# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Angeles Monge' _publ_contact_author_email amonge@icmm.csic.es loop_ _publ_author_name A.Monge N.Snejko E.Gutierrez-Puebla A.Platero M.Medina ; M.Bernini ; E.Lopez-Torres # Attachment 'CE-ART-02-2011-005196.R4-in1.cif' data_in1 _database_code_depnum_ccdc_archive 'CCDC 812721' #TrackingRef 'CE-ART-02-2011-005196.R4-in1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H42 In2 N4 O13' _chemical_formula_weight 1328.84 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' O O 0.0106 0.0060 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.835(2) _cell_length_b 13.839(3) _cell_length_c 21.881(5) _cell_angle_alpha 96.492(4) _cell_angle_beta 100.320(5) _cell_angle_gamma 104.967(4) _cell_volume 2790.5(10) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 2668 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 20.34 _exptl_crystal_description cubic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 0.899 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.764 _exptl_absorpt_correction_T_max 0.835 _exptl_absorpt_process_details sadabs _exptl_special_details ; After meassuring different crystals, we can conclude that all of them diffract poorly, it seems to be something inherent to these crystals. For this reason the data have less completeness than the usual and the alert The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.4999 is also due to this reason.In the total chem sum there are two hydrogen atoms from O water solvent molecule which have not been taken into account due to the partial occupancy of the Oxygen atom from the water solvent molecule ; _diffrn_ambient_temperature 295(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12374 _diffrn_reflns_av_R_equivalents 0.1929 _diffrn_reflns_av_sigmaI/netI 0.1750 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 0.96 _diffrn_reflns_theta_max 20.82 _reflns_number_total 5647 _reflns_number_gt 3656 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0884P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5647 _refine_ls_number_parameters 775 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1247 _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.2003 _refine_ls_wR_factor_gt 0.1614 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.002 _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 0.15001(10) 0.22663(7) 0.06088(5) 0.0345(4) Uani 1 1 d . . . In2 In 0.42124(10) 0.59408(7) 0.38465(5) 0.0341(4) Uani 1 1 d . . . O1 O 0.2644(10) 0.1468(7) 0.1411(5) 0.057(3) Uani 1 1 d . . . O2 O 0.0470(11) 0.0776(7) 0.0828(6) 0.054(3) Uani 1 1 d . . . O3 O -0.2924(11) -0.1505(9) -0.0131(6) 0.064(3) Uani 1 1 d . . . O4 O -0.1005(12) -0.1681(7) 0.0447(5) 0.052(3) Uani 1 1 d . . . O5 O 0.3469(10) 0.3545(7) 0.1049(5) 0.057(3) Uani 1 1 d . . . O6 O 0.2024(12) 0.3974(8) 0.0362(6) 0.079(4) Uani 1 1 d . . . O7 O 0.3714(10) 0.5489(7) 0.2752(5) 0.043(3) Uani 1 1 d . . . O8 O 0.2394(10) 0.6239(8) 0.3223(5) 0.047(3) Uani 1 1 d . . . O9 O 0.2223(12) 0.4913(8) 0.4227(6) 0.068(4) Uani 1 1 d . . . O10 O 0.3837(11) 0.4319(7) 0.3899(5) 0.041(3) Uani 1 1 d . . . O11 O 0.6590(12) 0.2703(8) 0.5360(5) 0.057(3) Uani 1 1 d . . . O12 O 0.4927(10) 0.3527(8) 0.5176(5) 0.043(3) Uani 1 1 d . . . N1 N 0.0765(13) 0.2839(8) 0.1501(6) 0.034(3) Uani 1 1 d . . . N2 N -0.0836(12) 0.2365(9) 0.0308(7) 0.042(3) Uani 1 1 d . . . N3 N 0.5505(13) 0.7496(9) 0.3680(6) 0.044(3) Uani 1 1 d . . . N4 N 0.6531(12) 0.5869(9) 0.3823(6) 0.038(3) Uani 1 1 d . . . C1 C 0.1474(18) 0.0765(11) 0.1264(8) 0.036(4) Uani 1 1 d . . . C2 C 0.1327(16) -0.0135(10) 0.1614(7) 0.041(4) Uani 1 1 d . . . C3 C 0.2624(16) -0.0348(12) 0.1851(8) 0.055(5) Uani 1 1 d . . . H3 H 0.3505 0.0036 0.1795 0.066 Uiso 1 1 calc R . . C4 C 0.2519(18) -0.1164(12) 0.2175(7) 0.049(5) Uani 1 1 d . . . H4 H 0.3350 -0.1346 0.2322 0.059 Uiso 1 1 calc R . . C5 C 0.123(2) -0.1711(13) 0.2287(9) 0.073(6) Uani 1 1 d . . . H5 H 0.1205 -0.2234 0.2521 0.087 Uiso 1 1 calc R . . C6 C 0.002(2) -0.1479(11) 0.2051(8) 0.057(5) Uani 1 1 d . . . H6 H -0.0851 -0.1858 0.2124 0.068 Uiso 1 1 calc R . . C7 C -0.0001(16) -0.0693(11) 0.1701(7) 0.042(4) Uani 1 1 d . . . C8 C -0.1366(16) -0.0427(11) 0.1506(9) 0.042(4) Uani 1 1 d . . . C9 C -0.2280(17) -0.0671(11) 0.0922(10) 0.053(5) Uani 1 1 d . . . C10 C -0.3502(17) -0.0291(13) 0.0834(10) 0.063(6) Uani 1 1 d . . . H10 H -0.4118 -0.0436 0.0439 0.076 Uiso 1 1 calc R . . C11 C -0.380(2) 0.0300(13) 0.1333(12) 0.070(6) Uani 1 1 d . . . H11 H -0.4612 0.0529 0.1273 0.084 Uiso 1 1 calc R . . C12 C -0.291(2) 0.0523(14) 0.1880(11) 0.078(6) Uani 1 1 d . . . H12 H -0.3084 0.0923 0.2210 0.094 Uiso 1 1 calc R . . C13 C -0.169(2) 0.0171(13) 0.1982(9) 0.066(6) Uani 1 1 d . . . H66 H -0.1073 0.0342 0.2378 0.079 Uiso 1 1 calc R . . C14 C -0.2049(18) -0.1357(12) 0.0378(8) 0.039(4) Uani 1 1 d . . . C15 C 0.3076(16) 0.4207(11) 0.0789(8) 0.037(4) Uani 1 1 d . . . C16 C 0.3983(14) 0.5299(10) 0.1041(6) 0.028(4) Uani 1 1 d . . . C17 C 0.5346(17) 0.5616(12) 0.0916(8) 0.055(5) Uani 1 1 d . . . H16 H 0.5678 0.5173 0.0669 0.066 Uiso 1 1 calc R . . C18 C 0.6213(16) 0.6594(13) 0.1160(8) 0.052(5) Uani 1 1 d . . . H17 H 0.7073 0.6837 0.1032 0.063 Uiso 1 1 calc R . . C19 C 0.5798(17) 0.7219(11) 0.1599(7) 0.044(4) Uani 1 1 d . . . H18 H 0.6419 0.7844 0.1805 0.053 Uiso 1 1 calc R . . C20 C 0.4473(17) 0.6882(11) 0.1710(7) 0.043(4) Uani 1 1 d . . . H19 H 0.4184 0.7308 0.1988 0.051 Uiso 1 1 calc R . . C21 C 0.3481(15) 0.5925(11) 0.1435(7) 0.034(4) Uani 1 1 d . . . C22 C 0.2000(14) 0.5714(10) 0.1526(8) 0.036(4) Uani 1 1 d . . . C23 C 0.0882(16) 0.5581(10) 0.0985(7) 0.044(4) Uani 1 1 d . . . H22 H 0.1095 0.5568 0.0588 0.052 Uiso 1 1 calc R . . C24 C -0.0498(17) 0.5474(11) 0.1049(9) 0.051(5) Uani 1 1 d . . . H23 H -0.1208 0.5374 0.0685 0.062 Uiso 1 1 calc R . . C25 C -0.0913(16) 0.5504(12) 0.1627(9) 0.055(5) Uani 1 1 d . . . H24 H -0.1859 0.5452 0.1659 0.065 Uiso 1 1 calc R . . C26 C 0.0187(16) 0.5617(10) 0.2151(8) 0.041(4) Uani 1 1 d . . . H25 H -0.0037 0.5622 0.2547 0.049 Uiso 1 1 calc R . . C27 C 0.1623(14) 0.5725(10) 0.2105(8) 0.033(4) Uani 1 1 d . . . C28 C 0.2637(15) 0.5800(11) 0.2727(7) 0.034(4) Uani 1 1 d . . . C29 C 0.1568(19) 0.3068(11) 0.2086(8) 0.053(5) Uani 1 1 d . . . H28 H 0.2537 0.3092 0.2147 0.063 Uiso 1 1 calc R . . C30 C 0.101(2) 0.3269(11) 0.2602(8) 0.055(5) Uani 1 1 d . . . H29 H 0.1589 0.3392 0.3003 0.066 Uiso 1 1 calc R . . C31 C -0.040(2) 0.3294(12) 0.2536(9) 0.066(6) Uani 1 1 d . . . H30 H -0.0769 0.3455 0.2885 0.079 Uiso 1 1 calc R . . C32 C -0.1253(19) 0.3068(11) 0.1929(9) 0.049(5) Uani 1 1 d . . . C33 C -0.0612(18) 0.2847(10) 0.1426(8) 0.042(4) Uani 1 1 d . . . C34 C -0.270(2) 0.3066(13) 0.1811(12) 0.084(7) Uani 1 1 d . . . H33 H -0.3127 0.3180 0.2147 0.101 Uiso 1 1 calc R . . C35 C -0.351(2) 0.2895(14) 0.1197(12) 0.080(7) Uani 1 1 d . . . H34 H -0.4447 0.2944 0.1124 0.096 Uiso 1 1 calc R . . C36 C -0.2875(17) 0.2642(11) 0.0674(9) 0.050(5) Uani 1 1 d . . . C37 C -0.1455(16) 0.2623(10) 0.0788(8) 0.035(4) Uani 1 1 d . . . C38 C -0.3671(19) 0.2408(13) 0.0041(12) 0.073(7) Uani 1 1 d . . . H37 H -0.4629 0.2413 -0.0053 0.087 Uiso 1 1 calc R . . C39 C -0.2997(19) 0.2176(14) -0.0425(10) 0.067(6) Uani 1 1 d . . . H38 H -0.3496 0.2028 -0.0843 0.080 Uiso 1 1 calc R . . C40 C -0.1571(17) 0.2158(12) -0.0279(8) 0.057(5) Uani 1 1 d . . . H39 H -0.1128 0.1997 -0.0602 0.068 Uiso 1 1 calc R . . C41 C 0.2730(18) 0.4194(14) 0.4138(8) 0.054(5) Uani 1 1 d . . . C42 C 0.2111(16) 0.3147(12) 0.4282(8) 0.050(5) Uani 1 1 d . . . C43 C 0.0862(17) 0.3051(14) 0.4526(7) 0.052(5) Uani 1 1 d . . . H42 H 0.0488 0.3601 0.4577 0.063 Uiso 1 1 calc R . . C44 C 0.0194(18) 0.2149(16) 0.4690(9) 0.069(6) Uani 1 1 d . . . H43 H -0.0618 0.2085 0.4861 0.082 Uiso 1 1 calc R . . C45 C 0.074(2) 0.1349(15) 0.4598(10) 0.081(7) Uani 1 1 d . . . H44 H 0.0291 0.0739 0.4714 0.098 Uiso 1 1 calc R . . C46 C 0.1917(19) 0.1412(12) 0.4343(8) 0.057(5) Uani 1 1 d . . . H45 H 0.2231 0.0839 0.4271 0.069 Uiso 1 1 calc R . . C47 C 0.2682(16) 0.2349(11) 0.4184(6) 0.036(4) Uani 1 1 d . . . C48 C 0.3980(16) 0.2358(11) 0.3939(9) 0.040(4) Uani 1 1 d . . . C49 C 0.379(2) 0.2025(12) 0.3313(10) 0.065(6) Uani 1 1 d . . . H48 H 0.2865 0.1864 0.3059 0.078 Uiso 1 1 calc R . . C50 C 0.496(2) 0.1914(13) 0.3030(9) 0.072(6) Uani 1 1 d . . . H49 H 0.4812 0.1707 0.2598 0.086 Uiso 1 1 calc R . . C51 C 0.628(2) 0.2116(12) 0.3404(10) 0.065(5) Uani 1 1 d . . . H50 H 0.7056 0.2053 0.3230 0.078 Uiso 1 1 calc R . . C52 C 0.6477(18) 0.2412(11) 0.4035(9) 0.052(5) Uani 1 1 d . . . H51 H 0.7376 0.2517 0.4297 0.063 Uiso 1 1 calc R . . C53 C 0.5317(16) 0.2559(10) 0.4293(7) 0.039(4) Uani 1 1 d . . . C54 C 0.5642(17) 0.2947(12) 0.4997(8) 0.043(4) Uani 1 1 d . . . C55 C 0.5007(18) 0.8285(12) 0.3640(8) 0.056(5) Uani 1 1 d . . . H54 H 0.4054 0.8216 0.3666 0.068 Uiso 1 1 calc R . . C56 C 0.585(3) 0.9227(14) 0.3559(9) 0.081(7) Uani 1 1 d . . . H55 H 0.5459 0.9765 0.3515 0.097 Uiso 1 1 calc R . . C57 C 0.731(2) 0.9335(15) 0.3547(10) 0.081(7) Uani 1 1 d . . . H56 H 0.7892 0.9957 0.3501 0.097 Uiso 1 1 calc R . . C58 C 0.789(2) 0.8516(15) 0.3604(9) 0.071(6) Uani 1 1 d . . . C59 C 0.6930(18) 0.7601(12) 0.3673(8) 0.055(5) Uani 1 1 d . . . C60 C 0.939(2) 0.8567(17) 0.3618(10) 0.098(9) Uani 1 1 d . . . H59 H 1.0026 0.9160 0.3560 0.117 Uiso 1 1 calc R . . C61 C 0.985(2) 0.7781(18) 0.3712(10) 0.088(7) Uani 1 1 d . . . H60 H 1.0832 0.7853 0.3748 0.106 Uiso 1 1 calc R . . C62 C 0.8948(17) 0.6818(14) 0.3764(7) 0.052(5) Uani 1 1 d . . . C63 C 0.7459(16) 0.6734(13) 0.3746(7) 0.047(4) Uani 1 1 d . . . C64 C 0.9363(18) 0.5934(15) 0.3848(8) 0.066(6) Uani 1 1 d . . . H63 H 1.0308 0.5937 0.3844 0.080 Uiso 1 1 calc R . . C65 C 0.844(2) 0.5090(15) 0.3933(8) 0.065(5) Uani 1 1 d . . . H64 H 0.8740 0.4519 0.3999 0.078 Uiso 1 1 calc R . . C66 C 0.7036(18) 0.5085(13) 0.3919(8) 0.064(5) Uani 1 1 d . . . H65 H 0.6401 0.4496 0.3982 0.077 Uiso 1 1 calc R . . O40 O 0.335(2) 0.9332(13) 0.4775(12) 0.064(7) Uani 0.50 1 d P . . O41 O 0.564(3) 0.449(2) 0.2334(12) 0.104(11) Uani 0.50 1 d P . . 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 0.0259(6) 0.0357(7) 0.0388(8) 0.0079(6) 0.0013(5) 0.0066(5) In2 0.0310(7) 0.0328(7) 0.0365(8) 0.0055(5) 0.0001(5) 0.0109(5) O1 0.035(7) 0.038(6) 0.094(10) 0.031(6) 0.008(6) -0.002(6) O2 0.031(6) 0.055(7) 0.075(9) 0.015(6) -0.001(6) 0.020(6) O3 0.045(7) 0.088(9) 0.053(9) 0.015(7) 0.003(7) 0.015(6) O4 0.050(7) 0.054(7) 0.059(9) -0.003(6) 0.013(6) 0.033(6) O5 0.048(7) 0.033(6) 0.087(10) 0.020(6) 0.002(6) 0.012(6) O6 0.058(8) 0.053(8) 0.101(11) 0.003(7) -0.027(8) 0.005(7) O7 0.043(7) 0.042(6) 0.046(8) 0.006(5) 0.001(6) 0.022(5) O8 0.036(6) 0.056(7) 0.038(8) -0.011(6) -0.003(6) 0.011(5) O9 0.060(8) 0.046(7) 0.104(11) 0.016(7) 0.017(7) 0.025(7) O10 0.034(6) 0.032(6) 0.042(7) -0.002(5) -0.004(6) -0.002(5) O11 0.062(8) 0.055(7) 0.049(8) 0.016(6) -0.006(6) 0.019(6) O12 0.040(6) 0.054(7) 0.027(7) -0.004(5) 0.002(5) 0.012(6) N1 0.044(8) 0.037(8) 0.023(9) -0.007(6) 0.009(7) 0.021(6) N2 0.032(7) 0.047(8) 0.044(10) 0.018(7) -0.003(8) 0.010(6) N3 0.043(9) 0.039(8) 0.046(10) 0.013(7) 0.004(7) 0.009(7) N4 0.039(8) 0.049(8) 0.034(9) 0.018(7) 0.016(6) 0.016(7) C1 0.044(11) 0.038(10) 0.041(12) 0.003(9) 0.038(9) 0.019(9) C2 0.049(11) 0.026(9) 0.045(11) 0.010(8) 0.014(9) 0.002(8) C3 0.037(10) 0.050(11) 0.079(15) 0.009(10) 0.009(10) 0.018(9) C4 0.060(13) 0.041(11) 0.049(13) 0.006(10) -0.002(10) 0.029(10) C5 0.089(15) 0.040(11) 0.081(17) 0.034(11) -0.017(13) 0.018(11) C6 0.078(14) 0.038(10) 0.039(12) 0.006(9) 0.019(10) -0.014(10) C7 0.054(11) 0.038(10) 0.040(11) 0.020(9) 0.020(9) 0.010(9) C8 0.045(11) 0.024(9) 0.068(14) -0.001(9) 0.038(11) 0.015(8) C9 0.039(11) 0.027(10) 0.085(17) 0.034(11) -0.006(11) -0.003(8) C10 0.038(11) 0.064(13) 0.079(16) 0.025(12) 0.008(10) -0.005(10) C11 0.067(14) 0.049(12) 0.10(2) 0.005(13) 0.028(14) 0.029(11) C12 0.088(16) 0.066(14) 0.066(17) -0.026(12) 0.029(13) 0.005(13) C13 0.062(13) 0.051(12) 0.076(17) 0.016(12) 0.006(12) 0.004(10) C14 0.033(10) 0.040(11) 0.035(12) 0.003(9) 0.027(10) -0.016(9) C15 0.037(10) 0.029(10) 0.047(12) -0.006(9) 0.011(9) 0.019(9) C16 0.029(9) 0.044(10) 0.010(9) 0.015(8) -0.003(7) 0.008(8) C17 0.048(11) 0.042(11) 0.078(15) 0.024(10) 0.017(10) 0.011(9) C18 0.041(10) 0.070(13) 0.042(13) 0.028(10) 0.007(9) 0.005(10) C19 0.051(12) 0.039(10) 0.033(12) -0.001(9) 0.003(9) 