Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Michael Hill' _publ_contact_author_address ; Department of Chemistry Imperial College London South Kensington London SW7 2AZ UNITED KINGDOM ; _publ_contact_author_email MIKE.HILL@IMPERIAL.AC.UK _publ_section_title ; Solid- and Solution-state Structures of Indium alkene analogues ; _publ_requested_category FM loop_ _publ_author_name 'Michael Hill' 'Peter B. Hitchcock' 'Ruti Pongtavornpinyo' # Attachment 'msh-oct-2006.cif' data_(8)-may605 _database_code_depnum_ccdc_archive 'CCDC 625827' _audit_creation_date 2005-05-11T13:56:11-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C42 H50 In2 N4' _chemical_formula_sum 'C42 H50 In2 N4' _chemical_formula_weight 840.5 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6989(5) _cell_length_b 10.0246(6) _cell_length_c 12.3181(7) _cell_angle_alpha 67.338(3) _cell_angle_beta 82.783(3) _cell_angle_gamma 83.862(3) _cell_volume 981.38(10) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5113 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 428 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.208 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8505 _exptl_absorpt_correction_T_max 0.9404 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.174272E-1 _diffrn_orient_matrix_ub_12 0.152925E-1 _diffrn_orient_matrix_ub_13 0.762957E-1 _diffrn_orient_matrix_ub_21 0.102093 _diffrn_orient_matrix_ub_22 0.44824E-1 _diffrn_orient_matrix_ub_23 -0.17323E-1 _diffrn_orient_matrix_ub_31 -0.524914E-1 _diffrn_orient_matrix_ub_32 0.974201E-1 _diffrn_orient_matrix_ub_33 -0.410404E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_unetI/netI 0.0481 _diffrn_reflns_number 7198 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 26.03 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.882 _diffrn_measured_fraction_theta_max 0.882 _reflns_number_total 3420 _reflns_number_gt 3013 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0326P)^2^+0.4666P] 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_number_reflns 3420 _refine_ls_number_parameters 223 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0757 _refine_ls_wR_factor_gt 0.0725 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.694 _refine_diff_density_min -0.669 _refine_diff_density_rms 0.088 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.31 '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' 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 In In 0.31893(3) 0.56192(2) 0.526299(19) 0.03380(10) Uani 1 1 d . . . N1 N 0.2913(3) 0.8035(3) 0.4212(2) 0.0301(6) Uani 1 1 d . . . N2 N 0.2942(3) 0.6370(3) 0.6799(2) 0.0295(6) Uani 1 1 d . . . C1 C 0.2937(4) 0.9123(3) 0.4570(3) 0.0343(8) Uani 1 1 d . . . C2 C 0.3015(4) 0.8953(3) 0.5741(3) 0.0369(8) Uani 1 1 d . . . H2 H 0.3172 0.9813 0.5853 0.044 Uiso 1 1 calc R . . C3 C 0.2895(4) 0.7708(3) 0.6777(3) 0.0316(7) Uani 1 1 d . . . C4 C 0.2773(5) 1.0666(3) 0.3681(3) 0.0465(9) Uani 1 1 d . . . H4A H 0.3505 1.0777 0.2984 0.07 Uiso 1 1 calc R . . H4B H 0.2997 1.1336 0.4039 0.07 Uiso 1 1 calc R . . H4C H 0.171 1.0881 0.3447 0.07 Uiso 1 1 calc R . . C5 C 0.2612(5) 0.7961(4) 0.7921(3) 0.0444(9) Uani 1 1 d . . . H5A H 0.1566 0.7689 0.8287 0.067 Uiso 1 1 calc R . . H5B H 0.2705 0.8987 0.7758 0.067 Uiso 1 1 calc R . . H5C H 0.338 0.7371 0.8459 0.067 Uiso 1 1 calc R . . C6 C 0.2565(4) 0.8351(3) 0.3029(3) 0.0304(7) Uani 1 1 d . . . C7 C 0.3752(4) 0.8571(3) 0.2117(3) 0.0336(8) Uani 1 1 d . . . C8 C 0.3346(5) 0.8854(3) 0.0985(3) 0.0413(9) Uani 1 1 d . . . H8 H 0.4135 0.9035 0.0348 0.05 Uiso 1 1 calc R . . C9 C 0.1824(5) 0.8876(4) 0.0774(3) 0.0464(10) Uani 1 1 d . . . H9 H 0.1573 0.9067 -0.0003 0.056 Uiso 1 1 calc R . . C10 C 0.0669(5) 0.8622(4) 0.1685(4) 0.0477(9) Uani 1 1 d . . . H10 H -0.0377 0.8634 0.1534 0.057 Uiso 1 1 calc R . . C11 C 0.1015(4) 0.8348(4) 0.2828(3) 0.0397(8) Uani 1 1 d . . . C12 C 0.5419(4) 0.8510(4) 0.2348(3) 0.0436(9) Uani 1 1 d . . . H12A H 0.5554 0.9258 0.265 0.065 Uiso 1 1 calc R . . H12B H 0.6087 0.8677 0.1611 0.065 Uiso 1 1 calc R . . H12C H 0.5704 0.7554 0.2933 0.065 Uiso 1 1 calc