . . yes C4 N2 C6 112.1(3) . . . yes C4 N2 C7 126.6(3) . . . yes C8 N3 C10 122.5(3) . . . yes C8 N3 C9 124.3(3) . . . yes C9 N3 C10 112.5(3) . . . yes C11 N4 C21 119.6(3) . . . yes C9 N4 C11 111.7(3) . . . yes C9 N4 C21 128.7(3) . . . yes Re1 N5 C30 178.3(3) . . . yes Re1 C1 O1 176.9(3) . . . yes Re1 C2 O2 167.6(3) . . . yes Re1 C3 O3 170.1(3) . . . yes N1 C4 N2 102.5(3) . . . yes Re1 C4 N1 127.0(2) . . . yes Re1 C4 N2 130.5(2) . . . yes N1 C5 C6 106.6(3) . . . yes N2 C6 C5 107.0(3) . . . yes N2 C7 C8 113.0(3) . . . yes N3 C8 C7 110.6(3) . . . yes N3 C9 N4 102.4(3) . . . yes Re1 C9 N3 128.6(2) . . . yes Re1 C9 N4 128.8(2) . . . yes N3 C10 C11 106.3(3) . . . yes N4 C11 C10 107.1(3) . . . yes N1 C12 C13 119.0(3) . . . yes N1 C12 C17 117.9(3) . . . yes C13 C12 C17 122.8(3) . . . no C12 C13 C18 121.8(3) . . . no C14 C13 C18 120.9(3) . . . no C12 C13 C14 117.3(3) . . . no C13 C14 C15 122.1(4) . . . no C14 C15 C19 120.8(4) . . . no C16 C15 C19 120.8(4) . . . no C14 C15 C16 118.4(3) . . . no C15 C16 C17 122.1(3) . . . no C12 C17 C20 121.3(3) . . . no C16 C17 C20 121.3(3) . . . no C12 C17 C16 117.3(3) . . . no N4 C21 C26 118.4(3) . . . yes N4 C21 C22 118.5(3) . . . yes C22 C21 C26 122.7(3) . . . no C21 C22 C23 117.1(3) . . . no C21 C22 C27 121.6(3) . . . no C23 C22 C27 121.3(3) . . . no C22 C23 C24 122.0(4) . . . no C23 C24 C28 120.8(4) . . . no C23 C24 C25 118.7(4) . . . no C25 C24 C28 120.5(4) . . . no C24 C25 C26 121.9(4) . . . no C21 C26 C25 117.4(3) . . . no C25 C26 C29 120.6(3) . . . no C21 C26 C29 121.9(3) . . . no N5 C30 C31 178.2(4) . . . yes C6 C5 H51 127.00 . . . no N1 C5 H51 127.00 . . . no N2 C6 H61 126.00 . . . no C5 C6 H61 127.00 . . . no N2 C7 H71 109.00 . . . no N2 C7 H72 109.00 . . . no C8 C7 H71 109.00 . . . no C8 C7 H72 109.00 . . . no H71 C7 H72 108.00 . . . no N3 C8 H81 109.00 . . . no N3 C8 H82 109.00 . . . no C7 C8 H81 110.00 . . . no H81 C8 H82 108.00 . . . no C7 C8 H82 109.00 . . . no C11 C10 H101 127.00 . . . no N3 C10 H101 127.00 . . . no N4 C11 H111 126.00 . . . no C10 C11 H111 127.00 . . . no C13 C14 H141 119.00 . . . no C15 C14 H141 119.00 . . . no C15 C16 H161 119.00 . . . no C17 C16 H161 119.00 . . . no C13 C18 H183 109.00 . . . no H181 C18 H182 109.00 . . . no H181 C18 H183 110.00 . . . no H182 C18 H183 110.00 . . . no C13 C18 H181 109.00 . . . no C13 C18 H182 109.00 . . . no C15 C19 H191 110.00 . . . no H191 C19 H193 110.00 . . . no H192 C19 H193 109.00 . . . no C15 C19 H192 109.00 . . . no C15 C19 H193 110.00 . . . no H191 C19 H192 109.00 . . . no C17 C20 H201 110.00 . . . no C17 C20 H202 109.00 . . . no C17 C20 H203 109.00 . . . no H201 C20 H203 109.00 . . . no H202 C20 H203 109.00 . . . no H201 C20 H202 109.00 . . . no C22 C23 H231 119.00 . . . no C24 C23 H231 119.00 . . . no C24 C25 H251 119.00 . . . no C26 C25 H251 119.00 . . . no H271 C27 H272 109.00 . . . no H271 C27 H273 109.00 . . . no H272 C27 H273 109.00 . . . no C22 C27 H271 110.00 . . . no C22 C27 H272 110.00 . . . no C22 C27 H273 110.00 . . . no C24 C28 H281 109.00 . . . no C24 C28 H282 109.00 . . . no C24 C28 H283 109.00 . . . no H282 C28 H283 110.00 . . . no