0.003(9) C20 0.048(11) 0.038(10) 0.030(11) -0.002(8) -0.001(9) 0.002(9) C21 0.045(10) 0.038(10) 0.029(10) 0.014(8) 0.004(8) 0.028(9) C22 0.024(9) 0.023(8) 0.055(13) 0.016(8) -0.001(9) 0.001(7) C23 0.045(11) 0.050(10) 0.027(11) 0.008(8) -0.013(9) 0.012(8) C24 0.042(12) 0.052(11) 0.057(14) 0.007(10) -0.006(10) 0.022(9) C25 0.022(9) 0.073(13) 0.067(15) 0.018(11) -0.002(10) 0.017(9) C26 0.049(11) 0.030(9) 0.054(12) 0.023(8) 0.022(10) 0.013(8) C27 0.027(9) 0.032(9) 0.051(13) 0.006(8) 0.024(9) 0.015(7) C28 0.024(9) 0.037(10) 0.031(12) -0.001(8) -0.015(8) 0.006(8) C29 0.068(12) 0.051(11) 0.024(12) -0.019(9) -0.018(11) 0.018(9) C30 0.096(16) 0.042(11) 0.025(12) -0.001(9) 0.004(11) 0.023(11) C31 0.114(18) 0.049(12) 0.040(15) -0.006(10) 0.033(13) 0.025(12) C32 0.065(13) 0.031(10) 0.054(15) 0.000(9) 0.037(12) 0.004(9) C33 0.063(12) 0.021(9) 0.038(13) 0.004(8) 0.007(10) 0.011(8) C34 0.096(18) 0.051(12) 0.14(3) 0.030(14) 0.068(17) 0.050(13) C35 0.052(13) 0.088(16) 0.11(2) 0.029(15) 0.025(15) 0.034(12) C36 0.039(11) 0.040(10) 0.071(15) 0.007(9) 0.028(11) 0.003(8) C37 0.040(10) 0.043(10) 0.033(11) 0.010(8) 0.008(9) 0.027(8) C38 0.035(11) 0.069(13) 0.11(2) 0.033(13) -0.015(14) 0.014(10) C39 0.048(13) 0.074(14) 0.071(17) 0.031(12) -0.006(12) 0.011(10) C40 0.049(12) 0.080(13) 0.036(13) 0.018(10) -0.010(10) 0.018(10) C41 0.038(11) 0.068(14) 0.053(13) 0.032(11) -0.001(10) 0.009(10) C42 0.029(9) 0.048(11) 0.074(14) 0.022(10) 0.008(9) 0.006(8) C43 0.043(11) 0.094(15) 0.021(11) 0.032(10) 0.000(8) 0.018(10) C44 0.044(11) 0.101(16) 0.063(15) 0.040(13) 0.017(10) 0.008(12) C45 0.049(13) 0.068(15) 0.11(2) 0.053(14) -0.004(13) -0.012(11) C46 0.054(12) 0.029(10) 0.080(15) -0.007(9) 0.017(11) 0.000(9) C47 0.051(11) 0.037(10) 0.017(10) -0.003(7) -0.010(8) 0.022(9) C48 0.030(10) 0.031(9) 0.057(14) 0.011(9) 0.000(10) 0.008(8) C49 0.060(13) 0.058(12) 0.063(16) 0.007(11) -0.028(12) 0.021(10) C50 0.105(17) 0.059(13) 0.054(15) -0.008(10) 0.019(15) 0.036(13) C51 0.070(14) 0.062(13) 0.063(17) 0.000(11) 0.020(12) 0.018(11) C52 0.066(13) 0.054(11) 0.046(14) 0.002(10) 0.013(10) 0.035(10) C53 0.042(10) 0.039(9) 0.037(12) -0.004(8) 0.002(9) 0.021(8) C54 0.034(10) 0.039(10) 0.051(14) 0.016(10) -0.002(10) 0.004(8) C55 0.065(12) 0.038(11) 0.072(14) 0.033(10) 0.007(10) 0.019(10) C56 0.13(2) 0.054(14) 0.069(16) 0.027(11) 0.023(15) 0.039(14) C57 0.100(18) 0.052(13) 0.092(18) 0.034(12) 0.032(14) 0.008(13) C58 0.062(13) 0.063(14) 0.079(16) 0.037(12) 0.015(11) -0.007(12) C59 0.060(13) 0.044(11) 0.066(14) 0.036(10) 0.016(10) 0.011(10) C60 0.088(19) 0.088(18) 0.10(2) 0.052(16) 0.039(15) -0.032(14) C61 0.053(13) 0.115(19) 0.078(18) 0.027(15) 0.023(12) -0.020(15) C62 0.039(11) 0.078(14) 0.036(12) 0.006(10) 0.005(8) 0.014(11) C63 0.040(11) 0.064(12) 0.031(11) 0.009(9) 0.005(8) 0.006(10) C64 0.047(12) 0.094(16) 0.071(16) 0.021(13) 0.032(11) 0.026(12) C65 0.072(14) 0.081(15) 0.065(15) 0.031(11) 0.033(11) 0.044(12) C66 0.055(13) 0.071(13) 0.086(16) 0.023(11) 0.026(11) 0.040(11) O40 0.069(15) 0.022(11) 0.12(2) 0.024(12) 0.023(14) 0.035(11) O41 0.12(2) 0.19(3) 0.07(2) 0.030(19) 0.030(17) 0.14(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag In1 O2 2.198(10) . ? In1 O5 2.233(9) . ? In1 O4 2.279(11) 2 ? In1 O3 2.282(12) 2 ? In1 N2 2.318(11) . ? In1 N1 2.326(11) . ? In1 O6 2.429(11) . ? In1 O1 2.437(10) . ? In1 C14 2.587(17) 2 ? In1 C1 2.651(15) . ? In1 C15 2.676(14) . ? In2 O12 2.124(9) 2_666 ? In2 O10 2.198(9) . ? In2 O8 2.205(9) . ? In2 N3 2.304(12) . ? In2 N4 2.318(12) . ? In2 O7 2.334(10) . ? In2 O9 2.441(11) . ? In2 C28 2.610(14) . ? In2 C41 2.690(17) . ? O1 C1 1.262(16) . ? O2 C1 1.247(17) . ? O3 C14 1.239(17) . ? O3 In1 2.282(12) 2 ? O4 C14 1.215(17) . ? O4 In1 2.279(11) 2 ? O5 C15 1.239(15) . ? O6 C15 1.209(16) . ? O7 C28 1.237(16) . ? O8 C28 1.274(17) . ? O9 C41 1.234(19) . ? O10 C41 1.271(19) . ? O11 C54 1.254(16) . ? O12 C54 1.270(18) . ? O12 In2 2.124(9) 2_666 ? N1 C29 1.335(17) . ? N1 C33 1.337(18) . ? N2 C40 1.316(18) . ? N2 C37 1.363(18) . ? N3 C55 1.312(17) . ? N3 C59 1.375(19) . ? N4 C66 1.327(17) . ? N4 C63 1.354(17) . ? C1 C2 1.524(19) . ? C2 C7 1.392(19) . ? C2 C3 1.405(19) . ? C3 C4 1.39(2) . ? C3 H3 0.9300 . ? C4 C5 1.37(2) . ? C4 H4 0.9300 . ? C5 C6 1.35(2) . ? C5 H5 0.9300 . ? C6 C7 1.401(19) . ? C6 H6 0.9300 . ? C7 C8 1.48(2) . ? C8 C9 1.37(2) . ? C8 C13 1.39(2) . ? C9 C10 1.42(2) . ? C9 C14 1.52(2) . ? C10 C11 1.41(2) . ? C10 H10 0.9300 . ? C11 C12 1.30(2) . ? C11 H11 0.9300 . ? C12 C13 1.40(2) . ? C12 H12 0.9300 . ? C13 H66 0.9300 . ? C14 In1 2.587(17) 2 ? C15 C16 1.524(19) . ? C16 C17 1.386(19) . ? C16 C21 1.393(19) . ? C17 C18 1.39(2) . ? C17 H16 0.9300 . ? C18 C19 1.40(2) . ? C18 H17 0.9300 . ? C19 C20 1.34(2) . ? C19 H18 0.9300 . ? C20 C21 1.418(19) . ? C20 H19 0.9300 . ? C21 C22 1.46(2) . ? C22 C27 1.381(19) . ? C22 C23 1.423(18) . ? C23 C24 1.36(2) . ? C23 H22 0.9300 . ? C24 C25 1.40(2) . ? C24 H23 0.9300 . ? C25 C26 1.393(19) . ? C25 H24 0.9300 . ? C26 C27 1.405(18) . ? C26 H25 0.9300 . ? C27 C28 1.512(19) . ? C29 C30 1.37(2) . ? C29 H28 0.9300 . ? C30 C31 1.37(2) . ? C30 H29 0.9300 . ? C31 C32 1.39(2) . ? C31 H30 0.9300 . ? C32 C34 1.40(2) . ? C32 C33 1.41(2) . ? C33 C37 1.45(2) . ? C34 C35 1.39(3) . ? C34 H33 0.9300 . ? C35 C36 1.45(3) . ? C35 H34 0.9300 . ? C36 C37 1.38(2) . ? C36 C38 1.42(2) . ? C38 C39 1.36(3) . ? C38 H37 0.9300 . ? C39 C40 1.39(2) . ? C39 H38 0.9300 . ? C40 H39 0.9300 . ? C41 C42 1.51(2) . ? C42 C47 1.376(19) . ? C42 C43 1.41(2) . ? C43 C44 1.37(2) . ? C43 H42 0.9300 . ? C44 C45 1.36(2) . ? C44 H43 0.9300 . ? C45 C46 1.36(2) . ? C45 H44 0.9300 . ? C46 C47 1.43(2) . ? C46 H45 0.9300 . ? C47 C48 1.47(2) . ? C48 C53 1.343(19) . ? C48 C49 1.36(2) . ? C49 C50 1.44(3) . ? C49 H48 0.9300 . ? C50 C51 1.35(2) . ? C50 H49 0.9300 . ? C51 C52 1.36(2) . ? C51 H50 0.9300 . ? C52 C53 1.41(2) . ? C52 H51 0.9300 . ? C53 C54 1.52(2) . ? C55 C56 1.40(2) . ? C55 H54 0.9300 . ? C56 C57 1.41(2) . ? C56 H55 0.9300 . ? C57 C58 1.40(2) . ? C57 H56 0.9300 . ? C58 C59 1.41(2) . ? C58 C60 1.46(3) . ? C59 C63 1.44(2) . ? C60 C61 1.30(3) . ? C60 H59 0.9300 . ? C61 C62 1.43(2) . ? C61 H60 0.9300 . ? C62 C64 1.41(2) . ? C62 C63 1.43(2) . ? C64 C65 1.34(2) . ? C64 H63 0.9300 . ? C65 C66 1.37(2) . ? C65 H64 0.9300 . ? C66 H65 0.9300 . ? 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 O2 In1 O5 135.8(4) . . ? O2 In1 O4 93.3(4) . 2 ? O5 In1 O4 119.9(4) . 2 ? O2 In1 O3 87.4(4) . 2 ? O5 In1 O3 88.1(4) . 2 ? O4 In1 O3 56.6(4) 2 2 ? O2 In1 N2 84.8(4) . . ? O5 In1 N2 127.0(4) . . ? O4 In1 N2 78.7(5) 2 . ? O3 In1 N2 134.0(5) 2 . ? O2 In1 N1 82.3(4) . . ? O5 In1 N1 81.3(4) . . ? O4 In1 N1 150.0(4) 2 . ? O3 In1 N1 151.7(4) 2 . ? N2 In1 N1 71.3(5) . . ? O2 In1 O6 165.1(4) . . ? O5 In1 O6 54.0(3) . . ? O4 In1 O6 87.7(4) 2 . ? O3 In1 O6 105.4(4) 2 . ? N2 In1 O6 80.8(4) . . ? N1 In1 O6 89.4(4) . . ? O2 In1 O1 56.1(3) . . ? O5 In1 O1 80.3(4) . . ? O4 In1 O1 124.1(4) 2 . ? O3 In1 O1 74.8(4) 2 . ? N2 In1 O1 132.9(4) . . ? N1 In1 O1 77.6(4) . . ? O6 In1 O1 134.0(4) . . ? O2 In1 C14 89.0(4) . 2 ? O5 In1 C14 106.6(4) . 2 ? O4 In1 C14 28.0(4) 2 2 ? O3 In1 C14 28.6(4) 2 2 ? N2 In1 C14 105.9(6) . 2 ? N1 In1 C14 171.1(4) . 2 ? O6 In1 C14 98.6(5) . 2 ? O1 In1 C14 99.4(5) . 2 ? O2 In1 C1 27.9(4) . . ? O5 In1 C1 108.2(5) . . ? O4 In1 C1 111.1(4) 2 . ? O3 In1 C1 80.9(4) 2 . ? N2 In1 C1 108.9(4) . . ? N1 In1 C1 77.7(4) . . ? O6 In1 C1 159.9(5) . . ? O1 In1 C1 28.3(4) . . ? C14 In1 C1 95.6(5) 2 . ? O2 In1 C15 159.5(5) . . ? O5 In1 C15 27.4(4) . . ? O4 In1 C15 106.8(4) 2 . ? O3 In1 C15 100.0(4) 2 . ? N2 In1 C15 102.8(4) . . ? N1 In1 C15 82.2(4) . . ? O6 In1 C15 26.8(4) . . ? O1 In1 C15 107.1(4) . . ? C14 In1 C15 106.7(4) 2 . ? C1 In1 C15 134.2(5) . . ? O12 In2 O10 96.2(4) 2_666 . ? O12 In2 O8 129.4(4) 2_666 . ? O10 In2 O8 112.1(4) . . ? O12 In2 N3 87.1(4) 2_666 . ? O10 In2 N3 154.4(5) . . ? O8 In2 N3 84.2(4) . . ? O12 In2 N4 84.2(4) 2_666 . ? O10 In2 N4 82.9(4) . . ? O8 In2 N4 138.2(4) . . ? N3 In2 N4 72.1(4) . . ? O12 In2 O7 169.1(4) 2_666 . ? O10 In2 O7 87.6(3) . . ? O8 In2 O7 57.4(4) . . ? N3 In2 O7 85.2(4) . . ? N4 In2 O7 86.1(4) . . ? O12 In2 O9 82.7(4) 2_666 . ? O10 In2 O9 55.2(4) . . ? O8 In2 O9 80.8(4) . . ? N3 In2 O9 150.1(4) . . ? N4 In2 O9 134.0(4) . . ? O7 In2 O9 107.7(4) . . ? O12 In2 C28 158.1(5) 2_666 . ? O10 In2 C28 99.4(4) . . ? O8 In2 C28 29.2(4) . . ? N3 In2 C28 85.5(4) . . ? N4 In2 C28 112.9(5) . . ? O7 In2 C28 28.3(4) . . ? O9 In2 C28 93.6(4) . . ? O12 In2 C41 88.5(5) 2_666 . ? O10 In2 C41 27.9(5) . . ? O8 In2 C41 97.5(4) . . ? N3 In2 C41 175.4(5) . . ? N4 In2 C41 108.8(5) . . ? O7 In2 C41 99.3(5) . . ? O9 In2 C41 27.3(4) . . ? C28 In2 C41 98.1(4) . . ? C1 O1 In1 85.3(9) . . ? C1 O2 In1 96.7(9) . . ? C14 O3 In1 89.5(10) . 2 ? C14 O4 In1 90.2(10) . 2 ? C15 O5 In1 96.7(9) . . ? C15 O6 In1 88.1(9) . . ? C28 O7 In2 88.4(9) . . ? C28 O8 In2 93.3(8) . . ? C41 O9 In2 87.7(10) . . ? C41 O10 In2 98.1(10) . . ? C54 O12 In2 106.7(9) . 2_666 ? C29 N1 C33 117.6(14) . . ? C29 N1 In1 125.0(11) . . ? C33 N1 In1 117.0(10) . . ? C40 N2 C37 120.4(13) . . ? C40 N2 In1 124.0(12) . . ? C37 N2 In1 115.5(9) . . ? C55 N3 C59 119.2(13) . . ? C55 N3 In2 124.8(11) . . ? C59 N3 In2 115.8(9) . . ? C66 N4 C63 118.2(13) . . ? C66 N4 In2 125.7(11) . . ? C63 N4 In2 115.9(10) . . ? O2 C1 O1 121.7(14) . . ? O2 C1 C2 119.9(14) . . ? O1 C1 C2 118.4(14) . . ? O2 C1 In1 55.4(7) . . ? O1 C1 In1 66.4(8) . . ? C2 C1 In1 175.2(12) . . ? C7 C2 C3 122.6(14) . . ? C7 C2 C1 122.0(14) . . ? C3 C2 C1 115.3(14) . . ? C4 C3 C2 116.5(15) . . ? C4 C3 H3 121.8 . . ? C2 C3 H3 121.8 . . ? C5 C4 C3 122.5(15) . . ? C5 C4 H4 118.8 . . ? C3 C4 H4 118.8 . . ? C6 C5 C4 119.0(15) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C5 C6 C7 123.0(16) . . ? C5 C6 H6 118.5 . . ? C7 C6 H6 118.5 . . ? C2 C7 C6 116.4(14) . . ? C2 C7 C8 123.6(13) . . ? C6 C7 C8 119.6(15) . . ? C9 C8 C13 118.4(16) . . ? C9 C8 C7 128.1(16) . . ? C13 C8 C7 113.5(17) . . ? C8 C9 C10 118.4(18) . . ? C8 C9 C14 122.1(15) . . ? C10 C9 C14 119.4(17) . . ? C11 C10 C9 121.2(18) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C12 C11 C10 118.9(18) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C11 C12 C13 121.3(19) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C8 C13 C12 121.7(18) . . ? C8 C13 H66 119.1 . . ? C12 C13 H66 119.1 . . ? O4 C14 O3 123.4(16) . . ? O4 C14 C9 120.1(15) . . ? O3 C14 C9 116.4(16) . . ? O4 C14 In1 61.8(9) . 2 ? O3 C14 In1 61.9(9) . 2 ? C9 C14 In1 171.2(10) . 2 ? O6 C15 O5 120.2(14) . . ? O6 C15 C16 123.5(14) . . ? O5 C15 C16 116.2(13) . . ? O6 C15 In1 65.1(8) . . ? O5 C15 In1 56.0(7) . . ? C16 C15 In1 167.6(11) . . ? C17 C16 C21 121.5(14) . . ? C17 C16 C15 118.7(14) . . ? C21 C16 C15 119.6(13) . . ? C16 C17 C18 119.8(16) . . ? C16 C17 H16 120.1 . . ? C18 C17 H16 120.1 . . ? C17 C18 C19 120.3(16) . . ? C17 C18 H17 119.9 . . ? C19 C18 H17 119.9 . . ? C20 C19 C18 117.6(14) . . ? C20 C19 H18 121.2 . . ? C18 C19 H18 121.2 . . ? C19 C20 C21 124.8(15) . . ? C19 C20 H19 117.6 . . ? C21 C20 H19 117.6 . . ? C16 C21 C20 115.5(14) . . ? C16 C21 C22 125.3(13) . . ? C20 C21 C22 118.9(14) . . ? C27 C22 C23 117.6(14) . . ? C27 C22 C21 124.7(13) . . ? C23 C22 C21 117.5(15) . . ? C24 C23 C22 120.1(16) . . ? C24 C23 H22 120.0 . . ? C22 C23 H22 120.0 . . ? C23 C24 C25 124.0(15) . . ? C23 C24 H23 118.0 . . ? C25 C24 H23 118.0 . . ? C26 C25 C24 115.3(15) . . ? C26 C25 H24 122.3 . . ? C24 C25 H24 122.3 . . ? C25 C26 C27 122.4(16) . . ? C25 C26 H25 118.8 . . ? C27 C26 H25 118.8 . . ? C22 C27 C26 120.6(14) . . ? C22 C27 C28 125.3(13) . . ? C26 C27 C28 114.0(14) . . ? O7 C28 O8 120.6(13) . . ? O7 C28 C27 121.1(15) . . ? O8 C28 C27 118.2(13) . . ? O7 C28 In2 63.3(7) . . ? O8 C28 In2 57.5(7) . . ? C27 C28 In2 175.2(12) . . ? N1 C29 C30 122.0(16) . . ? N1 C29 H28 119.0 . . ? C30 C29 H28 119.0 . . ? C31 C30 C29 121.3(16) . . ? C31 C30 H29 119.3 . . ? C29 C30 H29 119.3 . . ? C30 C31 C32 117.6(17) . . ? C30 C31 H30 121.2 . . ? C32 C31 H30 121.2 . . ? C31 C32 C34 122(2) . . ? C31 C32 C33 117.8(17) . . ? C34 C32 C33 120.0(18) . . ? N1 C33 C32 123.6(15) . . ? N1 C33 C37 116.9(15) . . ? C32 C33 C37 119.5(16) . . ? C35 C34 C32 121(2) . . ? C35 C34 H33 119.4 . . ? C32 C34 H33 119.4 . . ? C34 C35 C36 119.4(18) . . ? C34 C35 H34 120.3 . . ? C36 C35 H34 120.3 . . ? C37 C36 C38 118.4(17) . . ? C37 C36 C35 119.6(18) . . ? C38 C36 C35 122.0(18) . . ? N2 C37 C36 121.1(15) . . ? N2 