R . . C13 C -0.0257(5) 0.8057(5) 0.3828(4) 0.0571(11) Uani 1 1 d . . . H13A H -0.0055 0.7092 0.443 0.086 Uiso 1 1 calc R . . H13B H -0.1258 0.8103 0.3525 0.086 Uiso 1 1 calc R . . H13C H -0.0282 0.8788 0.4178 0.086 Uiso 1 1 calc R . . C14 C 0.2670(4) 0.5213(3) 0.7934(3) 0.0313(7) Uani 1 1 d . . . C15 C 0.3927(4) 0.4540(3) 0.8604(3) 0.0356(8) Uani 1 1 d . . . C16 C 0.3606(5) 0.3432(4) 0.9698(3) 0.0487(10) Uani 1 1 d . . . H16 H 0.443 0.2976 1.0179 0.058 Uiso 1 1 calc R . . C17 C 0.2130(6) 0.2984(4) 1.0099(3) 0.0525(11) Uani 1 1 d . . . H17 H 0.1946 0.222 1.0844 0.063 Uiso 1 1 calc R . . C18 C 0.0928(5) 0.3635(4) 0.9426(3) 0.0468(10) Uani 1 1 d . . . H18 H -0.0089 0.3319 0.9711 0.056 Uiso 1 1 calc R . . C19 C 0.1165(4) 0.4764(4) 0.8321(3) 0.0377(8) Uani 1 1 d . . . C20 C 0.5539(4) 0.4999(4) 0.8160(4) 0.0502(10) Uani 1 1 d . . . H20A H 0.5858 0.4827 0.7431 0.075 Uiso 1 1 calc R . . H20B H 0.6249 0.4439 0.8758 0.075 Uiso 1 1 calc R . . H20C H 0.5569 0.6033 0.8001 0.075 Uiso 1 1 calc R . . C21 C -0.0178(4) 0.5472(5) 0.7601(4) 0.0525(10) Uani 1 1 d . . . H21A H -0.0108 0.6525 0.7275 0.079 Uiso 1 1 calc R . . H21B H -0.1153 0.5226 0.8105 0.079 Uiso 1 1 calc R . . H21C H -0.0148 0.5127 0.6954 0.079 Uiso 1 1 calc R . . 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 In 0.04722(18) 0.02752(13) 0.02631(14) -0.01030(9) -0.00239(11) -0.00148(10) N1 0.0383(16) 0.0257(13) 0.0244(13) -0.0070(11) -0.0033(13) -0.0026(11) N2 0.0355(16) 0.0295(13) 0.0240(13) -0.0102(11) -0.0020(12) -0.0052(11) C1 0.039(2) 0.0292(16) 0.0319(17) -0.0097(14) -0.0019(16) -0.0007(14) C2 0.052(2) 0.0262(16) 0.0340(18) -0.0124(14) -0.0008(17) -0.0077(14) C3 0.0324(19) 0.0389(18) 0.0276(16) -0.0170(14) -0.0021(15) -0.0033(14) C4 0.072(3) 0.0293(18) 0.0354(19) -0.0096(15) -0.0059(19) 0.0012(17) C5 0.063(3) 0.042(2) 0.0316(18) -0.0170(15) -0.0015(18) -0.0073(17) C6 0.041(2) 0.0238(15) 0.0251(16) -0.0066(12) -0.0070(15) 0.0001(13) C7 0.042(2) 0.0254(15) 0.0288(17) -0.0059(13) -0.0028(16) -0.0017(13) C8 0.064(3) 0.0312(18) 0.0253(17) -0.0071(14) -0.0041(18) -0.0035(16) C9 0.071(3) 0.0357(19) 0.034(2) -0.0114(15) -0.024(2) 0.0053(18) C10 0.052(2) 0.044(2) 0.051(2) -0.0181(17) -0.023(2) 0.0057(17) C11 0.044(2) 0.0350(18) 0.039(2) -0.0126(15) -0.0101(18) 0.0045(15) C12 0.043(2) 0.047(2) 0.038(2) -0.0129(16) 0.0058(18) -0.0108(16) C13 0.037(2) 0.075(3) 0.058(3) -0.025(2) -0.005(2) 0.0035(19) C14 0.042(2) 0.0320(16) 0.0233(16) -0.0141(13) 0.0010(15) -0.0070(14) C15 0.044(2) 0.0390(18) 0.0286(17) -0.0182(14) -0.0071(17) 0.0021(15) C16 0.070(3) 0.046(2) 0.0307(18) -0.0144(16) -0.018(2) 0.0117(19) C17 0.088(3) 0.040(2) 0.0241(18) -0.0089(15) 0.007(2) -0.009(2) C18 0.057(3) 0.050(2) 0.036(2) -0.0196(17) 0.011(2) -0.0184(18) C19 0.043(2) 0.0413(19) 0.0313(18) -0.0166(15) 0.0045(17) -0.0095(15) C20 0.044(2) 0.060(2) 0.053(2) -0.026(2) -0.013(2) 0.0009(18) C21 0.035(2) 0.071(3) 0.051(2) -0.021(2) -0.0012(19) -0.0071(18) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 In N1 2.266(2) . ? In N2 2.270(2) . ? In In 3.3400(5) 2_666 ? N1 C1 1.328(4) . ? N1 C6 1.432(4) . ? N2 C3 1.328(4) . ? N2 C14 1.443(4) . ? C1 C2 1.396(5) . ? C1 C4 1.516(4) . ? C2 C3 1.402(4) . ? C2 H2 0.95 . ? C3 C5 1.511(4) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 C7 1.394(5) . ? C6 C11 1.402(5) . ? C7 C8 1.395(5) . ? C7 C12 1.504(5) . ? C8 C9 1.377(6) . ? C8 H8 0.95 . ? C9 C10 1.373(6) . ? C9 H9 0.95 . ? C10 C11 1.392(5) . ? C10 H10 0.95 . ? C11 C13 1.509(5) . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 C19 1.396(5) . ? C14 C15 1.404(5) . ? C15 C16 1.395(5) . ? C15 C20 1.493(5) . ? C16 C17 1.374(6) . ? C16 H16 0.95 . ? C17 C18 1.364(6) . ? C17 H17 0.95 . ? C18 C19 1.403(5) . ? C18 H18 0.95 . ? C19 C21 1.500(5) . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? 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 N1 In N2 82.00(9) . . ? N1 In In 109.72(7) . 2_666 ? N2 In In 112.33(7) . 