# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- ccdc_887941-887946.cif' _publ_contact_author ; Zeckert, Kornelia Structure Determination: Zeckert, Kornelia Institut f\"ur Anorganische Chemie Universit\"at Leipzig Johannisallee 29 04103 Leipzig Bundesrepublik Deutschland ; _publ_contact_author_phone '49 / 341 / 9736130' _publ_contact_author_fax '49 / 341 / 9736199' _publ_contact_author_email zeckert@uni-leipzig.de _publ_section_title ; Syntheses and structures of lanthanoid(II) complexes featuring Sn^II^-M^II^ (M = Al, Ga, In) bonds ; loop_ _publ_author_address ; Institut f\"ur Anorganische Chemie Universit\"at Leipzig Johannisallee 29 04103 Leipzig Bundesrepublik Deutschland ; _publ_requested_category FM _publ_contact_author_name 'Zeckert, Kornelia' _publ_author_name K.Zeckert #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-03-01 at 09:16:07 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\software\wingx\files\archive.dat # CIF files read : x1110 x1110m data_x1110 #TrackingRef '- ccdc_887941-887946.cif' _database_code_depnum_ccdc_archive 'CCDC 887941' _audit_creation_date 2011-03-01T09:16:07-00:00 _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 'C24 H33 N3 Ga Li Sn' _chemical_formula_sum 'C24 H33 Ga Li N3 Sn' _chemical_formula_weight 558.88 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 15.2718(2) _cell_length_b 15.6336(3) _cell_length_c 10.9156(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2606.13(8) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 29116 _cell_measurement_theta_min 2.9217 _cell_measurement_theta_max 32.3681 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.006 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.58 (release 29-01-2010 CrysAlis171 .NET) (compiled Jan 29 2010,16:49:25) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.91291 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.356 _diffrn_orient_matrix_ub_11 0.0447929 _diffrn_orient_matrix_ub_12 -0.0068883 _diffrn_orient_matrix_ub_13 -0.0109697 _diffrn_orient_matrix_ub_21 -0.0122611 _diffrn_orient_matrix_ub_22 -0.0220613 _diffrn_orient_matrix_ub_23 -0.0409426 _diffrn_orient_matrix_ub_31 0.0006297 _diffrn_orient_matrix_ub_32 0.0607591 _diffrn_orient_matrix_ub_33 -0.0161361 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.029 _diffrn_reflns_av_unetI/netI 0.015 _diffrn_reflns_number 52538 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 30.5 _diffrn_reflns_theta_full 30.5 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 4100 _reflns_number_gt 3602 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.58 (release 29-01-2010 CrysAlis171 .NET) (compiled Jan 29 2010,16:49:25) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.58 (release 29-01-2010 CrysAlis171 .NET) (compiled Jan 29 2010,16:49:25) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.58 (release 29-01-2010 CrysAlis171 .NET) (compiled Jan 29 2010,16:49:25) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0357P)^2^+4.6265P] 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 4100 _refine_ls_number_parameters 164 _refine_ls_number_restraints 43 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.079 _refine_ls_wR_factor_gt 0.0772 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.03 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.028 _refine_diff_density_min -1.133 _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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 '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 Ga1 Ga 0.03115(2) 0.25 1.06345(3) 0.02450(9) Uani 1 2 d SDU . . C15A C 0.0630(4) 0.3508(4) 1.1648(5) 0.0389(14) Uani 0.620(9) 1 d PDU A 1 H15A H 0.017 0.3595 1.2274 0.047 Uiso 0.620(9) 1 calc PR A 1 H15B H 0.1184 0.3382 1.2083 0.047 Uiso 0.620(9) 1 calc PR A 1 C16A C 0.0741(5) 0.4321(4) 1.0939(5) 0.0581(19) Uani 0.620(9) 1 d PDU A 1 H16A H 0.0891 0.4787 1.1502 0.087 Uiso 0.620(9) 1 calc PR A 1 H16B H 0.0193 0.4458 1.0515 0.087 Uiso 0.620(9) 1 calc PR A 1 H16C H 0.1211 0.425 1.0336 0.087 Uiso 0.620(9) 1 calc PR A 1 C15B C 0.0372(6) 0.3711(5) 1.1334(8) 0.0311(18) Uani 0.380(9) 1 d PDU A 2 H15C H 0.0108 0.4112 1.0737 0.037 Uiso 0.380(9) 1 calc PR A 2 H15D H 0.0017 0.3735 1.2093 0.037 Uiso 0.380(9) 1 calc PR A 2 C16B C 0.1307(7) 0.4013(8) 1.1629(11) 0.067(3) Uiso 0.380(9) 1 d PDU A 2 H16D H 0.1289 0.4598 1.195 0.1 Uiso 0.380(9) 1 calc PR A 2 H16E H 0.1662 0.4 1.0881 0.1 Uiso 0.380(9) 1 calc PR A 2 H16F H 0.1567 0.3632 1.2242 0.1 Uiso 0.380(9) 1 calc PR A 2 C1 C 0.15547(14) 0.35343(14) 0.7451(2) 0.0234(4) Uani 1 1 d . . . C2 C 0.09084(17) 0.41616(17) 0.7357(3) 0.0372(6) Uani 1 1 d . A . H2 H 0.0452 0.4186 0.7947 0.045 Uiso 1 1 calc R . . C3 C 0.0930(2) 0.47486(18) 0.6407(4) 0.0528(9) Uani 1 1 d . . . H3 H 0.0486 0.5171 0.6344 0.063 Uiso 1 1 calc R A . C4 C 0.1592(2) 0.4721(2) 0.5556(4) 0.0542(10) Uani 1 1 d . A . C5 C 0.22325(17) 0.4106(2) 0.5731(3) 0.0415(7) Uani 1 1 d . . . H5 H 0.2712 0.4096 0.5176 0.05 Uiso 1 1 calc R A . C6 C 0.1630(2) 0.5297(3) 0.4439(4) 0.0786(13) Uani 1 1 d . . . H6A H 0.2156 0.5165 0.3961 0.118 Uiso 1 1 calc R A . H6B H 0.1649 0.5897 0.4702 0.118 Uiso 1 1 calc R . . H6C H 0.1109 0.5203 0.3933 0.118 Uiso 1 1 calc R . . C7 C 0.2877(2) 0.25 0.9354(3) 0.0266(7) Uani 1 2 d S . . C8 C 0.3124(3) 0.25 1.0576(3) 0.0670(19) Uani 1 2 d S A . H8 H 0.2688 0.25 1.1197 0.08 Uiso 1 2 calc SR . . C9 C 0.4001(3) 0.25 1.0898(4) 0.075(2) Uani 1 2 d S . . H9 H 0.4168 0.25 1.1736 0.09 Uiso 1 2 calc SR A . C10 C 0.4632(2) 0.25 0.9992(3) 0.0399(10) Uani 1 2 d S A . C11 C 0.43420(19) 0.25 0.8800(3) 0.0214(6) Uani 1 2 d S . . H11 H 0.4769 0.25 0.8168 0.026 Uiso 1 2 calc SR A . C12 C 0.5598(4) 0.25 1.0288(6) 0.0786(13) Uani 1 2 d S . . H12A H 0.5678 0.25 1.1179 0.118 Uiso 1 2 calc SR A . H12B H 0.5872 0.3012 0.9939 0.118 Uiso 0.5 1 calc PR . . H12C H 0.5872 0.1988 0.9939 0.118 Uiso 0.5 1 calc PR . . C13 C -0.0884(2) 0.25 0.9863(3) 0.0363(9) Uani 1 2 d S . . H13A H -0.0949 0.3013 0.9338 0.044 Uiso 0.5 1 calc PR . . H13B H -0.0949 0.1987 0.9338 0.044 Uiso 0.5 1 calc PR . . C14 C -0.1604(2) 0.25 1.0854(4) 0.0570(15) Uani 1 2 d S . . H14A H -0.2181 0.25 1.046 0.085 Uiso 1 2 calc SR A . H14B H -0.1544 0.3012 1.1365 0.085 Uiso 0.5 1 calc PR . . H14C H -0.1544 0.1988 1.1365 0.085 Uiso 0.5 1 calc PR . . N1 N 0.22207(12) 0.35207(13) 0.66333(19) 0.0262(4) Uani 1 1 d . A . N2 N 0.34952(15) 0.25 0.8469(2) 0.0182(5) Uani 1 2 d S A . Sn1 Sn 0.149728(13) 0.25 0.880701(19) 0.02076(6) Uani 1 2 d S . . Li1 Li 0.3026(4) 0.25 0.6759(5) 0.0255(11) Uani 1 2 d S . . 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 Ga1 0.01567(15) 0.0416(2) 0.01626(16) 0 0.00126(12) 0 C15A 0.029(3) 0.064(4) 0.024(3) -0.012(2) 0.0016(19) -0.005(2) C16A 0.086(5) 0.045(3) 0.043(3) -0.014(2) 0.010(3) 0.005(3) C15B 0.028(4) 0.040(4) 0.025(4) -0.001(3) 0.001(3) -0.001(3) C1 0.0197(9) 0.0207(9) 0.0297(11) -0.0010(8) -0.0011(8) 0.0000(8) C2 0.0276(12) 0.0271(12) 0.0569(17) -0.0079(12) -0.0048(12) 0.0056(10) C3 0.0390(15) 0.0228(13) 0.097(3) 0.0097(15) -0.0228(17) 0.0044(11) C4 0.0385(16) 0.0397(16) 0.084(3) 0.0360(17) -0.0222(16) -0.0120(13) C5 0.0259(12) 0.0467(16) 0.0517(16) 0.0289(14) -0.0058(11) -0.0098(11) C6 0.0474(16) 0.096(3) 0.093(3) 0.071(3) -0.0237(17) -0.0195(19) C7 0.0164(13) 0.045(2) 0.0185(14) 0 0.0001(11) 0 C8 0.0184(17) 0.168(6) 0.0144(16) 0 0.0032(13) 0 C9 0.0183(17) 0.193(7) 0.0129(16) 0 0.0005(13) 0 C10 0.0185(15) 0.083(3) 0.0182(15) 0 0.0007(12) 0 C11 0.0148(12) 0.0322(16) 0.0172(13) 0 0.0013(10) 0 C12 0.0474(16) 0.096(3) 0.093(3) 0.071(3) -0.0237(17) -0.0195(19) C13 0.0184(14) 0.072(3) 0.0186(15) 0 0.0000(12) 0 C14 0.0165(16) 0.132(5) 0.0227(17) 0 0.0009(13) 0 N1 0.0194(8) 0.0286(10) 0.0306(10) 0.0098(8) -0.0011(7) -0.0019(7) N2 0.0150(10) 0.0234(12) 0.0161(11) 0 0.0004(8) 0 Sn1 0.01448(9) 0.03234(12) 0.01545(10) 0 0.00217(7) 0 Li1 0.022(3) 0.036(3) 0.018(2) 0 -0.003(2) 0 #----------------------------------------------------------------------------# # 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 Ga1 C15A 1.986(5) . ? Ga1 C15A 1.986(5) 7_565 ? Ga1 C13 2.010(3) . ? Ga1 C15B 2.044(8) . ? Ga1 C15B 2.044(8) 7_565 ? Ga1 Sn1 2.6942(4) . ? C15A C16A 1.498(8) . ? C15A H15A 0.99 . ? C15A H15B 0.99 . ? C16A H16A 0.98 . ? C16A H16B 0.98 . ? C16A H16C 0.98 . ? C15B C16B 1.538(11) . ? C15B H15C 0.99 . ? C15B H15D 0.99 . ? C16B H16D 0.98 . ? C16B H16E 0.98 . ? C16B H16F 0.98 . ? C1 N1 1.353(3) . ? C1 C2 1.395(3) . ? C1 Sn1 2.194(2) . ? C2 C3 1.385(5) . ? C2 H2 0.95 . ? C3 C4 1.374(6) . ? C3 H3 0.95 . ? C4 C5 1.385(4) . ? C4 C6 1.517(5) . ? C5 N1 1.344(3) . ? C5 H5 0.95 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 N2 1.351(4) . ? C7 C8 1.386(5) . ? C7 Sn1 2.189(3) . ? C8 C9 1.386(5) . ? C8 H8 0.95 . ? C9 C10 1.381(5) . ? C9 H9 0.95 . ? C10 C11 1.375(5) . ? C10 C12 1.510(6) . ? C11 N2 1.343(4) . ? C11 H11 0.95 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 C14 1.543(5) . ? C13 Li1 2.430(7) 6_557 ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? N1 Li1 2.019(4) . ? N2 Li1 1.999(6) . ? Sn1 C1 2.194(2) 7_565 ? Sn1 Li1 3.232(6) . ? Li1 N1 2.019(4) 7_565 ? Li1 C13 2.430(7) 6_657 ? 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 C15A Ga1 C15A 105.0(4) . 7_565 ? C15A Ga1 C13 117.1(2) . . ? C15A Ga1 C13 117.1(2) 7_565 . ? C15A Ga1 C15B 17.4(2) . . ? C15A Ga1 C15B 121.1(4) 7_565 . ? C13 Ga1 C15B 101.4(3) . . ? C15A Ga1 C15B 121.1(4) . 7_565 ? C15A Ga1 C15B 17.4(2) 7_565 7_565 ? C13 Ga1 C15B 101.4(3) . 7_565 ? C15B Ga1 C15B 135.8(5) . 7_565 ? C15A Ga1 Sn1 104.34(16) . . ? C15A Ga1 Sn1 104.34(16) 7_565 . ? C13 Ga1 Sn1 107.46(10) . . ? C15B Ga1 Sn1 104.3(2) . . ? C15B Ga1 Sn1 104.3(2) 7_565 . ? C16A C15A Ga1 114.4(4) . . ? C16A C15A H15A 108.7 . . ? Ga1 C15A H15A 108.7 . . ? C16A C15A H15B 108.7 . . ? Ga1 C15A H15B 108.7 . . ? H15A C15A H15B 107.6 . . ? C15A C16A H16A 109.5 . . ? C15A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C15A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? C16B C15B Ga1 113.8(7) . . ? C16B C15B H15C 108.8 . . ? Ga1 C15B H15C 108.8 . . ? C16B C15B H15D 108.8 . . ? Ga1 C15B H15D 108.8 . . ? H15C C15B H15D 107.7 . . ? C15B C16B H16D 109.5 . . ? C15B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C15B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? N1 C1 C2 119.6(2) . . ? N1 C1 Sn1 117.61(15) . . ? C2 C1 Sn1 122.63(19) . . ? C3 C2 C1 120.2(3) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C4 C3 C2 120.2(3) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 116.6(3) . . ? C3 C4 C6 123.5(3) . . ? C5 C4 C6 119.8(4) . . ? N1 C5 C4 124.3(3) . . ? N1 C5 H5 117.8 . . ? C4 C5 H5 117.8 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 119.8(3) . . ? N2 C7 Sn1 118.6(2) . . ? C8 C7 Sn1 121.6(2) . . ? C9 C8 C7 120.5(3) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C10 C9 C8 119.6(4) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C11 C10 C9 116.9(3) . . ? C11 C10 C12 121.2(4) . . ? C9 C10 C12 121.9(4) . . ? N2 C11 C10 124.4(3) . . ? N2 C11 H11 117.8 . . ? C10 C11 H11 117.8 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 Ga1 110.7(2) . . ? C14 C13 Li1 91.3(2) . 6_557 ? Ga1 C13 Li1 158.0(2) . 