data_1234 _audit_creation_method 'SHELXL-97 & ZCIF' _chemical_name_systematic ; CB10 @ bis-diammonium tetraidodide hydrate ; _chemical_name_common 'CB10 @ bis-diammonium tetraidodide hydrate' _chemical_melting_point ? _chemical_formula_moiety '(C60 H60 N40 O20), (C17 H21 N7 O)2, I4, (H2 O) 32.94' _chemical_formula_sum 'C94 H167.87 I4 N54 O54.94' _chemical_formula_weight 3441.25 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' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnnm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' _cell_length_a 19.476(4) _cell_length_b 20.192(4) _cell_length_c 18.567(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7302(3) _cell_formula_units_Z 2 _cell_measurement_temperature 233(2) _cell_measurement_reflns_used 5532 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 21.0 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.315 _exptl_crystal_size_mid 0.285 _exptl_crystal_size_min 0.200 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_method not_measured _exptl_crystal_F_000 3523 _exptl_absorpt_coefficient_mu 0.957 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.680 _exptl_absorpt_correction_T_max 0.826 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _diffrn_ambient_temperature 233(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 'three-circle diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_decay_% 1.52 _diffrn_reflns_number 41685 _diffrn_reflns_av_R_equivalents 0.0887 _diffrn_reflns_av_sigmaI/netI 0.0506 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4924 _reflns_number_gt 3619 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Platon (Spek, 1990)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.06P)^2^+122.7P], P=(max(Fo^2^,0)+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4924 _refine_ls_number_parameters 623 _refine_ls_number_restraints 283 _refine_ls_R_factor_all 0.1188 _refine_ls_R_factor_gt 0.0874 _refine_ls_wR_factor_ref 0.2375 _refine_ls_wR_factor_gt 0.2053 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 0.980 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.01845(6) 0.31738(6) 0.0000 0.0726(4) Uani 1 2 d S . . I2 I 0.80907(7) 0.49018(6) 0.0000 0.0738(4) Uani 1 2 d S . . O1 O 0.8936(6) 0.1399(6) 0.0000 0.075(3) Uani 1 2 d S . . O2 O 0.6611(7) 0.3409(7) 0.0000 0.103(5) Uani 1 2 d S . . O3 O 0.8275(5) 0.0878(5) 0.1848(5) 0.085(3) Uani 1 1 d . . . O4 O 0.6127(5) 0.3045(5) 0.1908(6) 0.104(3) Uani 1 1 d . . . O5 O 0.6890(5) -0.0389(4) 0.2723(5) 0.085(3) Uani 1 1 d . . . O6 O 0.4778(5) 0.1881(4) 0.2803(4) 0.075(2) Uani 1 1 d . . . N1 N 0.5872(5) -0.0045(4) 0.3258(5) 0.061(2) Uani 1 1 d . . . N2 N 0.7535(5) 0.1447(5) 0.2591(6) 0.075(3) Uani 1 1 d . . . N3 N 0.8516(5) 0.2324(5) 0.0601(5) 0.067(3) Uani 1 1 d . . . N4 N 0.8162(5) 0.2007(5) 0.1803(6) 0.074(3) Uani 1 1 d . . . N5 N 0.6710(5) 0.0694(5) 0.3105(5) 0.067(3) Uani 1 1 d . . . N6 N 0.5037(5) 0.0847(4) 0.3253(5) 0.061(2) Uani 1 1 d . . . N7 N 0.5875(5) 0.1581(5) 0.3139(5) 0.066(3) Uani 1 1 d . . . N8 N 0.7615(5) 0.3133(5) 0.0591(6) 0.071(3) Uani 1 1 d . . . N9 N 0.6707(5) 0.2335(5) 0.2649(6) 0.080(3) Uani 1 1 d . . . N10 N 0.7282(6) 0.2855(5) 0.1803(6) 0.081(3) Uani 1 1 d . . . C1 C 0.8674(8) 0.1954(10) 0.0000 0.068(5) Uani 1 2 d S . . C2 C 0.6530(7) 0.0036(6) 0.2991(7) 0.070(3) Uani 1 1 d . . . C3 C 0.8007(6) 0.1391(6) 0.2041(7) 0.070(3) Uani 1 1 d . . . C4 C 0.7420(6) 0.0911(7) 0.3085(7) 0.078(4) Uani 1 1 d . . . H4A H 0.7557 0.1052 0.3569 0.094 Uiso 1 1 calc R . . H4B H 0.7711 0.0536 0.2948 0.094 Uiso 1 1 calc R . . C5 C 0.8734(6) 0.2133(7) 0.1306(7) 0.074(3) Uani 1 1 d . . . H5A H 0.9024 0.2484 0.1507 0.089 Uiso 1 1 calc R . . H5B H 0.9014 0.1731 0.1268 0.089 Uiso 1 1 calc R . . C6 C 0.6195(6) 0.1042(5) 0.3516(6) 0.061(3) Uani 1 1 d . . . H6 H 0.6374 0.1185 0.3989 0.073 Uiso 1 1 calc R . . C7 C 0.5622(5) 0.0541(5) 0.3599(6) 0.059(3) Uani 1 1 d . . . H7 H 0.5525 0.0458 0.4114 0.071 Uiso 1 1 calc R . . C8 C 0.7805(7) 0.2514(6) 0.2188(7) 0.077(4) Uani 1 1 d . . . H8A H 0.8130 0.2828 0.2414 0.093 Uiso 1 1 calc R . . C9 C 0.8313(6) 0.2981(5) 0.0425(6) 0.064(3) Uani 1 1 d . . . H9 H 0.8633 0.3315 0.0624 0.077 Uiso 1 1 calc R . . C10 C 0.7397(7) 0.2128(6) 0.2763(6) 0.071(3) Uani 1 1 d . . . H10 H 0.7555 0.2240 0.3255 0.085 Uiso 1 1 calc R . . C11 C 0.5199(7) 0.1474(6) 0.3039(6) 0.067(3) Uani 1 1 d . . . C12 C 0.7204(11) 0.3249(8) 0.0000 0.076(5) Uani 1 2 d S . . C13 C 0.4355(6) 0.0693(5) 0.3483(7) 0.067(3) Uani 1 1 d . . . H13A H 0.4039 0.1026 0.3290 0.081 Uiso 1 1 calc R . . H13B H 0.4335 0.0718 0.4010 0.081 Uiso 1 1 calc R . . C14 C 0.6158(7) 0.2235(6) 0.3177(7) 0.076(4) Uani 1 1 d . . . H14A H 0.6341 0.2310 0.3662 0.091 Uiso 1 1 calc R . . H14B H 0.5793 0.2559 0.3092 0.091 Uiso 1 1 calc R . . C15 C 0.6654(8) 0.2776(7) 0.2091(8) 0.086(4) Uani 1 1 d . . . C16 C 0.7414(7) 0.3378(6) 0.1308(7) 0.085(4) Uani 1 1 d . . . H16A H 0.7782 0.3658 0.1500 0.102 Uiso 1 1 calc R . . H16B H 0.7001 0.3652 0.1261 0.102 Uiso 1 1 calc R . . O1A O 0.3802(7) 0.2871(6) 0.1421(7) 0.127(8) Uani 0.50 1 d PRDU A 1 C1A C 0.4182(8) 0.2406(8) 0.1317(5) 0.088(9) Uani 0.50 1 d PGDU A 1 N2A N 0.4860(8) 0.2525(7) 0.1121(9) 0.098(7) Uani 0.50 1 d PGDU A 1 C3A C 0.5304(6) 0.1997(9) 0.1000(11) 0.083(7) Uani 0.50 1 d PGDU A 1 N4A N 0.5069(8) 0.1350(8) 0.1075(10) 0.082(7) Uani 0.50 1 d PGDU A 1 C5A C 0.4392(9) 0.1231(7) 0.1271(11) 0.083(7) Uani 0.50 1 d PGDU A 1 N6A N 0.3948(7) 0.1759(9) 0.1392(10) 0.091(8) Uani 0.50 1 d PGDU A 1 H6A H 0.3524 0.1685 0.1514 0.17(17) Uiso 0.50 1 calc PR A 1 N1B N 0.5918(7) 0.2083(10) 0.0816(11) 0.090(6) Uani 0.50 1 d PDU . . H1B H 0.6059 0.2491 0.0790 0.109 Uiso 0.50 1 calc PR A 1 C2B C 0.6398(5) 0.1591(6) 0.0648(9) 0.079(6) Uani 0.50 1 d PGDU A . C3B C 0.6772(7) 0.1603(7) 0.0002(9) 0.081(5) Uani 1 2 d SGDU A 2 H3B H 0.6702 0.1945 -0.0334 0.098 Uiso 0.50 1 calc PR A 2 C4B C 0.7244(7) 0.1105(8) -0.0135(8) 0.074(6) Uani 0.50 1 d PGDU A 2 H4B1 H 0.7500 0.1113 -0.0564 0.088 Uiso 0.50 1 calc PR A 2 C5B C 0.7343(6) 0.0595(7) 0.0357(9) 0.085(7) Uani 0.50 1 d PGDU A 2 C6B C 0.6970(9) 0.0583(8) 0.0995(8) 0.104(10) Uani 0.50 1 d PGDU A 2 H6B H 0.7037 0.0238 0.1327 0.125 Uiso 0.50 1 calc PR A 2 C7B C 0.6497(8) 0.1081(9) 0.1140(7) 0.099(9) Uani 0.50 1 d PGDU A 2 H7B H 0.6244 0.1073 0.1571 0.119 Uiso 0.50 1 calc PR A 2 C8B C 0.7853(11) 0.0062(11) 0.0190(14) 0.102(11) Uani 0.50 1 d PDU A 2 H8B1 H 0.7668 -0.0366 0.0345 0.122 Uiso 0.50 1 calc PR A 2 H8B2 H 0.7927 0.0043 -0.0332 0.122 Uiso 0.50 1 calc PR A 2 N9B N 0.8495(10) 0.0177(11) 0.0542(14) 0.100(7) Uani 0.50 1 d PDU A 2 H9B1 H 0.8701 0.0532 0.0344 0.149 Uiso 0.50 1 calc PR A 2 H9B2 H 0.8766 -0.0181 0.0489 0.149 Uiso 0.50 1 calc PR A 2 H9B3 H 0.8422 0.0252 0.1013 0.149 Uiso 0.50 1 calc PR A 2 N1C N 0.4174(11) 0.0665(8) 0.1329(11) 0.100(7) Uani 0.50 1 d PDU . . H1C H 0.3752 0.0643 0.1481 0.121 Uiso 0.50 1 calc PR A 1 C2C C 0.4471(9) 0.0046(7) 0.1198(8) 0.124(10) Uani 0.50 1 d PGDU A . C3C C 0.5134(9) -0.0037(9) 0.0935(12) 0.124(10) Uani 0.50 1 d PGDU A 3 H3C H 0.5408 0.0335 0.0835 0.149 Uiso 0.50 1 calc PR A 3 C4C C 0.5391(8) -0.0671(11) 0.0820(12) 0.142(15) Uani 