# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # the Centre National de la Recherche Scientifique, 2006 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Sergey Gromov' _publ_contact_author_address ; Photochemistry Center of the RAS 7A Novatorov str Moscow 119421 RUSSIAN FEDERATION ; _publ_contact_author_email GROMOV@PHOTONICS.RU _publ_section_title ; Photoinduced and dark complexation of unsaturated viologen analogues containing two ammonium tails with cucurbit[8]uril ; loop_ _publ_author_name 'Sergey Gromov' 'Michael V. Alfimov' 'Vladimir P. Fedin' 'J Howard' L.G.Kuz'mina ; N.A.Lobova ; 'Yuri A. Strelenko' 'Artem I. Vedernikov' # Attachment 'B511456J_4a_ref.cif' data_ccc _database_code_depnum_ccdc_archive 'CCDC 288096' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H48 Cl N32 O24' _chemical_formula_weight 1492.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)/ncm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z+1/2' 'y, -x+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' 'y+1/2, x+1/2, -z' '-y, -x, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z-1/2' '-y, x-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' '-y-1/2, -x-1/2, z' 'y, x, z' _cell_length_a 26.2548(8) _cell_length_b 26.2548(8) _cell_length_c 12.7555(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8792.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6161 _cell_measurement_theta_min 2.357 _cell_measurement_theta_max 20.907 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3076 _exptl_absorpt_coefficient_mu 0.121 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9691 _exptl_absorpt_correction_T_max 0.9832 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60288 _diffrn_reflns_av_R_equivalents 0.0964 _diffrn_reflns_av_sigmaI/netI 0.0562 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.10 _diffrn_reflns_theta_max 27.00 _reflns_number_total 4966 _reflns_number_gt 2776 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Oxygen atoms of water molecules were refined with partial occupations. These s.o.f. were first refined and then fixed at obtained values. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4966 _refine_ls_number_parameters 266 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2546 _refine_ls_R_factor_gt 0.1903 _refine_ls_wR_factor_ref 0.5266 _refine_ls_wR_factor_gt 0.4958 _refine_ls_goodness_of_fit_ref 1.941 _refine_ls_restrained_S_all 1.941 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.2500 0.7500 0.7500 0.0675(12) Uani 1 4 d S . . O1A O 0.2143(2) 0.7759(3) 0.8153(6) 0.087(2) Uani 1 1 d . . . O1 O 0.1452(3) 0.3548(3) 1.0980(6) 0.093(3) Uani 1 2 d S . . O2 O 0.2091(2) 0.4850(2) 1.1355(4) 0.0633(16) Uani 1 1 d . . . O3 O 0.1651(2) 0.6102(2) 1.2228(4) 0.0604(15) Uani 1 1 d . . . O4 O 0.1558(2) 0.5378(2) 0.6862(4) 0.0722(17) Uani 1 1 d . . . O5 O 0.0962(3) 0.4038(3) 0.6439(7) 0.082(3) Uani 1 2 d S . . N1 N 0.1826(2) 0.3766(2) 0.9422(5) 0.0584(17) Uani 1 1 d . . . N2 N 0.2235(2) 0.4587(2) 0.9656(4) 0.0538(16) Uani 1 1 d . . . N3 N 0.2295(2) 0.5404(2) 1.0029(4) 0.0500(15) Uani 1 1 d . . . N4 N 0.2024(2) 0.6240(2) 1.0617(4) 0.0499(15) Uani 1 1 d . . . N5 N 0.1785(3) 0.6440(2) 0.8823(4) 0.0567(17) Uani 1 1 d . . . N6 N 0.2080(2) 0.5622(2) 0.8226(4) 0.0524(15) Uani 1 1 d . . . N7 N 0.2001(2) 0.4796(2) 0.7874(4) 0.0525(15) Uani 1 1 d . . . N8 N 0.1622(2) 0.3967(2) 0.7621(5) 0.0592(17) Uani 1 1 d . . . C1 C 0.1496(3) 0.3504(3) 1.0073(9) 0.062(3) Uani 1 2 d S . . C2 C 0.2255(3) 0.4049(3) 0.9858(7) 0.068(2) Uani 1 1 d . . . H2A H 0.2265 0.3993 1.0626 0.082 Uiso 1 1 calc R . . H2B H 0.2575 0.3910 0.9561 0.082 Uiso 1 1 calc R . . C3 C 0.2197(3) 0.4942(3) 1.0433(5) 0.0533(19) Uani 1 1 d . . . C4 C 0.2391(3) 0.5843(3) 1.0691(6) 0.059(2) Uani 1 1 d . . . H4A H 0.2407 0.5727 1.1429 0.071 Uiso 1 1 calc R . . H4B H 0.2729 0.5985 1.0508 0.071 Uiso 1 1 calc R . . C5 C 0.1701(3) 0.6350(3) 1.1429(6) 0.0540(19) Uani 1 1 d . . . C6 C 0.2066(3) 0.6158(3) 0.8042(5) 0.057(2) Uani 1 1 d . . . H6A H 0.1911 0.6221 0.7347 0.068 Uiso 1 1 calc R . . H6B H 0.2420 0.6289 0.8020 0.068 Uiso 1 1 calc R . . C7 C 0.1848(3) 0.5270(3) 0.7579(5) 0.057(2) Uani 1 1 d . . . C8 C 0.1937(4) 0.4361(3) 0.7184(6) 0.068(2) Uani 1 1 d . . . H8A H 0.1785 0.4478 0.6517 0.082 Uiso 1 1 calc R . . H8B H 0.2277 0.4216 0.7023 0.082 Uiso 1 1 calc R . . C9 C 0.1188(3) 0.3812(3) 0.7166(8) 0.058(3) Uani 1 2 d S . . C10 C 0.1812(3) 0.3602(3) 0.8357(6) 0.0579(19) Uani 1 1 d . . . H10A H 0.2149 0.3462 0.8130 0.069 Uiso 1 1 calc R . . C11 C 0.2391(3) 0.4810(3) 0.8684(6) 0.0523(18) Uani 1 1 d . . . H11A H 0.2721 0.4664 0.8431 0.063 Uiso 1 1 calc R . . C12 C 0.2439(3) 0.5377(3) 0.8943(6) 0.0505(18) Uani 1 1 d . . . H12A H 0.2795 0.5503 0.8831 0.061 Uiso 1 1 calc R . . C13 C 0.2011(3) 0.6617(3) 0.9797(5) 0.0501(17) Uani 1 1 d . . . H13A H 0.2352 0.6775 0.9681 0.060 Uiso 1 1 calc R . . O1W O 0.1485(5) 0.4846(8) 0.4701(10) 0.046(5) Uani 0.25 1 d P . . O2W O 0.2500 0.2500 0.4057(18) 0.056(5) Uani 0.50 4 d SP . . O3W O 0.0953(12) 0.4047(12) 0.399(5) 0.13(2) Uani 0.25 2 d SP . . O4W O 0.110(2) 0.456(2) 0.212(5) 0.100(17) Uiso 0.13 1 d P . . O5W O 0.3597(7) 0.5848(8) 0.9286(17) 0.057(5) Uiso 0.25 1 d P . . O6W O 0.1865(8) 0.3135(8) 0.597(3) 0.064(8) Uiso 0.25 2 d SP . . 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 Cl1 0.0554(14) 0.0554(14) 0.092(3) 0.000 0.000 0.000 O1A 0.054(3) 0.103(5) 0.103(5) -0.006(4) -0.004(3) 0.010(3) O1 0.124(5) 0.124(5) 0.031(4) 0.009(3) -0.009(3) -0.009(6) O2 0.068(3) 0.087(4) 0.035(3) 0.002(3) -0.010(2) 0.020(3) O3 0.082(4) 0.072(3) 0.027(2) -0.004(2) -0.001(2) 0.009(3) O4 0.086(4) 0.102(4) 0.029(3) 0.001(3) -0.008(3) -0.009(3) O5 0.094(4) 0.094(4) 0.058(5) 0.021(4) -0.021(4) -0.029(5) N1 0.064(4) 0.070(4) 0.041(3) 0.002(3) -0.009(3) -0.003(3) N2 0.062(4) 0.063(4) 0.036(3) -0.004(3) -0.005(3) 0.001(3) N3 0.057(3) 0.057(4) 0.037(3) -0.010(3) -0.007(3) 0.010(3) N4 0.058(3) 0.063(4) 0.028(3) -0.009(3) 0.006(2) 0.007(3) N5 0.076(4) 0.063(4) 0.031(3) -0.008(3) 0.008(3) 0.008(3) N6 0.069(4) 0.058(4) 0.030(3) -0.007(3) 0.004(3) 0.003(3) N7 0.063(4) 0.062(4) 0.033(3) -0.010(3) 0.002(3) -0.010(3) N8 0.065(4) 0.072(4) 0.040(3) 0.001(3) -0.001(3) -0.019(3) C1 0.068(4) 0.068(4) 0.049(6) 0.007(4) -0.007(4) 0.002(6) C2 0.076(5) 0.065(5) 0.063(5) 0.000(4) -0.020(4) 0.004(4) C3 0.058(4) 0.071(5) 0.031(3) -0.002(3) -0.013(3) 0.016(3) C4 0.066(5) 0.073(5) 0.038(4) -0.016(3) -0.015(3) 0.009(4) C5 0.070(5) 0.056(4) 0.037(4) -0.012(3) -0.010(3) 0.003(4) C6 0.080(5) 0.060(5) 0.031(3) -0.003(3) 0.018(3) 0.014(4) C7 0.068(5) 0.071(5) 0.033(4) -0.004(3) 0.009(3) -0.016(4) C8 0.090(6) 0.083(6) 0.032(4) -0.015(4) 0.012(4) -0.030(4) C9 0.070(4) 0.070(4) 0.034(5) -0.004(4) 0.004(4) -0.018(6) C10 0.054(4) 0.064(5) 0.055(4) -0.014(4) 0.010(3) 0.007(3) C11 0.054(4) 0.064(4) 0.039(4) -0.010(3) 0.002(3) -0.003(3) C12 0.047(4) 0.064(4) 0.040(4) -0.009(3) 0.007(3) 0.001(3) C13 0.051(4) 0.057(4) 0.042(4) -0.014(3) 0.006(3) -0.009(3) O1W 0.024(7) 0.105(14) 0.010(6) 0.028(8) 0.008(6) 0.025(8) O2W 0.035(6) 0.035(6) 0.097(16) 