# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mn2088 #TrackingRef 'CIF (1)' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common In(S2CNCy2)3.2py _chemical_melting_point ? _chemical_formula_moiety 'C39 H66 In N3 S6, 2(C5 H5 N)' _chemical_formula_sum 'C49 H76 In N5 S6' _chemical_formula_weight 1042.33 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.5733(2) _cell_length_b 22.1491(6) _cell_length_c 22.3726(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.804(2) _cell_angle_gamma 90.00 _cell_volume 5236.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6941 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 21.8 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2200 _exptl_absorpt_coefficient_mu 0.728 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8389 _exptl_absorpt_correction_T_max 0.9785 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker SMART Apex II' _diffrn_measurement_method '\w and \f' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 49516 _diffrn_reflns_av_R_equivalents 0.0679 _diffrn_reflns_av_sigmaI/netI 0.0633 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.49 _reflns_number_total 12019 _reflns_number_gt 8749 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2009)' _computing_cell_refinement 'SAINT (Bruker, 2011)' _computing_data_reduction 'SAINT (Bruker, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL, XP (Bruker, 1997)' _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' _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. The two molecules of pyridine were disordered into two orientations. The two sets of atoms comprising the pyridine molecules were refined as rigid idealized hexagonal groups with occupanices that were initially refined and then fixed at {0.50/0.50} and {0.30/0.70} for the sets involving N4 and N5, respectively. These atoms were also kept isotropic. ; _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^)+(0.0379P)^2^+7.3089P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12019 _refine_ls_number_parameters 490 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1055 _refine_ls_wR_factor_gt 0.0949 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.001 _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 In1 In 0.18160(2) 0.296896(10) 0.537572(11) 0.01794(7) Uani 1 1 d . . . S1 S 0.40229(8) 0.25602(4) 0.57045(4) 0.0247(2) Uani 1 1 d . . . S2 S 0.16392(8) 0.22187(4) 0.62610(4) 0.02360(19) Uani 1 1 d . . . S3 S 0.16454(8) 0.23074(4) 0.44203(4) 0.02339(19) Uani 1 1 d . . . S4 S -0.05250(8) 0.28301(4) 0.50312(4) 0.02143(18) Uani 1 1 d . . . S5 S 0.23947(8) 0.39307(4) 0.47888(4) 0.02061(18) Uani 1 1 d . . . S6 S 0.17405(8) 0.39116(4) 0.60563(4) 0.02147(18) Uani 1 1 d . . . N1 N 0.3902(3) 0.17750(13) 0.66178(13) 0.0208(6) Uani 1 1 d . . . N2 N -0.0754(3) 0.21349(12) 0.40484(13) 0.0218(6) Uani 1 1 d . . . N3 N 0.2374(2) 0.49291(12) 0.54697(12) 0.0175(6) Uani 1 1 d . . . C1 C 0.3276(3) 0.21440(15) 0.62376(15) 0.0214(7) Uani 1 1 d . . . C2 C 0.5299(3) 0.16791(16) 0.66315(17) 0.0256(8) Uani 1 1 d . . . H2 H 0.5468 0.1395 0.6972 0.031 Uiso 1 1 calc R . . C3 C 0.6064(4) 0.22412(18) 0.67875(18) 0.0325(9) Uani 1 1 d . . . H3A H 0.5761 0.2419 0.7163 0.039 Uiso 1 1 calc R . . H3B H 0.5951 0.2544 0.6465 0.039 Uiso 1 1 calc R . . C4 C 0.7466(4) 0.2079(2) 0.6865(2) 0.0460(12) Uani 1 1 d . . . H4A H 0.7963 0.2454 0.6924 0.055 Uiso 1 1 calc R . . H4B H 0.7589 0.1829 0.7228 0.055 Uiso 1 1 calc R . . C5 C 0.7958(4) 0.1741(3) 0.6336(2) 0.0540(14) Uani 1 1 d . . . H5A H 0.8842 0.1614 0.6426 0.065 Uiso 1 1 calc R . . H5B H 0.7963 0.2014 0.5986 0.065 Uiso 1 1 calc R . . C6 C 0.7172(4) 0.1190(2) 0.61809(19) 0.0414(11) Uani 1 1 d . . . H6A H 0.7265 0.0891 0.6508 0.050 Uiso 1 1 calc R . . H6B H 0.7486 0.1004 0.5812 0.050 Uiso 1 1 calc R . . C7 C 0.5765(4) 0.13521(19) 0.60865(18) 0.0341(9) Uani 1 1 d . . . H7A H 0.5653 0.1613 0.5729 0.041 Uiso 1 1 calc R . . H7B H 0.5264 0.0979 0.6018 0.041 Uiso 1 1 calc R . . C8 C 0.3217(3) 0.14453(16) 0.70898(16) 0.0236(8) Uani 1 1 d . . . H8A H 0.2294 0.1527 0.7019 0.028 Uiso 1 1 calc R . . C9 C 0.3572(4) 0.1693(2) 0.77038(18) 0.0411(11) Uani 1 1 d . . . H9A H 0.3400 0.2132 0.7714 0.049 Uiso 1 1 calc R . . H9B H 0.4488 0.1632 0.7788 0.049 Uiso 1 1 calc R . . C10 C 0.2813(5) 0.1375(2) 0.81832(19) 0.0485(12) Uani 1 1 d . . . H10A H 0.3106 0.1518 0.8583 0.058 Uiso 1 1 calc R . . H10B H 0.1908 0.1482 0.8129 0.058 Uiso 1 1 calc R . . C11 C 0.2959(4) 0.0697(2) 0.8152(2) 0.0483(12) Uani 1 1 d . . . H11A H 0.3845 0.0587 0.8259 0.058 Uiso 1 1 calc R . . H11B H 0.2406 0.0506 0.8446 0.058 Uiso 1 1 calc R . . C12 C 0.2621(4) 0.04597(19) 0.7537(2) 0.0414(11) Uani 1 1 d . . . H12A H 0.1708 0.0527 0.7449 0.050 Uiso 1 1 calc R . . H12B H 0.2778 0.0019 0.7527 0.050 Uiso 1 1 calc R . . C13 C 0.3392(4) 0.07679(18) 0.7054(2) 0.0414(11) Uani 1 1 d . . . H13A H 0.4299 0.0666 0.7113 0.050 Uiso 1 1 calc R . . H13B H 0.3106 0.0622 0.6654 0.050 Uiso 1 1 calc R . . C14 C 0.0020(3) 0.23936(14) 0.44534(15) 0.0195(7) Uani 1 1 d . . . C15 C -0.0243(3) 0.17635(16) 0.35531(16) 0.0267(8) Uani 1 1 d . . . H15 H 0.0699 0.1774 0.3609 0.032 Uiso 1 1 calc R . . C16 C -0.0623(4) 0.11050(16) 0.36077(17) 0.0287(8) Uani 1 1 d . . . H16A H -0.1557 0.1072 0.3583 0.034 Uiso 1 1 calc R . . H16B H -0.0327 0.0947 0.4002 0.034 Uiso 1 1 calc R . . C17 C -0.0058(4) 0.07294(18) 0.31144(18) 0.0361(10) Uani 1 1 d . . . H17A H 0.0874 0.0717 0.3174 0.043 Uiso 1 1 calc R . . H17B H -0.0379 0.0311 0.3139 0.043 Uiso 1 1 calc R . . C18 C -0.0383(4) 0.09834(19) 0.24989(18) 0.0387(10) Uani 1 1 d . . . H18A H -0.1307 0.0953 0.2419 0.046 Uiso 1 1 calc R . . H18B H 0.0047 0.0742 0.2193 0.046 Uiso 1 1 calc R . . C19 C 0.0023(4) 0.16391(19) 0.24538(18) 0.0369(10) Uani 1 1 d . . . H19A H -0.0254 0.1801 0.2058 0.044 Uiso 1 1 calc R . . H19B H 0.0958 0.1662 0.2483 0.044 Uiso 1 1 calc R . . C20 C -0.0530(4) 0.20258(19) 0.29418(17) 0.0348(9) Uani 1 1 d . . . H20A H -0.0174 0.2438 0.2921 0.042 Uiso 1 1 calc R . . H20B H -0.1458 0.2055 0.2875 0.042 Uiso 1 1 calc R . . C21 C -0.2155(3) 0.22004(16) 0.40295(17) 0.0265(8) Uani 1 1 d . . . H21A H -0.2442 0.1955 0.3675 0.032 Uiso 1 1 calc R . . C22 C -0.2596(3) 0.28373(17) 0.38784(16) 0.0271(8) Uani 1 1 d . . . H22A H -0.2351 0.3113 0.4211 0.033 Uiso 1 1 calc R . . H22B H -0.2177 0.2978 0.3514 0.033 Uiso 1 1 calc R . . C23 C -0.4022(3) 0.28556(19) 0.37748(19) 0.0358(10) Uani 1 1 d . . . H23A H -0.4296 0.3280 0.3723 0.043 Uiso 1 1 calc R . . H23B H -0.4249 0.2635 0.3402 0.043 Uiso 1 1 calc R . . C24 C -0.4704(4) 0.2582(2) 0.4280(2) 0.0397(10) Uani 1 1 d . . . H24A H -0.5624 0.2581 0.4183 0.048 Uiso 1 1 calc R . . H24B H -0.4559 0.2832 0.4643 0.048 Uiso 1 1 calc R . . C25 C -0.4264(3) 0.19335(18) 0.44096(18) 0.0320(9) Uani 1 1 d . . . H25A H -0.4472 0.1674 0.4060 0.038 Uiso 1 1 calc R . . H25B H -0.4711 0.1772 0.4757 0.038 Uiso 1 1 calc R . . C26 C -0.2822(3) 0.19233(18) 0.45423(17) 0.0308(9) Uani 1 1 d . . . H26A H -0.2621 0.2152 0.4913 0.037 Uiso 1 1 calc R . . H26B H -0.2533 0.1502 0.4602 0.037 Uiso 1 1 calc R . . C27 C 0.2194(3) 0.43335(15) 0.54454(15) 0.0177(7) Uani 1 1 d . . . C28 C 0.2737(3) 0.52639(15) 0.49271(15) 0.0202(7) Uani 1 1 d . . . H28 H 0.2950 0.4956 0.4619 0.024 Uiso 1 1 calc R . . C29 C 0.3902(3) 0.56633(16) 0.50221(16) 0.0242(8) Uani 1 1 d . . . H29A H 0.4613 0.5421 0.5193 0.029 Uiso 1 1 calc R . . H29B H 0.3716 0.5992 0.5306 0.029 Uiso 1 1 calc R . . C30 C 0.4265(3) 0.59317(17) 0.44197(17) 0.0297(9) Uani 1 1 d . . . H30A H 0.5016 0.6195 0.4478 0.036 Uiso 1 1 calc R . . H30B H 0.4486 0.5602 0.4143 0.036 Uiso 1 1 calc R . . C31 C 0.3172(3) 0.62974(17) 0.41494(18) 0.0303(9) Uani 1 1 d . . . H31A H 0.3011 0.6650 0.4408 0.036 Uiso 1 1 calc R . . H31B H 0.3408 0.6450 0.3752 0.036 Uiso 1 1 calc R . . C32 C 0.1973(4) 0.59264(17) 0.40810(17) 0.0303(9) Uani 1 1 d . . . H32A H 0.2094 0.5608 0.3777 0.036 Uiso 1 1 calc R . . H32B H 0.1271 0.6190 0.3937 0.036 Uiso 1 1 calc R . . C33 C 0.1619(3) 0.56331(16) 0.46697(16) 0.0234(8) Uani 1 1 d . . . H33A H 0.0878 0.5366 0.4601 0.028 Uiso 1 1 calc R . . H33B H 0.1386 0.5949 0.4959 0.028 Uiso 1 1 calc R . . C34 C 0.2161(3) 0.53153(16) 0.60032(15) 0.0215(7) Uani 1 1 d . . . H34 H 0.2346 0.5737 0.5873 0.026 Uiso 1 1 calc R . . C35 C 0.0785(3) 0.53210(17) 0.61885(18) 0.0291(8) Uani 1 1 d . . . H35A H 0.0524 0.4908 0.6300 0.035 Uiso 1 1 calc R . . H35B H 0.0234 0.5456 0.5848 0.035 Uiso 1 1 calc R . . C36 C 0.0632(4) 0.5747(2) 0.6720(2) 0.0452(12) Uani 1 1 d . . . H36A H 0.0795 0.6168 0.6593 0.054 Uiso 1 1 calc R . . H36B H -0.0249 0.5726 0.6856 0.054 Uiso 1 1 calc R . . C37 C 0.1529(4) 0.5585(2) 0.7230(2) 0.0524(14) Uani 1 1 d . . . H37A H 0.1329 0.5174 0.7375 0.063 Uiso 1 1 calc R . . H37B H 0.1416 0.5871 0.7564 0.063 Uiso 1 1 calc R . . C38 C 0.2896(4) 0.5604(2) 0.70416(18) 0.0374(10) Uani 1 1 d . . . H38A H 0.3458 0.5480 0.7382 0.045 Uiso 1 1 calc R . . H38B H 0.3120 0.6022 0.6931 0.045 Uiso 1 1 calc R . . C39 C 0.3105(4) 0.51841(17) 0.65101(16) 0.0282(8) Uani 1 1 d . . . H39A H 0.3975 0.5239 0.6368 0.034 Uiso 1 1 calc R . . H39B H 0.3014 0.4759 0.6639 0.034 Uiso 1 1 calc R . . N4 N -0.1275(7) -0.0853(3) 0.4707(3) 0.091(4) Uiso 0.50 1 d PG A 1 C40 C -0.0757(5) -0.0279(4) 0.4772(4) 0.078(4) Uiso 0.50 1 d PG A 1 H40 H 0.0125 -0.0220 0.4727 0.093 Uiso 0.50 1 calc PR A 1 C41 C -0.1528(8) 0.0208(3) 0.4903(4) 0.106(5) Uiso 0.50 1 d PG A 1 H41 H -0.1174 0.0600 0.4947 0.127 Uiso 0.50 1 calc PR A 1 C42 C -0.2819(7) 0.0122(3) 0.4968(4) 0.081(4) Uiso 0.50 1 d PG A 1 H42 H -0.3346 0.0455 0.5057 0.098 Uiso 0.50 1 calc PR A 1 C43 C -0.3338(5) -0.0452(4) 0.4902(4) 0.071(3) Uiso 0.50 1 d PG A 1 H43 H -0.4220 -0.0511 0.4947 0.085 Uiso 0.50 1 calc PR A 1 C44 C -0.2566(7) -0.0939(3) 0.4772(3) 0.057(3) Uiso 0.50 1 d PG A 1 H44 H -0.2920 -0.1332 0.4727 0.069 Uiso 0.50 1 calc PR A 1 N4B N -0.2710(7) 0.0077(3) 0.4381(3) 0.076(3) Uiso 0.50 1 d PG B 2 C40B C -0.3554(6) 0.0139(3) 0.4841(3) 0.059(3) Uiso 0.50 1 d PG B 2 H40B H -0.4100 0.0479 0.4850 0.070 Uiso 0.50 1 calc PR B 2 C41B C -0.3598(7) -0.0297(4) 0.5287(3) 0.091(4) Uiso 0.50 1 d PG B 2 H41B H -0.4175 -0.0255 0.5601 0.110 Uiso 0.50 1 calc PR B 2 C42B C -0.2798(7) -0.0795(3) 0.5273(3) 0.068(3) Uiso 0.50 1 d PG B 2 H42B H -0.2828 -0.1093 0.5577 0.082 Uiso 0.50 1 calc PR B 2 C43B C -0.1954(6) -0.0857(3) 0.4813(3) 0.043(2) Uiso 0.50 1 d PG B 2 H43B H -0.1408 -0.1197 0.4803 0.051 Uiso 0.50 1 calc PR B 2 C44B C -0.1910(6) -0.0421(3) 0.4367(3) 0.074(3) Uiso 0.50 1 d PG B 2 H44B H -0.1334 -0.0463 0.4052 0.088 Uiso 0.50 1 calc PR B 2 N5 N 0.5579(14) -0.0598(5) 0.6661(6) 0.105(7) Uiso 0.30 1 d PG C 1 C45 C 0.5056(13) -0.0582(6) 0.7223(7) 0.104(8) Uiso 0.30 1 d PG C 1 H45 H 0.4510 -0.0259 0.7326 0.124 Uiso 0.30 1 calc PR C 1 C46 C 0.5330(12) -0.1037(6) 0.7635(5) 0.089(8) Uiso 0.30 1 d PG C 1 H46 H 0.4973 -0.1025 0.8019 0.107 Uiso 0.30 1 calc PR C 1 C47 C 0.6128(11) -0.1508(5) 0.7485(5) 0.046(4) Uiso 0.30 1 d PG C 1 H47 H 0.6316 -0.1819 0.7766 0.055 Uiso 0.30 1 calc PR C 1 C48 C 0.6652(10) -0.1524(5) 0.6923(5) 0.054(4) Uiso 0.30 1 d PG C 1 H48 H 0.7197 -0.1846 0.6820 0.065 Uiso 0.30 1 calc PR C 1 C49 C 0.6377(13) -0.1069(6) 0.6511(4) 0.081(6) Uiso 0.30 1 d PG C 1 H49 H 0.6735 -0.1080 0.6127 0.097 Uiso 0.30 1 calc PR C 1 N5B N 0.3929(3) -0.0926(2) 0.6948(2) 0.0558(15) Uiso 0.70 1 d PG D 2 C45B C 0.4884(4) -0.0642(2) 0.66409(18) 0.068(2) Uiso 0.70 1 d PG D 2 H45B H 0.4688 -0.0432 0.6280 0.081 Uiso 0.70 1 calc PR D 2 C46B C 0.6126(4) -0.0666(2) 0.6862(2) 0.058(2) Uiso 0.70 1 d PG D 2 H46B H 0.6779 -0.0472 0.6652 0.069 Uiso 0.70 1 calc PR D 2 C47B C 0.6413(3) -0.0974(2) 0.7391(2) 0.0574(19) Uiso 0.70 1 d PG D 2 H47B H 0.7262 -0.0990 0.7542 0.069 Uiso 0.70 1 calc PR D 2 C48B C 0.5457(4) -0.1258(2) 0.76978(17) 0.0425(16) Uiso 0.70 1 d PG D 2 H48B H 0.5653 -0.1468 0.8059 0.051 Uiso 0.70 1 calc PR D 2 C49B C 0.4215(3) -0.1234(2) 0.74765(19) 0.0546(18) Uiso 0.70 1 d PG D 2 H49B H 0.3562 -0.1428 0.7686 0.066 Uiso 0.70 1 calc PR D 2 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 In1 0.01816(11) 0.01662(11) 0.01869(12) -0.00049(10) -0.00498(8) -0.00097(10) S1 0.0189(4) 0.0311(5) 0.0241(5) 0.0085(4) -0.0013(3) 0.0000(4) S2 0.0194(4) 0.0250(5) 0.0263(5) 0.0044(4) -0.0004(3) 0.0004(3) S3 0.0181(4) 0.0240(5) 0.0279(5) -0.0074(4) -0.0018(3) 0.0013(3) S4 0.0188(4) 0.0222(4) 0.0231(5) -0.0060(3) -0.0024(3) 0.0011(3) S5 0.0279(4) 0.0185(4) 0.0154(4) -0.0026(3) -0.0003(3) -0.0013(3) S6 0.0279(4) 0.0205(4) 0.0159(4) -0.0005(3) -0.0004(3) -0.0046(3) N1 0.0201(14) 0.0217(15) 0.0205(16) 0.0025(12) -0.0013(12) -0.0004(12) N2 0.0192(14) 0.0219(16) 0.0240(16) -0.0031(12) -0.0040(12) -0.0013(12) N3 0.0161(13) 0.0195(14) 0.0170(15) -0.0046(11) 0.0003(11) -0.0017(11) C1 0.0234(17) 0.0230(18) 0.0175(18) -0.0002(13) -0.0046(13) -0.0006(14) C2 0.0197(17) 0.028(2) 0.029(2) 0.0043(15) -0.0040(15) 0.0004(15) C3 0.032(2) 0.033(2) 0.032(2) 0.0092(17) -0.0066(17) -0.0098(17) C4 0.030(2) 0.064(3) 0.044(3) 0.018(2) -0.0122(19) -0.015(2) C5 0.024(2) 0.092(4) 0.046(3) 0.027(3) 0.001(2) -0.005(2) C6 0.031(2) 0.061(3) 0.033(2) 0.013(2) 0.0076(18) 0.016(2) C7 0.030(2) 0.040(2) 0.032(2) 0.0043(18) 0.0008(17) 0.0027(18) C8 0.0244(18) 0.0235(18) 0.0229(19) 0.0050(14) 0.0006(15) -0.0010(14) C9 0.058(3) 0.042(3) 0.024(2) -0.0015(18) 0.0004(19) -0.019(2) C10 0.065(3) 0.059(3) 0.022(2) 0.002(2) 0.008(2) -0.022(3) C11 0.040(2) 0.057(3) 0.048(3) 0.029(2) 0.003(2) -0.005(2) C12 0.041(2) 0.026(2) 0.058(3) 0.005(2) 0.023(2) -0.0015(18) C13 0.045(2) 0.028(2) 0.053(3) 0.001(2) 0.023(2) -0.0082(19) C14 0.0225(17) 0.0138(16) 0.0221(18) 0.0023(13) -0.0023(14) 0.0001(13) C15 0.0268(18) 0.0264(19) 0.027(2) -0.0091(15) -0.0023(15) -0.0001(15) C16 0.036(2) 0.0240(19) 0.026(2) -0.0037(15) 0.0020(16) 0.0048(16) C17 0.046(2) 0.028(2) 0.034(2) -0.0059(17) -0.0042(19) 0.0069(18) C18 0.048(3) 0.043(3) 0.026(2) -0.0126(18) 0.0021(18) 0.008(2) C19 0.039(2) 0.046(3) 0.025(2) 0.0001(18) 0.0054(17) 0.0050(19) C20 0.044(2) 0.032(2) 0.029(2) 0.0004(18) 0.0102(17) -0.0003(19) C21 0.0182(17) 0.0263(19) 0.034(2) 0.0006(16) -0.0068(15) -0.0046(14) C22 0.0277(19) 0.033(2) 0.0205(19) 0.0025(15) 0.0029(15) 0.0057(16) C23 0.029(2) 0.040(2) 0.038(2) 0.0014(18) -0.0086(17) 0.0063(17) C24 0.027(2) 0.052(3) 0.040(3) 0.001(2) 0.0012(18) 0.0036(19) C25 0.0293(19) 0.040(2) 0.027(2) -0.0011(17) 0.0055(16) -0.0067(17) C26 0.0304(19) 0.033(2) 0.029(2) 0.0011(16) -0.0029(16) -0.0015(17) C27 0.0140(15) 0.0219(17) 0.0172(17) -0.0017(13) -0.0034(13) -0.0014(13) C28 0.0237(17) 0.0197(17) 0.0172(18) -0.0016(13) 0.0018(14) -0.0005(14) C29 0.0147(16) 0.0258(19) 0.032(2) 0.0020(15) 0.0007(14) 0.0006(14) C30 0.0260(19) 0.028(2) 0.036(2) 0.0033(16) 0.0091(16) -0.0021(16) C31 0.034(2) 0.026(2) 0.032(2) 0.0058(16) 0.0085(17) -0.0045(16) C32 0.035(2) 0.028(2) 0.027(2) 0.0064(16) -0.0047(17) -0.0025(17) C33 0.0210(17) 0.0229(18) 0.026(2) 0.0040(15) -0.0019(14) -0.0033(14) C34 0.0250(17) 0.0214(18) 0.0184(18) -0.0081(14) 0.0034(14) -0.0035(14) C35 0.0255(19) 0.026(2) 0.036(2) -0.0093(17) 0.0067(16) -0.0048(15) C36 0.036(2) 0.047(3) 0.054(3) -0.026(2) 0.023(2) -0.017(2) C37 0.058(3) 0.066(3) 0.034(3) -0.025(2) 0.018(2) -0.033(3) C38 0.045(2) 0.044(2) 0.023(2) -0.0104(18) 0.0044(18) -0.019(2) C39 0.034(2) 0.0256(19) 0.025(2) -0.0051(15) -0.0054(16) -0.0083(16) _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 In1 S5 2.5859(9) . ? In1 S6 2.5867(9) . ? In1 S4 2.5875(8) . ? In1 S1 2.5879(9) . ? In1 S3 2.5933(9) . ? In1 S2 2.5966(9) . ? S1 C1 1.719(4) . ? S2 C1 1.741(3) . ? S3 C14 1.733(3) . ? S4 C14 1.728(4) . ? S5 C27 1.737(3) . ? S6 C27 1.736(3) . ? N1 C1 1.339(4) . ? N1 C8 1.490(4) . ? N1 C2 1.492(4) . ? N2 C14 1.332(4) . ? N2 C21 1.488(4) . ? N2 C15 1.495(4) . ? N3 C27 1.334(4) . ? N3 C28 1.483(4) . ? N3 C34 1.491(4) . ? C2 C7 1.514(5) . ? C2 C3 1.520(5) . ? C2 H2 1.0000 . ? C3 C4 1.529(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.508(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.510(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.538(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C13 1.514(5) . ? C8 C9 1.516(5) . ? C8 H8A 1.0000 . ? C9 C10 1.531(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.512(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.506(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.534(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C15 C20 1.508(5) . ? C15 C16 1.519(5) . ? C15 H15 1.0000 . ? C16 C17 1.520(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.517(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.519(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.519(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C26 1.497(5) . ? C21 C22 1.520(5) . ? C21 H21A 1.0000 . ? C22 C23 1.519(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.489(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.535(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.544(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C28 C29 1.526(5) . ? C28 C33 1.534(5) . ? C28 H28 1.0000 . ? C29 C30 1.533(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.521(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.514(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.526(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C39 1.515(5) . ? C34 C35 1.526(5) . ? C34 H34 1.0000 . ? C35 C36 1.531(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.505(7) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.519(6) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.531(5) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? N4 C40 1.3900 . ? N4 C44 1.3900 . ? C40 C41 1.3900 . ? C40 H40 0.9500 . ? C41 C42 1.3900 . ? C41 H41 0.9500 . ? C42 C43 1.3900 . ? C42 H42 0.9500 . ? C43 C44 1.3900 . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? N4B C40B 1.3900 . ? N4B C44B 1.3900 . ? C40B C41B 1.3900 . ? C40B H40B 0.9500 . ? C41B C42B 1.3900 . ? C41B H41B 0.9500 . ? C42B C43B 1.3900 . ? C42B H42B 0.9500 . ? C43B C44B 1.3900 . ? C43B H43B 0.9500 . ? C44B H44B 0.9500 . ? N5 C45 1.3900 . ? N5 C49 1.3900 . ? C45 C46 1.3900 . ? C45 H45 0.9500 . ? C46 C47 1.3900 . ? C46 H46 0.9500 . ? C47 C48 1.3900 . ? C47 H47 0.9500 . ? C48 C49 1.3900 . ? C48 H48 0.9500 . ? C49 H49 0.9500 . ? N5B C45B 1.3900 . ? N5B C49B 1.3900 . ? C45B C46B 1.3900 . ? C45B H45B 0.9500 . ? C46B C47B 1.3900 . ? C46B H46B 0.9500 . ? C47B C48B 1.3900 . ? C47B H47B 0.9500 . ? C48B C49B 1.3900 . ? C48B H48B 0.9500 . ? C49B H49B 0.9500 . ? 