# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Paul Beer' _publ_contact_author_address ; University of Oxford Department of Chemistry Inorganic Chemistry Laboratory Oxford OX1 3QR UNITED KINGDOM ; _publ_contact_author_email PAUL.BEER@CHEM.OX.AC.UK _publ_section_title ; Halide anion directed assembly of luminescent pseudorotaxanes ; loop_ _publ_author_name 'Paul Beer' 'Andrew Cowley' 'David Curiel' 'Rowena L. Paul' data_Compund_6+7a_dichloromethane_solvate _database_code_depnum_ccdc_archive 'CCDC 231488' #============================================================= # Diffractometer details #============================================================= _diffrn_measurement_device_type ; Nonius KappaCCD ; _diffrn_radiation_monochromator graphite _computing_data_collection ; KappaCCD software 'Collect' (Nonius, 2000) ; _computing_data_reduction ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; KappaCCD software 'DENZO' (Otwinowski & Minor, 1996) ; #============================================================= # General computing #============================================================= _computing_structure_refinement ; CRYSTALS (Watkin et al, 2001) ; _computing_publication_material ; CRYSTALS (Watkin et al, 2001) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' _chemical_name_systematic # IUPAC name, in full ; ? ; _chemical_melting_point ? _refine_ls_matrix_type full _atom_sites_solution_primary direct _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_special_details ; The Cl ligand and the trans carbonyl are disordered. The coordinates, site occupancies and anistropic thermal parameters have been refined for the predominant positions (Cl1, C1, O1) and coordinates, site occupancies and isotropic thermal parameters for the minor positions (Cl91, C91, O91). The refined thermal parameters of the polyether and hexyl fragments of the title compound are highly large and anisotropic, but attempts to include this in the model did not lead to any improvement in agreement with the X-ray data. A number of geometric restraints were applied. The Re-Cl, Re-C and C-O distances of the two positions of the disordered ligand were restrained to their common mean (su 0.01 \%A), the Cl-Re-C and Re-C-O angles were restrained to their common mean (su 1 \%), the N-C bond lengths of the hexyl groups to 1.50(1) \%A, the C-C bonds to 1.52(1) \%A and the N-C-C and C-C-C angles to 112(1) \%. Similarity restraints were applied to the thermal parameters of directly-bonded pairs of atoms within the disordered groups ; #============================================================= _cell_length_a 13.6751(2) _cell_angle_alpha 90 _cell_length_b 22.3512(2) _cell_angle_beta 105.9996(5) _cell_length_c 22.6383(3) _cell_angle_gamma 90 _cell_volume 6651.47(14) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 # choose from: rm (reference molecule of # known chirality), ad (anomolous # dispersion - ie. Flack param), rmad # (both rm and ad), syn (known from # synthetic pathway), unk (unknown) # or . (not applicable). _chemical_absolute_configuration . loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B 'Re ' -1.5980 7.2320 28.7621 1.6719 15.7189 9.0923 14.5564 0.3505 5.4417 52.0861 10.4720 International_Tables_Vol_IV_Table_2.2B _cell_formula_units_Z 4 _chemical_formula_sum ' C59.23 H74.45 Cl2.45 N7 O14 Re1 ' _chemical_formula_moiety ' C59.23 H74.45 Cl2.45 N7 O14 Re1 ' _chemical_compound_source ; ? ; _chemical_formula_weight 1381.51 _cell_measurement_reflns_used 15355 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description ' block ' _exptl_crystal_colour ' orange ' _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.20 _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2829.843 _exptl_absorpt_coefficient_mu 1.989 _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Denzo/Scalepack (Otwinowski & Minor, 1996) ; _exptl_absorpt_correction_T_min 0.67 _exptl_absorpt_correction_T_max 0.82 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 29701 _reflns_number_total 15081 _diffrn_reflns_av_R_equivalents 0.02 _diffrn_reflns_theta_min 5.101 _diffrn_reflns_theta_max 27.482 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.932 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _reflns_limit_h_min -17 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 28 _reflns_limit_l_min 0 _reflns_limit_l_max 29 _refine_diff_density_min -0.89 _refine_diff_density_max 1.58 _refine_ls_number_reflns 8504 _refine_ls_number_restraints 118 _refine_ls_number_parameters 781 #_refine_ls_R_factor_ref 0.0541 _refine_ls_wR_factor_ref 0.0604 _refine_ls_goodness_of_fit_ref 1.0886 #_reflns_number_all 15081 _refine_ls_R_factor_all 0.1000 _refine_ls_wR_factor_all 0.0809 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 8504 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_gt 0.0604 _refine_ls_shift/su_max 0.049040 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.70 1.29 1.28 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 # Replace trailing . with the number of unfound # hydrogen atoms attaced to relavent atom loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_disorder_assembly _atom_site_refinement_disorder_group _atom_site_attached_hydrogens Re1 Re 0.17009(2) 0.660747(10) 0.310025(11) 0.0643 1.0000 Uani D U . . . . Cl1 Cl 0.3237(2) 0.71933(10) 0.36169(13) 0.0798 0.745(11) Uani D . P . 1 1 C1 C 0.0558(6) 0.6137(4) 0.2704(4) 0.0815 0.745(11) Uani D U P 1 1 . O1 O -0.0138(8) 0.5854(4) 0.2499(5) 0.1257 0.745(11) Uani D U P 1 1 . Cl91 Cl 0.0394(9) 0.5824(5) 0.2626(6) 0.106(4) 0.255(11) Uiso D . P 1 2 . C91 C 0.2720(17) 0.7141(11) 0.3512(8) 0.085(11) 0.255(11) Uiso D . P 1 2 . O91 O 0.3310(18) 0.7456(12) 0.3791(10) 0.103(8) 0.255(11) Uiso D . P 1 2 . C2 C 0.0865(6) 0.6990(3) 0.3541(4) 0.0864 1.0000 Uani . . . . . . O2 O 0.0385(6) 0.7220(3) 0.3815(3) 0.1305 1.0000 Uani . . . . . . C3 C 0.1257(6) 0.7193(3) 0.2471(4) 0.0853 1.0000 Uani . . . . . . O3 O 0.1021(6) 0.7539(3) 0.2070(3) 0.1211 1.0000 Uani . . . . . . N1 N 0.2687(4) 0.60976(18) 0.2680(2) 0.0555 1.0000 Uani . . . . . . C4 C 0.2821(5) 0.6206(2) 0.2125(2) 0.0580 1.0000 Uani . . . . . . C5 C 0.3409(4) 0.5845(2) 0.1860(2) 0.0559 1.0000 Uani . . . . . . C6 C 0.3863(4) 0.5343(2) 0.2176(2) 0.0524 1.0000 Uani . . . . . . C7 C 0.3745(4) 0.5234(2) 0.2753(2) 0.0525 1.0000 Uani . . . . . . C8 C 0.3163(4) 0.5615(2) 0.2996(2) 0.0519 1.0000 Uani . . . . . . C9 C 0.3026(5) 0.5538(2) 0.3611(2) 0.0561 1.0000 Uani . . . . . . C10 C 0.3528(5) 0.5098(2) 0.4015(3) 0.0675 1.0000 Uani . . . . . . C11 C 0.3405(6) 0.5068(3) 0.4595(3) 0.0734 1.0000 Uani . . . . . . C12 C 0.2792(7) 0.5477(3) 0.4767(3) 0.0831 1.0000 Uani . . . . . . C13 C 0.2282(6) 0.5893(3) 0.4348(3) 0.0752 1.0000 Uani . . . . . . N2 N 0.2384(4) 0.5934(2) 0.3769(2) 0.0642 1.0000 Uani . . . . . . C14 C 0.4503(4) 0.4955(2) 0.1877(2) 0.0563 1.0000 Uani . . . . . . O4 O 0.4754(4) 0.51439(18) 0.14311(19) 0.0706 1.0000 Uani . . . . . . N3 N 0.4773(4) 0.4415(2) 0.2112(3) 0.0605 1.0000 Uani . . . . . . C15 C 0.5410(6) 0.4022(3) 0.1862(3) 0.0737 1.0000 Uani . . . . . . C16 C 0.5275(5) 0.3375(2) 0.2036(3) 0.0682 1.0000 Uani . . . . . . O5 O 0.4233(4) 0.32274(18) 0.1771(2) 0.0717 1.0000 Uani . . . . . . C17 C 0.3954(5) 0.2640(3) 0.1802(3) 0.0659 1.0000 Uani . . . . . . C18 C 0.2934(5) 0.2515(3) 0.1536(3) 0.0721 1.0000 Uani . . . . . . C19 C 0.2579(5) 0.1937(3) 0.1522(3) 0.0730 1.0000 Uani . . . . . . C20 C 0.3242(5) 0.1470(3) 0.1781(3) 0.0657 1.0000 Uani . . . . . . C21 C 0.4251(5) 0.1601(3) 0.2050(3) 0.0659 1.0000 Uani . . . . . . C22 C 0.4615(5) 0.2183(2) 0.2065(3) 0.0612 1.0000 Uani . . . . . . O6 O 0.2822(4) 0.09096(19) 0.1737(2) 0.0730 1.0000 Uani . . . . . . C23 C 0.3508(5) 0.0418(3) 0.1857(3) 0.0682 1.0000 Uani . . . . . . C24 C 0.2947(6) -0.0151(3) 0.1668(3) 0.0726 1.0000 Uani . . . . . . O7 O 0.2366(4) -0.0284(2) 0.2084(2) 0.0797 1.0000 Uani . . . . . . C25 C 0.1849(7) -0.0835(3) 0.1968(4) 0.0919 1.0000 Uani . . . . . . C26 C 0.1348(7) -0.0948(4) 0.2476(6) 0.1136 1.0000 Uani . . . . . . O8 O 0.2126(5) -0.1046(2) 0.3026(3) 0.1005 1.0000 Uani . . . . . . C27 C 0.1765(11) -0.1214(4) 0.3536(8) 0.1383 1.0000 Uani . . . . . . C28 C 0.2582(16) -0.1230(5) 0.4104(7) 0.1535 1.0000 Uani . . . . . . O9 O 0.2855(8) -0.0638(3) 0.4250(4) 0.1484 1.0000 Uani . . . . . . C29 C 0.303(3) -0.0538(6) 0.4846(7) 0.3050 1.0000 Uani . . . . . . C30 C 0.360(3) 0.0082(7) 0.4976(8) 0.3673 1.0000 Uani . . . . . . O10 O 0.2770(14) 0.0492(3) 0.4779(4) 0.2299 1.0000 Uani . . . . . . C31 C 