0.000 0.000 -0.020(7) O3W 0.085(17) 0.085(17) 0.22(6) 0.04(2) -0.04(2) -0.02(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 O1A 1.426(7) 2_565 ? Cl1 O1A 1.426(7) 11_567 ? Cl1 O1A 1.426(7) . ? Cl1 O1A 1.426(7) 12_667 ? O1 C1 1.168(13) . ? O2 C3 1.233(9) . ? O3 C5 1.216(9) . ? O4 C7 1.223(9) . ? O5 C9 1.250(13) . ? N1 C1 1.384(9) . ? N1 C10 1.426(9) . ? N1 C2 1.460(10) . ? N2 C3 1.365(9) . ? N2 C11 1.431(9) . ? N2 C2 1.436(10) . ? N3 C3 1.343(10) . ? N3 C12 1.437(9) . ? N3 C4 1.451(9) . ? N4 C5 1.368(9) . ? N4 C4 1.423(10) . ? N4 C13 1.439(9) . ? N5 C5 1.372(10) 7_457 ? N5 C6 1.444(9) . ? N5 C13 1.453(9) . ? N6 C7 1.381(9) . ? N6 C6 1.428(10) . ? N6 C12 1.461(10) . ? N7 C7 1.361(10) . ? N7 C8 1.452(9) . ? N7 C11 1.455(9) . ? N8 C9 1.343(9) . ? N8 C8 1.436(10) . ? N8 C10 1.433(10) . ? C1 N1 1.384(9) 15_665 ? C5 N5 1.372(10) 7_457 ? C9 N8 1.343(9) 15_665 ? C10 C10 1.537(16) 15_665 ? C11 C12 1.532(10) . ? C13 C13 1.551(14) 7_457 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A Cl1 O1A 109.9(3) 2_565 11_567 ? O1A Cl1 O1A 108.5(6) 2_565 . ? O1A Cl1 O1A 109.9(3) 11_567 . ? O1A Cl1 O1A 109.9(3) 2_565 12_667 ? O1A Cl1 O1A 108.5(6) 11_567 12_667 ? O1A Cl1 O1A 109.9(3) . 12_667 ? C1 N1 C10 113.9(7) . . ? C1 N1 C2 120.5(7) . . ? C10 N1 C2 122.5(7) . . ? C3 N2 C11 111.7(6) . . ? C3 N2 C2 123.0(7) . . ? C11 N2 C2 123.2(6) . . ? C3 N3 C12 112.1(6) . . ? C3 N3 C4 121.8(6) . . ? C12 N3 C4 123.6(6) . . ? C5 N4 C4 121.5(6) . . ? C5 N4 C13 113.0(6) . . ? C4 N4 C13 124.6(6) . . ? C5 N5 C6 121.4(6) 7_457 . ? C5 N5 C13 112.3(6) 7_457 . ? C6 N5 C13 123.0(6) . . ? C7 N6 C6 123.3(6) . . ? C7 N6 C12 111.4(6) . . ? C6 N6 C12 123.6(6) . . ? C7 N7 C8 121.2(6) . . ? C7 N7 C11 112.5(6) . . ? C8 N7 C11 122.1(7) . . ? C9 N8 C8 122.7(7) . . ? C9 N8 C10 112.0(7) . . ? C8 N8 C10 122.4(7) . . ? O1 C1 N1 127.4(5) . . ? O1 C1 N1 127.4(5) . 15_665 ? N1 C1 N1 105.2(9) . 15_665 ? N2 C2 N1 113.7(6) . . ? O2 C3 N3 125.9(7) . . ? O2 C3 N2 125.2(7) . . ? N3 C3 N2 109.0(6) . . ? N4 C4 N3 115.3(6) . . ? O3 C5 N4 126.1(7) . . ? O3 C5 N5 126.0(7) . 7_457 ? N4 C5 N5 107.9(6) . 7_457 ? N6 C6 N5 113.9(6) . . ? O4 C7 N7 127.1(7) . . ? O4 C7 N6 124.6(8) . . ? N7 C7 N6 108.4(6) . . ? N8 C8 N7 113.4(6) . . ? O5 C9 N8 125.4(5) . 15_665 ? O5 C9 N8 125.4(5) . . ? N8 C9 N8 109.2(10) 15_665 . ? N1 C10 N8 115.5(6) . . ? N1 C10 C10 103.4(4) . 15_665 ? N8 C10 C10 103.2(4) . 15_665 ? N2 C11 N7 113.8(6) . . ? N2 C11 C12 103.6(6) . . ? N7 C11 C12 103.6(6) . . ? N3 C12 N6 114.3(6) . . ? N3 C12 C11 103.5(6) . . ? N6 C12 C11 103.9(6) . . ? N4 C13 N5 114.3(6) . . ? N4 C13 C13 103.4(6) . 7_457 ? N5 C13 C13 103.1(7) . 7_457 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.063 _refine_diff_density_min -0.589 _refine_diff_density_rms 0.223 # Attachment 'B511456J_4b_rev.cif' data_p21n _database_code_depnum_ccdc_archive 'CCDC 288097' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C98 H104 Br1.52 Cl2.48 N52 O35.10' _chemical_formula_weight 2781.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.5210(7) _cell_length_b 25.5665(11) _cell_length_c 32.4483(14) _cell_angle_alpha 90.00 _cell_angle_beta 101.039(2) _cell_angle_gamma 90.00 _cell_volume 12637.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 120.0(2) _cell_measurement_reflns_used 6535 _cell_measurement_theta_min 2.304 _cell_measurement_theta_max 29.983 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5729 _exptl_absorpt_coefficient_mu 0.641 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7745 _exptl_absorpt_correction_T_max 0.9270 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 150412 _diffrn_reflns_av_R_equivalents 0.2618 _diffrn_reflns_av_sigmaI/netI 0.3021 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.02 _diffrn_reflns_theta_max 28.00 _reflns_number_total 30519 _reflns_number_gt 8509 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Atoms Br(3) and perchlorate Cl(3), as well as Br(4) and perchlorate Cl(4) were refined as free variables with the sums of their occupancies constrained to 1. Perchlorate atoms Cl(2) was found and refined with four oxygens, whereas its second disordered component [Cl(2')] was refined without corresponding oxygens. These atoms were first refined as free variables and, at the final frefinement, their occupancies were fixed with obtained values. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1782P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0087(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 30519 _refine_ls_number_parameters 1679 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.3045 _refine_ls_R_factor_gt 0.1253 _refine_ls_wR_factor_ref 0.3702 _refine_ls_wR_factor_gt 0.3255 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 0.924 _refine_ls_shift/su_max 0.061 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br -0.58719(8) 0.77552(5) 0.14737(4) 0.0630(4) Uiso 1 1 d . . . Cl3 Cl -0.3092(3) 1.14175(15) -0.45097(15) 0.0395(10) Uiso 0.725(7) 1 d P A 1 Br3 Br -0.3346(3) 1.13591(16) -0.46177(15) 0.0363(15) Uiso 0.275(7) 1 d P A 2 Cl4 Cl -1.4338(3) 0.86485(18) -0.44406(18) 0.0511(15) Uiso 0.753(7) 1 d P B 3 Br4 Br -1.4165(4) 0.8589(2) -0.4332(2) 0.0392(18) Uiso 0.247(7) 1 d P B 4 Cl2' Cl -0.5206(4) 0.7573(3) 0.0075(2) 0.065(2) Uiso 0.479(8) 1 d P C 5 Cl2 Cl -0.4863(9) 0.7387(6) -0.0329(5) 0.231(7) Uiso 0.521(8) 1 d PD C 6 O21 O -0.4897(12) 0.7517(8) -0.0805(5) 0.114(7) Uiso 0.521(8) 1 d PD C 6 O22 O -0.3821(10) 0.7353(7) -0.0131(5) 0.097(6) Uiso 0.521(8) 1 d PD C 6 O23 O -0.5261(11) 0.6843(7) -0.0329(5) 0.097(6) Uiso 0.521(8) 1 d PD C 6 O24 O -0.517(2) 0.7809(12) -0.0041(11) 0.31(3) Uiso 0.521(8) 1 d PD C 6 O1A O -1.0030(4) 0.7971(2) 0.08156(18) 0.0409(15) Uani 1 1 d . . . O2A O -0.7862(4) 0.8609(2) 0.12646(17) 0.0332(14) Uani 1 1 d . . . O3A O -0.7138(4) 1.0015(2) 0.15034(18) 0.0375(15) Uani 1 1 d . . . O4A O -0.8295(4) 1.1376(2) 0.14133(19) 0.0399(15) Uani 1 1 d . . . O5A O -0.9265(4) 0.8217(2) -0.09469(18) 0.0430(16) Uani 1 1 d . . . O6A O -0.6930(4) 0.8802(2) -0.0483(2) 0.0441(16) Uani 1 1 d . . . O7A O -0.6238(4) 1.0176(2) -0.02520(19) 0.0431(16) Uani 1 1 d . . . O8A O -0.7598(4) 1.1512(2) -0.04013(19) 0.0436(16) Uani 1 1 d . . . N1A N -1.0473(4) 0.7712(3) 0.0123(2) 0.0328(17) Uani 1 1 d . . . N2A N -0.9063(4) 0.7725(3) 0.0403(2) 0.0292(16) Uani 1 1 d . . . N3A N -0.7657(4) 0.8131(3) 0.0687(2) 0.0347(17) Uani 1 1 d . . . N4A N -0.6767(4) 0.8797(3) 0.0894(2) 0.0283(16) Uani 1 1 d . . . N5A N -0.6261(4) 0.9681(3) 0.1077(2) 0.0336(17) Uani 1 1 d . . . N6A N -0.6454(4) 1.0529(3) 0.1088(2) 0.0316(16) Uani 1 1 d . . . N7A N -0.7220(4) 1.1364(3) 0.1014(2) 0.0328(17) Uani 1 1 d . . . N8A N -0.8361(5) 1.1901(3) 0.0833(2) 0.0341(17) Uani 1 1 d . . . N9A N -1.0165(4) 0.7776(3) -0.0582(2) 0.0321(17) Uani 1 1 d . . . N10A N -0.8745(4) 0.7851(3) -0.0294(2) 0.0321(17) Uani 1 1 d . . . N11A N -0.7314(5) 0.8222(3) -0.0013(2) 0.0355(17) Uani 1 1 d . . . N12A N -0.6333(5) 0.8829(3) 0.0220(2) 0.0373(18) Uani 1 1 d . . . N13A N -0.5907(4) 0.9741(3) 0.0375(2) 0.0318(17) Uani 1 1 d . . . N14A N -0.6117(5) 1.0594(3) 