6_557 ? C14 C13 H13A 109.5 . . ? Ga1 C13 H13A 109.5 . . ? Li1 C13 H13A 60.6 6_557 . ? C14 C13 H13B 109.5 . . ? Ga1 C13 H13B 109.5 . . ? Li1 C13 H13B 60.6 6_557 . ? H13A C13 H13B 108.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C5 N1 C1 118.9(2) . . ? C5 N1 Li1 125.4(2) . . ? C1 N1 Li1 115.2(2) . . ? C11 N2 C7 118.7(3) . . ? C11 N2 Li1 126.6(3) . . ? C7 N2 Li1 114.6(3) . . ? C7 Sn1 C1 98.36(8) . 7_565 ? C7 Sn1 C1 98.36(8) . . ? C1 Sn1 C1 94.96(12) 7_565 . ? C7 Sn1 Ga1 116.42(8) . . ? C1 Sn1 Ga1 121.76(6) 7_565 . ? C1 Sn1 Ga1 121.76(6) . . ? C7 Sn1 Li1 59.57(13) . . ? C1 Sn1 Li1 60.30(8) 7_565 . ? C1 Sn1 Li1 60.30(8) . . ? Ga1 Sn1 Li1 175.99(10) . . ? N2 Li1 N1 106.4(2) . 7_565 ? N2 Li1 N1 106.4(2) . . ? N1 Li1 N1 104.4(3) 7_565 . ? N2 Li1 C13 115.8(3) . 6_657 ? N1 Li1 C13 111.57(19) 7_565 6_657 ? N1 Li1 C13 111.57(19) . 6_657 ? N2 Li1 Sn1 67.25(17) . . ? N1 Li1 Sn1 66.87(16) 7_565 . ? N1 Li1 Sn1 66.87(16) . . ? C13 Li1 Sn1 177.0(2) 6_657 . ? #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2012-05-15 at 16:04:47 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\software\wingx\files\archive.dat # CIF files read : x1552 x1552m data_x1552 #TrackingRef '- ccdc_887941-887946.cif' _database_code_depnum_ccdc_archive 'CCDC 887942' _audit_creation_date 2012-05-15T16:04:47-00:00 _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 'C28 H41 Ga Li N3 O Sn' _chemical_formula_sum 'C28 H41 Ga Li N3 O Sn' _chemical_formula_weight 630.99 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.5639(8) _cell_length_b 21.5517(6) _cell_length_c 17.2611(8) _cell_angle_alpha 90 _cell_angle_beta 117.100(6) _cell_angle_gamma 90 _cell_volume 6147.7(4) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5238 _cell_measurement_theta_min 2.8089 _cell_measurement_theta_max 30.4541 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description rods _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.363 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2576 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.711 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.99042 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.356 _diffrn_orient_matrix_ub_11 0.0146366 _diffrn_orient_matrix_ub_12 0.0090669 _diffrn_orient_matrix_ub_13 0.0441149 _diffrn_orient_matrix_ub_21 0.0257616 _diffrn_orient_matrix_ub_22 0.0220856 _diffrn_orient_matrix_ub_23 -0.0052157 _diffrn_orient_matrix_ub_31 -0.031079 _diffrn_orient_matrix_ub_32 0.0226201 _diffrn_orient_matrix_ub_33 -0.0126617 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0984 _diffrn_reflns_av_unetI/netI 0.1176 _diffrn_reflns_number 39268 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 25.35 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 11248 _reflns_number_gt 5805 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0343P)^2^+0.7181P] 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 11248 _refine_ls_number_parameters 672 _refine_ls_number_restraints 353 _refine_ls_R_factor_all 0.1454 _refine_ls_R_factor_gt 0.0624 _refine_ls_wR_factor_ref 0.1351 _refine_ls_wR_factor_gt 0.104 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.924 _refine_diff_density_min -0.598 _refine_diff_density_rms 0.091 #----------------------------------------------------------------------------# # 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' 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' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 '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 C1 C 0.4844(4) 0.7806(4) 0.0635(4) 0.0481(19) Uani 1 1 d . A . C2 C 0.5477(5) 0.8172(4) 0.0673(5) 0.061(2) Uani 1 1 d . . . H2 H 0.5481 0.8604 0.0789 0.073 Uiso 1 1 calc R . . C3 C 0.6101(5) 0.7919(4) 0.0544(5) 0.061(2) Uani 1 1 d . . . H3 H 0.6533 0.8175 0.0584 0.073 Uiso 1 1 calc R . . C4 C 0.6094(4) 0.7300(4) 0.0359(4) 0.054(2) Uani 1 1 d . . . C5 C 0.5464(5) 0.6968(4) 0.0347(4) 0.055(2) Uani 1 1 d . . . H5 H 0.546 0.6534 0.0244 0.066 Uiso 1 1 calc R . . C6 C 0.6758(4) 0.7004(4) 0.0209(5) 0.074(3) Uani 1 1 d . . . H6A H 0.7077 0.7328 0.0109 0.11 Uiso 1 1 calc R . . H6B H 0.6518 0.6732 -0.03 0.11 Uiso 1 1 calc R . . H6C H 0.7111 0.6761 0.0722 0.11 Uiso 1 1 calc R . . C7 C 0.2875(4) 0.7805(4) -0.0385(5) 0.057(2) Uani 1 1 d . A . C8 C 0.2256(5) 0.8164(4) -0.1008(5) 0.068(2) Uani 1 1 d . . . H8 H 0.2252 0.8601 -0.0931 0.082 Uiso 1 1 calc R . . C9 C 0.1651(5) 0.7887(5) -0.1736(6) 0.079(3) Uani 1 1 d . . . H9 H 0.1231 0.8134 -0.2158 0.094 Uiso 1 1 calc R . . C10 C 0.1654(5) 0.7266(6) -0.1848(5) 0.077(3) Uani 1 1 d . . . C11 C 0.2283(5) 0.6934(4) -0.1213(6) 0.067(2) Uani 1 1 d . . . H11 H 0.2287 0.6497 -0.1284 0.081 Uiso 1 1 calc R . . C12 C 0.0995(5) 0.6928(5) -0.2623(6) 0.110(4) Uani 1 1 d . . . H12A H 0.0552 0.6818 -0.2489 0.166 Uiso 1 1 calc R . . H12B H 0.122 0.6551 -0.2744 0.166 Uiso 1 1 calc R . . H12C H 0.0789 0.72 -0.3135 0.166 Uiso 1 1 calc R . . C13 C 0.3790(4) 0.7491(3) 0.1699(4) 0.0470(19) Uani 1 1 d . A . C14 C 0.3757(4) 0.7658(4) 0.2457(5) 0.061(2) Uani 1 1 d . . . H14 H 0.3722 0.8085 0.2575 0.073 Uiso 1 1 calc R . . C15 C 0.3775(5) 0.7211(4) 0.3050(5) 0.063(2) Uani 1 1 d . . . H15 H 0.3771 0.7331 0.3578 0.076 Uiso 1 1 calc R . . C16 C 0.3798(4) 0.6597(4) 0.2863(5) 0.053(2) Uani 1 1 d . . . C17 C 0.3812(4) 0.6458(3) 0.2091(4) 0.0496(19) Uani 1 1 d . . . H17 H 0.3815 0.6033 0.1949 0.06 Uiso 1 1 calc R . . C18 C 0.3809(5) 0.6077(3) 0.3459(5) 0.072(2) Uani 1 1 d . . . H18A H 0.4087 0.6218 0.4065 0.108 Uiso 1 1 calc R . . H18B H 0.4095 0.5719 0.3383 0.108 Uiso 1 1 calc R . . H18C H 0.3253 0.5959 0.3315 0.108 Uiso 1 1 calc R . . C19 C 0.3633(8) 0.5347(5) 0.0263(7) 0.149(3) Uani 1 1 d U . . H19A H 0.3092 0.5404 0.0234 0.179 Uiso 1 1 calc R . . H19B H 0.4022 0.5248 0.0872 0.179 Uiso 1 1 calc R . . C20 C 0.3608(9) 0.4826(5) -0.0325(7) 0.149(3) Uani 1 1 d U . . H20A H 0.4083 0.455 -0.0032 0.179 Uiso 1 1 calc R . . H20B H 0.3108 0.4578 -0.051 0.179 Uiso 1 1 calc R . . C21 C 0.3624(9) 0.5135(5) -0.1045(8) 0.156(5) Uani 1 1 d U . . H21A H 0.3994 0.4917 -0.1223 0.187 Uiso 1 1 calc R . . H21B H 0.3076 0.5138 -0.1545 0.187 Uiso 1 1 calc R . . C22 C 0.3894(7) 0.5751(5) -0.0790(7) 0.112(3) Uani 1 1 d U . . H22A H 0.3543 0.6045 -0.1246 0.134 Uiso 1 1 calc R . . H22B H 0.4454 0.5798 -0.0708 0.134 Uiso 1 1 calc R . . C23 C 0.4905(6) 0.9558(5) 0.2310(6) 0.149(3) Uani 1 1 d DU . . H23A H 0.5296 0.9712 0.2111 0.179 Uiso 1 1 calc R . . H23B H 0.4821 0.9897 0.2647 0.179 Uiso 1 1 calc R . . C24 C 0.5290(7) 0.9036(5) 0.2913(7) 0.149(3) Uani 1 1 d DU . . H24A H 0.4898 0.8849 0.3076 0.224 Uiso 1 1 calc R . . H24B H 0.5756 0.9189 0.3436 0.224 Uiso 1 1 calc R . . H24C H 0.5471 0.8725 0.2627 0.224 Uiso 1 1 calc R . . C25 C 0.2888(5) 0.9499(4) 0.1466(7) 0.112(3) Uani 1 1 d DU . . H25A H 0.2921 0.9196 0.1912 0.134 Uiso 0.729(11) 1 calc PR A 1 H25B H 0.2878 0.992 0.1688 0.134 Uiso 0.729(11) 1 calc PR A 1 C26 C 0.2123(5) 0.9391(4) 0.0639(7) 0.136(5) Uani 0.729(11) 1 d PRDU A 1 H26A H 0.2237 0.9116 0.0256 0.203 Uiso 0.729(11) 1 calc PR A 1 H26B H 0.1916 0.9788 0.0346 0.203 Uiso 0.729(11) 1 calc PR A 1 H26C H 0.1717 0.9198 0.0777 0.203 Uiso 0.729(11) 1 calc PR A 1 H25C H 0.2972 0.9867 0.1841 0.163 Uiso 0.271(11) 1 d PR A 2 H25D H 0.2441 0.9603 0.0888 0.163 Uiso 0.271(11) 1 d PR A 2 C26F C 0.243(2) 0.9067(14) 0.176(3) 0.136(5) Uani 0.271(11) 1 d PDU A 2 H26D H 0.2223 0.8718 0.1349 0.203 Uiso 0.271(11) 1 calc PR A 2 H26E H 0.1975 0.9289 0.1771 0.203 Uiso 0.271(11) 1 calc PR A 2 H26F H 0.2789 0.8911 0.234 0.203 Uiso 0.271(11) 1 calc PR A 2 C27 C 0.335(2) 0.994(2) 0.017(2) 0.133(4) Uani 0.244(11) 1 d PDU A 3 H27A H 0.294 0.969 -0.031 0.16 Uiso 0.244(11) 1 calc PR A 3 H27B H 0.3082 1.0298 0.0275 0.16 Uiso 0.244(11) 1 calc PR A 3 C28 C 0.398(3) 1.016(2) -0.009(3) 0.133(4) Uani 0.244(11) 1 d PDU A 3 H28A H 0.4479 1.0256 0.0437 0.2 Uiso 0.244(11) 1 calc PR A 3 H28B H 0.378 1.0529 -0.0448 0.2 Uiso 0.244(11) 1 calc PR A 3 H28C H 0.4086 0.983 -0.0415 0.2 Uiso 0.244(11) 1 calc PR A 3 C27F C 0.3835(11) 0.9902(5) 0.0255(9) 0.133(4) Uani 0.756(11) 1 d PDU A 4 H27C H 0.4353 0.9849 0.0229 0.16 Uiso 0.756(11) 1 calc PR A 4 H27D H 0.3393 0.9748 -0.0298 0.16 Uiso 0.756(11) 1 calc PR A 4 C28F C 0.3705(10) 1.0565(5) 0.0367(10) 0.133(4) Uani 0.756(11) 1 d PDU A 4 H28D H 0.3215 1.0612 0.0442 0.2 Uiso 0.756(11) 1 calc PR A 4 H28E H 0.3642 1.0797 -0.0148 0.2 Uiso 0.756(11) 1 calc PR A 4 H28F H 0.4171 1.0727 0.0883 0.2 Uiso 0.756(11) 1 calc PR A 4 C29 C 0.0093(5) 0.2071(4) 0.1281(5) 0.054(2) Uani 1 1 d . . . C30 C -0.0575(5) 0.1804(4) 0.0593(6) 0.069(2) Uani 1 1 d . . . H30 H -0.0668 0.1371 0.0605 0.083 Uiso 1 1 calc R . . C31 C -0.1107(5) 0.2151(5) -0.0109(6) 0.081(3) Uani 1 1 d . . . H31 H -0.1568 0.196 -0.0562 0.097 Uiso 1 1 calc R . . C32 C -0.0970(5) 0.2768(5) -0.0149(5) 0.069(2) Uani 1 1 d . . . C33 C -0.0279(5) 0.3008(4) 0.0530(5) 0.065(2) Uani 1 1 d . . . H33 H -0.0167 0.3436 0.0505 0.078 Uiso 1 1 calc R . . C34 C -0.1564(5) 0.3172(5) -0.0882(5) 0.102(3) Uani 1 1 d . . . H34A H -0.1826 0.2925 -0.1415 0.154 Uiso 1 1 calc R . . H34B H -0.1274 0.352 -0.0978 0.154 Uiso 1 1 calc R . . H34C H -0.1974 0.3332 -0.0726 0.154 Uiso 1 1 calc R . . C35 C 0.1054(4) 0.2327(4) 0.3393(4) 0.052(2) Uani 1 1 d . . . C36 C 0.0936(4) 0.2237(4) 0.4128(5) 0.059(2) Uani 1 1 d . . . H36 H 0.078 0.1841 0.4239 0.071 Uiso 1 1 calc R . . C37 C 0.1046(4) 0.2722(4) 0.4693(5) 0.063(2) Uani 1 1 d . . . H37 H 0.0968 0.2656 0.5194 0.076 Uiso 1 1 calc R . . C38 C 0.1265(4) 0.3297(4) 0.4541(5) 0.056(2) Uani 1 1 d . . . C39 C 0.1377(4) 0.3350(4) 0.3801(5) 0.054(2) Uani 1 1 d . . . H39 H 0.1534 0.3744 0.3682 0.065 Uiso 1 1 calc R . . C40 C 0.1365(5) 0.3843(4) 0.5118(5) 0.082(3) Uani 1 1 d . . . H40A H 0.1005 0.3797 0.539 0.123 Uiso 1 1 calc R . . H40B H 0.1227 0.4225 0.477 0.123 Uiso 1 1 calc R . . H40C H 0.1927 0.3866 0.5571 0.123 Uiso 1 1 calc R . . C41 C 0.1998(4) 0.1706(4) 0.2378(4) 0.051(2) Uani 1 1 d . . . C42 C 0.2538(5) 0.1236(4) 0.2490(4) 0.056(2) Uani 1 1 d . . . H42 H 0.2437 0.0835 0.2647 0.068 Uiso 1 1 calc R . . C43 C 0.3226(5) 0.1330(4) 0.2381(5) 0.064(2) Uani 1 1 d . . . H43 H 0.3592 0.0998 0.2466 0.077 Uiso 1 1 calc R . . C44 C 0.3370(4) 0.1913(4) 0.2147(5) 0.056(2) Uani 1 1 d . . . C45 C 0.2814(4) 0.2367(4) 0.2048(4) 0.055(2) Uani 1 1 d . . . H45 H 0.2906 0.2769 0.1887 0.066 Uiso 1 1 calc R . . C46 C 0.4091(5) 0.2048(4) 0.1995(5) 0.079(3) Uani 1 1 d . . . H46A H 0.3974 0.1921 0.1404 0.118 Uiso 1 1 calc R . . H46B H 0.4561 0.1817 0.2417 0.118 Uiso 1 1 calc R . . H46C H 0.4209 0.2494 0.2064 0.118 Uiso 1 1 calc R . . C47 C 0.2434(6) 0.4076(5) 0.2594(6) 0.105(3) Uani 1 1 d DU . . H47A H 0.29 0.3793 0.2891 0.126 Uiso 0.66(2) 1 calc PR B 5 H47B H 0.228 0.4246 0.3031 0.126 Uiso 0.66(2) 1 calc PR B 5 H47C H 0.2812 0.3782 0.303 0.126 Uiso 0.34(2) 1 d PR B 6 H47D H 0.2242 0.4374 0.2896 0.126 Uiso 0.34(2) 1 d PR B 6 C48 C 0.2647(12) 0.4589(9) 0.2153(11) 0.121(7) Uani 0.66(2) 1 d PDU B 5 H48A H 0.323 0.4692 0.2461 0.145 Uiso 0.66(2) 1 calc PR B 5 H48B H 0.2324 0.4967 0.2096 0.145 Uiso 0.66(2) 1 calc PR B 5 C49 C 0.2410(10) 0.4277(10) 0.1244(10) 0.119(7) Uani 0.66(2) 1 d PDU B 5 H49A H 0.2336 0.4586 0.0789 0.143 Uiso 0.66(2) 1 calc PR B 5 H49B H 0.2807 0.3959 0.1275 0.143 Uiso 0.66(2) 1 calc PR B 5 C48F C 0.2913(14) 0.4347(15) 0.2185(16) 0.114(8) Uani 