0.3084(17) 0.1103(5) 0.4851(5) 0.1608 1.0000 Uani . . . . . . C32 C 0.4094(19) 0.1314(7) 0.5149(5) 0.2044 1.0000 Uani . . . . . . C33 C 0.4287(12) 0.1934(6) 0.5171(4) 0.1398 1.0000 Uani . . . . . . C34 C 0.3493(9) 0.2286(4) 0.4894(4) 0.1014 1.0000 Uani . . . . . . C35 C 0.2521(10) 0.2093(4) 0.4590(6) 0.1222 1.0000 Uani . . . . . . C36 C 0.2335(12) 0.1488(4) 0.4566(7) 0.1347 1.0000 Uani . . . . . . O11 O 0.3657(7) 0.2891(3) 0.4857(3) 0.1355 1.0000 Uani . . . . . . C37 C 0.4153(9) 0.3204(4) 0.5418(4) 0.1041 1.0000 Uani . . . . . . C38 C 0.4836(7) 0.3649(3) 0.5274(3) 0.0863 1.0000 Uani . . . . . . N4 N 0.4333(5) 0.4127(2) 0.4858(3) 0.0767 1.0000 Uani . . . . . . C39 C 0.3947(7) 0.4606(3) 0.5066(3) 0.0835 1.0000 Uani . . . . . . O12 O 0.4029(6) 0.4690(2) 0.5616(2) 0.1125 1.0000 Uani . . . . . . N5 N 0.3035(6) 0.1168(3) 0.3297(3) 0.0787 1.0000 Uani . . . . . . C40 C 0.2379(8) 0.1591(4) 0.3016(4) 0.0939 1.0000 Uani . . . . . . C41 C 0.2637(6) 0.2187(3) 0.3032(3) 0.0779 1.0000 Uani . . . . . . C42 C 0.3624(5) 0.2345(3) 0.3346(3) 0.0651 1.0000 Uani . . . . . . C43 C 0.4312(5) 0.1906(2) 0.3634(2) 0.0614 1.0000 Uani . . . . . . C44 C 0.3976(6) 0.1319(3) 0.3596(3) 0.0733 1.0000 Uani . . . . . . C45 C 0.2716(9) 0.0534(3) 0.3292(4) 0.1080 1.0000 Uani . . . . . . C46 C 0.1826(7) 0.2629(5) 0.2713(4) 0.1014 1.0000 Uani . . . . . . O13 O 0.0971(5) 0.2451(5) 0.2486(4) 0.1516 1.0000 Uani . . . . . . N6 N 0.2126(8) 0.3183(5) 0.2696(7) 0.1514 1.0000 Uani D U . . . . C47 C 0.1424(9) 0.3686(6) 0.2414(8) 0.1793 1.0000 Uani D U . . . . C48 C 0.1824(10) 0.4055(6) 0.1963(8) 0.1826 1.0000 Uani D U . . . . C49 C 0.1132(12) 0.4575(7) 0.1691(8) 0.2084 1.0000 Uani D U . . . . C50 C 0.1264(14) 0.4779(8) 0.1077(8) 0.2325 1.0000 Uani D U . . . . C51 C 0.0717(16) 0.5365(8) 0.0850(10) 0.2494 1.0000 Uani D U . . . . C52 C -0.0268(17) 0.5420(11) 0.1023(12) 0.2632 1.0000 Uani D U . . . . C53 C 0.5383(5) 0.2025(2) 0.3992(3) 0.0653 1.0000 Uani . . . . . . O14 O 0.5972(4) 0.16059(19) 0.4195(2) 0.0789 1.0000 Uani . . . . . . N7 N 0.5661(4) 0.2597(2) 0.4065(3) 0.0790 1.0000 Uani D U . . . . C54 C 0.6709(5) 0.2771(3) 0.4399(3) 0.0905 1.0000 Uani D U . . . . C55 C 0.7401(6) 0.2774(4) 0.3972(4) 0.1129 1.0000 Uani D U . . . . C56 C 0.8489(7) 0.2892(5) 0.4321(5) 0.1354 1.0000 Uani D U . . . . C57 C 0.8901(9) 0.2328(6) 0.4681(7) 0.1696 1.0000 Uani D U . . . . C58 C 1.0038(9) 0.2284(7) 0.4875(7) 0.1743 1.0000 Uani D U . . . . C59 C 1.0366(12) 0.1755(7) 0.5296(7) 0.1783 1.0000 Uani D U . . . . Cl2 Cl 0.4466 0.3810 0.3436 0.0715 1.0000 Uani . . . . . . C60 C 0.830(3) 0.615(2) 0.617(2) 0.109(12) 0.225(7) Uiso . . P . . . Cl3 Cl 0.9067(8) 0.6716(4) 0.6286(5) 0.098(4) 0.225(7) Uiso . . P . . . Cl4 Cl 0.8800(8) 0.5470(5) 0.6490(5) 0.107(4) 0.225(7) Uiso . . P . . . H1 H 0.460(3) 0.430(2) 0.232(2) 0.018(12) 1.0000 Uiso . . . . . . H2 H 0.431(4) 0.416(3) 0.450(3) 0.050(15) 1.0000 Uiso . . . . . . H3 H 0.257(5) 0.328(3) 0.282(3) 0.045(17) 1.0000 Uiso . . . . . . H4 H 0.521(4) 0.289(3) 0.387(2) 0.049(14) 1.0000 Uiso . . . . . . H41 H 0.2481 0.6564 0.1891 0.0703 1.0000 Uiso . . . . . . H51 H 0.3501 0.5945 0.1448 0.0670 1.0000 Uiso . . . . . . H71 H 0.4082 0.4879 0.2994 0.0631 1.0000 Uiso . . . . . . H101 H 0.3978 0.4804 0.3883 0.0816 1.0000 Uiso . . . . . . H121 H 0.2716 0.5474 0.5194 0.1042 1.0000 Uiso . . . . . . H131 H 0.1815 0.6179 0.4475 0.0931 1.0000 Uiso . . . . . . H151 H 0.6139 0.4141 0.2031 0.0951 1.0000 Uiso . . . . . . H152 H 0.5211 0.4060 0.1404 0.0951 1.0000 Uiso . . . . . . H161 H 0.5452 0.3334 0.2494 0.0843 1.0000 Uiso . . . . . . H162 H 0.5720 0.3106 0.1871 0.0843 1.0000 Uiso . . . . . . H181 H 0.2454 0.2846 0.1353 0.0850 1.0000 Uiso . . . . . . H191 H 0.1844 0.1851 0.1325 0.0853 1.0000 Uiso . . . . . . H211 H 0.4731 0.1272 0.2237 0.0782 1.0000 Uiso . . . . . . H221 H 0.5349 0.2271 0.2263 0.0728 1.0000 Uiso . . . . . . H231 H 0.3863 0.0402 0.2306 0.0827 1.0000 Uiso . . . . . . H232 H 0.4022 0.0471 0.1621 0.0827 1.0000 Uiso . . . . . . H241 H 0.3442 -0.0482 0.1674 0.0879 1.0000 Uiso . . . . . . H242 H 0.2483 -0.0108 0.1243 0.0879 1.0000 Uiso . . . . . . H251 H 0.2343 -0.1164 0.1962 0.1109 1.0000 Uiso . . . . . . H252 H 0.1320 -0.0820 0.1563 0.1109 1.0000 Uiso . . . . . . H261 H 0.0900 -0.1308 0.2376 0.1375 1.0000 Uiso . . . . . . H262 H 0.0933 -0.0592 0.2524 0.1375 1.0000 Uiso . . . . . . H271 H 0.1448 -0.1619 0.3458 0.1845 1.0000 Uiso . . . . . . H272 H 0.1243 -0.0917 0.3581 0.1845 1.0000 Uiso . . . . . . H281 H 0.2342 -0.1420 0.4439 0.1982 1.0000 Uiso . . . . . . H282 H 0.3175 -0.1460 0.4044 0.1982 1.0000 Uiso . . . . . . H291 H 0.3461 -0.0863 0.5088 0.3484 1.0000 Uiso . . . . . . H292 H 0.2370 -0.0518 0.4958 0.3484 1.0000 Uiso . . . . . . H301 H 0.3955 0.0133 0.5423 0.3774 1.0000 Uiso . . . . . . H302 H 0.4101 0.0128 0.4731 0.3774 1.0000 Uiso . . . . . . H321 H 0.4650 0.1025 0.5339 0.2229 1.0000 Uiso . . . . . . H331 H 0.4973 0.2102 0.5379 0.1590 1.0000 Uiso . . . . . . H351 H 0.1973 0.2384 0.4394 0.1578 1.0000 Uiso . . . . . . H361 H 0.1649 0.1332 0.4340 0.1824 1.0000 Uiso . . . . . . H371 H 0.3634 0.3406 0.5584 0.1236 1.0000 Uiso . . . . . . H372 H 0.4552 0.2914 0.5729 0.1236 1.0000 Uiso . . . . . . H381 H 0.5233 0.3837 0.5668 0.0997 1.0000 Uiso . . . . . . H382 H 0.5313 0.3438 0.5079 0.0997 1.0000 Uiso . . . . . . H401 H 0.1674 0.1470 0.2784 0.1162 1.0000 Uiso . . . . . . H421 H 0.3841 0.2774 0.3366 0.0803 1.0000 Uiso . . . . . . H441 H 0.4461 0.0998 0.3801 0.0918 1.0000 Uiso . . . . . . H451 H 0.1988 0.0495 0.3048 0.1406 1.0000 Uiso . . . . . . H452 H 0.2793 0.0397 0.3723 0.1406 1.0000 Uiso . . . . . . H453 H 0.3151 0.0281 0.3101 0.1406 1.0000 Uiso . . . . . . H471 H 0.1341 0.3955 0.2750 0.2112 1.0000 Uiso . . . . . . H472 H 0.0748 0.3515 0.2191 0.2112 1.0000 Uiso . . . . . . H481 H 0.2509 0.4216 0.2184 0.2129 1.0000 Uiso . . . . . . H482 H 0.1887 0.3788 0.1621 0.2129 1.0000 Uiso . . . . . . H491 H 0.1291 0.4919 0.1986 0.2371 1.0000 Uiso . . . . . . H492 H 0.0410 0.4449 0.1631 0.2371 1.0000 Uiso . . . . . . H501 H 0.2006 0.4834 0.1122 0.2638 1.0000 Uiso . . . . . . H502 H 0.0988 0.4461 0.0765 0.2638 1.0000 Uiso . . . . . . H511 H 0.1171 0.5706 0.1037 0.2804 1.0000 Uiso . . . . . . H512 H 0.0567 0.5382 0.0393 0.2804 1.0000 Uiso . . . . . . H521 H -0.0603 0.5809 0.0867 0.2990 1.0000 Uiso . . . . . . H522 H -0.0126 0.5406 0.1481 0.2990 1.0000 Uiso . . . . . . H523 H -0.0729 0.5082 0.0837 0.2990 1.0000 Uiso . . . . . . H541 H 0.6698 0.3181 0.4575 0.1069 1.0000 Uiso . . . . . . H542 H 0.6981 0.2479 0.4740 0.1069 1.0000 Uiso . . . . . . H551 H 0.7168 0.3094 0.3656 0.1368 1.0000 Uiso . . . . . . H552 H 0.7357 0.2377 0.3764 0.1368 1.0000 Uiso . . . . . . H561 H 0.8525 0.3235 0.4609 0.1660 1.0000 Uiso . . . . . . H562 H 0.8896 0.2987 0.4027 0.1660 1.0000 Uiso . . . . . . H571 H 0.8656 0.2319 0.5059 0.2028 1.0000 Uiso . . . . . . H572 H 0.8625 0.1974 0.4418 0.2028 1.0000 Uiso . . . . . . H581 H 1.0330 0.2659 0.5096 0.2107 1.0000 Uiso . . . . . . H582 H 1.0289 0.2233 0.4503 0.2107 1.0000 Uiso . . . . . . H591 H 1.1125 0.1728 0.5423 0.2158 1.0000 Uiso . . . . . . H592 H 1.0116 0.1806 0.5669 0.2158 1.0000 Uiso . . . . . . H593 H 1.0074 0.1380 0.5076 0.2158 1.0000 Uiso . . . . . . H601 H 0.7724 0.6250 0.6343 0.1304 0.2253 Uiso . . . . . . H602 H 0.8040 0.6088 0.5717 0.1304 0.2253 Uiso . . . . . . 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 0.08385(18) 0.04925(12) 0.06756(15) 0.00729(11) 0.03400(11) 0.01677(11) Cl1 0.101(3) 0.0465(13) 0.0912(18) 0.0020(11) 0.0251(15) -0.0033(12) C1 0.067(6) 0.070(6) 0.106(8) 0.013(5) 0.021(5) 0.010(4) O1 0.110(8) 0.083(6) 0.176(10) -0.025(6) 0.025(8) -0.006(5) C2 0.108(5) 0.074(4) 0.092(5) 0.007(4) 0.053(4) 0.027(4) O2 0.168(6) 0.125(5) 0.123(5) 0.005(4) 0.081(5) 0.061(5) C3 0.107(5) 0.074(4) 0.089(5) 0.010(4) 0.051(4) 0.035(4) O3 0.159(6) 0.107(4) 0.109(4) 0.046(4) 0.056(4) 0.067(4) N1 0.066(3) 0.043(2) 0.059(2) 0.0045(18) 0.021(2) 0.0072(19) C4 0.073(3) 0.051(3) 0.052(3) 0.010(2) 0.020(3) 0.012(2) C5 0.067(3) 0.049(3) 0.052(3) 0.006(2) 0.016(2) -0.002(2) C6 0.065(3) 0.039(2) 0.053(3) 0.002(2) 0.016(2) 0.000(2) C7 0.068(3) 0.040(2) 0.049(3) 0.0015(19) 0.017(2) 0.004(2) C8 0.062(3) 0.041(2) 0.053(3) 0.006(2) 0.018(2) 0.005(2) C9 0.077(4) 0.042(2) 0.051(3) -0.001(2) 0.019(3) 0.000(2) C10 0.104(5) 0.045(3) 0.055(3) 0.006(2) 0.024(3) 0.013(3) C11 0.118(5) 0.049(3) 0.059(3) 0.010(2) 0.034(3) 0.008(3) C12 0.137(6) 0.063(4) 0.061(4) 0.002(3) 0.046(4) 0.007(4) C13 0.108(5) 0.067(4) 0.058(3) 0.003(3) 0.035(3) 0.007(3) N2 0.097(4) 0.044(2) 0.061(3) 0.0007(19) 0.038(3) 