0.0389(2) 0.0350(17) Uani 1 1 d . . . N15A N -0.6948(4) 1.1406(3) 0.0293(2) 0.0335(17) Uani 1 1 d . . . N16A N -0.8049(4) 1.1981(3) 0.0127(2) 0.0347(17) Uani 1 1 d . . . C1A C -0.9856(6) 0.7817(3) 0.0488(2) 0.031(2) Uani 1 1 d . . . C2A C -0.8278(6) 0.7716(3) 0.0729(3) 0.035(2) Uani 1 1 d . . . H2AA H -0.7983 0.7374 0.0722 0.042 Uiso 1 1 calc R . . H2AB H -0.8451 0.7749 0.1006 0.042 Uiso 1 1 calc R . . C3A C -0.7477(5) 0.8532(3) 0.0983(3) 0.0283(19) Uani 1 1 d . . . C4A C -0.6272(6) 0.9139(3) 0.1209(2) 0.0312(19) Uani 1 1 d . . . H4AA H -0.5660 0.9010 0.1282 0.037 Uiso 1 1 calc R . . H4AB H -0.6527 0.9122 0.1466 0.037 Uiso 1 1 calc R . . C5A C -0.6670(5) 1.0072(3) 0.1248(3) 0.0309(19) Uani 1 1 d . . . C6A C -0.6595(6) 1.1036(3) 0.1284(3) 0.036(2) Uani 1 1 d . . . H6AA H -0.6807 1.0971 0.1548 0.044 Uiso 1 1 calc R . . H6AB H -0.6028 1.1224 0.1355 0.044 Uiso 1 1 calc R . . C7A C -0.7983(6) 1.1528(3) 0.1114(3) 0.031(2) Uani 1 1 d . . . C8A C -1.0930(6) 0.7765(4) -0.0908(3) 0.038(2) Uani 1 1 d . . . C9A C -0.9385(6) 0.7978(4) -0.0642(3) 0.039(2) Uani 1 1 d . . . C10A C -0.7804(5) 0.7862(3) -0.0309(3) 0.034(2) Uani 1 1 d . . . H10C H -0.7558 0.7506 -0.0251 0.041 Uiso 1 1 calc R . . H10D H -0.7733 0.7961 -0.0596 0.041 Uiso 1 1 calc R . . C11A C -0.6875(6) 0.8631(3) -0.0127(3) 0.034(2) Uani 1 1 d . . . C12A C -0.5695(6) 0.9253(3) 0.0209(3) 0.041(2) Uani 1 1 d . . . H12C H -0.5117 0.9138 0.0369 0.049 Uiso 1 1 calc R . . H12D H -0.5633 0.9307 -0.0086 0.049 Uiso 1 1 calc R . . C13A C -0.6101(6) 1.0168(4) 0.0130(3) 0.037(2) Uani 1 1 d . . . C14A C -0.6189(6) 1.1131(3) 0.0228(3) 0.040(2) Uani 1 1 d . . . H14C H -0.5663 1.1329 0.0364 0.047 Uiso 1 1 calc R . . H14D H -0.6190 1.1122 -0.0077 0.047 Uiso 1 1 calc R . . C15A C -0.7538(6) 1.1629(4) -0.0032(3) 0.041(2) Uani 1 1 d . . . C16A C -0.8604(6) 1.2349(4) -0.0135(3) 0.039(2) Uani 1 1 d . . . C17A C -1.0077(6) 0.7475(3) -0.0202(3) 0.034(2) Uani 1 1 d . . . H17A H -1.0277 0.7106 -0.0259 0.041 Uiso 1 1 calc R . . C18A C -0.9078(5) 0.7504(3) -0.0015(2) 0.0306(19) Uani 1 1 d . . . H18C H -0.8793 0.7152 -0.0001 0.037 Uiso 1 1 calc R . . C19A C -0.7008(5) 0.8085(3) 0.0427(3) 0.033(2) Uani 1 1 d . . . H19A H -0.6713 0.7736 0.0459 0.039 Uiso 1 1 calc R . . C20A C -0.6361(5) 0.8534(3) 0.0589(3) 0.0311(19) Uani 1 1 d . . . H20C H -0.5768 0.8396 0.0719 0.037 Uiso 1 1 calc R . . C21A C -0.5664(6) 0.9874(3) 0.0821(3) 0.036(2) Uani 1 1 d . . . H21A H -0.5041 0.9780 0.0941 0.043 Uiso 1 1 calc R . . C22A C -0.5818(6) 1.0467(3) 0.0822(3) 0.037(2) Uani 1 1 d . . . H22C H -0.5262 1.0657 0.0939 0.044 Uiso 1 1 calc R . . C23A C -0.6962(6) 1.1693(3) 0.0688(3) 0.036(2) Uani 1 1 d . . . H23A H -0.6398 1.1881 0.0793 0.043 Uiso 1 1 calc R . . C24A C -0.7747(6) 1.2075(3) 0.0573(3) 0.035(2) Uani 1 1 d . . . H24C H -0.7565 1.2447 0.0631 0.042 Uiso 1 1 calc R . . O1 O -0.9982(4) 0.8883(2) -0.20719(18) 0.0380(15) Uani 1 1 d . . . O2 O -0.9136(4) 0.9941(2) -0.13398(18) 0.0381(15) Uani 1 1 d . . . O3 O -0.7205(4) 1.0750(2) -0.12832(18) 0.0356(14) Uani 1 1 d . . . O4 O -0.5284(4) 1.0837(2) -0.19856(18) 0.0388(15) Uani 1 1 d . . . O5 O -0.4388(4) 1.0291(3) -0.2898(2) 0.0470(17) Uani 1 1 d . . . O6 O -0.5155(5) 0.9238(3) -0.3565(2) 0.0544(18) Uani 1 1 d . . . O7 O -0.7335(4) 0.8339(3) -0.3595(2) 0.0535(19) Uani 1 1 d . . . O8 O -0.9273(4) 0.8240(2) -0.29923(19) 0.0372(15) Uani 1 1 d . . . O9 O -1.2346(4) 1.0359(2) -0.32344(19) 0.0412(15) Uani 1 1 d . . . O10 O -1.1312(4) 1.1449(2) -0.2540(2) 0.0407(15) Uani 1 1 d . . . O11 O -0.9352(4) 1.2277(2) -0.25044(19) 0.0436(16) Uani 1 1 d . . . O12 O -0.7301(5) 1.2527(2) -0.3138(2) 0.0496(17) Uani 1 1 d . . . O13 O -0.6329(5) 1.1944(3) -0.4072(2) 0.0572(19) Uani 1 1 d . . . O14 O -0.7329(4) 1.0907(3) -0.4614(2) 0.0518(18) Uani 1 1 d . . . O15 O -0.9435(4) 1.0066(3) -0.45843(18) 0.0418(16) Uani 1 1 d . . . O16 O -1.1622(4) 0.9789(2) -0.41374(18) 0.0408(15) Uani 1 1 d . . . N1 N -1.1184(5) 0.8898(3) -0.2617(2) 0.0357(18) Uani 1 1 d . . . N2 N -1.1162(4) 0.9436(3) -0.2082(2) 0.0279(15) Uani 1 1 d . . . N3 N -1.0559(4) 1.0147(2) -0.1625(2) 0.0290(16) Uani 1 1 d . . . N4 N -0.9653(4) 1.0793(3) -0.1377(2) 0.0295(16) Uani 1 1 d . . . N5 N -0.8360(4) 1.1321(3) -0.13476(19) 0.0274(15) Uani 1 1 d . . . N6 N -0.7168(4) 1.1566(2) -0.1570(2) 0.0281(16) Uani 1 1 d . . . N7 N -0.6056(4) 1.1605(3) -0.1996(2) 0.0326(17) Uani 1 1 d . . . N8 N -0.5146(5) 1.1517(3) -0.2445(2) 0.0342(17) Uani 1 1 d . . . N9 N -0.4472(5) 1.1192(3) -0.3000(2) 0.045(2) Uani 1 1 d . . . N10 N -0.4506(5) 1.0664(3) -0.3548(2) 0.0393(18) Uani 1 1 d . . . N11 N -0.5053(5) 0.9932(3) -0.4003(2) 0.0417(19) Uani 1 1 d . . . N12 N -0.6095(5) 0.9363(3) -0.4199(2) 0.0420(19) Uani 1 1 d . . . N13 N -0.7430(5) 0.8810(3) -0.4210(2) 0.045(2) Uani 1 1 d . . . N14 N -0.8651(5) 0.8504(3) -0.4056(2) 0.0378(18) Uani 1 1 d . . . N15 N -0.9870(5) 0.8416(3) -0.3693(2) 0.0357(17) Uani 1 1 d . . . N16 N -1.0710(4) 0.8527(3) -0.3221(2) 0.0286(16) Uani 1 1 d . . . N17 N -1.2153(4) 0.9481(3) -0.3079(2) 0.0347(17) Uani 1 1 d . . . N18 N -1.2061(4) 1.0050(3) -0.2556(2) 0.0304(16) Uani 1 1 d . . . N19 N -1.1477(4) 1.0764(3) -0.2098(2) 0.0301(16) Uani 1 1 d . . . N20 N -1.0535(4) 1.1395(3) -0.1856(2) 0.0312(16) Uani 1 1 d . . . N21 N -0.9232(4) 1.1922(3) -0.1845(2) 0.0311(16) Uani 1 1 d . . . N22 N -0.8020(5) 1.2182(3) -0.2061(2) 0.0348(17) Uani 1 1 d . . . N23 N -0.6849(4) 1.2267(3) -0.2454(2) 0.0297(16) Uani 1 1 d . . . N24 N -0.5926(5) 1.2183(3) -0.2885(2) 0.045(2) Uani 1 1 d . . . N25 N -0.5290(5) 1.1844(3) -0.3463(3) 0.049(2) Uani 1 1 d . . . N26 N -0.5213(5) 1.1353(3) -0.4030(2) 0.044(2) Uani 1 1 d . . . N27 N -0.5909(5) 1.0617(3) -0.4418(2) 0.0400(19) Uani 1 1 d . . . N28 N -0.6969(4) 1.0033(3) -0.4592(2) 0.0354(17) Uani 1 1 d . . . N29 N -0.8275(5) 0.9511(3) -0.4597(2) 0.0394(19) Uani 1 1 d . . . N30 N -0.9508(5) 0.9182(3) -0.4452(2) 0.0351(17) Uani 1 1 d . . . N31 N -1.0763(4) 0.9036(3) -0.4125(2) 0.0282(16) Uani 1 1 d . . . N32 N -1.1688(4) 0.9089(3) -0.3682(2) 0.0309(16) Uani 1 1 d . . . C1 C -1.0708(5) 0.9054(3) -0.2246(3) 0.031(2) Uani 1 1 d . . . C2 C -1.0906(5) 0.9624(3) -0.1654(2) 0.0305(19) Uani 1 1 d . . . H2A H -1.1424 0.9614 -0.1517 0.037 Uiso 1 1 calc R . . H2B H -1.0458 0.9385 -0.1498 0.037 Uiso 1 1 calc R . . C3 C -0.9732(6) 1.0266(4) -0.1437(2) 0.030(2) Uani 1 1 d . . . C4 C -0.8900(5) 1.1025(3) -0.1109(3) 0.032(2) Uani 1 1 d . . . H4A H -0.8540 1.0746 -0.0950 0.038 Uiso 1 1 calc R . . H4B H -0.9102 1.1260 -0.0905 0.038 Uiso 1 1 calc R . . C5 C -0.7565(5) 1.1171(3) -0.1392(2) 0.0281(19) Uani 1 1 d . . . C6 C -0.6242(5) 1.1568(3) -0.1571(3) 0.034(2) Uani 1 1 d . . . H6A H -0.5977 1.1243 -0.1437 0.041 Uiso 1 1 calc R . . H6B H -0.5966 1.1867 -0.1402 0.041 Uiso 1 1 calc R . . C7 C -0.5466(5) 1.1270(3) -0.2127(3) 0.033(2) Uani 1 1 d . . . C8 C -0.4332(6) 1.1332(4) -0.2564(3) 0.045(2) Uani 1 1 d . . . H8A H -0.3882 1.1611 -0.2508 0.054 Uiso 1 1 calc R . . H8B H -0.4109 1.1025 -0.2391 0.054 Uiso 1 1 calc R . . C9 C -0.4433(6) 1.0669(4) -0.3119(3) 0.041(2) Uani 1 1 d . . . C10 C -0.4296(6) 1.0189(4) -0.3761(3) 