H281 C28 H282 109.00 . . . no H281 C28 H283 110.00 . . . no C26 C29 H291 109.00 . . . no H291 C29 H292 109.00 . . . no C26 C29 H292 109.00 . . . no C26 C29 H293 109.00 . . . no H292 C29 H293 110.00 . . . no H291 C29 H293 109.00 . . . no C30 C31 H313 109.00 . . . no C30 C31 H312 109.00 . . . no H312 C31 H313 109.00 . . . no H311 C31 H312 109.00 . . . no H311 C31 H313 110.00 . . . no C30 C31 H311 110.00 . . . no O4 C32 C33 111.1(3) . . . yes O4 C32 C34 111.4(3) . . . yes O4 C32 C35 106.9(3) . . . yes C33 C32 C34 108.3(3) . . . no C33 C32 C35 109.8(3) . . . no C34 C32 C35 109.3(3) . . . no F1 C33 F2 107.1(4) . . . yes F1 C33 F3 107.4(4) . . . yes F1 C33 C32 111.0(4) . . . yes F2 C33 F3 107.9(4) . . . yes F2 C33 C32 111.9(4) . . . yes F3 C33 C32 111.4(4) . . . yes F4 C34 F5 107.6(4) . . . yes F4 C34 F6 107.4(4) . . . yes F4 C34 C32 112.7(3) . . . yes F5 C34 F6 107.3(4) . . . yes F5 C34 C32 110.6(4) . . . yes F6 C34 C32 111.1(4) . . . yes F7 C35 F8 106.7(4) . . . yes F7 C35 F9 108.1(4) . . . yes F7 C35 C32 110.1(4) . . . yes F8 C35 F9 107.3(4) . . . yes F8 C35 C32 112.4(4) . . . yes F9 C35 C32 112.0(4) . . . yes O5 C36 C37 108.2(3) . . . yes O5 C36 C38 110.9(3) . . . yes O5 C36 C39 110.7(3) . . . yes C37 C36 C38 110.1(4) . . . no C37 C36 C39 108.4(3) . . . no C38 C36 C39 108.5(3) . . . no F10 C37 F11 108.1(4) . . . yes F10 C37 F12 107.2(4) . . . yes F10 C37 C36 111.2(4) . . . yes F11 C37 F12 107.7(4) . . . yes F11 C37 C36 110.2(3) . . . yes F12 C37 C36 112.2(4) . . . yes F13 C38 F14 107.8(4) . . . yes F13 C38 F15 108.0(4) . . . yes F13 C38 C36 113.1(4) . . . yes F14 C38 F15 106.5(4) . . . yes F14 C38 C36 110.1(4) . . . yes F15 C38 C36 111.1(4) . . . yes F16 C39 F17 108.1(4) . . . yes F16 C39 F18 108.3(4) . . . yes F16 C39 C36 110.4(4) . . . yes F17 C39 F18 107.9(4) . . . yes F17 C39 C36 111.5(4) . . . yes F18 C39 C36 110.5(4) . . . yes O6 C40 C41 111.1(3) . . . yes O6 C40 C42 107.9(3) . . . yes O6 C40 C43 111.2(3) . . . yes C41 C40 C42 109.3(4) . . . no C41 C40 C43 109.3(4) . . . no C42 C40 C43 107.9(3) . . . no F19 C41 F20 105.8(7) . . . yes F19 C41 F21 106.6(5) . . . yes F19 C41 C40 114.5(5) . . . yes F20 C41 F21 108.0(6) . . . yes F20 C41 C40 114.9(5) . . . yes F21 C41 C40 106.7(5) . . . yes F22 C42 F23 109.3(5) . . . yes F22 C42 F24 104.7(5) . . . yes F22 C42 C40 108.2(5) . . . yes F23 C42 F24 106.8(5) . . . yes F23 C42 C40 113.3(4) . . . yes F24 C42 C40 114.2(4) . . . yes F25 C43 F26 106.2(5) . . . yes F25 C43 F27 108.2(5) . . . yes F25 C43 C40 114.0(5) . . . yes F26 C43 F27 107.4(6) . . . yes F26 C43 C40 106.1(5) . . . yes F27 C43 C40 114.3(5) . . . yes O7 C44 C45 110.1(4) . . . yes O7 C44 C46 107.5(4) . . . yes O7 C44 C47 111.7(3) . . . yes C45 C44 C46 109.7(4) . . . no C45 C44 C47 110.3(4) . . . no C46 C44 C47 107.5(4) . . . no F28 C45 F29 106.2(5) . . . yes F28 C45 F30 110.1(5) . . . yes F28 C45 C44 108.5(4) . . . yes F29 C45 F30 109.8(4) . . . yes F29 C45 C44 112.0(5) . . . yes F30 C45 C44 110.2(5) . . . yes F31 C46 F32 108.7(4) . . . yes F31 C46 F33 107.3(4) . . . yes F31 C46 C44 110.3(4) . . . yes F32 C46 F33 109.1(4) . . . yes F32 C46 