C37 C33 118.8(14) . . ? C36 C37 C33 120.1(17) . . ? C39 C38 C36 118.4(17) . . ? C39 C38 H37 120.8 . . ? C36 C38 H37 120.8 . . ? C38 C39 C40 120.5(18) . . ? C38 C39 H38 119.8 . . ? C40 C39 H38 119.8 . . ? N2 C40 C39 121.1(18) . . ? N2 C40 H39 119.4 . . ? C39 C40 H39 119.4 . . ? O9 C41 O10 119.0(15) . . ? O9 C41 C42 124.6(17) . . ? O10 C41 C42 116.4(17) . . ? O9 C41 In2 65.1(9) . . ? O10 C41 In2 54.0(8) . . ? C42 C41 In2 170.2(14) . . ? C47 C42 C43 122.0(15) . . ? C47 C42 C41 124.5(16) . . ? C43 C42 C41 113.5(16) . . ? C44 C43 C42 120.1(17) . . ? C44 C43 H42 119.9 . . ? C42 C43 H42 119.9 . . ? C45 C44 C43 119.0(18) . . ? C45 C44 H43 120.5 . . ? C43 C44 H43 120.5 . . ? C44 C45 C46 122.0(17) . . ? C44 C45 H44 119.0 . . ? C46 C45 H44 119.0 . . ? C45 C46 C47 121.1(16) . . ? C45 C46 H45 119.5 . . ? C47 C46 H45 119.5 . . ? C42 C47 C46 115.8(15) . . ? C42 C47 C48 127.0(14) . . ? C46 C47 C48 117.2(13) . . ? C53 C48 C49 117.3(16) . . ? C53 C48 C47 125.2(17) . . ? C49 C48 C47 117.0(15) . . ? C48 C49 C50 121.9(16) . . ? C48 C49 H48 119.0 . . ? C50 C49 H48 119.0 . . ? C51 C50 C49 118.7(18) . . ? C51 C50 H49 120.7 . . ? C49 C50 H49 120.7 . . ? C50 C51 C52 119.9(19) . . ? C50 C51 H50 120.1 . . ? C52 C51 H50 120.1 . . ? C51 C52 C53 120.0(16) . . ? C51 C52 H51 120.0 . . ? C53 C52 H51 120.0 . . ? C48 C53 C52 122.1(16) . . ? C48 C53 C54 121.1(16) . . ? C52 C53 C54 116.8(14) . . ? O11 C54 O12 124.0(16) . . ? O11 C54 C53 119.9(16) . . ? O12 C54 C53 116.1(13) . . ? N3 C55 C56 122.7(17) . . ? N3 C55 H54 118.6 . . ? C56 C55 H54 118.6 . . ? C55 C56 C57 118.2(17) . . ? C55 C56 H55 120.9 . . ? C57 C56 H55 120.9 . . ? C58 C57 C56 120.7(18) . . ? C58 C57 H56 119.7 . . ? C56 C57 H56 119.7 . . ? C57 C58 C59 116.2(18) . . ? C57 C58 C60 124.5(19) . . ? C59 C58 C60 119.2(18) . . ? N3 C59 C58 123.0(16) . . ? N3 C59 C63 117.8(14) . . ? C58 C59 C63 119.2(17) . . ? C61 C60 C58 120.1(19) . . ? C61 C60 H59 120.0 . . ? C58 C60 H59 120.0 . . ? C60 C61 C62 124(2) . . ? C60 C61 H60 118.0 . . ? C62 C61 H60 118.0 . . ? C64 C62 C61 127.1(18) . . ? C64 C62 C63 115.5(16) . . ? C61 C62 C63 117.4(17) . . ? N4 C63 C62 121.8(15) . . ? N4 C63 C59 118.3(14) . . ? C62 C63 C59 119.8(16) . . ? C65 C64 C62 121.9(16) . . ? C65 C64 H63 119.0 . . ? C62 C64 H63 119.0 . . ? C64 C65 C66 118.5(17) . . ? C64 C65 H64 120.7 . . ? C66 C65 H64 120.7 . . ? N4 C66 C65 123.9(17) . . ? N4 C66 H65 118.0 . . ? C65 C66 H65 118.0 . . ? 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 O2 In1 O1 C1 -1.9(8) . . . . ? O5 In1 O1 C1 170.2(9) . . . . ? O4 In1 O1 C1 -70.1(9) 2 . . . ? O3 In1 O1 C1 -99.1(9) 2 . . . ? N2 In1 O1 C1 37.8(11) . . . . ? N1 In1 O1 C1 87.1(8) . . . . ? O6 In1 O1 C1 164.0(8) . . . . ? C14 In1 O1 C1 -84.3(9) 2 . . . ? C15 In1 O1 C1 164.8(8) . . . . ? O5 In1 O2 C1 -9.3(12) . . . . ? O4 In1 O2 C1 131.6(9) 2 . . . ? O3 In1 O2 C1 75.3(9) 2 . . . ? N2 In1 O2 C1 -150.1(10) . . . . ? N1 In1 O2 C1 -78.3(9) . . . . ? O6 In1 O2 C1 -135.0(16) . . . . ? O1 In1 O2 C1 1.9(8) . . . . ? C14 In1 O2 C1 103.9(10) 2 . . . ? C15 In1 O2 C1 -36.9(16) . . . . ? O2 In1 O5 C15 -159.3(9) . . . . ? O4 In1 O5 C15 67.4(10) 2 . . . ? O3 In1 O5 C15 116.4(10) 2 . . . ? N2 In1 O5 C15 -31.3(12) . . . . ? N1 In1 O5 C15 -89.9(10) . . . . ? O6 In1 O5 C15 5.7(9) . . . . ? O1 In1 O5 C15 -168.7(10) . . . . ? C14 In1 O5 C15 94.4(10) 2 . . . ? C1 In1 O5 C15 -163.8(9) . . . . ? O2 In1 O6 C15 129.7(16) . . . . ? O5 In1 O6 C15 -5.8(9) . . . . ? O4 In1 O6 C15 -136.1(10) 2 . . . ? O3 In1 O6 C15 -81.7(11) 2 . . . ? N2 In1 O6 C15 145.0(11) . . . . ? N1 In1 O6 C15 73.8(10) . . . . ? O1 In1 O6 C15 1.8(13) . . . . ? C14 In1 O6 C15 -110.2(11) 2 . . . ? C1 In1 O6 C15 24.2(19) . . . . ? O12 In2 O7 C28 -134.6(19) 2_666 . . . ? O10 In2 O7 C28 115.2(8) . . . . ? O8 In2 O7 C28 -3.2(8) . . . . ? N3 In2 O7 C28 -89.4(8) . . . . ? N4 In2 O7 C28 -161.8(8) . . . . ? O9 In2 O7 C28 63.0(8) . . . . ? C41 In2 O7 C28 89.8(9) . . . . ? O12 In2 O8 C28 172.5(8) 2_666 . . . ? O10 In2 O8 C28 -68.5(9) . . . . ? N3 In2 O8 C28 91.1(9) . . . . ? N4 In2 O8 C28 36.3(11) . . . . ? O7 In2 O8 C28 3.1(8) . . . . ? O9 In2 O8 C28 -114.9(9) . . . . ? C41 In2 O8 C28 -93.2(9) . . . . ? O12 In2 O9 C41 -101.1(10) 2_666 . . . ? O10 In2 O9 C41 1.7(9) . . . . ? O8 In2 O9 C41 127.0(10) . . . . ? N3 In2 O9 C41 -172.0(10) . . . . ? N4 In2 O9 C41 -26.5(12) . . . . ? O7 In2 O9 C41 75.6(10) . . . . ? C28 In2 O9 C41 100.7(10) . . . . ? O12 In2 O10 C41 75.0(9) 2_666 . . . ? O8 In2 O10 C41 -62.2(10) . . . . ? N3 In2 O10 C41 171.1(10) . . . . ? N4 In2 O10 C41 158.3(10) . . . . ? O7 In2 O10 C41 -115.3(9) . . . . ? O9 In2 O10 C41 -1.7(9) . . . . ? C28 In2 O10 C41 -89.5(10) . . . . ? O2 In1 N1 C29 92.8(12) . . . . ? O5 In1 N1 C29 -46.0(11) . . . . ? O4 In1 N1 C29 176.0(10) 2 . . . ? O3 In1 N1 C29 23.1(16) 2 . . . ? N2 In1 N1 C29 179.9(12) . . . . ? O6 In1 N1 C29 -99.6(12) . . . . ? O1 In1 N1 C29 35.9(11) . . . . ? C14 In1 N1 C29 107(3) 2 . . . ? C1 In1 N1 C29 64.8(12) . . . . ? C15 In1 N1 C29 -73.7(12) . . . . ? O2 In1 N1 C33 -80.7(10) . . . . ? O5 In1 N1 C33 140.5(10) . . . . ? O4 In1 N1 C33 2.6(14) 2 . . . ? O3 In1 N1 C33 -150.3(9) 2 . . . ? N2 In1 N1 C33 6.5(9) . . . . ? O6 In1 N1 C33 86.9(10) . . . . ? O1 In1 N1 C33 -137.6(10) . . . . ? C14 In1 N1 C33 -67(4) 2 . . . ? C1 In1 N1 C33 -108.6(10) . . . . ? C15 In1 N1 C33 112.9(10) . . . . ? O2 In1 N2 C40 -98.5(12) . . . . ? O5 In1 N2 C40 115.0(12) . . . . ? O4 In1 N2 C40 -4.1(11) 2 . . . ? O3 In1 N2 C40 -17.1(14) 2 . . . ? N1 In1 N2 C40 177.9(12) . . . . ? O6 In1 N2 C40 85.4(12) . . . . ? O1 In1 N2 C40 -130.7(11) . . . . ? C14 In1 N2 C40 -11.0(12) 2 . . . ? C1 In1 N2 C40 -112.8(12) . . . . ? C15 In1 N2 C40 100.8(12) . . . . ? O2 In1 N2 C37 79.2(10) . . . . ? O5 In1 N2 C37 -67.3(11) . . . . ? O4 In1 N2 C37 173.6(10) 2 . . . ? O3 In1 N2 C37 160.5(9) 2 . . . ? N1 In1 N2 C37 -4.4(9) . . . . ? O6 In1 N2 C37 -96.9(10) . . . . ? O1 In1 N2 C37 47.0(12) . . . . ? C14 In1 N2 C37 166.7(10) 2 . . . ? C1 In1 N2 C37 64.9(10) . . . . ? C15 In1 N2 C37 -81.5(10) . . . . ? O12 In2 N3 C55 -92.1(13) 2_666 . . . ? O10 In2 N3 C55 169.7(11) . . . . ? O8 In2 N3 C55 38.0(13) . . . . ? N4 In2 N3 C55 -176.9(14) . . . . ? O7 In2 N3 C55 95.7(13) . . . . ? O9 In2 N3 C55 -22.2(17) . . . . ? C28 In2 N3 C55 67.3(13) . . . . ? C41 In2 N3 C55 -74(6) . . . . ? O12 In2 N3 C59 82.8(12) 2_666 . . . ? O10 In2 N3 C59 -15.4(17) . . . . ? O8 In2 N3 C59 -147.1(12) . . . . ? N4 In2 N3 C59 -2.0(11) . . . . ? O7 In2 N3 C59 -89.5(12) . . . . ? O9 In2 N3 C59 152.7(11) . . . . ? C28 In2 N3 C59 -117.9(12) . . . . ? C41 In2 N3 C59 101(6) . . . . ? O12 In2 N4 C66 88.2(13) 2_666 . . . ? O10 In2 N4 C66 -8.8(13) . . . . ? O8 In2 N4 C66 -124.3(12) . . . . ? N3 In2 N4 C66 177.0(14) . . . . ? O7 In2 N4 C66 -96.8(13) . . . . ? O9 In2 N4 C66 14.2(15) . . . . ? C28 In2 N4 C66 -106.0(13) . . . . ? C41 In2 N4 C66 1.8(14) . . . . ? O12 In2 N4 C63 -87.1(10) 2_666 . . . ? O10 In2 N4 C63 175.9(11) . . . . ? O8 In2 N4 C63 60.4(12) . . . . ? N3 In2 N4 C63 1.7(10) . . . . ? O7 In2 N4 C63 87.9(10) . . . . ? O9 In2 N4 C63 -161.1(9) . . . . ? C28 In2 N4 C63 78.7(11) . . . . ? C41 In2 N4 C63 -173.5(10) . . . . ? In1 O2 C1 O1 -3.6(15) . . . . ? In1 O2 C1 C2 179.1(11) . . . . ? In1 O1 C1 O2 3.2(14) . . . . ? In1 O1 C1 C2 -179.4(12) . . . . ? O5 In1 C1 O2 173.2(9) . . . . ? O4 In1 C1 O2 -53.2(10) 2 . . . ? O3 In1 C1 O2 -101.9(9) 2 . . . ? N2 In1 C1 O2 31.7(10) . . . . ? N1 In1 C1 O2 96.7(9) . . . . ? O6 In1 C1 O2 148.0(12) . . . . ? O1 In1 C1 O2 -176.7(14) . . . . ? C14 In1 C1 O2 -77.3(9) 2 . . . ? C15 In1 C1 O2 162.9(8) . . . . ? O2 In1 C1 O1 176.7(14) . . . . ? O5 In1 C1 O1 -10.1(9) . . . . ? O4 In1 C1 O1 123.5(8) 2 . . . ? O3 In1 C1 O1 74.8(8) 2 . . . ? N2 In1 C1 O1 -151.7(8) . . . . ? N1 In1 C1 O1 -86.6(9) . . . . ? O6 In1 C1 O1 -35.3(17) . . . . ? C14 In1 C1 O1 99.4(9) 2 . . . ? C15 In1 C1 O1 -20.4(11) . . . . ? O2 In1 C1 C2 -10(12) . . . . ? O5 In1 C1 C2 163(12) . . . . ? O4 In1 C1 C2 -63(12) 2 . . . ? O3 In1 C1 C2 -112(12) 2 . . . ? N2 In1 C1 C2 22(12) . . . . ? N1 In1 C1 C2 87(12) . . . . ? O6 In1 C1 C2 138(12) . . . . ? O1 In1 C1 C2 173(13) . . . . ? C14 In1 C1 C2 -87(12) 2 . . . ? C15 In1 C1 C2 153(12) . . . . ? O2 C1 C2 C7 -31(2) . . . . ? O1 C1 C2 C7 151.3(15) . . . . ? In1 C1 C2 C7 -22(13) . . . . ? O2 C1 C2 C3 149.8(14) . . . . ? O1 C1 C2 C3 -28(2) . . . . ? In1 C1 C2 C3 159(12) . . . . ? C7 C2 C3 C4 1(2) . . . . ? C1 C2 C3 C4 179.7(14) . . . . ? C2 C3 C4 C5 -3(3) . . . . ? C3 C4 C5 C6 3(3) . . . . ? C4 C5 C6 C7 -1(3) . . . . ? C3 C2 C7 C6 1(2) . . . . ? C1 C2 C7 C6 -177.8(14) . . . . ? C3 C2 C7 C8 174.3(15) . . . . ? C1 C2 C7 C8 -5(2) . . . . ? C5 C6 C7 C2 -1(3) . . . . ? C5 C6 C7 C8 -174.7(17) . . . . ? C2 C7 C8 C9 84(2) . . . . ? C6 C7 C8 C9 -102.8(19) . . . . ? C2 C7 C8 C13 -93.4(19) . . . . ? C6 C7 C8 C13 79.7(18) . . . . ? C13 C8 C9 C10 1(2) . . . . ? C7 C8 C9 C10 -176.9(14) . . . . ? C13 C8 C9 C14 -177.6(13) . . . . ? C7 C8 C9 C14 5(2) . . . . ? C8 C9 C10 C11 -2(2) . . . . ? C14 C9 C10 C11 176.6(14) . . . . ? C9 C10 C11 C12 2(3) . . . . ? C10 C11 C12 C13 -1(3) . . . . ? C9 C8 C13 C12 0(2) . . . . ? C7 C8 C13 C12 178.0(15) . . . . ? C11 C12 C13 C8 0(3) . . . . ? In1 O4 C14 O3 5.6(15) 2 . . . ? In1 O4 C14 C9 -170.1(11) 2 . . . ? In1 O3 C14 O4 -5.6(15) 2 . . . ? In1 O3 C14 C9 170.3(11) 2 . . . ? C8 C9 C14 O4 -2(2) . . . . ? C10 C9 C14 O4 179.5(13) . . . . ? C8 C9 C14 O3 -178.4(13) . . . . ? C10 C9 C14 O3 4(2) . . . . ? C8 C9 C14 In1 -102(8) . . . 2 ? C10 C9 C14 In1 80(8) . . . 2 ? In1 O6 C15 O5 9.9(16) . . . . ? In1 O6 C15 C16 -169.7(14) . . . . ? In1 O5 C15 O6 -10.8(17) . . . . ? In1 O5 C15 C16 168.8(11) . . . . ? O2 In1 C15 O6 -145.7(12) . . . . ? O5 In1 C15 O6 169.7(17) . . . . ? O4 In1 C15 O6 46.4(11) 2 . . . ? O3 In1 C15 O6 104.3(10) 2 . . . ? N2 In1 C15 O6 -35.5(11) . . . . ? N1 In1 C15 O6 -104.2(11) . . . . ? O1 In1 C15 O6 -178.7(10) . . . . ? C14 In1 C15 O6 75.7(11) 2 . . . ? C1 In1 C15 O6 -168.7(9) . . . . ? O2 In1 C15 O5 44.6(16) . . . . ? O4 In1 C15 O5 -123.3(9) 2 . . . ? O3 In1 C15 O5 -65.4(10) 2 . . . ? N2 In1 C15 O5 154.8(9) . . . . ? N1 In1 C15 O5 86.1(10) . . . . ? O6 In1 C15 O5 -169.7(17) . . . . ? O1 In1 C15 O5 11.7(10) . . . . ? C14 In1 C15 O5 -94.0(10) 2 . . . ? C1 In1 C15 O5 21.6(12) . . . . ? O2 In1 C15 C16 -9(6) . . . . ? O5 In1 C15 C16 -54(5) . . . . ? O4 In1 C15 C16 -177(5) 2 . . . ? O3 In1 C15 C16 -119(5) 2 . . . ? N2 In1 C15 C16 101(5) . . . . ? N1 In1 C15 C16 32(5) . . . . ? O6 In1 C15 C16 136(5) . . . . ? O1 In1 C15 C16 -42(5) . . . . ? C14 In1 C15 C16 -148(5) 2 . . . ? C1 In1 C15 C16 -32(5) . . . . ? O6 C15 C16 C17 -108.6(18) . . . . ? O5 C15 C16 C17 71.7(19) . . . . ? In1 C15 C16 C17 120(5) . . . . ? O6 C15 C16 C21 77(2) . . . . ? O5 C15 C16 C21 -102.7(16) . . . . ? In1 C15 C16 C21 -54(5) . . . . ? C21 C16 C17 C18 -3(2) . . . . ? C15 C16 C17 C18 -177.6(13) . . . . ? C16 C17 C18 C19 8(2) . . . . ? C17 C18 C19 C20 -8(2) . . . . ? C18 C19 C20 C21 2(2) . . . . ? C17 C16 C21 C20 -2(2) . . . . ? C15 C16 C21 C20 172.3(12) . . . . ? C17 C16 C21 C22 171.2(13) . . . . ? C15 C16 C21 C22 -15(2) . . . . ? C19 C20 C21 C16 2(2) . . . . ? C19 C20 C21 C22 -171.2(14) . . . . ? C16 C21 C22 C27 127.3(16) . . . . ? C20 C21 C22 C27 -59.7(19) . . . . ? C16 C21 C22 C23 -58.8(18) . . . . ? C20 C21 C22 C23 114.1(15) . . . . ? C27 C22 C23 C24 0(2) . . . . ? C21 C22 C23 C24 -174.1(13) . . . . ? C22 C23 C24 C25 1(2) . . . . ? C23 C24 C25 C26 -2(2) . . . . ? C24 C25 C26 C27 2(2) . . . . ? C23 C22 C27 C26 0(2) . . . . ? C21 C22 C27 C26 173.3(12) . . . . ? C23 C22 C27 C28 176.5(12) . . . . ? C21 C22 C27 C28 -10(2) . . . . ? C25 C26 C27 C22 -1(2) . . . . ? C25 C26 C27 C28 -177.9(13) . . . . ? In2 O7 C28 O8 5.4(14) . . . . ? In2 O7 C28 C27 -178.0(12) . . . . ? In2 O8 C28 O7 -5.8(14) . . . . ? In2 O8 C28 C27 177.6(11) . . . . ? C22 C27 C28 O7 -27(2) . . . . ? C26 C27 C28 O7 149.9(13) . . . . ? C22 C27 C28 O8 149.3(14) . . . . ? C26 C27 C28 O8 -33.5(18) . . . . ? C22 C27 C28 In2 174(11) . . . . ? C26 C27 C28 In2 -9(13) . . . . ? O12 In2 C28 O7 158.9(9) 2_666 . . . ? O10 In2 C28 O7 -66.4(8) . . . . ? O8 In2 C28 O7 174.5(14) . . . . ? N3 In2 C28 O7 88.3(8) . . . . ? N4 In2 C28 O7 19.8(9) . . . . ? O9 In2 C28 O7 -121.7(8) . . . . ? C41 In2 C28 O7 -94.6(9) . . . . ? O12 In2 C28 O8 -15.6(16) 2_666 . . . ? O10 In2 C28 O8 119.1(8) . . . . ? N3 In2 C28 O8 -86.2(9) . . . . ? N4 In2 C28 O8 -154.6(8) . . . . ? O7 In2 C28 O8 -174.5(14) . . . . ? O9 In2 C28 O8 63.8(9) . . . . ? C41 In2 C28 O8 90.9(9) . . . . ? O12 In2 C28 C27 -42(12) 2_666 . . . ? O10 In2 C28 C27 93(12) . . . . ? O8 In2 C28 C27 -26(11) . . . . ? N3 In2 C28 C27 -112(12) . . . . ? N4 In2 C28 C27 179(100) . . . . ? O7 In2 C28 C27 159(12) . . . . ? O9 In2 C28 C27 38(12) . . . . ? C41 In2 C28 C27 65(12) . . . . ? C33 N1 C29 C30 2(2) . . . . ? In1 N1 C29 C30 -171.0(11) . . . . ? N1 C29 C30 C31 -3(3) . . . . ? C29 C30 C31 C32 2(3) . . . . ? C30 C31 C32 C34 179.6(16) . . . . ? C30 C31 C32 C33 -1(2) . . . . ? C29 N1 C33 C32 -1(2) . . . . ? In1 N1 C33 C32 173.0(11) . . . . ? C29 N1 C33 C37 178.4(12) . . . . ? In1 N1 C33 C37 -7.7(16) . . . . ? C31 C32 C33 N1 0(2) . . . . ? C34 C32 C33 N1 179.7(14) . . . . ? C31 C32 C33 C37 -179.1(13) . . . . ? C34 C32 C33 C37 0(2) . . . . ? C31 C32 C34 C35 176.3(17) . . . . ? C33 C32 C34 C35 -3(3) . . . . ? C32 C34 C35 C36 5(3) . . . . ? C34 C35 C36 C37 -3(3) . . . . ? C34 C35 C36 C38 176.6(16) . . . . ? C40 N2 C37 C36 2(2) . . . . ? In1 N2 C37 C36 -175.6(11) . . . . ? C40 N2 C37 C33 -179.9(13) . . . . ? In1 N2 C37 C33 2.3(16) . . . . ? C38 C36 C37 N2 -1(2) . . . . ? C35 C36 C37 N2 178.5(14) . . . . ? C38 C36 C37 C33 -179.4(14) . . . . ? C35 C36 C37 C33 1(2) . . . . ? N1 C33 C37 N2 4(2) . . . . ? C32 C33 C37 N2 -177.1(13) . . . . ? N1 C33 C37 C36 -178.5(13) . . . . ? C32 C33 C37 C36 1(2) . . . . ? C37 C36 C38 C39 0(3) . . . . ? C35 C36 C38 C39 -179.9(16) . . . . ? C36 C38 C39 C40 1(3) . . . . ? C37 N2 C40 C39 -1(2) . . . . ? In1 N2 C40 C39 176.3(12) . . . . ? C38 C39 C40 N2 0(3) . . . . ? In2 O9 C41 O10 -2.8(15) . . . . ? In2 O9 C41 C42 178.3(15) . . . . ? In2 O10 C41 O9 3.1(17) . . . . ? In2 O10 C41 C42 -177.9(12) . . . . ? O12 In2 C41 O9 76.8(10) 2_666 . . . ? O10 In2 C41 O9 -177.0(16) . . . . ? O8 In2 C41 O9 -52.7(10) . . . . ? N3 In2 C41 O9 59(6) . . . . ? N4 In2 C41 O9 160.2(9) . . . . ? O7 In2 C41 O9 -110.8(10) . . . . ? C28 In2 C41 O9 -82.2(10) . . . . ? O12 In2 C41 O10 -106.2(9) 2_666 . . . ? O8 In2 C41 O10 124.3(9) . . . . ? N3 In2 C41 O10 -124(6) . . . . ? N4 In2 C41 O10 -22.8(10) . . . . ? O7 In2 C41 O10 66.2(9) . . . . ? O9 In2 C41 O10 177.0(16) . . . . ? C28 In2 C41 O10 94.8(9) . . . . ? O12 In2 C41 C42 -95(7) 2_666 . . . ? O10 In2 C41 C42 11(7) . . . . ? O8 In2 C41 C42 136(7) . . . . ? N3 In2 C41 C42 -113(9) . . . . ? N4 In2 C41 C42 -11(7) . . . . ? O7 In2 C41 C42 78(7) . . . . ? O9 In2 C41 C42 -172(8) . . . . ? C28 In2 C41 C42 106(7) . . . . ? O9 C41 C42 C47 -179.7(15) . . . . ? O10 C41 C42 C47 1(2) . . . . ? In2 C41 C42 C47 -9(8) . . . . ? O9 C41 C42 C43 1(2) . . . . ? O10 C41 C42 C43 -178.1(14) . . . . ? In2 C41 C42 C43 172(6) . . . . ? C47 C42 C43 C44 2(2) . . . . ? C41 C42 C43 C44 -178.9(14) . . . . ? C42 C43 C44 C45 -2(3) . . . . ? C43 C44 C45 C46 -1(3) . . . . ? C44 C45 C46 C47 3(3) . . . . ? C43 C42 C47 C46 0(2) . . . . ? C41 C42 C47 C46 -179.0(14) . . . . ? C43 C42 C47 C48 -179.4(15) . . . . ? C41 C42 C47 C48 1(3) . . . . ? C45 C46 C47 C42 -3(2) . . . . ? C45 C46 C47 C48 177.2(17) . . . . ? C42 C47 C48 C53 92(2) . . . . ? C46 C47 C48 C53 -88.1(19) . . . . ? C42 C47 C48 C49 -96.2(19) . . . . ? C46 C47 C48 C49 84.0(18) . . . . ? C53 C48 C49 C50 -2(2) . . . . ? C47 C48 C49 C50 -174.4(15) . . . . ? C48 C49 C50 C51 2(3) . . . . ? C49 C50 C51 C52 0(3) . . . . ? C50 C51 C52 C53 -3(3) . . . . ? C49 C48 C53 C52 -1(2) . . . . ? C47 C48 C53 C52 170.6(14) . . . . ? C49 C48 C53 C54 179.2(13) . . . . ? C47 C48 C53 C54 -9(2) . . . . ? C51 C52 C53 C48 4(2) . . . . ? C51 C52 C53 C54 -176.6(14) . . . . ? In2 O12 C54 O11 4.8(17) 2_666 . . . ? In2 O12 C54 C53 -173.9(10) 2_666 . . . ? C48 C53 C54 O11 147.1(14) . . . . ? C52 C53 C54 O11 -32(2) . . . . ? C48 C53 C54 O12 -34(2) . . . . ? C52 C53 C54 O12 146.5(14) . . . . ? C59 N3 C55 C56 3(2) . . . . ? In2 N3 C55 C56 177.8(13) . . . . ? N3 C55 C56 C57 -3(3) . . . . ? C55 C56 C57 C58 1(3) . . . . ? C56 C57 C58 C59 0(3) . . . . ? C56 C57 C58 C60 -178(2) . . . . ? C55 N3 C59 C58 -2(3) . . . . ? In2 N3 C59 C58 -177.3(14) . . . . ? C55 N3 C59 C63 177.4(15) . . . . ? In2 N3 C59 C63 2.2(19) . . . . ? C57 C58 C59 N3 1(3) . . . . ? C60 C58 C59 N3 178.4(18) . . . . ? C57 C58 C59 C63 -178.8(16) . . . . ? C60 C58 C59 C63 -1(3) . . . . ? C57 C58 C60 C61 176(2) . . . . ? C59 C58 C60 C61 -2(3) . . . . ? C58 C60 C61 C62 4(4) . . . . ? C60 C61 C62 C64 178(2) . . . . ? C60 C61 C62 C63 -4(3) . . . . ? C66 N4 C63 C62 0(2) . . . . ? In2 N4 C63 C62 175.9(11) . . . . ? C66 N4 C63 C59 -176.9(15) . . . . ? In2 N4 C63 C59 -1.2(18) . . . . ? C64 C62 C63 N4 2(2) . . . . ? C61 C62 C63 N4 -176.6(15) . . . . ? C64 C62 C63 C59 178.9(15) . . . . ? C61 C62 C63 C59 0(2) . . . . ? N3 C59 C63 N4 -1(2) . . . . ? C58 C59 C63 N4 178.9(15) . . . . ? N3 C59 C63 C62 -177.8(15) . . . . ? C58 C59 C63 C62 2(2) . . . . ? C61 C62 C64 C65 175.4(19) . . . . ? C63 C62 C64 C65 -3(3) . . . . ? C62 C64 C65 C66 2(3) . . . . ? C63 N4 C66 C65 -1(3) . . . . ? In2 N4 C66 C65 -176.6(14) . . . . ? C64 C65 C66 N4 0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 20.82 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.055 _refine_diff_density_min -0.945 _refine_diff_density_rms 0.141 ### end of compound-1 CIF ### data_InCompound2 _database_code_depnum_ccdc_archive 'CCDC 812722' #TrackingRef '- mostuptodate_In_Compound2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H13.5 In N O5.25' _chemical_formula_weight 454.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In 0.0822 5.0449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.7789(3) _cell_length_b 8.2923(2) _cell_length_c 19.6538(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.031(1) _cell_angle_gamma 90.00 _cell_volume 1749.93(8) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2758 _cell_measurement_theta_min 4.52 _cell_measurement_theta_max 53.19 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.725 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 901 _exptl_absorpt_coefficient_mu 11.083 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4709 _exptl_absorpt_correction_T_max 0.6655 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22655 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0404 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.52 _diffrn_reflns_theta_max 63.28 _reflns_number_total 2832 _reflns_number_gt 1984 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1472P)^2^+12.5862P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2832 _refine_ls_number_parameters 230 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0918 _refine_ls_R_factor_gt 0.0739 _refine_ls_wR_factor_ref 0.2452 _refine_ls_wR_factor_gt 0.2276 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.25074(5) 1.01060(7) 0.25027(3) 0.0297(4) Uani 1 1 d . . . C1 C 0.3979(13) 0.9214(14) 0.3594(7) 0.058(3) Uani 1 1 d . . . C2 C 0.4576(15) 0.8455(16) 0.4228(6) 0.072(4) Uani 1 1 d . . . C3 C 0.5746(18) 0.7571(15) 0.4204(10) 0.080(5) Uani 1 1 d . . . C4 C 0.611(2) 0.693(2) 0.4852(10) 0.116(6) Uani 1 1 d . . . H4 H 0.6872 0.6398 0.4895 0.139 Uiso 1 1 calc R . . C5 C 0.552(2) 0.700(2) 0.5400(10) 0.107(6) Uani 1 1 d . . . H5 H 0.5858 0.6531 0.5803 0.128 Uiso 1 1 calc R . . C6 C 0.443(3) 0.774(2) 0.5388(11) 0.116(6) Uani 1 1 d . . . H6 H 0.3996 0.7700 0.5777 0.139 Uiso 1 1 calc R . . C7 C 0.3902(17) 0.857(2) 0.4828(7) 0.094(5) Uani 1 1 d . . . H7 H 0.3168 0.9152 0.4837 0.113 Uiso 1 1 calc R . . C8 C 0.6441(12) 0.7455(13) 0.3621(11) 0.073(5) Uani 1 1 d . . . C9 C 0.7685(17) 0.800(2) 0.3774(11) 0.106(6) Uani 1 1 d . . . H9 H 0.7957 0.8490 0.4187 0.127 Uiso 1 1 calc R . . C10 C 0.849(2) 0.775(3) 0.3235(19) 0.141(10) Uani 1 1 d . . . H10 H 0.9311 0.8094 0.3306 0.169 Uiso 1 1 calc R . . C11 C 0.812(2) 0.704(3) 0.2639(18) 0.138(10) Uani 1 1 d . . . H11 H 0.8671 0.6947 0.2302 0.165 Uiso 1 1 calc R . . C12 C 0.6954(15) 0.647(2) 0.2528(10) 0.104(6) Uani 1 1 d . . . H12 H 0.6704 0.5945 0.2121 0.124 Uiso 1 1 calc R . . C13 C 0.6115(13) 0.6657(17) 0.3027(9) 0.080(4) Uani 1 1 d . . . C14 C 0.4761(11) 0.5922(13) 0.2844(6) 0.046(3) Uani 1 1 d . . . C15 C 0.444(2) 0.906(2) 0.1446(9) 0.162(8) Uani 1 1 d . . . H15 H 0.4679 0.8321 0.1789 0.194 Uiso 1 1 calc R . . C16 C 0.503(2) 0.901(3) 0.0850(9) 0.162(8) Uani 1 1 d . . . H16 H 0.5667 0.8261 0.0812 0.194 Uiso 1 1 calc R . . C17 C 0.4709(19) 1.0013(17) 0.0323(9) 0.087(4) Uani 1 1 d . . . C18 C 0.3849(16) 1.1138(19) 0.0446(7) 0.101(6) Uani 1 1 d . . . H18 H 0.3622 1.1915 0.0117 0.121 Uiso 1 1 calc R . . C19 C 0.3301(15) 1.1140(18) 0.1062(7) 0.087(4) Uani 1 1 d . . . H19 H 0.2717 1.1936 0.1132 0.105 Uiso 1 1 calc R . . O1 O 0.4447(6) 0.9418(9) 0.3056(4) 0.0473(18) Uani 1 1 d . . . O2 O 0.2785(11) 0.9597(11) 0.3620(4) 0.073(3) Uani 1 1 d . . . O3 O 0.2018(7) 0.7588(6) 0.2346(4) 0.0313(15) Uani 1 1 d D . . H3W H 0.127(7) 0.772(12) 0.201(5) 0.06(4) Uiso 1 1 d D . . O4 O 0.4475(8) 0.5662(11) 0.2223(5) 0.075(3) Uani 1 1 d . . . O5 O 0.4121(8) 0.5751(11) 0.3289(5) 0.063(2) Uani 1 1 d . . . N1 N 0.3566(12) 1.0075(11) 0.1551(6) 0.068(3) Uani 1 1 d . . . O100 O 0.052(5) 0.043(7) 0.441(3) 0.120(19) Uani 0.25 1 d P . . 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 0.0388(5) 0.0231(5) 0.0285(5) 0.0012(2) 0.0108(3) 0.0023(2) C1 0.066(8) 0.037(7) 0.069(9) 0.003(6) -0.008(7) -0.005(6) C2 0.115(11) 0.048(8) 0.050(7) 0.011(6) 0.000(7) -0.007(8) C3 0.088(13) 0.048(9) 0.095(14) 0.015(7) -0.041(11) -0.010(7) C4 0.164(15) 0.104(10) 0.074(10) 0.038(8) -0.025(10) -0.028(10) C5 0.153(19) 0.096(13) 0.064(11) 0.018(10) -0.032(12) -0.020(13) C6 0.164(15) 0.104(10) 0.074(10) 0.038(8) -0.025(10) -0.028(10) C7 0.139(14) 0.088(12) 0.056(9) -0.005(8) 0.012(9) -0.024(11) C8 0.032(7) 0.037(7) 0.143(16) 0.007(7) -0.039(8) -0.005(5) C9 0.079(12) 0.093(12) 0.143(17) -0.004(11) -0.008(11) -0.019(10) C10 0.087(15) 0.083(14) 0.25(3) 0.057(18) 0.03(2) 0.003(12) C11 0.090(16) 0.091(15) 0.24(3) -0.050(17) 0.040(16) -0.040(13) C12 0.074(10) 0.082(13) 0.160(17) 0.004(11) 0.041(10) 0.000(10) C13 0.062(8) 0.051(8) 0.128(13) 0.017(9) 0.019(9) 0.011(7) C14 0.059(7) 0.033(6) 0.044(7) -0.003(5) -0.010(6) 0.011(5) C15 0.222(16) 0.169(14) 0.113(10) 0.100(10) 0.121(11) 0.150(13) C16 0.222(16) 0.169(14) 0.113(10) 0.100(10) 0.121(11) 0.150(13) C17 0.118(9) 0.080(8) 0.071(7) 0.026(5) 0.047(6) 0.033(6) C18 0.143(14) 0.102(12) 0.068(9) 0.046(8) 0.071(10) 0.071(11) C19 0.118(9) 0.080(8) 0.071(7) 0.026(5) 0.047(6) 0.033(6) O1 0.043(4) 0.040(4) 0.059(5) 0.016(4) 0.000(4) 0.005(4) O2 0.115(9) 0.059(5) 0.047(5) -0.001(4) 0.013(5) -0.013(6) O3 0.036(4) 0.021(4) 0.038(4) 0.001(2) 0.011(3) 0.000(2) O4 0.074(6) 0.066(6) 0.091(7) 0.008(5) 0.034(5) 0.002(5) O5 0.069(5) 0.049(5) 0.067(6) 0.009(4) -0.006(5) -0.011(4) N1 0.095(9) 0.045(6) 0.072(8) 0.015(5) 0.044(7) 0.007(5) O100 0.12(4) 0.15(4) 0.10(4) -0.03(3) 0.05(3) -0.05(4) _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 O3 2.136(6) 2 ? In1 O3 2.169(5) . ? In1 O2 2.230(8) . ? In1 N1 2.274(10) . ? In1 O4 2.296(8) 2 ? In1 O5 2.305(8) 2 ? In1 O1 2.341(7) . ? In1 C14 2.571(12) 2 ? In1 C1 2.659(12) . ? C1 O1 1.223(15) . ? C1 O2 1.332(16) . ? C1 C2 1.490(17) . ? C2 C7 1.442(19) . ? C2 C3 1.46(2) . ? C3 C4 1.40(2) . ? C3 C8 1.43(3) . ? C4 C5 1.30(3) . ? C4 H4 0.9300 . ? C5 C6 1.32(3) . ? C5 H5 0.9300 . ? C6 C7 1.37(2) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C13 1.36(2) . ? C8 C9 1.42(2) . ? C9 C10 1.44(3) . ? C9 H9 0.9300 . ? C10 C11 1.34(4) . ? C10 H10 0.9300 . ? C11 C12 1.34(3) . ? C11 H11 0.9300 . ? C12 C13 1.40(2) . ? C12 H12 0.9300 . ? C13 C14 1.593(19) . ? C14 O5 1.169(13) . ? C14 O4 1.252(13) . ? C14 In1 2.571(12) 2_545 ? C15 N1 1.293(17) . ? C15 C16 1.383(19) . ? C15 H15 0.9300 . ? C16 C17 1.35(2) . ? C16 H16 0.9300 . ? C17 C18 1.352(19) . ? C17 C17 1.47(3) 3_675 ? C18 C19 1.393(16) . ? C18 H18 0.9300 . ? C19 N1 1.318(16) . ? C19 H19 0.9300 . ? O3 In1 2.136(6) 2_545 ? O3 H3W 1.00(2) . ? O4 In1 2.296(8) 2_545 ? O5 In1 2.305(8) 2_545 ? 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 O3 In1 O3 179.74(8) 2 . ? O3 In1 O2 92.0(3) 2 . ? O3 In1 O2 88.2(3) . . ? O3 In1 N1 89.7(3) 2 . ? O3 In1 N1 90.3(3) . . ? O2 In1 N1 140.7(5) . . ? O3 In1 O4 89.4(3) 2 2 ? O3 In1 O4 90.4(3) . 2 ? O2 In1 O4 81.6(4) . 2 ? N1 In1 O4 137.7(5) . 2 ? O3 In1 O5 91.7(3) 2 2 ? O3 In1 O5 88.0(3) . 2 ? O2 In1 O5 137.5(4) . 2 ? N1 In1 O5 81.6(4) . 