0.34(2) 1 d PDU B 6 H48C H 0.3242 0.4033 0.2067 0.137 Uiso 0.34(2) 1 calc PR B 6 H48D H 0.3259 0.4697 0.2522 0.137 Uiso 0.34(2) 1 calc PR B 6 C49F C 0.2149(17) 0.4564(12) 0.1334(17) 0.119(10) Uani 0.34(2) 1 d PDU B 6 H49C H 0.1884 0.4926 0.1449 0.143 Uiso 0.34(2) 1 calc PR B 6 H49D H 0.2294 0.4668 0.0864 0.143 Uiso 0.34(2) 1 calc PR B 6 C50 C 0.1620(6) 0.3994(5) 0.1113(6) 0.115(4) Uani 1 1 d DU . . H50A H 0.1188 0.4312 0.0919 0.138 Uiso 0.66(2) 1 calc PR B 5 H50B H 0.1453 0.366 0.0671 0.138 Uiso 0.66(2) 1 calc PR B 5 H50C H 0.1037 0.4075 0.0744 0.138 Uiso 0.34(2) 1 d PR B 6 H50D H 0.1819 0.3707 0.0805 0.138 Uiso 0.34(2) 1 d PR B 6 Ga2 Ga 0.04217(7) 0.04495(5) 0.28114(7) 0.0881(4) Uani 1 1 d DU . . C51 C 0.1387(8) 0.0125(6) 0.3790(10) 0.112(5) Uani 0.737(18) 1 d PDU C 7 H51A H 0.1787 0.0011 0.3582 0.135 Uiso 0.737(18) 1 calc PR C 7 H51B H 0.1629 0.0458 0.4228 0.135 Uiso 0.737(18) 1 calc PR C 7 C52 C 0.1229(12) -0.0461(8) 0.4246(12) 0.136(8) Uani 0.737(18) 1 d PDU C 7 H52A H 0.0909 -0.0768 0.3803 0.203 Uiso 0.737(18) 1 calc PR C 7 H52B H 0.0932 -0.0333 0.4565 0.203 Uiso 0.737(18) 1 calc PR C 7 H52C H 0.1748 -0.0645 0.4651 0.203 Uiso 0.737(18) 1 calc PR C 7 C53 C -0.0110(10) -0.0002(10) 0.1730(11) 0.143(3) Uani 0.595(11) 1 d PDU C 7 H53A H -0.0348 -0.0392 0.1812 0.171 Uiso 0.595(11) 1 calc PR C 7 H53B H -0.0544 0.0251 0.1281 0.171 Uiso 0.595(11) 1 calc PR C 7 C54 C 0.0614(12) -0.0149(12) 0.1447(13) 0.143(3) Uani 0.595(11) 1 d PDU C 7 H54A H 0.0706 0.0219 0.117 0.214 Uiso 0.595(11) 1 calc PR C 7 H54B H 0.045 -0.0498 0.1037 0.214 Uiso 0.595(11) 1 calc PR C 7 H54C H 0.1114 -0.0256 0.1966 0.214 Uiso 0.595(11) 1 calc PR C 7 C51F C 0.091(3) 0.0362(16) 0.4089(12) 0.097(11) Uani 0.263(18) 1 d PDU C 8 H51C H 0.1497 0.0434 0.4354 0.117 Uiso 0.263(18) 1 calc PR C 8 H51D H 0.0667 0.0668 0.4333 0.117 Uiso 0.263(18) 1 calc PR C 8 C52F C 0.072(3) -0.0343(18) 0.430(3) 0.14(2) Uani 0.263(18) 1 d PDU C 8 H52D H 0.0151 -0.0376 0.4173 0.207 Uiso 0.263(18) 1 calc PR C 8 H52E H 0.1066 -0.0439 0.4912 0.207 Uiso 0.263(18) 1 calc PR C 8 H52F H 0.0831 -0.0638 0.3932 0.207 Uiso 0.263(18) 1 calc PR C 8 C53F C 0.0759(17) -0.0168(13) 0.2175(15) 0.143(3) Uani 0.405(11) 1 d PDU C 8 H53C H 0.1353 -0.0157 0.2394 0.171 Uiso 0.405(11) 1 calc PR C 8 H53D H 0.0601 -0.0592 0.2257 0.171 Uiso 0.405(11) 1 calc PR C 8 C54F C 0.0301(18) 0.0025(17) 0.1154(15) 0.143(3) Uani 0.405(11) 1 d PDU C 8 H54D H 0.0091 0.0449 0.1099 0.214 Uiso 0.405(11) 1 calc PR C 8 H54E H -0.0148 -0.0261 0.0838 0.214 Uiso 0.405(11) 1 calc PR C 8 H54F H 0.0684 0.0005 0.0909 0.214 Uiso 0.405(11) 1 calc PR C 8 C55 C -0.0292(11) 0.0711(13) 0.3379(14) 0.143(3) Uani 0.515(11) 1 d PDU C 9 H55A H -0.0163 0.0467 0.3912 0.171 Uiso 0.515(11) 1 calc PR C 9 H55B H -0.0229 0.1158 0.3526 0.171 Uiso 0.515(11) 1 calc PR C 9 C56 C -0.1229(11) 0.0552(13) 0.2596(15) 0.143(3) Uani 0.515(11) 1 d PDU C 9 H56A H -0.1206 0.0453 0.2054 0.214 Uiso 0.515(11) 1 calc PR C 9 H56B H -0.1578 0.0914 0.2505 0.214 Uiso 0.515(11) 1 calc PR C 9 H56C H -0.1448 0.0196 0.2774 0.214 Uiso 0.515(11) 1 calc PR C 9 C55F C -0.0766(10) 0.0387(13) 0.2306(13) 0.143(3) Uani 0.485(11) 1 d PDU C 10 H55C H -0.1051 0.0687 0.1828 0.171 Uiso 0.485(11) 1 calc PR C 10 H55D H -0.0969 -0.0039 0.2111 0.171 Uiso 0.485(11) 1 calc PR C 10 C56F C -0.0796(15) 0.0587(14) 0.3235(16) 0.143(3) Uani 0.485(11) 1 d PDU C 10 H56D H -0.0657 0.0227 0.3622 0.214 Uiso 0.485(11) 1 calc PR C 10 H56E H -0.1341 0.0731 0.3101 0.214 Uiso 0.485(11) 1 calc PR C 10 H56F H -0.0405 0.0921 0.3522 0.214 Uiso 0.485(11) 1 calc PR C 10 N1 N 0.4844(3) 0.7196(3) 0.0467(4) 0.0518(16) Uani 1 1 d . . . N2 N 0.2889(4) 0.7186(3) -0.0504(4) 0.0588(18) Uani 1 1 d . . . N3 N 0.3822(3) 0.6882(3) 0.1522(4) 0.0480(15) Uani 1 1 d . . . N4 N 0.0242(4) 0.2685(3) 0.1218(4) 0.0550(17) Uani 1 1 d . B . N5 N 0.1280(4) 0.2890(3) 0.3242(4) 0.0544(16) Uani 1 1 d . B . N6 N 0.2147(3) 0.2286(3) 0.2162(3) 0.0501(16) Uani 1 1 d . B . O1 O 0.3865(4) 0.5882(3) 0.0007(4) 0.0838(17) Uani 1 1 d U . . O2 O 0.1769(3) 0.3754(2) 0.1930(3) 0.0704(15) Uani 1 1 d DU B . Ga1 Ga 0.38595(6) 0.94100(4) 0.12595(7) 0.0754(3) Uani 1 1 d DU A . Sn1 Sn 0.38345(3) 0.81993(2) 0.08038(3) 0.05303(17) Uani 1 1 d . . . Sn2 Sn 0.08741(3) 0.15709(3) 0.24683(3) 0.05718(18) Uani 1 1 d . B . Li1 Li 0.3847(7) 0.6728(6) 0.0370(7) 0.056(3) Uani 1 1 d . A . Li2 Li 0.1334(8) 0.2970(6) 0.2103(7) 0.058(3) 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 C1 0.053(5) 0.057(5) 0.039(4) 0.000(4) 0.025(4) -0.005(4) C2 0.076(6) 0.059(6) 0.057(5) -0.005(4) 0.038(5) -0.009(5) C3 0.056(5) 0.076(7) 0.056(5) -0.001(5) 0.031(4) -0.019(5) C4 0.053(5) 0.075(6) 0.041(5) -0.002(4) 0.027(4) -0.004(5) C5 0.067(5) 0.050(5) 0.050(5) -0.001(4) 0.028(4) 0.002(4) C6 0.056(5) 0.115(8) 0.058(5) -0.004(5) 0.034(5) 0.007(5) C7 0.048(5) 0.089(7) 0.043(5) 0.006(5) 0.028(4) 0.008(5) C8 0.067(6) 0.094(7) 0.053(6) -0.002(5) 0.035(5) 0.005(5) C9 0.069(7) 0.109(9) 0.061(6) 0.014(6) 0.032(6) 0.036(6) C10 0.056(6) 0.132(9) 0.037(5) 0.004(6) 0.017(5) 0.003(6) C11 0.065(6) 0.079(7) 0.063(6) -0.015(5) 0.034(5) -0.012(5) C12 0.070(7) 0.167(11) 0.067(7) -0.013(7) 0.008(6) -0.008(7) C13 0.047(5) 0.052(5) 0.046(5) -0.016(4) 0.025(4) -0.012(4) C14 0.076(6) 0.066(6) 0.054(5) -0.013(4) 0.043(5) -0.004(5) C15 0.085(6) 0.073(6) 0.049(5) -0.005(4) 0.046(5) -0.005(5) C16 0.061(5) 0.055(5) 0.048(5) -0.002(4) 0.031(4) -0.007(4) C17 0.057(5) 0.052(5) 0.042(5) -0.007(4) 0.024(4) -0.008(4) C18 0.103(7) 0.065(6) 0.065(6) 0.005(5) 0.054(6) -0.004(5) C19 0.255(9) 0.073(5) 0.121(7) -0.028(5) 0.087(7) -0.039(6) C20 0.255(9) 0.073(5) 0.121(7) -0.028(5) 0.087(7) -0.039(6) C21 0.237(13) 0.112(9) 0.145(10) -0.060(7) 0.110(10) -0.054(9) C22 0.146(9) 0.091(7) 0.117(8) -0.043(6) 0.076(8) -0.022(7) C23 0.139(6) 0.119(9) 0.145(7) -0.030(6) 0.026(5) -0.016(6) C24 0.139(6) 0.119(9) 0.145(7) -0.030(6) 0.026(5) -0.016(6) C25 0.150(7) 0.079(7) 0.140(9) -0.029(7) 0.095(7) 0.009(7) C26 0.108(7) 0.113(12) 0.207(15) -0.049(11) 0.090(8) -0.013(9) C26F 0.108(7) 0.113(12) 0.207(15) -0.049(11) 0.090(8) -0.013(9) C27 0.213(10) 0.077(6) 0.159(7) 0.026(6) 0.127(7) 0.001(8) C28 0.213(10) 0.077(6) 0.159(7) 0.026(6) 0.127(7) 0.001(8) C27F 0.213(10) 0.077(6) 0.159(7) 0.026(6) 0.127(7) 0.001(8) C28F 0.213(10) 0.077(6) 0.159(7) 0.026(6) 0.127(7) 0.001(8) C29 0.057(5) 0.058(6) 0.060(5) -0.003(4) 0.040(5) -0.003(4) C30 0.069(6) 0.084(7) 0.070(6) -0.007(5) 0.046(6) -0.019(5) C31 0.051(6) 0.135(10) 0.052(6) 0.007(6) 0.019(5) -0.015(6) C32 0.051(6) 0.110(8) 0.054(6) 0.007(6) 0.030(5) 0.011(6) C33 0.064(6) 0.076(6) 0.066(6) -0.001(5) 0.039(5) 0.004(5) C34 0.070(6) 0.163(10) 0.057(6) 0.024(6) 0.015(5) 0.036(7) C35 0.044(5) 0.071(6) 0.044(5) 0.015(4) 0.023(4) 0.011(4) C36 0.065(6) 0.072(6) 0.051(5) 0.014(4) 0.036(5) 0.011(4) C37 0.062(5) 0.095(7) 0.039(5) 0.007(5) 0.029(4) 0.009(5) C38 0.050(5) 0.074(6) 0.042(5) 0.003(4) 0.018(4) 0.015(4) C39 0.059(5) 0.061(6) 0.047(5) 0.006(4) 0.028(4) 0.006(4) C40 0.109(8) 0.087(7) 0.056(6) -0.014(5) 0.043(6) 0.007(6) C41 0.063(5) 0.060(6) 0.032(4) 0.006(4) 0.023(4) 0.004(4) C42 0.062(5) 0.057(6) 0.051(5) 0.006(4) 0.027(4) 0.006(4) C43 0.061(6) 0.075(7) 0.054(5) 0.005(5) 0.024(5) 0.023(5) C44 0.046(5) 0.080(7) 0.043(5) -0.011(4) 0.021(4) 0.004(5) C45 0.059(5) 0.062(5) 0.050(5) 0.004(4) 0.031(4) 0.004(4) C46 0.057(5) 0.103(7) 0.083(7) 0.001(5) 0.037(5) 0.003(5) C47 0.103(8) 0.115(8) 0.081(6) -0.008(6) 0.028(5) -0.015(6) C48 0.087(13) 0.113(14) 0.168(12) -0.027(9) 0.062(11) -0.036(10) C49 0.138(12) 0.107(14) 0.126(10) 0.029(9) 0.072(11) -0.022(11) C48F 0.088(13) 0.124(19) 0.151(15) -0.061(14) 0.073(9) -0.025(12) C49F 0.149(18) 0.098(17) 0.137(14) 0.014(13) 0.089(13) -0.031(14) C50 0.133(8) 0.121(9) 0.076(6) 0.015(6) 0.035(6) -0.044(7) Ga2 0.0902(8) 0.0796(8) 0.0983(8) 0.0166(6) 0.0462(7) -0.0165(6) C51 0.122(10) 0.101(11) 0.132(10) 0.037(8) 0.074(7) 0.015(9) C52 0.17(2) 0.093(12) 0.159(15) 0.053(9) 0.084(14) 0.024(12) C53 0.124(6) 0.153(7) 0.165(7) -0.037(6) 0.079(6) -0.024(6) C54 0.124(6) 0.153(7) 0.165(7) -0.037(6) 0.079(6) -0.024(6) C51F 0.10(3) 0.10(2) 0.104(9) 0.049(14) 0.058(16) -0.02(2) C52F 0.15(4) 0.09(3) 0.15(3) 0.07(3) 0.04(3) -0.01(3) C53F 0.124(6) 0.153(7) 0.165(7) -0.037(6) 0.079(6) -0.024(6) C54F 0.124(6) 0.153(7) 0.165(7) -0.037(6) 0.079(6) -0.024(6) C55 0.124(6) 0.153(7) 0.165(7) -0.037(6) 0.079(6) -0.024(6) C56 0.124(6) 0.153(7) 0.165(7) -0.037(6) 0.079(6) -0.024(6) C55F 0.124(6) 0.153(7) 0.165(7) -0.037(6) 0.079(6) -0.024(6) C56F 0.124(6) 0.153(7) 0.165(7) -0.037(6) 0.079(6) -0.024(6) N1 0.048(4) 0.060(5) 0.049(4) -0.001(3) 0.024(3) -0.003(3) N2 0.049(4) 0.082(6) 0.051(4) -0.009(4) 0.028(4) -0.004(4) N3 0.044(4) 0.055(4) 0.046(4) -0.011(3) 0.021(3) -0.008(3) N4 0.051(4) 0.083(5) 0.033(4) 0.007(3) 0.021(3) 0.015(4) N5 0.068(4) 0.059(4) 0.042(4) 0.005(3) 0.031(3) 0.009(4) N6 0.049(4) 0.063(5) 0.045(4) 0.001(3) 0.028(3) 0.006(3) O1 0.117(5) 0.062(4) 0.078(4) -0.016(3) 0.049(4) -0.018(4) O2 0.086(4) 0.067(4) 0.052(3) 0.008(3) 0.027(3) -0.009(3) Ga1 0.0957(8) 0.0575(6) 0.0765(7) -0.0043(5) 0.0423(6) -0.0053(5) Sn1 0.0587(3) 0.0566(4) 0.0517(3) -0.0012(3) 0.0320(3) -0.0006(3) Sn2 0.0659(4) 0.0612(4) 0.0562(4) 0.0038(3) 0.0380(3) -0.0041(3) Li1 0.053(8) 0.072(9) 0.041(7) -0.007(6) 0.019(6) -0.005(7) Li2 0.082(10) 0.060(9) 0.032(7) 0.005(6) 0.026(7) 0.004(7) #----------------------------------------------------------------------------# # 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 C1 N1 1.348(8) . ? C1 C2 1.392(9) . ? C1 Sn1 2.193(7) . ? C2 C3 1.388(9) . ? C2 H2 0.95 . ? C3 C4 1.369(10) . ? C3 H3 0.95 . ? C4 C5 1.365(9) . ? C4 C6 1.511(9) . ? C5 N1 1.350(8) . ? C5 H5 0.95 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 N2 1.352(9) . ? C7 C8 1.396(10) . ? C7 Sn1 2.186(8) . ? C8 C9 1.383(11) . ? C8 H8 0.95 . ? C9 C10 1.353(12) . ? C9 H9 0.95 . ? C10 C11 1.383(11) . ? C10 C12 1.525(11) . ? C11 N2 1.343(9) . ? C11 H11 0.95 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 N3 1.355(8) . ? C13 C14 1.385(8) . ? C13 Sn1 2.199(7) . ? C14 C15 1.396(9) . ? C14 H14 0.95 . ? C15 C16 1.366(9) . ? C15 H15 0.95 . ? C16 C17 1.379(9) . ? C16 C18 1.515(9) . ? C17 N3 1.347(8) . ? C17 H17 0.95 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 O1 1.372(11) . ? C19 C20 1.500(12) . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? C20 C21 1.422(13) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? C21 C22 1.416(12) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 O1 1.428(9) . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? C23 C24 1.476(8) . ? C23 Ga1 1.988(8) . ? C23 H23A 0.99 . ? C23 H23B 0.99 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 C26F 1.493(10) . ? C25 C26 1.5036 . ? C25 Ga1 2.000(6) . ? C25 H25A 0.99 . ? C25 H25B 0.99 . ? C25 H25C 0.99 . ? C25 H25D 0.99 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C26 H25D 0.7157 . ? C26F H26D 0.98 . ? C26F H26E 0.98 . ? C26F H26F 0.98 . ? C27 C28 1.495(10) . ? C27 Ga1 2.022(10) . ? C27 H27A 0.99 . ? C27 H27B 0.99 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C27F C28F 1.478(9) . ? C27F Ga1 2.014(8) . ? C27F H27C 0.99 . ? C27F H27D 0.99 . ? C28F H28D 0.98 . ? C28F H28E 0.98 . ? C28F H28F 0.98 . ? C29 N4 1.366(9) . ? C29 C30 1.393(10) . ? C29 Sn2 2.181(8) . ? C30 C31 1.383(11) . ? C30 H30 0.95 . ? C31 C32 1.361(12) . ? C31 H31 0.95 . ? C32 C33 1.384(11) . ? C32 C34 1.518(11) . ? C33 N4 1.336(9) . ? C33 H33 0.95 . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 N5 1.347(8) . ? C35 C36 1.396(8) . ? C35 Sn2 2.198(8) . ? C36 C37 1.380(10) . ? C36 H36 0.95 . ? C37 C38 1.366(10) . ? C37 H37 0.95 . ? C38 C39 1.388(9) . ? C38 C40 1.499(10) . ? C39 N5 1.338(8) . ? C39 H39 0.95 . ? C40 H40A 0.98 . ? C40 H40B 0.98 . ? C40 H40C 0.98 . ? C41 N6 1.368(8) . ? C41 C42 1.376(9) . ? C41 Sn2 2.181(7) . ? C42 C43 1.388(9) . ? C42 H42 0.95 . ? C43 C44 1.385(10) . ? C43 H43 0.95 . ? C44 C45 1.375(9) . ? C44 C46 1.505(9) . ? C45 N6 1.350(8) . ? C45 H45 0.95 . ? C46 H46A 0.98 . ? C46 H46B 0.98 . ? C46 H46C 0.98 . ? C47 O2 1.424(10) . ? C47 C48F 1.484(15) . ? C47 C48 1.493(14) . ? C47 H47A 0.99 . ? C47 H47B 0.99 . ? C47 H47C 0.99 . ? C47 H47D 0.99 . ? C48 C49 1.57(2) . ? C48 H48A 0.99 . ? C48 H48B 0.99 . ? C49 C50 1.507(14) . ? C49 H49A 0.99 . ? C49 H49B 0.99 . ? C48F C49F 1.58(2) . ? C48F H48C 0.99 . ? C48F H48D 0.99 . ? C49F C50 1.509(15) . ? C49F H49C 0.99 . ? C49F H49D 0.99 . ? C50 O2 1.407(9) . ? C50 H50A 0.99 . ? C50 H50B 0.99 . ? C50 H50C 0.99 . ? C50 H50D 0.99 . ? Ga2 C53 1.930(14) . ? Ga2 C51 1.948(11) . ? Ga2 C55F 1.973(16) . ? Ga2 C51F 1.976(17) . ? Ga2 C53F 1.999(17) . ? Ga2 C55 2.053(15) . ? Ga2 Sn2 2.7111(11) . ? C51 C52 1.586(12) . ? C51 H51A 0.99 . ? C51 H51B 0.99 . ? C52 H52A 0.98 . ? C52 H52B 0.98 . ? C52 H52C 0.98 . ? C53 C54 1.656(15) . ? C53 H53A 0.99 . ? C53 H53B 0.99 . ? C54 H54A 0.98 . ? C54 H54B 0.98 . ? C54 H54C 0.98 . ? C51F C52F 1.634(17) . ? C51F H51C 0.99 . ? C51F H51D 0.99 . ? C52F H52D 0.98 . ? C52F H52E 0.98 . ? C52F H52F 0.98 . ? C53F C54F 1.625(17) . ? C53F H53C 0.99 . ? C53F H53D 0.99 . ? C54F H54D 0.98 . ? C54F H54E 0.98 . ? C54F H54F 0.98 . ? C55 C56 1.681(16) . ? C55 H55A 0.99 . ? C55 H55B 0.99 . ? C56 H56A 0.98 . ? C56 H56B 0.98 . ? C56 H56C 0.98 . ? C55F C56F 1.685(16) . ? C55F H55C 0.99 . ? C55F H55D 0.99 . ? C56F H56D 0.98 . ? C56F H56E 0.98 . ? C56F H56F 0.98 . ? N1 Li1 2.048(13) . ? N2 Li1 1.992(14) . ? N3 Li1 2.037(12) . ? N4 Li2 2.000(14) . ? N5 Li2 2.021(12) . ? N6 Li2 2.080(14) . ? O1 Li1 1.934(14) . ? O2 Li2 1.953(13) . ? Ga1 Sn1 2.7196(11) . ? Sn1 Li1 3.261(13) . ? Sn2 Li2 3.273(12) . ? 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 C1 C2 118.7(7) . . ? N1 C1 Sn1 119.4(5) . . ? C2 C1 Sn1 121.9(6) . . ? C3 C2 C1 121.2(7) . . ? C3 C2 H2 119.4 . . ? C1 C2 H2 119.4 . . ? C4 C3 C2 120.1(7) . . ? C4 C3 H3 120 . . ? C2 C3 H3 120 . . ? C5 C4 C3 115.6(7) . . ? C5 C4 C6 122.4(8) . . ? C3 C4 C6 122.0(7) . . ? N1 C5 C4 126.2(7) . . ? N1 C5 H5 116.9 . . ? C4 C5 H5 116.9 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 119.8(8) . . ? N2 C7 Sn1 117.5(6) . . ? C8 C7 Sn1 122.7(7) . . ? C9 C8 C7 120.2(9) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C10 C9 C8 120.2(9) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 117.2(9) . . ? C9 C10 C12 122.9(9) . . ? C11 C10 C12 119.9(10) . . ? N2 C11 C10 124.6(9) . . ? N2 C11 H11 117.7 . . ? C10 C11 H11 117.7 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C14 119.3(7) . . ? N3 C13 Sn1 119.6(5) . . ? C14 C13 Sn1 121.0(5) . . ? C13 C14 C15 121.1(7) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C16 C15 C14 119.2(7) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C15 C16 C17 117.1(7) . . ? C15 C16 C18 123.2(6) . . ? C17 C16 C18 119.7(7) . . ? N3 C17 C16 124.7(7) . . ? N3 C17 H17 117.6 . . ? C16 C17 H17 117.6 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O1 C19 C20 109.1(9) . . ? O1 C19 H19A 109.9 . . ? C20 C19 H19A 109.9 . . ? O1 C19 H19B 109.9 . . ? C20 C19 H19B 109.9 . . ? H19A C19 H19B 108.3 . . ? C21 C20 C19 103.6(9) . . ? C21 C20 H20A 111 . . ? C19 C20 H20A 111 . . ? C21 C20 H20B 111 . . ? C19 C20 H20B 111 . . ? H20A C20 H20B 109 . . ? C22 C21 C20 108.1(10) . . ? C22 C21 H21A 110.1 . . ? C20 C21 H21A 110.1 . . ? C22 C21 H21B 110.1 . . ? C20 C21 H21B 110.1 . . ? H21A C21 H21B 108.4 . . ? C21 C22 O1 108.8(9) . . ? C21 C22 H22A 109.9 . . ? O1 C22 H22A 109.9 . . ? C21 C22 H22B 109.9 . . ? O1 C22 H22B 109.9 . . ? H22A C22 H22B 108.3 . . ? C24 C23 Ga1 118.6(8) . . ? C24 C23 H23A 107.7 . . ? Ga1 C23 H23A 107.7 . . ? C24 C23 H23B 107.7 . . ? Ga1 C23 H23B 107.7 . . ? H23A C23 H23B 107.1 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26F C25 C26 77.7(17) . . ? C26F C25 Ga1 134.3(16) . . ? C26 C25 Ga1 110.8(3) . . ? C26F C25 H25A 34 . . ? C26 C25 H25A 109.5 . . ? Ga1 C25 H25A 109.5 . . ? C26F C25 H25B 109.2 . . ? C26 C25 H25B 109.5 . . ? Ga1 C25 H25B 109.5 . . ? H25A C25 H25B 108.1 . . ? C26F C25 H25C 102.9 . . ? C26 C25 H25C 122.9 . . ? Ga1 C25 H25C 107.8 . . ? H25A C25 H25C 94.8 . . ? H25B C25 H25C 15.5 . . ? C26F C25 H25D 97.8 . . ? C26 C25 H25D 23.6 . . ? Ga1 C25 H25D 104.6 . . ? H25A C25 H25D 131.4 . . ? H25B C25 H25D 91.5 . . ? H25C C25 H25D 106.6 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? C25 C26 H25D 33.6 . . ? H26A C26 H25D 114.8 . . ? H26B C26 H25D 76.8 . . ? H26C C26 H25D 129.9 . . ? C25 C26F H26D 109.5 . . ? C25 C26F H26E 109.5 . . ? H26D C26F H26E 109.5 . . ? C25 C26F H26F 109.5 . . ? H26D C26F H26F 109.5 . . ? H26E C26F H26F 109.5 . . ? C28 C27 Ga1 111(2) . . ? C28 C27 H27A 109.4 . . ? Ga1 C27 H27A 109.4 . . ? C28 C27 H27B 109.4 . . ? Ga1 C27 H27B 109.4 . . ? H27A C27 H27B 108 . . ? C28F C27F Ga1 109.7(8) . . ? C28F C27F H27C 109.7 . . ? Ga1 C27F H27C 109.7 . . ? C28F C27F H27D 109.7 . . ? Ga1 C27F H27D 109.7 . . ? H27C C27F H27D 108.2 . . ? N4 C29 C30 117.9(7) . . ? N4 C29 Sn2 118.8(6) . . ? C30 C29 Sn2 123.3(6) . . ? C31 C30 C29 121.7(9) . . ? C31 C30 H30 119.1 . . ? C29 C30 H30 119.1 . . ? C32 C31 C30 119.8(9) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C31 C32 C33 116.4(9) . . ? C31 C32 C34 121.4(9) . . ? C33 C32 C34 122.2(10) . . ? N4 C33 C32 125.0(9) . . ? N4 C33 H33 117.5 . . ? C32 C33 H33 117.5 . . ? 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 . . ? N5 C35 C36 119.5(7) . . ? N5 C35 Sn2 119.0(5) . . ? C36 C35 Sn2 121.5(6) . . ? C37 C36 C35 120.2(7) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C38 C37 C36 120.7(7) . . ? C38 C37 H37 119.6 . . ? C36 C37 H37 119.6 . . ? C37 C38 C39 115.8(7) . . ? C37 C38 C40 122.8(7) . . ? C39 C38 C40 121.4(8) . . ? N5 C39 C38 125.1(7) . . ? N5 C39 H39 117.5 . . ? C38 C39 H39 117.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N6 C41 C42 119.0(6) . . ? N6 C41 Sn2 117.4(5) . . ? C42 C41 Sn2 123.5(6) . . ? C41 C42 C43 122.1(7) . . ? C41 C42 H42 119 . . ? C43 C42 H42 119 . . ? C44 C43 C42 119.0(7) . . ? C44 C43 H43 120.5 . . ? C42 C43 H43 120.5 . . ? C45 C44 C43 116.6(7) . . ? C45 C44 C46 121.3(8) . . ? C43 C44 C46 122.2(7) . . ? N6 C45 C44 125.3(7) . . ? N6 C45 H45 117.4 . . ? C44 C45 H45 117.4 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O2 C47 C48F 107.2(12) . . ? O2 C47 C48 106.5(9) . . ? C48F C47 C48 27.4(17) . . ? O2 C47 H47A 110.4 . . ? C48F C47 H47A 85.2 . . ? C48 C47 H47A 110.4 . . ? O2 C47 H47B 110.4 . . ? C48F C47 H47B 131.3 . . ? C48 C47 H47B 110.4 . . ? H47A C47 H47B 108.6 . . ? O2 C47 H47C 110.7 . . ? C48F C47 H47C 104 . . ? C48 C47 H47C 126.9 . . ? H47A C47 H47C 20.2 . . ? H47B C47 H47C 90.5 . . ? O2 C47 H47D 110.6 . . ? C48F C47 H47D 115.6 . . ? C48 C47 H47D 91.7 . . ? H47A C47 H47D 124.4 . . ? H47B C47 H47D 20.2 . . ? H47C C47 H47D 108.4 . . ? C47 C48 C49 100.0(12) . . ? C47 C48 H48A 111.8 . . ? C49 C48 H48A 111.8 . . ? C47 C48 H48B 111.8 . . ? C49 C48 H48B 111.8 . . ? H48A C48 H48B 109.5 . . ? C50 C49 C48 97.7(13) . . ? C50 C49 H49A 112.2 . . ? C48 C49 H49A 112.2 . . ? C50 C49 H49B 112.2 . . ? C48 C49 H49B 112.2 . . ? H49A C49 H49B 109.8 . . ? C47 C48F C49F 94.6(16) . . ? C47 C48F H48C 112.8 . . ? C49F C48F H48C 112.8 . . ? C47 C48F H48D 112.8 . . ? C49F C48F H48D 112.8 . . ? H48C C48F H48D 110.3 . . ? C50 C49F C48F 101.6(16) . . ? C50 C49F H49C 111.5 . . ? C48F C49F H49C 111.5 . . ? C50 C49F H49D 111.5 . . ? C48F C49F H49D 111.5 . . ? H49C C49F H49D 109.3 . . ? O2 C50 C49 105.3(9) . . ? O2 C50 C49F 103.7(12) . . ? C49 C50 C49F 32.4(16) . . ? O2 C50 H50A 110.7 . . ? C49 C50 H50A 110.7 . . ? C49F C50 H50A 81.7 . . ? O2 C50 H50B 110.7 . . ? C49 C50 H50B 110.7 . . ? C49F C50 H50B 136.6 . . ? H50A C50 H50B 108.8 . . ? O2 C50 H50C 111.5 . . ? C49 C50 H50C 136.9 . . ? C49F C50 H50C 114.5 . . ? H50A C50 H50C 35 . . ? H50B C50 H50C 76.5 . . ? O2 C50 H50D 111 . . ? C49 C50 H50D 76 . . ? C49F C50 H50D 106.6 . . ? H50A C50 H50D 133.9 . . ? H50B C50 H50D 36.4 . . ? H50C C50 H50D 109.4 . . ? C53 Ga2 C51 121.4(8) . . ? C53 Ga2 C55F 64.0(7) . . ? C51 Ga2 C55F 139.5(9) . . ? C53 Ga2 C51F 143.5(11) . . ? C51 Ga2 C51F 39.3(12) . . ? C55F Ga2 C51F 109.6(14) . . ? C53 Ga2 C53F 44.2(9) . . ? C51 Ga2 C53F 80.9(9) . . ? C55F Ga2 C53F 106.2(10) . . ? C51F Ga2 C53F 116.9(16) . . ? C53 Ga2 C55 116.3(7) . . ? C51 Ga2 C55 102.9(9) . . ? C55F Ga2 C55 52.8(8) . . ? C51F Ga2 C55 63.8(16) . . ? C53F Ga2 C55 151.2(11) . . ? C53 Ga2 Sn2 108.1(6) . . ? C51 Ga2 Sn2 104.8(4) . . ? C55F Ga2 Sn2 111.1(8) . . ? C51F Ga2 Sn2 107.5(8) . . ? C53F Ga2 Sn2 105.5(9) . . ? C55 Ga2 Sn2 101.0(8) . . ? C52 C51 Ga2 114.3(9) . . ? C52 C51 H51A 108.7 . . ? Ga2 C51 H51A 108.7 . . ? C52 C51 H51B 108.7 . . ? Ga2 C51 H51B 108.7 . . ? H51A C51 H51B 107.6 . . ? C54 C53 Ga2 104.8(11) . . ? C54 C53 H53A 110.8 . . ? Ga2 C53 H53A 110.8 . . ? C54 C53 H53B 110.8 . . ? Ga2 C53 H53B 110.8 . . ? H53A C53 H53B 108.9 . . ? C52F C51F Ga2 107.5(18) . . ? C52F C51F H51C 110.2 . . ? Ga2 C51F H51C 110.2 . . ? C52F C51F H51D 110.2 . . ? Ga2 C51F H51D 110.2 . . ? H51C C51F H51D 108.5 . . ? C54F C53F Ga2 106.6(15) . . ? C54F C53F H53C 110.4 . . ? Ga2 C53F H53C 110.4 . . ? C54F C53F H53D 110.4 . . ? Ga2 C53F H53D 110.4 . . ? H53C C53F H53D 108.6 . . ? C56 C55 Ga2 102.5(12) . . ? C56 C55 H55A 111.3 . . ? Ga2 C55 H55A 111.3 . . ? C56 C55 H55B 111.3 . . ? Ga2 C55 H55B 111.3 . . ? H55A C55 H55B 109.2 . . ? C56F C55F Ga2 94.3(12) . . ? C56F C55F H55C 112.9 . . ? Ga2 C55F H55C 112.9 . . ? C56F C55F H55D 112.9 . . ? Ga2 C55F H55D 112.9 . . ? H55C C55F H55D 110.3 . . ? C1 N1 C5 118.2(6) . . ? C1 N1 Li1 114.1(6) . . ? C5 N1 Li1 127.6(6) . . ? C11 N2 C7 118.1(7) . . ? C11 N2 Li1 125.3(7) . . ? C7 N2 Li1 116.5(6) . . ? C17 N3 C13 118.5(6) . . ? C17 N3 Li1 127.9(6) . . ? C13 N3 Li1 113.6(6) . . ? C33 N4 C29 119.0(7) . . ? C33 N4 Li2 126.2(7) . . ? C29 N4 Li2 114.2(6) . . ? C39 N5 C35 118.7(6) . . ? C39 N5 Li2 126.0(6) . . ? C35 N5 Li2 115.0(6) . . ? C45 N6 C41 118.1(6) . . ? C45 N6 Li2 126.4(6) . . ? C41 N6 Li2 115.4(6) . . ? C19 O1 C22 107.4(7) . . ? C19 O1 Li1 129.3(7) . . ? C22 O1 Li1 120.8(6) . . ? C50 O2 C47 109.3(7) . . ? C50 O2 Li2 124.4(6) . . ? C47 O2 Li2 124.5(6) . . ? C23 Ga1 C25 114.1(5) . . ? C23 Ga1 C27F 109.3(7) . . ? C25 Ga1 C27F 115.7(5) . . ? C23 Ga1 C27 127.2(13) . . ? C25 Ga1 C27 92.2(11) . . ? C27F Ga1 C27 24.0(11) . . ? C23 Ga1 Sn1 107.4(3) . . ? C25 Ga1 Sn1 104.2(2) . . ? C27F Ga1 Sn1 105.4(4) . . ? C27 Ga1 Sn1 109.3(15) . . ? C7 Sn1 C1 96.0(3) . . ? C7 Sn1 C13 96.6(3) . . ? C1 Sn1 C13 97.6(3) . . ? C7 Sn1 Ga1 123.0(2) . . ? C1 Sn1 Ga1 120.4(2) . . ? C13 Sn1 Ga1 117.61(18) . . ? C7 Sn1 Li1 59.6(3) . . ? C1 Sn1 Li1 59.9(3) . . ? C13 