0.002(2) C14 0.072(3) 0.041(2) 0.059(3) -0.005(2) 0.023(3) 0.002(2) O4 0.107(3) 0.050(2) 0.066(2) 0.0062(17) 0.044(2) 0.007(2) N3 0.086(4) 0.042(2) 0.063(3) 0.004(2) 0.037(3) 0.004(2) C15 0.105(5) 0.048(3) 0.085(4) -0.007(3) 0.054(4) 0.006(3) C16 0.089(4) 0.044(3) 0.078(4) -0.004(3) 0.033(3) 0.016(3) O5 0.087(3) 0.0479(19) 0.077(3) 0.0002(18) 0.018(2) 0.0111(19) C17 0.089(4) 0.050(3) 0.061(3) -0.005(2) 0.025(3) 0.006(3) C18 0.070(4) 0.073(4) 0.069(4) 0.001(3) 0.013(3) 0.013(3) C19 0.069(4) 0.070(4) 0.074(4) -0.001(3) 0.010(3) 0.011(3) C20 0.081(4) 0.057(3) 0.060(3) 0.000(2) 0.020(3) -0.001(3) C21 0.077(4) 0.055(3) 0.064(3) 0.008(3) 0.016(3) 0.006(3) C22 0.073(4) 0.051(3) 0.059(3) -0.001(2) 0.015(3) 0.005(2) O6 0.078(3) 0.062(2) 0.077(3) 0.001(2) 0.016(2) -0.001(2) C23 0.086(4) 0.059(3) 0.061(3) -0.001(3) 0.024(3) 0.002(3) C24 0.089(4) 0.065(3) 0.065(3) -0.006(3) 0.025(3) -0.001(3) O7 0.095(3) 0.062(2) 0.088(3) -0.013(2) 0.036(3) -0.013(2) C25 0.103(6) 0.060(4) 0.114(6) -0.017(4) 0.033(5) -0.018(4) C26 0.079(5) 0.072(5) 0.192(11) -0.014(6) 0.042(6) -0.020(4) O8 0.103(4) 0.068(3) 0.150(5) 0.010(3) 0.067(4) -0.002(3) C27 0.168(11) 0.051(4) 0.242(15) 0.006(7) 0.134(11) -0.015(5) C28 0.282(19) 0.072(6) 0.141(9) 0.019(6) 0.117(12) -0.011(8) O9 0.264(10) 0.058(3) 0.153(6) -0.002(4) 0.108(7) -0.006(4) C29 0.69(6) 0.076(7) 0.107(9) 0.029(7) 0.036(18) 0.054(16) C30 0.72(6) 0.096(10) 0.128(11) -0.004(8) -0.15(2) 0.060(19) O10 0.54(2) 0.060(4) 0.115(5) -0.001(4) 0.133(9) 0.013(7) C31 0.33(2) 0.089(7) 0.078(6) 0.000(5) 0.084(10) -0.017(10) C32 0.38(3) 0.115(9) 0.060(5) 0.001(6) -0.033(10) 0.056(13) C33 0.204(12) 0.116(8) 0.078(6) 0.014(5) 0.002(7) 0.027(8) C34 0.158(9) 0.081(5) 0.072(4) 0.013(4) 0.044(5) 0.006(6) C35 0.140(9) 0.079(5) 0.175(10) 0.003(6) 0.090(8) -0.009(5) C36 0.209(13) 0.072(6) 0.175(10) -0.013(6) 0.140(10) -0.016(6) O11 0.208(8) 0.089(4) 0.084(4) 0.036(3) -0.003(4) -0.043(4) C37 0.158(8) 0.084(5) 0.067(4) 0.025(4) 0.025(5) 0.004(5) C38 0.128(6) 0.056(3) 0.066(4) 0.018(3) 0.011(4) 0.005(4) N4 0.123(5) 0.050(3) 0.057(3) 0.012(2) 0.025(3) 0.009(3) C39 0.140(7) 0.056(3) 0.055(3) 0.013(3) 0.027(4) 0.012(4) O12 0.208(7) 0.080(3) 0.055(3) 0.017(2) 0.047(3) 0.024(4) N5 0.119(5) 0.060(3) 0.069(3) -0.015(3) 0.046(3) -0.026(3) C40 0.119(6) 0.095(6) 0.077(4) -0.020(4) 0.042(4) -0.044(5) C41 0.091(5) 0.077(4) 0.072(4) 0.001(3) 0.034(4) -0.007(3) C42 0.076(4) 0.055(3) 0.069(3) -0.001(3) 0.029(3) -0.005(3) C43 0.093(4) 0.043(3) 0.051(3) -0.003(2) 0.026(3) -0.005(3) C44 0.128(6) 0.043(3) 0.059(3) -0.003(2) 0.042(4) -0.009(3) C45 0.176(9) 0.064(4) 0.112(6) -0.028(4) 0.086(6) -0.045(5) C46 0.079(5) 0.116(7) 0.111(6) 0.022(5) 0.028(5) -0.003(5) O13 0.070(4) 0.197(8) 0.179(7) 0.025(6) 0.021(4) -0.011(5) N6 0.081(5) 0.119(6) 0.257(11) 0.067(7) 0.051(6) 0.032(5) C47 0.113(6) 0.138(7) 0.277(10) 0.070(7) 0.037(6) 0.046(5) C48 0.136(7) 0.126(7) 0.270(10) 0.068(7) 0.030(7) 0.034(5) C49 0.161(8) 0.146(7) 0.285(11) 0.075(8) 0.007(8) 0.037(6) C50 0.189(9) 0.191(9) 0.279(11) 0.071(9) 0.001(9) 0.020(8) C51 0.204(11) 0.205(10) 0.292(12) 0.069(10) -0.010(11) 0.026(9) C52 0.216(12) 0.228(12) 0.304(14) 0.061(12) 0.001(12) 0.026(12) C53 0.093(4) 0.044(3) 0.064(3) 0.001(2) 0.029(3) 0.005(3) O14 0.102(3) 0.054(2) 0.080(3) 0.010(2) 0.025(2) 0.017(2) N7 0.089(3) 0.050(2) 0.092(4) -0.004(2) 0.013(3) 0.002(3) C54 0.094(4) 0.073(4) 0.100(4) -0.008(3) 0.019(3) -0.004(3) C55 0.123(5) 0.105(5) 0.114(5) 0.012(4) 0.038(4) -0.022(4) C56 0.120(5) 0.155(7) 0.140(6) -0.003(5) 0.050(5) -0.013(5) C57 0.161(6) 0.187(8) 0.159(7) 0.015(6) 0.041(7) 0.000(7) C58 0.165(7) 0.193(9) 0.169(8) -0.005(7) 0.052(7) -0.001(8) C59 0.179(9) 0.195(11) 0.166(10) -0.010(7) 0.055(8) 0.011(9) Cl2 0.1076 0.0387 0.0721 0.0051 0.0310 0.0083 _refine_ls_extinction_method None loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Re1 . Cl1 . 2.478(3) yes Re1 . C1 . 1.892(7) yes Re1 . Cl91 . 2.521(9) yes Re1 . C91 . 1.875(10) yes Re1 . C2 . 1.914(7) yes Re1 . C3 . 1.907(7) yes Re1 . N1 . 2.174(4) yes Re1 . N2 . 2.158(5) yes C1 . O1 . 1.130(8) yes C91 . O91 . 1.125(10) yes C2 . O2 . 1.143(9) yes C3 . O3 . 1.167(9) yes N1 . C4 . 1.342(7) yes N1 . C8 . 1.357(6) yes C4 . C5 . 1.388(8) yes C4 . H41 . 1.000 no C5 . C6 . 1.383(7) yes C5 . H51 . 