2 ? O4 In1 O5 56.1(3) 2 2 ? O3 In1 O1 88.7(3) 2 . ? O3 In1 O1 91.6(3) . . ? O2 In1 O1 57.3(3) . . ? N1 In1 O1 83.5(4) . . ? O4 In1 O1 138.7(3) 2 . ? O5 In1 O1 165.2(3) 2 . ? O3 In1 C14 89.7(3) 2 2 ? O3 In1 C14 90.1(3) . 2 ? O2 In1 C14 110.7(4) . 2 ? N1 In1 C14 108.6(5) . 2 ? O4 In1 C14 29.1(3) 2 2 ? O5 In1 C14 27.0(3) 2 2 ? O1 In1 C14 167.8(4) . 2 ? O3 In1 C1 92.1(3) 2 . ? O3 In1 C1 88.1(3) . . ? O2 In1 C1 30.0(4) . . ? N1 In1 C1 110.7(5) . . ? O4 In1 C1 111.6(4) 2 . ? O5 In1 C1 167.1(4) 2 . ? O1 In1 C1 27.4(3) . . ? C14 In1 C1 140.7(5) 2 . ? O1 C1 O2 118.2(11) . . ? O1 C1 C2 127.0(13) . . ? O2 C1 C2 114.6(12) . . ? O1 C1 In1 61.7(6) . . ? O2 C1 In1 56.9(6) . . ? C2 C1 In1 167.2(9) . . ? C7 C2 C3 123.8(14) . . ? C7 C2 C1 116.5(14) . . ? C3 C2 C1 119.6(13) . . ? C4 C3 C8 125.3(18) . . ? C4 C3 C2 109(2) . . ? C8 C3 C2 125.1(13) . . ? C5 C4 C3 128(2) . . ? C5 C4 H4 116.1 . . ? C3 C4 H4 116.1 . . ? C4 C5 C6 120(2) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C7 123(2) . . ? C5 C6 H6 118.4 . . ? C7 C6 H6 118.4 . . ? C6 C7 C2 115(2) . . ? C6 C7 H7 122.6 . . ? C2 C7 H7 122.6 . . ? C13 C8 C3 127.4(13) . . ? C13 C8 C9 120.3(19) . . ? C3 C8 C9 111.1(17) . . ? C8 C9 C10 114(2) . . ? C8 C9 H9 122.8 . . ? C10 C9 H9 122.8 . . ? C11 C10 C9 124(2) . . ? C11 C10 H10 118.1 . . ? C9 C10 H10 118.1 . . ? C10 C11 C12 120(3) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C11 C12 C13 120(2) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C8 C13 C12 121.4(16) . . ? C8 C13 C14 122.8(13) . . ? C12 C13 C14 115.8(15) . . ? O5 C14 O4 126.7(12) . . ? O5 C14 C13 117.8(11) . . ? O4 C14 C13 115.4(12) . . ? O5 C14 In1 63.7(7) . 2_545 ? O4 C14 In1 63.2(6) . 2_545 ? C13 C14 In1 172.6(8) . 2_545 ? N1 C15 C16 123.6(14) . . ? N1 C15 H15 118.2 . . ? C16 C15 H15 118.2 . . ? C17 C16 C15 121.4(14) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? C18 C17 C16 115.1(14) . . ? C18 C17 C17 121.1(17) . 3_675 ? C16 C17 C17 123.6(18) . 3_675 ? C17 C18 C19 120.4(13) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? N1 C19 C18 123.5(13) . . ? N1 C19 H19 118.3 . . ? C18 C19 H19 118.3 . . ? C1 O1 In1 90.9(7) . . ? C1 O2 In1 93.1(7) . . ? In1 O3 In1 148.8(4) 2_545 . ? In1 O3 H3W 112(6) 2_545 . ? In1 O3 H3W 99(6) . . ? C14 O4 In1 87.7(7) . 2_545 ? C14 O5 In1 89.3(7) . 2_545 ? C15 N1 C19 115.7(12) . . ? C15 N1 In1 124.3(9) . . ? C19 N1 In1 120.0(9) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 63.28 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.686 _refine_diff_density_min -1.126 _refine_diff_density_rms 0.219 # Attachment '- mostuptodate_In_Compound3.cif' data_incompound3 _database_code_depnum_ccdc_archive 'CCDC 812723' #TrackingRef '- mostuptodate_In_Compound3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H27 In N2 O9' _chemical_formula_weight 770.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.8039(9) _cell_length_b 14.0375(9) _cell_length_c 18.358(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3299.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6007 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 27.06 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 0.778 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.756 _exptl_absorpt_correction_T_max 0.856 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30563 _diffrn_reflns_av_R_equivalents 0.0594 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 28.32 _reflns_number_total 8003 _reflns_number_gt 6908 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; We have added two restrains to fix two hydrogen atoms in the water solvent molecule 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^)+(0.0245P)^2^+0.1471P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.002(15) _refine_ls_number_reflns 8003 _refine_ls_number_parameters 559 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.0646 _refine_ls_wR_factor_gt 0.0621 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.036 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group In1 In 0.367710(17) 0.097632(14) 0.786538(11) 0.03004(6) Uani 1 1 d . . . C1 C 0.2313(3) 0.1369(2) 0.89488(18) 0.0385(8) Uani 1 1 d . . . C2 C 0.5611(3) 0.4517(2) 0.63667(18) 0.0352(7) Uani 1 1 d . . . C3 C 0.5497(3) 0.1592(2) 0.73492(17) 0.0351(7) Uani 1 1 d . . . C4 C 0.2473(3) -0.0449(3) 0.67900(19) 0.0430(9) Uani 1 1 d . . . H4 H 0.281(3) -0.091(3) 0.711(2) 0.061(10) Uiso 1 1 d . . . C5 C 0.1855(3) -0.0759(3) 0.6223(2) 0.0523(11) Uani 1 1 d . . . H5 H 0.175(3) -0.145(3) 0.618(2) 0.071(14) Uiso 1 1 d . . . C6 C 0.1431(4) -0.0084(3) 0.5764(2) 0.0625(12) Uani 1 1 d . . . H6 H 0.108(3) -0.026(2) 0.5395(19) 0.045(10) Uiso 1 1 d . . . C7 C 0.1616(3) 0.0871(4) 0.5898(2) 0.0598(11) Uani 1 1 d . . . H7 H 0.139(3) 0.133(3) 0.555(2) 0.066(12) Uiso 1 1 d . . . C8 C 0.2230(2) 0.1125(2) 0.64788(17) 0.0397(8) Uani 1 1 d . . . C9 C 0.2436(3) 0.2133(3) 0.66805(19) 0.0463(9) Uani 1 1 d . . . C10 C 0.2030(4) 0.2902(4) 0.6292(3) 0.0728(14) Uani 1 1 d . . . H10 H 0.161(3) 0.276(3) 0.586(2) 0.073(14) Uiso 1 1 d . . . C11 C 0.2252(5) 0.3814(3) 0.6506(3) 0.0807(16) Uani 1 1 d . . . H11 H 0.210(5) 0.434(4) 0.633(3) 0.12(2) Uiso 1 1 d . . . C12 C 0.2848(4) 0.3953(3) 0.7112(3) 0.0670(11) Uani 1 1 d . . . H12 H 0.301(3) 0.452(3) 0.729(2) 0.076(15) Uiso 1 1 d . . . C13 C 0.3211(4) 0.3176(2) 0.7490(2) 0.0541(10) Uani 1 1 d . . . H13 H 0.375(4) 0.319(3) 0.787(2) 0.087(14) Uiso 1 1 d . . . C14 C 0.1583(2) 0.1448(2) 0.95771(16) 0.0339(8) Uani 1 1 d . . . C15 C 0.1216(3) 0.0608(2) 0.98906(18) 0.0423(8) Uani 1 1 d . . . H15 H 0.135(3) 0.002(3) 0.9661(19) 0.060(10) Uiso 1 1 d . . . C16 C 0.0663(3) 0.0635(3) 1.0539(2) 0.0485(10) Uani 1 1 d . . . H16 H 0.045(2) 0.006(2) 1.0804(16) 0.031(9) Uiso 1 1 d . . . C17 C 0.0485(3) 0.1501(3) 1.0870(2) 0.0471(9) Uani 1 1 d . . . H17 H 0.011(3) 0.154(2) 1.130(2) 0.057(11) Uiso 1 1 d . . . C18 C 0.0809(3) 0.2340(3) 1.0551(2) 0.0430(9) Uani 1 1 d . . . H18 H 0.063(3) 0.292(3) 1.0753(18) 0.045(10) Uiso 1 1 d . . . C19 C 0.1357(3) 0.2330(2) 0.98966(16) 0.0346(7) Uani 1 1 d . . . C20 C 0.1611(3) 0.3248(2) 0.95236(18) 0.0404(9) Uani 1 1 d . . . C21 C 0.0972(4) 0.3555(3) 0.8963(2) 0.0587(11) Uani 1 1 d . . . H21 H 0.043(3) 0.317(2) 0.8823(19) 0.043(11) Uiso 1 1 d . . . C22 C 0.1146(5) 0.4430(4) 0.8619(3) 0.0735(14) Uani 1 1 d . . . H22 H 0.064(4) 0.449(3) 0.822(3) 0.097(17) Uiso 1 1 d . . . C23 C 0.1940(5) 0.5003(3) 0.8849(3) 0.0760(16) Uani 1 1 d . . . H23 H 0.209(4) 0.565(3) 0.860(2) 0.093(16) Uiso 1 1 d . . . C24 C 0.2568(5) 0.4719(3) 0.9415(3) 0.0652(13) Uani 1 1 d . . . H24 H 0.319(4) 0.503(3) 0.957(3) 0.094(18) Uiso 1 1 d . . . C25 C 0.2433(3) 0.3843(2) 0.97478(19) 0.0436(9) Uani 1 1 d . . . C26 C 0.3188(3) 0.3550(3) 1.0318(2) 0.0480(9) Uani 1 1 d . . . C27 C 0.6531(2) 0.2012(2) 0.71538(19) 0.0342(7) Uani 1 1 d . . . C28 C 0.7363(3) 0.1871(3) 0.7609(2) 0.0433(9) Uani 1 1 d . . . H28 H 0.726(3) 0.153(2) 0.7977(19) 0.038(10) Uiso 1 1 d . . . C29 C 0.8324(3) 0.2259(3) 0.7458(2) 0.0513(10) Uani 1 1 d . . . H29 H 0.893(3) 0.211(2) 0.7726(18) 0.046(10) Uiso 1 1 d . . . C30 C 0.8450(3) 0.2844(3) 0.6871(2) 0.0521(10) Uani 1 1 d . . . H30 H 0.905(3) 0.309(3) 0.674(2) 0.066(13) Uiso 1 1 d . . . C31 C 0.7608(3) 0.3017(2) 0.6414(2) 0.0431(8) Uani 1 1 d . . . H31 H 0.768(3) 0.345(2) 0.6018(19) 0.043(10) Uiso 1 1 d . . . C32 C 0.6644(2) 0.2603(2) 0.65379(16) 0.0326(7) Uani 1 1 d . . . C33 C 0.5767(3) 0.2779(2) 0.60176(18) 0.0341(8) Uani 1 1 d . . . C34 C 0.5429(3) 0.2035(3) 0.55672(19) 0.0457(9) Uani 1 1 d . . . H34 H 0.574(3) 0.146(2) 0.5639(18) 0.047(10) Uiso 1 1 d . . . C35 C 0.4658(3) 0.2160(3) 0.5062(2) 0.0550(11) Uani 1 1 d . . . H35 H 0.447(3) 0.166(2) 0.4744(17) 0.038(9) Uiso 1 1 d . . . C36 C 0.4188(4) 0.3046(3) 0.4978(2) 0.0576(11) Uani 1 1 d . . . H36 H 0.364(3) 0.311(2) 0.4614(19) 0.053(10) Uiso 1 1 d . . . C37 C 0.4525(3) 0.3795(2) 0.5410(2) 0.0444(9) Uani 1 1 d . . . H37 H 0.422(2) 0.438(2) 0.5383(16) 0.029(9) Uiso 1 1 d . . . C38 C 0.5295(3) 0.3667(2) 0.59285(17) 0.0335(7) Uani 1 1 d . . . N1 N 0.2669(2) 0.04668(19) 0.69164(13) 0.0360(6) Uani 1 1 d . . . N2 N 0.3008(2) 0.22832(18) 0.72739(14) 0.0398(7) Uani 1 1 d . . . O1 O 0.30814(19) 0.19323(16) 0.89090(12) 0.0416(5) Uani 1 1 d . . . O2 O 0.21952(19) 0.07199(16) 0.84808(12) 0.0454(6) Uani 1 1 d . . . O3 O 0.5558(2) 0.53241(16) 0.60829(14) 0.0534(7) Uani 1 1 d . . . O4 O 0.59233(18) 0.44284(14) 0.70167(11) 0.0429(6) Uani 1 1 d . . . O5 O 0.50749(18) 0.18746(17) 0.79273(14) 0.0489(6) Uani 1 1 d . . . O6 O 0.50628(19) 0.09756(19) 0.69764(13) 0.0582(7) Uani 1 1 d . . . O7 O 0.3439(2) 0.4045(2) 1.08237(15) 0.0776(9) Uani 1 1 d . . . O8 O 0.3612(2) 0.26898(18) 1.02334(15) 0.0505(6) Uani 1 1 d . . . H8 H 0.345(3) 0.246(3) 0.987(2) 0.052(13) Uiso 1 1 d . . . O9 O 0.9976(4) 0.5057(5) 0.6806(4) 0.161(2) Uani 1 1 d D . . H91 H 0.989(5) 0.5754(17) 0.689(3) 0.11(2) Uiso 1 1 d D . . H92 H 0.921(3) 0.523(7) 0.683(6) 0.26(5) Uiso 1 1 d 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 0.03828(11) 0.02608(9) 0.02576(9) 0.00148(11) -0.00057(10) -0.00161(11) C1 0.045(2) 0.0385(18) 0.0320(17) 0.0053(15) 0.0052(16) 0.0081(16) C2 0.0332(19) 0.0347(18) 0.0378(19) -0.0087(15) 0.0050(15) -0.0037(14) C3 0.0418(19) 0.0291(16) 0.0345(18) 0.0082(13) -0.0011(15) -0.0007(14) C4 0.047(2) 0.045(2) 0.0371(19) -0.0040(16) -0.0002(17) -0.0063(17) C5 0.055(2) 0.060(3) 0.041(2) -0.0079(18) -0.0051(18) -0.0157(19) C6 0.054(3) 0.095(3) 0.039(2) -0.009(2) -0.018(2) -0.006(3) C7 0.067(3) 0.070(3) 0.043(2) 0.004(2) -0.0124(18) 0.002(2) C8 0.0402(18) 0.051(2) 0.0282(16) 0.0020(16) 0.0006(14) 0.0022(16) C9 0.050(2) 0.050(2) 0.039(2) 0.0056(17) 0.0015(17) 0.0064(18) C10 0.095(4) 0.061(3) 0.062(3) 0.014(2) -0.019(3) 0.010(3) C11 0.102(4) 0.054(3) 0.086(4) 0.024(3) 0.000(3) 0.026(3) C12 0.096(3) 0.035(2) 0.070(3) 0.010(3) 0.018(3) 0.009(2) C13 0.071(3) 0.034(2) 0.057(2) 0.0017(18) 0.002(2) 0.0053(18) C14 0.035(2) 0.0357(17) 0.0312(16) -0.0029(13) 0.0026(13) -0.0032(13) C15 0.047(2) 0.0385(17) 0.0419(18) -0.0027(15) 0.0030(19) -0.0087(18) C16 0.049(2) 0.052(2) 0.044(2) 0.0071(18) 0.0034(18) -0.0184(18) C17 0.045(2) 0.056(2) 0.040(2) -0.0010(18) 0.0142(18) -0.0061(18) C18 0.039(2) 0.048(2) 0.041(2) -0.0064(18) 0.0100(16) -0.0002(17) C19 0.0295(16) 0.0353(16) 0.0389(17) 0.0023(13) -0.0010(16) -0.0002(16) C20 0.045(2) 0.0370(18) 0.0394(18) 0.0012(15) 0.0147(16) 0.0107(15) C21 0.054(3) 0.061(3) 0.061(3) 0.010(2) 0.010(2) 0.015(2) C22 0.075(4) 0.079(3) 0.066(3) 0.028(3) 0.015(3) 0.037(3) C23 0.098(4) 0.050(3) 0.080(4) 0.024(3) 0.042(3) 0.021(3) C24 0.084(4) 0.044(2) 0.068(3) 0.001(2) 0.029(3) -0.004(2) C25 0.055(2) 0.0284(19) 0.047(2) -0.0028(15) 0.0198(17) -0.0023(15) C26 0.050(2) 0.050(2) 0.044(2) 0.0002(18) 0.0114(18) -0.0148(18) C27 0.0382(19) 0.0292(14) 0.0352(15) -0.0095(16) 0.0036(17) -0.0029(12) C28 0.050(2) 0.040(2) 0.040(2) -0.0023(17) -0.0043(18) 0.0003(17) C29 0.041(2) 0.053(2) 0.059(2) -0.014(2) -0.0108(19) 0.0112(18) C30 0.032(2) 0.056(2) 0.068(3) -0.011(2) 0.0090(18) -0.0066(17) C31 0.046(2) 0.0396(19) 0.043(2) -0.0036(17) 0.0148(18) -0.0056(16) C32 0.0352(18) 0.0293(15) 0.0333(16) -0.0079(13) 0.0085(13) 0.0017(12) C33 0.042(2) 0.0329(17) 0.0277(17) -0.0039(14) 0.0062(15) -0.0079(14) C34 0.064(3) 0.0304(18) 0.043(2) -0.0042(15) -0.0013(18) -0.0017(17) C35 0.077(3) 0.041(2) 0.047(2) -0.0134(18) -0.015(2) -0.013(2) C36 0.069(3) 0.055(2) 0.049(2) -0.0058(19) -0.026(2) -0.008(2) C37 0.052(2) 0.036(2) 0.045(2) -0.0020(15) -0.0069(18) 0.0006(16) C38 0.0364(19) 0.0332(16) 0.0309(17) -0.0008(13) 0.0029(14) -0.0025(14) N1 0.0402(16) 0.0398(15) 0.0280(14) -0.0003(11) -0.0006(11) -0.0017(12) N2 0.0506(17) 0.0339(14) 0.0348(17) 0.0031(12) -0.0015(13) 0.0026(12) O1 0.0448(14) 0.0384(12) 0.0416(13) -0.0010(10) 0.0138(11) 0.0006(11) O2 0.0546(15) 0.0470(15) 0.0346(13) -0.0124(11) 0.0086(11) -0.0009(11) O3 0.077(2) 0.0291(13) 0.0540(16) -0.0010(11) -0.0165(15) -0.0024(12) O4 0.0609(15) 0.0369(11) 0.0309(13) -0.0082(9) -0.0041(11) 0.0000(10) O5 0.0480(14) 0.0608(15) 0.0379(14) -0.0069(13) 0.0092(13) -0.0121(11) O6 0.0633(16) 0.0573(14) 0.0540(16) -0.0201(15) 0.0151(12) -0.0305(15) O7 0.090(2) 0.0798(18) 0.0629(17) -0.0252(18) 0.0024(15) -0.027(2) O8 0.0499(16) 0.0547(16) 0.0471(15) 0.0027(12) -0.0042(14) -0.0099(15) O9 0.091(4) 0.196(6) 0.197(6) 0.101(5) -0.001(3) 0.020(4) _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 O5 2.192(2) . ? In1 O2 2.237(2) . ? In1 O4 2.243(2) 3_646 ? In1 N1 2.283(3) . ? In1 N2 2.298(2) . ? In1 O3 2.351(2) 3_646 ? In1 O6 2.411(2) . ? In1 O1 2.460(2) . ? In1 C2 2.649(3) 3_646 ? In1 C3 2.660(3) . ? In1 C1 2.704(3) . ? C1 O2 1.261(4) . ? C1 O1 1.265(4) . ? C1 C14 1.489(4) . ? C2 O3 1.249(4) . ? C2 O4 1.265(4) . ? C2 C38 1.495(4) . ? C2 In1 2.649(3) 3_656 ? C3 O6 1.236(4) . ? C3 O5 1.255(4) . ? C3 C27 1.493(4) . ? C4 N1 1.330(4) . ? C4 C5 1.379(5) . ? C5 C6 1.379(6) . ? C6 C7 1.383(6) . ? C7 C8 1.371(5) . ? C8 N1 1.347(4) . ? C8 C9 1.486(5) . ? C9 N2 1.330(4) . ? C9 C10 1.395(5) . ? C10 C11 1.370(7) . ? C11 C12 1.364(7) . ? C12 C13 1.373(5) . ? C13 N2 1.340(4) . ? C14 C15 1.394(4) . ? C14 C19 1.401(4) . ? C15 C16 1.386(5) . ? C16 C17 1.377(5) . ? C17 C18 1.378(5) . ? C18 C19 1.391(5) . ? C19 C20 1.495(4) . ? C20 C21 1.384(5) . ? C20 C25 1.404(5) . ? C21 C22 1.399(6) . ? C22 C23 1.364(7) . ? C23 C24 1.373(7) . ? C24 C25 1.384(5) . ? C25 C26 1.482(5) . ? C26 O7 1.203(4) . ? C26 O8 1.333(5) . ? C27 C28 1.368(5) . ? C27 C32 1.409(4) . ? C28 C29 1.374(6) . ? C29 C30 1.365(6) . ? C30 C31 1.387(5) . ? C31 C32 1.384(5) . ? C32 C33 1.495(5) . ? C33 C34 1.400(5) . ? C33 C38 1.395(4) . ? C34 C35 1.366(5) . ? C35 C36 1.390(6) . ? C36 C37 1.387(5) . ? C37 C38 1.381(5) . ? O3 In1 2.351(2) 3_656 ? O4 In1 2.243(2) 3_656 ? 