Sn1 Li1 59.5(3) . . ? Ga1 Sn1 Li1 176.9(2) . . ? C41 Sn2 C29 96.6(3) . . ? C41 Sn2 C35 96.9(3) . . ? C29 Sn2 C35 97.6(3) . . ? C41 Sn2 Ga2 122.4(2) . . ? C29 Sn2 Ga2 120.4(2) . . ? C35 Sn2 Ga2 117.53(19) . . ? C41 Sn2 Li2 61.4(3) . . ? C29 Sn2 Li2 58.9(3) . . ? C35 Sn2 Li2 59.3(3) . . ? Ga2 Sn2 Li2 175.9(2) . . ? O1 Li1 N2 111.3(6) . . ? O1 Li1 N3 118.8(7) . . ? N2 Li1 N3 104.4(6) . . ? O1 Li1 N1 110.0(6) . . ? N2 Li1 N1 106.3(6) . . ? N3 Li1 N1 105.2(6) . . ? O1 Li1 Sn1 174.0(6) . . ? N2 Li1 Sn1 66.1(4) . . ? N3 Li1 Sn1 67.1(4) . . ? N1 Li1 Sn1 66.6(4) . . ? O2 Li2 N4 119.7(6) . . ? O2 Li2 N5 115.5(6) . . ? N4 Li2 N5 103.6(6) . . ? O2 Li2 N6 106.2(6) . . ? N4 Li2 N6 106.2(6) . . ? N5 Li2 N6 104.3(6) . . ? O2 Li2 Sn2 171.4(6) . . ? N4 Li2 Sn2 66.5(4) . . ? N5 Li2 Sn2 66.5(4) . . ? N6 Li2 Sn2 65.4(4) . . ? #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2012-05-16 at 12:58:47 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\software\wingx\files\archive.dat # CIF files read : x1273 x1273m data_x1273 #TrackingRef '- ccdc_887941-887946.cif' _database_code_depnum_ccdc_archive 'CCDC 887943' _audit_creation_date 2012-05-16T12:58:47-00:00 _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 'C28 H41 In Li N3 O Sn' _chemical_formula_sum 'C28 H41 In Li N3 O Sn' _chemical_formula_weight 676.09 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.6509(7) _cell_length_b 21.9927(5) _cell_length_c 17.3699(6) _cell_angle_alpha 90 _cell_angle_beta 116.967(4) _cell_angle_gamma 90 _cell_volume 6350.1(4) _cell_formula_units_Z 8 _cell_measurement_temperature 240(2) _cell_measurement_reflns_used 12291 _cell_measurement_theta_min 2.8655 _cell_measurement_theta_max 28.826 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.414 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2720 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.535 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.85312 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 240(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.356 _diffrn_orient_matrix_ub_11 -0.0354738 _diffrn_orient_matrix_ub_12 -0.0155122 _diffrn_orient_matrix_ub_13 -0.0059098 _diffrn_orient_matrix_ub_21 -0.0196552 _diffrn_orient_matrix_ub_22 0.028275 _diffrn_orient_matrix_ub_23 -0.0038758 _diffrn_orient_matrix_ub_31 -0.0132746 _diffrn_orient_matrix_ub_32 -0.0003832 _diffrn_orient_matrix_ub_33 -0.0452701 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_unetI/netI 0.0389 _diffrn_reflns_number 43930 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.87 _diffrn_reflns_theta_max 25.35 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 11615 _reflns_number_gt 7394 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0426P)^2^+9.2788P] 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 11615 _refine_ls_number_parameters 682 _refine_ls_number_restraints 194 _refine_ls_R_factor_all 0.0921 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1249 _refine_ls_wR_factor_gt 0.1059 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.714 _refine_diff_density_min -1.001 _refine_diff_density_rms 0.066 #----------------------------------------------------------------------------# # 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' 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' In In -0.7276 1.31 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 '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 C1 C 0.1250(3) 0.7527(3) 0.3349(3) 0.0629(14) Uani 1 1 d . . . C2 C 0.1264(4) 0.7363(3) 0.2583(4) 0.0769(17) Uani 1 1 d . . . H2 H 0.1272 0.695 0.2451 0.092 Uiso 1 1 calc R . . C3 C 0.1267(4) 0.7797(3) 0.2018(4) 0.0818(18) Uani 1 1 d . . . H3 H 0.1278 0.7679 0.1503 0.098 Uiso 1 1 calc R . . C4 C 0.1255(4) 0.8398(3) 0.2200(4) 0.0731(16) Uani 1 1 d . . . C5 C 0.1244(3) 0.8537(3) 0.2977(4) 0.0681(15) Uani 1 1 d . . . H5 H 0.1242 0.8949 0.3117 0.082 Uiso 1 1 calc R . . C6 C 0.1254(5) 0.8901(3) 0.1611(4) 0.101(2) Uani 1 1 d . . . H6A H 0.1732 0.8869 0.1525 0.151 Uiso 1 1 calc R . . H6B H 0.1251 0.9291 0.1869 0.151 Uiso 1 1 calc R . . H6C H 0.0779 0.8865 0.1058 0.151 Uiso 1 1 calc R . . C7 C 0.0204(3) 0.7218(3) 0.4418(3) 0.0664(15) Uani 1 1 d . . . C8 C -0.0424(4) 0.6853(3) 0.4381(4) 0.0793(17) Uani 1 1 d . . . H8 H -0.0432 0.6435 0.4261 0.095 Uiso 1 1 calc R . . C9 C -0.1036(4) 0.7105(3) 0.4520(4) 0.0839(19) Uani 1 1 d . . . H9 H -0.1455 0.6857 0.4499 0.101 Uiso 1 1 calc R . . C10 C -0.1034(4) 0.7715(3) 0.4689(4) 0.0744(17) Uani 1 1 d . . . C11 C -0.0395(4) 0.8045(3) 0.4707(4) 0.0709(16) Uani 1 1 d . . . H11 H -0.0382 0.8464 0.4819 0.085 Uiso 1 1 calc R . . C12 C -0.1694(4) 0.8011(3) 0.4834(4) 0.097(2) Uani 1 1 d . . . H12A H -0.1928 0.8343 0.4427 0.145 Uiso 1 1 calc R . . H12B H -0.1471 0.8169 0.5418 0.145 Uiso 1 1 calc R . . H12C H -0.2107 0.7714 0.4749 0.145 Uiso 1 1 calc R . . C13 C 0.2163(4) 0.7211(3) 0.5424(4) 0.0747(17) Uani 1 1 d . . . C14 C 0.2778(4) 0.6857(4) 0.6027(5) 0.092(2) Uani 1 1 d . . . H14 H 0.2785 0.6436 0.594 0.11 Uiso 1 1 calc R . . C15 C 0.3383(5) 0.7124(5) 0.6760(5) 0.108(3) Uani 1 1 d . . . H15 H 0.3792 0.6881 0.7173 0.13 Uiso 1 1 calc R . . C16 C 0.3383(4) 0.7731(5) 0.6881(5) 0.100(2) Uani 1 1 d . . . C17 C 0.4042(5) 0.8051(5) 0.7654(5) 0.148(4) Uani 1 1 d . . . H17A H 0.4221 0.7791 0.8158 0.222 Uiso 1 1 calc R . . H17B H 0.3834 0.8429 0.7762 0.222 Uiso 1 1 calc R . . H17C H 0.4491 0.8138 0.7535 0.222 Uiso 1 1 calc R . . C18 C 0.2750(4) 0.8057(4) 0.6263(4) 0.090(2) Uani 1 1 d . . . H18 H 0.2737 0.8479 0.6346 0.109 Uiso 1 1 calc R . . C19 C 0.0078(7) 0.5449(5) 0.2553(8) 0.199(5) Uani 1 1 d DU A . H19A H 0.0183 0.5156 0.2191 0.239 Uiso 1 1 calc R . . H19B H -0.0318 0.5265 0.2708 0.239 Uiso 1 1 calc R . . C20 C -0.0274(7) 0.5986(6) 0.2047(7) 0.197(5) Uani 1 1 d DU . . H20A H -0.0451 0.6258 0.2367 0.296 Uiso 1 1 calc R . . H20B H -0.073 0.5872 0.1508 0.296 Uiso 1 1 calc R . . H20C H 0.0124 0.6191 0.1925 0.296 Uiso 1 1 calc R . . In1 In 0.11985(4) 0.55901(2) 0.37421(4) 0.1058(2) Uani 1 1 d DU . . C21 C 0.1060(13) 0.5055(7) 0.4713(13) 0.158(2) Uani 0.579(10) 1 d PDU A 1 H21A H 0.1369 0.5243 0.5281 0.19 Uiso 0.579(10) 1 calc PR A 1 H21B H 0.0493 0.505 0.4588 0.19 Uiso 0.579(10) 1 calc PR A 1 C22 C 0.1338(12) 0.4433(6) 0.4733(13) 0.158(2) Uani 0.579(10) 1 d PDU A 1 H22A H 0.088 0.4171 0.4412 0.237 Uiso 0.579(10) 1 calc PR A 1 H22B H 0.1618 0.4295 0.5326 0.237 Uiso 0.579(10) 1 calc PR A 1 H22C H 0.1701 0.442 0.4472 0.237 Uiso 0.579(10) 1 calc PR A 1 C21F C 0.1646(13) 0.4992(11) 0.4960(14) 0.158(2) Uani 0.421(10) 1 d PDU A 2 H21C H 0.1987 0.4661 0.4936 0.19 Uiso 0.421(10) 1 calc PR A 2 H21D H 0.1952 0.5233 0.5482 0.19 Uiso 0.421(10) 1 calc PR A 2 C22F C 0.0921(14) 0.4760(11) 0.4943(19) 0.158(2) Uani 0.421(10) 1 d PDU A 2 H22D H 0.0567 0.5096 0.4899 0.237 Uiso 0.421(10) 1 calc PR A 2 H22E H 0.1051 0.4535 0.547 0.237 Uiso 0.421(10) 1 calc PR A 2 H22F H 0.0655 0.4493 0.445 0.237 Uiso 0.421(10) 1 calc PR A 2 C23 C 0.2282(14) 0.5414(10) 0.3673(19) 0.158(2) Uani 0.499(11) 1 d PDU A 3 H23A H 0.2702 0.5321 0.4255 0.19 Uiso 0.499(11) 1 calc PR A 3 H23B H 0.2206 0.5052 0.3316 0.19 Uiso 0.499(11) 1 calc PR A 3 C24 C 0.2562(13) 0.5910(8) 0.3320(15) 0.158(2) Uani 0.499(11) 1 d PDU A 3 H24A H 0.2201 0.5955 0.271 0.237 Uiso 0.499(11) 1 calc PR A 3 H24B H 0.3099 0.5819 0.3397 0.237 Uiso 0.499(11) 1 calc PR A 3 H24C H 0.2572 0.6284 0.362 0.237 Uiso 0.499(11) 1 calc PR A 3 C23F C 0.2274(13) 0.5581(11) 0.3455(17) 0.158(2) Uani 0.501(11) 1 d PDU A 4 H23C H 0.2292 0.5198 0.3177 0.19 Uiso 0.501(11) 1 calc PR A 4 H23D H 0.2234 0.5917 0.3066 0.19 Uiso 0.501(11) 1 calc PR A 4 C24F C 0.2985(12) 0.5647(9) 0.4261(15) 0.158(2) Uani 0.501(11) 1 d PDU A 4 H24D H 0.3073 0.6074 0.4415 0.237 Uiso 0.501(11) 1 calc PR A 4 H24E H 0.3444 0.5486 0.4207 0.237 Uiso 0.501(11) 1 calc PR A 4 H24F H 0.2918 0.5426 0.4708 0.237 Uiso 0.501(11) 1 calc PR A 4 O1 O 0.1173(12) 0.9111(6) 0.5046(11) 0.111(6) Uani 0.679(17) 1 d PD A 5 C25 C 0.1273(16) 0.9668(6) 0.4683(10) 0.155(7) Uani 0.679(17) 1 d PDU A 5 H25A H 0.0817 0.9727 0.4111 0.187 Uiso 0.679(17) 1 calc PR A 5 H25B H 0.1765 0.9649 0.4612 0.187 Uiso 0.679(17) 1 calc PR A 5 C26 C 0.1321(15) 1.0171(7) 0.5234(11) 0.155(6) Uani 0.679(17) 1 d PDU A 5 H26A H 0.0823 1.041 0.4988 0.186 Uiso 0.679(17) 1 calc PR A 5 H26B H 0.1775 1.0438 0.533 0.186 Uiso 0.679(17) 1 calc PR A 5 C27 C 0.1451(16) 0.9843(8) 0.6105(12) 0.168(7) Uani 0.679(17) 1 d PDU A 5 H27A H 0.2019 0.9852 0.6532 0.201 Uiso 0.679(17) 1 calc PR A 5 H27B H 0.113 1.0039 0.6352 0.201 Uiso 0.679(17) 1 calc PR A 5 C28 C 0.1190(11) 0.9240(7) 0.5851(10) 0.119(5) Uani 0.679(17) 1 d PDU A 5 H28A H 0.0651 0.9186 0.5806 0.142 Uiso 0.679(17) 1 calc PR A 5 H28B H 0.1555 0.8957 0.6289 0.142 Uiso 0.679(17) 1 calc PR A 5 O1F O 0.128(2) 0.9127(12) 0.496(2) 0.084(10) Uiso 0.321(17) 1 d PD A 6 C25F C 0.195(2) 0.9481(13) 0.504(2) 0.127(9) Uani 0.321(17) 1 d PDU A 6 H25C H 0.1875 0.9615 0.4474 0.152 Uiso 0.321(17) 1 calc PR A 6 H25D H 0.2442 0.9236 0.5308 0.152 Uiso 0.321(17) 1 calc PR A 6 C26F C 0.203(2) 1.0003(15) 0.558(3) 0.155(10) Uani 0.321(17) 1 d PDU A 6 H26C H 0.2063 1.0378 0.5293 0.186 Uiso 0.321(17) 1 calc PR A 6 H26D H 0.2506 0.9969 0.6135 0.186 Uiso 0.321(17) 1 calc PR A 6 C27F C 0.123(3) 1.0005(16) 0.571(3) 0.150(10) Uani 0.321(17) 1 d PDU A 6 H27C H 0.1362 1.0071 0.6314 0.18 Uiso 0.321(17) 1 calc PR A 6 H27D H 0.0853 1.0317 0.5351 0.18 Uiso 0.321(17) 1 calc PR A 6 C28F C 0.093(2) 0.9411(17) 0.543(3) 0.166(13) Uani 0.321(17) 1 d PDU A 6 H28C H 0.1028 0.9162 0.5937 0.199 Uiso 0.321(17) 1 calc PR A 6 H28D H 0.0344 0.9435 0.5072 0.199 Uiso 0.321(17) 1 calc PR A 6 C29 C 0.6114(3) 0.7326(3) 0.8428(3) 0.0657(15) Uani 1 1 d . . . C30 C 0.5993(4) 0.7242(3) 0.9151(4) 0.0792(18) Uani 1 1 d . . . H30 H 0.5839 0.6858 0.9261 0.095 Uiso 1 1 calc R . . C31 C 0.6095(4) 0.7714(4) 0.9709(4) 0.086(2) Uani 1 1 d . . . H31 H 0.601 0.7651 1.0197 0.103 Uiso 1 1 calc R . . C32 C 0.6320(4) 0.8276(3) 0.9559(4) 0.0832(19) Uani 1 1 d . . . C33 C 0.6435(4) 0.8319(3) 0.8823(4) 0.0803(18) Uani 1 1 d . . . H33 H 0.6592 0.87 0.8705 0.096 Uiso 1 1 calc R . . C34 C 0.6445(5) 0.8810(4) 1.0150(5) 0.120(3) Uani 1 1 d . . . H34A H 0.6046 0.88 1.0364 0.181 Uiso 1 1 calc R . . H34B H 0.6388 0.9185 0.9833 0.181 Uiso 1 1 calc R . . H34C H 0.6979 0.879 1.0632 0.181 Uiso 1 1 calc R . . C35 C 0.5151(4) 0.7090(3) 0.6318(4) 0.0752(16) Uani 1 1 d U . . C36 C 0.4480(4) 0.6826(4) 0.5658(4) 0.100(2) Uani 1 1 d U . . H36 H 0.4371 0.6412 0.5689 0.119 Uiso 1 1 calc R . . C37 C 0.3973(5) 0.7166(5) 0.4959(5) 0.115(3) Uani 1 1 d U . . H37 H 0.3529 0.6978 0.4507 0.138 Uiso 1 1 calc R . . C38 C 0.4099(5) 0.7764(5) 0.4909(5) 0.106(2) Uani 1 1 d U . . C39 C 0.4791(4) 0.7999(4) 0.5574(4) 0.0914(19) Uani 1 1 d U . . H39 H 0.4904 0.8412 0.5541 0.11 Uiso 1 1 calc R . . C40 C 0.3522(5) 0.8160(5) 0.4180(5) 0.160(4) Uani 1 1 d . . . H40A H 0.3184 0.7906 0.3693 0.24 Uiso 1 1 calc R . . H40B H 0.3824 0.844 0.4006 0.24 Uiso 1 1 calc R . . H40C H 0.3188 0.8388 0.4372 0.24 Uiso 1 1 calc R . . C41 C 0.7041(3) 0.6695(3) 0.7413(3) 0.0637(14) Uani 1 1 d . . . C42 C 0.7562(4) 0.6220(3) 0.7519(4) 0.0827(18) Uani 1 1 d . . . H42 H 0.7451 0.5833 0.7666 0.099 Uiso 1 1 calc R . . C43 C 0.8242(4) 0.6308(4) 