2_666 ? C1 N1 C6 118.8(3) . . ? C1 N1 In 129.0(2) . . ? C6 N1 In 112.03(18) . . ? C3 N2 C14 117.5(3) . . ? C3 N2 In 129.0(2) . . ? C14 N2 In 113.35(18) . . ? N1 C1 C2 124.3(3) . . ? N1 C1 C4 119.1(3) . . ? C2 C1 C4 116.4(3) . . ? C1 C2 C3 129.9(3) . . ? C1 C2 H2 115.1 . . ? C3 C2 H2 115.1 . . ? N2 C3 C2 124.2(3) . . ? N2 C3 C5 119.7(3) . . ? C2 C3 C5 115.9(3) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 121.1(3) . . ? C7 C6 N1 120.6(3) . . ? C11 C6 N1 118.3(3) . . ? C6 C7 C8 118.1(3) . . ? C6 C7 C12 120.8(3) . . ? C8 C7 C12 121.1(3) . . ? C9 C8 C7 121.3(4) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C10 C9 C8 120.1(3) . . ? C10 C9 H9 120 . . ? C8 C9 H9 120 . . ? C9 C10 C11 120.7(4) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C10 C11 C6 118.7(3) . . ? C10 C11 C13 120.6(3) . . ? C6 C11 C13 120.8(3) . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C14 C15 121.7(3) . . ? C19 C14 N2 118.9(3) . . ? C15 C14 N2 119.4(3) . . ? C16 C15 C14 117.3(3) . . ? C16 C15 C20 121.5(4) . . ? C14 C15 C20 121.1(3) . . ? C17 C16 C15 121.8(4) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C18 C17 C16 120.0(3) . . ? C18 C17 H17 120 . . ? C16 C17 H17 120 . . ? C17 C18 C19 121.2(4) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C14 C19 C18 117.9(3) . . ? C14 C19 C21 121.8(3) . . ? C18 C19 C21 120.3(3) . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? #===END data_(12)-apr1005 _database_code_depnum_ccdc_archive 'CCDC 625828' _audit_creation_date 2005-04-21T10:42:48-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C63 H75 In3 N6 O3' _chemical_formula_sum 'C63 H75 In3 N6 O3' _chemical_formula_weight 1308.75 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 13.9231(3) _cell_length_b 34.7614(10) _cell_length_c 14.0230(3) _cell_angle_alpha 90 _cell_angle_beta 118.272(1) _cell_angle_gamma 90 _cell_volume 5977.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 104298 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2664 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.196 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8175 _exptl_absorpt_correction_T_max 0.88 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.173544E-1 _diffrn_orient_matrix_ub_12 -0.129333E-1 _diffrn_orient_matrix_ub_13 -0.700258E-1 _diffrn_orient_matrix_ub_21 0.793416E-1 _diffrn_orient_matrix_ub_22 -0.4399E-3 _diffrn_orient_matrix_ub_23 0.208601E-1 _diffrn_orient_matrix_ub_31 0.73776E-2 _diffrn_orient_matrix_ub_32 -0.256926E-1 _diffrn_orient_matrix_ub_33 0.348928E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_unetI/netI 0.0535 _diffrn_reflns_number 24282 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 22.99 _diffrn_reflns_theta_full 22.99 _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.981 _reflns_number_total 8154 _reflns_number_gt 6212 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0301P)^2^+16.4146P] 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_number_reflns 8154 _refine_ls_number_parameters 694 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0781 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.106 _refine_ls_wR_factor_gt 0.0962 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.759 _refine_diff_density_min -0.653 _refine_diff_density_rms 0.083 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' In In -0.7276 1.31 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.65518(4) 0.106421(14) 0.23978(4) 0.04006(15) Uani 1 1 d . . . In2 In 0.37177(4) 0.103916(15) 0.06841(4) 0.04525(16) Uani 1 1 d . . . In3 In 0.50105(4) 0.191132(15) 0.17398(4) 0.04483(16) Uani 1 1 d . . . O1 O 0.5162(4) 0.07763(13) 0.1470(4) 0.0524(12) Uani 1 1 d . . . O2 O 0.3695(4) 0.16119(14) 0.0801(4) 0.0679(15) Uani 1 1 d . . . O3 O 0.6434(4) 0.16286(13) 0.2484(4) 0.0551(13) Uani 1 1 d . . . N1 N 0.7921(4) 0.09181(16) 0.2109(4) 0.0417(14) Uani 1 1 d . . . N2 N 0.7388(4) 0.07564(16) 0.3931(4) 0.0430(14) Uani 1 1 d . . . N3 N 0.2900(5) 0.08404(16) -0.0975(4) 0.0488(15) Uani 1 1 d . . . N4 N 0.2338(5) 0.08250(17) 0.0844(5) 0.0543(16) Uani 1 1 d . . . N5 N 0.4892(5) 0.23167(18) 0.2873(4) 0.0506(15) Uani 1 1 d . . . N6 N 0.5175(5) 0.24026(16) 0.0882(4) 0.0467(14) Uani 1 1 d . . . C1 C 0.8531(6) 0.0611(2) 0.2551(6) 0.0497(19) Uani 1 1 d . . . C2 C 0.8516(6) 