0.053(3) Uani 1 1 d . . . H10A H -0.3887 1.0279 -0.3949 0.063 Uiso 1 1 calc R . . H10B H -0.3991 0.9941 -0.3547 0.063 Uiso 1 1 calc R . . C11 C -0.5421(6) 0.9484(4) -0.3902(3) 0.042(2) Uani 1 1 d . . . C12 C -0.6501(6) 0.8809(4) -0.4230(3) 0.059(3) Uani 1 1 d . . . H12A H -0.6425 0.8648 -0.4498 0.071 Uiso 1 1 calc R . . H12B H -0.6180 0.8592 -0.3998 0.071 Uiso 1 1 calc R . . C13 C -0.7756(6) 0.8535(4) -0.3920(3) 0.046(2) Uani 1 1 d . . . C14 C -0.9199(6) 0.8150(3) -0.3861(3) 0.040(2) Uani 1 1 d . . . H14A H -0.9479 0.7892 -0.4072 0.048 Uiso 1 1 calc R . . H14B H -0.8819 0.7955 -0.3632 0.048 Uiso 1 1 calc R . . C15 C -0.9886(6) 0.8374(3) -0.3271(3) 0.032(2) Uani 1 1 d . . . C16 C -1.0980(6) 0.8429(3) -0.2825(3) 0.039(2) Uani 1 1 d . . . H16A H -1.0503 0.8240 -0.2637 0.046 Uiso 1 1 calc R . . H16B H -1.1503 0.8200 -0.2876 0.046 Uiso 1 1 calc R . . C17 C -1.2188(5) 1.0003(4) -0.2981(3) 0.033(2) Uani 1 1 d . . . C18 C -1.2225(5) 1.0523(3) -0.2350(3) 0.035(2) Uani 1 1 d . . . H18A H -1.2498 1.0777 -0.2566 0.041 Uiso 1 1 calc R . . H18B H -1.2656 1.0448 -0.2169 0.041 Uiso 1 1 calc R . . C19 C -1.1124(5) 1.1220(3) -0.2192(3) 0.032(2) Uani 1 1 d . . . C20 C -1.0156(5) 1.1920(3) -0.1830(3) 0.036(2) Uani 1 1 d . . . H20A H -1.0476 1.2133 -0.2065 0.043 Uiso 1 1 calc R . . H20B H -1.0240 1.2085 -0.1564 0.043 Uiso 1 1 calc R . . C21 C -0.8914(6) 1.2141(3) -0.2166(3) 0.034(2) Uani 1 1 d . . . C22 C -0.7526(6) 1.2520(3) -0.2284(3) 0.035(2) Uani 1 1 d . . . H22A H -0.7937 1.2688 -0.2517 0.042 Uiso 1 1 calc R . . H22B H -0.7255 1.2800 -0.2091 0.042 Uiso 1 1 calc R . . C23 C -0.6736(6) 1.2354(3) -0.2854(3) 0.038(2) Uani 1 1 d . . . C24 C -0.5535(7) 1.2305(4) -0.3267(3) 0.047(3) Uani 1 1 d . . . H24A H -0.5968 1.2503 -0.3472 0.056 Uiso 1 1 calc R . . H24B H -0.5011 1.2529 -0.3182 0.056 Uiso 1 1 calc R . . C25 C -0.5690(7) 1.1737(4) -0.3873(3) 0.047(3) Uani 1 1 d . . . C26 C -0.5488(7) 1.1114(4) -0.4428(3) 0.051(3) Uani 1 1 d . . . H26A H -0.5898 1.1354 -0.4608 0.061 Uiso 1 1 calc R . . H26B H -0.4969 1.1068 -0.4560 0.061 Uiso 1 1 calc R . . C27 C -0.6797(6) 1.0537(4) -0.4544(3) 0.041(2) Uani 1 1 d . . . C28 C -0.7807(6) 0.9864(4) -0.4834(3) 0.048(3) Uani 1 1 d . . . H28A H -0.7707 0.9683 -0.5091 0.058 Uiso 1 1 calc R . . H28B H -0.8177 1.0174 -0.4923 0.058 Uiso 1 1 calc R . . C29 C -0.9094(6) 0.9635(4) -0.4548(3) 0.035(2) Uani 1 1 d . . . C30 C -1.0448(5) 0.9152(4) -0.4512(3) 0.036(2) Uani 1 1 d . . . H30A H -1.0658 0.8877 -0.4722 0.043 Uiso 1 1 calc R . . H30B H -1.0701 0.9489 -0.4627 0.043 Uiso 1 1 calc R . . C31 C -1.1379(5) 0.9349(4) -0.3997(3) 0.032(2) Uani 1 1 d . . . C32 C -1.2427(5) 0.9283(4) -0.3510(3) 0.034(2) Uani 1 1 d . . . H32A H -1.2857 0.8997 -0.3510 0.041 Uiso 1 1 calc R . . H32B H -1.2722 0.9567 -0.3691 0.041 Uiso 1 1 calc R . . C33 C -1.2033(5) 0.9150(3) -0.2714(2) 0.0298(19) Uani 1 1 d . . . H33A H -1.2523 0.8892 -0.2728 0.036 Uiso 1 1 calc R . . C34 C -1.2008(5) 0.9543(3) -0.2351(2) 0.030(2) Uani 1 1 d . . . H34A H -1.2505 0.9487 -0.2200 0.036 Uiso 1 1 calc R . . C35 C -1.1135(5) 1.0609(3) -0.1665(3) 0.031(2) Uani 1 1 d . . . H35A H -1.1611 1.0572 -0.1498 0.038 Uiso 1 1 calc R . . C36 C -1.0478(5) 1.1063(3) -0.1494(2) 0.0289(19) Uani 1 1 d . . . H36A H -1.0648 1.1249 -0.1251 0.035 Uiso 1 1 calc R . . C37 C -0.8553(5) 1.1856(3) -0.1471(2) 0.0300(19) Uani 1 1 d . . . H37A H -0.8668 1.2075 -0.1231 0.036 Uiso 1 1 calc R . . C38 C -0.7699(5) 1.2031(3) -0.1624(2) 0.0283(19) Uani 1 1 d . . . H38A H -0.7403 1.2328 -0.1453 0.034 Uiso 1 1 calc R . . C39 C -0.6047(6) 1.2124(3) -0.2189(3) 0.034(2) Uani 1 1 d . . . H39A H -0.5839 1.2399 -0.1974 0.041 Uiso 1 1 calc R . . C40 C -0.5417(6) 1.2053(4) -0.2488(3) 0.040(2) Uani 1 1 d . . . H40A H -0.4901 1.2293 -0.2414 0.048 Uiso 1 1 calc R . . C41 C -1.1319(5) 0.8578(3) -0.3612(2) 0.0278(18) Uani 1 1 d . . . H41A H -1.1779 0.8299 -0.3650 0.033 Uiso 1 1 calc R . . C42 C -0.4483(7) 1.1563(4) -0.3341(3) 0.047(3) Uani 1 1 d . . . H42A H -0.3967 1.1804 -0.3284 0.056 Uiso 1 1 calc R . . C43 C -0.4439(7) 1.1188(4) -0.3721(3) 0.048(3) Uani 1 1 d . . . H43A H -0.3883 1.1235 -0.3830 0.058 Uiso 1 1 calc R . . C44 C -0.5470(6) 1.0110(4) -0.4420(3) 0.041(2) Uani 1 1 d . . . H44A H -0.5048 1.0110 -0.4617 0.049 Uiso 1 1 calc R . . C45 C -0.6170(6) 0.9720(4) -0.4543(3) 0.039(2) Uani 1 1 d . . . H45A H -0.6116 0.9538 -0.4809 0.047 Uiso 1 1 calc R . . C46 C -0.8093(6) 0.8959(4) -0.4568(3) 0.040(2) Uani 1 1 d . . . H46A H -0.7968 0.8814 -0.4837 0.048 Uiso 1 1 calc R . . C47 C -0.8946(6) 0.8726(4) -0.4457(3) 0.041(2) Uani 1 1 d . . . H47A H -0.9222 0.8459 -0.4667 0.049 Uiso 1 1 calc R . . C48 C -1.0717(5) 0.8538(3) -0.3940(3) 0.0289(19) Uani 1 1 d . . . H48A H -1.0922 0.8260 -0.4152 0.035 Uiso 1 1 calc R . . N1" N -0.7566(5) 0.9180(3) -0.2639(2) 0.0362(18) Uani 1 1 d . . . N2" N -0.9131(7) 1.1485(5) -0.3268(4) 0.087(4) Uani 1 1 d . . . N3" N -0.8273(5) 0.9020(3) -0.1222(2) 0.0432(19) Uani 1 1 d . . . H3"A H -0.8375 0.8781 -0.1030 0.065 Uiso 1 1 calc R . . H3"B H -0.8751 0.9231 -0.1295 0.065 Uiso 1 1 calc R . . H3"C H -0.7797 0.9217 -0.1111 0.065 Uiso 1 1 calc R . . N4" N -1.1759(9) 1.0867(5) -0.3922(4) 0.107(4) Uani 1 1 d . . . H4"A H -1.2301 1.0920 -0.4081 0.160 Uiso 1 1 calc R . . H4"B H -1.1782 1.0596 -0.3742 0.160 Uiso 1 1 calc R . . H4"C H -1.1373 1.0789 -0.4091 0.160 Uiso 1 1 calc R . . C1" C -0.6732(7) 0.9221(4) -0.2651(3) 0.050(3) Uani 1 1 d . . . H1"A H -0.6322 0.9005 -0.2472 0.060 Uiso 1 1 calc R . . C2" C -0.6426(7) 0.9573(4) -0.2918(3) 0.058(3) Uani 1 1 d . . . H2"A H -0.5814 0.9614 -0.2907 0.069 Uiso 1 1 calc R . . C3" C -0.7021(6) 0.9863(4) -0.3200(3) 0.043(2) Uani 1 1 d . . . C4" C -0.7927(6) 0.9770(4) -0.3235(3) 0.037(2) Uani 1 1 d . . . C5" C -0.8546(6) 1.0006(4) -0.3539(3) 0.040(2) Uani 1 1 d . . . H5"A H -0.8366 1.0201 -0.3756 0.048 Uiso 1 1 calc R . . C6" C -0.9416(7) 0.9958(3) -0.3529(3) 0.043(2) Uani 1 1 d . . . H6"A H -0.9842 1.0114 -0.3743 0.052 Uiso 1 1 calc R . . C7" C -0.9684(6) 0.9679(3) -0.3200(3) 0.040(2) Uani 1 1 d . . . H7"A H -1.0290 0.9667 -0.3187 0.048 Uiso 1 1 calc R . . C8" C -0.9089(6) 0.9426(3) -0.2900(3) 0.033(2) Uani 1 1 d . . . H8"A H -0.9275 0.9236 -0.2681 0.039 Uiso 1 1 calc R . . C9" C -0.8216(6) 0.9453(3) -0.2925(3) 0.035(2) Uani 1 1 d . . . C10" C -0.8725(10) 1.1611(5) -0.3576(5) 0.093(5) Uani 1 1 d . . . H10E H -0.8993 1.1844 -0.3790 0.112 Uiso 1 1 calc R . . C11" C -0.7888(9) 1.1398(6) -0.3586(6) 0.106(6) Uani 1 1 d . . . H11A H -0.7599 1.1496 -0.3807 0.127 Uiso 1 1 calc R . . C12" C -0.7494(8) 1.1062(5) -0.3295(6) 0.088(5) Uani 1 1 d . . . C13" C -0.7869(8) 1.1016(5) -0.2962(5) 0.065(3) Uani 1 1 d . . . C14" C -0.7453(10) 1.0736(6) -0.2633(6) 0.095(5) Uani 1 1 d . . . H14E H -0.6865 1.0631 -0.2631 0.114 Uiso 1 1 calc R . . C15" C -0.7846(12) 1.0587(6) -0.2283(5) 0.106(6) Uani 1 1 d . . . H15A H -0.7534 1.0389 -0.2055 0.127 Uiso 1 1 calc R . . C16" C -0.8709(14) 1.0746(7) -0.2297(5) 0.110(6) Uani 1 1 d . . . H16E H -0.8999 1.0655 -0.2074 0.132 Uiso 1 1 calc R . . C17" C -0.9141(10) 1.1034(6) -0.2629(5) 0.090(5) Uani 1 1 