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 O5 In1 O2 139.35(9) . . ? O5 In1 O4 111.47(9) . 3_646 ? O2 In1 O4 89.36(8) . 3_646 ? O5 In1 N1 132.95(9) . . ? O2 In1 N1 81.69(9) . . ? O4 In1 N1 84.21(9) 3_646 . ? O5 In1 N2 82.52(10) . . ? O2 In1 N2 92.90(9) . . ? O4 In1 N2 154.73(9) 3_646 . ? N1 In1 N2 71.25(9) . . ? O5 In1 O3 80.86(10) . 3_646 ? O2 In1 O3 82.88(10) . 3_646 ? O4 In1 O3 56.51(8) 3_646 3_646 ? N1 In1 O3 137.76(9) . 3_646 ? N2 In1 O3 148.72(9) . 3_646 ? O5 In1 O6 55.56(8) . . ? O2 In1 O6 165.00(8) . . ? O4 In1 O6 84.09(9) 3_646 . ? N1 In1 O6 84.23(9) . . ? N2 In1 O6 87.42(10) . . ? O3 In1 O6 104.42(10) 3_646 . ? O5 In1 O1 84.20(9) . . ? O2 In1 O1 55.36(8) . . ? O4 In1 O1 121.60(8) 3_646 . ? N1 In1 O1 126.14(9) . . ? N2 In1 O1 79.44(9) . . ? O3 In1 O1 72.67(8) 3_646 . ? O6 In1 O1 139.08(8) . . ? O5 In1 C2 97.83(10) . 3_646 ? O2 In1 C2 84.19(9) . 3_646 ? O4 In1 C2 28.44(9) 3_646 3_646 ? N1 In1 C2 111.00(10) . 3_646 ? N2 In1 C2 175.94(10) . 3_646 ? O3 In1 C2 28.14(9) 3_646 3_646 ? O6 In1 C2 96.12(10) . 3_646 ? O1 In1 C2 96.56(9) . 3_646 ? O5 In1 C3 27.91(9) . . ? O2 In1 C3 167.18(9) . . ? O4 In1 C3 98.60(9) 3_646 . ? N1 In1 C3 108.98(9) . . ? N2 In1 C3 84.20(10) . . ? O3 In1 C3 93.10(10) 3_646 . ? O6 In1 C3 27.65(8) . . ? O1 In1 C3 111.82(9) . . ? C2 In1 C3 98.02(10) 3_646 . ? O5 In1 C1 111.85(10) . . ? O2 In1 C1 27.55(9) . . ? O4 In1 C1 105.88(9) 3_646 . ? N1 In1 C1 105.06(10) . . ? N2 In1 C1 86.79(9) . . ? O3 In1 C1 75.19(10) 3_646 . ? O6 In1 C1 166.80(9) . . ? O1 In1 C1 27.85(9) . . ? C2 In1 C1 89.34(10) 3_646 . ? C3 In1 C1 139.63(11) . . ? O2 C1 O1 120.4(3) . . ? O2 C1 C14 120.4(3) . . ? O1 C1 C14 119.1(3) . . ? O2 C1 In1 55.18(17) . . ? O1 C1 In1 65.31(17) . . ? C14 C1 In1 172.2(2) . . ? O3 C2 O4 120.0(3) . . ? O3 C2 C38 119.0(3) . . ? O4 C2 C38 121.0(3) . . ? O3 C2 In1 62.54(17) . 3_656 ? O4 C2 In1 57.63(16) . 3_656 ? C38 C2 In1 175.5(2) . 3_656 ? O6 C3 O5 119.7(3) . . ? O6 C3 C27 122.9(3) . . ? O5 C3 C27 117.4(3) . . ? O6 C3 In1 64.89(18) . . ? O5 C3 In1 54.85(16) . . ? C27 C3 In1 172.2(2) . . ? N1 C4 C5 123.1(4) . . ? C6 C5 C4 118.0(4) . . ? C5 C6 C7 119.3(4) . . ? C8 C7 C6 119.3(4) . . ? N1 C8 C7 121.6(4) . . ? N1 C8 C9 115.5(3) . . ? C7 C8 C9 122.9(3) . . ? N2 C9 C10 120.1(4) . . ? N2 C9 C8 116.9(3) . . ? C10 C9 C8 122.9(4) . . ? C11 C10 C9 120.0(5) . . ? C12 C11 C10 118.9(4) . . ? C11 C12 C13 119.2(5) . . ? N2 C13 C12 121.8(4) . . ? C15 C14 C19 120.4(3) . . ? C15 C14 C1 117.9(3) . . ? C19 C14 C1 121.3(3) . . ? C16 C15 C14 120.2(3) . . ? C15 C16 C17 119.2(3) . . ? C18 C17 C16 121.1(3) . . ? C17 C18 C19 120.7(3) . . ? C14 C19 C18 118.3(3) . . ? C14 C19 C20 121.7(3) . . ? C18 C19 C20 119.8(3) . . ? C21 C20 C25 118.4(3) . . ? C21 C20 C19 118.7(3) . . ? C25 C20 C19 122.8(3) . . ? C20 C21 C22 121.0(5) . . ? C23 C22 C21 119.8(5) . . ? C22 C23 C24 119.9(4) . . ? C23 C24 C25 121.3(5) . . ? C24 C25 C20 119.5(4) . . ? C24 C25 C26 118.4(4) . . ? C20 C25 C26 122.1(3) . . ? O7 C26 O8 120.3(4) . . ? O7 C26 C25 124.0(4) . . ? O8 C26 C25 115.7(3) . . ? C28 C27 C32 119.7(3) . . ? C28 C27 C3 119.1(3) . . ? C32 C27 C3 121.1(3) . . ? C27 C28 C29 121.2(4) . . ? C28 C29 C30 120.2(4) . . ? C29 C30 C31 119.4(4) . . ? C32 C31 C30 121.4(4) . . ? C31 C32 C27 118.1(3) . . ? C31 C32 C33 119.7(3) . . ? C27 C32 C33 122.2(3) . . ? C34 C33 C38 117.6(3) . . ? C34 C33 C32 119.1(3) . . ? C38 C33 C32 123.3(3) . . ? C35 C34 C33 121.9(3) . . ? C34 C35 C36 120.2(3) . . ? C37 C36 C35 118.7(4) . . ? C36 C37 C38 121.2(3) . . ? C37 C38 C33 120.4(3) . . ? C37 C38 C2 117.4(3) . . ? C33 C38 C2 122.2(3) . . ? C4 N1 C8 118.7(3) . . ? C4 N1 In1 122.9(2) . . ? C8 N1 In1 118.4(2) . . ? C9 N2 C13 119.9(3) . . ? C9 N2 In1 117.8(2) . . ? C13 N2 In1 122.3(2) . . ? C1 O1 In1 86.84(19) . . ? C1 O2 In1 97.3(2) . . ? C2 O3 In1 89.3(2) . 3_656 ? C2 O4 In1 93.93(19) . 3_656 ? C3 O5 In1 97.2(2) . . ? C3 O6 In1 87.5(2) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.764 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.061 # Attachment '- mostuptodate_In_Compound4.cif' #============================================================================== data_InCompound4 _database_code_depnum_ccdc_archive 'CCDC 812724' #TrackingRef '- mostuptodate_In_Compound4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H54 In2 N4 O18' _chemical_formula_weight 1540.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9495(6) _cell_length_b 13.0898(8) _cell_length_c 13.2297(8) _cell_angle_alpha 82.543(1) _cell_angle_beta 85.472(1) _cell_angle_gamma 80.571(1) _cell_volume 1682.4(2) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 5692 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 25.09 _exptl_crystal_description cubic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 0.763 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8035 _exptl_absorpt_correction_T_max 0.8624 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13615 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0586 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 26.37 _reflns_number_total 6578 _reflns_number_gt 5157 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; We have added two restrains to fix two hydrogen atoms in the water solvent molecule 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^)+(0.0393P)^2^+0.3725P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6578 _refine_ls_number_parameters 460 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0922 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.008 _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 0.36952(2) 0.729066(19) 0.449200(18) 0.03720(9) Uani 1 1 d . . . C1 C 0.2088(4) 0.8840(3) 0.3452(3) 0.0394(8) Uani 1 1 d . . . C2 C 0.3272(4) 0.5819(3) 0.3415(3) 0.0431(8) Uani 1 1 d . . . C3 C 0.6578(4) 0.3754(3) 0.3669(3) 0.0423(8) Uani 1 1 d . . . C4 C 0.3239(4) 0.9074(3) 0.6003(3) 0.0485(9) Uani 1 1 d . . . H4 H 0.2330 0.9081 0.5882 0.058 Uiso 1 1 calc R . . C5 C 0.3531(5) 0.9626(3) 0.6753(3) 0.0591(11) Uani 1 1 d . . . H5 H 0.2835 0.9993 0.7135 0.071 Uiso 1 1 calc R . . C6 C 0.4875(5) 0.9620(3) 0.6923(3) 0.0647(12) Uani 1 1 d . . . H6 H 0.5109 0.9980 0.7429 0.078 Uiso 1 1 calc R . . C7 C 0.5873(4) 0.9072(3) 0.6331(3) 0.0571(10) Uani 1 1 d . . . H7 H 0.6788 0.9063 0.6435 0.068 Uiso 1 1 calc R . . C8 C 0.5521(3) 0.8538(3) 0.5589(3) 0.0418(8) Uani 1 1 d . . . C9 C 0.6543(4) 0.7931(3) 0.4929(3) 0.0445(9) Uani 1 1 d . . . C10 C 0.7933(4) 0.7899(3) 0.4965(3) 0.0652(12) Uani 1 1 d . . . H10 H 0.8266 0.8275 0.5414 0.078 Uiso 1 1 calc R . . C11 C 0.8828(4) 0.7312(4) 0.4338(4) 0.0772(14) Uani 1 1 d . . . H11 H 0.9765 0.7283 0.4361 0.093 Uiso 1 1 calc R . . C12 C 0.8316(4) 0.6777(4) 0.3688(4) 0.0802(15) Uani 1 1 d . . . H12 H 0.8897 0.6381 0.3250 0.096 Uiso 1 1 calc R . . C13 C 0.6925(4) 0.6828(3) 0.3682(3) 0.0654(12) Uani 1 1 d . . . H13 H 0.6581 0.6451 0.3240 0.079 Uiso 1 1 calc R . . C14 C 0.1240(3) 0.9727(3) 0.2857(3) 0.0363(8) Uani 1 1 d . . . C15 C 0.0533(3) 1.0505(3) 0.3407(3) 0.0474(9) Uani 1 1 d . . . H15 H 0.0526 1.0410 0.4116 0.057 Uiso 1 1 calc R . . C16 C -0.0157(4) 1.1413(3) 0.2922(3) 0.0546(10) Uani 1 1 d . . . H16 H -0.0592 1.1939 0.3298 0.066 Uiso 1 1 calc R . . C17 C -0.0195(4) 1.1533(3) 0.1883(4) 0.0608(11) Uani 1 1 d . . . H17 H -0.0653 1.2145 0.1551 0.073 Uiso 1 1 calc R . . C18 C 0.0439(4) 1.0755(3) 0.1324(3) 0.0544(10) Uani 1 1 d . . . H18 H 0.0375 1.0840 0.0620 0.065 Uiso 1 1 calc R . . C19 C 0.1176(3) 0.9842(3) 0.1795(3) 0.0409(8) Uani 1 1 d . . . C20 C 0.1781(4) 0.8991(3) 0.1175(3) 0.0469(9) Uani 1 1 d . . . C21 C 0.1409(5) 0.8015(3) 0.1398(3) 0.0614(11) Uani 1 1 d . . . H21 H 0.0824 0.7882 0.1967 0.074 Uiso 1 1 calc R . . C22 C 0.1889(5) 0.7216(4) 0.0788(4) 0.0725(13) Uani 1 1 d . . . H22 H 0.1636 0.6559 0.0955 0.087 Uiso 1 1 calc R . . C23 C 0.2729(5) 0.7415(4) -0.0049(4) 0.0701(13) Uani 1 1 d . . . H23 H 0.3061 0.6885 -0.0450 0.084 Uiso 1 1 calc R . . C24 C 0.3100(4) 0.8397(4) -0.0316(3) 0.0658(12) Uani 1 1 d . . . H24 H 0.3645 0.8532 -0.0907 0.079 Uiso 1 1 calc R . . C25 C 0.2650(4) 0.9178(3) 0.0307(3) 0.0526(10) Uani 1 1 d . . . C26 C 0.3195(4) 1.0194(3) 0.0069(3) 0.0575(10) Uani 1 1 d . . . C27 C 0.3132(3) 0.4896(3) 0.2890(3) 0.0431(9) Uani 1 1 d . . . C28 C 0.1912(4) 0.4512(3) 0.3042(3) 0.0599(11) Uani 1 1 d . . . H28 H 0.1203 0.4847 0.3438 0.072 Uiso 1 1 calc R . . C29 C 0.1723(4) 0.3641(3) 0.2622(4) 0.0722(13) Uani 1 1 d . . . H29 H 0.0889 0.3399 0.2724 0.087 Uiso 1 1 calc R . . C30 C 0.2773(5) 0.3129(3) 0.2050(3) 0.0667(12) Uani 1 1 d . . . H30 H 0.2657 0.2536 0.1768 0.080 Uiso 1 1 calc R . . C31 C 0.3990(4) 0.3502(3) 0.1899(3) 0.0568(10) Uani 1 1 d . . . H31 H 0.4698 0.3151 0.1513 0.068 Uiso 1 1 calc R . . C32 C 0.4203(4) 0.4390(3) 0.2305(3) 0.0419(8) Uani 1 1 d . . . C33 C 0.6688(3) 0.4370(3) 0.2644(3) 0.0416(8) Uani 1 1 d . . . C34 C 0.5558(4) 0.4727(3) 0.2050(3) 0.0419(8) Uani 1 1 d . . . C35 C 0.5768(4) 0.5338(3) 0.1122(3) 0.0588(11) Uani 1 1 d . . . H35 H 0.5036 0.5587 0.0716 0.071 Uiso 1 1 calc R . . C36 C 0.7046(6) 0.5580(4) 0.0797(4) 0.0800(15) Uani 1 1 d . . . H36 H 0.7161 0.5999 0.0183 0.096 Uiso 1 1 calc R . . C37 C 0.8141(5) 0.5206(4) 0.1376(4) 0.0764(14) Uani 1 1 d . . . H37 H 0.9003 0.5359 0.1150 0.092 Uiso 1 1 calc R . . C38 C 0.7962(4) 0.4606(3) 0.2288(3) 0.0604(11) Uani 1 1 d . . . H38 H 0.8710 0.4352 0.2677 0.072 Uiso 1 1 calc R . . O1 O 0.1667(2) 0.84915(19) 0.43179(18) 0.0502(6) Uani 1 1 d . . . O2 O 0.3271(2) 0.84741(18) 0.30939(18) 0.0442(6) Uani 1 1 d . . . O3 O 0.4363(2) 0.61907(19) 0.33109(19) 0.0488(6) Uani 1 1 d . . . O4 O 0.2325(3) 0.6201(2) 0.3986(2) 0.0767(9) Uani 1 1 d . . . O5 O 0.5482(3) 0.3858(2) 0.42124(18) 0.0520(7) Uani 1 1 d . . . O6 O 0.7593(3) 0.31315(19) 0.3988(2) 0.0559(7) Uani 1 1 d . . . O7 O 0.3593(3) 1.0639(3) 0.0688(2) 0.0766(9) Uani 1 1 d . . . O8 O 0.3204(3) 1.0536(3) -0.0930(2) 0.0757(9) Uani 1 1 d . . . H8 H 0.3691 1.0990 -0.1056 0.114 Uiso 1 1 calc R . . N1 N 0.4203(3) 0.8529(2) 0.5439(2) 0.0386(7) Uani 1 1 d . . . N2 N 0.6049(3) 0.7394(2) 0.4285(2) 0.0451(7) Uani 1 1 d . . . O9 O 0.5356(4) 0.7956(3) 0.1572(3) 0.0822(9) Uani 1 1 d D . . H91 H 0.580(11) 0.720(3) 0.164(9) 0.36(7) Uiso 1 1 d D . . H92 H 0.458(5) 0.810(6) 0.207(5) 0.21(4) Uiso 1 1 d 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 0.03081(14) 0.04138(15) 0.03987(15) -0.00977(10) -0.00123(10) -0.00344(10) C1 0.045(2) 0.0353(19) 0.042(2) -0.0080(16) -0.0100(17) -0.0127(16) C2 0.042(2) 0.037(2) 0.050(2) -0.0092(17) -0.0046(17) -0.0024(17) C3 0.043(2) 0.037(2) 0.047(2) -0.0100(17) -0.0084(18) -0.0007(16) C4 0.048(2) 0.054(2) 0.047(2) -0.0191(19) 0.0047(18) -0.0109(18) C5 0.070(3) 0.059(3) 0.052(2) -0.022(2) 0.013(2) -0.016(2) C6 0.081(3) 0.070(3) 0.056(3) -0.028(2) 0.002(2) -0.036(3) C7 0.054(2) 0.068(3) 0.058(2) -0.022(2) -0.005(2) -0.025(2) C8 0.040(2) 0.043(2) 0.045(2) -0.0056(16) -0.0019(16) -0.0147(16) C9 0.039(2) 0.046(2) 0.051(2) -0.0049(18) -0.0021(17) -0.0119(17) C10 0.043(2) 0.078(3) 0.083(3) -0.025(3) -0.008(2) -0.020(2) C11 0.033(2) 0.092(4) 0.111(4) -0.029(3) -0.001(3) -0.012(2) C12 0.035(2) 