0.0388(2) 0.3379(6) 0.0542(19) Uani 1 1 d . . . H2 H 0.887 0.0146 0.3495 0.065 Uiso 1 1 calc R . . C3 C 0.8067(6) 0.0466(2) 0.4058(6) 0.0507(18) Uani 1 1 d . . . C4 C 0.9356(6) 0.0487(2) 0.2191(6) 0.061(2) Uani 1 1 d . . . H4A H 0.9002 0.0477 0.1399 0.091 Uiso 1 1 calc R . . H4B H 0.9643 0.0233 0.2488 0.091 Uiso 1 1 calc R . . H4C H 0.9957 0.0673 0.2454 0.091 Uiso 1 1 calc R . . C5 C 0.8399(7) 0.0199(2) 0.5011(6) 0.067(2) Uani 1 1 d . . . H5A H 0.8816 0.0343 0.5684 0.1 Uiso 1 1 calc R . . H5B H 0.8851 -0.0009 0.4966 0.1 Uiso 1 1 calc R . . H5C H 0.7745 0.009 0.5002 0.1 Uiso 1 1 calc R . . C6 C 0.8198(5) 0.1157(2) 0.1439(5) 0.0444(18) Uani 1 1 d . . . C7 C 0.8996(6) 0.1441(2) 0.1928(6) 0.055(2) Uani 1 1 d . . . C8 C 0.9295(7) 0.1664(2) 0.1295(9) 0.074(3) Uani 1 1 d . . . H8 H 0.9836 0.1858 0.1623 0.089 Uiso 1 1 calc R . . C9 C 0.8820(8) 0.1608(3) 0.0209(9) 0.083(3) Uani 1 1 d . . . H9 H 0.9041 0.1761 -0.0216 0.1 Uiso 1 1 calc R . . C10 C 0.8029(8) 0.1336(3) -0.0281(7) 0.072(3) Uani 1 1 d . . . H10 H 0.7703 0.1304 -0.1043 0.087 Uiso 1 1 calc R . . C11 C 0.7686(6) 0.1101(2) 0.0321(6) 0.056(2) Uani 1 1 d . . . C12 C 0.9543(7) 0.1497(2) 0.3129(7) 0.075(2) Uani 1 1 d . . . H12A H 1.0113 0.1693 0.3337 0.113 Uiso 1 1 calc R . . H12B H 0.9872 0.1254 0.349 0.113 Uiso 1 1 calc R . . H12C H 0.9004 0.158 0.3348 0.113 Uiso 1 1 calc R . . C13 C 0.6827(7) 0.0802(3) -0.0199(7) 0.083(3) Uani 1 1 d . . . H13A H 0.7143 0.0547 0.0064 0.124 Uiso 1 1 calc R . . H13B H 0.6534 0.0813 -0.0986 0.124 Uiso 1 1 calc R . . H13C H 0.6239 0.0848 -0.0017 0.124 Uiso 1 1 calc R . . C14 C 0.7174(6) 0.0839(2) 0.4825(5) 0.0498(19) Uani 1 1 d . . . C15 C 0.7902(7) 0.1068(2) 0.5653(6) 0.061(2) Uani 1 1 d . . . C16 C 0.7733(8) 0.1127(3) 0.6553(6) 0.077(3) Uani 1 1 d . . . H16 H 0.8242 0.1274 0.7149 0.092 Uiso 1 1 calc R . . C17 C 0.6841(10) 0.0974(3) 0.6576(7) 0.094(3) Uani 1 1 d . . . H17 H 0.6728 0.102 0.7184 0.113 Uiso 1 1 calc R . . C18 C 0.6108(8) 0.0755(3) 0.5733(7) 0.080(3) Uani 1 1 d . . . H18 H 0.5487 0.0652 0.5757 0.097 Uiso 1 1 calc R . . C19 C 0.6266(7) 0.0681(2) 0.4843(6) 0.061(2) Uani 1 1 d . . . C20 C 0.8832(7) 0.1256(3) 0.5583(7) 0.078(3) Uani 1 1 d . . . H20A H 0.9273 0.106 0.5471 0.117 Uiso 1 1 calc R . . H20B H 0.9284 0.1395 0.6257 0.117 Uiso 1 1 calc R . . H20C H 0.8548 0.1438 0.4975 0.117 Uiso 1 1 calc R . . C21 C 0.5482(7) 0.0427(3) 0.3959(7) 0.086(3) Uani 1 1 d . . . H21A H 0.5151 0.0569 0.3274 0.129 Uiso 1 1 calc R . . H21B H 0.4911 0.0341 0.4131 0.129 Uiso 1 1 calc R . . H21C H 0.5871 0.0202 0.3891 0.129 Uiso 1 1 calc R . . C22 C 0.1820(6) 0.0794(2) -0.1533(6) 0.060(2) Uani 1 1 d . . . C23 C 0.1116(6) 0.0806(3) -0.1082(7) 0.074(2) Uani 1 1 d . . . H23 H 0.0363 0.0826 -0.1589 0.088 Uiso 1 1 calc R . . C24 C 0.1348(7) 0.0793(3) -0.0007(8) 0.070(2) Uani 1 1 d . . . C25 C 0.1327(6) 0.0707(3) -0.2735(6) 0.074(2) Uani 1 1 d . . . H25A H 0.1486 0.0919 -0.3099 0.111 Uiso 1 1 calc R . . H25B H 0.0535 0.0677 -0.3043 0.111 Uiso 1 1 calc R . . H25C H 0.1641 0.0468 -0.2838 0.111 Uiso 1 1 calc R . . C26 C 0.0368(6) 0.0713(3) 0.0186(7) 0.087(3) Uani 1 1 d . . . H26A H 0.0445 0.0458 0.0508 0.131 Uiso 1 1 calc R . . H26B H -0.0306 0.0724 -0.0506 0.131 Uiso 1 1 calc R . . H26C H 0.0341 0.0908 0.0678 0.131 Uiso 1 1 calc R . . C27 C 0.3518(6) 0.0752(2) -0.1523(5) 0.0473(18) Uani 1 1 d . . . C28 C 0.3850(6) 0.0356(3) -0.1491(6) 0.059(2) Uani 1 1 d . . . C29 C 0.4364(7) 0.0262(3) -0.2070(7) 0.077(3) Uani 1 1 d . . . H29 H 0.4596 0.0004 -0.2065 0.092 Uiso 1 1 calc R . . C30 C 0.4550(7) 0.0532(4) -0.2655(7) 0.082(3) Uani 1 1 d . . . H30 H 0.4884 0.045 -0.3074 0.099 Uiso 1 1 calc R . . C31 C 0.4300(8) 0.0909(4) -0.2693(7) 0.087(3) Uani 1 1 d . . . H31 H 0.4464 0.1088 -0.3108 0.105 Uiso 1 1 calc R . . C32 C 0.3764(7) 0.1026(3) -0.2064(6) 0.074(3) Uani 1 1 d . . . C33 C 0.3605(7) 0.0068(2) -0.0851(6) 0.069(2) Uani 1 1 d . . . H33A H 0.2813 0.0036 -0.1168 0.103 Uiso 1 1 calc R . . H33B H 0.39 0.0158 -0.0101 0.103 Uiso 1 1 calc R . . H33C H 0.394 -0.0179 -0.0861 0.103 Uiso 1 1 calc R . . C34 C 0.3449(9) 0.1434(3) -0.2046(9) 0.130(5) Uani 1 1 