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 S5 In1 S6 69.28(3) . . ? S5 In1 S4 100.72(3) . . ? S6 In1 S4 102.96(3) . . ? S5 In1 S1 101.94(3) . . ? S6 In1 S1 99.17(3) . . ? S4 In1 S1 152.69(3) . . ? S5 In1 S3 93.35(3) . . ? S6 In1 S3 159.82(3) . . ? S4 In1 S3 69.28(3) . . ? S1 In1 S3 94.32(3) . . ? S5 In1 S2 159.78(3) . . ? S6 In1 S2 93.63(3) . . ? S4 In1 S2 93.44(3) . . ? S1 In1 S2 69.22(3) . . ? S3 In1 S2 105.21(3) . . ? C1 S1 In1 87.44(11) . . ? C1 S2 In1 86.70(12) . . ? C14 S3 In1 86.90(12) . . ? C14 S4 In1 87.18(11) . . ? C27 S5 In1 87.51(11) . . ? C27 S6 In1 87.52(11) . . ? C1 N1 C8 120.5(3) . . ? C1 N1 C2 124.7(3) . . ? C8 N1 C2 114.8(3) . . ? C14 N2 C21 124.6(3) . . ? C14 N2 C15 120.8(3) . . ? C21 N2 C15 114.6(3) . . ? C27 N3 C28 120.1(3) . . ? C27 N3 C34 125.1(3) . . ? C28 N3 C34 114.7(3) . . ? N1 C1 S1 122.7(3) . . ? N1 C1 S2 120.7(3) . . ? S1 C1 S2 116.64(19) . . ? N1 C2 C7 113.5(3) . . ? N1 C2 C3 114.1(3) . . ? C7 C2 C3 113.1(3) . . ? N1 C2 H2 105.0 . . ? C7 C2 H2 105.0 . . ? C3 C2 H2 105.0 . . ? C2 C3 C4 109.9(3) . . ? C2 C3 H3A 109.7 . . ? C4 C3 H3A 109.7 . . ? C2 C3 H3B 109.7 . . ? C4 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? C5 C4 C3 112.7(3) . . ? C5 C4 H4A 109.1 . . ? C3 C4 H4A 109.1 . . ? C5 C4 H4B 109.1 . . ? C3 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? C4 C5 C6 112.3(4) . . ? C4 C5 H5A 109.1 . . ? C6 C5 H5A 109.1 . . ? C4 C5 H5B 109.1 . . ? C6 C5 H5B 109.1 . . ? H5A C5 H5B 107.9 . . ? C5 C6 C7 111.5(4) . . ? C5 C6 H6A 109.3 . . ? C7 C6 H6A 109.3 . . ? C5 C6 H6B 109.3 . . ? C7 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? C2 C7 C6 109.8(3) . . ? C2 C7 H7A 109.7 . . ? C6 C7 H7A 109.7 . . ? C2 C7 H7B 109.7 . . ? C6 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? N1 C8 C13 112.6(3) . . ? N1 C8 C9 110.6(3) . . ? C13 C8 C9 112.3(3) . . ? N1 C8 H8A 107.0 . . ? C13 C8 H8A 107.0 . . ? C9 C8 H8A 107.0 . . ? C8 C9 C10 110.4(3) . . ? C8 C9 H9A 109.6 . . ? C10 C9 H9A 109.6 . . ? C8 C9 H9B 109.6 . . ? C10 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? C11 C10 C9 111.6(4) . . ? C11 C10 H10A 109.3 . . ? C9 C10 H10A 109.3 . . ? C11 C10 H10B 109.3 . . ? C9 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C12 C11 C10 111.6(4) . . ? C12 C11 H11A 109.3 . . ? C10 C11 H11A 109.3 . . ? C12 C11 H11B 109.3 . . ? C10 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? C11 C12 C13 111.8(4) . . ? C11 C12 H12A 109.2 . . ? C13 C12 H12A 109.2 . . ? C11 C12 H12B 109.2 . . ? C13 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C8 C13 C12 109.6(3) . . ? C8 C13 H13A 109.8 . . ? C12 C13 H13A 109.8 . . ? C8 C13 H13B 109.8 . . ? C12 C13 H13B 109.8 . . ? H13A C13 H13B 108.2 . . ? N2 C14 S4 122.5(3) . . ? N2 C14 S3 120.9(3) . . ? S4 C14 S3 116.64(19) . . ? N2 C15 C20 113.2(3) . . ? N2 C15 C16 111.5(3) . . ? C20 C15 C16 113.4(3) . . ? N2 C15 H15 106.1 . . ? C20 C15 H15 106.1 . . ? C16 C15 H15 106.1 . . ? C15 C16 C17 110.9(3) . . ? C15 C16 H16A 109.5 . . ? C17 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C18 C17 C16 111.9(3) . . ? C18 C17 H17A 109.2 . . ? C16 C17 H17A 109.2 . . ? C18 C17 H17B 109.2 . . ? C16 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? C17 C18 C19 111.0(3) . . ? C17 C18 H18A 109.4 . . ? C19 C18 H18A 109.4 . . ? C17 C18 H18B 109.4 . . ? C19 C18 H18B 109.4 . . ? H18A C18 H18B 108.0 . . ? C18 C19 C20 112.0(3) . . ? C18 C19 H19A 109.2 . . ? C20 C19 H19A 109.2 . . ? C18 C19 H19B 109.2 . . ? C20 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? C15 C20 C19 111.3(3) . . ? C15 C20 H20A 109.4 . . ? C19 C20 H20A 109.4 . . ? C15 C20 H20B 109.4 . . ? C19 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? N2 C21 C26 115.5(3) . . ? N2 C21 C22 113.3(3) . . ? C26 C21 C22 113.7(3) . . ? N2 C21 H21A 104.2 . . ? C26 C21 H21A 104.2 . . ? C22 C21 H21A 104.2 . . ? C23 C22 C21 110.8(3) . . ? C23 C22 H22A 109.5 . . ? C21 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C24 C23 C22 112.1(3) . . ? C24 C23 H23A 109.2 . . ? C22 C23 H23A 109.2 . . ? C24 C23 H23B 109.2 . . ? C22 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C23 C24 C25 111.9(3) . . ? C23 C24 H24A 109.2 . . ? C25 C24 H24A 109.2 . . ? C23 C24 H24B 109.2 . . ? C25 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C24 C25 C26 110.0(3) . . ? C24 C25 H25A 109.7 . . ? C26 C25 H25A 109.7 . . ? C24 C25 H25B 109.7 . . ? C26 C25 H25B 109.7 . . ? H25A C25 H25B 108.2 . . ? C21 C26 C25 109.4(3) . . ? C21 C26 H26A 109.8 . . ? C25 C26 H26A 109.8 . . ? C21 C26 H26B 109.8 . . ? C25 C26 H26B 109.8 . . ? H26A C26 H26B 108.2 . . ? N3 C27 S6 122.9(2) . . ? N3 C27 S5 121.4(3) . . ? S6 C27 S5 115.68(19) . . ? N3 C28 C29 113.8(3) . . ? N3 C28 C33 111.0(3) . . ? C29 C28 C33 110.6(3) . . ? N3 C28 H28 107.0 . . ? C29 C28 H28 107.0 . . ? C33 C28 H28 107.0 . . ? C28 C29 C30 109.0(3) . . ? C28 C29 H29A 109.9 . . ? C30 C29 H29A 109.9 . . ? C28 C29 H29B 109.9 . . ? C30 C29 H29B 109.9 . . ? H29A C29 H29B 108.3 . . ? C31 C30 C29 110.3(3) . . ? C31 C30 H30A 109.6 . . ? C29 C30 H30A 109.6 . . ? C31 C30 H30B 109.6 . . ? C29 C30 H30B 109.6 . . ? H30A C30 H30B 108.1 . . ? C32 C31 C30 112.0(3) . . ? C32 C31 H31A 109.2 . . ? C30 C31 H31A 109.2 . . ? C32 C31 H31B 109.2 . . ? C30 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? C31 C32 C33 111.8(3) . . ? C31 C32 H32A 109.3 . . ? C33 C32 H32A 109.3 . . ? C31 C32 H32B 109.3 . . ? C33 C32 H32B 109.3 . . ? H32A C32 H32B 107.9 . . ? C32 C33 C28 110.1(3) . . ? C32 C33 H33A 109.6 . . ? C28 C33 H33A 109.6 . . ? C32 C33 H33B 109.6 . . ? C28 C33 H33B 109.6 . . ? H33A C33 H33B 108.2 . . ? N3 C34 C39 112.1(3) . . ? N3 C34 C35 113.1(3) . . ? C39 C34 C35 114.2(3) . . ? N3 C34 H34 105.5 . . ? C39 C34 H34 105.5 . . ? C35 C34 H34 105.5 . . ? C34 C35 C36 110.0(3) . . ? C34 C35 H35A 109.7 . . ? C36 C35 H35A 109.7 . . ? C34 C35 H35B 109.7 . . ? C36 C35 H35B 109.7 . . ? H35A C35 H35B 108.2 . . ? C37 C36 C35 111.2(4) . . ? C37 C36 H36A 109.4 . . ? C35 C36 H36A 109.4 . . ? C37 C36 H36B 109.4 . . ? C35 C36 H36B 109.4 . . ? H36A C36 H36B 108.0 . . ? C36 C37 C38 111.4(4) . . ? C36 C37 H37A 109.3 . . ? C38 C37 H37A 109.3 . . ? C36 C37 H37B 109.3 . . ? C38 C37 H37B 109.3 . . ? H37A C37 H37B 108.0 . . ? C37 C38 C39 111.2(3) . . ? C37 C38 H38A 109.4 . . ? C39 C38 H38A 109.4 . . ? C37 C38 H38B 109.4 . . ? C39 C38 H38B 109.4 . . ? H38A C38 H38B 108.0 . . ? C34 C39 C38 110.9(3) . . ? C34 C39 H39A 109.5 . . ? C38 C39 H39A 109.5 . . ? C34 C39 H39B 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 108.0 . . ? C40 N4 C44 120.0 . . ? C41 C40 N4 120.0 . . ? C41 C40 H40 120.0 . . ? N4 C40 H40 120.0 . . ? C42 C41 C40 120.0 . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C41 C42 C43 120.0 . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C44 C43 C42 120.0 . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 N4 120.0 . . ? C43 C44 H44 120.0 . . ? N4 C44 H44 120.0 . . ? C40B N4B C44B 120.0 . . ? N4B C40B C41B 120.0 . . ? N4B C40B H40B 120.0 . . ? C41B C40B H40B 120.0 . . ? C40B C41B C42B 120.0 . . ? C40B C41B H41B 120.0 . . ? C42B C41B H41B 120.0 . . ? C41B C42B C43B 120.0 . . ? C41B C42B H42B 120.0 . . ? C43B C42B H42B 120.0 . . ? C44B C43B C42B 120.0 . . ? C44B C43B H43B 120.0 . . ? C42B C43B H43B 120.0 . . ? C43B C44B N4B 120.0 . . ? C43B C44B H44B 120.0 . . ? N4B C44B H44B 120.0 . . ? C45 N5 C49 120.0 . . ? C46 C45 N5 120.0 . . ? C46 C45 H45 120.0 . . ? N5 C45 H45 120.0 . . ? C45 C46 C47 120.0 . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C48 C47 C46 120.0 . . ? C48 C47 H47 120.0 . . ? C46 C47 H47 120.0 . . ? C47 C48 C49 120.0 . . ? C47 C48 H48 120.0 . . ? C49 C48 H48 120.0 . . ? C48 C49 N5 120.0 . . ? C48 C49 H49 120.0 . . ? N5 C49 H49 120.0 . . ? C45B N5B C49B 120.0 . . ? C46B C45B N5B 120.0 . . ? C46B C45B H45B 120.0 . . ? N5B C45B H45B 120.0 . . ? C45B C46B C47B 120.0 . . ? C45B C46B H46B 120.0 . . ? C47B C46B H46B 120.0 . . ? C48B C47B C46B 120.0 . . ? C48B C47B H47B 120.0 . . ? C46B C47B H47B 120.0 . . ? C47B C48B C49B 120.0 . . ? C47B C48B H48B 120.0 . . ? C49B C48B H48B 120.0 . . ? C48B C49B N5B 120.0 . . ? C48B C49B H49B 120.0 . . ? N5B C49B H49B 120.0 . . ? 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 S5 In1 S1 C1 161.08(12) . . . . ? S6 In1 S1 C1 90.48(12) . . . . ? S4 In1 S1 C1 -53.42(14) . . . . ? S3 In1 S1 C1 -104.58(12) . . . . ? S2 In1 S1 C1 0.06(12) . . . . ? S5 In1 S2 C1 -67.11(14) . . . . ? S6 In1 S2 C1 -98.50(12) . . . . ? S4 In1 S2 C1 158.26(12) . . . . ? S1 In1 S2 C1 -0.06(11) . . . . ? S3 In1 S2 C1 88.81(12) . . . . ? S5 In1 S3 C14 -100.69(11) . . . . ? S6 In1 S3 C14 -70.97(14) . . . . ? S4 In1 S3 C14 -0.48(11) . . . . ? S1 In1 S3 C14 157.06(11) . . . . ? S2 In1 S3 C14 87.43(11) . . . . ? S5 In1 S4 C14 90.02(11) . . . . ? S6 In1 S4 C14 161.00(11) . . . . ? S1 In1 S4 C14 -55.65(13) . . . . ? S3 In1 S4 C14 0.49(11) . . . . ? S2 In1 S4 C14 -104.48(11) . . . . ? S6 In1 S5 C27 0.61(10) . . . . ? S4 In1 S5 C27 100.55(11) . . . . ? S1 In1 S5 C27 -94.79(11) . . . . ? S3 In1 S5 C27 170.08(10) . . . . ? S2 In1 S5 C27 -33.15(14) . . . . ? S5 In1 S6 C27 -0.62(10) . . . . ? S4 In1 S6 C27 -97.34(11) . . . . ? S1 In1 S6 C27 98.76(11) . . . . ? S3 In1 S6 C27 -32.56(14) . . . . ? S2 In1 S6 C27 168.29(11) . . . . ? C8 N1 C1 S1 177.2(2) . . . . ? C2 N1 C1 S1 0.2(5) . . . . ? C8 N1 C1 S2 -3.2(4) . . . . ? C2 N1 C1 S2 179.8(3) . . . . ? In1 S1 C1 N1 179.5(3) . . . . ? In1 S1 C1 S2 -0.10(18) . . . . ? In1 S2 C1 N1 -179.5(3) . . . . ? In1 S2 C1 S1 0.10(18) . . . . ? C1 N1 C2 C7 -68.2(4) . . . . ? C8 N1 C2 C7 114.6(3) . . . . ? C1 N1 C2 C3 63.3(5) . . . . ? C8 N1 C2 C3 -113.8(3) . . . . ? N1 C2 C3 C4 173.1(3) . . . . ? C7 C2 C3 C4 -55.2(4) . . . . ? C2 C3 C4 C5 52.8(5) . . . . ? C3 C4 C5 C6 -53.5(5) . . . . ? C4 C5 C6 C7 54.1(5) . . . . ? N1 C2 C7 C6 -171.6(3) . . . . ? C3 C2 C7 C6 56.4(4) . . . . ? C5 C6 C7 C2 -54.8(5) . . . . ? C1 N1 C8 C13 123.1(4) . . . . ? C2 N1 C8 C13 -59.6(4) . . . . ? C1 N1 C8 C9 -110.3(4) . . . . ? C2 N1 C8 C9 67.0(4) . . . . ? N1 C8 C9 C10 177.0(3) . . . . ? C13 C8 C9 C10 -56.2(5) . . . . ? C8 C9 C10 C11 54.4(5) . . . . ? C9 C10 C11 C12 -54.7(5) . . . . ? C10 C11 C12 C13 55.5(5) . . . . ? N1 C8 C13 C12 -177.9(3) . . . . ? C9 C8 C13 C12 56.4(5) . . . . ? C11 C12 C13 C8 -55.6(5) . . . . ? C21 N2 C14 S4 1.9(5) . . . . ? C15 N2 C14 S4 179.6(2) . . . . ? C21 N2 C14 S3 -177.9(3) . . . . ? C15 N2 C14 S3 -0.1(4) . . . . ? In1 S4 C14 N2 179.5(3) . . . . ? In1 S4 C14 S3 -0.76(17) . . . . ? In1 S3 C14 N2 -179.5(3) . . . . ? In1 S3 C14 S4 0.76(17) . . . . ? C14 N2 C15 C20 -116.5(4) . . . . ? C21 N2 C15 C20 61.5(4) . . . . ? C14 N2 C15 C16 114.4(4) . . . . ? C21 N2 C15 C16 -67.6(4) . . . . ? N2 C15 C16 C17 -178.0(3) . . . . ? C20 C15 C16 C17 53.0(4) . . . . ? C15 C16 C17 C18 -54.0(5) . . . . ? C16 C17 C18 C19 55.5(5) . . . . ? C17 C18 C19 C20 -55.0(5) . . . . ? N2 C15 C20 C19 179.2(3) . . . . ? C16 C15 C20 C19 -52.6(4) . . . . ? C18 C19 C20 C15 53.3(5) . . . . ? C14 N2 C21 C26 -66.6(4) . . . . ? C15 N2 C21 C26 115.5(4) . . . . ? C14 N2 C21 C22 67.1(4) . . . . ? C15 N2 C21 C22 -110.8(3) . . . . ? N2 C21 C22 C23 171.6(3) . . . . ? C26 C21 C22 C23 -53.9(4) . . . . ? C21 C22 C23 C24 52.6(5) . . . . ? C22 C23 C24 C25 -55.5(5) . . . . ? C23 C24 C25 C26 57.1(4) . . . . ? N2 C21 C26 C25 -170.7(3) . . . . ? C22 C21 C26 C25 55.9(4) . . . . ? C24 C25 C26 C21 -56.1(4) . . . . ? C28 N3 C27 S6 -178.8(2) . . . . ? C34 N3 C27 S6 -2.9(4) . . . . ? C28 N3 C27 S5 0.9(4) . . . . ? C34 N3 C27 S5 176.7(2) . . . . ? In1 S6 C27 N3 -179.4(3) . . . . ? In1 S6 C27 S5 0.95(16) . . . . ? In1 S5 C27 N3 179.3(3) . . . . ? In1 S5 C27 S6 -0.95(16) . . . . ? C27 N3 C28 C29 -128.3(3) . . . . ? C34 N3 C28 C29 55.5(4) . . . . ? C27 N3 C28 C33 106.1(3) . . . . ? C34 N3 C28 C33 -70.1(3) . . . . ? N3 C28 C29 C30 174.1(3) . . . . ? C33 C28 C29 C30 -60.2(4) . . . . ? C28 C29 C30 C31 58.7(4) . . . . ? C29 C30 C31 C32 -56.2(4) . . . . ? C30 C31 C32 C33 54.1(4) . . . . ? C31 C32 C33 C28 -54.3(4) . . . . ? N3 C28 C33 C32 -174.7(3) . . . . ? C29 C28 C33 C32 57.9(4) . . . . ? C27 N3 C34 C39 67.9(4) . . . . ? C28 N3 C34 C39 -116.1(3) . . . . ? C27 N3 C34 C35 -62.9(4) . . . . ? C28 N3 C34 C35 113.1(3) . . . . ? N3 C34 C35 C36 -177.5(3) . . . . ? C39 C34 C35 C36 52.7(4) . . . . ? C34 C35 C36 C37 -54.9(5) . . . . ? C35 C36 C37 C38 58.3(5) . . . . ? C36 C37 C38 C39 -57.0(5) . . . . ? N3 C34 C39 C38 177.8(3) . . . . ? C35 C34 C39 C38 -52.0(4) . . . . ? C37 C38 C39 C34 52.9(5) . . . . ? C44 N4 C40 C41 0.0 . . . . ? N4 C40 C41 C42 0.0 . . . . ? C40 C41 C42 C43 0.0 . . . . ? C41 C42 C43 C44 0.0 . . . . ? C42 C43 C44 N4 0.0 . . . . ? C40 N4 C44 C43 0.0 . . . . ? C44B N4B C40B C41B 0.0 . . . . ? N4B C40B C41B C42B 0.0 . . . . ? C40B C41B C42B C43B 0.0 . . . . ? C41B C42B C43B C44B 0.0 . . . . ? C42B C43B C44B N4B 0.0 . . . . ? C40B N4B C44B C43B 0.0 . . . . ? C49 N5 C45 C46 0.0 . . . . ? N5 C45 C46 C47 0.0 . . . . ? C45 C46 C47 C48 0.0 . . . . ? C46 C47 C48 C49 0.0 . . . . ? C47 C48 C49 N5 0.0 . . . . ? C45 N5 C49 C48 0.0 . . . . ? C49B N5B C45B C46B 0.0 . . . . ? N5B C45B C46B C47B 0.0 . . . . ? C45B C46B C47B C48B 0.0 . . . . ? C46B C47B C48B C49B 0.0 . . . . ? C47B C48B C49B N5B 0.0 . . . . ? C45B N5B C49B C48B 0.0 . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.040 _refine_diff_density_min -0.747 _refine_diff_density_rms 0.094 _iucr_refine_instructions_details ; TITL sad in P2(1)/c In(N,N-dicy-dtc)3.2py CELL 0.71073 10.5733 22.1491 22.3726 90.000 91.804 90.000 ZERR 4.00 0.0002 0.0006 0.0006 0.000 0.002 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N S IN UNIT 196 304 20 24 4 TEMP -173 L.S. 12 omit 0 1 1 bond $h conf SIZE 0.03 0.06 0.25 ! colorless acta rem eadp N4 c43b WGHT 0.037900 7.308900 FVAR 0.07819 IN1 5 0.181603 0.296896 0.537572 11.00000 0.01816 0.01662 = 0.01869 -0.00049 -0.00498 -0.00097 S1 4 0.402292 0.256021 0.570449 11.00000 0.01886 0.03108 = 0.02410 0.00848 -0.00128 0.00003 S2 4 0.163925 0.221872 0.626098 11.00000 0.01941 0.02500 = 0.02633 0.00442 -0.00041 0.00041 S3 4 0.164541 0.230737 0.442026 11.00000 0.01811 0.02401 = 0.02789 -0.00744 -0.00183 0.00130 S4 4 -0.052496 0.283008 0.503116 11.00000 0.01876 0.02219 = 0.02314 -0.00603 -0.00243 0.00108 S5 4 0.239473 0.393071 0.478884 11.00000 0.02788 0.01854 = 0.01535 -0.00264 -0.00031 -0.00129 S6 4 0.174054 0.391157 0.605625 11.00000 0.02794 0.02047 = 0.01593 -0.00048 -0.00044 -0.00456 N1 3 0.390172 0.177497 0.661778 11.00000 0.02015 0.02175 = 0.02053 0.00249 -0.00129 -0.00043 N2 3 -0.075440 0.213487 0.404842 11.00000 0.01922 0.02194 = 0.02397 -0.00314 -0.00400 -0.00132 N3 3 0.237440 0.492906 0.546967 11.00000 0.01610 0.01946 = 0.01700 -0.00460 0.00033 -0.00166 C1 1 0.327645 0.214396 0.623758 11.00000 0.02339 0.02298 = 0.01751 -0.00025 -0.00465 -0.00063 C2 1 0.529872 0.167912 0.663148 11.00000 0.01971 0.02778 = 0.02915 0.00433 -0.00396 0.00042 AFIX 13 H2 2 0.546799 0.139536 0.697233 11.00000 -1.20000 AFIX 0 C3 1 0.606436 0.224119 0.678750 11.00000 0.03216 0.03321 = 0.03155 0.00918 -0.00664 -0.00976 AFIX 23 H3A 2 0.576068 0.241941 0.716259 11.00000 -1.20000 H3B 2 0.595062 0.254436 0.646512 11.00000 -1.20000 AFIX 0 C4 1 0.746570 0.207913 0.686482 11.00000 0.02954 0.06365 = 0.04410 0.01767 -0.01217 -0.01533 AFIX 23 H4A 2 0.796289 0.245439 0.692351 11.00000 -1.20000 H4B 2 0.758892 0.182860 0.722846 11.00000 -1.20000 AFIX 0 C5 1 0.795839 0.174056 0.633578 11.00000 0.02362 0.09214 = 0.04637 0.02715 0.00091 -0.00463 AFIX 23 H5A 2 0.884189 0.161401 0.642606 11.00000 -1.20000 H5B 2 0.796262 0.201363 0.598553 11.00000 -1.20000 AFIX 0 C6 1 0.717181 0.119034 0.618094 11.00000 0.03054 0.06146 = 0.03265 0.01256 0.00758 0.01598 AFIX 23 H6A 2 0.726485 0.089055 0.650758 11.00000 -1.20000 H6B 2 0.748595 0.100417 0.581168 11.00000 -1.20000 AFIX 0 C7 1 0.576495 0.135215 0.608652 11.00000 0.02983 0.04035 = 0.03207 0.00427 0.00078 0.00266 AFIX 23 H7A 2 0.565316 0.161297 0.572940 11.00000 -1.20000 H7B 2 0.526414 0.097945 0.601815 11.00000 -1.20000 AFIX 0 C8 1 0.321656 0.144527 0.708981 11.00000 0.02437 0.02352 = 0.02290 0.00499 0.00064 -0.00104 AFIX 13 H8A 2 0.229403 0.152724 0.701862 11.00000 -1.20000 AFIX 0 C9 1 0.357235 0.169311 0.770381 11.00000 0.05789 0.04176 = 0.02368 -0.00154 0.00039 -0.01872 AFIX 23 H9A 2 0.339983 0.213226 0.771356 11.00000 -1.20000 H9B 2 0.448822 0.163153 0.778763 11.00000 -1.20000 AFIX 0 C10 1 0.281338 0.137541 0.818319 11.00000 0.06491 0.05928 = 0.02184 0.00161 0.00754 -0.02153 AFIX 23 H10A 2 0.310587 0.151850 0.858334 11.00000 -1.20000 H10B 2 0.190771 0.148190 0.812876 11.00000 -1.20000 AFIX 0 C11 1 0.295922 0.069717 0.815179 11.00000 0.03989 0.05685 = 0.04835 0.02861 0.00290 -0.00538 AFIX 23 H11A 2 0.384516 0.058707 0.825876 11.00000 -1.20000 H11B 2 0.240581 0.050606 0.844634 11.00000 -1.20000 AFIX 0 C12 1 0.262091 0.045970 0.753668 11.00000 0.04111 0.02589 = 0.05843 0.00500 0.02295 -0.00149 AFIX 23 H12A 2 0.170819 0.052736 0.744930 11.00000 -1.20000 H12B 2 0.277785 0.001923 0.752672 11.00000 -1.20000 AFIX 0 C13 1 0.339153 0.076795 0.705367 11.00000 0.04467 0.02759 = 0.05341 0.00068 0.02297 -0.00816 AFIX 23 H13A 2 0.429853 0.066612 0.711292 11.00000 -1.20000 H13B 2 0.310639 0.062179 0.665354 11.00000 -1.20000 AFIX 0 C14 1 0.002032 0.239358 0.445336 11.00000 0.02254 0.01380 = 0.02206 0.00233 -0.00226 0.00007 C15 1 -0.024306 0.176354 0.355312 11.00000 0.02683 0.02644 = 0.02655 -0.00911 -0.00227 -0.00006 AFIX 13 H15 2 0.069873 0.177367 0.360929 11.00000 -1.20000 AFIX 0 C16 1 -0.062331 0.110502 0.360774 11.00000 0.03562 0.02404 = 0.02646 -0.00369 0.00198 0.00484 AFIX 23 H16A 2 -0.155720 0.107163 0.358311 11.00000 -1.20000 H16B 2 -0.032742 0.094738 0.400191 11.00000 -1.20000 AFIX 0 C17 1 -0.005770 0.072938 0.311441 11.00000 0.04612 0.02811 = 0.03370 -0.00594 -0.00419 0.00687 AFIX 23 H17A 2 0.087361 0.071683 0.317439 11.00000 -1.20000 H17B 2 -0.037886 0.031054 0.313885 11.00000 -1.20000 AFIX 0 C18 1 -0.038273 0.098341 0.249892 11.00000 0.04760 0.04262 = 0.02585 -0.01263 0.00211 0.00811 AFIX 23 H18A 2 -0.130675 0.095283 0.241897 11.00000 -1.20000 H18B 2 0.004670 0.074249 0.219261 11.00000 -1.20000 AFIX 0 C19 1 0.002312 0.163910 0.245380 11.00000 0.03941 0.04627 = 0.02521 0.00006 0.00539 0.00504 AFIX 23 H19A 2 -0.025360 0.180066 0.205835 11.00000 -1.20000 H19B 2 0.095806 0.166232 0.248338 11.00000 -1.20000 AFIX 0 C20 1 -0.053002 0.202575 0.294181 11.00000 0.04364 0.03218 = 0.02925 0.00044 0.01020 -0.00025 AFIX 23 H20A 2 -0.017395 0.243836 0.292134 11.00000 -1.20000 H20B 2 -0.145813 0.205518 0.287546 11.00000 -1.20000 AFIX 0 C21 1 -0.215527 0.220043 0.402947 11.00000 0.01822 0.02628 = 0.03444 0.00059 -0.00685 -0.00462 AFIX 13 H21A 2 -0.244157 0.195475 0.367544 11.00000 -1.20000 AFIX 0 C22 1 -0.259609 0.283733 0.387840 11.00000 0.02772 0.03320 = 0.02051 0.00246 0.00288 0.00568 AFIX 23 H22A 2 -0.235075 0.311280 0.421069 11.00000 -1.20000 H22B 2 -0.217722 0.297833 0.351426 11.00000 -1.20000 AFIX 0 C23 1 -0.402183 0.285557 0.377477 11.00000 0.02879 0.04018 = 0.03789 0.00139 -0.00860 0.00627 AFIX 23 H23A 2 -0.429599 0.328020 0.372264 11.00000 -1.20000 H23B 2 -0.424896 0.263492 0.340182 11.00000 -1.20000 AFIX 0 C24 1 -0.470376 0.258222 0.428007 11.00000 0.02703 0.05208 = 0.03996 0.00124 0.00125 0.00359 AFIX 23 H24A 2 -0.562359 0.258130 0.418256 11.00000 -1.20000 H24B 2 -0.455864 0.283171 0.464293 11.00000 -1.20000 AFIX 0 C25 1 -0.426371 0.193349 0.440957 11.00000 0.02931 0.04022 = 0.02663 -0.00106 0.00550 -0.00668 AFIX 23 H25A 2 -0.447151 0.167369 0.406003 11.00000 -1.20000 H25B 2 -0.471087 0.177229 0.475749 11.00000 -1.20000 AFIX 0 C26 1 -0.282192 0.192326 0.454228 11.00000 0.03038 0.03320 = 0.02854 0.00106 -0.00289 -0.00151 AFIX 23 H26A 2 -0.262063 0.215213 0.491328 11.00000 -1.20000 H26B 2 -0.253268 0.150178 0.460163 11.00000 -1.20000 AFIX 0 C27 1 0.219371 0.433353 0.544539 11.00000 0.01397 0.02187 = 0.01715 -0.00171 -0.00344 -0.00142 C28 1 0.273665 0.526393 0.492707 11.00000 0.02375 0.01965 = 0.01724 -0.00161 0.00181 -0.00048 AFIX 13 H28 2 0.295003 0.495613 0.461916 11.00000 -1.20000 AFIX 0 C29 1 0.390161 0.566333 0.502209 11.00000 0.01470 0.02579 = 0.03206 0.00198 0.00068 0.00055 AFIX 23 H29A 2 0.461296 0.542142 0.519251 11.00000 -1.20000 H29B 2 0.371597 0.599179 0.530635 11.00000 -1.20000 AFIX 0 C30 1 0.426506 0.593174 0.441970 11.00000 0.02597 0.02791 = 0.03582 0.00326 0.00908 -0.00207 AFIX 23 H30A 2 0.501604 0.619472 0.447766 11.00000 -1.20000 H30B 2 0.448648 0.560237 0.414274 11.00000 -1.20000 AFIX 0 C31 1 0.317160 0.629739 0.414940 11.00000 0.03373 0.02567 = 0.03190 0.00577 0.00850 -0.00452 AFIX 23 H31A 2 0.301149 0.664990 0.440835 11.00000 -1.20000 H31B 2 0.340768 0.645049 0.375241 11.00000 -1.20000 AFIX 0 C32 1 0.197275 0.592644 0.408097 11.00000 0.03540 0.02767 = 0.02735 0.00638 -0.00472 -0.00252 AFIX 23 H32A 2 0.209356 0.560831 0.377722 11.00000 -1.20000 H32B 2 0.127062 0.618986 0.393710 11.00000 -1.20000 AFIX 0 C33 1 0.161886 0.563307 0.466967 11.00000 0.02097 0.02290 = 0.02620 0.00399 -0.00189 -0.00326 AFIX 23 H33A 2 0.087763 0.536592 0.460149 11.00000 -1.20000 H33B 2 0.138596 0.594923 0.495902 11.00000 -1.20000 AFIX 0 C34 1 0.216131 0.531525 0.600323 11.00000 0.02497 0.02139 = 0.01842 -0.00811 0.00343 -0.00353 AFIX 13 H34 2 0.234551 0.573729 0.587313 11.00000 -1.20000 AFIX 0 C35 1 0.078498 0.532102 0.618852 11.00000 0.02546 0.02618 = 0.03613 -0.00928 0.00670 -0.00478 AFIX 23 H35A 2 0.052412 0.490795 0.630035 11.00000 -1.20000 H35B 2 0.023422 0.545614 0.584831 11.00000 -1.20000 AFIX 0 C36 1 0.063182 0.574746 0.672013 11.00000 0.03572 0.04735 = 0.05388 -0.02619 0.02298 -0.01653 AFIX 23 H36A 2 0.079538 0.616751 0.659253 11.00000 -1.20000 H36B 2 -0.024901 0.572560 0.685610 11.00000 -1.20000 AFIX 0 C37 1 0.152918 0.558482 0.723031 11.00000 0.05799 0.06625 = 0.03396 -0.02460 0.01803 -0.03346 AFIX 23 H37A 2 0.132877 0.517440 0.737482 11.00000 -1.20000 H37B 2 0.141588 0.587081 0.756446 11.00000 -1.20000 AFIX 0 C38 1 0.289590 0.560357 0.704164 11.00000 0.04546 0.04358 = 0.02343 -0.01044 0.00443 -0.01856 AFIX 23 H38A 2 0.345813 0.548002 0.738214 11.00000 -1.20000 H38B 2 0.311954 0.602200 0.693075 11.00000 -1.20000 AFIX 0 C39 1 0.310501 0.518410 0.651014 11.00000 0.03364 0.02559 = 0.02493 -0.00511 -0.00541 -0.00835 AFIX 23 H39A 2 0.397495 0.523902 