0.50 1 d PGDU A 3 H4C H 0.5839 -0.0727 0.0642 0.170 Uiso 0.50 1 calc PR A 3 C5C C 0.4985(11) -0.1221(9) 0.0968(9) 0.102(12) Uani 0.50 1 d PGDU A 3 C6C C 0.4323(10) -0.1137(8) 0.1231(10) 0.103(8) Uani 0.50 1 d PGDU A 3 H6C H 0.4048 -0.1509 0.1331 0.123 Uiso 0.50 1 calc PR A 3 C7C C 0.4066(8) -0.0504(9) 0.1346(9) 0.091(7) Uani 0.50 1 d PGDU A 3 H7C H 0.3618 -0.0447 0.1524 0.109 Uiso 0.50 1 calc PR A 3 C8C C 0.5267(17) -0.1901(13) 0.0842(14) 0.128(12) Uani 0.50 1 d PDU A 3 H8C1 H 0.4890 -0.2222 0.0851 0.153 Uiso 0.50 1 calc PR A 3 H8C2 H 0.5479 -0.1918 0.0364 0.153 Uiso 0.50 1 calc PR A 3 N9C N 0.5765(19) -0.2083(15) 0.1372(19) 0.128(14) Uani 0.50 1 d PDU A 3 H9C1 H 0.6187 -0.2075 0.1174 0.193 Uiso 0.50 1 calc PR A 3 H9C2 H 0.5674 -0.2493 0.1534 0.193 Uiso 0.50 1 calc PR A 3 H9C3 H 0.5748 -0.1794 0.1741 0.193 Uiso 0.50 1 calc PR A 3 O1W O 0.5329(10) 0.3804(12) 0.0743(14) 0.187(14) Uani 0.73(4) 1 d PU . . O2W O 0.361(3) 0.366(3) 0.0000 0.209(17) Uani 0.50 2 d SPU . . O3W O 0.199(7) 0.218(5) 0.0000 0.209(18) Uani 0.50 2 d SPU . . O4W O 0.222(3) 0.322(3) 0.0000 0.209(17) Uani 0.50 2 d SPU . . O5W O 0.2701(14) 0.1552(10) 0.1183(14) 0.273(11) Uani 1 1 d U . . O7W O 0.084(4) 0.029(4) 0.276(4) 0.38(3) Uani 0.50 1 d PU . . O8W O 0.8073(14) 0.9251(15) 0.1948(15) 0.316(14) Uani 1 1 d U . . O9W O 0.084(4) 0.164(3) 0.0000 0.18(2) Uani 0.39(7) 2 d SPU . . O10W O 0.366(3) 0.487(3) 0.0000 0.24(2) Uani 0.50 2 d SPU . . O11W O 0.422(3) 0.431(4) 0.831(5) 0.39(4) Uani 0.50 1 d PU . . O12W O 0.047(2) 0.061(2) 0.054(3) 0.20(2) Uani 0.39(3) 1 d PU . . O13W O 0.288(3) 0.274(3) 0.0000 0.232(15) Uani 0.50 2 d SPU . . O14W O 0.048(3) 0.095(3) 0.180(4) 0.32(2) Uani 0.50 1 d PU . . O15W O 0.206(6) 0.193(4) 0.0000 0.20(2) Uani 0.50 2 d SPU . . O16W O 0.386(2) 0.338(2) 0.139(3) 0.232(17) Uani 0.50 1 d PU . . O17W O 0.368(3) 0.514(3) -0.096(4) 0.25(3) Uani 0.40(5) 1 d PU . . O18W O 0.265(4) 0.350(3) 0.0000 0.220(16) Uani 0.50 2 d SPU . . O19W O 0.058(4) 0.155(3) 0.055(6) 0.18(2) Uani 0.26(4) 1 d PU . . O20W O -0.004(3) 0.131(3) 0.247(4) 0.30(2) Uani 0.50 1 d PU . . 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 I1 0.0718(8) 0.0900(9) 0.0559(7) 0.000 0.000 -0.0079(6) I2 0.0849(9) 0.0685(8) 0.0679(8) 0.000 0.000 -0.0069(6) O1 0.072(8) 0.075(8) 0.076(8) 0.000 0.000 -0.001(7) O2 0.070(9) 0.075(9) 0.163(15) 0.000 0.000 0.012(7) O3 0.084(6) 0.080(6) 0.091(7) 0.016(5) 0.029(5) 0.009(5) O4 0.098(7) 0.109(8) 0.105(8) 0.045(6) 0.032(6) 0.029(6) O5 0.089(6) 0.077(6) 0.090(7) 0.003(5) 0.029(5) 0.022(5) O6 0.097(6) 0.070(5) 0.057(5) 0.003(4) 0.008(5) 0.021(5) N1 0.058(6) 0.064(6) 0.060(6) 0.005(5) 0.011(5) 0.009(5) N2 0.068(6) 0.074(7) 0.081(7) 0.014(6) 0.022(6) -0.002(5) N3 0.070(6) 0.071(6) 0.059(6) -0.002(5) 0.007(5) -0.007(5) N4 0.066(6) 0.073(7) 0.083(7) 0.013(6) 0.014(6) 0.005(5) N5 0.061(6) 0.071(7) 0.070(7) 0.015(5) 0.014(5) 0.006(5) N6 0.069(6) 0.052(5) 0.062(6) 0.000(5) -0.002(5) 0.009(5) N7 0.071(7) 0.064(6) 0.061(6) 0.014(5) 0.017(5) 0.014(5) N8 0.074(7) 0.070(6) 0.069(7) 0.009(5) 0.012(6) -0.012(5) N9 0.077(7) 0.071(7) 0.091(8) 0.011(6) 0.028(6) 0.005(6) N10 0.077(7) 0.071(7) 0.096(8) 0.030(6) 0.032(6) 0.008(6) C1 0.046(9) 0.086(13) 0.071(12) 0.000 0.000 -0.025(10) C2 0.079(9) 0.063(8) 0.068(8) 0.010(7) -0.007(7) 0.015(7) C3 0.063(8) 0.066(8) 0.079(9) 0.012(7) 0.004(7) 0.008(7) C4 0.074(9) 0.084(9) 0.075(9) 0.018(7) 0.012(7) 0.005(7) C5 0.057(7) 0.089(9) 0.077(9) 0.010(7) 0.007(6) -0.015(6) C6 0.067(7) 0.062(7) 0.053(7) 0.003(6) 0.002(6) 0.011(6) C7 0.056(7) 0.061(7) 0.060(7) 0.007(6) 0.002(5) 0.008(6) C8 