d . . . H17B H -0.9735 1.1134 -0.2641 0.108 Uiso 1 1 calc R . . C18" C -0.8716(8) 1.1176(5) -0.2942(4) 0.070(4) Uani 1 1 d . . . C19" C -0.6737(9) 1.0792(5) -0.3397(6) 0.119(7) Uani 1 1 d . . . H19B H -0.6251 1.1003 -0.3430 0.143 Uiso 1 1 calc R . . C20" C -0.6660(7) 1.0286(5) -0.3448(3) 0.062(3) Uani 1 1 d . . . H20D H -0.6352 1.0175 -0.3659 0.074 Uiso 1 1 calc R . . C21" C -0.7822(7) 0.8832(4) -0.2310(3) 0.044(2) Uani 1 1 d . . . H21B H -0.7367 0.8560 -0.2230 0.053 Uiso 1 1 calc R . . H21C H -0.8381 0.8655 -0.2428 0.053 Uiso 1 1 calc R . . C22" C -0.7929(6) 0.9130(3) -0.1926(3) 0.039(2) Uani 1 1 d . . . H22D H -0.7390 0.9332 -0.1817 0.047 Uiso 1 1 calc R . . H22E H -0.8426 0.9378 -0.1996 0.047 Uiso 1 1 calc R . . C23" C -0.8103(6) 0.8745(3) -0.1601(3) 0.040(2) Uani 1 1 d . . . H23B H -0.8617 0.8526 -0.1720 0.048 Uiso 1 1 calc R . . H23C H -0.7589 0.8511 -0.1522 0.048 Uiso 1 1 calc R . . C24" C -1.0090(8) 1.1674(8) -0.3336(4) 0.130(8) Uani 1 1 d . . . H24D H -1.0206 1.1948 -0.3555 0.156 Uiso 1 1 calc R . . H24E H -1.0237 1.1812 -0.3073 0.156 Uiso 1 1 calc R . . C25" C -1.0675(12) 1.1103(7) -0.3498(4) 0.107(5) Uani 1 1 d . . . H25A H -1.0386 1.0897 -0.3691 0.128 Uiso 1 1 calc R . . H25B H -1.0736 1.0882 -0.3254 0.128 Uiso 1 1 calc R . . C26" C -1.1499(15) 1.1294(8) -0.3705(8) 0.181(11) Uani 1 1 d . . . H26C H -1.1887 1.1386 -0.3506 0.218 Uiso 1 1 calc R . . H26D H -1.1443 1.1597 -0.3888 0.218 Uiso 1 1 calc R . . O1S O -0.6803(5) 0.9733(3) -0.1029(2) 0.061(2) Uiso 1 1 d . . . O2S O -1.3481(5) 0.9732(3) -0.4548(3) 0.079(2) Uiso 1 1 d . . . O3S O -1.2388(5) 0.8435(3) -0.4658(3) 0.080(2) Uiso 1 1 d . . . O4S O -1.0589(7) 1.0827(4) -0.4512(3) 0.032(3) Uiso 0.50 1 d P . . O5S O -0.4269(7) 1.1501(4) 0.0970(4) 0.039(3) Uiso 0.50 1 d P . . O6S O -0.7470(9) 1.2851(5) 0.3108(4) 0.052(3) Uiso 0.50 1 d P . . O7S O -0.4305(9) 1.1777(5) 0.3135(4) 0.055(4) Uiso 0.50 1 d P . . O8S O -0.4986(9) 1.0252(6) 0.1893(5) 0.063(4) Uiso 0.50 1 d P . . O9S O -0.6596(9) 1.2410(5) 0.1476(4) 0.058(4) Uiso 0.50 1 d P . . O10S O -0.8482(10) 1.2113(6) 0.2039(5) 0.067(4) Uiso 0.50 1 d P . . O11S O -0.7536(11) 1.2938(7) 0.1952(5) 0.084(5) Uiso 0.50 1 d P . . O12S O -0.4274(10) 1.1191(6) 0.1747(5) 0.070(4) Uiso 0.50 1 d P . . O13S O -0.4060(11) 0.9304(7) -0.2601(5) 0.086(5) Uiso 0.50 1 d P . . O14S O -0.6742(11) 1.2326(7) -0.0688(5) 0.080(5) Uiso 0.50 1 d P . . O15S O -0.5920(13) 1.1843(8) -0.0641(6) 0.099(6) Uiso 0.50 1 d P . . O16S O -1.3627(14) 0.8153(8) -0.3348(7) 0.112(7) Uiso 0.50 1 d P . . H8AA H -1.1150 0.7409 -0.0940 0.040 Uiso 1 1 d . . . H8AB H -1.0765 0.7861 -0.1169 0.040 Uiso 1 1 d . . . H16C H -0.8509 1.2334 -0.0421 0.040 Uiso 1 1 d . . . H16D H -0.8440 1.2708 -0.0040 0.040 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1A 0.042(4) 0.048(4) 0.037(4) -0.007(3) 0.017(3) 0.001(3) O2A 0.030(3) 0.040(4) 0.031(3) -0.001(3) 0.010(3) 0.007(3) O3A 0.039(4) 0.042(4) 0.035(4) -0.001(3) 0.016(3) 0.003(3) O4A 0.044(4) 0.034(4) 0.046(4) -0.002(3) 0.021(3) 0.002(3) O5A 0.051(4) 0.050(4) 0.032(4) 0.009(3) 0.017(3) 0.012(3) O6A 0.048(4) 0.044(4) 0.042(4) 0.003(3) 0.013(3) -0.011(3) O7A 0.053(4) 0.047(4) 0.032(4) 0.000(3) 0.015(3) 0.001(3) O8A 0.038(4) 0.057(4) 0.037(4) -0.011(3) 0.013(3) 0.009(3) N1A 0.022(4) 0.051(5) 0.027(4) -0.003(3) 0.009(3) 0.009(3) N2A 0.028(4) 0.037(4) 0.024(4) -0.004(3) 0.010(3) -0.002(3) N3A 0.032(4) 0.040(5) 0.035(4) 0.002(3) 0.011(3) 0.002(3) N4A 0.028(4) 0.031(4) 0.026(4) -0.007(3) 0.007(3) 0.000(3) N5A 0.032(4) 0.030(4) 0.044(5) -0.008(3) 0.020(3) -0.006(3) N6A 0.025(4) 0.031(4) 0.043(4) -0.002(3) 0.016(3) -0.001(3) N7A 0.031(4) 0.039(4) 0.033(4) 0.009(3) 0.018(3) 0.007(3) N8A 0.035(4) 0.039(4) 0.030(4) -0.009(3) 0.010(3) 0.005(3) N9A 0.028(4) 0.040(4) 0.032(4) 0.002(3) 0.015(3) 0.002(3) N10A 0.030(4) 0.044(5) 0.024(4) 0.001(3) 0.008(3) -0.001(3) N11A 0.040(5) 0.042(5) 0.025(4) 0.000(3) 0.008(3) -0.007(3) N12A 0.043(5) 0.036(4) 0.036(5) 0.005(3) 0.015(4) -0.001(3) N13A 0.033(4) 0.031(4) 0.034(4) 0.001(3) 0.015(3) 0.003(3) N14A 0.042(5) 0.030(4) 0.037(4) 0.001(3) 0.017(3) -0.004(3) N15A 0.029(4) 0.046(5) 0.029(4) -0.007(3) 0.013(3) 0.010(3) N16A 0.032(4) 0.045(5) 0.026(4) 0.001(3) 0.004(3) 0.016(3) C1A 0.042(6) 0.033(5) 0.022(5) 0.002(4) 0.011(4) 0.004(4) C2A 0.041(6) 0.033(5) 0.032(5) 0.002(4) 0.009(4) -0.003(4) C3A 0.025(5) 0.020(4) 0.039(5) 0.002(4) 0.005(4) 0.001(3) C4A 0.038(5) 0.031(5) 0.025(5) 0.003(4) 0.008(4) -0.002(4) C5A 0.023(5) 0.036(5) 0.034(5) -0.003(4) 0.007(4) 0.000(4) C6A 0.030(5) 0.043(6) 0.036(5) 0.001(4) 0.008(4) 0.004(4) C7A 0.038(5) 0.031(5) 0.026(5) -0.004(4) 0.014(4) -0.005(4) C8A 0.045(6) 0.046(6) 0.025(5) -0.005(4) 0.010(4) 0.009(4) C9A 0.044(6) 0.050(6) 0.026(5) -0.006(4) 0.016(4) 0.006(5) C10A 0.034(5) 0.042(5) 0.027(5) 0.000(4) 0.010(4) 0.000(4) C11A 0.032(5) 0.039(5) 0.032(5) 0.000(4) 0.011(4) -0.004(4) C12A 0.041(6) 0.045(6) 0.042(6) -0.001(4) 0.022(4) -0.004(4) C13A 0.027(5) 0.041(6) 0.048(6) -0.003(5) 0.019(4) -0.003(4) C14A 0.039(6) 0.044(6) 0.037(5) 0.003(4) 0.012(4) 0.005(4) C15A 0.035(5) 0.049(6) 0.038(6) -0.010(5) 0.007(4) 0.007(4) C16A 0.042(6) 0.052(6) 0.025(5) -0.003(4) 0.012(4) 0.002(4) C17A 0.035(5) 0.038(5) 0.029(5) -0.004(4) 0.010(4) 0.003(4) C18A 0.035(5) 0.026(5) 0.034(5) 0.004(4) 0.016(4) 0.001(4) C19A 0.028(5) 0.032(5) 0.039(5) -0.003(4) 0.008(4) 0.003(4) C20A 0.026(5) 0.034(5) 0.033(5) -0.003(4) 0.004(4) 0.005(4) C21A 0.027(5) 0.038(5) 0.043(6) -0.010(4) 0.009(4) -0.007(4) C22A 0.027(5) 0.042(6) 0.040(6) -0.002(4) 0.004(4) -0.003(4) C23A 0.037(5) 0.040(5) 0.033(5) -0.002(4) 0.010(4) -0.004(4) C24A 0.040(5) 0.034(5) 0.034(5) -0.003(4) 0.014(4) 0.011(4) O1 0.039(4) 0.042(4) 0.034(4) -0.003(3) 0.011(3) 0.001(3) O2 0.034(4) 0.034(4) 0.046(4) -0.004(3) 0.008(3) -0.001(3) O3 0.040(4) 0.031(4) 0.038(4) 0.008(3) 0.014(3) -0.003(3) O4 0.042(4) 0.029(4) 0.045(4) 0.001(3) 0.005(3) 0.001(3) O5 0.046(4) 0.055(5) 0.041(4) 0.002(3) 0.011(3) 0.016(3) O6 0.062(5) 0.057(5) 0.042(4) 0.009(3) 0.002(3) 0.022(4) O7 0.032(4) 0.064(5) 0.062(5) 0.028(4) 0.004(3) 0.002(3) O8 0.035(4) 0.028(3) 0.044(4) -0.006(3) -0.004(3) 0.006(3) O9 0.037(4) 0.046(4) 0.039(4) -0.002(3) 0.003(3) 0.006(3) O10 0.036(4) 0.036(4) 0.049(4) 0.002(3) 0.005(3) 0.006(3) O11 0.036(4) 0.056(4) 0.038(4) 0.009(3) 0.006(3) -0.001(3) O12 0.067(5) 0.038(4) 0.046(4) 0.009(3) 0.018(4) 0.005(3) O13 0.065(5) 0.047(5) 0.060(5) 0.015(4) 0.014(4) -0.001(4) O14 0.041(4) 0.056(5) 0.063(5) 0.009(4) 0.021(3) 0.001(3) O15 0.043(4) 0.049(4) 0.035(4) 0.009(3) 0.009(3) 0.008(3) O16 0.044(4) 0.046(4) 0.035(4) 0.009(3) 0.013(3) 0.013(3) N1 0.035(4) 0.042(5) 0.027(4) -0.012(3) -0.002(3) 0.013(3) N2 0.031(4) 0.031(4) 0.024(4) -0.003(3) 0.010(3) 0.002(3) N3 0.029(4) 0.023(4) 0.038(4) -0.004(3) 0.015(3) 0.000(3) N4 0.023(4) 0.031(4) 0.037(4) -0.001(3) 0.014(3) -0.001(3) N5 0.031(4) 0.031(4) 0.022(4) -0.001(3) 0.011(3) -0.002(3) N6 0.028(4) 0.024(4) 0.032(4) 0.006(3) 0.007(3) -0.004(3) N7 0.037(4) 0.030(4) 0.033(4) 0.007(3) 0.013(3) -0.007(3) N8 0.040(4) 0.033(4) 0.032(4) 0.005(3) 0.013(3) 0.003(3) N9 0.052(5) 0.058(6) 