0.636819 11.00000 -1.20000 H39B 2 0.301440 0.475914 0.663911 11.00000 -1.20000 AFIX 66 PART 1 10.5 N4 3 -0.127536 -0.085320 0.470668 10.50000 0.09120 C40 1 -0.075667 -0.027944 0.477200 10.50000 0.07778 AFIX 43 H40 2 0.012532 -0.022048 0.472744 10.50000 -1.20000 AFIX 65 C41 1 -0.152845 0.020806 0.490252 10.50000 0.10611 AFIX 43 H41 2 -0.117393 0.060020 0.494717 10.50000 -1.20000 AFIX 65 C42 1 -0.281893 0.012181 0.496773 10.50000 0.08128 AFIX 43 H42 2 -0.334641 0.045500 0.505693 10.50000 -1.20000 AFIX 65 C43 1 -0.333765 -0.045194 0.490241 10.50000 0.07124 AFIX 43 H43 2 -0.421964 -0.051089 0.494697 10.50000 -1.20000 AFIX 65 C44 1 -0.256588 -0.093945 0.477189 10.50000 0.05730 AFIX 43 H44 2 -0.292040 -0.133159 0.472724 10.50000 -1.20000 AFIX 66 PART 2 10.5 N4B 3 -0.271003 0.007672 0.438070 10.50000 0.07626 C40B 1 -0.355384 0.013850 0.484078 10.50000 0.05869 AFIX 43 H40B 2 -0.410040 0.047856 0.485045 10.50000 -1.20000 AFIX 65 C41B 1 -0.359797 -0.029726 0.528673 10.50000 0.09134 AFIX 43 H41B 2 -0.417468 -0.025503 0.560118 10.50000 -1.20000 AFIX 65 C42B 1 -0.279829 -0.079481 0.527259 10.50000 0.06841 AFIX 43 H42B 2 -0.282846 -0.109264 0.557738 10.50000 -1.20000 AFIX 65 C43B 1 -0.195447 -0.085660 0.481251 10.50000 0.04283 AFIX 43 H43B 2 -0.140792 -0.119666 0.480285 10.50000 -1.20000 AFIX 65 C44B 1 -0.191032 -0.042084 0.436656 10.50000 0.07371 AFIX 43 H44B 2 -0.133361 -0.046308 0.405211 10.50000 -1.20000 AFIX 66 PART 1 10.3000 N5 3 0.557902 -0.059788 0.666127 10.30000 0.10497 C45 1 0.505576 -0.058160 0.722327 10.30000 0.10353 AFIX 43 H45 2 0.451045 -0.025948 0.732590 10.30000 -1.20000 AFIX 65 C46 1 0.533038 -0.103660 0.763511 10.30000 0.08950 AFIX 43 H46 2 0.497275 -0.102547 0.801921 10.30000 -1.20000 AFIX 65 C47 1 0.612825 -0.150790 0.748495 10.30000 0.04620 AFIX 43 H47 2 0.631594 -0.181888 0.776642 10.30000 -1.20000 AFIX 65 C48 1 0.665152 -0.152420 0.692295 10.30000 0.05399 AFIX 43 H48 2 0.719683 -0.184631 0.682033 10.30000 -1.20000 AFIX 65 C49 1 0.637691 -0.106919 0.651111 10.30000 0.08089 AFIX 43 H49 2 0.673454 -0.108033 0.612701 10.30000 -1.20000 AFIX 66 PART 2 10.7000 N5B 3 0.392855 -0.092585 0.694806 10.70000 0.05583 C45B 1 0.488414 -0.064196 0.664094 10.70000 0.06765 AFIX 43 H45B 2 0.468827 -0.043152 0.627978 10.70000 -1.20000 AFIX 65 C46B 1 0.612633 -0.066596 0.686226 10.70000 0.05760 AFIX 43 H46B 2 0.677944 -0.047193 0.665236 10.70000 -1.20000 AFIX 65 C47B 1 0.641294 -0.097386 0.739070 10.70000 0.05736 AFIX 43 H47B 2 0.726192 -0.099026 0.754196 10.70000 -1.20000 AFIX 65 C48B 1 0.545735 -0.125775 0.769783 10.70000 0.04250 AFIX 43 H48B 2 0.565324 -0.146819 0.805899 10.70000 -1.20000 AFIX 65 C49B 1 0.421515 -0.123376 0.747651 10.70000 0.05459 AFIX 43 H49B 2 0.356205 -0.142779 0.768642 10.70000 -1.20000 PART 0 HKLF 4 REM sad in P2(1)/c In(N,N-dicy-dtc)3.2py REM R1 = 0.0476 for 8749 Fo > 4sig(Fo) and 0.0769 for all 12019 data REM 490 parameters refined using 0 restraints END WGHT 0.0374 7.1051 REM Highest difference peak 1.040, deepest hole -0.747, 1-sigma level 0.094 Q1 1 -0.3236 -0.0207 0.5398 11.00000 0.05 1.04 Q2 1 0.4545 -0.0739 0.6793 11.00000 0.05 0.86 Q3 1 -0.3059 -0.0910 0.4989 11.00000 0.05 0.83 Q4 1 0.4407 -0.1157 0.7324 11.00000 0.05 0.82 Q5 1 0.4541 -0.0907 0.7574 11.00000 0.05 0.82 Q6 1 0.6387 -0.1249 0.6882 11.00000 0.05 0.66 Q7 1 0.5478 -0.0439 0.7213 11.00000 0.05 0.60 Q8 1 0.5372 -0.1400 0.7907 11.00000 0.05 0.60 Q9 1 -0.3312 0.0068 0.4524 11.00000 0.05 0.59 Q10 1 0.5907 0.1116 0.6466 11.00000 0.05 0.59 Q11 1 -0.3921 -0.0436 0.4996 11.00000 0.05 0.58 Q12 1 -0.3185 0.1670 0.4184 11.00000 0.05 0.56 Q13 1 -0.2292 -0.0837 0.4589 11.00000 0.05 0.56 Q14 1 0.1137 0.2917 0.5181 11.00000 0.05 0.55 Q15 1 -0.5018 0.2254 0.3901 11.00000 0.05 0.54 Q16 1 -0.1440 -0.0245 0.4590 11.00000 0.05 0.53 Q17 1 -0.4281 0.2910 0.4112 11.00000 0.05 0.52 Q18 1 0.1651 0.2977 0.5748 11.00000 0.05 0.52 Q19 1 0.6503 -0.1628 0.7521 11.00000 0.05 0.51 Q20 1 0.2511 0.3004 0.5542 11.00000 0.05 0.51 ; _database_code_depnum_ccdc_archive 'CCDC 924187' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 #TrackingRef 'CIF (2)' _audit_creation_method SHELXL-2012 _chemical_name_systematic ; ? ; _chemical_name_common In(di-i-Pr-dithiocarbamate)3.1.5 _chemical_melting_point ? _chemical_formula_moiety 'C21 H42 In N3 S6, 1.5(C5 H5 N)' _chemical_formula_sum 'C28.50 H49.50 In N4.50 S6' _chemical_formula_weight 762.40 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' In In -0.7276 1.3100 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6384(4) _cell_length_b 11.9426(4) _cell_length_c 14.4945(3) _cell_angle_alpha 92.781(2) _cell_angle_beta 102.078(2) _cell_angle_gamma 111.637(3) _cell_volume 1813.63(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 12746 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 30.2 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_F_000 794 _exptl_transmission_factor_min 0.927 _exptl_transmission_factor_max 0.961 _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.050 _exptl_absorpt_coefficient_mu 1.022 _shelx_estimated_absorpt_T_min 0.905 _shelx_estimated_absorpt_T_max 0.951 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details '(CrysAlis Pro; Agilent, 2012)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'SuperNova (Mo) X-ray Source' _diffrn_source_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16509 _diffrn_reflns_av_unetI/netI 0.0306 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.425 _diffrn_reflns_theta_max 30.313 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.863 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.863 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.863 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 9388 _reflns_number_gt 8595 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'CrysAlis Pro (Agilent ,2012)' _computing_cell_refinement 'CrysAlis Pro (Agilent ,2012)' _computing_data_reduction 'CrysAlis Pro (Agilent ,2012)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material 'pubCIF (Westrip, 2010)' _refine_special_details ; ? ; _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^)+(0.0176P)^2^+0.8341P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 9388 _refine_ls_number_parameters 422 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0272 _refine_ls_R_factor_gt 0.0219 _refine_ls_wR_factor_ref 0.0515 _refine_ls_wR_factor_gt 0.0502 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.012 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group In1 In 0.29840(2) 0.18263(2) 0.27799(2) 0.01451(3) Uani 1 1 d . . . . . S1 S 0.28522(4) -0.03545(4) 0.29994(3) 0.02003(8) Uani 1 1 d . . . . . S2 S 0.51717(4) 0.16823(3) 0.28764(3) 0.01719(7) Uani 1 1 d . . . . . S3 S 0.36560(3) 0.31920(4) 0.43890(3) 0.01805(7) Uani 1 1 d . . . . . S4 S 0.10316(3) 0.14745(3) 0.35044(3) 0.01739(7) Uani 1 1 d . . . . . S5 S 0.34638(4) 0.37186(4) 0.18719(3) 0.02113(8) Uani 1 1 d . . . A . S6 S 0.16317(4) 0.12535(4) 0.10362(3) 0.02276(8) Uani 1 1 d . . . A . N1 N 0.51303(12) -0.05175(11) 0.32149(9) 0.0158(2) Uani 1 1 d . . . . . N2 N 0.16614(12) 0.29966(11) 0.51123(8) 0.0150(2) Uani 1 1 d . . . . . C1 C 0.44638(14) 0.01780(13) 0.30507(10) 0.0153(3) Uani 1 1 d . . . . . C2 C 0.65337(14) -0.00057(14) 0.33228(11) 0.0184(3) Uani 1 1 d . . . . . H2 H 0.6813 0.0895 0.3338 0.022 Uiso 1 1 calc R U . . . C3 C 0.72300(16) -0.02318(16) 0.42606(12) 0.0278(4) Uani 1 1 d . . . . . H3A H 0.6995 0.0103 0.4789 0.042 Uiso 1 1 calc R U . . . H3B H 0.8152 0.0164 0.4333 0.042 Uiso 1 1 calc R U . . . H3C H 0.6991 -0.1109 0.4264 0.042 Uiso 1 1 calc R U . . . C4 C 0.68656(17) -0.04840(16) 0.24657(12) 0.0275(4) Uani 1 1 d . . . . . H4A H 0.6627 -0.1364 0.2440 0.041 Uiso 1 1 calc R U . . . H4B H 0.7784 -0.0084 0.2523 0.041 Uiso 1 1 calc R U . . . H4C H 0.6399 -0.0312 0.1882 0.041 Uiso 1 1 calc R U . . . C5 C 0.45565(15) -0.18468(14) 0.32834(12) 0.0233(3) Uani 1 1 d . . . . . H5 H 0.5286 -0.2117 0.3388 0.028 Uiso 1 1 calc R U . . . C6 C 0.36492(18) -0.25920(16) 0.23521(15) 0.0339(4) Uani 1 1 d . . . . . H6A H 0.2862 -0.2442 0.2246 0.051 Uiso 1 1 calc R U . . . H6B H 0.3449 -0.3459 0.2388 0.051 Uiso 1 1 calc R U . . . H6C H 0.4053 -0.2355 0.1824 0.051 Uiso 1 1 calc R U . . . C7 C 0.40082(19) -0.21162(19) 0.41516(15) 0.0365(5) Uani 1 1 d . . . . . H7A H 0.3217 -0.1973 0.4055 0.055 Uiso 1 1 calc R U . . . H7B H 0.4626 -0.1582 0.4717 0.055 Uiso 1 1 calc R U . . . H7C H 0.3828 -0.2967 0.4242 0.055 Uiso 1 1 calc R U . . . C8 C 0.20690(14) 0.26083(13) 0.44176(10) 0.0143(3) Uani 1 1 d . . . . . C9 C 0.03186(15) 0.23806(14) 0.51739(11) 0.0204(3) Uani 1 1 d . . . . . H9 H -0.0069 0.1618 0.4707 0.024 Uiso 1 1 calc R U . . . C10 C 0.02560(17) 0.20023(15) 0.61572(12) 0.0265(4) Uani 1 1 d . . . . . H10A H 0.0782 0.1527 0.6319 0.040 Uiso 1 1 calc R U . . . H10B H -0.0629 0.1507 0.6155 0.040 Uiso 1 1 calc R U . . . H10C H 0.0575 0.2730 0.6630 0.040 Uiso 1 1 calc R U . . . C11 C -0.04454(16) 0.31533(17) 0.48732(12) 0.0264(3) Uani 1 1 d . . . . . H11A H -0.0390 0.3348 0.4231 0.040 Uiso 1 1 calc R U . . . H11B H -0.0099 0.3908 0.5320 0.040 Uiso 1 1 calc R U . . . H11C H -0.1339 0.2702 0.4875 0.040 Uiso 1 1 calc R U . . . C12 C 0.24268(15) 0.41175(13) 0.58171(10) 0.0177(3) Uani 1 1 d . . . . . H12 H 0.1829 0.4223 0.6187 0.021 Uiso 1 1 calc R U . . . C13 C 0.28486(16) 0.52506(14) 0.53299(12) 0.0219(3) Uani 1 1 d . . . . . H13A H 0.2120 0.5255 0.4849 0.033 Uiso 1 1 calc R U . . . H13B H 0.3522 0.5249 0.5022 0.033 Uiso 1 1 calc R U . . . H13C H 0.3175 0.5977 0.5805 0.033 Uiso 1 1 calc R U . . . C14 C 0.35151(16) 0.40053(16) 0.65482(11) 0.0248(3) Uani 1 1 d . . . . . H14A H 0.3881 0.4709 0.7048 0.037 Uiso 1 1 calc R U . . . H14B H 0.4174 0.3976 0.6234 0.037 Uiso 1 1 calc R U . . . H14C H 0.3190 0.3259 0.6833 0.037 Uiso 1 1 calc R U . . . C15 C 0.23102(15) 0.27700(15) 0.09025(11) 0.0203(3) Uani 1 1 d . . . . . N3 N 0.2019(2) 0.3251(2) 0.01184(14) 0.0205(4) Uani 0.83 1 d . . P A 1 C16 C 0.0948(2) 0.2550(2) -0.07248(13) 0.0261(4) Uani 0.83 1 d . . P A 1 H16 H 0.0939 0.3155 -0.1176 0.031 Uiso 0.83 1 calc R U P A 1 C17 C -0.0346(2) 0.2145(2) -0.04964(16) 0.0296(5) Uani 0.83 1 d . . P A 1 H17A H -0.0428 0.1512 -0.0080 0.044 Uiso 0.83 1 calc R U P A 1 H17B H -0.1017 0.1820 -0.1088 0.044 Uiso 0.83 1 calc R U P A 1 H17C H -0.0429 0.2841 -0.0173 0.044 Uiso 0.83 1 calc R U P A 1 C18 C 0.1156(2) 0.15488(19) -0.12800(14) 0.0403(5) Uani 1 1 d . . . . . H18A H 0.1998 0.1881 -0.1417 0.060 Uiso 1 1 calc R U . A 1 H18B H 0.0498 0.1241 -0.1880 0.060 Uiso 1 1 calc R U . A 1 H18C H 0.1105 0.0884 -0.0900 0.060 Uiso 1 1 calc R U . A 1 C21 C 0.1885(2) 0.52519(19) 0.00218(15) 0.0421(5) Uani 1 1 d . . . . . H21A H 0.2389 0.6121 0.0050 0.063 Uiso 1 1 calc R U . B 1 H21B H 0.1517 0.5119 0.0576 0.063 Uiso 1 1 calc R U . B 1 H21C H 0.1199 0.4969 -0.0563 0.063 Uiso 1 1 calc R U . B 1 C19 C 0.2724(2) 0.4561(2) 0.00259(16) 0.0295(5) Uani 0.83 1 d . . P A 1 H19 H 0.3434 0.4911 0.0614 0.035 Uiso 0.83 1 calc R U P A 1 C20 C 0.3341(3) 0.4659(3) -0.0810(2) 0.0431(7) Uani 0.83 1 d . . P A 1 H20A H 0.3852 0.4160 -0.0755 0.065 Uiso 0.83 1 calc R U P A 1 H20B H 0.3893 0.5510 -0.0805 0.065 Uiso 0.83 1 calc R U P A 1 H20C H 0.2677 0.4371 -0.1407 0.065 Uiso 0.83 1 calc R U P A 1 N3B N 0.1658(10) 0.2885(9) 0.0035(8) 0.016(3) Uiso 0.17 1 d . . P A 2 C16B C 0.0523(9) 0.1927(9) -0.0623(6) 0.0131(16) Uiso 0.17 1 d . . P A 2 H16A H 0.0193 0.1236 -0.0258 0.016 Uiso 0.17 1 calc R U P A 2 C17B C -0.0533(12) 0.2409(12) -0.0923(9) 0.035(3) Uiso 0.17 1 d . . P A 2 H17D H -0.0667 0.2775 -0.0356 0.053 Uiso 0.17 1 calc R U P A 2 H17E H -0.1325 0.1737 -0.1259 0.053 Uiso 0.17 1 calc R U P A 2 H17F H -0.0281 0.3024 -0.1346 0.053 Uiso 0.17 1 calc R U P A 2 C19B C 0.2181(11) 0.4087(10) -0.0268(8) 0.023(2) Uiso 0.17 1 d . . P A 2 H19A H 0.1708 0.3885 -0.0954 0.028 Uiso 0.17 1 calc R U P A 2 C20B C 0.3544(13) 0.4427(12) -0.0385(10) 0.037(3) Uiso 0.17 1 d . . P A 2 H20D H 0.4128 0.4560 0.0242 0.056 Uiso 0.17 1 calc R U P A 2 H20E H 0.3795 0.5173 -0.0681 0.056 Uiso 0.17 1 calc R U P A 2 H20F H 0.3579 0.3765 -0.0790 0.056 Uiso 0.17 1 calc R U P A 2 N4 N 0.90384(15) 0.49785(14) 0.26549(11) 0.0286(3) Uani 1 1 d . . . . . C22 C 0.81576(18) 0.38581(17) 0.23425(13) 0.0304(4) Uani 1 1 d . . . . . H22 H 0.7300 0.3713 0.2349 0.036 Uiso 1 1 calc R U . . . C23 C 0.8419(2) 0.29023(18) 0.20116(13) 0.0393(5) Uani 1 1 d . . . . . H23 H 0.7759 0.2122 0.1788 0.047 Uiso 1 1 calc R U . . . C24 C 0.9663(3) 0.3105(2) 0.20123(13) 0.0462(6) Uani 1 1 d . . . . . H24 H 0.9877 0.2466 0.1785 0.055 Uiso 1 1 calc R U . . . C25 C 1.0590(2) 0.4248(2) 0.23485(14) 0.0427(5) Uani 1 1 d . . . . . H25 H 1.1459 0.4411 0.2367 0.051 Uiso 1 1 calc R U . . . C26 C 1.02323(18) 0.51463(19) 0.26560(13) 0.0336(4) Uani 1 1 d . . . . . H26 H 1.0876 0.5934 0.2883 0.040 Uiso 1 1 calc R U . . . N5 N 0.4694(7) 0.1135(5) 0.0291(5) 0.0569(18) Uani 0.5 1 d . . P C -1 C27 C 0.3975(8) -0.0088(8) 0.0350(6) 0.0404(18) Uani 0.5 1 d . . P C -1 H27 H 0.3247 -0.0310 0.0607 0.048 Uiso 0.5 1 calc R U P C -1 C28 C 0.4370(7) -0.0949(7) 0.0021(4) 0.0436(14) Uani 0.5 1 d . . P C -1 H28 H 0.3926 -0.1796 0.0015 0.052 Uiso 0.5 1 calc R U P C -1 C29 C 0.5700(6) 0.1546(6) -0.0048(4) 0.0489(17) Uani 0.5 1 d . . P C -1 H29 H 0.6120 0.2383 -0.0093 0.059 Uiso 0.5 1 calc R U P C -1 C30 C 0.6067(8) 0.0760(10) -0.0307(7) 0.069(3) Uani 0.5 1 d . . P C -1 H30 H 0.6825 0.1051 -0.0527 0.082 Uiso 0.5 1 calc R U P C -1 C31 C 0.5534(11) -0.0451(10) -0.0320(5) 0.064(3) Uani 0.5 1 d . . P C -1 H31 H 0.5901 -0.0969 -0.0543 0.077 Uiso 0.5 1 calc R U P C -1 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 In1 0.01668(5) 0.01636(5) 0.01364(5) 0.00364(4) 0.00512(4) 0.00902(4) S1 0.01588(17) 0.01917(18) 0.0300(2) 0.01052(15) 0.01040(15) 0.00896(14) S2 0.01704(17) 0.01404(17) 0.02301(18) 0.00467(13) 0.00801(14) 0.00692(13) S3 0.01368(17) 0.02267(19) 0.01725(17) -0.00040(13) 0.00494(13) 0.00621(14) S4 0.01466(17) 0.01874(18) 0.01782(17) -0.00086(13) 0.00389(13) 0.00586(14) S5 0.02090(19) 0.01830(18) 0.02380(19) 0.00705(14) 0.00426(15) 0.00730(15) S6 0.0243(2) 0.0231(2) 0.01686(17) -0.00052(14) 0.00314(15) 0.00601(16) N1 0.0136(6) 0.0144(6) 0.0205(6) 0.0052(5) 0.0059(5) 0.0056(5) N2 0.0146(6) 0.0136(6) 0.0167(6) 0.0017(4) 0.0063(5) 0.0041(5) C1 0.0167(7) 0.0169(7) 0.0134(6) 0.0036(5) 0.0060(5) 0.0065(5) C2 0.0131(7) 0.0171(7) 0.0263(8) 0.0048(6) 0.0057(6) 0.0065(6) C3 0.0206(8) 0.0281(9) 0.0311(9) 0.0054(7) 0.0001(7) 0.0085(7) C4 0.0242(8) 0.0298(9) 0.0337(9) 0.0061(7) 0.0153(7) 0.0119(7) C5 0.0180(7) 0.0159(7) 0.0392(9) 0.0117(6) 0.0088(7) 0.0081(6) C6 0.0265(9) 0.0168(8) 0.0532(12) -0.0003(8) 0.0044(8) 0.0060(7) C7 0.0297(10) 0.0394(11) 0.0525(12) 0.0332(9) 0.0200(9) 0.0186(8) C8 0.0157(7) 0.0144(7) 0.0150(6) 0.0055(5) 0.0046(5) 0.0075(5) C9 0.0169(7) 0.0186(7) 0.0241(8) 0.0005(6) 0.0103(6) 0.0026(6) C10 0.0300(9) 0.0218(8) 0.0326(9) 0.0083(7) 0.0195(7) 0.0087(7) C11 0.0183(8) 0.0350(9) 0.0265(8) 0.0054(7) 0.0072(7) 0.0101(7) C12 0.0191(7) 0.0156(7) 0.0176(7) -0.0005(5) 0.0060(6) 0.0054(6) C13 0.0217(8) 0.0157(7) 0.0284(8) 0.0027(6) 0.0088(6) 0.0059(6) C14 0.0269(9) 0.0265(8) 0.0196(7) -0.0006(6) 0.0023(6) 0.0112(7) C15 0.0212(8) 0.0286(8) 0.0172(7) 0.0053(6) 0.0076(6) 0.0148(7) N3 0.0198(10) 0.0254(11) 0.0162(9) 0.0064(8) 0.0031(8) 0.0092(9) C16 0.0289(11) 0.0340(12) 0.0155(9) 0.0023(8) 0.0015(8) 0.0147(10) C17 0.0273(11) 0.0310(12) 0.0248(11) -0.0007(9) 0.0006(9) 0.0087(9) C18 0.0549(13) 0.0393(11) 0.0339(10) 0.0041(8) 0.0212(9) 0.0210(10) C21 0.0456(12) 0.0309(10) 0.0441(11) -0.0022(8) 0.0104(10) 0.0097(9) C19 0.0268(11) 0.0271(11) 0.0295(11) 0.0161(9) 0.0042(10) 0.0048(10) C20 0.0361(14) 0.0521(17) 0.0524(16) 0.0335(14) 0.0222(13) 0.0205(12) N4 0.0280(8) 0.0285(8) 0.0322(8) 0.0012(6) 0.0138(6) 0.0110(6) C22 0.0286(9) 0.0313(10) 0.0311(9) 0.0068(7) 0.0110(7) 0.0090(7) C23 0.0651(15) 0.0253(9) 0.0255(9) 0.0063(7) 0.0055(9) 0.0179(9) C24 0.0890(19) 0.0572(14) 0.0222(9) 0.0131(9) 0.0180(10) 0.0587(14) C25 0.0439(12) 0.0745(16) 0.0318(10) 0.0177(10) 0.0174(9) 0.0420(12) C26 0.0275(9) 0.0403(11) 0.0322(9) 0.0062(8) 0.0114(8) 0.0100(8) N5 0.051(3) 0.075(4) 0.024(2) 0.006(3) 0.0076(18) 0.002(3) C27 0.031(3) 0.055(5) 0.027(3) 0.010(3) 0.017(2) 0.002(3) C28 0.049(4) 0.050(4) 0.028(2) 0.000(3) 0.012(2) 0.014(3) C29 0.041(3) 0.042(3) 0.040(3) 0.008(3) 0.008(2) -0.010(3) C30 0.030(3) 0.109(8) 0.050(4) 0.037(6) 0.005(3) 0.008(5) C31 0.089(9) 0.111(11) 0.023(3) 0.014(7) 0.019(5) 0.071(9) _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 In1 S3 2.5765(4) . ? In1 S6 2.5897(4) . ? In1 S2 2.5900(4) . ? In1 S1 2.5912(4) . ? In1 S4 2.6038(4) . ? In1 S5 2.6109(4) . ? S1 C1 1.7278(15) . ? S2 C1 1.7348(15) . ? S3 C8 1.7276(15) . ? S4 C8 1.7306(15) . ? S5 C15 1.7304(16) . ? S6 C15 1.7276(17) . ? N1 C1 1.3286(18) . ? N1 C2 1.4878(19) . ? N1 C5 1.4957(19) . ? N2 C8 1.3306(18) . ? N2 C9 1.4862(19) . ? N2 C12 1.4954(18) . ? C2 C3 1.521(2) . ? C2 C4 1.521(2) . ? C2 H2 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C7 1.523(2) . ? C5 C6 1.524(2) . ? C5 H5 1.0000 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C9 C11 1.521(2) . ? C9 C10 1.524(2) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.523(2) . ? C12 C14 1.524(2) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 N3 1.335(2) . ? C15 N3B 1.368(11) . ? N3 C16 1.498(3) . ? N3 C19 1.503(3) . ? C16 C17 1.516(3) . ? C16 C18 1.529(3) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C16B 1.467(9) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C21 C19 1.492(3) . ? C21 C19B 1.609(11) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C19 C20 1.521(3) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? N3B C19B 1.467(14) . ? N3B C16B 1.489(12) . ? C16B C17B 1.534(15) . ? C16B H16A 1.0000 . ? C17B H17D 0.9800 . ? C17B H17E 0.9800 . ? C17B H17F 0.9800 . ? C19B C20B 1.534(17) . ? C19B H19A 1.0000 . ? C20B H20D 0.9800 . ? C20B H20E 0.9800 . ? C20B H20F 0.9800 . ? N4 C26 1.328(2) . ? N4 C22 1.335(2) . ? C22 C23 1.375(3) . ? C22 H22 0.9500 . ? C23 C24 1.376(3) . ? C23 H23 0.9500 . ? C24 C25 1.377(3) . ? C24 H24 0.9500 . ? C25 C26 1.373(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? N5 C29 1.301(9) . ? N5 C27 1.408(8) . ? C27 C28 1.373(13) . ? C27 H27 0.9500 . ? C28 C31 1.465(12) . ? C28 H28 0.9500 . ? C29 C30 1.239(13) . ? C29 H29 0.9500 . ? C30 C31 1.345(12) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? 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 S3 In1 S6 147.677(13) . . ? S3 In1 S2 96.035(12) . . ? S6 In1 S2 110.278(13) . . ? S3 In1 S1 111.904(13) . . ? S6 In1 S1 95.268(14) . . ? S2 In1 S1 69.114(12) . . ? S3 In1 S4 69.260(12) . . ? S6 In1 S4 94.080(13) . . ? S2 In1 S4 149.278(12) . . ? S1 In1 S4 90.892(13) . . ? S3 In1 S5 91.220(13) . . ? S6 In1 S5 68.760(13) . . ? S2 In1 S5 94.909(13) . . ? S1 In1 S5 152.605(13) . . ? S4 In1 S5 111.674(13) . . ? C1 S1 In1 87.36(5) . . ? C1 S2 In1 87.26(5) . . ? C8 S3 In1 87.39(5) . . ? C8 S4 In1 86.45(5) . . ? C15 S5 In1 87.05(5) . . ? C15 S6 In1 87.79(5) . . ? C1 N1 C2 120.87(12) . . ? C1 N1 C5 124.07(13) . . ? C2 N1 C5 115.04(12) . . ? C8 N2 C9 120.41(12) . . ? C8 N2 C12 124.74(12) . . ? C9 N2 C12 114.58(11) . . ? N1 C1 S1 122.31(11) . . ? N1 C1 S2 121.54(11) . . ? S1 C1 S2 116.15(8) . . ? N1 C2 C3 111.29(13) . . ? N1 C2 C4 110.64(13) . . ? C3 C2 C4 112.63(14) . . ? N1 C2 H2 107.3 . . ? C3 C2 H2 107.3 . . ? C4 C2 H2 107.3 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 C7 113.19(14) . . ? N1 C5 C6 112.72(13) . . ? C7 C5 C6 113.95(15) . . ? N1 C5 H5 105.3 . . ? C7 C5 H5 105.3 . . ? C6 C5 H5 105.3 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 S3 121.90(11) . . ? N2 C8 S4 121.39(11) . . ? S3 C8 S4 116.70(8) . . ? N2 C9 C11 111.19(13) . . ? N2 C9 C10 111.05(13) . . ? C11 C9 C10 113.16(13) . . ? N2 C9 H9 107.0 . . ? C11 C9 H9 107.0 . . ? C10 C9 H9 107.0 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 C13 111.81(12) . . ? N2 C12 C14 113.80(12) . . ? C13 C12 C14 113.12(13) . . ? N2 C12 H12 105.8 . . ? C13 C12 H12 105.8 . . ? C14 C12 H12 105.8 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 S6 125.25(15) . . ? N3B C15 S6 105.9(4) . . ? N3 C15 S5 118.49(15) . . ? N3B C15 S5 137.5(4) . . ? S6 C15 S5 116.26(9) . . ? C15 N3 C16 123.2(2) . . ? C15 N3 C19 122.24(19) . . ? C16 N3 C19 114.51(18) . . ? N3 C16 C17 112.74(17) . . ? N3 C16 C18 114.65(18) . . ? C17 C16 C18 114.0(2) . . ? N3 C16 H16 104.7 . . ? C17 C16 H16 104.7 . . ? C18 C16 H16 104.7 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C21 C19 N3 110.49(19) . . ? C21 C19 C20 115.34(19) . . ? N3 C19 C20 110.7(2) . . ? C21 C19 H19 106.6 . . ? N3 C19 H19 106.6 . . ? C20 C19 H19 106.6 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C15 N3B C19B 114.7(8) . . ? C15 N3B C16B 127.1(8) . . ? C19B N3B C16B 118.1(10) . . ? C18 C16B N3B 99.3(7) . . ? C18 C16B C17B 124.5(8) . . ? N3B C16B C17B 109.9(9) . . ? C18 C16B H16A 107.3 . . ? N3B C16B H16A 107.3 . . ? C17B C16B H16A 107.3 . . ? C16B C17B H17D 109.5 . . ? C16B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? C16B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? N3B C19B C20B 113.0(10) . . ? N3B C19B C21 126.0(8) . . ? C20B C19B C21 113.0(9) . . ? N3B C19B H19A 99.4 . . ? C20B C19B H19A 99.4 . . ? C21 C19B H19A 99.4 . . ? C19B C20B H20D 109.5 . . ? C19B C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? C19B C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? C26 N4 C22 116.66(16) . . ? N4 C22 C23 123.80(19) . . ? N4 C22 H22 118.1 . . ? C23 C22 H22 118.1 . . ? C22 C23 C24 118.3(2) . . ? C22 C23 H23 120.8 . . ? C24 C23 H23 120.8 . . ? C25 C24 C23 118.84(18) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? C26 C25 C24 118.5(2) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? N4 C26 C25 123.9(2) . . ? N4 C26 H26 118.1 . . ? C25 C26 H26 118.1 . . ? C29 N5 C27 126.9(8) . . ? C28 C27 N5 117.2(7) . . ? C28 C27 H27 121.4 . . ? N5 C27 H27 121.4 . . ? C27 C28 C31 114.4(6) . . ? C27 C28 H28 122.8 . . ? C31 C28 H28 122.8 . . ? C30 C29 N5 114.7(7) . . ? C30 C29 H29 122.6 . . ? N5 C29 H29 122.6 . . ? C29 C30 C31 128.6(9) . . ? C29 C30 H30 115.7 . . ? C31 C30 H30 115.7 . . ? C30 C31 C28 118.0(7) . . ? C30 C31 H31 121.0 . . ? C28 C31 H31 121.0 . . ? 