d . . . H34A H 0.2678 0.1447 -0.2231 0.195 Uiso 1 1 calc R . . H34B H 0.3568 0.1582 -0.2575 0.195 Uiso 1 1 calc R . . H34C H 0.3895 0.1541 -0.1321 0.195 Uiso 1 1 calc R . . C35 C 0.2449(6) 0.0752(3) 0.1899(6) 0.059(2) Uani 1 1 d . . . C36 C 0.2368(7) 0.1061(3) 0.2493(7) 0.071(2) Uani 1 1 d . . . C37 C 0.2476(8) 0.0985(3) 0.3509(9) 0.092(3) Uani 1 1 d . . . H37 H 0.2439 0.1191 0.3935 0.11 Uiso 1 1 calc R . . C38 C 0.2635(8) 0.0621(4) 0.3909(8) 0.090(3) Uani 1 1 d . . . H38 H 0.2706 0.0576 0.4608 0.108 Uiso 1 1 calc R . . C39 C 0.2693(7) 0.0319(3) 0.3313(8) 0.085(3) Uani 1 1 d . . . H39 H 0.2806 0.0067 0.3605 0.102 Uiso 1 1 calc R . . C40 C 0.2590(6) 0.0376(3) 0.2287(7) 0.069(2) Uani 1 1 d . . . C41 C 0.2151(8) 0.1460(3) 0.2046(8) 0.093(3) Uani 1 1 d . . . H41A H 0.2124 0.1636 0.2578 0.14 Uiso 1 1 calc R . . H41B H 0.1452 0.1466 0.1379 0.14 Uiso 1 1 calc R . . H41C H 0.2736 0.1539 0.1886 0.14 Uiso 1 1 calc R . . C42 C 0.2663(8) 0.0049(2) 0.1625(8) 0.088(3) Uani 1 1 d . . . H42A H 0.1994 0.0039 0.0929 0.132 Uiso 1 1 calc R . . H42B H 0.275 -0.0194 0.2015 0.132 Uiso 1 1 calc R . . H42C H 0.3291 0.0088 0.15 0.132 Uiso 1 1 calc R . . C43 C 0.5435(6) 0.2651(2) 0.3087(6) 0.055(2) Uani 1 1 d . . . C44 C 0.5846(6) 0.2812(2) 0.2453(6) 0.058(2) Uani 1 1 d . . . H44 H 0.6348 0.3016 0.2789 0.07 Uiso 1 1 calc R . . C45 C 0.5649(6) 0.2725(2) 0.1401(6) 0.0505(18) Uani 1 1 d . . . C46 C 0.5612(7) 0.2878(2) 0.4081(6) 0.073(2) Uani 1 1 d . . . H46A H 0.4978 0.3043 0.3901 0.109 Uiso 1 1 calc R . . H46B H 0.6266 0.3038 0.4324 0.109 Uiso 1 1 calc R . . H46C H 0.5705 0.27 0.4661 0.109 Uiso 1 1 calc R . . C47 C 0.5969(6) 0.3023(2) 0.0830(6) 0.064(2) Uani 1 1 d . . . H47A H 0.6307 0.2897 0.0438 0.095 Uiso 1 1 calc R . . H47B H 0.649 0.3203 0.1363 0.095 Uiso 1 1 calc R . . H47C H 0.5319 0.3164 0.0317 0.095 Uiso 1 1 calc R . . C48 C 0.4318(6) 0.2221(2) 0.3466(6) 0.0536(19) Uani 1 1 d . . . C49 C 0.3310(7) 0.2387(3) 0.3170(7) 0.071(2) Uani 1 1 d . . . C50 C 0.2783(8) 0.2292(3) 0.3772(8) 0.094(3) Uani 1 1 d . . . H50 H 0.2092 0.2403 0.3577 0.112 Uiso 1 1 calc R . . C51 C 0.3221(9) 0.2048(3) 0.4621(9) 0.089(3) Uani 1 1 d . . . H51 H 0.2842 0.199 0.5017 0.107 Uiso 1 1 calc R . . C52 C 0.4216(8) 0.1884(3) 0.4908(6) 0.074(2) Uani 1 1 d . . . H52 H 0.4537 0.1716 0.5514 0.089 Uiso 1 1 calc R . . C53 C 0.4749(7) 0.1963(2) 0.4318(6) 0.060(2) Uani 1 1 d . . . C54 C 0.2777(8) 0.2643(3) 0.2194(8) 0.102(3) Uani 1 1 d . . . H54A H 0.3279 0.285 0.2254 0.153 Uiso 1 1 calc R . . H54B H 0.211 0.2754 0.2151 0.153 Uiso 1 1 calc R . . H54C H 0.2593 0.2492 0.1539 0.153 Uiso 1 1 calc R . . C55 C 0.5862(7) 0.1784(3) 0.4667(6) 0.077(3) Uani 1 1 d . . . H55A H 0.587 0.166 0.4043 0.115 Uiso 1 1 calc R . . H55B H 0.601 0.1591 0.523 0.115 Uiso 1 1 calc R . . H55C H 0.6423 0.1984 0.4953 0.115 Uiso 1 1 calc R . . C56 C 0.4798(6) 0.2393(2) -0.0280(5) 0.0480(18) Uani 1 1 d . . . C57 C 0.3792(6) 0.2556(2) -0.0954(6) 0.0523(19) Uani 1 1 d . . . C58 C 0.3474(7) 0.2562(2) -0.2062(6) 0.063(2) Uani 1 1 d . . . H58 H 0.2802 0.2681 -0.2544 0.076 Uiso 1 1 calc R . . C59 C 0.4089(8) 0.2406(2) -0.2468(6) 0.067(2) Uani 1 1 d . . . H59 H 0.3847 0.2414 -0.3225 0.081 Uiso 1 1 calc R . . C60 C 0.5075(7) 0.2234(2) -0.1782(6) 0.063(2) Uani 1 1 d . . . H60 H 0.5501 0.2123 -0.2076 0.076 Uiso 1 1 calc R . . C61 C 0.5453(7) 0.2221(2) -0.0671(6) 0.061(2) Uani 1 1 d . . . C62 C 0.3091(6) 0.2716(2) -0.0523(6) 0.069(2) Uani 1 1 d . . . H62A H 0.278 0.2505 -0.0293 0.104 Uiso 1 1 calc R . . H62B H 0.25 0.2866 -0.1089 0.104 Uiso 1 1 calc R . . H62C H 0.3527 0.2882 0.0097 0.104 Uiso 1 1 calc R . . C63 C 0.6514(8) 0.2046(3) 0.0078(7) 0.088(3) Uani 1 1 d . . . H63A H 0.7024 0.2248 0.0514 0.131 Uiso 1 1 calc R . . H63B H 0.6808 0.191 -0.034 0.131 Uiso 1 1 calc R . . H63C H 0.6412 0.1864 0.0556 0.131 Uiso 1 1 calc R . . 