C44 110.4(4) . . . yes F33 C46 C44 111.0(4) . . . yes F34 C47 F35 108.2(4) . . . yes F34 C47 F36 107.3(4) . . . yes F34 C47 C44 111.0(4) . . . yes F35 C47 F36 108.0(4) . . . yes F35 C47 C44 109.8(4) . . . yes F36 C47 C44 112.5(4) . . . yes C48 C49 C50 153.5(17) . . . no C49 C50 C51 163.6(17) . . . no C50 C51 C52 155.1(16) . . . no C49 C48 H481 110.00 . . . no C49 C48 H482 110.00 . . . no C49 C48 H483 109.00 . . . no H481 C48 H482 110.00 . . . no H481 C48 H483 109.00 . . . no H482 C48 H483 109.00 . . . no C48 C49 H491 98.00 . . . no C48 C49 H492 98.00 . . . no C50 C49 H491 98.00 . . . no C50 C49 H492 98.00 . . . no H491 C49 H492 104.00 . . . no C49 C50 H501 95.00 . . . no C49 C50 H502 95.00 . . . no C51 C50 H501 95.00 . . . no C51 C50 H502 95.00 . . . no H501 C50 H502 103.00 . . . no C50 C51 H511 98.00 . . . no C50 C51 H512 98.00 . . . no C52 C51 H511 98.00 . . . no C52 C51 H512 98.00 . . . no H511 C51 H512 104.00 . . . no C51 C52 H521 110.00 . . . no C51 C52 H522 109.00 . . . no C51 C52 H523 109.00 . . . no H521 C52 H522 109.00 . . . no H521 C52 H523 110.00 . . . no H522 C52 H523 109.00 . . . no # End of Crystallographic Information File _database_code_depnum_ccdc_archive 'CCDC 959157' ####################################################################### # # 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_Compound_5d #=================================================================== #=================================================================== # 5. CHEMICAL DATA #=================================================================== _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety 'C31 H33 N4 O3 Re' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C31 H33 N4 O3 Re' _chemical_formula_weight 695.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=================================================================== # 6. CRYSTAL DATA #=================================================================== _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,y,1/2-z 3 -x,-y,-z 4 x,-y,1/2+z 5 1/2+x,1/2+y,z 6 1/2-x,1/2+y,1/2-z 7 1/2-x,1/2-y,-z 8 1/2+x,1/2-y,1/2+z _cell_length_a 36.8760(8) _cell_length_b 8.5127(2) _cell_length_c 20.0287(5) _cell_angle_alpha 90 _cell_angle_beta 114.3982(8) _cell_angle_gamma 90 _cell_volume 5725.8(2) _cell_formula_units_Z 8 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 9321 _cell_measurement_theta_min 1.21 _cell_measurement_theta_max 25.47 _exptl_crystal_description fragment _exptl_crystal_colour colorless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method none _exptl_crystal_F_000 2768 _exptl_absorpt_coefficient_mu 4.283 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4028 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_process_details 'SADABS, Bruker, 2008b' _exptl_special_details ; Diffractometer operator E. Herdtweck scanspeed 10 s per frame dx 60 6302 frames measured in 12 data sets phi-scan with delta_phi = 0.50 omega-scans with delta_omega = 0.50 ; #=================================================================== # 7. EXPERIMENTAL DATA #=================================================================== _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'rotating anode FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' \k-geometry diffractometer ' _diffrn_measurement_device_type ' Bruker APEX-II CCD ' _diffrn_measurement_method ' phi- and omega-rotation ' _diffrn_detector ' CCD plate ' _diffrn_detector_area_resol_mean 16 # 8 for binned mode _diffrn_standards_decay_% 0 # number of measured reflections (redundant set) _diffrn_reflns_number 70708 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0135 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 25.47 _reflns_number_total 5301 _reflns_number_gt 5170 # number of observed reflections (> n sig(I)) _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX II Control Software (Bruker, 2008a)' _computing_cell_refinement 'SAINT (Bruker, 2008b)' _computing_data_reduction 'SAINT (Bruker, 2008b)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2010)' _computing_publication_material 'PLATON (Spek, 2010)' #=================================================================== # 8. REFINEMENT DATA #=================================================================== _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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 sigma _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0131P)^2^+10.6504P] 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_number_reflns 5301 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0143 _refine_ls_R_factor_gt 0.0138 _refine_ls_wR_factor_ref 0.0345 _refine_ls_wR_factor_gt 0.0342 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 1.102 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.47 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.599 _refine_diff_density_min -0.676 _refine_diff_density_rms 0.057 #=================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=================================================================== loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Re1 Re Uani 0.16369(1) -0.03082(1) 0.10471(1) 1.000 0.0149(1) . . O1 O Uani 0.07717(4) -0.12404(19) 0.00277(8) 1.000 0.0284(5) . . O2 O Uani 0.20235(4) -0.33400(18) 0.07874(9) 1.000 0.0293(5) . . O3 O Uani 0.14873(5) -0.20442(18) 0.22667(8) 1.000 0.0298(5) . . N1 N Uani 0.15910(5) 0.0911(2) -0.05269(9) 1.000 0.0220(5) . . N2 N Uani 0.19872(5) 0.2341(2) 0.03491(9) 1.000 0.0203(5) . . N3 N Uani 0.18001(5) 0.23742(19) 0.21115(9) 1.000 0.0190(5) . . N4 N Uani 0.12247(5) 0.29860(19) 0.13024(9) 1.000 0.0181(5) . . C1 C Uani 0.10965(6) -0.0850(2) 0.03815(10) 1.000 0.0195(6) . . C2 C Uani 0.18697(6) -0.2201(2) 0.08520(11) 1.000 0.0192(6) . . C3 C Uani 0.15499(6) -0.1391(2) 0.18133(11) 1.000 0.0200(6) . . C4 C Uani 0.17463(6) 0.1064(2) 0.02230(10) 1.000 0.0185(6) . . C5 C Uani 0.17333(6) 0.2073(3) -0.08451(12) 1.000 0.0280(7) . . C6 C Uani 0.19804(6) 0.2970(3) -0.02919(12) 1.000 0.0263(6) . . C7 C Uani 0.22574(6) 0.2912(2) 0.10770(11) 1.000 0.0224(6) . . C8 C Uani 0.24829(6) 0.1560(2) 0.15776(11) 1.000 0.0235(6) . . C9 C Uani 0.22391(6) 0.0547(2) 0.18722(11) 1.000 