0.076(8) 0.069(8) 0.087(10) 0.005(7) 0.023(7) 0.001(7) C9 0.071(8) 0.055(7) 0.067(7) -0.001(6) -0.004(6) -0.008(6) C10 0.086(9) 0.076(8) 0.050(7) 0.007(6) 0.015(6) -0.001(7) C11 0.076(9) 0.075(9) 0.048(7) -0.002(6) 0.012(6) 0.019(7) C12 0.081(14) 0.034(9) 0.112(17) 0.000 0.000 -0.007(9) C13 0.054(7) 0.061(7) 0.086(9) -0.007(6) -0.001(6) 0.005(6) C14 0.082(9) 0.065(8) 0.080(9) 0.007(7) 0.027(7) 0.008(7) C15 0.087(10) 0.072(9) 0.100(11) 0.019(8) 0.025(9) 0.003(8) C16 0.097(10) 0.073(8) 0.084(10) 0.003(7) 0.023(8) 0.002(7) O1A 0.103(14) 0.106(14) 0.172(19) 0.017(16) 0.028(14) 0.016(12) C1A 0.071(14) 0.101(16) 0.09(3) -0.01(2) -0.022(16) 0.004(13) N2A 0.068(11) 0.103(15) 0.12(2) 0.004(16) -0.014(13) -0.005(10) C3A 0.071(13) 0.110(16) 0.068(17) 0.010(16) -0.009(14) -0.007(11) N4A 0.077(14) 0.102(14) 0.069(19) 0.004(16) -0.016(15) -0.002(11) C5A 0.092(16) 0.099(14) 0.058(15) 0.022(15) 0.002(15) 0.001(12) N6A 0.091(17) 0.106(13) 0.076(18) 0.029(17) 0.008(14) 0.005(12) N1B 0.067(11) 0.101(15) 0.104(18) -0.015(13) -0.007(11) -0.006(9) C2B 0.070(15) 0.094(16) 0.074(15) -0.014(12) -0.012(11) -0.004(12) C3B 0.081(13) 0.087(12) 0.076(11) 0.000 0.000 -0.017(9) C4B 0.076(13) 0.107(15) 0.037(19) -0.002(11) -0.003(10) -0.012(10) C5B 0.093(17) 0.085(16) 0.077(15) 0.006(12) -0.002(12) -0.009(12) C6B 0.11(2) 0.12(2) 0.086(19) 0.042(17) 0.017(15) 0.012(16) C7B 0.067(17) 0.14(2) 0.10(2) 0.023(16) 0.013(14) 0.002(14) C8B 0.112(18) 0.108(18) 0.08(4) -0.003(15) -0.001(14) 0.006(14) N9B 0.093(14) 0.092(16) 0.11(2) 0.008(14) 0.019(13) -0.024(13) N1C 0.099(17) 0.087(11) 0.12(2) 0.024(15) -0.004(15) -0.015(11) C2C 0.13(3) 0.092(9) 0.15(2) 0.02(2) 0.04(2) 0.003(13) C3C 0.13(3) 0.092(9) 0.15(2) 0.02(2) 0.04(2) 0.003(13) C4C 0.11(2) 0.099(16) 0.22(5) 0.02(3) -0.01(3) 0.019(16) C5C 0.13(3) 0.097(14) 0.08(3) 0.01(2) -0.03(2) 0.004(15) C6C 0.12(2) 0.093(14) 0.10(2) 0.014(17) -0.034(18) -0.005(15) C7C 0.108(19) 0.089(13) 0.075(18) -0.005(15) -0.027(15) -0.020(13) C8C 0.18(3) 0.104(17) 0.10(3) 0.00(2) -0.05(2) 0.03(2) N9C 0.17(4) 0.14(3) 0.07(2) -0.03(2) -0.03(2) 0.06(3) O1W 0.155(18) 0.20(2) 0.20(2) 0.059(17) 0.032(15) 0.060(15) O2W 0.20(3) 0.21(3) 0.21(3) 0.000 0.000 0.05(3) O3W 0.22(3) 0.22(3) 0.19(2) 0.000 0.000 0.02(3) O4W 0.20(3) 0.21(3) 0.23(3) 0.000 0.000 0.07(2) O5W 0.37(3) 0.177(16) 0.27(2) -0.062(16) 0.00(2) -0.013(18) O7W 0.34(5) 0.41(5) 0.38(5) 0.02(4) 0.06(4) -0.04(4) O8W 0.33(3) 0.36(3) 0.26(3) -0.02(2) 0.11(2) 0.10(2) O9W 0.20(4) 0.13(3) 0.22(4) 0.000 0.000 0.03(3) O10W 0.17(3) 0.29(4) 0.26(4) 0.000 0.000 0.03(3) O11W 0.35(5) 0.41(5) 0.43(6) -0.06(4) -0.05(4) -0.05(4) O12W 0.19(3) 0.17(3) 0.24(3) 0.05(2) 0.00(2) 0.03(2) O13W 0.24(3) 0.22(3) 0.23(2) 0.000 0.000 0.06(2) O14W 0.32(4) 0.27(3) 0.37(4) 0.00(3) -0.03(3) -0.02(3) O15W 0.21(3) 0.22(4) 0.18(3) 0.000 0.000 0.03(3) O16W 0.18(3) 0.18(3) 0.33(4) 0.03(3) 0.06(3) 0.05(2) O17W 0.21(4) 0.26(4) 0.29(5) -0.04(3) 0.03(3) 0.05(3) O18W 0.23(3) 0.20(3) 0.23(2) 0.000 0.000 0.07(2) O19W 0.18(3) 0.13(3) 0.22(4) 0.01(2) -0.02(2) 0.03(2) O20W 0.30(4) 0.29(3) 0.31(4) -0.01(3) -0.06(3) -0.05(3) _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 O1 C1 1.23(2) . ? O2 C12 1.20(2) . ? O3 C3 1.214(14) . ? O4 C15 1.210(16) . ? O5 C2 1.215(14) . ? O6 C11 1.242(13) . ? N1 C2 1.385(16) . ? N1 C7 1.428(14) . ? N1 C13 1.441(14) 2_655 ? N2 C3 1.379(15) . ? N2 C4 1.437(15) . ? N2 C10 1.437(15) . ? N3 C1 1.378(15) . ? N3 C9 1.421(14) . ? N3 C5 1.429(15) . ? N4 C3 1.353(15) . ? N4 C8 1.430(15) . ? N4 C5 1.468(14) . ? N5 C2 1.390(15) . ? N5 C6 1.444(14) . ? N5 C4 1.450(15) . ? N6 