0.027(4) 0.000(4) 0.014(4) 0.005(4) N10 0.033(4) 0.052(5) 0.035(5) -0.005(4) 0.011(3) 0.005(4) N11 0.028(4) 0.069(6) 0.028(4) -0.005(4) 0.005(3) 0.004(4) N12 0.044(5) 0.043(5) 0.039(5) 0.005(4) 0.007(4) 0.000(4) N13 0.033(5) 0.052(5) 0.054(5) 0.014(4) 0.017(4) -0.001(4) N14 0.031(4) 0.041(5) 0.042(5) 0.013(4) 0.011(3) 0.002(3) N15 0.034(4) 0.034(4) 0.039(5) -0.004(3) 0.007(3) 0.004(3) N16 0.035(4) 0.027(4) 0.023(4) -0.005(3) 0.004(3) -0.003(3) N17 0.026(4) 0.044(5) 0.035(4) -0.001(3) 0.008(3) 0.007(3) N18 0.029(4) 0.030(4) 0.031(4) -0.008(3) 0.001(3) 0.000(3) N19 0.026(4) 0.037(4) 0.027(4) -0.005(3) 0.004(3) -0.004(3) N20 0.033(4) 0.029(4) 0.033(4) -0.002(3) 0.010(3) -0.002(3) N21 0.033(4) 0.036(4) 0.027(4) -0.002(3) 0.012(3) -0.004(3) N22 0.029(4) 0.039(5) 0.036(4) 0.007(3) 0.006(3) -0.002(3) N23 0.031(4) 0.034(4) 0.024(4) 0.010(3) 0.005(3) 0.005(3) N24 0.055(5) 0.043(5) 0.041(5) 0.010(4) 0.021(4) 0.001(4) N25 0.051(5) 0.057(6) 0.043(5) 0.012(4) 0.018(4) 0.006(4) N26 0.041(5) 0.054(5) 0.037(5) 0.006(4) 0.008(4) -0.001(4) N27 0.037(5) 0.044(5) 0.040(5) 0.008(4) 0.010(4) -0.001(4) N28 0.029(4) 0.034(5) 0.045(5) 0.007(3) 0.010(3) 0.000(3) N29 0.030(4) 0.052(5) 0.038(5) 0.007(4) 0.013(3) -0.003(4) N30 0.034(4) 0.042(5) 0.032(4) 0.007(3) 0.013(3) 0.002(3) N31 0.026(4) 0.032(4) 0.027(4) -0.001(3) 0.007(3) 0.005(3) N32 0.024(4) 0.043(5) 0.027(4) 0.005(3) 0.007(3) 0.004(3) C1 0.025(5) 0.038(5) 0.032(5) 0.000(4) 0.011(4) -0.001(4) C2 0.031(5) 0.035(5) 0.028(5) -0.001(4) 0.011(4) -0.004(4) C3 0.030(5) 0.044(6) 0.018(4) 0.001(4) 0.005(4) 0.002(4) C4 0.036(5) 0.031(5) 0.032(5) 0.000(4) 0.016(4) -0.008(4) C5 0.032(5) 0.028(5) 0.026(5) 0.001(4) 0.009(4) -0.001(4) C6 0.029(5) 0.041(5) 0.036(5) 0.005(4) 0.014(4) -0.006(4) C7 0.026(5) 0.032(5) 0.042(5) -0.008(4) 0.007(4) -0.001(4) C8 0.045(6) 0.060(7) 0.034(6) -0.007(5) 0.015(4) 0.006(5) C9 0.032(5) 0.065(7) 0.029(5) -0.001(5) 0.012(4) 0.000(5) C10 0.042(6) 0.074(8) 0.045(6) -0.011(5) 0.016(5) 0.015(5) C11 0.038(6) 0.045(6) 0.043(6) -0.001(5) 0.009(5) 0.004(5) C12 0.038(6) 0.081(9) 0.061(7) 0.001(6) 0.015(5) 0.014(6) C13 0.025(5) 0.047(6) 0.066(7) 0.007(5) 0.010(5) 0.002(4) C14 0.035(5) 0.037(5) 0.052(6) 0.005(4) 0.021(5) 0.006(4) C15 0.038(6) 0.024(5) 0.037(6) -0.004(4) 0.012(4) 0.001(4) C16 0.043(6) 0.034(5) 0.041(6) 0.006(4) 0.012(4) 0.012(4) C17 0.017(4) 0.036(6) 0.043(6) 0.005(4) -0.001(4) 0.000(4) C18 0.025(5) 0.039(5) 0.038(5) -0.001(4) 0.002(4) 0.002(4) C19 0.025(5) 0.036(5) 0.034(5) -0.001(4) 0.006(4) 0.017(4) C20 0.031(5) 0.034(5) 0.046(6) -0.003(4) 0.016(4) -0.001(4) C21 0.042(6) 0.027(5) 0.032(5) 0.001(4) 0.005(4) 0.001(4) C22 0.041(6) 0.026(5) 0.040(5) 0.004(4) 0.013(4) -0.006(4) C23 0.041(6) 0.035(5) 0.041(6) 0.013(4) 0.015(5) 0.002(4) C24 0.059(7) 0.044(6) 0.045(6) 0.012(5) 0.030(5) 0.005(5) C25 0.043(6) 0.051(7) 0.050(7) 0.021(5) 0.016(5) -0.011(5) C26 0.051(7) 0.068(7) 0.034(6) 0.016(5) 0.011(5) -0.006(5) C27 0.036(6) 0.060(7) 0.031(5) 0.011(5) 0.016(4) 0.009(5) C28 0.049(6) 0.058(7) 0.039(6) 0.014(5) 0.010(5) 0.001(5) C29 0.033(5) 0.051(6) 0.022(5) 0.003(4) 0.004(4) 0.000(5) C30 0.027(5) 0.056(6) 0.025(5) 0.010(4) 0.006(4) -0.002(4) C31 0.022(5) 0.046(6) 0.024(5) -0.005(4) -0.007(4) -0.006(4) C32 0.023(5) 0.049(6) 0.031(5) 0.003(4) 0.007(4) -0.001(4) C33 0.027(5) 0.032(5) 0.031(5) -0.002(4) 0.007(4) -0.003(4) C34 0.028(5) 0.039(5) 0.025(5) -0.010(4) 0.008(4) -0.005(4) C35 0.027(5) 0.032(5) 0.037(5) -0.006(4) 0.011(4) 0.003(4) C36 0.035(5) 0.026(5) 0.029(5) -0.005(4) 0.014(4) -0.003(4) C37 0.039(5) 0.029(5) 0.023(5) -0.004(3) 0.010(4) -0.003(4) C38 0.027(5) 0.029(5) 0.028(5) -0.001(4) 0.003(4) -0.001(4) C39 0.039(5) 0.032(5) 0.035(5) -0.001(4) 0.014(4) -0.010(4) C40 0.037(6) 0.046(6) 0.038(6) 0.001(4) 0.011(4) -0.003(4) C41 0.020(4) 0.032(5) 0.030(5) -0.005(4) 0.001(3) -0.002(3) C42 0.053(7) 0.062(7) 0.029(5) -0.009(5) 0.017(5) -0.015(5) C43 0.051(7) 0.056(7) 0.047(6) -0.005(5) 0.036(5) -0.017(5) C44 0.032(5) 0.066(7) 0.026(5) 0.003(4) 0.011(4) 0.002(5) C45 0.039(6) 0.053(6) 0.028(5) 0.001(4) 0.011(4) 0.001(5) C46 0.029(5) 0.062(7) 0.032(5) -0.002(4) 0.010(4) 0.003(4) C47 0.036(5) 0.044(6) 0.044(6) -0.001(4) 0.011(4) 0.007(4) C48 0.022(5) 0.031(5) 0.030(5) -0.002(4) -0.003(4) 0.002(3) N1" 0.031(4) 0.045(5) 0.031(4) -0.005(3) 0.003(3) 0.002(3) N2" 0.045(6) 0.151(11) 0.069(8) -0.045(8) 0.020(6) 0.007(7) N3" 0.051(5) 0.034(4) 0.049(5) 0.009(4) 0.021(4) 0.007(4) N4" 0.138(11) 0.100(10) 0.090(9) 0.019(8) 0.042(8) 0.017(8) C1" 0.040(6) 0.069(8) 0.042(6) -0.008(5) 0.009(5) 0.010(5) C2" 0.052(7) 0.072(8) 0.055(7) -0.018(6) 0.024(6) -0.010(6) C3" 0.037(6) 0.057(7) 0.040(6) -0.006(5) 0.019(5) 0.003(5) C4" 0.042(6) 0.044(6) 0.028(5) -0.007(4) 0.011(4) 0.007(4) C5" 0.046(6) 0.045(6) 0.031(5) -0.011(4) 0.010(4) -0.010(5) C6" 0.054(7) 0.035(6) 0.041(6) -0.005(4) 0.009(5) 0.003(5) C7" 0.028(5) 0.038(6) 0.053(6) -0.009(5) 0.004(4) -0.009(4) C8" 0.037(5) 0.027(5) 0.036(5) 0.001(4) 0.011(4) 0.000(4) C9" 0.036(5) 0.037(5) 0.029(5) -0.003(4) 0.000(4) -0.003(4) C10" 0.089(11) 0.070(10) 0.119(13) -0.026(9) 0.014(10) 0.004(8) C11" 0.073(10) 0.077(10) 0.191(17) 0.002(11) 0.084(11) 0.001(8) C12" 0.053(8) 0.051(8) 0.176(15) 0.040(9) 0.060(9) 0.011(6) C13" 0.051(8) 0.048(7) 0.091(10) -0.019(7) 0.003(7) -0.005(6) C14" 0.086(11) 0.070(10) 0.135(15) -0.061(10) 0.034(11) -0.026(8) C15" 0.106(13) 0.095(12) 0.103(13) -0.080(10) -0.012(10) 0.020(10) C16" 0.151(17) 0.128(15) 0.057(10) -0.052(10) 0.038(11) -0.029(13) C17" 0.079(10) 0.109(12) 0.092(11) -0.059(10) 0.038(9) -0.004(8) C18" 0.043(7) 0.099(10) 0.067(9) -0.040(7) 0.009(7) -0.011(7) C19" 0.064(9) 0.061(10) 0.26(2) 0.022(11) 0.098(12) 0.002(7) C20" 0.061(8) 0.075(9) 0.061(7) -0.001(6) 0.042(6) -0.008(6) C21" 0.054(6) 0.037(6) 0.037(6) 0.000(4) -0.002(5) -0.004(4) C22" 0.040(6) 0.038(6) 0.038(5) 0.004(4) 0.003(4) -0.007(4) C23" 0.035(5) 0.038(6) 0.046(6) 0.005(4) 0.005(4) -0.003(4) C24" 0.054(9) 0.26(2) 0.075(10) -0.067(12) 0.019(7) 0.041(11) C25" 0.115(14) 0.156(17) 0.057(9) -0.018(10) 0.033(9) 0.005(12) C26" 0.15(2) 0.135(18) 0.25(3) -0.127(19) 0.021(19) -0.027(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl2 O23 1.522(15) . ? Cl2 O24 1.561(18) . ? Cl2 O21 1.569(16) . ? Cl2 O22 1.623(16) . ? O1A C1A 1.213(9) . ? O2A C3A 1.199(9) . ? O3A C5A 1.212(9) . ? O4A C7A 1.228(9) . ? O5A C9A 1.206(10) . ? O6A C11A 1.223(10) . ? O7A C13A 1.218(10) . ? O8A C15A 1.220(10) . ? N1A C1A 1.399(10) . ? N1A C17A 1.450(10) . ? N1A C16A 1.450(11) 3_375 ? N2A C1A 1.332(10) . ? N2A C2A 1.452(10) . ? N2A C18A 1.466(10) . ? N3A C3A 1.397(10) . ? N3A C19A 1.436(10) . ? N3A C2A 1.457(10) . ? N4A C3A 1.370(10) . ? N4A C4A 1.451(10) . ? N4A C20A 1.436(10) . ? N5A C5A 1.359(10) . ? N5A C21A 1.443(10) . ? N5A C4A 1.451(10) . ? N6A C5A 1.347(10) . ? N6A C22A 1.439(10) . ? N6A C6A 1.479(10) . ? N7A C7A 1.353(10) . ? N7A C6A 1.443(10) . ? N7A C23A 1.466(10) . ? N8A C7A 1.370(11) . ? N8A C8A 1.450(11) 3_375 ? N8A C24A 1.459(11) . ? N9A C9A 1.363(11) . ? N9A C8A 1.431(11) . ? N9A C17A 1.440(10) . ? N10A C9A 1.392(11) . ? N10A C18A 1.433(10) . ? N10A