0.0192(6) . . C10 C Uani 0.21632(6) 0.1424(2) 0.24678(11) 1.000 0.0225(6) . . C11 C Uani 0.15104(5) 0.1861(2) 0.14727(10) 1.000 0.0170(5) . . C12 C Uani 0.17039(6) 0.3793(2) 0.23287(11) 1.000 0.0232(6) . . C13 C Uani 0.13420(6) 0.4182(3) 0.18234(11) 1.000 0.0234(6) . . C14 C Uani 0.13528(7) -0.0389(2) -0.09453(11) 1.000 0.0233(6) . . C15 C Uani 0.15480(7) -0.1744(3) -0.10123(11) 1.000 0.0263(7) . . C16 C Uani 0.13156(7) -0.3001(3) -0.13997(12) 1.000 0.0318(7) . . C17 C Uani 0.09027(7) -0.2911(3) -0.17337(12) 1.000 0.0334(7) . . C18 C Uani 0.07237(7) -0.1516(3) -0.16800(12) 1.000 0.0323(7) . . C19 C Uani 0.09401(7) -0.0233(3) -0.12890(12) 1.000 0.0269(7) . . C20 C Uani 0.19972(7) -0.1839(3) -0.07032(13) 1.000 0.0346(8) . . C21 C Uani 0.06585(9) -0.4294(3) -0.21542(15) 1.000 0.0491(10) . . C22 C Uani 0.07338(7) 0.1257(3) -0.12347(14) 1.000 0.0378(8) . . C23 C Uani 0.08401(5) 0.3004(2) 0.06846(10) 1.000 0.0177(5) . . C24 C Uani 0.07823(6) 0.4040(2) 0.01104(11) 1.000 0.0205(6) . . C25 C Uani 0.04000(6) 0.4165(2) -0.04404(11) 1.000 0.0232(6) . . C26 C Uani 0.00854(6) 0.3271(2) -0.04366(11) 1.000 0.0219(6) . . C27 C Uani 0.01567(6) 0.2235(2) 0.01404(11) 1.000 0.0216(6) . . C28 C Uani 0.05325(6) 0.2093(2) 0.07177(11) 1.000 0.0193(6) . . C29 C Uani 0.11220(7) 0.4990(3) 0.00845(14) 1.000 0.0293(7) . . C30 C Uani -0.03263(6) 0.3442(3) -0.10460(12) 1.000 0.0300(7) . . C31 C Uani 0.05972(6) 0.1022(3) 0.13555(11) 1.000 0.0246(6) . . H51 H Uiso 0.16690 0.22050 -0.13530 1.000 0.0340 calc R H61 H Uiso 0.21230 0.38660 -0.03340 1.000 0.0310 calc R H71 H Uiso 0.21020 0.34820 0.13020 1.000 0.0270 calc R H72 H Uiso 0.24500 0.36580 0.10260 1.000 0.0270 calc R H81 H Uiso 0.27120 0.20010 0.20000 1.000 0.0280 calc R H82 H Uiso 0.25910 0.08740 0.13040 1.000 0.0280 calc R H91 H Uiso 0.24020 -0.04020 0.21050 1.000 0.0230 calc R H101 H Uiso 0.21290 0.06660 0.28120 1.000 0.0270 calc R H102 H Uiso 0.23920 0.21110 0.27480 1.000 0.0270 calc R H121 H Uiso 0.18630 0.43790 0.27530 1.000 0.0280 calc R H131 H Uiso 0.11940 0.50980 0.18210 1.000 0.0280 calc R H161 H Uiso 0.14430 -0.39470 -0.14370 1.000 0.0380 calc R H181 H Uiso 0.04420 -0.14340 -0.19200 1.000 0.0390 calc R H201 H Uiso 0.20790 -0.29430 -0.06580 1.000 0.0520 calc R H202 H Uiso 0.21120 -0.13400 -0.02190 1.000 0.0520 calc R H203 H Uiso 0.20920 -0.12950 -0.10320 1.000 0.0520 calc R H211 H Uiso 0.08310 -0.50400 -0.22580 1.000 0.0740 calc R H212 H Uiso 0.04490 -0.39260 -0.26160 1.000 0.0740 calc R H213 H Uiso 0.05370 -0.48140 -0.18610 1.000 0.0740 calc R H221 H Uiso 0.08210 0.21250 -0.14540 1.000 0.0570 calc R H222 H Uiso 0.08010 0.14910 -0.07180 1.000 0.0570 calc R H223 H Uiso 0.04450 0.11230 -0.14970 1.000 0.0570 calc R H251 H Uiso 0.03520 0.48820 -0.08310 1.000 0.0280 calc R H271 H Uiso -0.00560 0.16070 0.01420 1.000 0.0260 calc R H291 H Uiso 0.12420 0.56290 0.05300 1.000 0.0440 calc R H292 H Uiso 0.10220 0.56790 -0.03460 1.000 0.0440 calc R H293 H Uiso 0.13230 0.42800 0.00530 1.000 0.0440 calc R H301 H Uiso -0.03920 0.45600 -0.11370 1.000 0.0450 calc R H302 H Uiso -0.05210 0.29270 -0.09030 1.000 0.0450 calc R H303 H Uiso -0.03320 