1.000 no C6 . C7 . 1.380(7) yes C6 . C14 . 1.517(7) yes C7 . C8 . 1.380(7) yes C7 . H71 . 1.000 no C8 . C9 . 1.464(7) yes C9 . C10 . 1.389(8) yes C9 . N2 . 1.362(7) yes C10 . C11 . 1.372(8) yes C10 . H101 . 1.000 no C11 . C12 . 1.368(10) yes C11 . C39 . 1.521(9) yes C12 . C13 . 1.373(10) yes C12 . H121 . 1.000 no C13 . N2 . 1.359(7) yes C13 . H131 . 1.000 no C14 . O4 . 1.227(6) yes C14 . N3 . 1.330(7) yes N3 . C15 . 1.457(8) yes N3 . H1 . 0.64(4) no C15 . C16 . 1.523(8) yes C15 . H151 . 1.000 no C15 . H152 . 1.000 no C16 . O5 . 1.423(8) yes C16 . H161 . 1.000 no C16 . H162 . 1.000 no O5 . C17 . 1.374(7) yes C17 . C18 . 1.388(10) yes C17 . C22 . 1.384(8) yes C18 . C19 . 1.376(10) yes C18 . H181 . 1.000 no C19 . C20 . 1.402(9) yes C19 . H191 . 1.000 no C20 . C21 . 1.377(9) yes C20 . O6 . 1.369(7) yes C21 . C22 . 1.389(8) yes C21 . H211 . 1.000 no C22 . H221 . 1.000 no O6 . C23 . 1.422(8) yes C23 . C24 . 1.486(9) yes C23 . H231 . 1.000 no C23 . H232 . 1.000 no C24 . O7 . 1.422(8) yes C24 . H241 . 1.000 no C24 . H242 . 1.000 no O7 . C25 . 1.408(8) yes C25 . C26 . 1.512(14) yes C25 . H251 . 1.000 no C25 . H252 . 1.000 no C26 . O8 . 1.414(13) yes C26 . H261 . 1.000 no C26 . H262 . 1.000 no O8 . C27 . 1.425(14) yes C27 . C28 . 1.45(2) yes C27 . H271 . 1.000 no C27 . H272 . 1.000 no C28 . O9 . 1.388(13) yes C28 . H281 . 1.000 no C28 . H282 . 1.000 no O9 . C29 . 1.324(17) yes C29 . C30 . 1.58(3) yes C29 . H291 . 1.000 no C29 . H292 . 1.000 no C30 . O10 . 1.43(3) yes C30 . H301 . 1.000 no C30 . H302 . 1.000 no O10 . C31 . 1.428(15) yes C31 . C32 . 1.44(3) yes C31 . C36 . 1.36(2) yes C32 . C33 . 1.41(2) yes C32 . H321 . 1.000 no C33 . C34 . 1.348(16) yes C33 . H331 . 1.000 no C34 . C35 . 1.386(15) yes C34 . O11 . 1.379(10) yes C35 . C36 . 1.373(13) yes C35 . H351 . 1.000 no C36 . H361 . 1.000 no O11 . C37 . 1.444(11) yes C37 . C38 . 1.463(13) yes C37 . H371 . 1.000 no C37 . H372 . 1.000 no C38 . N4 . 1.464(8) yes C38 . H381 . 1.000 no C38 . H382 . 1.000 no N4 . C39 . 1.336(9) yes N4 . H2 . 0.80(6) no C39 . O12 . 1.232(8) yes N5 . C40 . 1.339(12) yes N5 . C44 . 1.321(10) yes N5 . C45 . 1.482(9) yes C40 . C41 . 1.375(11) yes C40 . H401 . 1.000 no C41 . C42 . 1.387(10) yes C41 . C46 . 1.512(12) yes C42 . C43 . 1.392(9) yes C42 . H421 . 1.000 no C43 . C44 . 1.384(8) yes C43 . C53 . 1.489(9) yes C44 . H441 . 1.000 no C45 . H451 . 1.000 no C45 . H452 . 1.000 no C45 . H453 . 1.000 no C46 . O13 . 1.207(11) yes C46 . N6 . 1.308(14) yes N6 . C47 . 1.502(8) yes N6 . H3 . 0.63(6) no C47 . C48 . 1.526(9) yes C47 . H471 . 1.000 no C47 . H472 . 1.000 no C48 . C49 . 1.518(9) yes C48 . H481 . 1.000 no C48 . H482 . 1.000 no C49 . C50 . 1.520(9) yes C49 . H491 . 1.000 no C49 . H492 . 1.000 no C50 . C51 . 1.525(9) yes C50 . H501 . 1.000 no C50 . H502 . 1.000 no C51 . C52 . 1.508(10) yes C51 . H511 . 1.000 no C51 . H512 . 1.000 no C52 . H521 . 1.000 no C52 . H522 . 1.000 no C52 . H523 . 1.000 no C53 . O14 . 1.239(7) yes C53 . N7 . 1.332(8) yes N7 . C54 . 1.476(7) yes N7 . H4 . 0.92(6) no C54 . C55 . 1.530(8) yes C54 . H541 . 1.000 no C54 . H542 . 1.000 no C55 . C56 . 1.502(8) yes C55 . H551 . 1.000 no C55 . H552 . 1.000 no C56 . C57 . 1.523(9) yes C56 . H561 . 1.000 no C56 . H562 . 1.000 no C57 . C58 . 1.498(9) yes C57 . H571 . 1.000 no C57 . H572 . 1.000 no C58 . C59 . 1.508(9) yes C58 . H581 . 1.000 no C58 . H582 . 1.000 no C59 . H591 . 1.000 no C59 . H592 . 1.000 no C59 . H593 . 1.000 no C60 . Cl3 . 1.62(5) yes C60 . Cl4 . 1.73(5) yes C60 . H601 . 1.000 no C60 . H602 . 1.000 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag Cl1 . Re1 . C1 . 178.0(3) yes C1 . Re1 . C91 . 173.0(9) yes Cl91 . Re1 . C91 . 174.8(7) yes Cl1 . Re1 . C2 . 93.9(3) yes C1 . Re1 . C2 . 87.8(4) yes Cl91 . Re1 . C2 . 94.4(4) yes C91 . Re1 . C2 . 85.8(9) yes Cl1 . Re1 . C3 . 92.5(3) yes C1 . Re1 . C3 . 88.6(4) yes Cl91 . Re1 . C3 . 96.7(4) yes C91 . Re1 . C3 . 88.5(8) yes C2 . Re1 . C3 . 88.2(3) yes Cl1 . Re1 . N1 . 86.33(14) yes C1 . Re1 . N1 . 91.9(3) yes Cl91 . Re1 . N1 . 84.4(3) yes C91 . Re1 . N1 . 94.8(9) yes C2 . Re1 . N1 . 173.6(2) yes Cl1 . Re1 . N2 . 83.73(15) yes C1 . Re1 . N2 . 95.0(3) yes Cl91 . Re1 . N2 . 86.2(3) yes C91 . Re1 . N2 . 88.6(8) yes C2 . Re1 . N2 . 98.8(3) yes C3 . Re1 . N1 . 98.1(2) yes C3 . Re1 . N2 . 