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 C2 N1 C1 S1 -175.62(10) . . . . ? C5 N1 C1 S1 5.8(2) . . . . ? C2 N1 C1 S2 4.29(19) . . . . ? C5 N1 C1 S2 -174.26(11) . . . . ? In1 S1 C1 N1 176.63(12) . . . . ? In1 S1 C1 S2 -3.28(7) . . . . ? In1 S2 C1 N1 -176.63(12) . . . . ? In1 S2 C1 S1 3.28(7) . . . . ? C1 N1 C2 C3 124.80(15) . . . . ? C5 N1 C2 C3 -56.53(17) . . . . ? C1 N1 C2 C4 -109.19(15) . . . . ? C5 N1 C2 C4 69.49(16) . . . . ? C1 N1 C5 C7 -67.25(19) . . . . ? C2 N1 C5 C7 114.13(15) . . . . ? C1 N1 C5 C6 63.9(2) . . . . ? C2 N1 C5 C6 -114.72(15) . . . . ? C9 N2 C8 S3 -173.13(11) . . . . ? C12 N2 C8 S3 13.20(19) . . . . ? C9 N2 C8 S4 5.99(19) . . . . ? C12 N2 C8 S4 -167.69(11) . . . . ? In1 S3 C8 N2 -176.59(12) . . . . ? In1 S3 C8 S4 4.25(7) . . . . ? In1 S4 C8 N2 176.63(12) . . . . ? In1 S4 C8 S3 -4.21(7) . . . . ? C8 N2 C9 C11 -106.52(15) . . . . ? C12 N2 C9 C11 67.77(16) . . . . ? C8 N2 C9 C10 126.53(14) . . . . ? C12 N2 C9 C10 -59.18(16) . . . . ? C8 N2 C12 C13 58.11(18) . . . . ? C9 N2 C12 C13 -115.89(14) . . . . ? C8 N2 C12 C14 -71.59(18) . . . . ? C9 N2 C12 C14 114.40(15) . . . . ? In1 S6 C15 N3 -176.94(16) . . . . ? In1 S6 C15 N3B -171.3(5) . . . . ? In1 S6 C15 S5 3.51(8) . . . . ? In1 S5 C15 N3 176.94(14) . . . . ? In1 S5 C15 N3B 169.1(7) . . . . ? In1 S5 C15 S6 -3.48(8) . . . . ? N3B C15 N3 C16 -9.0(15) . . . . ? S6 C15 N3 C16 7.0(3) . . . . ? S5 C15 N3 C16 -173.44(15) . . . . ? N3B C15 N3 C19 169.0(17) . . . . ? S6 C15 N3 C19 -174.97(15) . . . . ? S5 C15 N3 C19 4.6(3) . . . . ? C15 N3 C16 C17 64.0(3) . . . . ? C19 N3 C16 C17 -114.2(2) . . . . ? C15 N3 C16 C18 -68.7(3) . . . . ? C19 N3 C16 C18 113.1(2) . . . . ? N3 C16 C18 C16B 106.5(7) . . . . ? C17 C16 C18 C16B -25.6(7) . . . . ? C19B C21 C19 N3 -41.0(9) . . . . ? C19B C21 C19 C20 85.5(9) . . . . ? C15 N3 C19 C21 -110.9(2) . . . . ? C16 N3 C19 C21 67.3(2) . . . . ? C15 N3 C19 C20 120.2(2) . . . . ? C16 N3 C19 C20 -61.7(3) . . . . ? N3 C15 N3B C19B -7.0(9) . . . . ? S6 C15 N3B C19B -173.4(7) . . . . ? S5 C15 N3B C19B 13.4(13) . . . . ? N3 C15 N3B C16B 171(2) . . . . ? S6 C15 N3B C16B 4.9(11) . . . . ? S5 C15 N3B C16B -168.2(6) . . . . ? C16 C18 C16B N3B -48.1(7) . . . . ? C16 C18 C16B C17B 74.0(10) . . . . ? C15 N3B C16B C18 -98.7(10) . . . . ? C19B N3B C16B C18 79.6(10) . . . . ? C15 N3B C16B C17B 129.3(11) . . . . ? C19B N3B C16B C17B -52.4(13) . . . . ? C15 N3B C19B C20B 61.8(13) . . . . ? C16B N3B C19B C20B -116.7(11) . . . . ? C15 N3B C19B C21 -84.6(12) . . . . ? C16B N3B C19B C21 96.9(12) . . . . ? C19 C21 C19B N3B 112.9(15) . . . . ? C19 C21 C19B C20B -33.5(8) . . . . ? C26 N4 C22 C23 -1.4(3) . . . . ? N4 C22 C23 C24 0.8(3) . . . . ? C22 C23 C24 C25 0.4(3) . . . . ? C23 C24 C25 C26 -1.0(3) . . . . ? C22 N4 C26 C25 0.8(3) . . . . ? C24 C25 C26 N4 0.4(3) . . . . ? C29 N5 C27 C28 0.3(13) . . . . ? N5 C27 C28 C31 2.1(11) . . . . ? C27 N5 C29 C30 -2.9(12) . . . . ? N5 C29 C30 C31 3.1(12) . . . . ? C29 C30 C31 C28 -0.7(13) . . . . ? C27 C28 C31 C30 -2.0(11) . . . . ? _refine_diff_density_max 0.570 _refine_diff_density_min -0.533 _refine_diff_density_rms 0.072 _shelxl_version_number 2012-5 _shelx_res_file ; TITL exp_2637 In(di-i-Pr-dithiocarbamate)3 .1.5 pyridine CELL 0.71073 11.6384 11.9426 14.4945 92.781 102.078 111.637 ZERR 2 0.0004 0.0004 0.0003 0.002 0.002 0.003 LATT 1 SFAC C H IN N S UNIT 57 99 2 9 12 TEMP -173 L.S. 10 size 0.05 0.08 0.10 ! colorless block htab omit 0 1 1 ACTA BOND $H CONF WGHT 0.017600 0.834100 FVAR 2.79972 IN1 3 0.298401 0.182629 0.277993 11.00000 0.01668 0.01636 = 0.01364 0.00364 0.00512 0.00902 S1 5 0.285221 -0.035452 0.299936 11.00000 0.01588 0.01917 = 0.03001 0.01052 0.01040 0.00896 S2 5 0.517168 0.168231 0.287642 11.00000 0.01704 0.01404 = 0.02301 0.00467 0.00801 0.00692 S3 5 0.365604 0.319203 0.438901 11.00000 0.01368 0.02267 = 0.01725 -0.00040 0.00494 0.00621 S4 5 0.103159 0.147450 0.350440 11.00000 0.01466 0.01874 = 0.01782 -0.00086 0.00389 0.00586 S5 5 0.346377 0.371856 0.187186 11.00000 0.02090 0.01830 = 0.02380 0.00705 0.00426 0.00730 S6 5 0.163167 0.125349 0.103619 11.00000 0.02430 0.02305 = 0.01686 -0.00052 0.00314 0.00601 N1 4 0.513027 -0.051749 0.321489 11.00000 0.01364 0.01438 = 0.02054 0.00525 0.00592 0.00559 N2 4 0.166145 0.299656 0.511226 11.00000 0.01463 0.01361 = 0.01669 0.00167 0.00629 0.00414 C1 1 0.446382 0.017803 0.305065 11.00000 0.01672 0.01689 = 0.01344 0.00360 0.00595 0.00650 C2 1 0.653373 -0.000567 0.332276 11.00000 0.01308 0.01714 = 0.02632 0.00479 0.00573 0.00650 AFIX 13 H2 2 0.681273 0.089498 0.333797 11.00000 -1.20000 AFIX 0 C3 1 0.723002 -0.023179 0.426055 11.00000 0.02057 0.02814 = 0.03113 0.00535 0.00007 0.00851 AFIX 137 H3A 2 0.699538 0.010333 0.478924 11.00000 -1.50000 H3B 2 0.815218 0.016428 0.433270 11.00000 -1.50000 H3C 2 0.699114 -0.110869 0.426397 11.00000 -1.50000 AFIX 0 C4 1 0.686558 -0.048404 0.246574 11.00000 0.02420 0.02984 = 0.03367 0.00615 0.01526 0.01188 AFIX 137 H4A 2 0.662707 -0.136433 0.244033 11.00000 -1.50000 H4B 2 0.778416 -0.008443 0.252289 11.00000 -1.50000 H4C 2 0.639932 -0.031158 0.188179 11.00000 -1.50000 AFIX 0 C5 1 0.455651 -0.184678 0.328339 11.00000 0.01796 0.01590 = 0.03925 0.01174 0.00881 0.00806 AFIX 13 H5 2 0.528551 -0.211712 0.338839 11.00000 -1.20000 AFIX 0 C6 1 0.364918 -0.259197 0.235212 11.00000 0.02648 0.01683 = 0.05325 -0.00025 0.00435 0.00604 AFIX 137 H6A 2 0.286174 -0.244194 0.224557 11.00000 -1.50000 H6B 2 0.344908 -0.345853 0.238777 11.00000 -1.50000 H6C 2 0.405332 -0.235460 0.182422 11.00000 -1.50000 AFIX 0 C7 1 0.400824 -0.211625 0.415156 11.00000 0.02967 0.03944 = 0.05255 0.03321 0.01997 0.01860 AFIX 137 H7A 2 0.321743 -0.197304 0.405459 11.00000 -1.50000 H7B 2 0.462593 -0.158226 0.471731 11.00000 -1.50000 H7C 2 0.382848 -0.296690 0.424158 11.00000 -1.50000 AFIX 0 C8 1 0.206904 0.260832 0.441761 11.00000 0.01572 0.01436 = 0.01501 0.00552 0.00456 0.00747 C9 1 0.031857 0.238063 0.517391 11.00000 0.01686 0.01865 = 0.02407 0.00048 0.01031 0.00256 AFIX 13 H9 2 -0.006944 0.161783 0.470746 11.00000 -1.20000 AFIX 0 C10 1 0.025601 0.200228 0.615715 11.00000 0.03004 0.02183 = 0.03262 0.00833 0.01953 0.00869 AFIX 137 H10A 2 0.078204 0.152733 0.631882 11.00000 -1.50000 H10B 2 -0.062926 0.150665 0.615465 11.00000 -1.50000 H10C 2 0.057501 0.272955 0.663031 11.00000 -1.50000 AFIX 0 C11 1 -0.044541 0.315330 0.487320 11.00000 0.01831 0.03497 = 0.02653 0.00537 0.00719 0.01013 AFIX 137 H11A 2 -0.039036 0.334785 0.423068 11.00000 -1.50000 H11B 2 -0.009904 0.390813 0.531983 11.00000 -1.50000 H11C 2 -0.133901 0.270169 0.487536 11.00000 -1.50000 AFIX 0 C12 1 0.242677 0.411751 0.581710 11.00000 0.01915 0.01563 = 0.01763 -0.00050 0.00598 0.00538 AFIX 13 H12 2 0.182939 0.422300 0.618661 11.00000 -1.20000 AFIX 0 C13 1 0.284860 0.525062 0.532988 11.00000 0.02170 0.01567 = 0.02837 0.00273 0.00877 0.00586 AFIX 137 H13A 2 0.212042 0.525507 0.484911 11.00000 -1.50000 H13B 2 0.352189 0.524905 0.502207 11.00000 -1.50000 H13C 2 0.317495 0.597695 0.580490 11.00000 -1.50000 AFIX 0 C14 1 0.351514 0.400534 0.654824 11.00000 0.02694 0.02647 = 0.01962 -0.00063 0.00232 0.01117 AFIX 137 H14A 2 0.388140 0.470950 0.704769 11.00000 -1.50000 H14B 2 0.417396 0.397568 0.623448 11.00000 -1.50000 H14C 2 0.318990 0.325873 0.683269 11.00000 -1.50000 AFIX 0 C15 1 0.231018 0.276998 0.090255 11.00000 0.02122 0.02860 = 0.01716 0.00535 0.00759 0.01478 PART 1 10.83 N3 4 0.201936 0.325058 0.011837 10.83000 0.01984 0.02544 = 0.01624 0.00642 0.00306 0.00921 C16 1 0.094752 0.254982 -0.072478 10.83000 0.02890 0.03395 = 0.01553 0.00227 0.00152 0.01467 AFIX 13 H16 2 0.093908 0.315539 -0.117634 10.83000 -1.20000 AFIX 0 C17 1 -0.034626 0.214511 -0.049645 10.83000 0.02732 0.03098 = 0.02481 -0.00066 0.00056 0.00865 AFIX 137 H17A 2 -0.042826 0.151194 -0.008002 10.83000 -1.50000 H17B 2 -0.101747 0.182050 -0.108830 10.83000 -1.50000 H17C 2 -0.042948 0.284125 -0.017340 10.83000 -1.50000 AFIX 0 PART 0 C18 1 0.115576 0.154879 -0.128003 11.00000 0.05489 0.03930 = 0.03385 0.00406 0.02117 0.02104 AFIX 137 H18A 2 0.199843 0.188059 -0.141667 11.00000 -1.50000 H18B 2 0.049753 0.124061 -0.187980 11.00000 -1.50000 H18C 2 0.110479 0.088351 -0.089952 11.00000 -1.50000 AFIX 0 C21 1 0.188506 0.525192 0.002179 11.00000 0.04555 0.03086 = 0.04413 -0.00217 0.01037 0.00967 AFIX 137 H21A 2 0.238878 0.612125 0.004958 11.00000 -1.50000 H21B 2 0.151687 0.511927 0.057602 11.00000 -1.50000 H21C 2 0.119871 0.496921 -0.056293 11.00000 -1.50000 AFIX 0 PART 1 10.83 C19 1 0.272391 0.456055 0.002592 10.83000 0.02677 0.02712 = 0.02950 0.01607 0.00419 0.00483 AFIX 13 H19 2 0.343404 0.491073 0.061387 10.83000 -1.20000 AFIX 0 C20 1 0.334147 0.465921 -0.080990 10.83000 0.03615 0.05213 = 0.05243 0.03350 0.02219 0.02049 AFIX 137 H20A 2 0.385224 0.416048 -0.075549 10.83000 -1.50000 H20B 2 0.389257 0.550979 -0.080536 10.83000 -1.50000 H20C 2 0.267747 0.437094 -0.140732 10.83000 -1.50000 AFIX 0 PART 2 10.17 N3B 4 0.165802 0.288500 0.003490 10.17000 0.01617 C16B 1 0.052273 0.192676 -0.062284 10.17000 0.01307 AFIX 13 H16A 2 0.019339 0.123616 -0.025843 10.17000 -1.20000 AFIX 0 C17B 1 -0.053287 0.240930 -0.092278 10.17000 0.03538 AFIX 137 H17D 2 -0.066704 0.277549 -0.035572 10.17000 -1.50000 H17E 2 -0.132505 0.173670 -0.125875 10.17000 -1.50000 H17F 2 -0.028088 0.302399 -0.134550 10.17000 -1.50000 AFIX 0 C19B 1 0.218087 0.408706 -0.026820 10.17000 0.02303 AFIX 13 H19A 2 0.170764 0.388471 -0.095429 10.17000 -1.20000 AFIX 0 C20B 1 0.354406 0.442687 -0.038486 10.17000 0.03729 AFIX 137 H20D 2 0.412850 0.456024 0.024172 10.17000 -1.50000 H20E 2 0.379502 0.517260 -0.068096 10.17000 -1.50000 H20F 2 0.357930 0.376479 -0.078984 10.17000 -1.50000 AFIX 0 PART 0 N4 4 0.903845 0.497850 0.265487 11.00000 0.02799 0.02851 = 0.03223 0.00116 0.01385 0.01099 C22 1 0.815765 0.385806 0.234247 11.00000 0.02862 0.03126 = 0.03106 0.00679 0.01100 0.00903 AFIX 43 H22 2 0.730022 0.371266 0.234916 11.00000 -1.20000 AFIX 0 C23 1 0.841935 0.290232 0.201159 11.00000 0.06510 0.02526 = 0.02553 0.00631 0.00545 0.01788 AFIX 43 H23 2 0.775867 0.212210 0.178812 11.00000 -1.20000 AFIX 0 C24 1 0.966291 0.310453 0.201231 11.00000 0.08904 0.05724 = 0.02221 0.01311 0.01798 0.05869 AFIX 43 H24 2 0.987746 0.246632 0.178475 11.00000 -1.20000 AFIX 0 C25 1 1.059026 0.424770 0.234852 11.00000 0.04389 0.07448 = 0.03179 0.01770 0.01735 0.04200 AFIX 43 H25 2 1.145854 0.441117 0.236734 11.00000 -1.20000 AFIX 0 C26 1 1.023234 0.514630 0.265604 11.00000 0.02749 0.04033 = 0.03216 0.00615 0.01144 0.00997 AFIX 43 H26 2 1.087637 0.593446 0.288300 11.00000 -1.20000 AFIX 0 PART -1 N5 4 0.469404 0.113481 0.029149 10.50000 0.05101 0.07502 = 0.02390 0.00565 0.00760 0.00195 C27 1 0.397542 -0.008833 0.035026 10.50000 0.03079 0.05507 = 0.02740 0.01002 0.01700 0.00198 AFIX 43 H27 2 0.324747 -0.030966 0.060702 10.50000 -1.20000 AFIX 0 C28 1 0.437014 -0.094855 0.002105 10.50000 0.04898 0.04972 = 0.02820 -0.00012 0.01230 0.01379 AFIX 43 H28 2 0.392556 -0.179569 0.001488 10.50000 -1.20000 AFIX 0 C29 1 0.569989 0.154596 -0.004763 10.50000 0.04097 0.04193 = 0.04021 0.00764 0.00784 -0.00965 AFIX 43 H29 2 0.611981 0.238341 -0.009251 10.50000 -1.20000 AFIX 0 C30 1 0.606684 0.075985 -0.030728 10.50000 0.02990 0.10898 = 0.05034 0.03656 0.00537 0.00769 AFIX 43 H30 2 0.682510 0.105096 -0.052654 10.50000 -1.20000 AFIX 0 C31 1 0.553376 -0.045115 -0.031981 10.50000 0.08923 0.11059 = 0.02340 0.01414 0.01939 0.07071 AFIX 43 H31 2 0.590075 -0.096881 -0.054306 10.50000 -1.20000 PART 0 AFIX 0 HKLF 4 REM exp_2637 In(di-i-Pr-dithiocarbamate)3 .1.5 pyridine REM R1 = 0.0219 for 8595 Fo > 4sig(Fo) and 0.0272 for all 9388 data REM 422 parameters refined using 0 restraints END WGHT 0.0175 0.8394 REM Instructions for potential hydrogen bonds HTAB C2 S2 HTAB C9 S4 EQIV $1 -x+1, -y+1, -z+1 HTAB C12 N4_$1 HTAB C19_a S5 HTAB C16B_b S6 EQIV $2 -x, -y, -z HTAB C16B_b S6_$2 HTAB C22 S2 REM Highest difference peak 0.570, deepest hole -0.533, 1-sigma level 0.072 Q1 1 0.1994 0.5059 0.0513 11.00000 0.05 0.57 Q2 1 0.2245 0.1111 0.1329 11.00000 0.05 0.57 Q3 1 0.2368 0.1169 0.2095 11.00000 0.05 0.55 Q4 1 0.3397 0.2247 0.2196 11.00000 0.05 0.53 Q5 1 0.2591 0.1423 0.3335 11.00000 0.05 0.47 Q6 1 0.2530 0.2264 0.3162 11.00000 0.05 0.46 Q7 1 0.2387 0.0972 0.2746 11.00000 0.05 0.43 Q8 1 0.2827 0.2648 0.4343 11.00000 0.05 0.42 Q9 1 0.3578 0.2486 0.3426 11.00000 0.05 0.41 Q10 1 0.4662 0.0808 0.2882 11.00000 0.05 0.41 Q11 1 0.2628 0.4582 0.5542 11.00000 0.05 0.41 Q12 1 -0.0056 0.2852 0.5054 11.00000 0.05 0.40 Q13 1 0.3690 0.2518 0.2847 11.00000 0.05 0.39 Q14 1 0.5627 -0.1843 -0.0549 11.00000 0.05 0.39 Q15 1 0.0024 0.2523 -0.1115 11.00000 0.05 0.38 Q16 1 0.1828 0.2220 0.0934 11.00000 0.05 0.38 Q17 1 0.8429 0.3501 0.2050 11.00000 0.05 0.37 Q18 1 0.2889 0.3200 0.1356 11.00000 0.05 0.36 Q19 1 0.1577 0.2114 0.4098 11.00000 0.05 0.36 Q20 1 0.6679 -0.0234 0.2885 11.00000 0.05 0.35 ; _shelx_res_checksum 71837 _shelx_hkl_file ; 0 0 -2 52877.0 645.042 4 0 0 -2 52429.1 660.796 2 0 0 -3 93535.0 1134.76 4 0 0 3 93339.7 1147.62 1 0 0 3 91678.5 1132.06 4 0 0 -3 93340.2 1158.22 2 0 0 4 137604. 1674.91 4 0 0 4 141218. 1631.80 3 0 0 -4 139869. 1710.72 2 0 0 4 138266. 1696.19 1 0 0 -4 142324. 1680.06 4 0 0 5 55798.2 765.375 1 0 0 5 55139.1 685.600 3 0 0 -5 56309.4 744.949 4 0 0 5 54422.4 738.881 4 0 0 -5 55291.7 778.404 2 0 0 -6 3923.98 147.154 2 0 0 6 3749.41 133.798 1 0 0 6 3899.66 121.587 4 0 0 6 3904.55 143.380 2 0 0 6 3822.28 89.0315 3 0 0 -6 4158.76 129.217 4 0 0 -7 47814.8 735.616 2 0 0 -7 48447.4 693.501 4 0 0 7 45915.1 714.921 1 0 0 7 48109.6 743.719 2 0 0 7 46414.9 680.376 4 0 0 7 46836.6 605.555 3 0 0 -8 2064.42 119.941 2 0 0 8 2031.80 64.7512 3 0 0 8 2049.98 113.222 1 0 0 8 2048.89 120.875 2 0 0 8 1986.65 97.8960 4 0 0 9 3192.48 84.9913 3 0 0 9 3214.12 160.823 2 0 0 9 3099.22 130.106 4 0 0 -9 3229.64 159.619 2 0 0 9 3360.14 153.324 1 0 0 10 12665.5 301.436 4 0 0 -10 13164.7 356.710 2 0 0 10 13155.4 211.958 3 0 0 10 13406.7 346.083 1 0 0 11 41899.8 695.074 4 0 0 -11 42086.9 774.030 2 0 0 11 42820.4 765.255 1 0 0 12 2372.72 130.128 4 0 0 -12 2313.82 160.682 2 0 0 12 2480.51 157.424 1 0 0 -13 24014.0 566.616 2 0 0 13 22959.3 480.236 4 0 0 -14 14097.7 436.197 2 0 0 -15 199.474 76.4298 2 0 0 -16 4400.58 255.343 2 0 0 -17 142.773 82.2500 2 0 0 -18 6201.70 328.928 2 0 0 18 6167.62 333.626 5 0 -1 19 2348.19 216.131 5 0 -1 18 1495.35 175.303 5 0 1 -18 1534.73 176.088 2 0 1 -17 5850.16 312.104 2 0 -1 17 6186.40 313.013 5 0 1 -16 3089.43 220.290 2 0 -1 16 3186.61 219.050 5 0 1 -15 2229.77 179.275 2 0 1 -14 75.0048 69.5313 2 0 -1 13 22673.1 347.508 3 0 -1 13 20416.4 430.402 4 0 1 -13 21168.5 540.838 2 0 1 -12 32876.3 684.759 2 0 -1 12 34438.3 499.445 3 0 -1 12 32836.1 572.103 4 0 -1 12 33351.1 678.123 1 0 -1 11 3886.06 119.602 3 0 -1 11 3557.13 143.931 4 0 1 -11 3808.04 194.510 2 0 -1 11 3591.94 182.203 1 0 -1 10 8497.05 222.634 4 0 -1 10 8855.11 277.538 1 0 1 -10 8775.74 285.792 2 0 -1 10 8754.63 193.840 3 0 -1 9 11257.3 226.551 3 0 1 -9 11017.4 310.842 2 0 -1 9 11197.6 302.428 1 0 -1 9 11626.7 319.800 2 0 -1 9 10602.4 244.494 4 0 -1 8 6140.67 204.373 1 0 -1 8 5909.68 160.990 4 0 1 -8 6084.51 210.641 2 0 -1 7 13540.4 260.314 4 0 1 -7 14590.6 315.789 1 0 1 -7 14375.6 323.981 2 0 -1 7 13535.2 309.385 1 0 1 -6 31585.1 512.094 1 0 1 -6 31646.1 525.403 2 0 -1 6 30073.0 450.396 4 0 -1 6 31347.2 513.438 1 0 -1 5 12966.6 220.942 4 0 1 -5 13442.1 275.543 2 0 1 -5 13606.9 270.994 1 0 -1 5 12658.3 265.979 1 0 1 -4 4875.64 139.885 2 0 1 -4 4920.95 135.833 1 0 -1 4 4738.80 102.776 4 0 -1 4 4723.22 133.746 1 0 1 -3 5192.13 128.569 2 0 -1 3 5107.66 127.637 1 0 1 -3 5324.40 130.151 1 0 1 -2 47942.8 622.329 1 0 1 -2 47778.7 614.676 2 0 -1 -1 108785. 1301.51 4 0 -1 -2 33868.1 442.189 2 0 -1 -2 33168.1 460.067 4 0 1 2 33727.0 442.895 2 0 -1 -3 290644. 3376.16 2 0 1 3 285790. 3386.58 4 0 -1 -3 287375. 3389.47 4 0 1 3 286475. 3376.00 2 0 -1 -4 14446.5 264.331 2 0 1 4 14338.6 265.800 4 0 -1 -4 14634.7 269.216 4 0 1 4 14608.9 266.436 2 0 -1 -5 169554. 2054.02 2 0 1 5 166376. 2058.05 2 0 -1 -5 168931. 2054.72 4 0 1 5 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879.268 125.475 2 1 -4 -17 25.9704 67.0038 2 1 -4 -16 10224.7 372.649 2 1 -4 -15 2045.57 171.332 4 1 -4 -15 2026.26 158.263 2 1 -4 -14 364.842 83.5483 4 1 -4 -14 381.130 79.5448 2 1 -4 -13 4159.54 207.129 2 1 -4 -13 4400.27 233.989 4 1 -4 -12 36.6879 43.2877 4 1 -4 -12 109.123 54.0964 2 1 -4 -11 21418.9 472.197 2 1 -4 -11 21694.7 524.873 4 -1 4 10 10920.4 312.620 2 1 -4 -10 11024.2 226.897 3 1 -4 -10 10904.7 300.577 2 1 -4 -10 11749.0 353.518 4 1 -4 -9 11290.9 337.110 4 1 -4 -9 11152.3 289.233 2 1 -4 -9 11218.6 238.727 3 -1 4 9 11088.1 298.564 2 -1 4 9 11531.8 320.924 4 -1 4 8 10956.9 277.402 2 -1 4 8 11489.7 307.464 4 1 -4 -8 10917.0 317.314 4 1 -4 -8 10733.9 236.592 3 1 -4 -8 10738.7 266.050 2 -1 4 7 3551.16 137.226 2 -1 4 7 3534.18 157.275 4 1 -4 -7 3669.29 169.741 4 1 -4 -7 3465.54 132.025 2 1 -4 -7 3449.61 124.411 3 -1 4 6 10865.6 241.437 2 1 -4 -6 10825.8 294.289 4 1 -4 -6 10996.4 237.928 2 -1 4 6 10957.4 285.097 4 1 -4 -6 10629.9 245.566 3 1 -4 -5 27504.3 515.153 4 1 -4 -5 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196.143 57.1015 1 1 -4 8 178.441 54.6207 2 -1 4 -9 2819.53 157.513 1 -1 4 -9 3028.04 167.290 2 -1 4 -10 34262.2 676.580 2 -1 4 -10 34037.7 657.897 1 1 -4 10 33428.1 545.283 4 1 -4 11 3172.31 130.358 4 1 -4 11 3213.84 158.908 5 -1 4 -11 3291.85 179.548 1 -1 4 -11 3303.60 191.361 2 1 -4 12 27346.1 482.324 4 -1 4 -12 26698.9 623.134 2 1 -4 12 26389.0 550.192 5 -1 4 -12 27119.2 595.662 1 1 -4 13 3643.23 148.416 4 -1 4 -13 3684.08 204.518 1 -1 4 -13 3596.75 217.784 2 1 -4 13 3340.59 184.146 5 1 -4 14 22827.7 537.963 5 -1 4 -14 22617.8 603.602 2 -1 4 -15 219.869 94.8197 2 1 -4 15 25.1630 78.0135 5 1 -4 16 19471.0 526.389 5 -1 4 -16 20235.0 604.180 2 1 -4 17 5046.85 269.180 5 -1 4 -17 5734.56 322.480 2 1 -4 18 1738.18 174.814 5 1 -4 19 1000.03 141.721 5 1 -3 -18 193.045 83.8774 2 1 -3 -17 19188.1 555.511 2 1 -3 -16 562.339 101.350 2 1 -3 -15 8846.79 336.755 2 1 -3 -14 9958.17 345.979 2 1 -3 -14 10571.3 358.717 4 1 -3 -13 109.038 56.0491 2 1 -3 -13 56.0924 50.2908 4 1 -3 -12 6814.05 257.892 2 1 -3 -12 7010.92 271.147 4 -1 3 11 81.4611 48.6983 1 -1 3 11 216.866 53.2270 4 1 -3 -11 186.960 60.3028 4 1 -3 -11 161.986 57.1510 2 -1 3 10 37272.8 685.493 2 -1 3 10 38256.3 673.025 4 1 -3 -10 37051.9 661.208 2 1 -3 -10 37134.1 692.019 4 -1 3 9 13093.3 326.188 4 1 -3 -9 12074.2 332.782 4 1 -3 -9 12559.6 236.598 3 1 -3 -9 12303.3 311.150 2 -1 3 9 13178.7 330.530 2 1 -3 -8 11.8288 32.5273 2 1 -3 -8 31.1477 18.7874 3 -1 3 8 35.0009 30.7516 4 -1 3 8 39.2453 29.3535 2 1 -3 -8 35.9279 36.0377 4 1 -3 -7 17018.3 300.606 3 -1 3 7 16964.2 361.102 4 1 -3 -7 17218.9 376.400 4 -1 3 7 16796.4 347.927 2 1 -3 -7 16535.6 336.043 2 1 -3 -6 12899.4 263.814 2 -1 3 6 12615.9 269.181 2 1 -3 -6 12597.8 249.017 3 -1 3 6 13009.9 290.900 4 1 -3 -6 12712.5 301.645 4 -1 3 5 65.6757 33.2073 2 1 -3 -5 36.7975 34.0945 4 1 -3 -5 32.0090 24.9493 2 1 -3 -5 70.5102 27.5799 3 -1 3 5 46.0140 27.0599 4 1 -3 -4 55472.0 797.582 4 -1 3 4 55225.2 727.196 2 1 -3 -4 56221.3 723.009 2 1 -3 -4 54824.2 759.157 3 -1 3 4 54452.5 781.783 4 1 -3 -3 227.511 41.5708 4 1 -3 -3 455.904 29.9254 2 -1 3 3 240.501 23.4217 2 1 -3 -2 8494.26 128.702 2 1 -3 -2 8561.44 195.217 4 1 -3 -1 32499.2 478.564 4 1 -3 0 2997.70 95.7830 4 1 -3 0 2893.27 59.3061 2 1 -3 1 107511. 