0.7412(4) 0.088(2) Uani 1 1 d . . . H43 H 0.8592 0.5981 0.7486 0.106 Uiso 1 1 calc R . . C44 C 0.8410(4) 0.6870(4) 0.7198(4) 0.0791(18) Uani 1 1 d . . . C45 C 0.7869(4) 0.7325(3) 0.7108(4) 0.0729(16) Uani 1 1 d . . . H45 H 0.7973 0.7715 0.6961 0.088 Uiso 1 1 calc R . . C46 C 0.9137(4) 0.6993(4) 0.7048(5) 0.119(3) Uani 1 1 d . . . H46A H 0.962 0.6857 0.7546 0.178 Uiso 1 1 calc R . . H46B H 0.9176 0.7426 0.6965 0.178 Uiso 1 1 calc R . . H46C H 0.9081 0.6775 0.6539 0.178 Uiso 1 1 calc R . . C47 C 0.4694(17) 0.5037(12) 0.6606(13) 0.197(4) Uani 0.446(12) 1 d PDU B 7 H47A H 0.4335 0.4728 0.6651 0.237 Uiso 0.446(12) 1 calc PR B 7 H47B H 0.4363 0.5344 0.6186 0.237 Uiso 0.446(12) 1 calc PR B 7 C48 C 0.529(2) 0.4735(13) 0.630(2) 0.197(4) Uani 0.446(12) 1 d PDU B 7 H48A H 0.5176 0.489 0.5739 0.296 Uiso 0.446(12) 1 calc PR B 7 H48B H 0.521 0.4298 0.6274 0.296 Uiso 0.446(12) 1 calc PR B 7 H48C H 0.5835 0.4831 0.6714 0.296 Uiso 0.446(12) 1 calc PR B 7 C47F C 0.5750(15) 0.4760(8) 0.7110(13) 0.197(4) Uani 0.554(12) 1 d PDU B 8 H47C H 0.6336 0.4711 0.7385 0.237 Uiso 0.554(12) 1 calc PR B 8 H47D H 0.5503 0.4364 0.7094 0.237 Uiso 0.554(12) 1 calc PR B 8 C48F C 0.5434(17) 0.5029(11) 0.6168(13) 0.197(4) Uani 0.554(12) 1 d PDU B 8 H48D H 0.4906 0.5207 0.5987 0.296 Uiso 0.554(12) 1 calc PR B 8 H48E H 0.5398 0.4707 0.5771 0.296 Uiso 0.554(12) 1 calc PR B 8 H48F H 0.5803 0.534 0.6167 0.296 Uiso 0.554(12) 1 calc PR B 8 C49 C 0.6375(12) 0.5011(9) 0.8749(13) 0.197(4) Uani 0.586(10) 1 d PDU B 9 H49A H 0.6691 0.4859 0.8467 0.237 Uiso 0.586(10) 1 calc PR B 9 H49B H 0.6706 0.5315 0.9174 0.237 Uiso 0.586(10) 1 calc PR B 9 C50 C 0.6244(15) 0.4492(8) 0.9230(13) 0.197(4) Uani 0.586(10) 1 d PDU B 9 H50A H 0.6027 0.4645 0.9605 0.296 Uiso 0.586(10) 1 calc PR B 9 H50B H 0.6753 0.429 0.9575 0.296 Uiso 0.586(10) 1 calc PR B 9 H50C H 0.5869 0.4205 0.8822 0.296 Uiso 0.586(10) 1 calc PR B 9 C49F C 0.587(2) 0.5325(12) 0.9162(13) 0.197(4) Uani 0.414(10) 1 d PDU B 10 H49C H 0.6459 0.5342 0.9408 0.237 Uiso 0.414(10) 1 calc PR B 10 H49D H 0.5701 0.5665 0.9406 0.237 Uiso 0.414(10) 1 calc PR B 10 C50F C 0.564(2) 0.4743(12) 0.9440(17) 0.197(4) Uani 0.414(10) 1 d PDU B 10 H50D H 0.514 0.4797 0.9467 0.296 Uiso 0.414(10) 1 calc PR B 10 H50E H 0.6061 0.4628 1.0005 0.296 Uiso 0.414(10) 1 calc PR B 10 H50F H 0.5583 0.4425 0.9027 0.296 Uiso 0.414(10) 1 calc PR B 10 C51 C 0.4669(12) 0.5723(10) 0.8573(15) 0.219(7) Uani 0.588(9) 1 d PDU B 11 H51A H 0.4857 0.5494 0.9113 0.262 Uiso 0.588(9) 1 calc PR B 11 H51B H 0.4728 0.6159 0.8706 0.262 Uiso 0.588(9) 1 calc PR B 11 C52 C 0.3803(12) 0.5567(10) 0.7966(17) 0.219(7) Uani 0.588(9) 1 d PDU B 11 H52A H 0.3744 0.5512 0.7386 0.328 Uiso 0.588(9) 1 calc PR B 11 H52B H 0.3455 0.5894 0.7967 0.328 Uiso 0.588(9) 1 calc PR B 11 H52C H 0.3655 0.5193 0.8156 0.328 Uiso 0.588(9) 1 calc PR B 11 C51F C 0.4084(11) 0.5494(16) 0.735(3) 0.219(7) Uani 0.412(9) 1 d PDU B 12 H51C H 0.3933 0.5296 0.7765 0.262 Uiso 0.412(9) 1 calc PR B 12 H51D H 0.391 0.592 0.7293 0.262 Uiso 0.412(9) 1 calc PR B 12 C52F C 0.371(2) 0.5197(14) 0.654(2) 0.219(7) Uani 0.412(9) 1 d PDU B 12 H52D H 0.3902 0.5366 0.6157 0.328 Uiso 0.412(9) 1 calc PR B 12 H52E H 0.3128 0.5255 0.6292 0.328 Uiso 0.412(9) 1 calc PR B 12 H52F H 0.3827 0.4765 0.6618 0.328 Uiso 0.412(9) 1 calc PR B 12 C53 C 0.7502(7) 0.9015(5) 0.7626(7) 0.167(4) Uani 1 1 d U . . H53A H 0.7932 0.873 0.7971 0.2 Uiso 1 1 calc R . . H53B H 0.7321 0.9219 0.8009 0.2 Uiso 1 1 calc R . . C54 C 0.7792(10) 0.9452(7) 0.7232(11) 0.233(6) Uani 1 1 d U . . H54A H 0.7684 0.9864 0.7367 0.28 Uiso 1 1 calc R . . H54B H 0.8374 0.9406 0.7446 0.28 Uiso 1 1 calc R . . C55 C 0.7403(10) 0.9355(8) 0.6361(10) 0.239(7) Uani 1 1 d U . . H55A H 0.7772 0.9172 0.6166 0.287 Uiso 1 1 calc R . . H55B H 0.7208 0.9742 0.6057 0.287 Uiso 1 1 calc R . . C56 C 0.6724(7) 0.8945(5) 0.6176(7) 0.175(4) Uani 1 1 d U . . H56A H 0.6215 0.9169 0.5915 0.211 Uiso 1 1 calc R . . H56B H 0.6705 0.8622 0.5779 0.211 Uiso 1 1 calc R . . N1 N 0.1238(3) 0.8122(2) 0.3536(3) 0.0620(11) Uani 1 1 d . A . N2 N 0.0205(3) 0.7817(2) 0.4578(3) 0.0664(12) Uani 1 1 d . A . N3 N 0.2158(3) 0.7816(3) 0.5559(3) 0.0756(14) Uani 1 1 d . A . N4 N 0.6344(3) 0.7874(2) 0.8274(3) 0.0708(13) Uani 1 1 d . B . N5 N 0.5310(3) 0.7685(3) 0.6259(3) 0.0755(14) Uani 1 1 d . B . N6 N 0.7206(3) 0.7251(2) 0.7213(3) 0.0660(12) Uani 1 1 d . B . O2 O 0.6856(3) 0.8700(2) 0.6972(3) 0.0980(14) Uani 1 1 d . B . In2 In 0.53818(4) 0.54486(3) 0.78262(4) 0.1158(2) Uani 1 1 d D . . Sn1 Sn 0.12053(3) 0.683305(19) 0.42368(3) 0.07161(14) Uani 1 1 d . A . Sn2 Sn 0.59159(3) 0.65895(2) 0.75019(3) 0.07548(15) Uani 1 1 d . B . Li1 Li 0.1201(6) 0.8275(5) 0.4674(6) 0.073(3) Uani 1 1 d . . . Li2 Li 0.6443(6) 0.7935(5) 0.7165(6) 0.071(3) 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 C1 0.065(4) 0.076(4) 0.052(3) -0.001(3) 0.030(3) -0.005(3) C2 0.092(5) 0.083(4) 0.070(4) -0.008(3) 0.049(4) -0.005(3) C3 0.099(5) 0.100(5) 0.063(4) -0.009(4) 0.051(4) -0.008(4) C4 0.072(4) 0.089(5) 0.064(4) 0.003(3) 0.036(3) -0.003(3) C5 0.073(4) 0.072(4) 0.063(4) -0.005(3) 0.035(3) -0.005(3) C6 0.133(6) 0.103(5) 0.082(5) 0.015(4) 0.063(5) 0.003(5) C7 0.067(4) 0.088(4) 0.046(3) 0.004(3) 0.027(3) -0.005(3) C8 0.083(5) 0.083(4) 0.081(4) -0.009(3) 0.045(4) -0.020(4) C9 0.069(4) 0.110(6) 0.081(4) -0.002(4) 0.042(4) -0.020(4) C10 0.063(4) 0.108(5) 0.052(3) 0.001(3) 0.026(3) 0.000(4) C11 0.072(4) 0.076(4) 0.066(4) -0.003(3) 0.033(3) -0.001(3) C12 0.073(5) 0.135(6) 0.090(5) 0.006(4) 0.044(4) 0.010(4) C13 0.069(4) 0.100(5) 0.067(4) 0.006(4) 0.041(3) 0.010(4) C14 0.082(5) 0.125(6) 0.080(5) 0.013(4) 0.048(4) 0.024(4) C15 0.075(5) 0.170(9) 0.073(5) 0.018(6) 0.028(4) 0.035(5) C16 0.068(5) 0.159(8) 0.072(5) -0.006(5) 0.030(4) 0.004(5) C17 0.084(6) 0.233(11) 0.089(6) -0.019(6) 0.006(5) -0.011(6) C18 0.070(4) 0.120(6) 0.074(4) -0.011(4) 0.026(4) -0.008(4) C19 0.179(7) 0.175(11) 0.194(8) -0.042(8) 0.042(7) -0.014(9) C20 0.162(10) 0.231(13) 0.139(9) -0.001(8) 0.017(7) -0.045(9) In1 0.1358(5) 0.0818(4) 0.1065(4) -0.0049(3) 0.0608(4) -0.0074(3) C21 0.187(5) 0.110(5) 0.226(7) 0.033(5) 0.136(5) 0.010(5) C22 0.187(5) 0.110(5) 0.226(7) 0.033(5) 0.136(5) 0.010(5) C21F 0.187(5) 0.110(5) 0.226(7) 0.033(5) 0.136(5) 0.010(5) C22F 0.187(5) 0.110(5) 0.226(7) 0.033(5) 0.136(5) 0.010(5) C23 0.187(5) 0.110(5) 0.226(7) 0.033(5) 0.136(5) 0.010(5) C24 0.187(5) 0.110(5) 0.226(7) 0.033(5) 0.136(5) 0.010(5) C23F 0.187(5) 0.110(5) 0.226(7) 0.033(5) 0.136(5) 0.010(5) C24F 0.187(5) 0.110(5) 0.226(7) 0.033(5) 0.136(5) 0.010(5) O1 0.181(14) 0.080(7) 0.092(8) -0.029(5) 0.080(8) -0.034(6) C25 0.25(2) 0.083(9) 0.118(10) 0.016(7) 0.072(12) 0.013(11) C26 0.201(16) 0.091(9) 0.174(14) -0.010(7) 0.087(13) 0.007(9) C27 0.231(17) 0.131(11) 0.133(12) -0.054(9) 0.076(13) -0.042(11) C28 0.161(13) 0.107(9) 0.101(10) -0.030(7) 0.071(10) -0.005(8) C25F 0.20(2) 0.085(16) 0.122(19) -0.011(13) 0.095(17) -0.034(16) C26F 0.20(2) 0.103(16) 0.15(2) -0.041(14) 0.071(18) -0.040(16) C27F 0.207(19) 0.104(16) 0.13(2) -0.051(17) 0.069(18) -0.006(15) C28F 0.19(2) 0.116(18) 0.16(2) -0.019(19) 0.05(2) -0.047(17) C29 0.065(4) 0.082(4) 0.054(3) 0.006(3) 0.030(3) 0.003(3) C30 0.085(5) 0.101(5) 0.061(4) 0.020(4) 0.041(3) 0.009(4) C31 0.089(5) 0.124(6) 0.054(4) 0.017(4) 0.041(4) 0.022(4) C32 0.093(5) 0.107(5) 0.052(4) 0.007(4) 0.035(3) 0.024(4) C33 0.091(5) 0.093(5) 0.062(4) 0.014(4) 0.039(4) 0.008(4) C34 0.170(8) 0.127(7) 0.075(5) -0.010(5) 0.066(5) 0.021(6) C35 0.067(4) 0.107(5) 0.066(4) 0.003(4) 0.042(3) 0.003(3) C36 0.081(5) 0.148(6) 0.073(4) -0.001(4) 0.038(4) -0.028(4) C37 0.073(5) 0.195(8) 0.070(4) -0.006(5) 0.026(4) -0.015(5) C38 0.083(5) 0.170(7) 0.063(4) 0.010(5) 0.033(4) 0.029(5) C39 0.086(5) 0.122(5) 0.074(4) 0.009(4) 0.042(4) 0.032(4) C40 0.114(7) 0.240(12) 0.089(6) 0.032(7) 0.015(5) 0.062(7) C41 0.073(4) 0.074(4) 0.043(3) 0.001(3) 0.026(3) 0.007(3) C42 0.091(5) 0.085(5) 0.072(4) 0.012(3) 0.037(4) 0.014(4) C43 0.078(5) 0.108(6) 0.069(4) 0.006(4) 0.025(4) 0.032(4) C44 0.062(4) 0.119(6) 0.052(3) -0.003(4) 0.021(3) 0.008(4) C45 0.066(4) 0.088(4) 0.064(4) -0.002(3) 0.030(3) 0.000(3) C46 0.072(5) 0.177(8) 0.114(6) 0.001(6) 0.049(5) 0.013(5) C47 0.274(12) 0.156(8) 0.188(9) 0.009(7) 0.127(8) -0.038(8) C48 0.274(12) 0.156(8) 0.188(9) 0.009(7) 0.127(8) -0.038(8) C47F 0.274(12) 0.156(8) 0.188(9) 0.009(7) 0.127(8) -0.038(8) C48F 0.274(12) 0.156(8) 0.188(9) 0.009(7) 0.127(8) -0.038(8) C49 0.274(12) 0.156(8) 0.188(9) 0.009(7) 0.127(8) -0.038(8) C50 0.274(12) 0.156(8) 0.188(9) 0.009(7) 0.127(8) -0.038(8) C49F 0.274(12) 0.156(8) 0.188(9) 0.009(7) 0.127(8) -0.038(8) C50F 0.274(12) 0.156(8) 0.188(9) 0.009(7) 0.127(8) -0.038(8) C51 0.198(14) 0.171(11) 0.35(2) -0.019(12) 0.179(16) -0.009(11) C52 0.198(14) 0.171(11) 0.35(2) -0.019(12) 0.179(16) -0.009(11) C51F 0.198(14) 0.171(11) 0.35(2) -0.019(12) 0.179(16) -0.009(11) C52F 0.198(14) 0.171(11) 0.35(2) -0.019(12) 0.179(16) -0.009(11) C53 0.212(12) 0.141(9) 0.145(8) -0.031(7) 0.078(8) -0.058(8) C54 0.235(14) 0.241(14) 0.262(13) -0.044(12) 0.147(12) -0.115(11) C55 0.240(14) 0.259(15) 0.228(11) 0.099(12) 0.114(12) -0.067(10) C56 0.214(11) 0.169(10) 0.140(8) 0.058(7) 0.078(8) -0.036(8) N1 0.060(3) 0.069(3) 0.057(3) -0.003(2) 0.026(2) -0.005(2) N2 0.070(3) 0.073(3) 0.061(3) -0.004(2) 0.034(2) -0.004(2) N3 0.059(3) 0.108(4) 0.058(3) -0.001(3) 0.025(3) -0.005(3) N4 0.090(4) 0.077(3) 0.057(3) 0.003(3) 0.044(3) 0.012(3) N5 0.066(3) 0.108(4) 0.056(3) 0.008(3) 0.031(3) 0.019(3) N6 0.066(3) 0.078(3) 0.060(3) 0.003(2) 0.034(2) 0.001(2) O2 0.124(4) 0.084(3) 0.092(3) 0.014(3) 0.055(3) -0.012(3) In2 0.1211(5) 0.1071(4) 0.1170(5) 0.0189(3) 0.0520(4) -0.0265(3) Sn1 0.0810(3) 0.0758(3) 0.0676(3) 0.0009(2) 0.0421(2) 0.0004(2) Sn2 0.0830(3) 0.0845(3) 0.0697(3) 0.0051(2) 0.0441(2) -0.0070(2) Li1 0.072(6) 0.092(7) 0.059(6) -0.007(5) 0.034(5) -0.018(5) Li2 0.082(7) 0.086(7) 0.055(5) 0.013(5) 0.039(5) 0.009(5) #----------------------------------------------------------------------------# # 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 C1 N1 1.350(7) . ? C1 C2 1.391(7) . ? C1 Sn1 2.199(5) . ? C2 C3 1.370(8) . ? C2 H2 0.94 . ? C3 C4 1.363(8) . ? C3 H3 0.94 . ? C4 C5 1.392(8) . ? C4 C6 1.506(8) . ? C5 N1 1.338(7) . ? C5 H5 0.94 . ? C6 H6A 0.97 . ? C6 H6B 0.97 . ? C6 H6C 0.97 . ? C7 N2 1.347(7) . ? C7 C8 1.397(8) . ? C7 Sn1 2.199(6) . ? C8 C9 1.385(8) . ? C8 H8 0.94 . ? C9 C10 1.373(9) . ? C9 H9 0.94 . ? C10 C11 1.385(8) . ? C10 C12 1.511(8) . ? C11 N2 1.334(7) . ? C11 H11 0.94 . ? C12 H12A 0.97 . ? C12 H12B 0.97 . ? C12 H12C 0.97 . ? C13 N3 1.352(8) . ? C13 C14 1.390(9) . ? C13 Sn1 2.189(7) . ? C14 C15 1.391(10) . ? C14 H14 0.94 . ? C15 C16 1.351(11) . ? C15 H15 0.94 . ? C16 C18 1.383(10) . ? C16 C17 1.521(10) . ? C17 H17A 0.97 . ? C17 H17B 0.97 . ? C17 H17C 0.97 . ? C18 N3 1.331(8) . ? C18 H18 0.94 . ? C19 C20 1.442(12) . ? C19 In1 2.194(10) . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C20 H20A 0.97 . ? C20 H20B 0.97 . ? C20 H20C 0.97 . ? In1 C23 2.114(17) . ? In1 C21 2.166(12) . ? In1 C23F 2.276(17) . ? In1 C21F 2.301(14) . ? In1 Sn1 2.8638(7) . ? C21 C22 1.457(14) . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C22 H22A 0.97 . ? C22 H22B 0.97 . ? C22 H22C 0.97 . ? C21F C22F 1.434(16) . ? C21F H21C 0.98 . ? C21F H21D 0.98 . ? C22F H22D 0.97 . ? C22F H22E 0.97 . ? C22F H22F 0.97 . ? C23 C24 1.458(19) . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C24 H24A 0.97 . ? C24 H24B 0.97 . ? C24 H24C 0.97 . ? C23F C24F 1.43(2) . ? C23F H23C 0.98 . ? C23F H23D 0.98 . ? C24F H24D 0.97 . ? C24F H24E 0.97 . ? C24F H24F 0.97 . ? O1 C28 1.413(15) . ? O1 C25 1.429(16) . ? O1 Li1 1.957(16) . ? C25 C26 1.440(16) . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C26 C27 1.59(2) . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C27 C28 1.412(15) . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? O1F C28F 1.41(2) . ? O1F C25F 1.43(2) . ? O1F Li1 1.93(3) . ? C25F C26F 1.44(2) . ? C25F H25C 0.98 . ? C25F H25D 0.98 . ? C26F C27F 1.59(2) . ? C26F H26C 0.98 . ? C26F H26D 0.98 . ? C27F C28F 1.42(2) . ? C27F H27C 0.98 . ? C27F H27D 0.98 . ? C28F H28C 0.98 . ? C28F H28D 0.98 . ? C29 N4 1.347(7) . ? C29 C30 1.386(7) . ? C29 Sn2 2.193(6) . ? C30 C31 1.373(9) . ? C30 H30 0.94 . ? C31 C32 1.366(9) . ? C31 H31 0.94 . ? C32 C33 1.393(8) . ? C32 C34 1.508(9) . ? C33 N4 1.322(7) . ? C33 H33 0.94 . ? C34 H34A 0.97 . ? C34 H34B 0.97 . ? C34 H34C 0.97 . ? C35 N5 1.354(8) . ? C35 C36 1.385(9) . ? C35 Sn2 2.195(6) . ? C36 C37 1.374(10) . ? C36 H36 0.94 . ? C37 C38 1.345(11) . ? C37 H37 0.94 . ? C38 C39 1.383(10) . ? C38 C40 1.512(10) . ? C39 N5 1.337(8) . ? C39 H39 0.94 . ? C40 H40A 0.97 . ? C40 H40B 0.97 . ? C40 H40C 0.97 . ? C41 N6 1.344(7) . ? C41 C42 1.380(8) . ? C41 Sn2 2.186(6) . ? C42 C43 1.377(9) . ? C42 H42 0.94 . ? C43 C44 1.365(9) . ? C43 H43 0.94 . ? C44 C45 1.378(8) . ? C44 C46 1.517(9) . ? C45 N6 1.340(7) . ? C45 H45 0.94 . ? C46 H46A 0.97 . ? C46 H46B 0.97 . ? C46 H46C 0.97 . ? C47 C48 1.567(19) . ? C47 In2 2.119(17) . ? C47 H47A 0.98 . ? C47 H47B 0.98 . ? C48 H48A 0.97 . ? C48 H48B 0.97 . ? C48 H48C 0.97 . ? C47F C48F 1.581(18) . ? C47F In2 2.256(15) . ? C47F H47C 0.98 . ? C47F H47D 0.98 . ? C48F H48D 0.97 . ? C48F H48E 0.97 . ? C48F H48F 0.97 . ? C49 C50 1.499(18) . ? C49 In2 2.057(17) . ? C49 H49A 0.98 . ? C49 H49B 0.98 . ? C50 H50A 0.97 . ? C50 H50B 0.97 . ? C50 H50C 0.97 . ? C49F C50F 1.50(2) . ? C49F In2 2.091(19) . ? C49F H49C 0.98 . ? C49F H49D 0.98 . ? C50F H50D 0.97 . ? C50F H50E 0.97 . ? C50F H50F 0.97 . ? C51 C52 1.514(17) . ? C51 In2 2.318(15) . ? C51 H51A 0.98 . ? C51 H51B 0.98 . ? C52 H52A 0.97 . ? C52 H52B 0.97 . ? C52 H52C 0.97 . ? C51F C52F 1.420(19) . ? C51F In2 2.178(17) . ? C51F H51C 0.98 . ? C51F H51D 0.98 . ? C52F H52D 0.97 . ? C52F H52E 0.97 . ? C52F H52F 0.97 . ? C53 O2 1.408(10) . ? C53 C54 1.421(15) . ? C53 H53A 0.98 . ? C53 H53B 0.98 . ? C54 C55 1.365(17) . ? C54 H54A 0.98 . ? C54 H54B 0.98 . ? C55 C56 1.468(15) . ? C55 H55A 0.98 . ? C55 H55B 0.98 . ? C56 O2 1.397(9) . ? C56 H56A 0.98 . ? C56 H56B 0.98 . ? N1 Li1 2.036(10) . ? N2 Li1 2.053(10) . ? N3 Li1 2.020(12) . ? N4 Li2 2.020(10) . ? N5 Li2 2.057(12) . ? N6 Li2 2.044(11) . ? O2 Li2 1.942(11) . ? In2 Sn2 2.8487(7) . ? Sn1 Li1 3.262(10) . ? Sn2 Li2 3.253(10) . ? 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 C1 C2 119.5(5) . . ? N1 C1 Sn1 119.6(4) . . ? C2 C1 Sn1 120.9(4) . . ? C3 C2 C1 120.8(6) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C4 C3 C2 120.2(6) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 116.5(6) . . ? C3 C4 C6 123.3(6) . . ? C5 C4 C6 120.1(6) . . ? N1 C5 C4 124.3(6) . . ? N1 C5 H5 117.9 . . ? C4 C5 H5 117.9 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 119.6(5) . . ? N2 C7 Sn1 118.9(4) . . ? C8 C7 Sn1 121.4(5) . . ? C9 C8 C7 120.1(6) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C10 C9 C8 120.4(6) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 115.8(6) . . ? C9 C10 C12 122.3(6) . . ? C11 C10 C12 121.9(7) . . ? N2 C11 C10 125.3(6) . . ? N2 C11 H11 117.3 . . ? C10 C11 H11 117.3 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C14 119.2(6) . . ? N3 C13 Sn1 118.1(4) . . ? C14 C13 Sn1 122.7(6) . . ? C13 C14 C15 120.3(8) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 120.1(7) . . ? C16 C15 H15 120 . . ? C14 C15 H15 120 . . ? C15 C16 C18 116.9(7) . . ? C15 C16 C17 122.5(8) . . ? C18 C16 C17 120.6(9) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C18 C16 124.5(7) . . ? N3 C18 H18 117.7 . . ? C16 C18 H18 117.7 . . ? C20 C19 In1 115.7(8) . . ? C20 C19 H19A 108.4 . . ? In1 C19 H19A 108.4 . . ? C20 C19 H19B 108.4 . . ? In1 C19 H19B 108.4 . . ? H19A C19 H19B 107.4 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C23 In1 C21 113.5(7) . . ? C23 In1 C19 116.6(9) . . ? C21 In1 C19 104.9(8) . . ? C23 In1 C23F 13.0(8) . . ? C21 In1 C23F 126.4(7) . . ? C19 In1 C23F 110.5(8) . . ? C23 In1 C21F 89.4(9) . . ? C21 In1 C21F 25.3(7) . . ? C19 In1 C21F 125.3(7) . . ? C23F In1 C21F 102.0(7) . . ? C23 In1 Sn1 108.5(7) . . ? C21 In1 Sn1 105.7(5) . . ? C19 In1 Sn1 106.9(3) . . ? C23F In1 Sn1 100.9(6) . . ? C21F In1 Sn1 108.6(7) . . ? C22 C21 In1 111.2(11) . . ? C22 C21 H21A 109.4 . . ? In1 C21 H21A 109.4 . . ? C22 C21 H21B 109.4 . . ? In1 C21 H21B 109.4 . . ? H21A C21 H21B 108 . . ? C22F C21F In1 103.8(14) . . ? C22F C21F H21C 111 . . ? In1 C21F H21C 111 . . ? C22F C21F H21D 111 . . ? In1 C21F H21D 111 . . ? H21C C21F H21D 109 . . ? C21F C22F H22D 109.5 . . ? C21F C22F H22E 109.5 . . ? H22D C22F H22E 109.5 . . ? C21F C22F H22F 109.5 . . ? H22D C22F H22F 109.5 . . ? H22E C22F H22F 109.5 . . ? C24 C23 In1 114.9(13) . . ? C24 C23 H23A 108.5 . . ? In1 C23 H23A 108.5 . . ? C24 C23 H23B 108.5 . . ? In1 C23 H23B 108.5 . . ? H23A C23 H23B 107.5 . . ? C24F C23F In1 107.5(14) . . ? C24F C23F H23C 110.2 . . ? In1 C23F H23C 110.2 . . ? C24F C23F H23D 110.2 . . ? In1 C23F H23D 110.2 . . ? H23C C23F H23D 108.5 . . ? C28 O1 C25 108.4(9) . . ? C28 O1 Li1 121.6(12) . . ? C25 O1 Li1 129.1(10) . . ? O1 C25 C26 110.3(12) . . ? O1 C25 H25A 109.6 . . ? C26 C25 H25A 109.6 . . ? O1 C25 H25B 109.6 . . ? C26 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? C25 C26 C27 102.7(12) . . ? C25 C26 H26A 111.2 . . ? C27 C26 H26A 111.2 . . ? C25 C26 H26B 111.2 . . ? C27 C26 H26B 111.2 . . ? H26A C26 H26B 109.1 . . ? C28 C27 C26 104.3(13) . . ? C28 C27 H27A 110.9 . . ? C26 C27 H27A 110.9 . . ? C28 C27 H27B 110.9 . . ? C26 C27 H27B 110.9 . . ? H27A C27 H27B 108.9 . . ? C27 C28 O1 110.3(12) . . ? C27 C28 H28A 109.6 . . ? O1 C28 H28A 109.6 . . ? C27 C28 H28B 109.6 . . ? O1 C28 H28B 109.6 . . ? H28A C28 H28B 108.1 . . ? C28F O1F C25F 108.3(16) . . ? C28F O1F Li1 126(2) . . ? C25F O1F Li1 121(2) . . ? O1F C25F C26F 109.0(17) . . ? O1F C25F H25C 109.9 . . ? C26F C25F H25C 109.9 . . ? O1F C25F H25D 109.9 . . ? C26F C25F H25D 109.9 . . ? H25C C25F H25D 108.3 . . ? C25F C26F C27F 105.6(17) . . ? C25F C26F H26C 110.6 . . ? C27F C26F H26C 110.6 . . ? C25F C26F H26D 110.6 . . ? C27F C26F H26D 110.6 . . ? H26C C26F H26D 108.8 . . ? C28F C27F C26F 101.9(18) . . ? C28F C27F H27C 111.4 . . ? C26F C27F H27C 111.4 . . ? C28F C27F H27D 111.4 . . ? C26F C27F H27D 111.4 . . ? H27C C27F H27D 109.3 . . ? O1F C28F C27F 112.7(19) . . ? O1F C28F H28C 109 . . ? C27F C28F H28C 109 . . ? O1F C28F H28D 109 . . ? C27F C28F H28D 109 . . ? H28C C28F H28D 107.8 . . ? N4 C29 C30 119.8(6) . . ? N4 C29 Sn2 118.6(4) . . ? C30 C29 Sn2 121.6(5) . . ? C31 C30 C29 120.8(6) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C32 C31 C30 120.3(6) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C31 C32 C33 115.2(6) . . ? C31 C32 C34 122.8(6) . . ? C33 C32 C34 122.1(7) . . ? N4 C33 C32 126.1(6) . . ? N4 C33 H33 117 . . ? C32 C33 H33 117 . . ? 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 . . ? N5 C35 C36 119.3(6) . . ? N5 C35 Sn2 119.0(4) . . ? C36 C35 Sn2 121.6(6) . . ? C37 C36 C35 120.3(8) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C38 C37 C36 121.3(8) . . ? C38 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? C37 C38 C39 115.8(8) . . ? C37 C38 C40 122.5(9) . . ? C39 C38 C40 121.6(9) . . ? N5 C39 C38 125.1(8) . . ? N5 C39 H39 117.5 . . ? C38 C39 H39 117.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N6 C41 C42 119.6(6) . . ? N6 C41 Sn2 117.0(4) . . ? C42 C41 Sn2 123.3(5) . . ? C43 C42 C41 120.7(6) . . ? C43 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C44 C43 C42 120.1(6) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C43 C44 C45 116.2(6) . . ? C43 C44 C46 122.7(7) . . ? C45 C44 C46 121.1(7) . . ? N6 C45 C44 124.8(6) . . ? N6 C45 H45 117.6 . . ? C44 C45 H45 117.6 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 In2 108.4(19) . . ? C48 C47 H47A 110 . . ? In2 C47 H47A 110 . . ? C48 C47 H47B 110 . . ? In2 C47 H47B 110 . . ? H47A C47 H47B 108.4 . . ? C48F C47F In2 104.8(13) . . ? C48F C47F H47C 110.8 . . ? In2 C47F H47C 110.8 . . ? C48F C47F H47D 110.8 . . ? In2 C47F H47D 110.8 . . ? H47C C47F H47D 108.9 . . ? C50 C49 In2 118.3(14) . . ? C50 C49 H49A 107.7 . . ? In2 C49 H49A 107.7 . . ? C50 C49 H49B 107.7 . . ? In2 C49 H49B 107.7 . . ? H49A C49 H49B 107.1 . . ? C50F C49F In2 115.1(17) . . ? C50F C49F H49C 108.5 . . ? In2 C49F H49C 108.5 . . ? C50F C49F H49D 108.5 . . ? In2 C49F H49D 108.5 . . ? H49C C49F H49D 107.5 . . ? C52 C51 In2 104.6(13) . . ? C52 C51 H51A 110.8 . . ? In2 C51 H51A 110.8 . . ? C52 C51 H51B 110.8 . . ? In2 C51 H51B 110.8 . . ? H51A C51 H51B 108.9 . . ? C52F C51F In2 109(2) . . ? C52F C51F H51C 109.9 . . ? In2 C51F H51C 110 . . ? C52F C51F H51D 110 . . ? In2 C51F H51D 110 . . ? H51C C51F H51D 108.3 . . ? O2 C53 C54 108.5(10) . . ? O2 C53 H53A 110 . . ? C54 C53 H53A 110 . . ? O2 C53 H53B 110 . . ? C54 C53 H53B 110 . . ? H53A C53 H53B 108.4 . . ? C55 C54 C53 107.5(12) . . ? C55 C54 H54A 110.2 . . ? C53 C54 H54A 110.2 . . ? C55 C54 H54B 110.2 . . ? C53 C54 H54B 110.2 . . ? H54A C54 H54B 108.5 . . ? C54 C55 C56 108.1(12) . . ? C54 C55 H55A 110.1 . . ? C56 C55 H55A 110.1 . . ? C54 C55 H55B 110.1 . . ? C56 C55 H55B 110.1 . . ? H55A C55 H55B 108.4 . . ? O2 C56 C55 105.8(10) . . ? O2 C56 H56A 110.6 . . ? C55 C56 H56A 110.6 . . ? O2 C56 H56B 110.6 . . ? C55 C56 H56B 110.6 . . ? H56A C56 H56B 108.7 . . ? C5 N1 C1 118.6(5) . . ? C5 N1 Li1 127.4(5) . . ? C1 N1 Li1 113.9(5) . . ? C11 N2 C7 118.7(5) . . ? C11 N2 Li1 126.8(5) . . ? C7 N2 Li1 114.4(5) . . ? C18 N3 C13 119.0(6) . . ? C18 N3 Li1 125.4(6) . . ? C13 N3 Li1 115.6(5) . . ? C33 N4 C29 117.8(5) . . ? C33 N4 Li2 127.0(5) . . ? C29 N4 Li2 115.1(5) . . ? C39 N5 C35 118.2(6) . . ? C39 N5 Li2 128.4(6) . . ? C35 N5 Li2 112.6(5) . . ? C45 N6 C41 118.5(5) . . ? C45 N6 Li2 125.0(5) . . ? C41 N6 Li2 116.3(5) . . ? C56 O2 C53 108.1(7) . . ? C56 O2 Li2 126.8(6) . . ? C53 O2 Li2 123.3(6) . . ? C49 In2 C49F 44.7(10) . . ? C49 In2 C47 120.1(11) . . ? C49F In2 C47 144.7(10) . . ? C49 In2 C51F 140.3(12) . . ? C49F In2 C51F 106.0(15) . . ? C47 In2 C51F 65.0(13) . . ? C49 In2 C47F 74.0(9) . . ? C49F In2 C47F 115.9(11) . . ? C47 In2 C47F 50.2(10) . . ? C51F In2 C47F 112.8(12) . . ? C49 In2 C51 103.2(9) . . ? C49F In2 C51 59.0(12) . . ? C47 In2 C51 115.4(10) . . ? C51F In2 C51 51.5(11) . . ? C47F In2 C51 151.4(8) . . ? C49 In2 Sn2 107.1(5) . . ? C49F In2 Sn2 108.5(7) . . ? C47 In2 Sn2 106.6(7) . . ? C51F In2 Sn2 108.3(10) . . ? C47F In2 Sn2 105.1(5) . . ? C51 In2 Sn2 102.8(5) . . ? C13 Sn1 C1 97.0(2) . . ? C13 Sn1 C7 95.9(2) . . ? C1 Sn1 C7 97.9(2) . . ? C13 Sn1 In1 122.41(18) . . ? C1 Sn1 In1 116.68(15) . . ? C7 Sn1 