C10A 1.471(10) . ? N11A C11A 1.340(11) . ? N11A C10A 1.439(10) . ? N11A C19A 1.456(11) . ? N12A C11A 1.367(11) . ? N12A C20A 1.422(10) . ? N12A C12A 1.473(11) . ? N13A C13A 1.349(11) . ? N13A C12A 1.421(11) . ? N13A C21A 1.466(11) . ? N14A C13A 1.378(11) . ? N14A C22A 1.430(11) . ? N14A C14A 1.466(11) . ? N15A C15A 1.381(11) . ? N15A C14A 1.421(10) . ? N15A C23A 1.481(10) . ? N16A C15A 1.366(11) . ? N16A C16A 1.439(11) . ? N16A C24A 1.450(10) . ? C8A N8A 1.450(11) 3_375 ? C16A N1A 1.450(11) 3_375 ? C17A C18A 1.554(12) . ? C19A C20A 1.550(12) . ? C21A C22A 1.536(12) . ? C23A C24A 1.551(12) . ? O1 C1 1.240(9) . ? O2 C3 1.239(10) . ? O3 C5 1.233(9) . ? O4 C7 1.211(10) . ? O5 C9 1.198(11) . ? O6 C11 1.259(11) . ? O7 C13 1.235(11) . ? O8 C15 1.229(10) . ? O9 C17 1.220(10) . ? O10 C19 1.257(10) . ? O11 C21 1.225(10) . ? O12 C23 1.227(10) . ? O13 C25 1.197(11) . ? O14 C27 1.247(11) . ? O15 C29 1.218(10) . ? O16 C31 1.247(10) . ? N1 C1 1.348(10) . ? N1 C33 1.446(10) . ? N1 C16 1.440(10) . ? N2 C1 1.369(10) . ? N2 C2 1.452(10) . ? N2 C34 1.456(10) . ? N3 C3 1.347(10) . ? N3 C2 1.436(10) . ? N3 C35 1.473(10) . ? N4 C3 1.362(10) . ? N4 C36 1.440(10) . ? N4 C4 1.445(10) . ? N5 C5 1.325(10) . ? N5 C37 1.439(10) . ? N5 C4 1.456(10) . ? N6 C5 1.369(10) . ? N6 C38 1.438(10) . ? N6 C6 1.437(10) . ? N7 C7 1.377(10) . ? N7 C39 1.468(10) . ? N7 C6 1.467(10) . ? N8 C7 1.382(11) . ? N8 C40 1.432(11) . ? N8 C8 1.468(11) . ? N9 C9 1.397(12) . ? N9 C8 1.433(11) . ? N9 C42 1.454(12) . ? N10 C9 1.375(11) . ? N10 C10 1.464(11) . ? N10 C43 1.464(12) . ? N11 C11 1.349(12) . ? N11 C10 1.440(12) . ? N11 C44 1.455(11) . ? N12 C11 1.317(11) . ? N12 C45 1.429(11) . ? N12 C12 1.546(13) . ? N13 C13 1.348(12) . ? N13 C46 1.448(11) . ? N13 C12 1.456(12) . ? N14 C13 1.378(11) . ? N14 C47 1.413(11) . ? N14 C14 1.466(10) . ? N15 C15 1.377(11) . ? N15 C14 1.435(10) . ? N15 C48 1.437(10) . ? N16 C15 1.377(10) . ? N16 C41 1.434(10) . ? N16 C16 1.448(10) . ? N17 C17 1.375(11) . ? N17 C33 1.441(10) . ? N17 C32 1.470(10) . ? N18 C17 1.359(11) . ? N18 C18 1.429(10) . ? N18 C34 1.452(10) . ? N19 C19 1.346(11) . ? N19 C18 1.425(10) . ? N19 C35 1.459(10) . ? N20 C19 1.358(10) . ? N20 C36 1.438(10) . ? N20 C20 1.460(10) . ? N21 C21 1.354(10) . ? N21 C20 1.446(10) . ? N21 C37 1.458(10) . ? N22 C21 1.369(11) . ? N22 C22 1.439(10) . ? N22 C38 1.462(10) . ? N23 C23 1.361(10) . ? N23 C39 1.420(11) . ? N23 C22 1.431(10) . ? N24 C23 1.353(11) . ? N24 C40 1.415(11) . ? N24 C24 1.512(11) . ? N25 C25 1.385(13) . ? N25 C42 1.433(12) . ? N25 C24 1.426(12) . ? N26 C25 1.384(13) . ? N26 C26 1.417(12) . ? N26 C43 1.471(13) . ? N27 C27 1.376(11) . ? N27 C26 1.431(12) . ? N27 C44 1.465(12) . ? N28 C27 1.319(12) . ? N28 C28 1.451(12) . ? N28 C45 1.458(11) . ? N29 C29 1.348(11) . ? N29 C46 1.440(12) . ? N29 C28 1.465(11) . ? N30 C29 1.388(11) . ? N30 C30 1.436(10) . ? N30 C47 1.459(11) . ? N31 C31 1.369(10) . ? N31 C48 1.405(10) . ? N31 C30 1.465(10) . ? N32 C31 1.378(10) . ? N32 C41 1.428(10) . ? N32 C32 1.457(10) . ? C33 C34 1.542(11) . ? C35 C36 1.573(11) . ? C37 C38 1.567(11) . ? C39 C40 1.516(12) . ? C41 C48 1.548(11) . ? C42 C43 1.574(13) . ? C44 C45 1.473(13) . ? C46 C47 1.556(12) . ? N1" C1" 1.306(11) . ? N1" C9" 1.417(11) . ? N1" C21" 1.500(11) . ? N2" C10" 1.318(18) . ? N2" C18" 1.377(17) . ? N2" C24" 1.540(16) . ? N3" C23" 1.482(11) . ? N4" C26" 1.320(18) . ? C1" C2" 1.396(14) . ? C2" C3" 1.383(14) . ? C3" C4" 1.409(12) . ? C3" C20" 1.518(14) . ? C4" C5" 1.377(12) . ? C4" C9" 1.430(12) . ? C5" C6" 1.361(12) . ? C6" C7" 1.409(13) . ? C7" C8" 1.371(12) . ? C8" C9" 1.374(12) . ? C10" C11" 1.414(18) . ? C11" C12" 1.34(2) . ? C12" C13" 1.327(18) . ? C12" C19" 1.454(17) . ? C13" C14" 1.344(19) . ? C13" C18" 1.390(16) . ? C14" C15" 1.44(2) . ? C15" C16" 1.39(2) . ? C16" C17" 1.37(2) . ? C17" C18" 1.362(18) . ? C19" C20" 1.314(16) . ? C21" C22" 1.496(12) . ? C22" C23" 1.507(12) . ? C24" C25" 1.75(2) . ? C25" C26" 1.41(2) . ? O14S O15S 1.76(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O23 Cl2 O24 117.4(16) . . ? O23 Cl2 O21 104.9(11) . . ? O24 Cl2 O21 119.1(16) . . ? O23 Cl2 O22 109.0(11) . . ? O24 Cl2 O22 101.1(14) . . ? O21 Cl2 O22 104.2(11) . . ? C1A N1A C17A 112.2(7) . . ? C1A N1A C16A 121.1(6) . 3_375 ? C17A N1A C16A 122.3(7) . 3_375 ? C1A N2A C2A 122.2(7) . . ? C1A N2A C18A 113.9(7) . . ? C2A N2A C18A 122.1(6) . . ? C3A N3A C19A 113.2(7) . . ? C3A N3A C2A 121.2(7) . . ? C19A N3A C2A 123.2(7) . . ? C3A N4A C4A 119.2(7) . . ? C3A N4A C20A 113.0(7) . . ? C4A N4A C20A 121.6(7) . . ? C5A N5A C21A 112.6(7) . . ? C5A N5A C4A 123.2(7) . . ? C21A N5A C4A 122.8(7) . . ? C5A N6A C22A 112.7(7) . . ? C5A N6A C6A 121.8(7) . . ? C22A N6A C6A 122.0(7) . . ? C7A N7A C6A 123.6(7) . . ? C7A N7A C23A 111.5(7) . . ? C6A N7A C23A 121.6(7) . . ? C7A N8A C8A 122.7(7) . 3_375 ? C7A N8A C24A 110.7(7) . . ? C8A N8A C24A 121.2(7) 3_375 . ? C9A N9A C8A 122.5(7) . . ? C9A N9A C17A 112.5(7) . . ? C8A N9A C17A 123.4(7) . . ? C9A N10A C18A 111.7(7) . . ? C9A N10A C10A 121.8(7) . . ? C18A N10A C10A 120.9(7) . . ? C11A N11A C10A 123.1(7) . . ? C11A N11A C19A 111.7(7) . . ? C10A N11A C19A 122.3(7) . . ? C11A N12A C20A 112.6(7) . . ? C11A N12A C12A 124.2(7) . . ? C20A N12A C12A 122.6(7) . . ? C13A N13A C12A 122.1(7) . . ? C13A N13A C21A 112.3(7) . . ? C12A N13A C21A 122.8(7) . . ? C13A N14A C22A 112.2(7) . . ? C13A N14A C14A 122.3(7) . . ? C22A N14A C14A 123.4(7) . . ? C15A N15A C14A 122.5(7) . . ? C15A N15A C23A 109.9(7) . . ? C14A N15A C23A 121.6(7) . . ? C15A N16A C16A 122.1(7) . . ? C15A N16A C24A 112.7(7) . . ? C16A N16A C24A 121.7(7) . . ? O1A C1A N2A 127.4(8) . . ? O1A C1A N1A 125.0(8) . . ? N2A C1A N1A 107.6(7) . . ? N2A C2A N3A 113.5(7) . . ? O2A C3A N4A 128.2(8) . . ? O2A C3A N3A 125.5(7) . . ? N4A C3A N3A 106.3(7) . . ? N4A C4A N5A 113.6(7) . . ? O3A C5A N6A 126.5(8) . . ? O3A C5A N5A 125.4(8) . . ? N6A C5A N5A 108.1(7) . . ? N7A C6A N6A 112.7(7) . . ? O4A C7A N7A 125.8(8) . . ? O4A C7A N8A 124.3(8) . . ? N7A C7A N8A 109.9(7) . . ? N9A C8A N8A 114.4(7) . 3_375 ? O5A C9A N9A 126.0(9) . . ? O5A C9A N10A 125.8(9) . . ? N9A C9A N10A 108.1(7) . . ? N11A C10A N10A 113.0(7) . . ? O6A C11A N11A 126.4(8) . . ? O6A C11A N12A 124.5(8) . . ? N11A C11A N12A 109.1(7) . . ? N13A C12A N12A 115.6(7) . . ? O7A C13A N13A 126.0(8) . . ? O7A C13A N14A 125.9(9) . . ? N13A C13A N14A 108.1(8) . . ? N15A C14A N14A 114.8(7) . . ? O8A C15A N16A 126.4(9) . . ? O8A C15A N15A 124.3(8) . . ? N16A C15A N15A 109.3(7) . . ? N16A C16A N1A 113.3(7) . 