172.2(2) yes N1 . Re1 . N2 . 74.92(17) yes Re1 . C1 . O1 . 176.0(7) yes Re1 . C91 . O91 . 175.5(10) yes Cl1 . C91 . O91 . 36.2(19) yes Cl1 . O91 . C91 . 35.7(18) yes Re1 . C2 . O2 . 178.4(8) yes Re1 . C3 . O3 . 176.4(6) yes Re1 . N1 . C4 . 125.2(3) yes Re1 . N1 . C8 . 116.8(3) yes C4 . N1 . C8 . 117.9(4) yes N1 . C4 . C5 . 123.0(5) yes N1 . C4 . H41 . 118.492 no C5 . C4 . H41 . 118.492 no C4 . C5 . C6 . 118.6(5) yes C4 . C5 . H51 . 120.688 no C6 . C5 . H51 . 120.688 no C5 . C6 . C7 . 118.7(5) yes C5 . C6 . C14 . 117.6(5) yes C7 . C6 . C14 . 123.6(4) yes C6 . C7 . C8 . 119.9(4) yes C6 . C7 . H71 . 120.028 no C8 . C7 . H71 . 120.028 no N1 . C8 . C7 . 121.7(5) yes N1 . C8 . C9 . 115.2(4) yes C7 . C8 . C9 . 123.1(4) yes C8 . C9 . C10 . 122.6(5) yes C8 . C9 . N2 . 115.8(4) yes C10 . C9 . N2 . 121.6(5) yes C9 . C10 . C11 . 119.8(5) yes C9 . C10 . H101 . 120.106 no C11 . C10 . H101 . 120.106 no C10 . C11 . C12 . 119.1(6) yes C10 . C11 . C39 . 122.7(6) yes C12 . C11 . C39 . 118.2(6) yes C11 . C12 . C13 . 119.4(6) yes C11 . C12 . H121 . 120.279 no C13 . C12 . H121 . 120.279 no C12 . C13 . N2 . 122.9(6) yes C12 . C13 . H131 . 118.557 no N2 . C13 . H131 . 118.558 no Re1 . N2 . C9 . 117.0(3) yes Re1 . N2 . C13 . 125.7(4) yes C9 . N2 . C13 . 117.1(5) yes C6 . C14 . O4 . 119.9(4) yes C6 . C14 . N3 . 118.1(5) yes O4 . C14 . N3 . 122.1(5) yes C14 . N3 . C15 . 121.4(5) yes C14 . N3 . H1 . 123(4) no C15 . N3 . H1 . 115(4) no N3 . C15 . C16 . 110.1(5) yes N3 . C15 . H151 . 109.322 no C16 . C15 . H151 . 109.323 no N3 . C15 . H152 . 109.322 no C16 . C15 . H152 . 109.323 no H151 . C15 . H152 . 109.467 no C15 . C16 . O5 . 106.9(5) yes C15 . C16 . H161 . 110.123 no O5 . C16 . H161 . 110.123 no C15 . C16 . H162 . 110.122 no O5 . C16 . H162 . 110.123 no H161 . C16 . H162 . 109.467 no C16 . O5 . C17 . 117.4(5) yes O5 . C17 . C18 . 115.5(5) yes O5 . C17 . C22 . 124.7(6) yes C18 . C17 . C22 . 119.8(6) yes C17 . C18 . C19 . 120.3(6) yes C17 . C18 . H181 . 119.846 no C19 . C18 . H181 . 119.846 no C18 . C19 . C20 . 120.4(6) yes C18 . C19 . H191 . 119.781 no C20 . C19 . H191 . 119.781 no C19 . C20 . C21 . 118.6(6) yes C19 . C20 . O6 . 116.2(6) yes C21 . C20 . O6 . 125.2(6) yes C20 . C21 . C22 . 121.3(5) yes C20 . C21 . H211 . 119.363 no C22 . C21 . H211 . 119.363 no C17 . C22 . C21 . 119.5(6) yes C17 . C22 . H221 . 120.228 no C21 . C22 . H221 . 120.227 no C20 . O6 . C23 . 116.8(5) yes O6 . C23 . C24 . 110.2(5) yes O6 . C23 . H231 . 109.293 no C24 . C23 . H231 . 109.293 no O6 . C23 . H232 . 109.293 no C24 . C23 . H232 . 109.292 no H231 . C23 . H232 . 109.466 no C23 . C24 . O7 . 109.1(5) yes C23 . C24 . H241 . 109.569 no O7 . C24 . H241 . 109.569 no C23 . C24 . H242 . 109.569 no O7 . C24 . H242 . 109.569 no H241 . C24 . H242 . 109.467 no C24 . O7 . C25 . 113.8(5) yes O7 . C25 . C26 . 108.3(6) yes O7 . C25 . H251 . 109.771 no C26 . C25 . H251 . 109.771 no O7 . C25 . H252 . 109.770 no C26 . C25 . H252 . 109.771 no H251 . C25 . H252 . 109.468 no C25 . C26 . O8 . 107.9(7) yes C25 . C26 . H261 . 109.874 no O8 . C26 . H261 . 109.874 no C25 . C26 . H262 . 109.873 no O8 . C26 . H262 . 109.872 no H261 . C26 . H262 . 109.466 no C26 . O8 . C27 . 114.2(9) yes O8 . C27 . C28 . 111.7(10) yes O8 . C27 . H271 . 108.916 no C28 . C27 . H271 . 108.915 no O8 . C27 . H272 . 108.917 no C28 . C27 . H272 . 108.916 no H271 . C27 . H272 . 109.469 no C27 . C28 . O9 . 106.0(10) yes C27 . C28 . H281 . 110.326 no O9 . C28 . H281 . 110.325 no C27 . C28 . H282 . 110.326 no O9 . C28 . H282 . 110.325 no H281 . C28 . H282 . 109.467 no C28 . O9 . C29 . 111.3(10) yes O9 . C29 . C30 . 106.2(17) yes O9 . C29 . H291 . 110.287 no C30 . C29 . H291 . 110.285 no O9 . C29 . H292 . 110.290 no C30 . C29 . H292 . 110.291 no H291 . C29 . H292 . 109.470 no C29 . C30 . O10 . 101(3) yes C29 . C30 . H301 . 111.490 no O10 . C30 . H301 . 111.491 no C29 . C30 . H302 . 111.497 no O10 . C30 . H302 . 111.496 no H301 . C30 . H302 . 109.473 no C30 . O10 . C31 . 112.9(19) yes O10 . C31 . C32 . 125.9(17) yes O10 . C31 . C36 . 112.9(17) yes C32 . C31 . C36 . 121.1(11) yes C31 . C32 . C33 . 119.0(13) yes C31 . C32 . H321 . 120.498 no C33 . C32 . H321 . 120.500 no C32 . C33 . C34 . 116.0(14) yes C32 . C33 . H331 . 121.980 no C34 . C33 . H331 . 121.983 no C33 . C34 . C35 . 