0.29520 -0.14930 1.000 0.0450 calc R H311 H Uiso 0.07570 0.01170 0.13390 1.000 0.0370 calc R H312 H Uiso 0.03390 0.06570 0.13270 1.000 0.0370 calc R H313 H Uiso 0.07370 0.15950 0.18150 1.000 0.0370 calc R loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.0139(1) 0.0134(1) 0.0161(1) -0.0001(1) 0.0048(1) -0.0006(1) O1 0.0178(7) 0.0362(9) 0.0278(8) -0.0055(7) 0.0060(6) -0.0059(6) O2 0.0291(8) 0.0208(8) 0.0385(9) -0.0016(7) 0.0144(7) 0.0039(7) O3 0.0373(9) 0.0278(8) 0.0254(8) 0.0048(6) 0.0142(7) -0.0034(7) N1 0.0242(9) 0.0223(9) 0.0201(8) 0.0018(7) 0.0099(7) -0.0002(7) N2 0.0201(8) 0.0176(9) 0.0242(9) 0.0024(7) 0.0101(7) 0.0003(7) N3 0.0185(8) 0.0186(9) 0.0180(8) -0.0024(6) 0.0055(7) -0.0013(7) N4 0.0167(8) 0.0159(8) 0.0208(8) -0.0023(6) 0.0068(7) -0.0010(6) C1 0.0219(10) 0.0193(10) 0.0187(9) 0.0004(8) 0.0098(8) 0.0021(8) C2 0.0168(9) 0.0177(10) 0.0215(10) 0.0004(8) 0.0063(8) -0.0026(8) C3 0.0182(9) 0.0177(10) 0.0200(10) -0.0026(8) 0.0039(8) 0.0000(8) C4 0.0174(9) 0.0168(10) 0.0210(10) -0.0002(8) 0.0076(8) 0.0030(8) C5 0.0332(12) 0.0288(12) 0.0242(11) 0.0067(9) 0.0142(9) 0.0005(9) C6 0.0277(11) 0.0239(11) 0.0305(11) 0.0074(9) 0.0153(9) -0.0001(9) C7 0.0198(10) 0.0198(10) 0.0259(11) -0.0003(8) 0.0077(8) -0.0058(8) C8 0.0159(9) 0.0235(11) 0.0269(11) 0.0004(9) 0.0047(8) -0.0022(8) C9 0.0149(9) 0.0152(10) 0.0221(10) 0.0015(7) 0.0021(8) 0.0012(7) C10 0.0178(10) 0.0218(11) 0.0204(10) 0.0010(8) 0.0005(8) -0.0007(8) C11 0.0152(9) 0.0160(10) 0.0197(9) 0.0007(7) 0.0071(7) -0.0024(7) C12 0.0231(10) 0.0216(11) 0.0256(10) -0.0083(8) 0.0108(8) -0.0052(8) C13 0.0228(10) 0.0187(10) 0.0298(11) -0.0081(9) 0.0119(9) -0.0024(8) C14 0.0307(11) 0.0240(11) 0.0157(10) -0.0011(8) 0.0101(9) -0.0031(8) C15 0.0346(12) 0.0278(12) 0.0206(10) 0.0022(9) 0.0154(9) 0.0026(9) C16 0.0526(15) 0.0240(12) 0.0270(11) -0.0016(9) 0.0246(11) 0.0005(10) C17 0.0490(14) 0.0341(13) 0.0200(11) -0.0047(9) 0.0172(10) -0.0121(11) C18 0.0317(12) 0.0427(14) 0.0195(11) -0.0026(10) 0.0075(9) -0.0058(10) C19 0.0298(12) 0.0315(12) 0.0178(10) -0.0008(9) 0.0081(9) 0.0011(9) C20 0.0381(13) 0.0358(13) 0.0372(13) 0.0022(10) 0.0228(11) 0.0080(10) C21 0.0689(19) 0.0447(16) 0.0378(14) -0.0160(12) 0.0263(14) -0.0244(15) C22 0.0317(12) 0.0367(14) 0.0365(13) -0.0005(11) 0.0055(10) 0.0069(10) C23 0.0152(9) 0.0165(10) 0.0202(9) -0.0026(8) 0.0060(8) 0.0022(7) C24 0.0215(10) 0.0154(10) 0.0266(10) -0.0007(8) 0.0119(8) 0.0010(8) C25 0.0265(11) 0.0194(10) 0.0241(10) 0.0036(8) 0.0109(9) 0.0050(9) C26 0.0194(10) 0.0205(11) 0.0242(10) -0.0022(8) 0.0073(8) 0.0042(8) C27 0.0179(10) 0.0198(10) 0.0279(11) -0.0015(8) 0.0103(8) -0.0008(8) C28 0.0197(9) 0.0174(10) 0.0217(10) -0.0016(8) 0.0096(8) 0.0016(8) C29 0.0277(12) 0.0241(11) 0.0381(13) 0.0057(10) 0.0155(10) -0.0022(9) C30 0.0224(11) 0.0329(13) 0.0285(11) 0.0022(9) 0.0042(9) 0.0048(9) C31 0.0235(10) 0.0256(11) 0.0260(11) 0.0032(9) 0.0114(9) -0.0012(9) #================================================================== # 10. MOLECULAR GEOMETRY #=================================================================== _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C1 