1323.71 4 -1 3 -1 111354. 1295.75 2 1 -3 1 105988. 1291.60 2 -1 3 -2 36956.4 505.345 2 1 -3 2 36510.4 502.304 4 1 -3 2 35632.7 501.957 2 -1 3 -3 37501.6 542.540 2 1 -3 3 36887.5 538.301 2 1 -3 4 93007.9 1226.30 2 -1 3 -4 95656.0 1234.89 2 -1 3 -5 20042.3 379.163 2 -1 3 -5 19493.4 379.614 1 -1 3 -6 14691.8 327.989 2 -1 3 -6 14214.8 318.547 1 -1 3 -7 35837.2 610.663 1 -1 3 -7 36161.9 627.414 2 -1 3 -8 3403.97 164.166 2 1 -3 8 3098.80 119.622 4 -1 3 -8 3316.58 151.791 1 -1 3 -9 2440.91 135.428 1 -1 3 -9 2288.15 143.487 2 1 -3 9 2275.17 104.615 4 -1 3 -10 481.903 82.6488 2 -1 3 -10 496.766 70.3935 1 1 -3 10 524.363 55.5500 4 1 -3 11 199.956 42.3337 4 -1 3 -11 184.958 72.0628 2 -1 3 -11 157.524 53.2464 1 1 -3 12 8915.25 248.313 4 -1 3 -12 9400.03 336.397 2 1 -3 13 3036.32 140.816 4 1 -3 13 3206.35 132.309 3 -1 3 -13 3089.93 200.211 2 1 -3 14 8941.10 226.577 3 -1 3 -14 8902.95 354.885 2 1 -3 15 22904.7 572.110 5 -1 3 -15 24012.4 634.051 2 -1 3 -16 2670.40 213.719 2 1 -3 16 2515.43 190.812 5 1 -3 17 10088.6 393.065 5 -1 3 -17 10657.2 435.602 2 -1 3 -18 607.139 120.782 2 1 -3 18 531.978 116.849 5 1 -3 19 6131.42 322.975 5 1 -2 -18 13481.0 479.355 2 -1 2 18 13860.5 519.923 5 1 -2 -17 1725.30 170.396 2 -1 2 17 1737.63 184.940 5 1 -2 -16 21310.6 576.287 2 1 -2 -15 410.717 90.9003 2 1 -2 -14 8437.21 315.747 2 1 -2 -13 11312.2 360.418 2 1 -2 -13 12350.1 355.904 4 -1 2 13 11720.9 329.247 4 1 -2 -12 50470.9 887.592 2 1 -2 -12 52418.2 878.206 4 -1 2 12 51639.4 847.746 4 1 -2 -11 71887.7 1122.64 2 -1 2 11 73650.4 1088.75 4 -1 2 11 73714.4 1154.27 1 1 -2 -11 72931.1 1113.54 4 -1 2 10 1149.44 100.563 1 -1 2 10 1289.18 107.089 2 1 -2 -10 1066.18 92.8164 4 -1 2 10 1196.97 93.4810 4 1 -2 -10 1111.28 98.8959 2 -1 2 9 11402.1 284.826 4 1 -2 -9 11334.9 298.014 4 -1 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407.098 4 2 -11 2 13052.5 284.265 2 2 -11 3 5275.02 238.770 4 2 -11 3-3.51765 16.6922 2 2 -11 4 648.674 94.6660 4 2 -11 5 1055.45 109.514 4 2 -11 5 1051.82 92.3165 2 2 -11 6-14.4600 48.2458 4 2 -11 7-10.5195 47.1332 4 2 -11 8-25.5402 46.9000 4 -2 11 -9 2815.68 235.599 1 2 -11 9 2789.74 163.806 4 -2 11 -10-12.3401 73.6721 1 2 -11 10 44.2237 40.3682 4 -2 11 -11 7475.73 393.532 1 -2 11 -12 2756.08 247.184 1 -2 11 -13 7166.37 396.998 1 -2 11 -14 8422.56 434.532 1 -2 11 -15 2531.20 243.757 1 -2 11 -16 1364.89 189.933 1 2 -10 -13 1193.91 167.424 4 2 -10 -12 7497.53 388.404 4 2 -10 -11 1449.01 173.793 4 2 -10 -10 17007.5 573.726 4 2 -10 -9 703.555 127.488 4 2 -10 -8 1613.61 164.917 4 2 -10 -7-29.1542 72.1580 4 2 -10 -6 5458.20 288.009 4 2 -10 -5 4594.97 256.445 4 2 -10 -4 945.884 119.792 4 2 -10 -3 7615.64 315.525 4 2 -10 -2 1814.08 159.401 4 2 -10 -1 8519.96 321.788 4 2 -10 -1 8900.46 161.850 2 2 -10 0 2540.82 87.9841 2 2 -10 0 2369.72 166.162 4 2 -10 1 67929.7 1119.72 4 2 -10 1 67351.3 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29998.2 541.076 4 2 -8 7 31235.6 604.336 2 2 -8 8 3886.29 158.547 4 -2 8 -8 3990.65 228.166 1 -2 8 -9 11889.3 412.208 1 2 -8 9 12058.5 293.377 4 -2 8 -10 8.52385 58.2472 1 2 -8 10-6.56922 41.6925 4 2 -8 11 14185.5 300.098 5 2 -8 11 13744.8 320.694 4 -2 8 -11 14704.8 475.136 1 2 -8 12 17554.1 366.781 4 2 -8 12 17977.7 367.283 5 -2 8 -12 17181.2 529.328 1 -2 8 -13 65.5819 66.8514 1 2 -8 13 120.118 59.1403 5 -2 8 -14 15560.2 516.684 1 -2 8 -15 621.818 114.683 1 -2 8 -16 7818.45 369.710 1 -2 8 -17 10470.0 438.041 1 2 -7 -17 410.573 109.270 4 2 -7 -16 2399.86 215.977 4 2 -7 -15 4567.18 285.101 4 2 -7 -14 8048.02 285.536 2 2 -7 -14 8059.17 372.145 4 2 -7 -13 585.772 106.125 4 2 -7 -13 673.061 84.1933 2 2 -7 -12 14633.7 481.418 4 2 -7 -12 14728.7 364.163 2 2 -7 -11 5844.29 288.732 4 2 -7 -11 6127.00 210.309 2 2 -7 -10 5955.04 271.290 4 2 -7 -10 5652.79 179.649 2 2 -7 -9 721.183 64.5097 2 2 -7 -9 658.845 98.2230 4 2 -7 -9 241.141 48.0997 3 2 -7 -8 3011.62 186.781 4 2 -7 -8 3331.05 122.603 2 2 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7135.54 208.546 4 2 -7 10 6972.66 195.662 5 -2 7 -10 6948.58 283.559 2 -2 7 -11-15.9762 54.9329 1 2 -7 11 25.7491 52.5167 5 -2 7 -11 22.6976 60.4765 2 2 -7 11 57.3611 42.0682 4 -2 7 -12 28210.2 681.056 1 -2 7 -12 28957.4 690.693 2 2 -7 12 30734.2 551.771 5 2 -7 12 30850.9 522.171 4 -2 7 -13 895.577 125.440 2 2 -7 13 1083.94 84.2633 4 -2 7 -13 1084.51 127.998 1 2 -7 13 883.885 95.9642 5 -2 7 -14 5235.16 289.180 2 -2 7 -14 4880.44 268.296 1 2 -7 14 5225.96 219.606 5 2 -7 15 2204.19 154.391 5 -2 7 -15 2375.66 190.799 1 -2 7 -16 1297.11 149.195 1 2 -6 -17 400.045 97.8335 4 2 -6 -16 4928.13 289.834 4 2 -6 -15-19.3221 52.9319 2 2 -6 -15 37.6862 67.5142 4 2 -6 -14 4297.20 256.005 4 2 -6 -14 4092.97 204.956 2 2 -6 -13 15102.4 394.098 2 2 -6 -13 14814.4 478.405 4 2 -6 -12 831.649 115.719 4 2 -6 -12 771.537 86.1904 2 2 -6 -11 18414.3 383.519 3 2 -6 -11 18298.3 405.290 2 2 -6 -11 17464.1 498.429 4 -2 6 11 17909.3 415.851 2 2 -6 -10 2557.51 129.144 2 2 -6 -10 2433.80 172.856 4 -2 6 10 2350.19 128.372 2 2 -6 -10 2273.49 123.933 3 -2 6 9 15337.5 341.700 2 2 -6 -9 15533.5 436.385 4 2 -6 -9 16144.8 338.424 2 2 -6 -9 15462.8 362.849 3 2 -6 -8 13807.8 287.918 2 2 -6 -8 13806.6 394.312 4 2 -6 -8 12888.3 328.329 3 2 -6 -7 43.1378 28.2978 2 2 -6 -7 78.4015 55.2317 4 2 -6 -7 30.8193 31.9834 3 -2 6 6 24492.4 498.784 4 2 -6 -6 24441.9 377.669 2 2 -6 -6 24273.4 521.061 4 2 -6 -6 22639.0 475.304 3 2 -6 -5 1108.59 98.1339 4 2 -6 -5 1194.87 52.5456 2 -2 6 5 1271.10 98.2042 4 2 -6 -5 1105.32 90.5139 3 2 -6 -4 4281.12 88.0585 2 2 -6 -4 4134.13 179.925 4 2 -6 -3 1333.26 101.152 4 2 -6 -2 14014.1 334.180 4 2 -6 -1 7054.99 217.182 4 2 -6 0 45299.7 716.942 4 2 -6 0 45928.1 584.931 2 -2 6 0 46265.6 703.778 4 -2 6 -1 489.882 22.4896 5 2 -6 1 618.346 66.8775 4 -2 6 -1 659.467 64.8828 4 2 -6 1 594.921 39.7538 2 2 -6 2 17281.6 349.481 4 2 -6 2 17248.7 300.358 2 2 -6 3 138.706 29.4811 2 2 -6 3 90.4035 48.7024 4 2 -6 4 12968.7 286.084 2 2 -6 4 12704.7 283.186 4 -2 6 -4 13343.1 294.157 2 -2 6 -5 40851.6 659.708 2 2 -6 5 42261.1 626.026 4 -2 6 -6 22941.2 462.238 2 2 -6 6 23085.1 331.128 5 2 -6 6 21971.8 405.705 4 -2 6 -7 3279.30 175.228 1 2 -6 7 3278.07 130.593 4 -2 6 -7 3043.63 157.538 2 2 -6 7 3077.31 100.609 5 -2 6 -8 670.624 86.9995 1 -2 6 -8 691.687 86.5062 2 2 -6 8 875.418 77.1929 4 2 -6 8 800.673 61.3901 5 -2 6 -9 652.684 88.6744 2 2 -6 9 659.916 64.0303 5 2 -6 9 763.403 75.7971 4 -2 6 -9 721.716 94.2568 1 -2 6 -10 288.525 79.0689 2 -2 6 -10 208.492 61.0312 1 2 -6 10 183.724 47.7396 5 -2 6 -11 12058.4 387.847 2 2 -6 11 12252.4 305.464 5 -2 6 -11 12108.5 381.486 1 -2 6 -12 1609.04 151.964 2 2 -6 12 1713.09 111.230 4 2 -6 12 1536.45 115.230 5 -2 6 -12 1637.94 142.651 1 2 -6 13 4639.67 201.260 5 -2 6 -13 4599.89 256.206 2 -2 6 -13 4511.71 239.349 1 -2 6 -14 2829.56 192.987 1 -2 6 -14 2976.13 215.878 2 2 -6 14 2858.74 171.064 5 -2 6 -15 5205.35 294.987 2 -2 6 -15 5057.60 265.598 1 2 -6 15 5007.94 234.743 5 -2 6 -16 3069.97 239.275 2 2 -6 16 2976.08 193.915 5 -2 6 -17 151.902 93.1628 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768.321 105.796 4 -7 8 -1 651.265 64.2924 2 7 -8 2 12015.3 246.127 5 7 -8 2 12893.4 373.410 4 -7 8 -2 11974.7 299.916 2 7 -8 3 15534.9 292.873 5 -7 8 -3 15873.7 373.277 2 -7 8 -4 52.3072 42.2119 2 -7 8 -5 1026.37 102.115 2 -7 8 -6 455.832 76.1742 2 -7 8 -7 1148.52 118.410 2 -7 8 -8 2827.33 187.061 2 -7 8 -9 28208.6 600.518 1 -7 8 -9 26408.8 645.253 2 -7 8 -10 1530.59 153.973 2 -7 8 -10 1481.65 125.268 1 -7 8 -11 13688.8 469.792 2 -7 8 -12 3551.96 245.294 2 -7 8 -13 3524.79 254.140 2 -7 8 -14 12135.0 488.698 2 -7 7 16 2849.09 238.226 5 -7 7 15 2730.46 223.510 5 7 -7 -15 2641.67 192.499 4 -7 7 14 12541.9 445.510 5 7 -7 -14 11838.2 411.114 4 -7 7 13 1346.89 159.166 5 7 -7 -13 1009.86 119.075 4 -7 7 12 9329.33 350.877 5 7 -7 -12 8310.93 323.582 4 -7 7 11-134.835 108.918 5 -7 7 10 38337.1 745.559 5 7 -7 -10 37652.3 751.596 4 -7 7 10 36467.7 632.563 2 -7 7 9 13625.8 385.318 5 7 -7 -9 13018.5 385.404 4 -7 7 9 13232.1 304.908 2 -7 7 8 3766.60 193.032 5 7 -7 -8 3907.29 199.261 4 -7 7 8 3549.90 137.683 2 -7 7 7 179.149 86.5350 5 7 -7 -7 154.470 59.9462 4 -7 7 7 117.169 32.9765 2 -7 7 6 1254.92 122.308 5 -7 7 6 980.481 65.8204 2 7 -7 -6 826.185 102.750 4 7 -7 -5 830.876 98.2042 4 7 -7 -4 1065.27 111.211 4 7 -7 -3 25821.9 554.797 4 -7 7 3 27501.2 426.546 2 7 -7 -3 25128.4 480.447 5 -7 7 2 937.182 64.8994 2 7 -7 -2 905.099 76.3994 5 7 -7 -2 1025.70 114.094 4 7 -7 -1 3118.23 131.033 5 -7 7 1 3529.69 131.016 2 7 -7 -1 3422.39 182.982 4 7 -7 0 189.190 51.7112 5 -7 7 0 303.600 45.9790 2 7 -7 0 502.083 102.364 4 -7 7 -1 25533.5 471.476 2 7 -7 1 24481.6 424.374 5 -7 7 -2 2536.47 131.836 2 -7 7 -3 24740.3 501.597 2 -7 7 -4 6751.03 242.655 2 -7 7 -5 173.891 54.8982 2 -7 7 -6 114.255 53.8848 2 -7 7 -7 1357.90 126.402 2 -7 7 -8 3460.32 169.233 1 -7 7 -8 3701.53 211.332 2 -7 7 -9 329.600 57.5817 1 -7 7 -9 231.038 80.8570 2 -7 7 -10 12846.1 341.375 1 -7 7 -10 13181.0 444.368 2 -7 7 -11 459.451 92.1609 2 -7 7 -12 7802.11 360.597 2 -7 7 -13 1799.26 186.434 2 -7 7 -14 10684.7 455.574 2 -7 6 17 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767.366 118.311 4 9 -10 -5 31516.8 723.238 4 9 -10 -4-9.56237 79.5442 4 9 -10 -3 40004.8 837.167 4 -9 10 3 41040.0 579.359 2 9 -10 -2 1271.11 143.527 4 -9 10 2 1240.65 73.0502 2 9 -10 -1 23147.8 581.142 4 -9 10 1 21596.0 405.447 2 9 -10 0 11152.0 388.277 4 -9 10 0 10459.0 268.100 2 -9 10 -1 390.781 60.6550 2 9 -10 1 370.837 94.9201 4 9 -10 2 30341.3 696.582 4 -9 10 -2 29770.9 575.515 2 9 -10 3 137.312 83.6136 4 -9 10 -3 77.5588 45.9659 2 9 -10 4 23588.9 600.096 4 -9 10 -4 21704.4 508.282 2 9 -10 5 6242.57 301.551 4 -9 10 -5 6288.83 261.277 2 -9 10 -6 14889.6 437.139 2 -9 10 -7 18331.0 510.876 2 -9 10 -8 4292.97 243.654 2 -9 10 -9 3552.26 230.975 2 -9 10 -10 531.218 102.313 2 -9 10 -11 2918.22 227.033 2 -9 10 -12 1628.25 182.370 2 -9 9 15 4638.74 295.911 5 9 -9 -15 4814.39 285.748 4 -9 9 14 2724.64 229.516 5 9 -9 -14 2363.00 199.413 4 -9 9 13 2513.06 211.416 5 9 -9 -13 2705.56 206.696 4 -9 9 12 3074.34 220.991 5 9 -9 -12 2826.01 208.527 4 -9 9 11 5512.91 275.289 5 9 -9 -11 5215.73 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982.494 142.678 2 -9 9 -12 7380.88 372.779 2 -9 8 15 7117.86 359.194 5 9 -8 -15 6699.86 321.281 4 -9 8 14 3566.83 254.802 5 9 -8 -14 3208.60 217.581 4 -9 8 13 3241.02 229.154 5 9 -8 -13 2734.67 198.474 4 -9 8 12 5008.45 271.853 5 9 -8 -12 4894.14 260.025 4 -9 8 11 7040.54 307.106 5 9 -8 -11 6713.75 298.367 4 -9 8 10 16470.7 465.244 5 9 -8 -10 15519.1 461.269 4 -9 8 9 4689.30 238.866 5 9 -8 -9 4423.36 234.986 4 9 -8 -8 13404.6 413.028 4 9 -8 -7 6405.82 275.962 4 9 -8 -6 319.287 82.9664 4 9 -8 -5 5614.72 255.678 4 9 -8 -4 9326.72 332.705 4 -9 8 4 9587.27 240.636 2 9 -8 -3 26714.0 532.088 5 -9 8 3 28854.5 500.775 2 9 -8 -3 28526.2 627.121 4 9 -8 -2-72.9198 64.0032 5 -9 8 2 10.4166 32.9916 2 9 -8 -1 13745.8 335.449 5 -9 8 1 14708.1 344.507 2 9 -8 -1 15193.1 436.490 4 9 -8 0 2839.95 139.933 5 -9 8 0 2884.84 148.049 2 9 -8 1 22791.4 449.344 5 -9 8 -1 24742.9 503.277 2 9 -8 2 9348.75 257.544 5 -9 8 -2 9960.50 305.646 2 -9 8 -3 38241.8 724.789 2 -9 8 -4 236.088 65.4950 2 -9 8 -5 7512.51 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522.941 104.355 1 -9 -6 4 11270.5 471.884 3 9 6 -4 11050.4 421.822 1 -9 -6 3 18759.6 615.106 3 9 6 -3 19483.3 563.459 1 -9 -6 2 1709.17 182.903 3 9 6 -2 1700.08 158.867 1 9 6 -1 1099.72 127.120 1 -9 -6 1 826.156 130.603 3 -9 -6 0 58.2965 64.0112 3 9 6 0 115.334 61.7035 1 -9 -6 -1 3826.47 254.306 3 -9 -6 -2 1095.82 140.682 3 -9 -6 -3 4504.11 271.962 3 -9 -6 -3 4584.70 279.461 2 -9 -6 -4 6054.42 326.828 2 -9 -6 -5 19.0353 75.1991 2 -9 -6 -6 118.892 74.3803 2 9 7 -11 5070.66 335.362 1 9 7 -10 2124.28 218.860 1 -9 -7 10 2138.23 235.422 3 9 7 -9 9080.02 436.018 1 -9 -7 9 10692.4 506.735 3 -9 -7 8 255.959 97.4699 3 9 7 -8 119.489 84.9611 1 -9 -7 7 84.6222 79.6823 3 9 7 -7 133.291 81.7347 1 -9 -7 6-11.3454 84.0316 3 9 7 -6-33.5037 69.8707 1 -9 -7 5 9064.17 441.981 3 9 7 -5 8340.94 388.053 1 -9 -7 4 4155.21 299.381 3 9 7 -4 4192.00 268.001 1 -9 -7 3 13272.6 529.971 3 9 7 -3 13599.3 485.089 1 -9 -7 2 7239.36 380.354 3 9 7 -2 7129.97 338.705 1 -9 -7 1 2937.19 239.629 3 9 7 -1 3288.58 222.510 1 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9898.09 383.276 4 -11 9 0 7470.10 271.812 2 -11 9 -1 2196.64 150.651 2 -11 9 -2 7570.20 292.093 2 -11 9 -3 6034.29 267.497 2 -11 9 -4 0.65466 56.4578 2 -11 9 -5 1872.57 161.384 2 -11 9 -6 593.056 104.492 2 -11 9 -7 4987.94 280.741 2 -11 9 -8 53.8663 69.1479 2 -11 9 -9 13324.0 493.675 2 -11 9 -10 11728.5 474.663 2 11 -8 -13 2953.23 210.142 4 11 -8 -12 4962.32 265.010 4 11 -8 -11 88.2815 67.5610 4 -11 8 11 33.2955 80.8218 3 11 -8 -10 1937.77 164.614 4 -11 8 10 1876.06 192.907 3 11 -8 -9 1074.25 129.373 4 -11 8 9 1379.40 165.672 3 -11 8 8 40.8020 68.3071 3 11 -8 -8 34.8392 69.3895 4 11 -8 -7 18.6267 64.8687 4 -11 8 7 14.3176 67.3171 3 11 -8 -6 995.600 125.969 4 -11 8 6 760.833 126.239 3 11 -8 -5 924.215 123.312 4 -11 8 5 896.643 141.901 3 11 -8 -4 739.271 121.359 4 -11 8 3 4717.18 200.800 2 11 -8 -3 4984.28 261.701 4 -11 8 2 11260.0 330.108 2 -11 8 1 1984.14 138.200 2 -11 8 0 3159.15 177.624 2 -11 8 -1 8095.56 299.131 2 -11 8 -2 1280.14 125.772 2 -11 8 -3 2970.54 191.683 2 -11 8 -4 772.103 108.101 2 -11 8 -5 292.633 79.3613 2 -11 8 -6 2893.80 209.708 2 -11 8 -7 5024.83 284.849 2 -11 8 -8 5342.97 300.947 2 -11 8 -9 667.606 126.201 2 -11 8 -10 8650.97 405.944 2 -11 7 15 4199.53 295.156 3 -11 7 14 225.811 86.8073 3 11 -7 -13 5702.27 271.903 4 -11 7 13 5029.82 318.925 3 -11 7 12 44.4089 69.6461 3 11 -7 -12 28.0850 55.3341 4 11 -7 -11 12010.3 396.282 4 -11 7 11 11784.5 479.782 3 11 -7 -10 2995.67 193.570 4 -11 7 10 3372.66 251.777 3 11 -7 -9 1266.41 130.514 4 -11 7 9 1331.15 161.956 3 11 -7 -8 1614.22 144.023 4 -11 7 8 1500.56 169.642 3 11 -7 -7 9224.15 335.953 4 -11 7 7 8614.10 392.990 3 -11 7 6 29.5693 67.4230 3 11 -7 -6 108.358 70.2937 4 11 -7 -5 8973.91 334.440 4 -11 7 5 8644.62 387.228 3 -11 7 4 72.8051 61.4254 3 11 -7 -4 171.902 84.3276 4 -11 7 3 140.270 79.0949 3 -11 7 2 11225.3 338.049 2 -11 7 2 10894.2 429.550 3 -11 7 1 534.576 106.537 3 -11 7 1 525.675 80.5002 2 -11 7 0 12475.7 376.485 2 -11 7 -1 2422.21 165.591 2 -11 7 -2 1339.40 131.705 2 -11 7 -3 8063.28 323.260 2 -11 7 -4-21.7936 66.0290 2 -11 7 -5 1172.99 133.640 2 -11 7 -6 3031.19 213.602 2 -11 7 -7 103.310 75.9286 2 -11 7 -8 1094.82 146.218 2 -11 7 -9 337.914 99.6562 2 -11 7 -10 76.9505 73.4355 2 -11 6 16 85.8610 68.8196 3 -11 6 15 5539.72 335.382 3 -11 6 14 1098.40 156.283 3 11 -6 -13 5763.14 257.906 4 -11 6 13 5234.03 318.193 3 11 -6 -12 14047.5 419.323 4 -11 6 12 13785.5 519.951 3 11 -6 -11 1310.89 126.291 4 -11 6 11 1426.65 166.644 3 11 -6 -10 5000.12 240.276 4 -11 6 10 4903.78 298.812 3 11 -6 -9 2403.40 168.176 4 -11 6 9 2494.66 211.199 3 11 -6 -8 6657.08 274.390 4 -11 6 8 6105.46 325.478 3 11 -6 -7 1256.30 129.277 4 -11 6 7 973.866 135.112 3 11 -6 -6 25236.2 584.583 4 -11 6 6 24451.5 678.777 3 -11 6 5 1623.83 166.721 3 -11 6 4 12473.7 456.461 3 -11 6 3 3022.29 220.838 3 -11 6 2 3139.63 224.316 3 -11 6 1 3084.58 221.417 3 -11 6 1 3023.43 177.655 2 -11 6 0 5147.26 240.017 2 -11 6 0 5498.21 294.692 3 -11 6 -1 18906.4 497.356 2 -11 6 -1 18339.9 555.395 3 -11 6 -2 9697.17 352.286 2 -11 6 -3 3369.15 210.229 2 -11 6 -4 6532.58 301.656 2 -11 6 -5 6313.33 306.055 2 -11 6 -6 293.993 86.4263 2 -11 6 -7 2420.41 200.940 2 -11 6 -8-13.1853 71.6189 2 -11 6 -9-89.3936 91.2222 2 -11 6 -10 1350.34 169.682 2 -11 5 17 4415.93 307.588 3 -11 5 16 1859.44 201.893 3 -11 5 15 821.204 133.841 3 -11 5 14 9813.75 442.617 3 -11 5 13 11.8120 74.1388 3 11 -5 -13 123.982 55.4722 4 11 -5 -12 15370.9 423.053 4 -11 5 12 15169.8 545.025 3 11 -5 -11 5048.17 231.983 4 -11 5 11 5144.29 305.269 3 11 -5 -10 909.339 106.363 4 -11 5 10 923.924 135.107 3 -11 5 9 337.263 95.6519 3 11 -5 -9 290.468 75.2651 4 -11 5 8 293.495 91.0977 3 11 -5 -8 394.948 85.5074 4 11 -5 -7 20014.2 498.024 4 -11 5 7 19747.9 596.966 3 -11 5 6 429.912 98.4361 3 -11 5 5 3352.26 232.007 3 -11 5 4 45.6042 68.9022 3 -11 5 3 8924.71 376.510 3 -11 5 2 549.125 104.845 3 -11 5 1 21015.5 590.406 3 -11 5 1 19176.4 465.287 1 -11 5 0 7924.70 304.340 2 -11 5 0 7717.78 341.986 3 -11 5 -1 3732.25 212.253 2 -11 5 -1 3723.08 237.170 3 -11 5 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23.2614 51.1327 2 -11 4 -2 1.12666 48.5684 3 -11 4 -2-6.47893 50.5650 2 -11 4 -3 2004.35 167.704 2 -11 4 -3 1921.79 167.521 3 -11 4 -4 86.1678 60.8492 3 -11 4 -4 78.4798 68.7182 2 -11 4 -5 6499.51 317.580 2 -11 4 -6 112.012 72.0452 2 -11 4 -7-20.8519 80.4704 2 -11 4 -8 79.7976 70.0864 2 -11 4 -9 10369.2 449.891 2 -11 3 17 1333.53 173.130 3 -11 3 16 156.983 84.5594 3 -11 3 15 6281.24 355.132 3 -11 3 14 13289.5 520.487 3 -11 3 13 1466.64 177.142 3 11 -3 -12 14028.0 360.691 4 -11 3 12 13478.9 514.448 3 -11 3 11 24.6922 70.1843 3 11 -3 -11 31.0643 52.1230 4 11 -3 -10 7842.48 270.140 4 -11 3 10 7456.53 365.329 3 -11 3 9 671.508 120.884 3 11 -3 -9 783.629 98.9137 4 -11 3 8 7976.37 370.893 3 -11 3 7 6911.85 338.211 3 -11 3 6 643.515 110.940 3 -11 3 5 149.683 77.4711 3 -11 3 4 683.413 111.162 3 -11 3 3 9381.78 380.781 3 -11 3 2 297.767 58.8726 1 -11 3 2 274.611 85.5292 3 -11 3 1 18349.9 541.099 3 -11 3 0 3.93777 19.4035 1 -11 3 0 1288.13 139.489 3 -11 3 -1 4166.89 242.988 3 -11 3 -2 158.770 68.4606 3 -11 3 -2 134.153 63.0846 2 -11 3 -3 6775.88 313.956 2 -11 3 -3 6341.81 299.032 3 -11 3 -4 1829.30 169.063 2 -11 3 -4 1644.46 153.774 3 -11 3 -5 2009.33 181.754 2 -11 3 -5 1889.48 160.532 3 -11 3 -6 6.74907 63.6662 2 -11 3 -7 192.944 92.6718 2 -11 3 -8-72.1598 92.3691 2 -11 3 -9 39.0649 72.8381 2 -11 2 17 2773.02 244.384 3 -11 2 16 3405.04 266.484 3 -11 2 15 1025.61 152.018 3 -11 2 14 12256.0 501.508 3 -11 2 13 6727.67 362.178 3 -11 2 12 3094.29 246.210 3 11 -2 -11 9380.55 281.293 4 -11 2 11 9211.46 416.848 3 11 -2 -10 3574.64 177.069 4 -11 2 10 3253.97 245.221 3 -11 2 9 35246.4 863.063 3 -11 2 8 1587.17 170.448 3 -11 2 7 6515.52 331.088 3 -11 2 6 110.111 74.5491 3 -11 2 5 1340.49 151.552 3 -11 2 4 1665.10 165.963 3 -11 2 3 3462.99 232.495 3 -11 2 2 8387.91 355.904 3 -11 2 1 2759.76 202.728 3 -11 2 0 15832.6 493.804 3 -11 2 -1 369.290 88.7137 3 -11 2 -2 9185.33 364.509 2 -11 2 -2 8748.84 354.513 3 -11 2 -3 1207.44 141.867 2 -11 2 -3 1130.01 130.395 3 -11 2 -4 7256.33 337.502 2 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85.2266 69.3662 2 -11 1 -7 840.025 137.783 2 -11 1 -8 529.724 119.795 2 -11 0 16 3598.80 286.485 3 -11 0 15 4830.40 326.303 3 -11 0 14 1952.00 208.690 3 -11 0 13 4299.58 302.655 3 -11 0 12 5844.87 348.259 3 -11 0 11 308.092 107.608 3 -11 0 10 4959.65 313.278 3 -11 0 9 12143.9 483.386 3 -11 0 8 2583.15 223.597 3 -11 0 7 55.6448 72.1157 3 -11 0 6 546.577 113.326 3 -11 0 5 6250.79 325.371 3 -11 0 4 4142.97 261.169 3 -11 0 3 2669.80 208.462 3 -11 0 2 8425.04 365.580 3 -11 0 1 1773.46 169.828 3 -11 0 0 4257.15 252.911 3 -11 0 -1 8564.09 359.856 3 -11 0 -2 9998.47 386.972 3 -11 0 -3 4627.69 272.292 2 -11 0 -3 4183.29 245.098 3 -11 0 -4 7688.61 358.897 2 -11 0 -4 7644.24 327.695 3 -11 0 -5 458.974 86.3681 3 -11 0 -5 574.001 118.303 2 -11 0 -6 3946.47 268.230 2 -11 0 -7 7.10962 78.0780 2 -11 -1 15 6758.28 393.126 3 -11 -1 14 4795.98 328.068 3 -11 -1 13 281.162 104.729 3 -11 -1 12 5123.29 329.442 3 -11 -1 11 13998.7 545.930 3 -11 -1 10 4570.56 304.072 3 -11 -1 9 4081.33 283.932 3 -11 -1 