126.0(10) yes C33 . C34 . O11 . 118.5(11) yes C35 . C34 . O11 . 115.2(9) yes C34 . C35 . C36 . 117.9(12) yes C34 . C35 . H351 . 121.039 no C36 . C35 . H351 . 121.038 no C31 . C36 . C35 . 119.9(14) yes C31 . C36 . H361 . 120.070 no C35 . C36 . H361 . 120.070 no C34 . O11 . C37 . 117.8(6) yes O11 . C37 . C38 . 107.9(6) yes O11 . C37 . H371 . 109.865 no C38 . C37 . H371 . 109.865 no O11 . C37 . H372 . 109.865 no C38 . C37 . H372 . 109.866 no H371 . C37 . H372 . 109.466 no C37 . C38 . N4 . 115.1(8) yes C37 . C38 . H381 . 108.045 no N4 . C38 . H381 . 108.046 no C37 . C38 . H382 . 108.044 no N4 . C38 . H382 . 108.045 no H381 . C38 . H382 . 109.467 no C38 . N4 . C39 . 121.3(6) yes C38 . N4 . H2 . 127(4) no C39 . N4 . H2 . 111(4) no C11 . C39 . N4 . 117.3(5) yes C11 . C39 . O12 . 119.8(6) yes N4 . C39 . O12 . 122.8(6) yes C40 . N5 . C44 . 119.5(6) yes C40 . N5 . C45 . 121.0(8) yes C44 . N5 . C45 . 119.4(8) yes N5 . C40 . C41 . 122.6(8) yes N5 . C40 . H401 . 118.723 no C41 . C40 . H401 . 118.721 no C40 . C41 . C42 . 117.9(8) yes C40 . C41 . C46 . 118.1(8) yes C42 . C41 . C46 . 124.0(7) yes C41 . C42 . C43 . 119.8(6) yes C41 . C42 . H421 . 120.113 no C43 . C42 . H421 . 120.115 no C42 . C43 . C44 . 118.0(6) yes C42 . C43 . C53 . 124.4(5) yes C44 . C43 . C53 . 117.6(6) yes N5 . C44 . C43 . 122.3(6) yes N5 . C44 . H441 . 118.860 no C43 . C44 . H441 . 118.858 no N5 . C45 . H451 . 109.466 no N5 . C45 . H452 . 109.465 no H451 . C45 . H452 . 109.476 no N5 . C45 . H453 . 109.467 no H451 . C45 . H453 . 109.478 no H452 . C45 . H453 . 109.477 no C41 . C46 . O13 . 119.0(9) yes C41 . C46 . N6 . 116.0(8) yes O13 . C46 . N6 . 125.0(10) yes C46 . N6 . C47 . 123.6(11) yes C46 . N6 . H3 . 125(6) no C47 . N6 . H3 . 111(6) no N6 . C47 . C48 . 112.6(7) yes N6 . C47 . H471 . 108.692 no C48 . C47 . H471 . 108.694 no N6 . C47 . H472 . 108.695 no C48 . C47 . H472 . 108.695 no H471 . C47 . H472 . 109.465 no C47 . C48 . C49 . 112.7(7) yes C47 . C48 . H481 . 108.655 no C49 . C48 . H481 . 108.655 no C47 . C48 . H482 . 108.656 no C49 . C48 . H482 . 108.656 no H481 . C48 . H482 . 109.468 no C48 . C49 . C50 . 112.5(8) yes C48 . C49 . H491 . 108.722 no C50 . C49 . H491 . 108.721 no C48 . C49 . H492 . 108.721 no C50 . C49 . H492 . 108.724 no H491 . C49 . H492 . 109.464 no C49 . C50 . C51 . 113.2(8) yes C49 . C50 . H501 . 108.528 no C51 . C50 . H501 . 108.531 no C49 . C50 . H502 . 108.524 no C51 . C50 . H502 . 108.528 no H501 . C50 . H502 . 109.468 no C50 . C51 . C52 . 111.9(9) yes C50 . C51 . H511 . 108.862 no C52 . C51 . H511 . 108.865 no C50 . C51 . H512 . 108.862 no C52 . C51 . H512 . 108.862 no H511 . C51 . H512 . 109.468 no C51 . C52 . H521 . 109.464 no C51 . C52 . H522 . 109.466 no H521 . C52 . H522 . 109.472 no C51 . C52 . H523 . 109.470 no H521 . C52 . H523 . 109.476 no H522 . C52 . H523 . 109.479 no C43 . C53 . O14 . 120.5(5) yes C43 . C53 . N7 . 116.4(5) yes O14 . C53 . N7 . 123.1(7) yes C53 . N7 . C54 . 121.4(6) yes C53 . N7 . H4 . 119(3) no C54 . N7 . H4 . 119(3) no N7 . C54 . C55 . 111.1(5) yes N7 . C54 . H541 . 109.060 no C55 . C54 . H541 . 109.061 no N7 . C54 . H542 . 109.061 no C55 . C54 . H542 . 109.061 no H541 . C54 . H542 . 109.467 no C54 . C55 . C56 . 111.4(6) yes C54 . C55 . H551 . 108.990 no C56 . C55 . H551 . 108.990 no C54 . C55 . H552 . 108.991 no C56 . C55 . H552 . 108.991 no H551 . C55 . H552 . 109.467 no C55 . C56 . C57 . 107.7(7) yes C55 . C56 . H561 . 109.924 no C57 . C56 . H561 . 109.925 no C55 . C56 . H562 . 109.924 no C57 . C56 . H562 . 109.926 no H561 . C56 . H562 . 109.466 no C56 . C57 . C58 . 114.3(7) yes C56 . C57 . H571 . 108.247 no C58 . C57 . H571 . 108.250 no C56 . C57 . H572 . 108.247 no C58 . C57 . H572 . 108.250 no H571 . C57 . H572 . 109.467 no C57 . C58 . C59 . 109.9(8) yes C57 . C58 . H581 . 109.364 no C59 . C58 . H581 . 109.365 no C57 . C58 . H582 . 109.364 no C59 . C58 . H582 . 109.366 no H581 . C58 . H582 . 109.467 no C58 . C59 . H591 . 109.467 no C58 . C59 . H592 . 109.465 no H591 . C59 . H592 . 109.477 no C58 . C59 . H593 . 109.465 no H591 . C59 . H593 . 109.478 no H592 . C59 . H593 . 109.475 no Cl3 . C60 . Cl4 . 117(3) yes Cl3 . C60 . H601 . 107.528 no Cl4 . C60 . H601 . 107.530 no Cl3 . C60 . H602 . 107.526 no Cl4 . C60 . H602 . 107.529 no H601 . C60 . H602 . 109.463 no