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 0.0405(3) 0.0477(3) 0.0359(3) 0.0002(2) 0.0213(2) 0.0004(2) In2 0.0404(3) 0.0530(3) 0.0435(3) 0.0009(3) 0.0209(2) 0.0032(3) In3 0.0516(3) 0.0480(3) 0.0403(3) 0.0017(2) 0.0262(2) 0.0058(3) O1 0.043(3) 0.054(3) 0.056(3) -0.001(2) 0.019(2) 0.000(2) O2 0.061(3) 0.058(3) 0.075(4) -0.006(3) 0.024(3) 0.005(3) O3 0.055(3) 0.054(3) 0.053(3) 0.003(2) 0.023(3) 0.006(2) N1 0.043(3) 0.045(4) 0.044(3) -0.001(3) 0.027(3) -0.001(3) N2 0.045(3) 0.049(4) 0.035(3) 0.007(3) 0.018(3) 0.003(3) N3 0.049(4) 0.049(4) 0.043(3) -0.002(3) 0.017(3) 0.003(3) N4 0.038(4) 0.065(4) 0.062(4) -0.002(3) 0.026(4) 0.001(3) N5 0.062(4) 0.052(4) 0.047(4) 0.001(3) 0.034(3) 0.013(3) N6 0.056(4) 0.044(4) 0.039(3) 0.006(3) 0.022(3) 0.005(3) C1 0.059(5) 0.041(5) 0.061(5) -0.008(4) 0.038(4) -0.003(4) C2 0.057(5) 0.043(5) 0.072(5) 0.004(4) 0.039(4) 0.007(4) C3 0.049(5) 0.050(5) 0.054(4) 0.002(4) 0.024(4) 0.000(4) C4 0.058(5) 0.058(5) 0.081(6) 0.004(4) 0.046(5) 0.012(4) C5 0.077(6) 0.063(5) 0.061(5) 0.022(4) 0.034(5) 0.015(5) C6 0.042(4) 0.053(5) 0.049(4) 0.004(4) 0.031(4) 0.011(4) C7 0.060(5) 0.050(5) 0.072(5) -0.006(4) 0.045(5) -0.001(4) C8 0.075(6) 0.054(6) 0.120(8) -0.005(6) 0.069(7) -0.008(5) C9 0.088(8) 0.080(7) 0.114(9) 0.012(6) 0.075(7) 0.008(6) C10 0.092(7) 0.087(7) 0.056(5) 0.011(5) 0.051(5) 0.022(6) C11 0.067(5) 0.057(5) 0.058(5) 0.003(4) 0.040(5) 0.010(4) C12 0.066(6) 0.064(6) 0.088(7) -0.015(5) 0.031(5) -0.016(5) C13 0.073(6) 0.112(8) 0.062(6) -0.013(5) 0.031(5) -0.004(6) C14 0.057(5) 0.056(5) 0.035(4) 0.006(4) 0.020(4) 0.006(4) C15 0.075(6) 0.055(5) 0.042(4) 0.004(4) 0.018(4) 0.004(5) C16 0.105(8) 0.071(6) 0.040(5) -0.005(4) 0.022(5) 0.003(6) C17 0.150(11) 0.093(8) 0.054(6) -0.001(5) 0.060(7) 0.009(7) C18 0.104(7) 0.101(7) 0.059(6) -0.003(5) 0.058(6) -0.001(6) C19 0.078(6) 0.066(6) 0.046(5) 0.002(4) 0.035(5) -0.003(5) C20 0.061(6) 0.079(6) 0.063(5) -0.005(5) 0.004(5) -0.014(5) C21 0.079(6) 0.125(8) 0.067(6) -0.018(6) 0.045(5) -0.048(6) C22 0.046(5) 0.060(5) 0.056(5) 0.000(4) 0.008(4) 0.007(4) C23 0.035(5) 0.099(7) 0.073(6) -0.003(5) 0.014(5) 0.007(4) C24 0.057(6) 0.079(6) 0.082(6) -0.001(5) 0.038(5) 0.006(5) C25 0.054(5) 0.086(6) 0.053(5) -0.010(5) 0.001(4) -0.003(5) C26 0.043(5) 0.116(8) 0.105(7) -0.019(6) 0.037(5) -0.010(5) C27 0.044(4) 0.055(5) 0.033(4) -0.003(4) 0.010(3) -0.003(4) C28 0.040(5) 0.091(7) 0.037(4) -0.014(4) 0.012(4) -0.001(4) C29 0.078(6) 0.092(7) 0.063(5) -0.009(5) 0.037(5) 0.005(5) C30 0.085(7) 0.118(9) 0.052(5) -0.004(6) 0.039(5) -0.027(7) C31 0.080(7) 0.111(9) 0.055(6) 0.021(6) 0.019(5) -0.036(6) C32 0.066(6) 0.082(7) 0.049(5) 0.017(5) 0.006(4) -0.018(5) C33 0.074(6) 0.061(6) 0.072(5) 0.003(5) 0.035(5) -0.003(5) C34 0.131(10) 0.092(9) 0.107(9) 0.050(7) 0.007(7) -0.023(7) C35 0.049(5) 0.071(6) 0.070(5) -0.002(5) 0.038(4) -0.006(4) C36 0.068(6) 0.076(7) 0.092(6) -0.006(6) 0.057(5) -0.014(5) C37 0.108(8) 0.095(8) 0.111(8) -0.035(7) 0.082(7) -0.035(7) C38 0.096(8) 0.117(9) 0.087(7) 0.000(7) 0.067(6) -0.023(7) C39 0.088(7) 0.095(8) 0.100(7) 0.025(6) 0.067(6) 0.001(6) C40 0.063(6) 0.077(7) 0.091(6) 0.008(5) 0.057(5) -0.002(5) C41 0.111(8) 0.083(8) 0.125(8) -0.020(6) 0.088(7) -0.012(6) C42 0.102(8) 0.067(6) 0.127(8) 0.018(6) 0.080(7) 0.014(5) C43 0.062(5) 0.052(5) 0.051(5) -0.004(4) 0.028(4) 0.005(4) C44 0.067(5) 0.062(5) 0.052(5) 0.003(4) 0.033(4) 0.000(4) C45 0.051(5) 0.053(5) 0.043(4) 0.005(4) 0.018(4) 0.004(4) C46 0.093(7) 0.071(6) 0.063(5) -0.015(4) 0.045(5) 0.006(5) C47 0.071(6) 0.061(5) 0.063(5) -0.003(4) 0.035(5) -0.012(4) C48 0.063(5) 0.059(5) 0.046(4) -0.004(4) 0.032(4) 0.004(4) C49 0.073(6) 0.082(7) 0.070(6) -0.013(5) 0.045(5) 0.013(5) C50 0.084(7) 0.127(9) 0.090(7) -0.026(7) 0.058(7) 0.013(7) C51 0.105(9) 0.109(8) 0.088(7) -0.017(6) 0.074(7) 0.000(7) C52 0.093(7) 0.089(7) 0.047(5) -0.002(5) 0.039(5) -0.006(6) C53 0.073(6) 0.065(6) 0.057(5) -0.009(4) 0.044(5) -0.005(5) C54 0.097(8) 0.119(9) 0.100(8) 0.004(7) 0.054(7) 0.040(7) C55 0.089(7) 0.097(7) 0.054(5) 0.020(5) 0.042(5) 0.019(5) C56 0.062(5) 0.044(5) 0.039(4) 0.005(3) 0.024(4) -0.006(4) C57 0.061(5) 0.045(5) 0.049(5) 0.001(4) 0.025(4) -0.008(4) C58 0.063(6) 0.065(6) 0.045(5) 0.005(4) 0.011(4) -0.009(4) C59 0.093(7) 0.064(6) 0.044(5) 0.004(4) 0.031(5) -0.017(5) C60 0.088(7) 0.061(5) 0.054(5) -0.001(4) 0.044(5) -0.010(5) C61 0.084(6) 0.049(5) 0.059(5) 0.005(4) 0.043(5) 0.000(4) C62 