8 2161.72 205.517 3 -11 -1 7 357.625 95.8635 3 -11 -1 6 3780.81 261.969 3 -11 -1 5 10.0874 69.8576 3 -11 -1 4 14258.5 505.984 3 -11 -1 3 1773.79 176.529 3 -11 -1 2 9.47577 60.0677 3 -11 -1 1 4711.97 272.758 3 -11 -1 0 3060.01 220.513 3 -11 -1 -1 152.749 78.5335 3 -11 -1 -2 4823.07 269.394 3 -11 -1 -3 1269.24 152.291 2 -11 -1 -3 1067.46 132.846 3 -11 -1 -4 2099.14 195.616 2 -11 -1 -4 1954.09 168.498 3 -11 -1 -5 3.81211 61.4508 2 -11 -1 -6 43.2706 76.6322 2 -11 -1 -7 9373.58 433.527 2 -11 -2 14 196.358 98.4296 3 -11 -2 13 16919.9 632.399 3 -11 -2 12 10267.8 478.847 3 -11 -2 11 1384.26 180.140 3 -11 -2 10 13256.3 535.474 3 -11 -2 9 1194.54 162.535 3 -11 -2 8 7065.13 376.005 3 -11 -2 7 1211.38 161.972 3 -11 -2 6 4481.48 291.149 3 -11 -2 5 18115.8 594.898 3 -11 -2 4 364.336 96.0673 3 -11 -2 3 2841.00 222.530 3 -11 -2 2 5462.47 306.088 3 -11 -2 1 339.213 93.4884 3 -11 -2 0 1573.20 164.847 3 -11 -2 -1 7027.47 338.023 3 -11 -2 -2 289.688 85.5432 3 -11 -2 -3 1207.36 152.043 2 -11 -2 -3 1211.92 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2 -12 10 -8 4545.38 280.874 2 12 -9 -13 2736.58 215.061 4 12 -9 -12 5110.20 285.074 4 12 -9 -11 126.976 72.4207 4 12 -9 -10 2467.61 196.589 4 12 -9 -9 778.859 124.245 4 12 -9 -8 551.376 105.763 4 12 -9 -7 390.458 97.5860 4 12 -9 -6 2233.46 184.574 4 12 -9 -5 6969.53 321.949 4 -12 9 5 7381.39 251.209 2 12 -9 -4 331.710 98.0081 4 -12 9 4 315.799 63.2700 2 -12 9 3 13119.3 367.617 2 12 -9 -3 13438.9 457.301 4 -12 9 2 4153.46 203.963 2 12 -9 -2 4461.96 265.083 4 -12 9 1 15575.0 427.609 2 12 -9 -1 17264.6 531.158 4 -12 9 0 6346.31 266.270 2 -12 9 -1 18734.2 496.643 2 -12 9 -2 17995.3 499.105 2 -12 9 -3 154.910 65.6791 2 -12 9 -4 1994.52 169.863 2 -12 9 -5 2430.04 192.858 2 -12 9 -6 5398.10 294.503 2 -12 9 -7 969.944 139.682 2 -12 9 -8 2350.88 207.318 2 -12 9 -9 7290.69 373.676 2 12 -8 -13 11070.7 410.014 4 -12 8 13 11022.6 497.148 3 12 -8 -12 35.7310 61.2475 4 -12 8 12 47.1066 78.1669 3 12 -8 -11 13513.4 453.582 4 -12 8 11 14321.7 560.112 3 12 -8 -10 5869.38 287.513 4 -12 8 10 5817.52 349.021 3 -12 8 9 631.795 131.012 3 12 -8 -9 425.092 94.3274 4 12 -8 -8 1758.20 160.389 4 -12 8 8 2039.71 205.945 3 -12 8 7 829.845 145.111 3 12 -8 -7 853.204 120.335 4 -12 8 6 449.730 110.153 3 12 -8 -6 543.664 107.339 4 12 -8 -5 5844.43 286.211 4 -12 8 5 6001.37 339.559 3 12 -8 -4 277.453 101.092 4 -12 8 4 255.850 86.6005 3 12 -8 -3 254.822 106.900 4 -12 8 3 24.7096 50.6950 2 -12 8 2 5412.84 240.316 2 -12 8 1 425.561 77.7456 2 -12 8 0 19597.5 510.206 2 -12 8 -1 1171.48 125.843 2 -12 8 -2 7838.24 322.272 2 -12 8 -3 13861.8 449.172 2 -12 8 -4 821.909 119.466 2 -12 8 -5 3248.18 222.401 2 -12 8 -6 1042.17 140.718 2 -12 8 -7 3781.37 255.620 2 -12 8 -8 1458.63 169.137 2 -12 7 15 1263.27 175.879 3 -12 7 14 1796.76 205.916 3 12 -7 -13 1632.20 150.917 4 -12 7 13 1611.28 196.155 3 12 -7 -12 10046.3 371.247 4 -12 7 12 10014.6 461.731 3 -12 7 11 26.6860 72.8427 3 12 -7 -11 43.9660 54.5572 4 12 -7 -10 8015.97 325.405 4 -12 7 10 8564.39 417.951 3 12 -7 -9 7338.61 309.717 4 -12 7 9 8016.12 398.432 3 12 -7 -8 4445.09 239.619 4 -12 7 8 4570.62 298.704 3 12 -7 -7 1631.20 153.921 4 -12 7 7 1329.16 170.438 3 12 -7 -6 11282.7 389.525 4 -12 7 6 10845.4 457.071 3 12 -7 -5 5069.23 263.920 4 -12 7 5 5032.56 308.457 3 -12 7 4 48.4845 67.1742 3 -12 7 3 1360.17 164.543 3 -12 7 2 334.127 102.188 3 -12 7 2 243.596 67.3153 2 -12 7 1 7340.22 294.075 2 -12 7 1 6925.28 353.925 3 -12 7 0-3.61450 53.5594 2 -12 7 0 56.1524 72.9390 3 -12 7 -1 8597.87 335.120 2 -12 7 -2 14618.0 458.808 2 -12 7 -3 1498.11 151.775 2 -12 7 -4 2766.45 204.779 2 -12 7 -5 3846.75 246.711 2 -12 7 -6 1984.90 184.045 2 -12 7 -7 798.511 130.313 2 -12 7 -8 546.639 117.759 2 -12 6 16 411.966 115.156 3 -12 6 15 476.703 115.759 3 -12 6 14 6594.23 377.517 3 -12 6 13 782.876 139.555 3 12 -6 -12 8261.10 321.131 4 -12 6 12 8217.34 413.043 3 12 -6 -11 3276.30 201.553 4 -12 6 11 3774.82 277.313 3 -12 6 10 293.494 94.6636 3 12 -6 -10 188.962 68.8929 4 12 -6 -9 2635.78 181.277 4 -12 6 9 2853.69 238.341 3 -12 6 8 134.892 86.8524 3 12 -6 -8 115.487 69.6225 4 12 -6 -7 26480.8 624.394 4 -12 6 7 27659.5 759.906 3 -12 6 6 542.359 116.217 3 12 -6 -6 563.804 106.196 4 -12 6 5 6665.33 348.399 3 -12 6 4 175.515 80.3496 3 -12 6 3 9359.99 407.961 3 -12 6 2 5844.51 319.622 3 -12 6 1 9028.53 334.730 2 -12 6 1 8939.29 397.193 3 -12 6 0 15045.3 450.346 2 -12 6 0 14091.6 505.698 3 -12 6 -1 452.866 100.897 3 -12 6 -1 571.759 96.5163 2 -12 6 -2 5796.63 283.101 2 -12 6 -2 5386.17 301.522 3 -12 6 -3 8174.46 349.265 2 -12 6 -4 12415.3 446.268 2 -12 6 -5 7872.27 359.308 2 -12 6 -6 2466.54 207.614 2 -12 6 -7 2336.86 208.197 2 -12 6 -8 56.1316 74.0400 2 -12 5 16 357.208 105.678 3 -12 5 15 3240.09 267.665 3 -12 5 14 75.5642 76.8383 3 -12 5 13 9749.79 454.498 3 -12 5 12 3.50006 68.0666 3 12 -5 -12 24.2936 49.1715 4 12 -5 -11 1939.85 152.070 4 -12 5 11 2444.78 223.875 3 -12 5 10 91.6567 73.8822 3 12 -5 -10 37.3681 56.9384 4 -12 5 9 221.777 89.7152 3 12 -5 -9 267.022 79.8422 4 12 -5 -8 10357.0 352.987 4 -12 5 8 10311.8 444.578 3 -12 5 7 49.9006 72.3227 3 12 -5 -7 202.581 80.6425 4 -12 5 6 4184.56 275.618 3 -12 5 5 805.350 129.568 3 -12 5 4 2746.80 220.721 3 -12 5 3 331.035 101.102 3 -12 5 2 49907.8 1053.42 3 -12 5 1 2692.88 218.154 3 -12 5 0 18625.7 522.361 2 -12 5 0 18867.3 579.553 3 -12 5 -1 4911.76 258.792 2 -12 5 -1 4666.75 277.699 3 -12 5 -2 702.494 120.727 3 -12 5 -2 614.627 106.815 2 -12 5 -3 17136.4 525.733 2 -12 5 -3 16989.0 540.969 3 -12 5 -4 4.11579 67.4449 2 -12 5 -5 24239.6 672.407 2 -12 5 -6 3055.98 234.843 2 -12 5 -7 1528.14 173.971 2 -12 5 -8 3386.16 258.479 2 -12 4 16 363.658 102.051 3 -12 4 15 1753.66 204.341 3 -12 4 14 10047.5 467.212 3 -12 4 13 33.5869 72.8056 3 -12 4 12 5872.18 346.697 3 -12 4 11 14.9265 78.6827 3 12 -4 -11-20.9056 59.6160 4 12 -4 -10 3698.84 200.169 4 -12 4 10 3540.28 264.694 3 -12 4 9-18.4675 66.1903 3 12 -4 -9 58.0741 63.0332 4 12 -4 -8 4560.00 228.103 4 -12 4 8 4516.45 291.715 3 -12 4 7 4070.62 272.981 3 -12 4 6 60.2845 68.1857 3 -12 4 5 189.111 77.7197 3 -12 4 4 228.499 85.0191 3 -12 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-14 9 3 2541.30 178.482 2 14 -9 -3 2596.62 222.935 4 -14 9 2 1467.18 140.207 2 14 -9 -2 1344.41 174.459 4 -14 9 1 1530.29 149.418 2 -14 9 0 7712.55 330.204 2 -14 9 -1 555.686 100.756 2 -14 9 -2 7184.55 333.636 2 -14 9 -3 1466.36 157.402 2 -14 9 -4 2607.56 213.111 2 -14 9 -5 2372.01 207.953 2 14 -8 -11 110.182 73.4524 4 14 -8 -10 14041.3 477.927 4 -14 8 9 6.65321 74.2320 3 14 -8 -9 19.1039 78.2635 4 14 -8 -8 13219.4 461.767 4 -14 8 8 13380.3 568.287 3 -14 8 7 122.528 87.9310 3 14 -8 -7 232.887 101.708 4 14 -8 -6 10456.1 409.483 4 -14 8 6 10356.8 489.949 3 14 -8 -5 7022.65 338.826 4 -14 8 5 6508.89 383.735 3 -14 8 4 122.616 86.7244 3 14 -8 -4 205.988 108.791 4 -14 8 4 25.1982 53.9762 2 -14 8 3 5792.88 277.186 2 -14 8 3 5708.93 355.908 3 -14 8 2 149.931 68.4891 2 -14 8 1 491.346 95.8723 2 -14 8 0-50.1780 63.0239 2 -14 8 -1 3921.73 245.628 2 -14 8 -2 115.134 73.1507 2 -14 8 -3 5512.21 303.652 2 -14 8 -4 46.5974 64.9072 2 -14 8 -5 3700.94 261.347 2 14 -7 -11 5625.62 288.399 4 -14 7 10 384.423 121.019 3 14 -7 -10 345.886 97.5022 4 14 -7 -9 19671.4 563.226 4 -14 7 9 20993.7 720.187 3 14 -7 -8 2377.59 195.447 4 -14 7 8 2297.73 240.453 3 14 -7 -7 21111.9 588.645 4 -14 7 7 21178.6 716.561 3 -14 7 6 1272.20 177.631 3 14 -7 -6 1524.35 167.328 4 -14 7 5 12849.7 537.664 3 -14 7 4 12401.8 524.872 3 -14 7 3 3134.93 262.010 3 -14 7 3 3195.15 210.052 2 -14 7 2 3746.27 231.477 2 -14 7 2 3626.19 281.517 3 -14 7 1 1535.17 153.706 2 -14 7 1 1507.30 186.699 3 -14 7 0 6395.75 314.462 2 -14 7 0 6104.56 357.889 3 -14 7 -1 2891.83 216.793 2 -14 7 -2 7535.93 355.007 2 -14 7 -3 49.7472 64.6842 2 -14 7 -4 8292.54 387.782 2 -14 7 -5 102.910 70.9346 2 14 -6 -11 2409.39 185.615 4 -14 6 11 2295.24 238.373 3 -14 6 10 185.268 114.483 3 14 -6 -10 19.6050 70.4944 4 14 -6 -9 18064.8 527.228 4 -14 6 9 19096.0 677.877 3 14 -6 -8 4150.30 243.876 4 -14 6 8 4345.12 318.860 3 14 -6 -7 17602.8 529.463 4 -14 6 7 18590.4 657.588 3 -14 6 6 42941.2 1057.21 3 -14 6 5 1516.87 193.584 3 -14 6 4 20551.4 683.496 3 -14 6 3 33.2032 83.1065 3 -14 6 2 14780.9 568.725 3 -14 6 2 15109.9 487.024 2 -14 6 1 3902.92 245.411 2 -14 6 1 3991.09 290.903 3 -14 6 0 938.678 149.374 3 -14 6 0 948.582 133.586 2 -14 6 -1 9314.60 396.122 2 -14 6 -1 9170.97 432.107 3 -14 6 -2 187.143 85.0822 2 -14 6 -2 105.494 79.7241 3 -14 6 -3 4938.99 297.964 2 -14 6 -4 1582.29 180.227 2 -14 5 11 2306.34 241.070 3 -14 5 10 1355.96 189.680 3 14 -5 -10 1338.69 142.755 4 14 -5 -9 5036.11 263.515 4 -14 5 9 5410.29 354.177 3 14 -5 -8 20356.6 561.420 4 -14 5 8 21723.0 716.159 3 -14 5 7 988.222 163.768 3 -14 5 6 3741.49 285.748 3 -14 5 5 4097.86 297.581 3 -14 5 4 8947.20 437.724 3 -14 5 3 22641.3 713.929 3 -14 5 2 4445.30 304.559 3 -14 5 1 15491.8 509.327 2 -14 5 1 14387.4 553.908 3 -14 5 0 1229.32 165.874 3 -14 5 0 1253.97 152.623 2 -14 5 -1 2399.02 208.251 2 -14 5 -1 2266.60 219.310 3 -14 5 -2 580.902 123.074 3 -14 5 -2 669.649 124.616 2 -14 5 -3 10737.4 446.867 2 -14 5 -3 10235.0 449.284 3 -14 5 -4 6005.21 340.748 2 -14 4 11 1672.43 209.083 3 14 -4 -10 6117.39 277.951 4 -14 4 10 5823.55 369.297 3 14 -4 -9 5978.03 283.778 4 -14 4 9 6300.55 377.356 3 -14 4 8 1789.95 209.850 3 -14 4 7 4338.00 310.120 3 -14 4 6 348.987 121.195 3 -14 4 5 1620.77 191.383 3 -14 4 4 2196.78 220.995 3 -14 4 3 9363.12 441.381 3 -14 4 2 6286.52 358.478 3 -14 4 1 412.337 108.668 3 -14 4 0 2100.69 194.432 2 -14 4 0 2115.38 211.531 3 -14 4 -1 2143.26 201.898 2 -14 4 -1 2144.79 209.263 3 -14 4 -2 7089.72 360.938 2 -14 4 -2 6455.05 354.586 3 -14 4 -3 689.324 128.919 3 -14 4 -3 575.288 117.796 2 -14 4 -4 5725.63 325.431 3 -14 3 10 4231.39 318.636 3 -14 3 9 9212.68 467.973 3 -14 3 8 10636.6 492.691 3 -14 3 7 400.511 106.765 3 -14 3 6 3259.18 270.111 3 -14 3 5-45.8160 84.6671 3 -14 3 4 13109.2 532.666 3 -14 3 3 11266.8 487.791 3 -14 3 2 134.936 90.6013 3 -14 3 1 5245.91 325.407 3 -14 3 0 0.26241 75.2596 3 -14 3 0 40.2057 73.2663 2 -14 3 -1 2059.91 195.677 2 -14 3 -1 1952.67 199.279 3 -14 3 -2 3197.35 247.769 2 -14 3 -2 3096.27 247.079 3 -14 3 -3 3695.66 263.538 3 -14 2 10 19643.4 702.792 3 -14 2 9 6640.32 393.910 3 -14 2 8 7242.48 408.057 3 -14 2 7 5287.47 344.774 3 -14 2 6 8930.07 445.020 3 -14 2 5 20841.8 695.143 3 -14 2 4 1430.47 187.656 3 -14 2 3 17887.9 629.936 3 -14 2 2 5570.89 339.555 3 -14 2 1 956.761 151.411 3 -14 2 0 8190.94 404.679 3 -14 2 -1 2330.07 214.238 2 -14 2 -1 1867.54 197.712 3 -14 2 -2 3629.64 264.095 3 -14 2 -3 752.161 128.772 3 -14 1 8 208.068 95.8139 3 -14 1 7 13762.9 565.215 3 -14 1 6 4362.52 315.584 3 -14 1 5 36720.4 963.986 3 -14 1 4 16411.7 609.604 3 -14 1 3 802.851 151.755 3 -14 1 2 5779.82 348.133 3 -14 1 1-5.71816 69.7358 3 -14 1 0 10190.9 458.338 3 -14 1 -1 4511.53 299.914 3 -14 1 -2 3302.07 253.068 3 -14 0 7 4432.37 324.120 3 -14 0 6 15708.2 611.281 3 -14 0 5 170.978 106.386 3 -14 0 4 17844.4 642.081 3 -14 0 3 1076.83 167.371 3 -14 0 2 7566.33 401.989 3 -14 0 1 6413.58 367.042 3 -14 0 0 1500.41 185.534 3 -14 0 -1 10158.2 455.573 3 -14 0 -2 28.8305 69.5520 3 -14 -1 5 7969.75 432.131 3 -14 -1 4 27.7739 88.4100 3 -14 -1 3 1091.23 174.087 3 -14 -1 2 155.105 90.2599 3 -14 -1 1 10530.9 479.370 3 -14 -1 0 6573.54 372.694 3 -14 -1 -1 2811.64 242.527 3 -14 -2 1 4937.09 333.764 3 -14 -2 0 3679.46 284.290 3 15 -9 -10 2429.83 209.297 4 15 -9 -9 235.242 91.3628 4 15 -9 -8 2031.35 191.875 4 15 -9 -7 221.697 98.5156 4 15 -9 -6 1022.14 146.772 4 15 -9 -5 3809.88 263.319 4 15 -9 -4 1509.59 177.653 4 15 -9 -3 6885.51 366.822 4 -15 9 2 928.531 119.688 2 -15 9 1 1018.91 128.321 2 -15 9 0 657.102 111.761 2 -15 9 -1 6061.74 314.804 2 -15 9 -2 1717.83 174.919 2 -15 9 -3 2266.15 200.294 2 15 -8 -10 3529.90 241.917 4 15 -8 -9 1879.16 180.455 4 15 -8 -8 259.642 100.754 4 15 -8 -7 3973.06 257.698 4 15 -8 -6 542.143 124.469 4 15 -8 -5 1131.68 162.363 4 -15 8 4 5183.57 272.222 2 15 -8 -4 5319.07 314.053 4 -15 8 4 5138.87 353.426 3 -15 8 3 1241.31 140.533 2 -15 8 3 1265.07 182.655 3 -15 8 2 24.7344 54.7629 2 -15 8 1 68.7679 61.1416 2 -15 8 0 691.178 118.391 2 -15 8 -1 5523.40 305.672 2 -15 8 -2 706.610 122.359 2 -15 8 -3 23.7578 65.0694 2 15 -7 -10 4970.84 277.024 4 15 -7 -9 364.571 103.758 4 15 -7 -8 6766.67 326.730 4 15 -7 -7 48.9720 80.2459 4 15 -7 -6 9573.07 399.202 4 -15 7 6 8694.09 463.350 3 -15 7 5 11355.5 523.861 3 -15 7 4 1377.94 189.806 3 -15 7 3 341.368 113.467 3 -15 7 3 346.008 98.5052 2 -15 7 2 239.805 102.332 3 -15 7 2 368.985 90.7631 2 -15 7 1 2722.39 211.454 2 -15 7 1 2497.74 241.962 3 -15 7 0 3506.91 244.983 2 -15 7 0 3519.55 283.362 3 -15 7 -1 2527.49 211.988 2 -15 7 -2 3819.93 266.276 2 15 -6 -10 1567.31 161.497 4 15 -6 -9 3349.14 226.305 4 15 -6 -8 4261.21 257.686 4 15 -6 -7 12226.0 446.005 4 -15 6 6 1053.62 177.421 3 -15 6 5 13427.0 568.000 3 -15 6 4 2218.19 234.714 3 -15 6 3 12243.5 536.027 3 -15 6 2 2757.08 215.488 2 -15 6 2 2737.12 255.856 3 -15 6 1 1104.20 173.174 3 -15 6 1 1084.43 143.024 2 -15 6 0 5752.89 319.205 2 -15 6 0 5649.14 356.881 3 -15 6 -1 2123.09 199.478 2 -15 6 -1 1965.96 212.718 3 -15 6 -2 1439.23 172.256 2 15 -5 -9 4120.07 247.815 4 15 -5 -8 181.229 95.0872 4 -15 5 6 3950.42 308.162 3 -15 5 5 464.824 121.920 3 -15 5 4 12927.7 552.930 3 -15 5 3 1396.85 188.384 3 -15 5 2 19002.4 671.928 3 -15 5 1 5437.05 311.027 2 -15 5 1 5323.16 347.959 3 -15 5 0 952.888 157.601 3 -15 5 0 1010.91 145.747 2 -15 5 -1 3532.23 259.406 2 -15 5 -1 3035.63 260.030 3 -15 5 -2 609.275 124.966 3 -15 5 -3 555.595 120.378 3 -15 4 6 516.751 137.274 3 -15 4 5 199.509 92.9028 3 -15 4 4 7135.58 403.960 3 -15 4 3 4204.40 308.553 3 -15 4 2 581.866 135.842 3 -15 4 1 8561.17 397.547 2 -15 4 1 8565.65 438.961 3 -15 4 0 423.457 116.994 3 -15 4 0 483.488 104.081 2 -15 4 -1 2336.84 228.596 3 -15 4 -2 398.327 110.215 3 -15 3 5 1180.57 181.168 3 -15 3 4 217.311 102.386 3 -15 3 3 3149.48 268.135 3 -15 3 2 5779.50 360.492 3 -15 3 1 1831.62 207.522 3 -15 3 0 3108.43 263.811 3 -15 3 -1 374.019 106.648 3 -15 3 -2 5301.75 335.111 3 -15 2 4 8851.23 454.538 3 -15 2 3 2701.09 255.810 3 -15 2 2 32.5540 72.2459 3 -15 2 1 4181.02 306.894 3 -15 2 0 1132.86 167.275 3 -15 2 -1 6332.22 369.420 3 -15 1 2 277.401 100.146 3 -15 1 1 2061.87 222.709 3 -15 1 0 551.097 129.623 3 -16 8 4 396.950 93.4919 2 -16 8 3 380.466 87.2902 2 -16 8 2 693.553 121.215 2 -16 8 1 1164.65 147.180 2 16 -7 -8-5.99622 77.4479 4 16 -7 -7 1986.14 192.372 4 -16 7 4 1009.10 134.734 2 -16 7 3 3890.57 257.968 2 -16 7 2 2526.30 213.478 2 -16 7 1 6.09787 63.2600 2 16 -6 -8 1952.07 185.436 4 16 -6 -7 68.8453 84.0528 4 -16 6 3 699.713 124.100 2 16 -5 -8 409.432 108.314 4 0 0 0 0.00 0.00 0 TITL exp_2637 in P-1 REM P-1 (#2 in standard setting) CELL 0.71073 11.638358 11.942616 14.494464 92.7814 102.0777 111.6367 ZERR 4.00 0.000384 0.000422 0.000308 0.0022 0.0023 0.0032 LATT 1 SFAC C H O S In UNIT 92.00 92.00 8.00 8.00 4.00 TREF HKLF 4 END ; _shelx_hkl_checksum 33062 _database_code_depnum_ccdc_archive 'CCDC 924188' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mn2089 #TrackingRef 'CIF (4)' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common In(BzMedtc)3 _chemical_melting_point ? _chemical_formula_moiety 'C27 H30 In N3 S6' _chemical_formula_sum 'C27 H30 In N3 S6' _chemical_formula_weight 703.72 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' In In -0.7276 1.3100 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7966(4) _cell_length_b 12.2791(8) _cell_length_c 12.7790(8) _cell_angle_alpha 96.142(4) _cell_angle_beta 92.353(4) _cell_angle_gamma 100.383(5) _cell_volume 1500.51(15) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7527 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 28.35 _exptl_crystal_description parallelepiped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 716 _exptl_absorpt_coefficient_mu 1.228 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.837 _exptl_absorpt_correction_T_max 0.930 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 13669 _diffrn_reflns_av_R_equivalents 0.0177 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 27.00 _reflns_number_total 6504 _reflns_number_gt 5800 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0185P)^2^+0.9288P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6504 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0283 _refine_ls_R_factor_gt 0.0228 _refine_ls_wR_factor_ref 0.0514 _refine_ls_wR_factor_gt 0.0493 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.001 _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 In1 In 0.371632(14) 0.868293(11) 0.659066(11) 0.01541(4) Uani 1 1 d . . . S1 S 0.32968(5) 0.99126(4) 0.51370(4) 0.01735(10) Uani 1 1 d . . . S2 S 0.18691(5) 0.98845(4) 0.71309(4) 0.01881(10) Uani 1 1 d . . . S3 S 0.19028(5) 0.68868(4) 0.58900(4) 0.01805(10) Uani 1 1 d . . . S4 S 0.48276(5) 0.73899(4) 0.52954(4) 0.02050(11) Uani 1 1 d . . . S5 S 0.39242(5) 0.80886(4) 0.84674(4) 0.02155(11) Uani 1 1 d . . . S6 S 0.60566(5) 0.96915(4) 0.75523(4) 0.01995(11) Uani 1 1 d . . . N1 N 0.12684(17) 1.10391(14) 0.55746(13) 0.0173(3) Uani 1 1 d . . . N2 N 0.30466(17) 0.55119(14) 0.45955(13) 0.0183(3) Uani 1 1 d . . . N3 N 0.62783(17) 0.90990(15) 0.95094(13) 0.0195(4) Uani 1 1 d . . . C1 C -0.0117(2) 1.33658(18) 0.69822(16) 0.0207(4) Uani 1 1 d . . . H1 H -0.1075 1.3125 0.6772 0.025 Uiso 1 1 calc R . . C2 C 0.0341(2) 1.44277(18) 0.74994(16) 0.0241(5) Uani 1 1 d . . . H2 H -0.0305 1.4906 0.7651 0.029 Uiso 1 1 calc R . . C3 C 0.1733(2) 1.47935(18) 0.77954(16) 0.0245(5) Uani 1 1 d . . . H3 H 0.2050 1.5529 0.8134 0.029 Uiso 1 1 calc R . . C4 C 0.2668(2) 1.40835(19) 0.75967(18) 0.0271(5) Uani 1 1 d . . . H4 H 0.3624 1.4328 0.7812 0.033 Uiso 1 1 calc R . . C5 C 0.2208(2) 1.30144(18) 0.70827(18) 0.0248(5) Uani 1 1 d . . . H5 H 0.2853 1.2532 0.6947 0.030 Uiso 1 1 calc R . . C6 C 0.0813(2) 1.26486(17) 0.67675(16) 0.0177(4) Uani 1 1 d . . . C7 C 0.0261(2) 1.14895(17) 0.62326(17) 0.0211(4) Uani 1 1 d . . . H7A H -0.0007 1.0988 0.6777 0.025 Uiso 1 1 calc R . . H7B H -0.0586 1.1501 0.5787 0.025 Uiso 1 1 calc R . . C8 C 0.1449(2) 1.14857(17) 0.45585(16) 0.0217(4) Uani 1 1 d . . . H8A H 0.2143 1.2177 0.4654 0.033 Uiso 1 1 calc R . . H8B H 0.0560 1.1640 0.4289 0.033 Uiso 1 1 calc R . . H8C H 0.1764 1.0939 0.4054 0.033 Uiso 1 1 calc R . . C9 C 0.20615(19) 1.03569(16) 0.59104(15) 0.0153(4) Uani 1 1 d . . . C10 C 0.3482(2) 0.4362(2) 0.20077(19) 0.0325(5) Uani 1 1 d . . . H10 H 0.3552 0.3653 0.2215 0.039 Uiso 1 1 calc R . . C11 C 0.3162(3) 0.4463(3) 0.0956(2) 0.0478(7) Uani 1 1 d . . . H11 H 0.3011 0.3824 0.0446 0.057 Uiso 1 1 calc R . . C12 C 0.3065(3) 0.5489(3) 0.0656(2) 0.0502(8) Uani 1 1 d . . . H12 H 0.2856 0.5559 -0.0064 0.060 Uiso 1 1 calc R . . C13 C 0.3267(2) 0.6418(2) 0.1391(2) 0.0384(6) Uani 1 1 d . . . H13 H 0.3183 0.7122 0.1179 0.046 Uiso 1 1 calc R . . C14 C 0.3594(2) 0.6326(2) 0.24410(18) 0.0258(5) Uani 1 1 d . . . H14 H 0.3746 0.6968 0.2947 0.031 Uiso 1 1 calc R . . C15 C 0.3699(2) 0.52892(18) 0.27513(16) 0.0203(4) Uani 1 1 d . . . C16 C 0.4086(2) 0.51860(17) 0.38877(16) 0.0204(4) Uani 1 1 d . . . H16A H 0.4170 0.4405 0.3957 0.024 Uiso 1 1 calc R . . H16B H 0.5001 0.5666 0.4100 0.024 Uiso 1 1 calc R . . C17 C 0.1725(2) 0.47193(17) 0.45633(17) 0.0230(4) Uani 1 1 d . . . H17A H 0.1594 0.4461 0.5258 0.035 Uiso 1 1 calc R . . H17B H 0.1742 0.4081 0.4037 0.035 Uiso 1 1 calc R . . H17C H 0.0957 0.5088 0.4374 0.035 Uiso 1 1 calc R . . C18 C 0.3240(2) 0.64894(16) 0.51978(15) 0.0172(4) Uani 1 1 d . . . C19 C 0.9145(2) 0.83967(18) 1.04416(16) 0.0226(4) Uani 1 1 d . . . H19 H 0.8880 0.8658 1.1116 0.027 Uiso 1 1 calc R . . C20 C 0.9969(2) 0.75874(19) 1.03537(18) 0.0271(5) Uani 1 1 d . . . H20 H 1.0258 0.7292 1.0965 0.033 Uiso 1 1 calc R . . C21 C 1.0369(2) 0.72104(19) 0.93758(19) 0.0287(5) Uani 1 1 d . . . H21 H 1.0932 0.6655 0.9314 0.034 Uiso 1 1 calc R . . C22 C 0.9949(2) 0.7643(2) 0.84885(18) 0.0287(5) Uani 1 1 d . . . H22 H 1.0231 0.7390 0.7817 0.034 Uiso 1 1 calc R . . C23 C 0.9114(2) 0.84470(19) 0.85728(17) 0.0235(5) Uani 1 1 d . . . H23 H 0.8822 0.8736 0.7958 0.028 Uiso 1 1 calc R . . C24 C 0.8703(2) 0.88306(17) 0.95509(16) 0.0192(4) Uani 1 1 d . . . C25 C 0.7749(2) 0.96760(18) 0.96356(17) 0.0208(4) Uani 1 1 d . . . H25A H 0.7926 1.0132 1.0331 0.025 Uiso 1 1 calc R . . H25B H 0.7939 1.0180 0.9083 0.025 Uiso 1 1 calc R . . C26 C 0.5753(2) 0.8521(2) 1.04002(16) 0.0255(5) Uani 1 1 d . . . H26A H 0.4817 0.8659 1.0531 0.038 Uiso 1 1 calc R . . H26B H 0.6373 0.8800 1.1031 0.038 Uiso 1 1 calc R . . H26C H 0.5719 0.7719 1.0234 0.038 Uiso 1 1 calc R . . C27 C 0.5516(2) 0.89779(17) 0.86044(16) 0.0183(4) Uani 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 In1 0.01622(7) 0.01382(7) 0.01592(7) 0.00062(5) -0.00190(5) 0.00338(5) S1 0.0179(2) 0.0176(2) 0.0175(2) 0.00352(19) 0.00222(19) 0.00478(19) S2 0.0212(2) 0.0195(3) 0.0166(2) 0.0010(2) 0.00229(19) 0.0065(2) S3 0.0170(2) 0.0171(2) 0.0190(2) 0.00050(19) 0.00192(19) 0.00106(19) S4 0.0158(2) 0.0162(2) 0.0284(3) -0.0019(2) 0.0016(2) 0.00229(19) S5 0.0193(2) 0.0237(3) 0.0208(2) 0.0062(2) -0.0024(2) 0.0004(2) S6 0.0182(2) 0.0218(3) 0.0184(2) 0.0032(2) -0.00128(19) -0.0001(2) N1 0.0160(8) 0.0152(8) 0.0203(8) -0.0006(7) -0.0010(7) 0.0038(7) N2 0.0208(9) 0.0156(9) 0.0180(8) 0.0014(7) 0.0006(7) 0.0027(7) N3 0.0184(8) 0.0223(9) 0.0171(8) -0.0001(7) -0.0011(7) 0.0035(7) C1 0.0207(10) 0.0242(11) 0.0192(10) 0.0037(9) 0.0014(8) 0.0090(9) C2 0.0335(12) 0.0230(11) 0.0192(10) 0.0015(9) 0.0037(9) 0.0140(10) C3 0.0356(12) 0.0181(11) 0.0183(10) -0.0028(8) 0.0039(9) 0.0034(9) C4 0.0210(11) 0.0267(12) 0.0304(12) -0.0034(10) 0.0017(9) -0.0004(9) C5 0.0195(10) 0.0236(11) 0.0313(12) -0.0029(9) 0.0030(9) 0.0071(9) C6 0.0198(10) 0.0164(10) 0.0179(10) 0.0032(8) 0.0029(8) 0.0053(8) C7 0.0141(9) 0.0178(10) 0.0308(11) -0.0007(9) -0.0008(8) 0.0045(8) C8 0.0224(10) 0.0184(11) 0.0248(11) 0.0045(9) -0.0032(8) 0.0046(8) C9 0.0149(9) 0.0113(9) 0.0175(9) -0.0021(7) -0.0025(7) -0.0002(7) C10 0.0289(12) 0.0349(14) 0.0317(13) -0.0051(11) -0.0011(10) 0.0070(10) C11 0.0438(16) 0.067(2) 0.0286(13) -0.0163(14) -0.0053(12) 0.0148(15) C12 0.0443(16) 0.090(3) 0.0199(12) 0.0038(14) -0.0016(11) 0.0246(16) C13 0.0276(13) 0.0564(18) 0.0375(14) 0.0237(13) 0.0071(11) 0.0129(12) C14 0.0200(10) 0.0303(12) 0.0282(11) 0.0066(10) 0.0036(9) 0.0052(9) C15 0.0145(9) 0.0251(11) 0.0212(10) 0.0009(9) 0.0018(8) 0.0041(8) C16 0.0218(10) 0.0169(10) 0.0231(10) -0.0016(8) -0.0015(8) 0.0081(8) C17 0.0268(11) 0.0167(10) 0.0229(11) -0.0002(9) 0.0013(9) -0.0017(9) C18 0.0182(10) 0.0161(10) 0.0174(9) 0.0041(8) -0.0021(8) 0.0033(8) C19 0.0257(11) 0.0261(12) 0.0164(10) 0.0002(9) 0.0018(8) 0.0069(9) C20 0.0300(12) 0.0286(12) 0.0251(11) 0.0069(10) 0.0016(9) 0.0096(10) C21 0.0262(12) 0.0262(12) 0.0364(13) 0.0030(10) 0.0083(10) 0.0107(10) C22 0.0283(12) 0.0352(13) 0.0222(11) -0.0038(10) 0.0085(9) 0.0074(10) C23 0.0219(11) 0.0295(12) 0.0185(10) 0.0041(9) 0.0026(8) 0.0018(9) C24 0.0162(10) 0.0199(10) 0.0200(10) 0.0009(8) 0.0009(8) 0.0001(8) C25 0.0188(10) 0.0202(11) 0.0212(10) -0.0010(8) -0.0036(8) 0.0007(8) C26 0.0243(11) 0.0356(13) 0.0168(10) 0.0040(9) 0.0000(8) 0.0052(10) C27 0.0168(10) 0.0186(10) 0.0197(10) -0.0004(8) 0.0013(8) 0.0056(8) _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 In1 S4 2.5796(6) . ? In1 S1 2.5808(5) . ? In1 S5 2.5911(5) . ? In1 S6 2.5922(5) . ? In1 S2 2.6030(5) . ? In1 S3 2.6185(5) . ? S1 C9 1.720(2) . ? S2 C9 1.727(2) . ? S3 C18 1.723(2) . ? S4 C18 1.730(2) . ? S5 C27 1.725(2) . ? S6 C27 1.732(2) . ? N1 C9 1.332(2) . ? N1 C7 1.467(3) . ? N1 C8 1.468(3) . ? N2 C18 1.333(3) . ? N2 C16 1.469(3) . ? N2 C17 1.469(3) . ? N3 C27 1.330(3) . ? N3 C26 1.467(3) . ? N3 C25 1.480(3) . ? C1 C2 1.385(3) . ? C1 C6 1.393(3) . ? C1 H1 0.9500 . ? C2 C3 1.380(3) . ? C2 H2 0.9500 . ? C3 C4 1.386(3) . ? C3 H3 0.9500 . ? C4 C5 1.391(3) . ? C4 H4 0.9500 . ? C5 C6 1.388(3) . ? C5 H5 0.9500 . ? C6 C7 1.507(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C10 C15 1.381(3) . ? C10 C11 1.391(4) . ? C10 H10 0.9500 . ? C11 C12 1.374(4) . ? C11 H11 0.9500 . ? C12 C13 1.377(4) . ? C12 H12 0.9500 . ? C13 C14 1.387(3) . ? C13 H13 0.9500 . ? C14 C15 1.393(3) . ? C14 H14 0.9500 . ? C15 C16 1.510(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C19 C20 1.387(3) . ? C19 C24 1.393(3) . ? C19 H19 0.9500 . ? C20 C21 1.383(3) . ? C20 H20 0.9500 . ? C21 C22 1.381(3) . ? C21 H21 0.9500 . ? C22 C23 1.389(3) . ? C22 H22 0.9500 . ? C23 C24 1.389(3) . ? C23 H23 0.9500 . ? C24 C25 1.516(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? 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 S4 In1 S1 91.525(17) . . ? S4 In1 S5 109.244(18) . . ? S1 In1 S5 158.610(18) . . ? S4 In1 S6 94.823(18) . . ? S1 In1 S6 104.226(17) . . ? S5 In1 S6 69.897(17) . . ? S4 In1 S2 154.058(17) . . ? S1 In1 S2 69.558(16) . . ? S5 In1 S2 91.988(17) . . ? S6 In1 S2 106.693(18) . . ? S4 In1 S3 69.637(17) . . ? S1 In1 S3 99.032(17) . . ? S5 In1 S3 93.160(17) . . ? S6 In1 S3 152.382(17) . . ? S2 In1 S3 95.186(17) . . ? C9 S1 In1 86.49(7) . . ? C9 S2 In1 85.65(7) . . ? C18 S3 In1 85.34(7) . . ? C18 S4 In1 86.45(7) . . ? C27 S5 In1 85.95(7) . . ? C27 S6 In1 85.78(7) . . ? C9 N1 C7 122.69(17) . . ? C9 N1 C8 121.89(17) . . ? C7 N1 C8 115.12(16) . . ? C18 N2 C16 122.97(17) . . ? C18 N2 C17 120.88(17) . . ? C16 N2 C17 116.07(16) . . ? C27 N3 C26 120.65(18) . . ? C27 N3 C25 122.93(17) . . ? C26 N3 C25 115.88(16) . . ? C2 C1 C6 120.6(2) . . ? C2 C1 H1 119.7 . . ? C6 C1 H1 119.7 . . ? C3 C2 C1 120.2(2) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 C4 119.7(2) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C3 C4 C5 120.1(2) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 120.4(2) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C1 118.89(19) . . ? C5 C6 C7 122.33(18) . . ? C1 C6 C7 118.75(18) . . ? N1 C7 C6 113.11(16) . . ? N1 C7 H7A 109.0 . . ? C6 C7 H7A 109.0 . . ? N1 C7 H7B 109.0 . . ? C6 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 S1 120.96(15) . . ? N1 C9 S2 120.91(15) . . ? S1 C9 S2 118.13(11) . . ? C15 C10 C11 120.2(2) . . ? C15 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C12 C11 C10 119.8(3) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 120.4(2) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C14 120.1(3) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C13 C14 C15 119.8(2) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C10 C15 C14 119.6(2) . . ? C10 C15 C16 120.3(2) . . ? C14 C15 C16 120.14(19) . . ? N2 C16 C15 111.77(16) . . ? N2 C16 H16A 109.3 . . ? C15 C16 H16A 109.3 . . ? N2 C16 H16B 109.3 . . ? C15 C16 H16B 109.3 . . ? H16A C16 H16B 107.9 . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 S3 120.49(15) . . ? N2 C18 S4 120.97(15) . . ? S3 C18 S4 118.54(12) . . ? C20 C19 C24 120.7(2) . . ? C20 C19 H19 119.7 . . ? C24 C19 H19 119.7 . . ? C21 C20 C19 120.0(2) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C20 119.8(2) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C23 120.3(2) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C22 C23 C24 120.4(2) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C23 C24 C19 118.82(19) . . ? C23 C24 C25 120.25(19) . . ? C19 C24 C25 120.90(18) . . ? N3 C25 C24 110.08(17) . . ? N3 C25 H25A 109.6 . . ? C24 C25 H25A 109.6 . . ? N3 C25 H25B 109.6 . . ? C24 C25 H25B 109.6 . . ? H25A C25 H25B 108.2 . . ? N3 C26 H26A 109.5 . . ? N3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 C27 S5 119.31(16) . . ? N3 C27 S6 122.31(16) . . ? S5 C27 S6 118.38(11) . . ? 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 S4 In1 S1 C9 159.29(7) . . . . ? S5 In1 S1 C9 -34.30(8) . . . . ? S6 In1 S1 C9 -105.34(7) . . . . ? S2 In1 S1 C9 -2.53(6) . . . . ? S3 In1 S1 C9 89.67(7) . . . . ? S4 In1 S2 C9 -42.95(8) . . . . ? S1 In1 S2 C9 2.52(6) . . . . ? S5 In1 S2 C9 171.44(6) . . . . ? S6 In1 S2 C9 101.85(7) . . . . ? S3 In1 S2 C9 -95.20(7) . . . . ? S4 In1 S3 C18 1.09(6) . . . . ? S1 In1 S3 C18 89.35(7) . . . . ? S5 In1 S3 C18 -108.28(7) . . . . ? S6 In1 S3 C18 -57.85(8) . . . . ? S2 In1 S3 C18 159.43(7) . . . . ? S1 In1 S4 C18 -100.15(7) . . . . ? S5 In1 S4 C18 85.06(7) . . . . ? S6 In1 S4 C18 155.44(6) . . . . ? S2 In1 S4 C18 -58.22(8) . . . . ? S3 In1 S4 C18 -1.08(6) . . . . ? S4 In1 S5 C27 88.31(7) . . . . ? S1 In1 S5 C27 -77.27(8) . . . . ? S6 In1 S5 C27 0.20(7) . . . . ? S2 In1 S5 C27 -106.86(7) . . . . ? S3 In1 S5 C27 157.84(7) . . . . ? S4 In1 S6 C27 -108.94(7) . . . . ? S1 In1 S6 C27 158.25(7) . . . . ? S5 In1 S6 C27 -0.20(7) . . . . ? S2 In1 S6 C27 85.72(7) . . . . ? S3 In1 S6 C27 -55.25(8) . . . . ? C6 C1 C2 C3 0.9(3) . . . . ? C1 C2 C3 C4 -1.6(3) . . . . ? C2 C3 C4 C5 1.3(3) . . . . ? C3 C4 C5 C6 -0.2(3) . . . . ? C4 C5 C6 C1 -0.5(3) . . . . ? C4 C5 C6 C7 -178.5(2) . . . . ? C2 C1 C6 C5 0.1(3) . . . . ? C2 C1 C6 C7 178.18(19) . . . . ? C9 N1 C7 C6 97.6(2) . . . . ? C8 N1 C7 C6 -76.2(2) . . . . ? C5 C6 C7 N1 -32.1(3) . . . . ? C1 C6 C7 N1 149.95(18) . . . . ? C7 N1 C9 S1 -176.32(14) . . . . ? C8 N1 C9 S1 -2.9(3) . . . . ? C7 N1 C9 S2 4.2(3) . . . . ? C8 N1 C9 S2 177.60(15) . . . . ? In1 S1 C9 N1 -175.45(16) . . . . ? In1 S1 C9 S2 4.05(10) . . . . ? In1 S2 C9 N1 175.48(16) . . . . ? In1 S2 C9 S1 -4.02(10) . . . . ? C15 C10 C11 C12 0.2(4) . . . . ? C10 C11 C12 C13 -0.7(4) . . . . ? C11 C12 C13 C14 1.0(4) . . . . ? C12 C13 C14 C15 -0.8(4) . . . . ? C11 C10 C15 C14 0.0(3) . . . . ? C11 C10 C15 C16 -178.3(2) . . . . ? C13 C14 C15 C10 0.3(3) . . . . ? C13 C14 C15 C16 178.62(19) . . . . ? C18 N2 C16 C15 -103.0(2) . . . . ? C17 N2 C16 C15 73.6(2) . . . . ? C10 C15 C16 N2 -119.2(2) . . . . ? C14 C15 C16 N2 62.5(2) . . . . ? C16 N2 C18 S3 172.26(14) . . . . ? C17 N2 C18 S3 -4.2(3) . . . . ? C16 N2 C18 S4 -7.3(3) . . . . ? C17 N2 C18 S4 176.27(14) . . . . ? In1 S3 C18 N2 178.74(16) . . . . ? In1 S3 C18 S4 -1.73(10) . . . . ? In1 S4 C18 N2 -178.72(16) . . . . ? In1 S4 C18 S3 1.75(10) . . . . ? C24 C19 C20 C21 0.6(3) . . . . ? C19 C20 C21 C22 0.1(4) . . . . ? C20 C21 C22 C23 -0.7(4) . . . . ? C21 C22 C23 C24 0.5(3) . . . . ? C22 C23 C24 C19 0.1(3) . . . . ? C22 C23 C24 C25 -177.7(2) . . . . ? C20 C19 C24 C23 -0.7(3) . . . . ? C20 C19 C24 C25 177.2(2) . . . . ? C27 N3 C25 C24 -98.9(2) . . . . ? C26 N3 C25 C24 72.6(2) . . . . ? C23 C24 C25 N3 87.7(2) . . . . ? C19 C24 C25 N3 -90.1(2) . . . . ? C26 N3 C27 S5 -2.5(3) . . . . ? C25 N3 C27 S5 168.63(15) . . . . ? C26 N3 C27 S6 176.98(16) . . . . ? C25 N3 C27 S6 -11.8(3) . . . . ? In1 S5 C27 N3 179.23(16) . . . . ? In1 S5 C27 S6 -0.32(11) . . . . ? In1 S6 C27 N3 -179.21(17) . . . . ? In1 S6 C27 S5 0.32(11) . . . . ? 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 C16 H16A S4 0.99 2.81 3.749(2) 159 2_666 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.528 _refine_diff_density_min -0.334 _refine_diff_density_rms 0.067 _iucr_refine_instructions_details ; TITL 3776 in P-1 [In(N-Me N-benzyldtcl2)3] CELL 0.71073 9.7966 12.2791 12.7790 96.142 92.353 100.383 ZERR 2.00 0.0004 0.0008 0.0008 0.004 0.004 0.005 LATT 1 SFAC C H In N S UNIT 54 60 2 6 12 OMIT -2 54 OMIT 0 0 1 OMIT -10 -3 9 OMIT -6 -7 4 OMIT 0 -1 6 L.S. 24 BOND $H eqiv $1 1-x, 1-y, 1-z htab C16 S4_$1 ACTA conf SIZE 0.060 0.080 0.150 ! colorless parallelepiped TEMP -173 WGHT 0.018500 0.928800 FVAR 0.14470 IN1 3 0.371632 0.868293 0.659066 11.00000 0.01622 0.01382 = 0.01592 0.00062 -0.00190 0.00338 S1 5 0.329676 0.991261 0.513702 11.00000 0.01785 0.01763 = 0.01754 0.00352 0.00222 0.00478 S2 5 0.186909 0.988454 0.713091 11.00000 0.02125 0.01946 = 0.01661 0.00096 0.00229 0.00653 S3 5 0.190283 0.688679 0.588998 11.00000 0.01702 0.01705 = 0.01901 0.00050 0.00192 0.00106 S4 5 0.482764 0.738992 0.529544 11.00000 0.01576 0.01616 = 0.02836 -0.00193 0.00158 0.00229 S5 5 0.392420 0.808864 0.846741 11.00000 0.01932 0.02366 = 0.02085 0.00623 -0.00240 0.00043 S6 5 0.605658 0.969150 0.755230 11.00000 0.01819 0.02183 = 0.01840 0.00322 -0.00128 -0.00008 N1 4 0.126844 1.103905 0.557463 11.00000 0.01602 0.01522 = 0.02034 -0.00062 -0.00100 0.00380 N2 4 0.304658 0.551186 0.459547 11.00000 0.02080 0.01558 = 0.01800 0.00145 0.00057 0.00265 N3 4 0.627830 0.909904 0.950935 11.00000 0.01836 0.02228 = 0.01705 -0.00009 -0.00107 0.00354 C1 1 -0.011683 1.336582 0.698221 11.00000 0.02069 0.02419 = 0.01917 0.00365 0.00136 0.00898 AFIX 43 H1 2 -0.107466 1.312457 0.677198 11.00000 -1.20000 AFIX 0 C2 1 0.034143 1.442774 0.749938 11.00000 0.03351 0.02298 = 0.01920 0.00149 0.00370 0.01399 AFIX 43 H2 2 -0.030465 1.490589 0.765083 11.00000 -1.20000 AFIX 0 C3 1 0.173320 1.479350 0.779538 11.00000 0.03556 0.01813 = 0.01825 -0.00275 0.00393 0.00336 AFIX 43 H3 2 0.204955 1.552862 0.813381 11.00000 -1.20000 AFIX 0 C4 1 0.266778 1.408353 0.759672 11.00000 0.02100 0.02670 = 0.03043 -0.00337 0.00172 -0.00041 AFIX 43 H4 2 0.362369 1.432755 0.781199 11.00000 -1.20000 AFIX 0 C5 1 0.220838 1.301437 0.708270 11.00000 0.01949 0.02358 = 0.03132 -0.00293 0.00297 0.00708 AFIX 43 H5 2 0.285336 1.253182 0.694662 11.00000 -1.20000 AFIX 0 C6 1 0.081323 1.264857 0.676753 11.00000 0.01984 0.01641 = 0.01788 0.00320 0.00293 0.00525 C7 1 0.026089 1.148948 0.623255 11.00000 0.01415 0.01779 = 0.03084 -0.00066 -0.00081 0.00449 AFIX 23 H7A 2 -0.000746 1.098809 0.677677 11.00000 -1.20000 H7B 2 -0.058619 1.150128 0.578717 11.00000 -1.20000 AFIX 0 C8 1 0.144881 1.148572 0.455846 11.00000 0.02237 0.01838 = 0.02477 0.00453 -0.00320 0.00459 AFIX 137 H8A 2 0.214259 1.217699 0.465371 11.00000 -1.50000 H8B 2 0.056041 1.163979 0.428912 11.00000 -1.50000 H8C 2 0.176384 1.093860 0.405411 11.00000 -1.50000 AFIX 0 C9 1 0.206151 1.035686 0.591045 11.00000 0.01488 0.01133 = 0.01752 -0.00208 -0.00248 -0.00024 C10 1 0.348218 0.436223 0.200774 11.00000 0.02889 0.03493 = 0.03171 -0.00515 -0.00110 0.00695 AFIX 43 H10 2 0.355226 0.365324 0.221538 11.00000 -1.20000 AFIX 0 C11 1 0.316181 0.446328 0.095591 11.00000 0.04379 0.06735 = 0.02863 -0.01626 -0.00534 0.01480 AFIX 43 H11 2 0.301065 0.382420 0.044641 11.00000 -1.20000 AFIX 0 C12 1 0.306458 0.548947 0.065577 11.00000 0.04426 0.09017 = 0.01992 0.00382 -0.00164 0.02461 AFIX 43 H12 2 0.285618 0.555900 -0.006394 11.00000 -1.20000 AFIX 0 C13 1 0.326718 0.641782 0.139124 11.00000 0.02759 0.05636 = 0.03754 0.02370 0.00714 0.01288 AFIX 43 H13 2 0.318310 0.712241 0.117946 11.00000 -1.20000 AFIX 0 C14 1 0.359388 0.632604 0.244099 11.00000 0.02005 0.03030 = 0.02819 0.00662 0.00361 0.00524 AFIX 43 H14 2 0.374563 0.696835 0.294665 11.00000 -1.20000 AFIX 0 C15 1 0.369872 0.528923 0.275129 11.00000 0.01446 0.02506 = 0.02116 0.00087 0.00180 0.00407 C16 1 0.408567 0.518604 0.388773 11.00000 0.02183 0.01689 = 0.02308 -0.00157 -0.00146 0.00810 AFIX 23 H16A 2 0.417040 0.440532 0.395727 11.00000 -1.20000 H16B 2 0.500127 0.566555 0.409952 11.00000 -1.20000 AFIX 0 C17 1 0.172500 0.471927 0.456333 11.00000 0.02679 0.01666 = 0.02289 -0.00016 0.00132 -0.00170 AFIX 137 H17A 2 0.159425 0.446069 0.525806 11.00000 -1.50000 H17B 2 0.174200 0.408074 0.403686 11.00000 -1.50000 H17C 2 0.095712 0.508764 0.437364 11.00000 -1.50000 AFIX 0 C18 1 0.323997 0.648940 0.519778 11.00000 0.01825 0.01610 = 0.01740 0.00408 -0.00212 0.00328 C19 1 0.914511 0.839668 1.044163 11.00000 0.02570 0.02609 = 0.01637 0.00025 0.00179 0.00687 AFIX 43 H19 2 0.887987 0.865757 1.111618 11.00000 -1.20000 AFIX 0 C20 1 0.996869 0.758743 1.035366 11.00000 0.03003 0.02864 = 0.02513 0.00691 0.00161 0.00957 AFIX 43 H20 2 1.025766 0.729207 1.096550 11.00000 -1.20000 AFIX 0 C21 1 1.036934 0.721035 0.937583 11.00000 0.02617 0.02617 = 0.03638 0.00301 0.00827 0.01074 AFIX 43 H21 2 1.093222 0.665521 0.931449 11.00000 -1.20000 AFIX 0 C22 1 0.994864 0.764331 0.848845 11.00000 0.02829 0.03521 = 0.02218 -0.00381 0.00850 0.00740 AFIX 43 H22 2 1.023149 0.739021 0.781729 11.00000 -1.20000 AFIX 0 C23 1 0.911397 0.844704 0.857279 11.00000 0.02190 0.02949 = 0.01849 0.00409 0.00262 0.00178 AFIX 43 H23 2 0.882243 0.873607 0.795801 11.00000 -1.20000 AFIX 0 C24 1 0.870308 0.883064 0.955087 11.00000 0.01620 0.01990 = 0.01999 0.00090 0.00090 0.00007 C25 1 0.774853 0.967600 0.963556 11.00000 0.01885 0.02019 = 0.02121 -0.00103 -0.00364 0.00072 AFIX 23 H25A 2 0.792636 1.013203 1.033136 11.00000 -1.20000 H25B 2 0.793920 1.018035 0.908282 11.00000 -1.20000 AFIX 0 C26 1 0.575313 0.852145 1.040019 11.00000 0.02426 0.03560 = 0.01675 0.00404 0.00001 0.00521 AFIX 137 H26A 2 0.481693 0.865935 1.053120 11.00000 -1.50000 H26B 2 0.637254 0.880041 1.103058 11.00000 -1.50000 H26C 2 0.571916 0.771882 1.023376 11.00000 -1.50000 AFIX 0 C27 1 0.551564 0.897791 0.860439 11.00000 0.01677 0.01858 = 0.01969 -0.00042 0.00131 0.00557 HKLF 4 REM 3776 in P-1 [In(N-Me N-benzyldtcl2)3] REM R1 = 0.0228 for 5800 Fo > 4sig(Fo) and 0.0283 for all 6504 data REM 337 parameters refined using 0 restraints END WGHT 0.0175 0.9900 REM Highest difference peak 0.528, deepest hole -0.334, 1-sigma level 0.067 Q1 1 0.5829 1.0207 0.7217 11.00000 0.05 0.53 Q2 1 0.4777 0.8450 0.8408 11.00000 0.05 0.49 Q3 1 0.1449 1.2848 0.6975 11.00000 0.05 0.38 Q4 1 0.2443 0.7458 0.6249 11.00000 0.05 0.38 Q5 1 0.7005 0.9391 0.9572 11.00000 0.05 0.36 Q6 1 0.2446 0.5135 0.4600 11.00000 0.05 0.34 Q7 1 0.3363 0.8820 0.7162 11.00000 0.05 0.33 Q8 1 0.4020 0.6842 0.5209 11.00000 0.05 0.33 Q9 1 0.2813 0.8625 0.6432 11.00000 0.05 0.32 Q10 1 0.0464 1.2990 0.7029 11.00000 0.05 0.32 Q11 1 0.2160 1.4442 0.7458 11.00000 0.05 0.32 Q12 1 0.5742 0.9456 0.8164 11.00000 0.05 0.31 Q13 1 0.1130 1.4677 0.7496 11.00000 0.05 0.31 Q14 1 0.0962 1.1358 0.5983 11.00000 0.05 0.30 Q15 1 0.0628 1.2264 0.6467 11.00000 0.05 0.30 Q16 1 0.4539 0.8776 0.6713 11.00000 0.05 0.30 Q17 1 0.3663 0.5198 0.3292 11.00000 0.05 0.30 Q18 1 0.3284 0.4833 0.2424 11.00000 0.05 0.29 Q19 1 0.0540 1.2074 0.6635 11.00000 0.05 0.29 Q20 1 0.2412 1.3601 0.7247 11.00000 0.05 0.28 ; _database_code_depnum_ccdc_archive 'CCDC 924189' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_sad #TrackingRef 'CiF (3)' _audit_creation_method SHELXL-97 _chemical_name_systematic ; In(N,N-pentamethylenethiocarbamato)3.0.5pyridine solvate ; _chemical_name_common '[In(S~2~CPip]0.5(py)' _chemical_melting_point ? _chemical_formula_moiety 'C18 H30 In N3 S6, 0.5(C5 H5 N)' _chemical_formula_sum 'C20.50 H32.50 In N3.50 S6' _chemical_formula_weight 635.18 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4396(2) _cell_length_b 10.7753(3) _cell_length_c 14.0452(3) _cell_angle_alpha 93.148(2) _cell_angle_beta 91.655(2) _cell_angle_gamma 107.443(3) _cell_volume 1359.31(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100 _cell_measurement_reflns_used 9962 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 31.00 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 650 _exptl_absorpt_coefficient_mu 1.346 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6576 _exptl_absorpt_correction_T_max 0.8445 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 13467 _diffrn_reflns_av_R_equivalents 0.0114 _diffrn_reflns_av_sigmaI/netI 0.0172 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 28.00 _reflns_number_total 6491 _reflns_number_gt 6176 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. The pyridine solvate molecule is disordered with respect to an inversion center and is therefore refined at 1/2 occupancy. ; _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^)+(0.0156P)^2^+0.4902P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6491 _refine_ls_number_parameters 295 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0174 _refine_ls_R_factor_gt 0.0162 _refine_ls_wR_factor_ref 0.0403 _refine_ls_wR_factor_gt 0.0395 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.004 _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 In1 In 0.163019(9) 0.154208(8) 0.812609(6) 0.02115(3) Uani 1 1 d . . . S1 S -0.00256(3) -0.03040(3) 0.69457(2) 0.02319(6) Uani 1 1 d . . . S2 S 0.32021(4) 0.09425(3) 0.67788(2) 0.02629(7) Uani 1 1 d . . . S3 S -0.05795(4) 0.22320(3) 0.87650(2) 0.02372(7) Uani 1 1 d . . . S4 S 0.14842(4) 0.36431(3) 0.73580(2) 0.02546(7) Uani 1 1 d . . . S5 S 0.39573(4) 0.28282(3) 0.91751(2) 0.02583(7) Uani 1 1 d . . . S6 S 0.20075(3) 0.01799(3) 0.95082(2) 0.02322(6) Uani 1 1 d . . . N1 N 0.15000(13) -0.08330(12) 0.54889(9) 0.0287(2) Uani 1 1 d . . . N2 N -0.07802(13) 0.43898(11) 0.80107(8) 0.0252(2) Uani 1 1 d . . . N3 N 0.44750(12) 0.14050(12) 1.05644(8) 0.0265(2) Uani 1 1 d . . . C1 C 0.01792(15) -0.18819(14) 0.51120(10) 0.0286(3) Uani 1 1 d . . . H1A H -0.0131 -0.1682 0.4474 0.034 Uiso 1 1 calc R . . H1B H -0.0651 -0.1947 0.5540 0.034 Uiso 1 1 calc R . . C2 C 0.05337(17) -0.31680(14) 0.50393(11) 0.0325(3) Uani 1 1 d . . . H2A H -0.0342 -0.3862 0.4754 0.039 Uiso 1 1 calc R . . H2B H 0.0750 -0.3405 0.5687 0.039 Uiso 1 1 calc R . . C3 C 0.18644(18) -0.30782(15) 0.44299(12) 0.0362(3) Uani 1 1 d . . . H3A H 0.1600 -0.2963 0.3760 0.043 Uiso 1 1 calc R . . H3B H 0.2130 -0.3899 0.4443 0.043 Uiso 1 1 calc R . . C4 C 0.31959(17) -0.19367(17) 0.47977(11) 0.0363(3) Uani 1 1 d . . . H4A H 0.3552 -0.2114 0.5431 0.044 Uiso 1 1 calc R . . H4B H 0.4014 -0.1841 0.4356 0.044 Uiso 1 1 calc R . . C5 C 0.27816(16) -0.06808(15) 0.48804(11) 0.0338(3) Uani 1 1 d . . . H5A H 0.3640 0.0036 0.5160 0.041 Uiso 1 1 calc R . . H5B H 0.2528 -0.0452 0.4238 0.041 Uiso 1 1 calc R . . C6 C 0.15560(14) -0.01485(12) 0.63093(9) 0.0228(2) Uani 1 1 d . . . C7 C -0.02300(18) 0.56176(14) 0.75398(11) 0.0327(3) Uani 1 1 d . . . H7A H -0.0978 0.5680 0.7051 0.039 Uiso 1 1 calc R . . H7B H 0.0697 0.5643 0.7219 0.039 Uiso 1 1 calc R . . C8 C 0.00664(16) 0.67528(14) 0.82849(12) 0.0330(3) Uani 1 1 d . . . H8A H 0.0853 0.6711 0.8753 0.040 Uiso 1 1 calc R . . H8B H 0.0424 0.7584 0.7972 0.040 Uiso 1 1 calc R . . C9 C -0.13357(17) 0.67159(14) 0.88004(12) 0.0334(3) Uani 1 1 d . . . H9A H -0.2090 0.6846 0.8345 0.040 Uiso 1 1 calc R . . H9B H -0.1109 0.7431 0.9308 0.040 Uiso 1 1 calc R . . C10 C -0.19510(17) 0.54115(14) 0.92391(11) 0.0326(3) Uani 1 1 d . . . H10A H -0.1259 0.5343 0.9762 0.039 Uiso 1 1 calc R . . H10B H -0.2917 0.5365 0.9515 0.039 Uiso 1 1 calc R . . C11 C -0.21612(15) 0.42819(14) 0.85022(11) 0.0285(3) Uani 1 1 d . . . H11A H -0.2465 0.3451 0.8820 0.034 Uiso 1 1 calc R . . H11B H -0.2963 0.4274 0.8029 0.034 Uiso 1 1 calc R . . C12 C -0.00403(14) 0.35216(12) 0.80430(9) 0.0215(2) Uani 1 1 d . . . C13 C 0.57881(16) 0.24917(16) 1.09002(12) 0.0368(3) Uani 1 1 d . . . H13A H 0.5963 0.3193 1.0451 0.044 Uiso 1 1 calc R . . H13B H 0.6677 0.2186 1.0929 0.044 Uiso 1 1 calc R . . C14 C 0.5527(2) 0.30130(17) 1.18856(13) 0.0448(4) Uani 1 1 d . . . H14A H 0.6433 0.3705 1.2132 0.054 Uiso 1 1 calc R . . H14B H 0.4705 0.3404 1.1838 0.054 Uiso 1 1 calc R . . C15 C 0.5141(2) 0.1939(2) 1.25772(12) 0.0526(5) Uani 1 1 d . . . H15A H 0.4868 0.2286 1.3189 0.063 Uiso 1 1 calc R . . H15B H 0.6024 0.1647 1.2706 0.063 Uiso 1 1 calc R . . C16 C 0.3856(2) 0.07802(18) 1.21776(11) 0.0411(4) Uani 1 1 d . . . H16A H 0.3703 0.0060 1.2609 0.049 Uiso 1 1 calc R . . H16B H 0.2933 0.1036 1.2143 0.049 Uiso 1 1 calc R . . C17 C 0.41724(15) 0.03178(14) 1.11926(10) 0.0283(3) Uani 1 1 d . . . H17A H 0.5042 -0.0014 1.1233 0.034 Uiso 1 1 calc R . . H17B H 0.3306 -0.0403 1.0927 0.034 Uiso 1 1 calc R . . C18 C 0.35840(13) 0.14681(12) 0.98351(9) 0.0220(2) Uani 1 1 d . . . N4 N 0.3957(5) 0.4197(4) 0.4352(3) 0.0487(11) Uiso 0.31 1 d P . 