1.941(2) . . yes Re1 C2 1.9399(19) . . yes Re1 C3 1.927(2) . . yes Re1 C4 2.191(2) . . yes Re1 C9 2.272(2) . . yes Re1 C11 2.1639(18) . . yes O1 C1 1.160(3) . . yes O2 C2 1.157(2) . . yes O3 C3 1.166(3) . . yes N1 C4 1.375(2) . . yes N1 C5 1.392(3) . . yes N1 C14 1.446(3) . . yes N2 C4 1.360(3) . . yes N2 C6 1.382(3) . . yes N2 C7 1.468(3) . . yes N3 C10 1.472(3) . . yes N3 C11 1.356(3) . . yes N3 C12 1.379(2) . . yes N4 C11 1.359(3) . . yes N4 C13 1.393(3) . . yes N4 C23 1.447(3) . . yes C5 C6 1.344(3) . . no C7 C8 1.527(3) . . no C8 C9 1.529(3) . . no C9 C10 1.528(3) . . no C12 C13 1.341(3) . . no C14 C15 1.395(3) . . no C14 C19 1.394(4) . . no C15 C16 1.390(4) . . no C15 C20 1.512(4) . . no C16 C17 1.389(4) . . no C17 C18 1.384(4) . . no C17 C21 1.510(4) . . no C18 C19 1.388(4) . . no C19 C22 1.506(4) . . no C23 C24 1.394(3) . . no C23 C28 1.398(3) . . no C24 C25 1.390(3) . . no C24 C29 1.510(4) . . no C25 C26 1.390(3) . . no C26 C27 1.390(3) . . no C26 C30 1.512(3) . . no C27 C28 1.396(3) . . no C28 C31 1.506(3) . . no C5 H51 0.9500 . . no C6 H61 0.9500 . . no C7 H71 0.9900 . . no C7 H72 0.9900 . . no C8 H81 0.9900 . . no C8 H82 0.9900 . . no C9 H91 1.0000 . . no C10 H101 0.9900 . . no C10 H102 0.9900 . . no C12 H121 0.9500 . . no C13 H131 0.9500 . . no C16 H161 0.9500 . . no C18 H181 0.9500 . . no C20 H201 0.9800 . . no C20 H202 0.9800 . . no C20 H203 0.9800 . . no C21 H211 0.9800 . . no C21 H212 0.9800 . . no C21 H213 0.9800 . . no C22 H221 0.9800 . . no C22 H222 0.9800 . . no C22 H223 0.9800 . . no C25 H251 0.9500 . . no C27 H271 0.9500 . . no C29 H291 0.9800 . . no C29 H292 0.9800 . . no C29 H293 0.9800 . . no C30 H301 0.9800 . . no C30 H302 0.9800 . . no C30 H303 0.9800 . . no C31 H311 0.9800 . . no C31 H312 0.9800 . . no C31 H313 0.9800 . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Re1 C2 94.50(9) . . . yes C1 Re1 C3 88.39(9) . . . yes C1 Re1 C4 93.76(8) . . . yes C1 Re1 C9 173.57(8) . . . yes C1 Re1 C11 98.40(8) . . . yes C2 Re1 C3 89.78(8) . . . yes C2 Re1 C4 93.24(8) . . . yes C2 Re1 C9 91.82(8) . . . yes C2 Re1 C11 166.78(8) . . . yes C3 Re1 C4 176.14(7) . . . yes C3 Re1 C9 90.47(8) . . . yes C3 Re1 C11 87.74(7) . . . yes C4 Re1 C9 87.04(7) . . . yes C4 Re1 C11 88.77(7) . . . yes C9 Re1 C11 75.23(7) . . . yes C4 N1 C5 111.55(17) . . . yes C4 N1 C14 125.80(17) . . . yes C5 N1 C14 122.17(17) . . . yes C4 N2 C6 112.18(17) . . . yes C4 N2 C7 124.93(16) . . . yes C6 N2 C7 122.61(18) . . . yes C10 N3 C11 118.98(16) . . . yes C10 N3 C12 129.01(17) . . . yes C11 N3 C12 112.00(17) . . . yes C11 N4 C13 111.01(17) . . . yes C11 N4 C23 127.35(16) . . . yes C13 N4 C23 121.63(17) . . . yes Re1 C1 O1 174.70(17) . . . yes Re1 C2 O2 175.27(18) . . . yes Re1 C3 O3 178.3(2) . . . yes Re1 C4 N1 130.48(14) . . . yes Re1 C4 N2 126.56(13) . . . yes N1 C4 N2 102.94(16) . . . yes N1 C5 C6 106.37(19) . . . yes N2 C6 C5 107.0(2) . . . yes N2 C7 C8 111.39(15) . . . yes C7 C8 C9 115.52(19) . . . no Re1 C9 C8 116.99(13) . . . yes Re1 C9 C10 106.57(15) . . . yes C8 C9 C10 110.62(15) . . . no N3 C10 C9 108.26(16) . . . yes Re1 C11 N3 115.62(13) . . . yes Re1 C11 