0.058(5) 0.077(6) 0.056(5) 0.003(4) 0.014(4) 0.011(5) C63 0.100(7) 0.105(8) 0.076(6) 0.014(5) 0.056(6) 0.033(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 1.977(5) . ? In1 O1 2.014(4) . ? In1 N2 2.179(5) . ? In1 N1 2.188(5) . ? In2 O1 1.998(4) . ? In2 O2 1.999(5) . ? In2 N3 2.163(5) . ? In2 N4 2.169(6) . ? In3 O2 1.972(5) . ? In3 O3 2.006(5) . ? In3 N6 2.163(5) . ? In3 N5 2.187(5) . ? N1 C1 1.323(8) . ? N1 C6 1.437(8) . ? N2 C3 1.337(8) . ? N2 C14 1.449(8) . ? N3 C22 1.337(9) . ? N3 C27 1.431(8) . ? N4 C24 1.333(10) . ? N4 C35 1.436(9) . ? N5 C43 1.341(9) . ? N5 C48 1.440(8) . ? N6 C45 1.329(9) . ? N6 C56 1.456(8) . ? C1 C2 1.403(9) . ? C1 C4 1.519(9) . ? C2 C3 1.390(9) . ? C2 H2 0.95 . ? C3 C5 1.507(9) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 C11 1.394(9) . ? C6 C7 1.400(10) . ? C7 C8 1.384(10) . ? C7 C12 1.497(10) . ? C8 C9 1.357(12) . ? C8 H8 0.95 . ? C9 C10 1.366(12) . ? C9 H9 0.95 . ? C10 C11 1.411(10) . ? C10 H10 0.95 . ? C11 C13 1.489(11) . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 C15 1.375(10) . ? C14 C19 1.390(10) . ? C15 C16 1.404(11) . ? C15 C20 1.496(11) . ? C16 C17 1.366(13) . ? C16 H16 0.95 . ? C17 C18 1.370(12) . ? C17 H17 0.95 . ? C18 C19 1.390(10) . ? C18 H18 0.95 . ? C19 C21 1.494(10) . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 C23 1.397(11) . ? C22 C25 1.518(10) . ? C23 C24 1.384(11) . ? C23 H23 0.95 . ? C24 C26 1.537(10) . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 C32 1.358(10) . ? C27 C28 1.446(10) . ? C28 C29 1.353(10) . ? C28 C33 1.488(10) . ? C29 C30 1.350(12) . ? C29 H29 0.95 . ? C30 C31 1.350(13) . ? C30 H30 0.95 . ? C31 C32 1.458(13) . ? C31 H31 0.95 . ? C32 C34 1.488(13) . ? C33 H33A 0.98 . ? C33 H33B 0.98 . ? C33 H33C 0.98 . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 C40 1.393(11) . ? C35 C36 1.398(11) . ? C36 C37 1.385(12) . ? C36 C41 1.492(12) . ? C37 C38 1.359(13) . ? C37 H37 0.95 . ? C38 C39 1.368(12) . ? C38 H38 0.95 . ? C39 C40 1.391(11) . ? C39 H39 0.95 . ? C40 C42 1.501(11) . ? C41 H41A 0.98 . ? C41 H41B 0.98 . ? C41 H41C 0.98 . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? C43 C44 1.383(10) . ? C43 C46 1.517(9) . ? C44 C45 1.400(9) . ? C44 H44 0.95 . ? C45 C47 1.500(9) . ? C46 H46A 0.98 . ? C46 H46B 0.98 . ? C46 H46C 0.98 . ? C47 H47A 0.98 . ? C47 H47B 0.98 . ? C47 H47C 0.98 . ? C48 C53 1.381(10) . ? C48 C49 1.387(10) . ? C49 C50 1.395(12) . ? C49 C54 1.502(12) . ? C50 C51 1.350(13) . ? C50 H50 0.95 . ? C51 C52 1.371(12) . ? C51 H51 0.95 . ? C52 C53 1.377(10) . ? C52 H52 0.95 . ? C53 C55 1.520(10) . ? C54 H54A 0.98 . ? C54 H54B 0.98 . ? C54 H54C 0.98 . ? C55 H55A 0.98 . ? C55 H55B 0.98 . ? C55 H55C 0.98 . ? C56 C57 1.387(10) . ? C56 C61 1.401(10) . ? C57 C58 1.399(10) . ? C57 C62 1.479(10) . ? C58 C59 1.348(11) . ? C58 H58 0.95 . ? C59 C60 1.383(11) . ? C59 H59 0.95 . ? C60 C61 1.389(10) . ? C60 H60 0.95 . ? C61 C63 1.479(11) . ? C62 H62A 0.98 . ? C62 H62B 0.98 . ? C62 H62C 0.98 . ? C63 H63A 0.98 . ? C63 H63B 0.98 . ? C63 H63C 0.98 . ? 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 116.77(19) . . ? O3 In1 N2 116.61(19) . . ? O1 In1 N2 107.10(19) . . ? O3 In1 N1 110.3(2) . . ? O1 In1 N1 114.84(19) . . ? N2 In1 N1 87.9(2) . . ? O1 In2 O2 117.5(2) . . ? O1 In2 N3 109.1(2) . . ? O2 In2 N3 112.7(2) . . ? O1 In2 N4 119.7(2) . . ? O2 In2 N4 106.5(2) . . ? N3 In2 N4 87.8(2) . . ? O2 In3 O3 117.7(2) . . ? O2 In3 N6 110.8(2) . . ? O3 In3 N6 109.7(2) . . ? O2 In3 N5 117.3(2) . . ? O3 In3 N5 109.5(2) . . ? N6 In3 N5 87.7(2) . . ? In2 O1 In1 122.5(2) . . ? In3 O2 In2 122.3(2) . . ? In1 O3 In3 123.0(2) . . ? C1 N1 C6 117.5(5) . . ? C1 N1 In1 121.6(4) . . ? C6 N1 In1 121.0(4) . . ? C3 N2 C14 117.2(5) . . ? C3 N2 In1 121.1(4) . . ? C14 N2 In1 121.6(4) . . ? C22 N3 C27 117.1(6) . . ? C22 N3 In2 122.8(5) . . ? C27 N3 In2 120.1(4) . . ? C24 N4 C35 118.0(6) . . ? C24 N4 In2 121.7(5) . . ? C35 N4 In2 120.0(5) . . ? C43 N5 C48 118.7(6) . . ? C43 N5 In3 119.5(4) . . ? C48 N5 In3 121.6(5) . . ? C45 N6 C56 117.0(6) . . ? C45 N6 In3 121.2(4) . . ? C56 N6 In3 121.8(4) . . ? N1 C1 C2 125.1(6) . . ? N1 C1 C4 