0.105(4) 0.108(4) -0.049(3) 0.013(2) -0.013(2) C13 0.035(2) 0.083(3) 0.085(3) -0.044(3) 0.010(2) -0.008(2) C14 0.0276(17) 0.0369(19) 0.045(2) -0.0062(16) -0.0018(15) -0.0071(14) C15 0.037(2) 0.051(2) 0.056(2) -0.0138(19) 0.0052(17) -0.0127(18) C16 0.038(2) 0.044(2) 0.083(3) -0.017(2) 0.007(2) -0.0047(18) C17 0.045(2) 0.047(2) 0.086(3) 0.000(2) -0.014(2) 0.0053(19) C18 0.054(2) 0.058(3) 0.050(2) -0.002(2) -0.0127(19) -0.003(2) C19 0.0362(19) 0.042(2) 0.044(2) -0.0063(17) -0.0063(16) -0.0027(16) C20 0.050(2) 0.051(2) 0.040(2) -0.0083(18) -0.0140(18) -0.0015(18) C21 0.075(3) 0.058(3) 0.052(2) -0.010(2) -0.008(2) -0.007(2) C22 0.090(4) 0.056(3) 0.073(3) -0.014(2) -0.020(3) -0.004(3) C23 0.082(3) 0.061(3) 0.067(3) -0.026(2) -0.014(3) 0.009(2) C24 0.069(3) 0.073(3) 0.055(3) -0.021(2) -0.004(2) 0.000(2) C25 0.056(2) 0.060(3) 0.043(2) -0.0135(19) -0.0105(19) -0.004(2) C26 0.051(2) 0.072(3) 0.049(2) -0.013(2) 0.003(2) -0.006(2) C27 0.041(2) 0.0359(19) 0.054(2) -0.0094(17) -0.0130(17) -0.0012(16) C28 0.040(2) 0.047(2) 0.097(3) -0.022(2) -0.005(2) -0.0048(18) C29 0.051(3) 0.057(3) 0.115(4) -0.020(3) -0.021(3) -0.015(2) C30 0.076(3) 0.042(2) 0.089(3) -0.021(2) -0.029(3) -0.009(2) C31 0.061(3) 0.048(2) 0.063(3) -0.022(2) -0.010(2) 0.000(2) C32 0.044(2) 0.038(2) 0.043(2) -0.0071(16) -0.0123(16) -0.0003(16) C33 0.039(2) 0.040(2) 0.043(2) -0.0064(16) 0.0031(16) 0.0012(16) C34 0.047(2) 0.039(2) 0.040(2) -0.0123(16) -0.0003(16) -0.0019(16) C35 0.070(3) 0.059(3) 0.044(2) 0.001(2) -0.010(2) -0.001(2) C36 0.092(4) 0.085(4) 0.057(3) 0.006(3) 0.016(3) -0.018(3) C37 0.058(3) 0.087(4) 0.079(3) -0.006(3) 0.022(3) -0.012(3) C38 0.043(2) 0.071(3) 0.062(3) -0.008(2) 0.005(2) -0.001(2) O1 0.0501(15) 0.0595(17) 0.0403(14) 0.0009(13) -0.0043(12) -0.0113(13) O2 0.0395(14) 0.0424(14) 0.0484(14) -0.0054(11) -0.0036(11) 0.0005(11) O3 0.0383(14) 0.0466(15) 0.0649(16) -0.0190(12) -0.0068(12) -0.0051(12) O4 0.0580(19) 0.077(2) 0.104(2) -0.0496(19) 0.0290(17) -0.0220(16) O5 0.0461(15) 0.0587(17) 0.0445(14) -0.0010(12) -0.0004(12) 0.0067(13) O6 0.0476(16) 0.0475(15) 0.0658(17) 0.0025(13) -0.0090(13) 0.0081(13) O7 0.085(2) 0.098(2) 0.0568(18) -0.0226(17) -0.0018(16) -0.0337(19) O8 0.086(2) 0.089(3) 0.0540(18) -0.0095(16) 0.0064(16) -0.0236(18) N1 0.0391(16) 0.0396(16) 0.0371(15) -0.0075(13) 0.0011(13) -0.0058(13) N2 0.0323(16) 0.0534(19) 0.0533(18) -0.0180(15) -0.0002(14) -0.0091(14) O9 0.081(2) 0.081(2) 0.079(2) -0.0016(19) 0.0145(19) -0.0109(19) _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 O5 2.240(2) 2_666 ? In1 O3 2.250(2) . ? In1 O2 2.273(2) . ? In1 N1 2.313(3) . ? In1 O4 2.317(3) . ? In1 O6 2.351(3) 2_666 ? In1 O1 2.353(2) . ? In1 N2 2.360(3) . ? In1 C2 2.645(4) . ? In1 C3 2.649(4) 2_666 ? In1 C1 2.669(3) . ? C1 O1 1.244(4) . ? C1 O2 1.275(4) . ? C1 C14 1.492(5) . ? C2 O4 1.241(4) . ? C2 O3 1.251(4) . ? C2 C27 1.499(5) . ? C3 O5 1.256(4) . ? C3 O6 1.254(4) . ? C3 C33 1.490(5) . ? C3 In1 2.649(4) 2_666 ? C4 N1 1.336(4) . ? C4 C5 1.375(5) . ? C4 H4 0.9300 . ? C5 C6 1.372(6) . ? C5 H5 0.9300 . ? C6 C7 1.381(6) . ? C6 H6 0.9300 . ? C7 C8 1.373(5) . ? C7 H7 0.9300 . ? C8 N1 1.344(4) . ? C8 C9 1.484(5) . ? C9 N2 1.340(4) . ? C9 C10 1.382(5) . ? C10 C11 1.377(6) . ? C10 H10 0.9300 . ? C11 C12 1.354(6) . ? C11 H11 0.9300 . ? C12 C13 1.375(5) . ? C12 H12 0.9300 . ? C13 N2 1.333(4) . ? C13 H13 0.9300 . ? C14 C15 1.392(5) . ? C14 C19 1.399(5) . ? C15 C16 1.379(5) . ? C15 H15 0.9300 . ? C16 C17 1.365(6) . ? C16 H16 0.9300 . ? C17 C18 1.375(5) . ? C17 H17 0.9300 . ? C18 C19 1.395(5) . ? C18 H18 0.9300 . ? C19 C20 1.490(5) . ? C20 C21 1.377(5) . ? C20 C25 1.401(5) . ? C21 C22 1.403(6) . ? C21 H21 0.9300 . ? C22 C23 1.357(6) . ? C22 H22 0.9300 . ? C23 C24 1.390(6) . ? C23 H23 0.9300 . ? C24 C25 1.392(5) . ? C24 H24 0.9300 . ? C25 C26 1.503(6) . ? C26 O7 1.191(5) . ? C26 O8 1.339(5) . ? C27 C28 1.379(5) . ? C27 C32 1.395(5) . ? C28 C29 1.377(5) . ? C28 H28 0.9300 . ? C29 C30 1.374(6) . ? C29 H29 0.9300 . ? C30 C31 1.369(6) . ? C30 H30 0.9300 . ? C31 C32 1.395(5) . ? C31 H31 0.9300 . ? C32 C34 1.487(5) . ? C33 C38 1.386(5) . ? C33 C34 1.404(5) . ? C34 C35 1.396(5) . ? C35 C36 1.382(6) . ? C35 H35 0.9300 . ? C36 C37 1.369(6) . ? C36 H36 0.9300 . ? C37 C38 1.367(6) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? O5 In1 2.240(2) 2_666 ? O6 In1 2.351(3) 2_666 ? O8 H8 0.8200 . ? O9 H91 1.01(2) . ? O9 H92 0.98(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 In1 O3 94.01(9) 2_666 . ? O5 In1 O2 169.44(8) 2_666 . ? O3 In1 O2 82.88(9) . . ? O5 In1 N1 84.66(10) 2_666 . ? O3 In1 N1 148.95(9) . . ? O2 In1 N1 92.80(9) . . ? O5 In1 O4 94.30(11) 2_666 . ? O3 In1 O4 56.09(9) . . ? O2 In1 O4 92.32(11) . . ? N1 In1 O4 154.95(10) . . ? O5 In1 O6 56.45(8) 2_666 2_666 ? O3 In1 O6 123.96(9) . 2_666 ? O2 In1 O6 133.29(8) . 2_666 ? N1 In1 O6 80.74(9) . 2_666 ? O4 In1 O6 77.94(10) . 2_666 ? O5 In1 O1 133.02(8) 2_666 . ? O3 In1 O1 119.86(8) . . ? O2 In1 O1 56.25(8) . . ? N1 In1 O1 81.20(9) . . ? O4 In1 O1 81.35(10) . . ? O6 In1 O1 77.08(8) 2_666 . ? O5 In1 N2 78.36(10) 2_666 . ? O3 In1 N2 79.46(9) . . ? O2 In1 N2 91.14(9) . . ? N1 In1 N2 69.87(10) . . ? O4 In1 N2 134.51(10) . . ? O6 In1 N2 127.97(10) 2_666 . ? O1 In1 N2 135.33(9) . . ? O5 In1 C2 93.32(10) 2_666 . ? O3 In1 C2 28.17(9) . . ? O2 In1 C2 88.67(10) . . ? N1 In1 C2 176.47(10) . . ? O4 In1 C2 27.98(10) . . ? O6 In1 C2 100.58(10) 2_666 . ? O1 In1 C2 102.27(10) . . ? N2 In1 C2 106.91(11) . . ? O5 In1 C3 28.21(9) 2_666 2_666 ? O3 In1 C3 110.79(10) . 2_666 ? O2 In1 C3 161.30(10) . 2_666 ? N1 In1 C3 81.83(10) . 2_666 ? O4 In1 C3 85.53(11) . 2_666 ? O6 In1 C3 28.25(9) 2_666 2_666 ? O1 In1 C3 105.12(10) . 2_666 ? N2 In1 C3 103.61(11) . 2_666 ? C2 In1 C3 97.76(11) . 2_666 ? O5 In1 C1 160.51(10) 2_666 . ? O3 In1 C1 102.16(10) . . ? O2 In1 C1 28.48(9) . . ? N1 In1 C1 86.96(10) . . ? O4 In1 C1 85.93(11) . . ? O6 In1 C1 104.81(10) 2_666 . ? O1 In1 C1 27.77(9) . . ? N2 In1 C1 115.03(10) . . ? C2 In1 C1 95.83(10) . . ? C3 In1 C1 132.88(11) 2_666 . ? O1 C1 O2 120.0(3) . . ? O1 C1 C14 119.9(3) . . ? O2 C1 C14 120.0(3) . . ? O1 C1 In1 61.81(18) . . ? O2 C1 In1 58.22(17) . . ? C14 C1 In1 177.7(2) . . ? O4 C2 O3 119.1(3) . . ? O4 C2 C27 120.4(3) . . ? O3 C2 C27 120.4(3) . . ? O4 C2 In1 61.2(2) . . ? O3 C2 In1 58.11(18) . . ? C27 C2 In1 173.3(2) . . ? O5 C3 O6 120.0(3) . . ? O5 C3 C33 120.6(3) . . ? O6 C3 C33 119.4(3) . . ? O5 C3 In1 57.48(18) . 2_666 ? O6 C3 In1 62.56(19) . 2_666 ? C33 C3 In1 177.9(3) . 2_666 ? N1 C4 C5 123.0(4) . . ? N1 C4 H4 118.5 . . ? C5 C4 H4 118.5 . . ? C6 C5 C4 118.3(4) . . ? C6 C5 H5 120.9 . . ? C4 C5 H5 120.9 . . ? C5 C6 C7 118.8(4) . . ? C5 C6 H6 120.6 . . ? C7 C6 H6 120.6 . . ? C8 C7 C6 120.4(4) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? N1 C8 C7 120.6(3) . . ? N1 C8 C9 116.3(3) . . ? C7 C8 C9 123.1(3) . . ? N2 C9 C10 120.6(4) . . ? N2 C9 C8 116.3(3) . . ? C10 C9 C8 123.0(3) . . ? C11 C10 C9 120.2(4) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C12 C11 C10 118.7(4) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? C11 C12 C13 119.1(4) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? N2 C13 C12 122.8(4) . . ? N2 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? C15 C14 C19 119.2(3) . . ? C15 C14 C1 116.6(3) . . ? C19 C14 C1 124.2(3) . . ? C16 C15 C14 121.4(4) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C17 C16 C15 119.2(4) . . ? C17 C16 H16 120.4 . . ? C15 C16 H16 120.4 . . ? C16 C17 C18 120.6(4) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C17 C18 C19 121.2(4) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C18 C19 C14 118.3(3) . . ? C18 C19 C20 119.7(3) . . ? C14 C19 C20 121.8(3) . . ? C21 C20 C25 118.3(4) . . ? C21 C20 C19 120.2(3) . . ? C25 C20 C19 121.3(3) . . ? C20 C21 C22 121.6(4) . . ? C20 C21 H21 119.2 . . ? C22 C21 H21 119.2 . . ? C23 C22 C21 119.1(4) . . ? C23 C22 H22 120.5 . . ? C21 C22 H22 120.5 . . ? C22 C23 C24 121.1(4) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C23 C24 C25 119.5(4) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C24 C25 C20 120.3(4) . . ? C24 C25 C26 118.4(4) . . ? C20 C25 C26 121.1(3) . . ? O7 C26 O8 123.5(4) . . ? O7 C26 C25 124.4(4) . . ? O8 C26 C25 112.1(4) . . ? C28 C27 C32 119.5(3) . . ? C28 C27 C2 117.9(3) . . ? C32 C27 C2 122.5(3) . . ? C29 C28 C27 121.4(4) . . ? C29 C28 H28 119.3 . . ? C27 C28 H28 119.3 . . ? C30 C29 C28 119.8(4) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C31 C30 C29 119.3(4) . . ? C31 C30 H30 120.4 . . ? C29 C30 H30 120.4 . . ? C30 C31 C32 122.1(4) . . ? C30 C31 H31 118.9 . . ? C32 C31 H31 118.9 . . ? C27 C32 C31 117.9(3) . . ? C27 C32 C34 125.7(3) . . ? C31 C32 C34 116.4(3) . . ? C38 C33 C34 119.8(3) . . ? C38 C33 C3 117.6(3) . . ? C34 C33 C3 122.6(3) . . ? C35 C34 C33 117.8(3) . . ? C35 C34 C32 118.8(3) . . ? C33 C34 C32 123.1(3) . . ? C36 C35 C34 121.2(4) . . ? C36 C35 H35 119.4 . . ? C34 C35 H35 119.4 . . ? C37 C36 C35 120.3(4) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 C38 119.7(4) . . ? C36 C37 H37 120.2 . . ? C38 C37 H37 120.2 . . ? C37 C38 C33 121.3(4) . . ? C37 C38 H38 119.3 . . ? C33 C38 H38 119.3 . . ? C1 O1 In1 90.4(2) . . ? C1 O2 In1 93.3(2) . . ? C2 O3 In1 93.7(2) . . ? C2 O4 In1 90.8(2) . . ? C3 O5 In1 94.3(2) . 2_666 ? C3 O6 In1 89.2(2) . 2_666 ? C26 O8 H8 109.5 . . ? C4 N1 C8 118.9(3) . . ? C4 N1 In1 121.6(2) . . ? C8 N1 In1 118.0(2) . . ? C13 N2 C9 118.7(3) . . ? C13 N2 In1 123.6(2) . . ? C9 N2 In1 116.9(2) . . ? H91 O9 H92 113(7) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.643 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.071 #============================================================================== # Attachment '- mostuptodate_In_Compound5.cif' data_InCompound5 _database_code_depnum_ccdc_archive 'CCDC 812725' #TrackingRef '- mostuptodate_In_Compound5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H50 In2 N4 O16' _chemical_formula_weight 1504.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6135(12) _cell_length_b 11.6513(13) _cell_length_c 14.0949(15) _cell_angle_alpha 75.745(2) _cell_angle_beta 68.609(2) _cell_angle_gamma 88.736(2) _cell_volume 1568.5(3) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 4275 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 24.85 _exptl_crystal_description cubic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 0.814 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.783 _exptl_absorpt_correction_T_max 0.850 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13544 _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_av_sigmaI/netI 0.1023 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 28.85 _reflns_number_total 7022 _reflns_number_gt 5143 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; After meassuring different crystals, we can conclude that all of them diffract poorly, it seems to be something inherent to these crystals. For this reason the data have less completeness than the usual and the alert _diffrn_measured_fraction_theta_full Low ....... 0.85 is also due to this reason. 