N4 140.67(14) . . . yes N3 C11 N4 103.69(15) . . . yes N3 C12 C13 106.48(18) . . . yes N4 C13 C12 106.8(2) . . . yes N1 C14 C15 118.3(2) . . . yes N1 C14 C19 119.43(19) . . . yes C15 C14 C19 122.2(2) . . . no C14 C15 C16 117.8(2) . . . no C14 C15 C20 121.8(2) . . . no C16 C15 C20 120.4(2) . . . no C15 C16 C17 121.8(2) . . . no C16 C17 C18 118.2(2) . . . no C16 C17 C21 120.5(2) . . . no C18 C17 C21 121.2(2) . . . no C17 C18 C19 122.5(2) . . . no C14 C19 C18 117.4(2) . . . no C14 C19 C22 121.7(2) . . . no C18 C19 C22 120.9(2) . . . no N4 C23 C24 118.30(18) . . . yes N4 C23 C28 118.78(16) . . . yes C24 C23 C28 122.65(19) . . . no C23 C24 C25 117.56(19) . . . no C23 C24 C29 121.4(2) . . . no C25 C24 C29 121.05(18) . . . no C24 C25 C26 121.94(18) . . . no C25 C26 C27 118.7(2) . . . no C25 C26 C30 120.33(18) . . . no C27 C26 C30 121.0(2) . . . no C26 C27 C28 121.7(2) . . . no C23 C28 C27 117.39(17) . . . no C23 C28 C31 121.92(19) . . . no C27 C28 C31 120.7(2) . . . no N1 C5 H51 127.00 . . . no C6 C5 H51 127.00 . . . no N2 C6 H61 127.00 . . . no C5 C6 H61 126.00 . . . no N2 C7 H71 109.00 . . . no N2 C7 H72 109.00 . . . no C8 C7 H71 109.00 . . . no C8 C7 H72 109.00 . . . no H71 C7 H72 108.00 . . . no C7 C8 H81 108.00 . . . no C7 C8 H82 108.00 . . . no C9 C8 H81 108.00 . . . no C9 C8 H82 108.00 . . . no H81 C8 H82 107.00 . . . no Re1 C9 H91 107.00 . . . no C8 C9 H91 107.00 . . . no C10 C9 H91 107.00 . . . no N3 C10 H101 110.00 . . . no N3 C10 H102 110.00 . . . no C9 C10 H101 110.00 . . . no C9 C10 H102 110.00 . . . no H101 C10 H102 108.00 . . . no N3 C12 H121 127.00 . . . no C13 C12 H121 127.00 . . . no N4 C13 H131 127.00 . . . no C12 C13 H131 127.00 . . . no C15 C16 H161 119.00 . . . no C17 C16 H161 119.00 . . . no C17 C18 H181 119.00 . . . no C19 C18 H181 119.00 . . . no C15 C20 H201 109.00 . . . no C15 C20 H202 110.00 . . . no C15 C20 H203 110.00 . . . no H201 C20 H202 109.00 . . . no H201 C20 H203 109.00 . . . no H202 C20 H203 109.00 . . . no C17 C21 H211 109.00 . . . no C17 C21 H212 109.00 . . . no C17 C21 H213 109.00 . . . no H211 C21 H212 110.00 . . . no H211 C21 H213 109.00 . . . no H212 C21 H213 109.00 . . . no C19 C22 H221 110.00 . . . no C19 C22 H222 109.00 . . . no C19 C22 H223 109.00 . . . no H221 C22 H222 109.00 . . . no H221 C22 H223 109.00 . . . no H222 C22 H223 110.00 . . . no C24 C25 H251 119.00 . . . no C26 C25 H251 119.00 . . . no C26 C27 H271 119.00 . . . no C28 C27 H271 119.00 . . . no C24 C29 H291 110.00 . . . no C24 C29 H292 110.00 . . . no C24 C29 H293 109.00 . . . no H291 C29 H292 109.00 . . . no H291 C29 H293 109.00 . . . no H292 C29 H293 109.00 . . . no C26 C30 H301 109.00 . . . no C26 C30 H302 109.00 . . . no C26 C30 H303 109.00 . . . no H301 C30 H302 110.00 . . . no H301 C30 H303 109.00 . . . no H302 C30 H303 110.00 . . . no C28 C31 H311 110.00 . . . no C28 C31 H312 109.00 . . . no C28 C31 H313 109.00 . . . no H311 C31 H312 109.00 . . . no H311 C31 H313 109.00 . . . no H312 C31 H313 110.00 . . . no _iucr_refine_instructions_details ; ; # End of Crystallographic Information File _database_code_depnum_ccdc_archive 'CCDC 959156'