C11 1.363(15) . ? N6 C13 1.430(14) . ? N6 C7 1.445(13) . ? N7 C11 1.348(15) . ? N7 C14 1.431(15) . ? N7 C6 1.436(13) . ? N8 C12 1.379(15) . ? N8 C9 1.426(15) . ? N8 C16 1.474(15) . ? N9 C15 1.370(17) . ? N9 C10 1.424(16) . ? N9 C14 1.464(15) . ? N10 C15 1.343(16) . ? N10 C8 1.422(16) . ? N10 C16 1.424(14) . ? C1 N3 1.378(15) 6 ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 C7 1.514(15) . ? C6 H6 0.9900 . ? C7 H7 0.9900 . ? C8 C10 1.540(16) . ? C8 H8A 0.9900 . ? C9 C9 1.58(2) 6 ? C9 H9 0.9900 . ? C10 H10 0.9900 . ? C12 N8 1.379(15) 6 ? C13 N1 1.441(14) 2_655 ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? O1A C1A 1.211(17) . ? C1A N2A 1.3900 . ? C1A N6A 1.3900 . ? N2A C3A 1.3900 . ? C3A N1B 1.256(15) . ? C3A N4A 1.3900 . ? N4A C5A 1.3900 . ? C5A N1C 1.225(15) . ? C5A N6A 1.3900 . ? N6A O5W 2.49(3) . ? N6A H6A 0.8700 . ? N1B C2B 1.399(18) . ? N1B H1B 0.8700 . ? C2B C3B 1.4033 . ? C2B C7B 1.3900 . ? C3B C4B 1.3871 . ? C3B H3B 0.9400 . ? C4B C5B 1.3900 . ? C4B H4B1 0.9400 . ? C5B C6B 1.3900 . ? C5B C8B 1.50(2) . ? C6B C7B 1.3900 . ? C6B H6B 0.9400 . ? C7B H7B 0.9400 . ? C8B N9B 1.43(2) . ? C8B H8B1 0.9800 . ? C8B H8B2 0.9800 . ? N9B H9B1 0.9000 . ? N9B H9B2 0.9000 . ? N9B H9B3 0.9000 . ? N1C C2C 1.398(18) . ? N1C H1C 0.8700 . ? C2C C3C 1.3900 . ? C2C C7C 1.3900 . ? C3C C4C 1.3900 . ? C3C H3C 0.9400 . ? C4C C5C 1.3900 . ? C4C H4C 0.9400 . ? C5C C6C 1.3900 . ? C5C C8C 1.50(2) . ? C6C C7C 1.3900 . ? C6C H6C 0.9400 . ? C7C H7C 0.9400 . ? C8C N9C 1.43(2) . ? C8C H8C1 0.9800 . ? C8C H8C2 0.9800 . ? N9C H9C1 0.9000 . ? N9C H9C2 0.9000 . ? N9C H9C3 0.9000 . ? 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 C2 N1 C7 112.1(9) . . ? C2 N1 C13 119.7(9) . 2_655 ? C7 N1 C13 121.3(9) . 2_655 ? C3 N2 C4 121.0(10) . . ? C3 N2 C10 111.5(10) . . ? C4 N2 C10 123.4(10) . . ? C1 N3 C9 112.5(11) . . ? C1 N3 C5 121.9(11) . . ? C9 N3 C5 123.1(10) . . ? C3 N4 C8 112.7(10) . . ? C3 N4 C5 122.3(11) . . ? C8 N4 C5 124.0(10) . . ? C2 N5 C6 111.7(10) . . ? C2 N5 C4 121.7(10) . . ? C6 N5 C4 122.0(10) . . ? C11 N6 C13 120.2(10) . . ? C11 N6 C7 110.2(10) . . ? C13 N6 C7 120.3(9) . . ? C11 N7 C14 122.1(10) . . ? C11 N7 C6 111.6(10) . . ? C14 N7 C6 120.5(10) . . ? C12 N8 C9 114.8(12) . . ? C12 N8 C16 120.5(11) . . ? C9 N8 C16 121.4(10) . . ? C15 N9 C10 112.0(10) . . ? C15 N9 C14 122.8(11) . . ? C10 N9 C14 123.3(11) . . ? C15 N10 C8 113.3(11) . . ? C15 N10 C16 120.6(11) . . ? C8 N10 C16 123.6(11) . . ? O1 C1 N3 125.9(9) . 6 ? O1 C1 N3 125.9(9) . . ? N3 C1 N3 108.2(17) 6 . ? O5 C2 N1 126.7(12) . . ? O5 C2 N5 126.3(12) . . ? N1 C2 N5 107.0(11) . . ? O3 C3 N4 126.3(12) . . ? O3 C3 N2 125.1(11) . . ? N4 C3 N2 108.4(11) . . ? N2 C4 N5 113.1(10) . . ? N2 C4 H4A 109.0 . . ? N5 C4 H4A 109.0 . . ? N2 C4 H4B 109.0 . . ? N5 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? N3 C5 N4 113.4(10) . . ? N3 C5 H5A 108.9 . . ? N4 C5 H5A 108.9 . . ? N3 C5 H5B 108.9 . . ? N4 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? N7 C6 N5 114.4(9) . . ? N7 C6 C7 103.7(9) . . ? N5 C6 C7 104.0(9) . . ? N7 C6 H6 111.4 . . ? N5 C6 H6 111.4 . . ? C7 C6 H6 111.4 . . ? N1 C7 N6 115.2(10) . . ? N1 C7 C6 104.9(9) . . ? N6 C7 C6 104.4(9) . . ? N1 C7 H7 110.6 . . ? N6 C7 H7 110.6 . . ? C6 C7 H7 110.6 . . ? N10 C8 N4 116.3(12) . . ? N10 C8 C10 102.9(10) . . ? N4 C8 C10 103.6(10) . . ? N10 C8 H8A 111.1 . . ? N4 C8 H8A 111.1 . . ? C10 C8 H8A 111.1 . . ? N3 C9 N8 114.7(10) . . ? N3 C9 C9 103.3(6) . 6 ? N8 C9 C9 102.5(6) . 