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^)+(0.0315P)^2^+1.9901P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7022 _refine_ls_number_parameters 542 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1009 _refine_ls_R_factor_gt 0.0652 _refine_ls_wR_factor_ref 0.1072 _refine_ls_wR_factor_gt 0.0979 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 0.22851(3) 0.56952(3) 0.64388(3) 0.02463(11) Uani 1 1 d . . . C1 C 0.1049(5) 0.7193(4) 0.7938(4) 0.0336(12) Uani 1 1 d . . . C2 C 0.5130(5) 0.3283(5) 0.4004(4) 0.0351(12) Uani 1 1 d . . . C3 C 0.3068(4) 0.3539(4) 0.6631(4) 0.0277(10) Uani 1 1 d . . . C4 C 0.2290(5) 0.7381(5) 0.4270(4) 0.0379(13) Uani 1 1 d . . . H4 H 0.310(5) 0.747(4) 0.417(4) 0.045(16) Uiso 1 1 d . . . C5 C 0.1793(6) 0.7948(5) 0.3522(4) 0.0419(14) Uani 1 1 d . . . H5 H 0.237(5) 0.843(5) 0.294(4) 0.047(16) Uiso 1 1 d . . . C6 C 0.0461(5) 0.7713(5) 0.3683(4) 0.0394(13) Uani 1 1 d . . . H6 H 0.013(4) 0.808(4) 0.323(3) 0.023(12) Uiso 1 1 d . . . C7 C -0.0341(5) 0.6911(5) 0.4585(4) 0.0352(12) Uani 1 1 d . . . H7 H -0.126(4) 0.679(4) 0.473(3) 0.020(11) Uiso 1 1 d . . . C8 C 0.0199(4) 0.6365(4) 0.5323(3) 0.0260(10) Uani 1 1 d . . . C9 C -0.0629(4) 0.5522(4) 0.6332(4) 0.0272(10) Uani 1 1 d . . . C10 C -0.1980(5) 0.5198(5) 0.6608(4) 0.0376(12) Uani 1 1 d . . . H10 H -0.246(4) 0.549(4) 0.616(3) 0.025(12) Uiso 1 1 d . . . C11 C -0.2675(6) 0.4447(6) 0.7586(5) 0.0512(16) Uani 1 1 d . . . H11 H -0.356(6) 0.433(5) 0.778(4) 0.053(17) Uiso 1 1 d . . . C12 C -0.2008(6) 0.4017(5) 0.8256(5) 0.0513(15) Uani 1 1 d . . . H12 H -0.248(6) 0.351(6) 0.894(5) 0.08(2) Uiso 1 1 d . . . C13 C -0.0656(5) 0.4342(5) 0.7935(4) 0.0407(13) Uani 1 1 d . . . H13 H -0.010(4) 0.410(4) 0.830(3) 0.023(12) Uiso 1 1 d . . . C14 C 0.0948(5) 0.7674(4) 0.8853(4) 0.0291(11) Uani 1 1 d . . . C15 C 0.2122(6) 0.8106(5) 0.8908(4) 0.0409(13) Uani 1 1 d . . . H15 H 0.295(4) 0.798(3) 0.846(3) 0.015(11) Uiso 1 1 d . . . C16 C 0.2066(6) 0.8623(5) 0.9698(5) 0.0454(14) Uani 1 1 d . . . H16 H 0.281(5) 0.895(4) 0.973(4) 0.037(14) Uiso 1 1 d . . . C17 C 0.0824(6) 0.8698(5) 1.0445(4) 0.0395(13) Uani 1 1 d . . . H17 H 0.075(4) 0.899(4) 1.099(3) 0.020(11) Uiso 1 1 d . . . C18 C -0.0357(6) 0.8266(4) 1.0417(4) 0.0341(12) Uani 1 1 d . . . H18 H -0.119(4) 0.834(4) 1.095(3) 0.019(11) Uiso 1 1 d . . . C19 C -0.0317(5) 0.7747(4) 0.9621(3) 0.0248(10) Uani 1 1 d . . . C20 C -0.1609(5) 0.7229(4) 0.9658(3) 0.0273(10) Uani 1 1 d . . . C21 C -0.2050(6) 0.6055(5) 1.0251(4) 0.0364(12) Uani 1 1 d . . . H21 H -0.138(4) 0.560(4) 1.048(3) 0.027(12) Uiso 1 1 d . . . C22 C -0.3312(7) 0.5602(6) 1.0418(5) 0.0551(18) Uani 1 1 d . . . H22 H -0.351(4) 0.495(4) 1.078(3) 0.019(13) Uiso 1 1 d . . . C23 C -0.4180(6) 0.6265(6) 1.0039(5) 0.0541(17) Uani 1 1 d . . . H23 H -0.506(6) 0.602(5) 1.014(4) 0.067(19) Uiso 1 1 d . . . C24 C -0.3778(6) 0.7421(6) 0.9455(5) 0.0453(14) Uani 1 1 d . . . H24 H -0.434(5) 0.788(4) 0.928(3) 0.026(13) Uiso 1 1 d . . . C25 C -0.2494(5) 0.7898(4) 0.9257(4) 0.0347(12) Uani 1 1 d . . . C26 C -0.2126(6) 0.9166(5) 0.8620(4) 0.0371(13) Uani 1 1 d . . . C27 C 0.3984(5) 0.2345(4) 0.4379(4) 0.0330(12) Uani 1 1 d . . . C28 C 0.3435(6) 0.2223(6) 0.3646(5) 0.0427(14) Uani 1 1 d . . . C29 C 0.2433(7) 0.1353(7) 0.3894(6) 0.0592(19) Uani 1 1 d . . . H29 H 0.380(5) 0.277(4) 0.300(4) 0.036(15) Uiso 1 1 d . . . C30 C 0.1962(7) 0.0585(7) 0.4859(7) 0.063(2) Uani 1 1 d . . . H30 H 0.216(5) 0.126(5) 0.338(4) 0.051(16) Uiso 1 1 d . . . C31 C 0.2463(6) 0.0694(6) 0.5615(6) 0.0474(15) Uani 1 1 d . . . H31 H 0.128(6) 0.003(5) 0.509(5) 0.07(2) Uiso 1 1 d . . . C32 C 0.3476(5) 0.1575(4) 0.5399(4) 0.0331(11) Uani 1 1 d . . . H32 H 0.221(6) 0.025(5) 0.620(4) 0.06(2) Uiso 1 1 d . . . C33 C 0.3718(4) 0.2414(4) 0.6856(3) 0.0264(10) Uani 1 1 d . . . C34 C 0.3974(4) 0.1563(4) 0.6264(4) 0.0282(11) Uani 1 1 d . . . C35 C 0.4598(5) 0.0563(5) 0.6581(5) 0.0390(13) Uani 1 1 d . . . H35 H 0.474(5) 0.002(4) 0.623(4) 0.039(15) Uiso 1 1 d . . . C36 C 0.4987(5) 0.0398(5) 0.7438(4) 0.0414(13) Uani 1 1 d . . . H36 H 0.543(5) -0.030(4) 0.758(4) 0.043(14) Uiso 1 1 d . . . C37 C 0.4714(5) 0.1219(5) 0.8022(4) 0.0394(13) Uani 1 1 d . . . H37 H 0.495(4) 0.108(4) 0.862(3) 0.024(12) Uiso 1 1 d . . . C38 C 0.4098(5) 0.2215(4) 0.7728(4) 0.0317(11) Uani 1 1 d . . . H38 H 0.393(4) 0.279(4) 0.813(3) 0.026(12) Uiso 1 1 d . . . O1 O 0.1839(3) 0.6353(3) 0.7793(3) 0.0414(9) Uani 1 1 d . . . O2 O 0.0408(4) 0.7614(3) 0.7370(3) 0.0451(9) Uani 1 1 d . . . O3 O 0.6030(3) 0.3050(3) 0.4438(3) 0.0377(8) Uani 1 1 d . . . O4 O 0.5225(4) 0.4184(4) 0.3311(3) 0.0532(10) Uani 1 1 d . . . O5 O 0.2440(3) 0.3962(3) 0.7409(3) 0.0365(8) Uani 1 1 d . . . O6 O 0.3153(3) 0.4109(3) 0.5719(2) 0.0337(8) Uani 1 1 d . . . O7 O -0.2906(4) 0.9935(3) 0.8785(3) 0.0524(10) Uani 1 1 d . . . O8 O -0.0935(4) 0.9427(3) 0.7839(3) 0.0427(9) Uani 1 1 d . . . H8 H -0.048(6) 0.888(5) 0.767(4) 0.05(2) Uiso 1 1 d . . . N1 N 0.1514(4) 0.6597(3) 0.5162(3) 0.0279(9) Uani 1 1 d . . . N2 N 0.0029(4) 0.5085(3) 0.6991(3) 0.0297(9) 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 0.02443(18) 0.02629(19) 0.02396(17) -0.00645(13) -0.01011(13) 0.00615(13) C1 0.036(3) 0.030(3) 0.028(3) -0.005(2) -0.005(2) -0.009(2) C2 0.034(3) 0.043(3) 0.030(3) -0.016(3) -0.010(2) 0.011(2) C3 0.020(2) 0.029(3) 0.037(3) -0.012(2) -0.012(2) 0.001(2) C4 0.021(3) 0.048(3) 0.036(3) 0.004(2) -0.011(2) -0.003(3) C5 0.039(3) 0.043(3) 0.035(3) 0.005(3) -0.014(3) 0.003(3) C6 0.040(3) 0.047(3) 0.034(3) -0.002(3) -0.022(3) 0.011(3) C7 0.025(3) 0.047(3) 0.038(3) -0.012(3) -0.016(2) 0.012(2) C8 0.027(3) 0.025(3) 0.028(3) -0.010(2) -0.011(2) 0.007(2) C9 0.025(3) 0.028(3) 0.030(3) -0.010(2) -0.011(2) 0.004(2) C10 0.029(3) 0.036(3) 0.044(3) -0.007(3) -0.011(3) 0.004(2) C11 0.027(3) 0.060(4) 0.055(4) -0.009(3) -0.006(3) 0.000(3) C12 0.042(4) 0.051(4) 0.040(3) 0.007(3) -0.004(3) -0.006(3) C13 0.035(3) 0.046(3) 0.036(3) -0.002(3) -0.012(3) 0.001(3) C14 0.033(3) 0.022(3) 0.034(3) -0.008(2) -0.014(2) 0.004(2) C15 0.032(3) 0.048(4) 0.041(3) -0.014(3) -0.011(3) 0.004(3) C16 0.047(4) 0.045(4) 0.054(4) -0.014(3) -0.028(3) -0.009(3) C17 0.055(4) 0.040(3) 0.036(3) -0.019(3) -0.025(3) 0.001(3) C18 0.041(3) 0.032(3) 0.030(3) -0.009(2) -0.013(3) 0.000(2) C19 0.033(3) 0.020(2) 0.021(2) -0.0017(19) -0.011(2) 0.000(2) C20 0.031(3) 0.031(3) 0.022(2) -0.010(2) -0.009(2) 0.001(2) C21 0.046(3) 0.036(3) 0.028(3) -0.012(2) -0.011(2) -0.003(3) C22 0.068(5) 0.038(4) 0.046(4) -0.001(3) -0.011(3) -0.019(4) C23 0.039(4) 0.061(5) 0.064(4) -0.025(4) -0.014(3) -0.011(3) C24 0.031(3) 0.050(4) 0.063(4) -0.026(3) -0.021(3) 0.015(3) C25 0.035(3) 0.039(3) 0.031(3) -0.012(2) -0.011(2) 0.001(2) C26 0.048(4) 0.038(3) 0.040(3) -0.011(3) -0.032(3) 0.007(3) C27 0.026(3) 0.043(3) 0.043(3) -0.024(3) -0.020(2) 0.013(2) C28 0.040(3) 0.055(4) 0.045(4) -0.026(3) -0.022(3) 0.016(3) C29 0.057(4) 0.078(5) 0.079(5) -0.052(4) -0.047(4) 0.019(4) C30 0.043(4) 0.063(5) 0.104(6) -0.046(5) -0.035(4) 0.004(3) C31 0.038(3) 0.043(4) 0.063(4) -0.019(3) -0.018(3) 0.000(3) C32 0.025(3) 0.033(3) 0.048(3) -0.018(2) -0.016(2) 0.007(2) C33 0.021(2) 0.028(3) 0.028(2) -0.004(2) -0.008(2) 0.004(2) C34 0.019(2) 0.029(3) 0.031(3) -0.003(2) -0.006(2) -0.004(2) C35 0.042(3) 0.024(3) 0.052(4) -0.014(3) -0.016(3) 0.011(2) C36 0.033(3) 0.034(3) 0.048(3) 0.001(3) -0.013(3) 0.011(3) C37 0.032(3) 0.051(4) 0.032(3) -0.003(3) -0.013(2) 0.011(3) C38 0.028(3) 0.034(3) 0.034(3) -0.011(2) -0.011(2) 0.009(2) O1 0.045(2) 0.044(2) 0.041(2) -0.0229(18) -0.0159(18) 0.0110(18) O2 0.061(3) 0.048(2) 0.036(2) -0.0173(18) -0.0245(19) 0.013(2) O3 0.0297(19) 0.048(2) 0.036(2) -0.0080(17) -0.0150(16) -0.0012(16) O4 0.049(2) 0.051(3) 0.050(2) -0.001(2) -0.015(2) 0.002(2) O5 0.044(2) 0.033(2) 0.035(2) -0.0131(16) -0.0149(17) 0.0172(16) O6 0.042(2) 0.0345(19) 0.0284(18) -0.0095(15) -0.0165(16) 0.0104(16) O7 0.059(3) 0.044(2) 0.066(3) -0.014(2) -0.038(2) 0.019(2) O8 0.050(3) 0.032(2) 0.042(2) -0.0026(18) -0.017(2) 0.006(2) N1 0.022(2) 0.029(2) 0.034(2) -0.0066(18) -0.0131(18) 0.0045(17) N2 0.030(2) 0.028(2) 0.031(2) -0.0064(18) -0.0110(19) 0.0032(18) _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 O3 2.116(3) 2_666 ? In1 O1 2.122(3) . ? In1 O5 2.183(3) . ? In1 N1 2.262(4) . ? In1 N2 2.300(4) . ? In1 O6 2.336(3) . ? C1 O2 1.239(6) . ? C1 O1 1.280(6) . ? C1 C14 1.498(6) . ? C2 O4 1.222(6) . ? C2 O3 1.300(6) . ? C2 C27 1.503(7) . ? C3 O6 1.264(5) . ? C3 O5 1.268(5) . ? C3 C33 1.486(6) . ? C4 N1 1.344(6) . ? C4 C5 1.368(7) . ? C4 H4 0.82(5) . ? C5 C6 1.371(7) . ? C5 H5 0.89(5) . ? C6 C7 1.370(7) . ? C6 H6 0.86(4) . ? C7 C8 1.381(6) . ? C7 H7 0.92(4) . ? C8 N1 1.352(5) . ? C8 C9 1.483(6) . ? C9 N2 1.355(5) . ? C9 C10 1.376(7) . ? C10 C11 1.379(7) . ? C10 H10 0.95(4) . ? C11 C12 1.373(8) . ? C11 H11 0.88(5) . ? C12 C13 1.369(8) . ? C12 H12 0.95(6) . ? C13 N2 1.343(6) . ? C13 H13 0.91(4) . ? C14 C15 1.388(7) . ? C14 C19 1.400(6) . ? C15 C16 1.374(7) . ? C15 H15 0.91(4) . ? C16 C17 1.372(8) . ? C16 H16 0.90(5) . ? C17 C18 1.378(7) . ? C17 H17 0.89(4) . ? C18 C19 1.388(6) . ? C18 H18 0.95(4) . ? C19 C20 1.488(6) . ? C20 C25 1.396(6) . ? C20 C21 1.404(7) . ? C21 C22 1.366(8) . ? C21 H21 0.98(4) . ? C22 C23 1.362(9) . ? C22 H22 0.79(4) . ? C23 C24 1.378(8) . ? C23 H23 0.93(6) . ? C24 C25 1.387(7) . ? C24 H24 0.86(4) . ? C25 C26 1.503(7) . ? C26 O7 1.213(6) . ? C26 O8 1.319(6) . ? C27 C28 1.393(7) . ? C27 C32 1.408(7) . ? C28 C29 1.373(9) . ? C28 H29 0.93(5) . ? C29 C30 1.351(10) . ? C29 H30 0.90(5) . ? C30 C31 1.384(9) . ? C30 H31 0.89(6) . ? C31 C32 1.399(7) . ? C31 H32 0.81(5) . ? C32 C34 1.492(6) . ? C33 C38 1.394(6) . ? C33 C34 1.409(6) . ? C34 C35 1.387(7) . ? C35 C36 1.382(7) . ? C35 H35 0.87(5) . ? C36 C37 1.371(8) . ? C36 H36 0.94(5) . ? C37 C38 1.369(7) . ? C37 H37 0.93(4) . ? C38 H38 0.96(4) . ? O3 In1 2.116(3) 2_666 ? O8 H8 0.82(6) . ? 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 O3 In1 O1 92.02(13) 2_666 . ? O3 In1 O5 122.74(12) 2_666 . ? O1 In1 O5 87.57(13) . . ? O3 In1 N1 83.55(13) 2_666 . ? O1 In1 N1 119.62(13) . . ? O5 In1 N1 143.01(13) . . ? O3 In1 N2 152.26(13) 2_666 . ? O1 In1 N2 89.39(13) . . ? O5 In1 N2 85.00(13) . . ? N1 In1 N2 71.79(13) . . ? O3 In1 O6 98.41(12) 2_666 . ? O1 In1 O6 143.74(12) . . ? O5 In1 O6 57.64(11) . . ? N1 In1 O6 96.11(12) . . ? N2 In1 O6 96.71(12) . . ? O2 C1 O1 124.1(4) . . ? O2 C1 C14 120.4(5) . . ? O1 C1 C14 115.5(4) . . ? O4 C2 O3 122.7(5) . . ? O4 C2 C27 121.6(5) . . ? O3 C2 C27 115.6(4) . . ? O6 C3 O5 119.0(4) . . ? O6 C3 C33 124.1(4) . . ? O5 C3 C33 116.8(4) . . ? N1 C4 C5 122.2(5) . . ? N1 C4 H4 116(4) . . ? C5 C4 H4 121(4) . . ? C4 C5 C6 119.2(5) . . ? C4 C5 H5 117(3) . . ? C6 C5 H5 124(3) . . ? C7 C6 C5 119.3(5) . . ? C7 C6 H6 121(3) . . ? C5 C6 H6 120(3) . . ? C6 C7 C8 119.6(5) . . ? C6 C7 H7 120(3) . . ? C8 C7 H7 120(3) . . ? N1 C8 C7 121.1(4) . . ? N1 C8 C9 116.8(4) . . ? C7 C8 C9 122.1(4) . . ? N2 C9 C10 121.0(4) . . ? N2 C9 C8 115.5(4) . . ? C10 C9 C8 123.6(4) . . ? C9 C10 C11 119.0(5) . . ? C9 C10 H10 123(3) . . ? C11 C10 H10 118(3) . . ? C12 C11 C10 119.8(6) . . ? C12 C11 H11 122(4) . . ? C10 C11 H11 118(4) . . ? C13 C12 C11 118.9(5) . . ? C13 C12 H12 120(4) . . ? C11 C12 H12 121(4) . . ? N2 C13 C12 121.8(5) . . ? N2 C13 H13 111(3) . . ? C12 C13 H13 127(3) . . ? C15 C14 C19 119.9(4) . . ? C15 C14 C1 119.2(4) . . ? C19 C14 C1 120.8(4) . . ? C16 C15 C14 121.1(5) . . ? C16 C15 H15 118(3) . . ? C14 C15 H15 120(3) . . ? C17 C16 C15 118.8(5) . . ? C17 C16 H16 118(3) . . ? C15 C16 H16 123(3) . . ? C16 C17 C18 121.5(5) . . ? C16 C17 H17 122(3) . . ? C18 C17 H17 117(3) . . ? C17 C18 C19 120.4(5) . . ? C17 C18 H18 118(2) . . ? C19 C18 H18 122(2) . . ? C18 C19 C14 118.4(4) . . ? C18 C19 C20 118.5(4) . . ? C14 C19 C20 123.0(4) . . ? C25 C20 C21 117.9(4) . . ? C25 C20 C19 123.2(4) . . ? C21 C20 C19 118.3(4) . . ? C22 C21 C20 119.9(6) . . ? C22 C21 H21 124(3) . . ? C20 C21 H21 116(3) . . ? C23 C22 C21 121.9(6) . . ? C23 C22 H22 123(3) . . ? C21 C22 H22 115(3) . . ? C22 C23 C24 119.6(6) . . ? C22 C23 H23 127(4) . . ? C24 C23 H23 114(4) . . ? C23 C24 C25 119.7(6) . . ? C23 C24 H24 121(3) . . ? C25 C24 H24 119(3) . . ? C24 C25 C20 120.9(5) . . ? C24 C25 C26 116.9(5) . . ? C20 C25 C26 122.2(4) . . ? O7 C26 O8 119.9(5) . . ? O7 C26 C25 121.9(5) . . ? O8 C26 C25 118.2(4) . . ? C28 C27 C32 119.1(5) . . ? C28 C27 C2 116.7(5) . . ? C32 C27 C2 124.2(4) . . ? C29 C28 C27 121.2(6) . . ? C29 C28 H29 124(3) . . ? C27 C28 H29 114(3) . . ? C30 C29 C28 120.4(6) . . ? C30 C29 H30 121(3) . . ? C28 C29 H30 118(4) . . ? C29 C30 C31 120.0(7) . . ? C29 C30 H31 125(4) . . ? C31 C30 H31 115(4) . . ? C30 C31 C32 121.5(7) . . ? C30 C31 H32 123(4) . . ? C32 C31 H32 116(4) . . ? C31 C32 C27 117.7(5) . . ? C31 C32 C34 116.2(5) . . ? C27 C32 C34 125.9(4) . . ? C38 C33 C34 118.9(4) . . ? C38 C33 C3 115.7(4) . . ? C34 C33 C3 125.4(4) . . ? C35 C34 C33 117.9(4) . . ? C35 C34 C32 116.7(4) . . ? C33 C34 C32 125.0(4) . . ? C36 C35 C34 122.0(5) . . ? C36 C35 H35 119(3) . . ? C34 C35 H35 119(3) . . ? C37 C36 C35 119.9(5) . . ? C37 C36 H36 124(3) . . ? C35 C36 H36 116(3) . . ? C38 C37 C36 119.4(5) . . ? C38 C37 H37 121(3) . . ? C36 C37 H37 119(3) . . ? C37 C38 C33 121.9(5) . . ? C37 C38 H38 119(3) . . ? C33 C38 H38 119(3) . . ? C1 O1 In1 120.8(3) . . ? C2 O3 In1 107.9(3) . 2_666 ? C3 O5 In1 94.6(3) . . ? C3 O6 In1 87.6(3) . . ? C26 O8 H8 118(4) . . ? C4 N1 C8 118.6(4) . . ? C4 N1 In1 123.0(3) . . ? C8 N1 In1 118.3(3) . . ? C13 N2 C9 119.4(4) . . ? C13 N2 In1 123.0(3) . . ? C9 N2 In1 117.6(3) . . ? _diffrn_measured_fraction_theta_max 0.853 _diffrn_reflns_theta_full 28.85 _diffrn_measured_fraction_theta_full 0.853 _refine_diff_density_max 0.994 _refine_diff_density_min -0.831 _refine_diff_density_rms 0.110