1 C4A C 0.3957(5) 0.4197(4) 0.4352(3) 0.0487(11) Uiso 0.31 1 d P . 1 H4AA H 0.3267 0.3659 0.3940 0.058 Uiso 0.31 1 d PR . 1 C19 C 0.3995(5) 0.3947(4) 0.5300(3) 0.0428(10) Uiso 0.62 1 d P A 1 H19 H 0.3269 0.3198 0.5498 0.051 Uiso 0.62 1 d PR A 1 C20 C 0.5021(5) 0.4727(5) 0.5962(3) 0.0523(13) Uiso 0.62 1 d P . 1 H20 H 0.5019 0.4517 0.6610 0.063 Uiso 0.62 1 d PR . 1 N5 N 0.4802(8) 0.4444(7) 0.5797(6) 0.055(2) Uiso 0.19 1 d P . 2 C5A C 0.4802(8) 0.4444(7) 0.5797(6) 0.055(2) Uiso 0.19 1 d P . 2 H5AA H 0.4632 0.4048 0.6348 0.067 Uiso 0.19 1 d PR . 2 C21 C 0.3904(8) 0.3840(7) 0.5030(6) 0.0498(19) Uiso 0.38 1 d P B 2 H21 H 0.3176 0.3024 0.5091 0.060 Uiso 0.38 1 d PR B 2 C22 C 0.4054(10) 0.4405(9) 0.4171(7) 0.061(3) Uiso 0.38 1 d P . 2 H22 H 0.3454 0.4053 0.3608 0.073 Uiso 0.38 1 d PR . 2 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 In1 0.02211(5) 0.01971(5) 0.02222(5) 0.00011(3) 0.00201(3) 0.00735(3) S1 0.02191(14) 0.02397(15) 0.02375(15) -0.00007(12) 0.00387(11) 0.00705(12) S2 0.02198(15) 0.02635(16) 0.02912(17) -0.00419(13) 0.00405(12) 0.00593(12) S3 0.02406(15) 0.02041(14) 0.02705(16) 0.00390(12) 0.00733(12) 0.00629(12) S4 0.02755(16) 0.02448(15) 0.02739(16) 0.00597(12) 0.01033(13) 0.01091(13) S5 0.02275(15) 0.02044(15) 0.03065(17) 0.00014(12) 0.00336(12) 0.00111(12) S6 0.01913(14) 0.02087(14) 0.02656(15) 0.00222(12) -0.00234(11) 0.00156(11) N1 0.0254(6) 0.0287(6) 0.0285(6) -0.0056(5) 0.0072(5) 0.0034(5) N2 0.0276(6) 0.0237(5) 0.0269(6) 0.0031(4) 0.0072(4) 0.0110(4) N3 0.0191(5) 0.0305(6) 0.0251(6) -0.0016(5) -0.0014(4) 0.0009(4) C1 0.0257(6) 0.0284(7) 0.0285(7) -0.0050(5) 0.0021(5) 0.0045(5) C2 0.0379(8) 0.0281(7) 0.0300(7) 0.0029(6) 0.0018(6) 0.0078(6) C3 0.0384(8) 0.0329(8) 0.0391(8) -0.0056(6) 0.0019(7) 0.0147(6) C4 0.0307(7) 0.0489(9) 0.0308(7) -0.0065(7) 0.0009(6) 0.0161(7) C5 0.0286(7) 0.0370(8) 0.0306(7) -0.0073(6) 0.0106(6) 0.0029(6) C6 0.0242(6) 0.0206(6) 0.0251(6) 0.0024(5) 0.0031(5) 0.0085(5) C7 0.0404(8) 0.0307(7) 0.0347(8) 0.0125(6) 0.0122(6) 0.0197(6) C8 0.0308(7) 0.0236(7) 0.0460(9) 0.0088(6) 0.0020(6) 0.0095(6) C9 0.0376(8) 0.0265(7) 0.0383(8) -0.0032(6) 0.0013(6) 0.0140(6) C10 0.0331(7) 0.0316(7) 0.0348(8) -0.0031(6) 0.0085(6) 0.0129(6) C11 0.0211(6) 0.0264(7) 0.0386(8) -0.0021(6) 0.0058(5) 0.0084(5) C12 0.0231(6) 0.0210(6) 0.0200(6) -0.0008(5) 0.0027(5) 0.0061(5) C13 0.0217(6) 0.0371(8) 0.0436(9) -0.0060(7) -0.0088(6) -0.0006(6) C14 0.0435(9) 0.0434(9) 0.0470(10) -0.0175(8) -0.0192(8) 0.0180(8) C15 0.0746(13) 0.0637(12) 0.0294(8) -0.0145(8) -0.0132(8) 0.0401(11) C16 0.0482(9) 0.0584(11) 0.0266(7) 0.0073(7) 0.0079(7) 0.0298(8) C17 0.0240(6) 0.0353(7) 0.0257(7) 0.0022(5) -0.0008(5) 0.0094(6) C18 0.0182(5) 0.0230(6) 0.0231(6) -0.0028(5) 0.0046(5) 0.0040(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 In1 S6 2.5760(3) . ? In1 S3 2.5833(3) . ? In1 S5 2.5847(4) . ? In1 S4 2.5991(3) . ? In1 S1 2.6024(3) . ? In1 S2 2.6082(3) . ? S1 C6 1.7319(13) . ? S2 C6 1.7296(14) . ? S3 C12 1.7260(13) . ? S4 C12 1.7305(13) . ? S5 C18 1.7291(14) . ? S6 C18 1.7333(13) . ? N1 C6 1.3245(17) . ? N1 C1 1.4709(17) . ? N1 C5 1.4755(17) . ? N2 C12 1.3265(16) . ? N2 C11 1.4695(17) . ? N2 C7 1.4702(17) . ? N3 C18 1.3241(17) . ? N3 C17 1.4697(18) . ? N3 C13 1.4716(17) . ? C1 C2 1.519(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.523(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.525(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.517(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C7 C8 1.519(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.518(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.523(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.516(2) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C13 C14 1.520(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.519(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.524(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.513(2) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? N4 C20 1.371(6) 2_666 ? N4 C19 1.375(6) . ? C19 C20 1.373(6) . ? C19 H19 0.9500 . ? C20 C4A 1.371(6) 2_666 ? C20 N4 1.371(6) 2_666 ? C20 H20 0.9499 . ? N5 C21 1.356(10) . ? N5 C22 1.377(11) 2_666 ? N5 H20 1.1495 . ? C21 C22 1.373(11) . ? C21 H21 0.9500 . ? C22 C5A 1.377(11) 2_666 ? C22 N5 1.377(11) 2_666 ? C22 H22 0.9500 . ? 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 S6 In1 S3 98.541(11) . . ? S6 In1 S5 70.162(11) . . ? S3 In1 S5 106.975(11) . . ? S6 In1 S4 155.207(12) . . ? S3 In1 S4 69.788(10) . . ? S5 In1 S4 91.833(11) . . ? S6 In1 S1 99.855(11) . . ? S3 In1 S1 94.226(11) . . ? S5 In1 S1 157.511(11) . . ? S4 In1 S1 102.709(11) . . ? S6 In1 S2 103.971(11) . . ? S3 In1 S2 153.917(12) . . ? S5 In1 S2 93.075(11) . . ? S4 In1 S2 93.583(11) . . ? S1 In1 S2 69.245(10) . . ? C6 S1 In1 86.60(5) . . ? C6 S2 In1 86.46(4) . . ? C12 S3 In1 86.34(4) . . ? C12 S4 In1 85.75(4) . . ? C18 S5 In1 85.85(4) . . ? C18 S6 In1 86.04(5) . . ? C6 N1 C1 123.69(11) . . ? C6 N1 C5 123.71(12) . . ? C1 N1 C5 112.50(11) . . ? C12 N2 C11 123.93(11) . . ? C12 N2 C7 122.95(11) . . ? C11 N2 C7 112.94(11) . . ? C18 N3 C17 124.03(11) . . ? C18 N3 C13 123.09(12) . . ? C17 N3 C13 112.51(11) . . ? N1 C1 C2 109.70(12) . . ? N1 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? N1 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? C1 C2 C3 111.11(12) . . ? C1 C2 H2A 109.4 . . ? C3 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? C3 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C2 C3 C4 110.78(12) . . ? C2 C3 H3A 109.5 . . ? C4 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? C5 C4 C3 110.83(12) . . ? C5 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? N1 C5 C4 110.21(13) . . ? N1 C5 H5A 109.6 . . ? C4 C5 H5A 109.6 . . ? N1 C5 H5B 109.6 . . ? C4 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? N1 C6 S2 121.38(10) . . ? N1 C6 S1 121.04(10) . . ? S2 C6 S1 117.57(8) . . ? N2 C7 C8 109.03(12) . . ? N2 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? N2 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? C9 C8 C7 110.71(12) . . ? C9 C8 H8A 109.5 . . ? C7 C8 H8A 109.5 . . ? C9 C8 H8B 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C8 C9 C10 110.22(12) . . ? C8 C9 H9A 109.6 . . ? C10 C9 H9A 109.6 . . ? C8 C9 H9B 109.6 . . ? C10 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? C11 C10 C9 111.36(13) . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? N2 C11 C10 110.84(11) . . ? N2 C11 H11A 109.5 . . ? C10 C11 H11A 109.5 . . ? N2 C11 H11B 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? N2 C12 S3 120.86(10) . . ? N2 C12 S4 121.01(10) . . ? S3 C12 S4 118.12(7) . . ? N3 C13 C14 109.13(13) . . ? N3 C13 H13A 109.9 . . ? C14 C13 H13A 109.9 . . ? N3 C13 H13B 109.9 . . ? C14 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? C15 C14 C13 111.32(14) . . ? C15 C14 H14A 109.4 . . ? C13 C14 H14A 109.4 . . ? C15 C14 H14B 109.4 . . ? C13 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C14 C15 C16 111.37(14) . . ? C14 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? C14 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C17 C16 C15 110.64(14) . . ? C17 C16 H16A 109.5 . . ? C15 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? N3 C17 C16 109.55(12) . . ? N3 C17 H17A 109.8 . . ? C16 C17 H17A 109.8 . . ? N3 C17 H17B 109.8 . . ? C16 C17 H17B 109.8 . . ? H17A C17 H17B 108.2 . . ? N3 C18 S5 121.29(10) . . ? N3 C18 S6 120.83(10) . . ? S5 C18 S6 117.88(8) . . ? C20 N4 C19 119.5(4) 2_666 . ? C20 C19 N4 123.1(4) . . ? C20 C19 H19 119.3 . . ? N4 C19 H19 117.7 . . ? C4A C20 C19 117.4(4) 2_666 . ? N4 C20 C19 117.4(4) 2_666 . ? C4A C20 H20 121.9 2_666 . ? N4 C20 H20 121.9 2_666 . ? C19 C20 H20 120.6 . . ? C21 N5 C22 127.5(7) . 2_666 ? N5 C21 C22 120.0(7) . . ? N5 C21 H21 119.7 . . ? C22 C21 H21 120.3 . . ? C21 C22 C5A 112.4(8) . 2_666 ? C21 C22 N5 112.4(8) . 2_666 ? C21 C22 H22 125.0 . . ? C5A C22 H22 122.6 2_666 . ? N5 C22 H22 122.6 2_666 . ? 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 S6 In1 S1 C6 -103.44(4) . . . . ? S3 In1 S1 C6 157.12(4) . . . . ? S5 In1 S1 C6 -42.18(5) . . . . ? S4 In1 S1 C6 86.90(4) . . . . ? S2 In1 S1 C6 -2.13(4) . . . . ? S6 In1 S2 C6 97.54(4) . . . . ? S3 In1 S2 C6 -51.36(5) . . . . ? S5 In1 S2 C6 167.86(4) . . . . ? S4 In1 S2 C6 -100.11(4) . . . . ? S1 In1 S2 C6 2.13(4) . . . . ? S6 In1 S3 C12 157.08(4) . . . . ? S5 In1 S3 C12 85.32(4) . . . . ? S4 In1 S3 C12 -0.28(4) . . . . ? S1 In1 S3 C12 -102.28(4) . . . . ? S2 In1 S3 C12 -53.37(5) . . . . ? S6 In1 S4 C12 -64.91(5) . . . . ? S3 In1 S4 C12 0.28(4) . . . . ? S5 In1 S4 C12 -107.15(4) . . . . ? S1 In1 S4 C12 90.14(4) . . . . ? S2 In1 S4 C12 159.66(4) . . . . ? S6 In1 S5 C18 1.64(4) . . . . ? S3 In1 S5 C18 94.79(4) . . . . ? S4 In1 S5 C18 164.20(4) . . . . ? S1 In1 S5 C18 -65.05(5) . . . . ? S2 In1 S5 C18 -102.11(4) . . . . ? S3 In1 S6 C18 -106.68(4) . . . . ? S5 In1 S6 C18 -1.63(4) . . . . ? S4 In1 S6 C18 -47.21(5) . . . . ? S1 In1 S6 C18 157.48(4) . . . . ? S2 In1 S6 C18 86.59(4) . . . . ? C6 N1 C1 C2 -117.06(15) . . . . ? C5 N1 C1 C2 59.56(16) . . . . ? N1 C1 C2 C3 -56.18(16) . . . . ? C1 C2 C3 C4 53.95(17) . . . . ? C2 C3 C4 C5 -53.50(17) . . . . ? C6 N1 C5 C4 117.07(15) . . . . ? C1 N1 C5 C4 -59.55(16) . . . . ? C3 C4 C5 N1 55.58(17) . . . . ? C1 N1 C6 S2 172.51(10) . . . . ? C5 N1 C6 S2 -3.7(2) . . . . ? C1 N1 C6 S1 -8.11(19) . . . . ? C5 N1 C6 S1 175.64(11) . . . . ? In1 S2 C6 N1 176.02(11) . . . . ? In1 S2 C6 S1 -3.38(7) . . . . ? In1 S1 C6 N1 -176.01(11) . . . . ? In1 S1 C6 S2 3.38(7) . . . . ? C12 N2 C7 C8 -115.68(14) . . . . ? C11 N2 C7 C8 59.68(16) . . . . ? N2 C7 C8 C9 -58.36(16) . . . . ? C7 C8 C9 C10 55.95(17) . . . . ? C8 C9 C10 C11 -53.27(17) . . . . ? C12 N2 C11 C10 117.68(15) . . . . ? C7 N2 C11 C10 -57.62(16) . . . . ? C9 C10 C11 N2 53.51(16) . . . . ? C11 N2 C12 S3 -5.49(18) . . . . ? C7 N2 C12 S3 169.35(11) . . . . ? C11 N2 C12 S4 174.11(10) . . . . ? C7 N2 C12 S4 -11.05(18) . . . . ? In1 S3 C12 N2 -179.94(11) . . . . ? In1 S3 C12 S4 0.45(7) . . . . ? In1 S4 C12 N2 179.94(11) . . . . ? In1 S4 C12 S3 -0.45(7) . . . . ? C18 N3 C13 C14 112.61(16) . . . . ? C17 N3 C13 C14 -60.67(16) . . . . ? N3 C13 C14 C15 55.33(18) . . . . ? C13 C14 C15 C16 -52.7(2) . . . . ? C14 C15 C16 C17 52.97(19) . . . . ? C18 N3 C17 C16 -111.65(15) . . . . ? C13 N3 C17 C16 61.56(15) . . . . ? C15 C16 C17 N3 -56.30(16) . . . . ? C17 N3 C18 S5 175.80(10) . . . . ? C13 N3 C18 S5 3.30(19) . . . . ? C17 N3 C18 S6 -4.57(18) . . . . ? C13 N3 C18 S6 -177.08(11) . . . . ? In1 S5 C18 N3 177.05(11) . . . . ? In1 S5 C18 S6 -2.59(7) . . . . ? In1 S6 C18 N3 -177.04(11) . . . . ? In1 S6 C18 S5 2.59(7) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.379 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.051 _iucr_refine_instructions_details ;TITL sad in P-1 In(N,N-pentamethylenethiocarbamato)3.0.5py CELL 0.71073 9.4396 10.7753 14.0452 93.148 91.655 107.443 ZERR 2.00 0.0002 0.0003 0.0003 0.002 0.002 0.003 LATT 1 SFAC C H N S In UNIT 41 65 7 12 2 omit 0 0 1 omit 2 -4 1 omit 2 4 6 omit -10 7 8 omit -8 -6 3 omit 9 -4 11 omit 3 -8 4 omit -6 -4 7 omit 6 -1 9 omit 8 -3 10 omit 5 4 10 omit 5 3 10 omit -1 -1 1 omit 0 56 exyz N4 c4a eadp N4 c4a exyz n5 c5a eadp n5 c5a L.S. 10 ACTA 56 BOND $H conf SIZE 0.13 0.17 0.34 TEMP -173 WGHT 0.018000 0.513000 FVAR 0.47569 IN1 5 0.163019 0.154208 0.812609 11.00000 0.02211 0.01971 = 0.02222 0.00011 0.00201 0.00735 S1 4 -0.002560 -0.030399 0.694572 11.00000 0.02191 0.02397 = 0.02375 -0.00007 0.00387 0.00705 S2 4 0.320211 0.094246 0.677878 11.00000 0.02198 0.02635 = 0.02912 -0.00419 0.00405 0.00593 S3 4 -0.057952 0.223198 0.876500 11.00000 0.02406 0.02041 = 0.02705 0.00390 0.00733 0.00629 S4 4 0.148420 0.364315 0.735796 11.00000 0.02755 0.02448 = 0.02739 0.00597 0.01033 0.01091 S5 4 0.395732 0.282824 0.917507 11.00000 0.02275 0.02044 = 0.03065 0.00014 0.00336 0.00111 S6 4 0.200748 0.017995 0.950817 11.00000 0.01913 0.02087 = 0.02656 0.00222 -0.00234 0.00156 N1 3 0.149998 -0.083304 0.548893 11.00000 0.02537 0.02869 = 0.02853 -0.00564 0.00720 0.00341 N2 3 -0.078020 0.438979 0.801068 11.00000 0.02759 0.02370 = 0.02694 0.00314 0.00718 0.01099 N3 3 0.447498 0.140496 1.056439 11.00000 0.01914 0.03050 = 0.02505 -0.00159 -0.00144 0.00087 C1 1 0.017916 -0.188193 0.511198 11.00000 0.02574 0.02836 = 0.02850 -0.00496 0.00208 0.00448 AFIX 23 H1A 2 -0.013114 -0.168194 0.447358 11.00000 -1.20000 H1B 2 -0.065130 -0.194722 0.554023 11.00000 -1.20000 AFIX 0 C2 1 0.053368 -0.316800 0.503927 11.00000 0.03790 0.02810 = 0.03004 0.00289 0.00177 0.00777 AFIX 23 H2A 2 -0.034162 -0.386235 0.475426 11.00000 -1.20000 H2B 2 0.075003 -0.340524 0.568672 11.00000 -1.20000 AFIX 0 C3 1 0.186440 -0.307815 0.442991 11.00000 0.03839 0.03289 = 0.03908 -0.00563 0.00187 0.01471 AFIX 23 H3A 2 0.160007 -0.296294 0.376026 11.00000 -1.20000 H3B 2 0.212959 -0.389925 0.444295 11.00000 -1.20000 AFIX 0 C4 1 0.319591 -0.193669 0.479765 11.00000 0.03073 0.04893 = 0.03080 -0.00645 0.00089 0.01612 AFIX 23 H4A 2 0.355190 -0.211355 0.543092 11.00000 -1.20000 H4B 2 0.401438 -0.184124 0.435558 11.00000 -1.20000 AFIX 0 C5 1 0.278156 -0.068079 0.488037 11.00000 0.02865 0.03695 = 0.03057 -0.00729 0.01063 0.00293 AFIX 23 H5A 2 0.363962 0.003629 0.515965 11.00000 -1.20000 H5B 2 0.252812 -0.045220 0.423764 11.00000 -1.20000 AFIX 0 C6 1 0.155603 -0.014852 0.630935 11.00000 0.02421 0.02057 = 0.02509 0.00242 0.00310 0.00853 C7 1 -0.022996 0.561755 0.753978 11.00000 0.04035 0.03067 = 0.03474 0.01254 0.01217 0.01968 AFIX 23 H7A 2 -0.097814 0.567996 0.705102 11.00000 -1.20000 H7B 2 0.069720 0.564279 0.721859 11.00000 -1.20000 AFIX 0 C8 1 0.006641 0.675281 0.828494 11.00000 0.03084 0.02364 = 0.04598 0.00883 0.00196 0.00946 AFIX 23 H8A 2 0.085307 0.671085 0.875260 11.00000 -1.20000 H8B 2 0.042382 0.758393 0.797171 11.00000 -1.20000 AFIX 0 C9 1 -0.133570 0.671592 0.880042 11.00000 0.03758 0.02646 = 0.03827 -0.00321 0.00134 0.01397 AFIX 23 H9A 2 -0.209018 0.684639 0.834479 11.00000 -1.20000 H9B 2 -0.110893 0.743077 0.930837 11.00000 -1.20000 AFIX 0 C10 1 -0.195098 0.541150 0.923905 11.00000 0.03312 0.03162 = 0.03479 -0.00310 0.00851 0.01289 AFIX 23 H10A 2 -0.125851 0.534273 0.976228 11.00000 -1.20000 H10B 2 -0.291731 0.536543 0.951498 11.00000 -1.20000 AFIX 0 C11 1 -0.216125 0.428186 0.850219 11.00000 0.02113 0.02637 = 0.03865 -0.00211 0.00578 0.00836 AFIX 23 H11A 2 -0.246484 0.345092 0.881972 11.00000 -1.20000 H11B 2 -0.296264 0.427391 0.802921 11.00000 -1.20000 AFIX 0 C12 1 -0.004032 0.352155 0.804296 11.00000 0.02313 0.02095 = 0.02005 -0.00075 0.00267 0.00610 C13 1 0.578811 0.249174 1.090025 11.00000 0.02168 0.03715 = 0.04355 -0.00597 -0.00876 -0.00065 AFIX 23 H13A 2 0.596349 0.319298 1.045088 11.00000 -1.20000 H13B 2 0.667742 0.218608 1.092928 11.00000 -1.20000 AFIX 0 C14 1 0.552664 0.301301 1.188558 11.00000 0.04350 0.04337 = 0.04701 -0.01754 -0.01923 0.01805 AFIX 23 H14A 2 0.643290 0.370541 1.213194 11.00000 -1.20000 H14B 2 0.470466 0.340406 1.183839 11.00000 -1.20000 AFIX 0 C15 1 0.514123 0.193898 1.257722 11.00000 0.07465 0.06366 = 0.02935 -0.01452 -0.01322 0.04013 AFIX 23 H15A 2 0.486778 0.228580 1.318905 11.00000 -1.20000 H15B 2 0.602367 0.164719 1.270622 11.00000 -1.20000 AFIX 0 C16 1 0.385565 0.078019 1.217760 11.00000 0.04824 0.05840 = 0.02662 0.00731 0.00788 0.02984 AFIX 23 H16A 2 0.370284 0.006001 1.260920 11.00000 -1.20000 H16B 2 0.293266 0.103572 1.214320 11.00000 -1.20000 AFIX 0 C17 1 0.417241 0.031780 1.119262 11.00000 0.02398 0.03534 = 0.02570 0.00221 -0.00075 0.00943 AFIX 23 H17A 2 0.504219 -0.001357 1.123293 11.00000 -1.20000 H17B 2 0.330613 -0.040257 1.092738 11.00000 -1.20000 AFIX 0 C18 1 0.358402 0.146815 0.983510 11.00000 0.01819 0.02302 = 0.02308 -0.00279 0.00458 0.00403 PART 1 N4 3 0.395719 0.419714 0.435169 10.31000 0.04871 C4A 1 0.395719 0.419714 0.435169 10.31000 0.04871 AFIX 3 H4AA 2 0.326739 0.365914 0.393969 10.31000 -1.20000 AFIX 0 C19 1 0.399464 0.394682 0.529997 10.62000 0.04276 AFIX 3 H19 2 0.326864 0.319802 0.549827 10.62000 -1.20000 AFIX 0 C20 1 0.502108 0.472705 0.596217 10.62000 0.05231 AFIX 3 H20 2 0.501868 0.451685 0.661027 10.62000 -1.20000 AFIX 0 PART 2 N5 3 0.480174 0.444425 0.579656 10.19000 0.05547 C5A 1 0.480174 0.444425 0.579656 10.19000 0.05547 AFIX 3 H5AA 2 0.463224 0.404815 0.634796 10.19000 -1.20000 AFIX 0 C21 1 0.390352 0.384020 0.503042 10.38000 0.04981 AFIX 3 H21 2 0.317562 0.302370 0.509092 10.38000 -1.20000 AFIX 0 C22 1 0.405388 0.440467 0.417121 10.38000 0.06119 AFIX 3 H22 2 0.345368 0.405287 0.360821 10.38000 -1.20000 PART 0 HKLF 4 REM sad in P-1 In(N,N-pentamethylenethiocarbamato)3.0.5py REM R1 = 0.0164 for 6176 Fo > 4sig(Fo) and 0.0176 for all 6491 data REM 277 parameters refined using 0 restraints END WGHT 0.0173 0.4951 REM Highest difference peak 0.379, deepest hole -0.480, 1-sigma level 0.051 Q1 1 0.4102 0.4659 0.3617 11.00000 0.05 0.38 Q2 1 0.3537 0.3792 0.4114 11.00000 0.05 0.32 Q3 1 0.3739 0.1996 0.9550 11.00000 0.05 0.28 Q4 1 -0.0626 0.6787 0.8505 11.00000 0.05 0.28 Q5 1 -0.1478 0.4296 0.8271 11.00000 0.05 0.27 Q6 1 -0.2081 0.4795 0.8908 11.00000 0.05 0.27 Q7 1 0.1124 -0.3107 0.4734 11.00000 0.05 0.25 Q8 1 -0.0110 0.6205 0.7884 11.00000 0.05 0.25 Q9 1 0.4407 0.4600 0.4587 11.00000 0.05 0.25 Q10 1 0.4481 0.1444 1.2271 11.00000 0.05 0.24 Q11 1 -0.1691 0.6019 0.8960 11.00000 0.05 0.24 Q12 1 0.2113 -0.0731 0.5180 11.00000 0.05 0.24 Q13 1 0.1785 0.0494 0.9067 11.00000 0.05 0.24 Q14 1 0.1514 0.1851 0.7717 11.00000 0.05 0.24 Q15 1 0.3913 0.0607 1.1687 11.00000 0.05 0.24 Q16 1 0.5629 0.2777 1.1375 11.00000 0.05 0.23 Q17 1 0.4919 0.1998 1.0715 11.00000 0.05 0.23 Q18 1 -0.0332 0.4053 0.8146 11.00000 0.05 0.22 Q19 1 0.2832 0.0839 0.9675 11.00000 0.05 0.22 Q20 1 0.0459 0.3516 0.7580 11.00000 0.05 0.22 ; _database_code_depnum_ccdc_archive 'CCDC 924190'