6 ? N3 C9 H9 111.9 . . ? N8 C9 H9 111.9 . . ? C9 C9 H9 111.9 6 . ? N9 C10 N2 115.1(11) . . ? N9 C10 C8 103.6(10) . . ? N2 C10 C8 103.5(10) . . ? N9 C10 H10 111.4 . . ? N2 C10 H10 111.4 . . ? C8 C10 H10 111.4 . . ? O6 C11 N7 125.9(12) . . ? O6 C11 N6 124.5(12) . . ? N7 C11 N6 109.6(11) . . ? O2 C12 N8 127.3(8) . 6 ? O2 C12 N8 127.3(8) . . ? N8 C12 N8 105.4(17) 6 . ? N6 C13 N1 113.4(9) . 2_655 ? N6 C13 H13A 108.9 . . ? N1 C13 H13A 108.9 2_655 . ? N6 C13 H13B 108.9 . . ? N1 C13 H13B 108.9 2_655 . ? H13A C13 H13B 107.7 . . ? N7 C14 N9 112.1(10) . . ? N7 C14 H14A 109.2 . . ? N9 C14 H14A 109.2 . . ? N7 C14 H14B 109.2 . . ? N9 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? O4 C15 N10 127.4(13) . . ? O4 C15 N9 124.6(13) . . ? N10 C15 N9 108.0(13) . . ? N10 C16 N8 112.5(10) . . ? N10 C16 H16A 109.1 . . ? N8 C16 H16A 109.1 . . ? N10 C16 H16B 109.1 . . ? N8 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? O1A C1A N2A 119.2(14) . . ? O1A C1A N6A 120.8(14) . . ? N2A C1A N6A 120.0 . . ? C3A N2A C1A 120.0 . . ? N1B C3A N2A 122.0(16) . . ? N1B C3A N4A 118.0(16) . . ? N2A C3A N4A 120.0 . . ? C5A N4A C3A 120.0 . . ? N1C C5A N4A 120.9(17) . . ? N1C C5A N6A 119.1(17) . . ? N4A C5A N6A 120.0 . . ? C5A N6A C1A 120.0 . . ? C5A N6A H6A 120.0 . . ? C1A N6A H6A 120.0 . . ? C3A N1B C2B 126.8(15) . . ? C3A N1B H1B 116.6 . . ? C2B N1B H1B 116.6 . . ? C3B C2B C7B 120.2 . . ? C3B C2B N1B 121.6(13) . . ? C7B C2B N1B 118.2(13) . . ? C4B C3B C2B 119.3 . . ? C4B C3B H3B 120.4 . . ? C2B C3B H3B 120.4 . . ? C3B C4B C5B 120.6 . . ? C3B C4B H4B1 119.7 . . ? C5B C4B H4B1 119.7 . . ? C6B C5B C4B 120.0 . . ? C6B C5B C8B 120.7(14) . . ? C4B C5B C8B 119.3(14) . . ? C5B C6B C7B 120.0 . . ? C5B C6B H6B 120.0 . . ? C7B C6B H6B 120.0 . . ? C6B C7B C2B 120.0 . . ? C6B C7B H7B 120.0 . . ? C2B C7B H7B 120.0 . . ? N9B C8B C5B 111.7(14) . . ? N9B C8B H8B1 109.3 . . ? C5B C8B H8B1 109.3 . . ? N9B C8B H8B2 109.3 . . ? C5B C8B H8B2 109.3 . . ? H8B1 C8B H8B2 107.9 . . ? C8B N9B H9B1 109.5 . . ? C8B N9B H9B2 109.5 . . ? H9B1 N9B H9B2 109.5 . . ? C8B N9B H9B3 109.5 . . ? H9B1 N9B H9B3 109.5 . . ? H9B2 N9B H9B3 109.5 . . ? C5A N1C C2C 133(2) . . ? C5A N1C H1C 113.7 . . ? C2C N1C H1C 113.7 . . ? C3C C2C C7C 120.0 . . ? C3C C2C N1C 123.6(13) . . ? C7C C2C N1C 116.4(13) . . ? C4C C3C C2C 120.0 . . ? C4C C3C H3C 120.0 . . ? C2C C3C H3C 120.0 . . ? C5C C4C C3C 120.0 . . ? C5C C4C H4C 120.0 . . ? C3C C4C H4C 120.0 . . ? C4C C5C C6C 120.0 . . ? C4C C5C C8C 119.6(15) . . ? C6C C5C C8C 120.4(15) . . ? C7C C6C C5C 120.0 . . ? C7C C6C H6C 120.0 . . ? C5C C6C H6C 120.0 . . ? C6C C7C C2C 120.0 . . ? C6C C7C H7C 120.0 . . ? C2C C7C H7C 120.0 . . ? N9C C8C C5C 112.2(16) . . ? N9C C8C H8C1 109.2 . . ? C5C C8C H8C1 109.2 . . ? N9C C8C H8C2 109.2 . . ? C5C C8C H8C2 109.2 . . ? H8C1 C8C H8C2 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 N3 C1 O1 171.5(14) . . . . ? C5 N3 C1 O1 9(2) . . . . ? C9 N3 C1 N3 -6.0(17) . . . 6 ? C5 N3 C1 N3 -168.4(8) . . . 6 ? C7 N1 C2 O5 174.3(12) . . . . ? C13 N1 C2 O5 23.0(19) 2_655 . . . ? C7 N1 C2 N5 -4.0(13) . . . . ? C13 N1 C2 N5 -155.3(10) 2_655 . . . ? C6 N5 C2 O5 -172.7(12) . . . . ? C4 N5 C2 O5 -16.4(19) . . . . ? C6 N5 C2 N1 5.6(13) . . . . ? C4 N5 C2 N1 161.9(10) . . . . ? C8 N4 C3 O3 -173.9(13) . . . . ? C5 N4 C3 O3 -5(2) . . . . ? C8 N4 C3 N2 0.6(15) . . . . ? C5 N4 C3 N2 169.3(11) . . . . ? C4 N2 C3 O3 13(2) . . . . ? C10 N2 C3 O3 170.8(13) . . . . ? C4 N2 C3 N4 -161.9(11) . . . . ? C10 N2 C3 N4 -3.8(15) . . . . ? C3 N2 C4 N5 -122.8(13) . . . . ? C10 N2 C4 N5 81.8(15) . . . . ? C2 N5 C4 N2 125.6(12) . . . . ? C6 N5 C4 N2 -80.5(14) . . . . ? C1 N3 C5 N4 -118.7(13) . . . . ? C9 N3 C5 N4 80.8(14) . . . . ? C3 