3_375 ? N9A C17A N1A 114.5(7) . . ? N9A C17A C18A 103.5(6) . . ? N1A C17A C18A 103.1(6) . . ? N10A C18A N2A 113.8(7) . . ? N10A C18A C17A 103.7(7) . . ? N2A C18A C17A 102.6(6) . . ? N3A C19A N11A 115.0(7) . . ? N3A C19A C20A 102.8(7) . . ? N11A C19A C20A 103.0(7) . . ? N12A C20A N4A 114.8(7) . . ? N12A C20A C19A 103.2(7) . . ? N4A C20A C19A 103.8(6) . . ? N5A C21A N13A 114.7(7) . . ? N5A C21A C22A 102.8(7) . . ? N13A C21A C22A 102.7(7) . . ? N14A C22A N6A 115.7(7) . . ? N14A C22A C21A 104.2(7) . . ? N6A C22A C21A 103.5(7) . . ? N7A C23A N15A 113.1(7) . . ? N7A C23A C24A 103.0(6) . . ? N15A C23A C24A 104.1(7) . . ? N16A C24A N8A 113.9(7) . . ? N16A C24A C23A 103.1(6) . . ? N8A C24A C23A 103.8(7) . . ? C1 N1 C33 112.4(7) . . ? C1 N1 C16 122.3(7) . . ? C33 N1 C16 122.8(7) . . ? C1 N2 C2 122.7(7) . . ? C1 N2 C34 111.9(6) . . ? C2 N2 C34 124.2(6) . . ? C3 N3 C2 123.6(7) . . ? C3 N3 C35 111.5(7) . . ? C2 N3 C35 121.8(7) . . ? C3 N4 C36 112.7(7) . . ? C3 N4 C4 122.2(7) . . ? C36 N4 C4 122.5(7) . . ? C5 N5 C37 113.2(6) . . ? C5 N5 C4 123.2(7) . . ? C37 N5 C4 122.0(7) . . ? C5 N6 C38 111.5(6) . . ? C5 N6 C6 122.3(7) . . ? C38 N6 C6 123.3(6) . . ? C7 N7 C39 111.7(7) . . ? C7 N7 C6 120.8(7) . . ? C39 N7 C6 118.5(7) . . ? C7 N8 C40 111.6(7) . . ? C7 N8 C8 120.1(7) . . ? C40 N8 C8 122.2(7) . . ? C9 N9 C8 120.4(8) . . ? C9 N9 C42 114.0(7) . . ? C8 N9 C42 124.4(8) . . ? C9 N10 C10 120.1(8) . . ? C9 N10 C43 112.4(8) . . ? C10 N10 C43 122.8(7) . . ? C11 N11 C10 126.2(8) . . ? C11 N11 C44 111.1(8) . . ? C10 N11 C44 122.4(8) . . ? C11 N12 C45 110.9(8) . . ? C11 N12 C12 121.3(8) . . ? C45 N12 C12 124.2(8) . . ? C13 N13 C46 113.2(8) . . ? C13 N13 C12 122.6(8) . . ? C46 N13 C12 121.5(8) . . ? C13 N14 C47 113.7(7) . . ? C13 N14 C14 122.0(8) . . ? C47 N14 C14 122.3(7) . . ? C15 N15 C14 119.5(7) . . ? C15 N15 C48 112.5(7) . . ? C14 N15 C48 122.9(7) . . ? C15 N16 C41 113.1(6) . . ? C15 N16 C16 119.2(7) . . ? C41 N16 C16 123.1(7) . . ? C17 N17 C33 112.6(7) . . ? C17 N17 C32 122.5(7) . . ? C33 N17 C32 123.2(7) . . ? C17 N18 C18 123.0(7) . . ? C17 N18 C34 111.7(7) . . ? C18 N18 C34 122.8(7) . . ? C19 N19 C18 124.5(7) . . ? C19 N19 C35 111.3(7) . . ? C18 N19 C35 122.7(7) . . ? C19 N20 C36 112.7(7) . . ? C19 N20 C20 123.5(7) . . ? C36 N20 C20 122.3(7) . . ? C21 N21 C20 122.6(7) . . ? C21 N21 C37 112.2(7) . . ? C20 N21 C37 122.2(7) . . ? C21 N22 C22 122.2(7) . . ? C21 N22 C38 111.2(7) . . ? C22 N22 C38 122.2(7) . . ? C23 N23 C39 111.3(7) . . ? C23 N23 C22 122.1(7) . . ? C39 N23 C22 120.3(7) . . ? C23 N24 C40 112.0(7) . . ? C23 N24 C24 121.2(8) . . ? C40 N24 C24 123.5(8) . . ? C25 N25 C42 112.0(8) . . ? C25 N25 C24 118.9(9) . . ? C42 N25 C24 125.8(9) . . ? C25 N26 C26 123.4(9) . . ? C25 N26 C43 112.2(8) . . ? C26 N26 C43 124.1(8) . . ? C27 N27 C26 124.1(8) . . ? C27 N27 C44 107.9(8) . . ? C26 N27 C44 124.8(8) . . ? C27 N28 C28 119.7(8) . . ? C27 N28 C45 112.0(7) . . ? C28 N28 C45 123.4(8) . . ? C29 N29 C46 113.5(7) . . ? C29 N29 C28 119.4(8) . . ? C46 N29 C28 121.8(7) . . ? C29 N30 C30 121.0(7) . . ? C29 N30 C47 111.1(7) . . ? C30 N30 C47 123.3(7) . . ? C31 N31 C48 112.4(7) . . ? C31 N31 C30 120.7(7) . . ? C48 N31 C30 123.5(7) . . ? C31 N32 C41 111.9(7) . . ? C31 N32 C32 122.2(7) . . ? C41 N32 C32 124.8(7) . . ? O1 C1 N1 126.6(8) . . ? O1 C1 N2 124.4(8) . . ? N1 C1 N2 108.9(7) . . ? N3 C2 N2 113.6(6) . . ? O2 C3 N3 124.2(8) . . ? O2 C3 N4 125.8(8) . . ? N3 C3 N4 109.9(7) . . ? N4 C4 N5 112.1(6) . . ? O3 C5 N5 127.1(7) . . ? O3 C5 N6 123.2(7) . . ? N5 C5 N6 109.6(7) . . ? N6 C6 N7 112.3(7) . . ? O4 C7 N8 127.5(8) . . ? O4 C7 N7 124.9(8) . . ? N8 C7 N7 107.6(7) . . ? N9 C8 N8 111.4(7) . . ? O5 C9 N10 125.6(10) . . ? O5 C9 N9 127.4(8) . . ? N10 C9 N9 106.9(8) . . ? N11 C10 N10 113.8(8) . . ? O6 C11 N12 126.9(9) . . ? O6 C11 N11 123.6(9) . . ? N12 C11 N11 109.5(8) . . ? N13 C12 N12 113.0(8) . . ? O7 C13 N13 126.8(9) . . ? O7 C13 N14 126.0(9) . . ? N13 C13 N14 107.2(8) . . ? N15 C14 N14 113.3(7) . . ? O8 C15 N16 126.8(8) . . ? O8 C15 N15 126.5(8) . . ? N16 C15 N15 106.7(7) . . ? N16 C16 N1 113.5(7) . . ? O9 C17 N18 126.2(8) . . ? O9 C17 N17 125.3(8) . . ? N18 C17 N17 108.4(7) . . ? N19 C18 N18 115.9(7) . . ? O10 C19 N19 124.8(8) . . ? O10 C19 N20 125.0(8) . . ? N19 C19 N20 110.2(7) . . ? N21 C20 N20 113.2(7) . . ? O11 C21 N21 125.8(8) . . ? O11 C21 N22 124.3(8) . . ? N21 C21 N22 109.9(8) . . ? N23 C22 N22 115.2(7) . . ? O12 C23 N24 127.0(8) . . ? O12 C23 N23 124.9(8) . . ? N24 C23 N23 108.0(8) . . ? N25 C24 N24 112.2(7) . . ? O13 C25 N25 127.1(11) . . ? O13 C25 N26 124.2(10) . . ? N25 C25 N26 108.7(9) . . ? N27 C26 N26 115.0(7) . . ? O14 C27 N28 127.4(9) . . ? O14 C27 N27 122.2(10) . . ? N28 C27 N27 110.4(8) . . ? N28 C28 N29 112.5(7) . . ? O15 C29 N29 127.0(9) . . ? O15 C29 N30 124.4(8) . . ? N29 C29 N30 108.6(8) . . ? N30 C30 N31 113.0(7) . . ? O16 C31 N32 125.6(8) . . ? O16 C31 N31 126.6(8) . . ? N32 C31 N31 107.9(7) . . ? N32 C32 N17 112.2(6) . . ? N17 C33 N1 114.2(7) . . ? N17 C33 C34 103.0(6) . . ? N1 C33 C34 103.7(6) . . ? N2 C34 N18 114.0(6) . . ? N2 C34 C33 102.9(6) . . ? N18 C34 C33 104.0(6) . . ? N19 C35 N3 113.9(6) . . ? N19 C35 C36 103.3(6) . . ? N3 C35 C36 102.7(6) . . ? N20 C36 N4 114.3(6) . . ? N20 C36 C35 102.4(6) . . ? N4 C36 C35 102.9(6) . . ? N5 C37 N21 114.9(6) . . ? N5 C37 C38 102.4(6) . . ? N21 C37 C38 102.8(6) . . ? N6 C38 N22 114.7(6) . . ? N6 C38 C37 103.1(6) . . ? N22 C38 C37 103.4(6) . . ? N23 C39 N7 114.3(7) . . ? N23 C39 C40 103.9(7) . . ? N7 C39 C40 103.0(7) . . ? N24 C40 N8 114.6(7) . . ? N24 C40 C39 103.8(7) . . ? N8 C40 C39 105.4(7) . . ? N32 C41 N16 113.7(6) . . ? N32 C41 C48 103.2(6) . . ? N16 C41 C48 102.6(6) . . ? N25 C42 N9 114.7(7) . . ? N25 C42 C43 104.8(8) . . ? N9 C42 C43 101.8(8) . . ? N10 C43 N26 114.5(8) . . ? N10 C43 C42 103.9(7) . . ? N26 C43 C42 102.0(8) . . ? N27 C44 N11 113.4(7) . . ? N27 C44 C45 106.3(7) . . ? N11 C44 C45 102.3(7) . . ? N12 C45 N28 112.1(7) . . ? N12 C45 C44 106.0(7) . . ? N28 C45 C44 103.1(8) . . ? N29 C46 N13 114.3(8) . . ? N29 C46 C47 103.1(7) . . ? N13 C46 C47 102.7(7) . . ? N14 C47 N30 113.6(7) . . ? N14 C47 C46 103.1(7) . . ? N30 C47 C46 103.5(7) . . ? N31 C48 N15 113.7(7) . . ? N31 C48 C41 104.2(6) . . ? N15 C48 C41 103.9(6) . . ? C1" N1" C9" 121.8(8) . . ? C1" N1" C21" 117.9(8) . . ? C9" N1" C21" 120.3(7) . . ? C10" N2" C18" 120.0(12) . . ? C10" N2" C24" 113.9(14) . . ? C18" N2" C24" 125.9(12) . . ? N1" C1" C2" 121.7(10) . . ? C1" C2" C3" 119.6(10) . . ? C2" C3" C4" 119.5(9) . . ? C2" C3" C20" 117.7(9) . . ? C4" C3" C20" 122.7(9) . . ? C5" C4" C3" 122.3(9) . . ? C5" C4" C9" 118.8(8) . . ? C3" C4" C9" 118.8(8) . . ? C6" C5" C4" 120.3(9) . . ? C5" C6" C7" 120.1(9) . . ? C8" C7" C6" 121.4(9) . . ? C7" C8" C9" 118.2(8) . . ? C8" C9" N1" 121.5(8) . . ? C8" C9" C4" 121.1(8) . . ? N1" C9" C4" 117.4(8) . . ? N2" C10" C11" 120.0(15) . . ? C12" C11" C10" 121.9(14) . . ? C13" C12" C11" 114.9(13) . . ? C13" C12" C19" 130.0(14) . . ? C11" C12" C19" 115.1(14) . . ? C14" C13" C12" 118.4(14) . . ? C14" C13" C18" 115.8(15) . . ? C12" C13" C18" 125.3(14) . . ? C13" C14" C15" 123.8(16) . . ? C16" C15" C14" 116.6(17) . . ? C17" C16" C15" 120.3(16) . . ? C16" C17" C18" 119.7(15) . . ? C17" C18" C13" 123.6(15) . . ? C17" C18" N2" 120.2(13) . . ? C13" C18" N2" 116.1(13) . . ? C20" C19" C12" 126.4(11) . . ? C19" C20" C3" 125.7(10) . . ? N1" C21" C22" 112.2(7) . . ? C23" C22" C21" 108.2(7) . . ? N3" C23" C22" 110.7(7) . . ? N2" C24" C25" 102.3(13) . . ? C26" C25" C24" 103.0(15) . . ? N4" C26" C25" 97.1(18) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.773 _refine_diff_density_min -1.773 _refine_diff_density_rms 0.219