119.4(6) . . ? C2 C1 C4 115.5(6) . . ? C3 C2 C1 130.4(7) . . ? C3 C2 H2 114.8 . . ? C1 C2 H2 114.8 . . ? N2 C3 C2 125.0(7) . . ? N2 C3 C5 118.9(6) . . ? C2 C3 C5 116.1(7) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 C7 120.9(7) . . ? C11 C6 N1 120.1(6) . . ? C7 C6 N1 118.9(6) . . ? C8 C7 C6 119.5(8) . . ? C8 C7 C12 120.1(8) . . ? C6 C7 C12 120.4(7) . . ? C9 C8 C7 120.3(9) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 120.8(9) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C9 C10 C11 121.5(8) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C6 C11 C10 117.0(8) . . ? C6 C11 C13 120.8(7) . . ? C10 C11 C13 122.2(7) . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 121.7(7) . . ? C15 C14 N2 118.3(7) . . ? C19 C14 N2 119.9(6) . . ? C14 C15 C16 118.2(8) . . ? C14 C15 C20 120.8(7) . . ? C16 C15 C20 120.9(8) . . ? C17 C16 C15 120.4(8) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 120.7(8) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C17 C18 C19 120.4(9) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C14 C19 C18 118.5(8) . . ? C14 C19 C21 122.2(6) . . ? C18 C19 C21 119.4(8) . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N3 C22 C23 124.6(7) . . ? N3 C22 C25 117.8(7) . . ? C23 C22 C25 117.6(7) . . ? C24 C23 C22 129.8(8) . . ? C24 C23 H23 115.1 . . ? C22 C23 H23 115.1 . . ? N4 C24 C23 125.6(7) . . ? N4 C24 C26 119.0(7) . . ? C23 C24 C26 115.3(8) . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C32 C27 N3 121.6(8) . . ? C32 C27 C28 121.5(7) . . ? N3 C27 C28 116.9(6) . . ? C29 C28 C27 117.7(8) . . ? C29 C28 C33 122.5(8) . . ? C27 C28 C33 119.8(6) . . ? C30 C29 C28 120.2(9) . . ? C30 C29 H29 119.9 . . ? C28 C29 H29 119.9 . . ? C31 C30 C29 125.5(9) . . ? C31 C30 H30 117.3 . . ? C29 C30 H30 117.3 . . ? C30 C31 C32 116.2(9) . . ? C30 C31 H31 121.9 . . ? C32 C31 H31 121.9 . . ? C27 C32 C31 118.7(9) . . ? C27 C32 C34 120.3(9) . . ? C31 C32 C34 121.0(9) . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C40 C35 C36 121.7(8) . . ? C40 C35 N4 119.7(7) . . ? C36 C35 N4 118.5(8) . . ? C37 C36 C35 117.7(9) . . ? C37 C36 C41 120.8(9) . . ? C35 C36 C41 121.4(8) . . ? C38 C37 C36 121.3(9) . . ? C38 C37 H37 119.3 . . ? C36 C37 H37 119.3 . . ? C37 C38 C39 120.5(9) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C38 C39 C40 121.1(9) . . ? C38 C39 H39 119.4 . . ? C40 C39 H39 119.4 . . ? C39 C40 C35 117.5(9) . . ? C39 C40 C42 121.9(9) . . ? C35 C40 C42 120.5(7) . . ? C36 C41 H41A 109.5 . . ? C36 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C36 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N5 C43 C44 124.6(7) . . ? N5 C43 C46 119.1(7) . . ? C44 C43 C46 116.3(7) . . ? C43 C44 C45 131.0(8) . . ? C43 C44 H44 114.5 . . ? C45 C44 H44 114.5 . . ? N6 C45 C44 123.9(7) . . ? N6 C45 C47 119.1(6) . . ? C44 C45 C47 117.0(7) . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C53 C48 C49 119.5(7) . . ? C53 C48 N5 121.1(7) . . ? C49 C48 N5 119.4(7) . . ? C48 C49 C50 117.9(9) . . ? C48 C49 C54 120.9(7) . . ? C50 C49 C54 121.1(9) . . ? C51 C50 C49 122.4(9) . . ? C51 C50 H50 118.8 . . ? C49 C50 H50 118.8 . . ? C50 C51 C52 119.4(9) . . ? C50 C51 H51 120.3 . . ? C52 C51 H51 120.3 . . ? C51 C52 C53 119.9(8) . . ? C51 C52 H52 120.1 . . ? C53 C52 H52 120.1 . . ? C52 C53 C48 120.8(8) . . ? C52 C53 C55 118.8(8) . . ? C48 C53 C55 120.2(6) . . ? C49 C54 H54A 109.5 . . ? C49 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C49 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C57 C56 C61 122.8(7) . . ? C57 C56 N6 117.7(6) . . ? C61 C56 N6 119.5(7) . . ? C56 C57 C58 116.8(7) . . ? C56 C57 C62 121.6(6) . . ? C58 C57 C62 121.6(7) . . ? C59 C58 C57 122.1(8) . . ? C59 C58 H58 118.9 . . ? C57 C58 H58 118.9 . . ? C58 C59 C60 120.0(7) . . ? C58 C59 H59 120 . . ? C60 C59 H59 120 . . ? C59 C60 C61 121.2(8) . . ? C59 C60 H60 119.4 . . ? C61 C60 H60 119.4 . . ? C60 C61 C56 117.0(8) . . ? C60 C61 C63 122.1(8) . . ? C56 C61 C63 120.9(7) . . ? C57 C62 H62A 109.5 . . ? C57 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C57 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? #===END