N4 C5 N3 110.3(14) . . . . ? C8 N4 C5 N3 -82.3(16) . . . . ? C11 N7 C6 N5 116.5(11) . . . . ? C14 N7 C6 N5 -89.8(13) . . . . ? C11 N7 C6 C7 3.9(12) . . . . ? C14 N7 C6 C7 157.7(10) . . . . ? C2 N5 C6 N7 -117.3(11) . . . . ? C4 N5 C6 N7 86.5(13) . . . . ? C2 N5 C6 C7 -4.9(12) . . . . ? C4 N5 C6 C7 -161.1(10) . . . . ? C2 N1 C7 N6 115.3(11) . . . . ? C13 N1 C7 N6 -93.9(12) 2_655 . . . ? C2 N1 C7 C6 1.0(12) . . . . ? C13 N1 C7 C6 151.8(10) 2_655 . . . ? C11 N6 C7 N1 -119.3(10) . . . . ? C13 N6 C7 N1 93.9(12) . . . . ? C11 N6 C7 C6 -4.8(12) . . . . ? C13 N6 C7 C6 -151.6(10) . . . . ? N7 C6 C7 N1 122.2(9) . . . . ? N5 C6 C7 N1 2.3(11) . . . . ? N7 C6 C7 N6 0.6(11) . . . . ? N5 C6 C7 N6 -119.3(9) . . . . ? C15 N10 C8 N4 117.7(13) . . . . ? C16 N10 C8 N4 -80.3(16) . . . . ? C15 N10 C8 C10 5.1(15) . . . . ? C16 N10 C8 C10 167.2(11) . . . . ? C3 N4 C8 N10 -109.6(12) . . . . ? C5 N4 C8 N10 81.9(15) . . . . ? C3 N4 C8 C10 2.5(15) . . . . ? C5 N4 C8 C10 -166.0(11) . . . . ? C1 N3 C9 N8 114.2(12) . . . . ? C5 N3 C9 N8 -83.6(13) . . . . ? C1 N3 C9 C9 3.6(10) . . . 6 ? C5 N3 C9 C9 165.8(9) . . . 6 ? C12 N8 C9 N3 -113.5(12) . . . . ? C16 N8 C9 N3 87.3(13) . . . . ? C12 N8 C9 C9 -2.4(11) . . . 6 ? C16 N8 C9 C9 -161.6(8) . . . 6 ? C15 N9 C10 N2 -111.6(12) . . . . ? C14 N9 C10 N2 83.9(15) . . . . ? C15 N9 C10 C8 0.6(15) . . . . ? C14 N9 C10 C8 -163.9(11) . . . . ? C3 N2 C10 N9 117.5(11) . . . . ? C4 N2 C10 N9 -85.1(15) . . . . ? C3 N2 C10 C8 5.1(14) . . . . ? C4 N2 C10 C8 162.6(11) . . . . ? N10 C8 C10 N9 -3.3(13) . . . . ? N4 C8 C10 N9 -124.8(11) . . . . ? N10 C8 C10 N2 117.2(11) . . . . ? N4 C8 C10 N2 -4.4(14) . . . . ? C14 N7 C11 O6 18.4(18) . . . . ? C6 N7 C11 O6 171.6(11) . . . . ? C14 N7 C11 N6 -160.5(10) . . . . ? C6 N7 C11 N6 -7.2(13) . . . . ? C13 N6 C11 O6 -24.6(17) . . . . ? C7 N6 C11 O6 -171.4(10) . . . . ? C13 N6 C11 N7 154.3(10) . . . . ? C7 N6 C11 N7 7.5(13) . . . . ? C9 N8 C12 O2 -177.0(15) . . . . ? C16 N8 C12 O2 -18(2) . . . . ? C9 N8 C12 N8 3.9(17) . . . 6 ? C16 N8 C12 N8 163.3(8) . . . 6 ? C11 N6 C13 N1 142.5(11) . . . 2_655 ? C7 N6 C13 N1 -74.1(13) . . . 2_655 ? C11 N7 C14 N9 -124.5(12) . . . . ? C6 N7 C14 N9 84.6(14) . . . . ? C15 N9 C14 N7 115.0(14) . . . . ? C10 N9 C14 N7 -82.2(15) . . . . ? C8 N10 C15 O4 174.4(16) . . . . ? C16 N10 C15 O4 12(2) . . . . ? C8 N10 C15 N9 -5.0(17) . . . . ? C16 N10 C15 N9 -167.6(12) . . . . ? C10 N9 C15 O4 -176.8(15) . . . . ? C14 N9 C15 O4 -12(2) . . . . ? C10 N9 C15 N10 2.5(16) . . . . ? C14 N9 C15 N10 167.1(12) . . . . ? C15 N10 C16 N8 -117.5(14) . . . . ? C8 N10 C16 N8 81.7(16) . . . . ? C12 N8 C16 N10 115.4(13) . . . . ? C9 N8 C16 N10 -86.6(14) . . . . ? O1A C1A N2A C3A 180.00(11) . . . . ? N6A C1A N2A C3A 0.0 . . . . ? C1A N2A C3A N1B 179(2) . . . . ? C1A N2A C3A N4A 0.0 . . . . ? N1B C3A N4A C5A -179.4(19) . . . . ? N2A C3A N4A C5A 0.0 . . . . ? C3A N4A C5A N1C 179(2) . . . . ? C3A N4A C5A N6A 0.0 . . . . ? N1C C5A N6A C1A -179(2) . . . . ? N4A C5A N6A C1A 0.0 . . . . ? O1A C1A N6A C5A 180.00(11) . . . . ? N2A C1A N6A C5A 0.0 . . . . ? N2A C3A N1B C2B -176.8(12) . . . . ? N4A C3A N1B C2B 3(3) . . . . ? C3A N1B C2B C3B 127(2) . . . . ? C3A N1B C2B C7B -52(2) . . . . ? C7B C2B C3B C4B -0.7 . . . . ? N1B C2B C3B C4B 179.62(9) . . . . ? C2B C3B C4B C5B 0.7 . . . . ? C3B C4B C5B C6B -0.3 . . . . ? C3B C4B C5B C8B 179.5(4) . . . . ? C4B C5B C6B C7B 0.0 . . . . ? C8B C5B C6B C7B -179.9(4) . . . . ? C5B C6B C7B C2B 0.0 . . . . ? C3B C2B C7B C6B 0.3 . . . . ? N1B C2B C7B C6B -179.94(9) . . . . ? C6B C5B C8B N9B -82(2) . . . . ? C4B C5B C8B N9B 99(2) . . . . ? N4A C5A N1C C2C -4(3) . . . . ? N6A C5A N1C C2C 175.1(9) . . . . ? C5A N1C C2C C3C -2(2) . . . . ? C5A N1C C2C C7C 178(2) . . . . ? C7C C2C C3C C4C 0.0 . . . . ? N1C C2C C3C C4C -179.99(10) . . . . ? C2C C3C C4C C5C 0.0 . . . . ? C3C C4C C5C C6C 0.0 . . . . ? C3C C4C C5C C8C -179.9(4) . . . . ? C4C C5C C6C C7C 0.0 . . . . ? C8C C5C C6C C7C 179.9(4) . . . . ? C5C C6C C7C C2C 0.0 . . . . ? C3C C2C C7C C6C 0.0 . . . . ? N1C C2C C7C C6C 179.99(9) . . . . ? C4C C5C C8C N9C 73(3) . . . . ? C6C C5C C8C N9C -107(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N6A H6A O5W 0.87 1.74 2.49(3) 144.1 . N1B H1B O4 0.87 2.36 2.84(2) 114.7 . N9B H9B1 O1 0.90 1.92 2.80(2) 165.7 . N9B H9B2 O12W 0.90 1.73 2.57(5) 154.5 2_655 N9B H9B3 O3 0.90 2.02 2.84(3) 151.0 . N1C H1C O5 0.87 2.67 3.36(2) 137.1 2_655 N9C H9C1 O5W 0.90 2.41 3.19(5) 145.6 2_655 N9C H9C2 O16W 0.90 2.03 2.72(5) 133.2 2_655 N9C H9C3 O6 0.90 2.23 2.89(4) 129.8 2_655 loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_2 _geom_contact_publ_flag I1 O9W 3.36(6) . ? I1 O19W 3.52(6) 6 ? I1 O19W 3.52(6) . ? I1 O4W 3.96(6) . ? I2 O10W 3.44(5) 5_665 ? I2 O18W 3.55(6) 5_665 ? I2 O4W 3.84(6) 5_665 ? I2 O17W 3.88(5) 2_665 ? I2 O17W 3.88(5) 5_665 ? O2 O1W 2.96(2) . ? O2 O1W 2.96(2) 6 ? O4 O20w 2.86(5) 4 ? O5 O8w 2.81(2) 1_545 ? O1W O1W 2.76(5) 6 ? O1W O17W 2.91(6) 5_665 ? O1W O11W 2.97(8) 6_556 ? O2W O16W 2.69(5) 6 ? O2W O16W 2.69(5) . ? O2W O4W 2.85(8) . ? O3W O9W 2.50(16) . ? O3W O5W 2.89(7) 6 ? O3W O5W 2.89(7) . ? O3W O18W 2.96(13) . ? O4W O15W 2.62(11) . ? O5W O8W 2.63(4) 2_665 ? O5W O15W 2.64(6) . ? O7W O11W 2.22(10) 8_655 ? O7W O17W 2.57(10) 8_656 ? O7W O20W 2.74(10) . ? O7W O8W 2.76(7) 2_665 ? O8W O5W 2.63(4) 2_665 ? O8W O7W 2.76(7) 2_665 ? O8W O14W 2.87(7) 2_665 ? O11W O1W 2.97(8) 6_556 ? O12W O19W 2.79(10) 6 ? O12W O12W 3.06(9) 2 ? O14W O19W 2.62(12) . ? O14W O8W 2.87(7) 2_665 ? O15W O5W 2.64(6) 6 ? O15W O19W 3.17(15) 6 ? O15W O19W 3.17(15) . ? O16W O20W 3.07(9) 4 ? O17W O7W 2.57(10) 8_665 ? O17W O1W 2.91(6) 5_665 ? O19W O12W 2.79(10) 6 ? O20W O16W 3.07(9) 4_455 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.632 _refine_diff_density_min -1.003 _refine_diff_density_rms 0.150 _exptl_crystal_id 'Isaacs/Liu 1050B+KI #2 @-40C redo from non-split crystal' _diffrn_measurement_total_frames-CCD 1868 _diffrn_measurement_details NFRAMES=606,606,606,50 _diffrn_measurement_frame_width-CCD 0.3 _diffrn_detector_distance-CCD 4.99 _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_measurement_frame_time-CCD 15 _diffrn_measurement_total_time-CCD 11.5 _diffrn_measurement_frame_size-CCD 512 _diffrn_orient_matrix_type standard _diffrn_orient_matrix_UB_11 -0.0189565 _diffrn_orient_matrix_UB_12 0.0464241 _diffrn_orient_matrix_UB_13 0.0118754 _diffrn_orient_matrix_UB_21 0.0316626 _diffrn_orient_matrix_UB_22 0.0212636 _diffrn_orient_matrix_UB_23 -0.0344186 _diffrn_orient_matrix_UB_31 -0.0392302 _diffrn_orient_matrix_UB_32 -0.0053766 _diffrn_orient_matrix_UB_33 -0.0335718 _symmetry_space_group_name_Hall '-P 2 2n' _diffrn_measurement_specimen_support 'glass capillary' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker Smart1000' #_______________________________________________________________________________ # _publ_section_references ; Bruker (1999). SMART and SAINT. Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1990). Acta Cryst. A46, 467-473. Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany. Sheldrick, G. M. (1997). SHELXL-97. University of G\"ottingen, Germany. Spek, A. L. (1990). Acta Cryst., A46, C-34. ; #===END