In1 121.43(16) . . ? C13 Sn1 Li1 59.9(3) . . ? C1 Sn1 Li1 59.5(2) . . ? C7 Sn1 Li1 60.1(2) . . ? In1 Sn1 Li1 176.17(16) . . ? C41 Sn2 C29 97.2(2) . . ? C41 Sn2 C35 96.7(2) . . ? C29 Sn2 C35 97.9(2) . . ? C41 Sn2 In2 122.75(16) . . ? C29 Sn2 In2 117.60(15) . . ? C35 Sn2 In2 119.36(19) . . ? C41 Sn2 Li2 60.8(2) . . ? C29 Sn2 Li2 59.7(2) . . ? C35 Sn2 Li2 59.8(3) . . ? In2 Sn2 Li2 176.31(17) . . ? O1F Li1 O1 8.8(12) . . ? O1F Li1 N3 110.8(12) . . ? O1 Li1 N3 111.3(8) . . ? O1F Li1 N1 112.2(11) . . ? O1 Li1 N1 119.6(7) . . ? N3 Li1 N1 104.4(5) . . ? O1F Li1 N2 117.2(11) . . ? O1 Li1 N2 109.2(7) . . ? N3 Li1 N2 105.7(5) . . ? N1 Li1 N2 105.5(5) . . ? O1F Li1 Sn1 176.1(11) . . ? O1 Li1 Sn1 173.4(6) . . ? N3 Li1 Sn1 66.2(3) . . ? N1 Li1 Sn1 67.0(3) . . ? N2 Li1 Sn1 66.5(3) . . ? O2 Li2 N4 115.9(5) . . ? O2 Li2 N6 108.7(5) . . ? N4 Li2 N6 106.0(5) . . ? O2 Li2 N5 116.7(5) . . ? N4 Li2 N5 101.8(5) . . ? N6 Li2 N5 106.8(5) . . ? O2 Li2 Sn2 174.2(5) . . ? N4 Li2 Sn2 66.6(3) . . ? N6 Li2 Sn2 65.5(3) . . ? N5 Li2 Sn2 66.7(3) . . ? #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2012-06-15 at 16:12:38 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\software\wingx\files\archive.dat # CIF files read : x1206 x1206m data_x1206 #TrackingRef '- ccdc_887941-887946.cif' _database_code_depnum_ccdc_archive 'CCDC 887944' _audit_creation_date 2012-06-15T16:12:38-00:00 _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 'C48 H66 Eu Ga2 N6 Sn2' _chemical_formula_sum 'C48 H66 Eu Ga2 N6 Sn2' _chemical_formula_weight 1255.85 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.7309(4) _cell_length_b 12.1475(2) _cell_length_c 20.4128(3) _cell_angle_alpha 90 _cell_angle_beta 99.906(2) _cell_angle_gamma 90 _cell_volume 5063.89(15) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 15724 _cell_measurement_theta_min 2.9278 _cell_measurement_theta_max 32.3874 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2484 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.281 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.87435 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.356 _diffrn_orient_matrix_ub_11 0.0068506 _diffrn_orient_matrix_ub_12 -0.0557974 _diffrn_orient_matrix_ub_13 -0.0064109 _diffrn_orient_matrix_ub_21 -0.0322739 _diffrn_orient_matrix_ub_22 -0.0148094 _diffrn_orient_matrix_ub_23 0.0036641 _diffrn_orient_matrix_ub_31 -0.0108393 _diffrn_orient_matrix_ub_32 0.0087328 _diffrn_orient_matrix_ub_33 -0.0345052 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_unetI/netI 0.0279 _diffrn_reflns_number 36008 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 29.13 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 6822 _reflns_number_gt 5711 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0163P)^2^+22.3319P] 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 6822 _refine_ls_number_parameters 267 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0621 _refine_ls_wR_factor_gt 0.0586 _refine_ls_goodness_of_fit_ref 1.07 _refine_ls_restrained_S_all 1.07 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.544 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.109 #----------------------------------------------------------------------------# # 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 '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 C1 C 0.37142(15) 0.3664(3) 0.17257(14) 0.0189(6) Uani 1 1 d . . . C2 C 0.33807(16) 0.2672(3) 0.15926(15) 0.0217(6) Uani 1 1 d . . . H2 H 0.2918 0.2657 0.1557 0.026 Uiso 1 1 calc R . . C3 C 0.37143(16) 0.1707(3) 0.15115(15) 0.0232(6) Uani 1 1 d . . . H3 H 0.3481 0.1035 0.1424 0.028 Uiso 1 1 calc R . . C4 C 0.43896(16) 0.1726(3) 0.15589(15) 0.0210(6) Uani 1 1 d . . . C5 C 0.46875(16) 0.2736(3) 0.16958(16) 0.0249(7) Uani 1 1 d . . . H5 H 0.515 0.2766 0.1733 0.03 Uiso 1 1 calc R . . C7 C 0.37237(15) 0.6335(2) 0.13295(14) 0.0193(6) Uani 1 1 d . . . C8 C 0.34391(17) 0.6812(3) 0.07296(16) 0.0265(7) Uani 1 1 d . . . H8 H 0.2988 0.6688 0.0563 0.032 Uiso 1 1 calc R . . C9 C 0.38008(17) 0.7465(3) 0.03716(17) 0.0279(7) Uani 1 1 d . . . H9 H 0.3603 0.7766 -0.0044 0.033 Uiso 1 1 calc R . . C10 C 0.44539(17) 0.7677(3) 0.06235(16) 0.0257(7) Uani 1 1 d . . . C11 C 0.46989(17) 0.7211(3) 0.12324(17) 0.0263(7) Uani 1 1 d . . . H11 H 0.5142 0.7365 0.1418 0.032 Uiso 1 1 calc R . . C13 C 0.34440(15) 0.5454(2) 0.28836(15) 0.0190(6) Uani 1 1 d . . . C14 C 0.29744(16) 0.5775(3) 0.32560(16) 0.0240(7) Uani 1 1 d . . . H14 H 0.2543 0.5946 0.3038 0.029 Uiso 1 1 calc R . . C15 C 0.31283(17) 0.5850(3) 0.39427(16) 0.0274(7) Uani 1 1 d . . . H15 H 0.2804 0.607 0.4193 0.033 Uiso 1 1 calc R . . C16 C 0.37546(18) 0.5603(3) 0.42630(16) 0.0273(7) Uani 1 1 d . . . C17 C 0.41935(17) 0.5287(3) 0.38611(16) 0.0309(7) Uani 1 1 d . . . H17 H 0.4625 0.5103 0.4072 0.037 Uiso 1 1 calc R . . C19 C 0.17673(17) 0.4802(3) 0.03546(16) 0.0280(7) Uani 1 1 d . . . H19A H 0.1312 0.4913 0.0123 0.034 Uiso 1 1 calc R . . H19B H 0.2053 0.5312 0.0157 0.034 Uiso 1 1 calc R . . C20 C 0.1974(2) 0.3618(3) 0.02503(17) 0.0347(8) Uani 1 1 d . . . H20A H 0.1943 0.3475 -0.0227 0.052 Uiso 1 1 calc R . . H20B H 0.1686 0.3111 0.0437 0.052 Uiso 1 1 calc R . . H20C H 0.2428 0.3509 0.0473 0.052 Uiso 1 1 calc R . . C21 C 0.14306(19) 0.3919(3) 0.17753(18) 0.0316(8) Uani 1 1 d . . . H21A H 0.0983 0.3784 0.1529 0.038 Uiso 1 1 calc R . . H21B H 0.1691 0.3246 0.1735 0.038 Uiso 1 1 calc R . . C22 C 0.1387(2) 0.4077(3) 0.25053(19) 0.0390(9) Uani 1 1 d . . . H22A H 0.1189 0.3424 0.267 0.059 Uiso 1 1 calc R . . H22B H 0.1117 0.4724 0.2555 0.059 Uiso 1 1 calc R . . H22C H 0.1827 0.4186 0.2762 0.059 Uiso 1 1 calc R . . C23 C 0.15219(17) 0.6659(3) 0.15548(17) 0.0274(7) Uani 1 1 d . . . H23A H 0.1139 0.6861 0.1216 0.033 Uiso 1 1 calc R . . H23B H 0.1367 0.6604 0.1986 0.033 Uiso 1 1 calc R . . C24 C 0.2014(2) 0.7599(3) 0.1604(2) 0.0412(10) Uani 1 1 d . . . H24A H 0.1806 0.8281 0.1717 0.062 Uiso 1 1 calc R . . H24B H 0.2162 0.7689 0.1176 0.062 Uiso 1 1 calc R . . H24C H 0.239 0.7432 0.195 0.062 Uiso 1 1 calc R . . N1 N 0.43756(13) 0.3680(2) 0.17811(13) 0.0226(6) Uani 1 1 d . . . N2 N 0.43610(13) 0.6559(2) 0.15833(13) 0.0231(6) Uani 1 1 d . . . N3 N 0.40579(13) 0.5219(2) 0.31955(12) 0.0250(6) Uani 1 1 d . . . Ga1 Ga 0.182373(17) 0.51572(3) 0.132654(17) 0.02013(7) Uani 1 1 d . . . Sn1 Sn 0.313648(10) 0.516949(17) 0.180952(9) 0.01728(5) Uani 1 1 d . . . Eu1 Eu 0.5 0.526967(18) 0.25 0.01716(5) Uani 1 2 d S . . C6 C 0.47719(18) 0.0700(3) 0.14726(18) 0.0305(7) Uani 1 1 d . . . H6A H 0.4471 0.0076 0.1379 0.046 Uiso 1 1 calc R . . H6B H 0.5085 0.0556 0.1881 0.046 Uiso 1 1 calc R . . H6C H 0.5009 0.08 0.1101 0.046 Uiso 1 1 calc R . . C12 C 0.48805(18) 0.8338(3) 0.02426(18) 0.0334(8) Uani 1 1 d . . . H12A H 0.4619 0.8596 -0.0175 0.05 Uiso 1 1 calc R . . H12B H 0.524 0.7876 0.0145 0.05 Uiso 1 1 calc R . . H12C H 0.506 0.8973 0.051 0.05 Uiso 1 1 calc R . . C18 C 0.3958(2) 0.5697(4) 0.50061(17) 0.0402(9) Uani 1 1 d . . . H18A H 0.3582 0.5929 0.5205 0.06 Uiso 1 1 calc R . . H18B H 0.431 0.6242 0.5108 0.06 Uiso 1 1 calc R . . H18C H 0.4115 0.4981 0.5189 0.06 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 C1 0.0190(15) 0.0229(15) 0.0143(13) 0.0007(11) 0.0012(11) 0.0012(12) C2 0.0170(15) 0.0219(15) 0.0254(15) 0.0026(12) 0.0018(12) -0.0005(12) C3 0.0250(17) 0.0203(15) 0.0237(15) -0.0001(12) 0.0022(12) -0.0036(13) C4 0.0239(16) 0.0202(15) 0.0194(14) -0.0008(11) 0.0049(12) 0.0012(12) C5 0.0190(16) 0.0260(17) 0.0302(17) -0.0031(13) 0.0054(13) -0.0006(13) C7 0.0189(15) 0.0186(14) 0.0204(14) -0.0011(11) 0.0034(12) 0.0009(12) C8 0.0198(16) 0.0305(18) 0.0280(17) 0.0064(14) 0.0008(13) 0.0012(13) C9 0.0282(18) 0.0294(18) 0.0246(16) 0.0073(13) 0.0005(13) 0.0012(14) C10 0.0270(18) 0.0230(16) 0.0278(16) 0.0030(13) 0.0070(13) -0.0004(13) C11 0.0204(16) 0.0261(17) 0.0311(17) 0.0044(13) 0.0012(13) -0.0015(13) C13 0.0185(15) 0.0171(14) 0.0218(14) 0.0016(11) 0.0042(11) -0.0011(11) C14 0.0241(17) 0.0219(16) 0.0264(16) -0.0035(12) 0.0059(13) 0.0040(13) C15 0.0326(19) 0.0246(17) 0.0274(16) -0.0024(13) 0.0123(14) 0.0031(14) C16 0.035(2) 0.0262(17) 0.0205(15) 0.0009(13) 0.0055(13) -0.0042(14) C17 0.0227(17) 0.045(2) 0.0239(16) 0.0042(15) -0.0007(13) -0.0007(16) C19 0.0283(18) 0.0293(17) 0.0237(15) -0.0015(13) -0.0033(13) -0.0002(15) C20 0.046(2) 0.035(2) 0.0231(16) -0.0056(14) 0.0043(15) 0.0034(17) C21 0.033(2) 0.0261(17) 0.0368(19) -0.0032(14) 0.0090(15) -0.0067(15) C22 0.046(2) 0.034(2) 0.039(2) 0.0071(16) 0.0149(18) 0.0007(18) C23 0.0240(17) 0.0251(17) 0.0320(17) -0.0026(13) 0.0023(14) 0.0063(13) C24 0.038(2) 0.0225(18) 0.064(3) -0.0102(17) 0.010(2) -0.0002(16) N1 0.0174(13) 0.0235(14) 0.0266(14) -0.0026(11) 0.0031(11) -0.0009(11) N2 0.0209(14) 0.0226(14) 0.0253(13) 0.0044(10) 0.0021(11) -0.0009(11) N3 0.0192(13) 0.0358(15) 0.0197(12) 0.0020(11) 0.0029(10) -0.0003(12) Ga1 0.01636(16) 0.02007(16) 0.02323(16) -0.00226(13) 0.00136(12) -0.00004(13) Sn1 0.01430(10) 0.01923(10) 0.01777(10) 0.00016(8) 0.00121(7) 0.00065(8) Eu1 0.01428(10) 0.01940(10) 0.01721(10) 0 0.00108(7) 0 C6 0.0321(19) 0.0216(16) 0.0402(19) -0.0015(14) 0.0131(15) 0.0026(14) C12 0.033(2) 0.0315(19) 0.0363(19) 0.0088(15) 0.0087(16) -0.0016(16) C18 0.052(3) 0.047(2) 0.0206(17) 0.0015(16) 0.0045(16) -0.002(2) #----------------------------------------------------------------------------# # 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 C1 N1 1.356(4) . ? C1 C2 1.393(4) . ? C1 Sn1 2.208(3) . ? C2 C3 1.385(4) . ? C2 H2 0.95 . ? C3 C4 1.387(4) . ? C3 H3 0.95 . ? C4 C5 1.381(4) . ? C4 C6 1.503(4) . ? C5 N1 1.342(4) . ? C5 H5 0.95 . ? C7 N2 1.361(4) . ? C7 C8 1.392(4) . ? C7 Sn1 2.204(3) . ? C8 C9 1.383(5) . ? C8 H8 0.95 . ? C9 C10 1.387(5) . ? C9 H9 0.95 . ? C10 C11 1.380(4) . ? C10 C12 1.506(5) . ? C11 N2 1.343(4) . ? C11 H11 0.95 . ? C13 N3 1.352(4) . ? C13 C14 1.390(4) . ? C13 Sn1 2.203(3) . ? C14 C15 1.386(4) . ? C14 H14 0.95 . ? C15 C16 1.382(5) . ? C15 H15 0.95 . ? C16 C17 1.380(5) . ? C16 C18 1.507(5) . ? C17 N3 1.342(4) . ? C17 H17 0.95 . ? C19 C20 1.526(5) . ? C19 Ga1 2.014(3) . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 C22 1.521(5) . ? C21 Ga1 2.006(3) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 C24 1.523(5) . ? C23 Ga1 2.009(3) . ? C23 H23A 0.99 . ? C23 H23B 0.99 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? N1 Eu1 2.628(3) . ? N2 Eu1 2.618(3) . ? N3 Eu1 2.605(3) . ? Ga1 Sn1 2.7304(4) . ? Sn1 Eu1 3.8798(2) . ? Eu1 N3 2.605(3) 2_655 ? Eu1 N2 2.618(3) 2_655 ? Eu1 N1 2.628(3) 2_655 ? Eu1 Sn1 3.8798(2) 2_655 ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 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 C1 C2 119.3(3) . . ? N1 C1 Sn1 122.4(2) . . ? C2 C1 Sn1 118.3(2) . . ? C3 C2 C1 120.9(3) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C2 C3 C4 119.8(3) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 116.0(3) . . ? C5 C4 C6 122.3(3) . . ? C3 C4 C6 121.7(3) . . ? N1 C5 C4 125.2(3) . . ? N1 C5 H5 117.4 . . ? C4 C5 H5 117.4 . . ? N2 C7 C8 119.2(3) . . ? N2 C7 Sn1 122.3(2) . . ? C8 C7 Sn1 118.4(2) . . ? C9 C8 C7 121.2(3) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C10 C9 C8 119.6(3) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C11 C10 C9 116.2(3) . . ? C11 C10 C12 121.7(3) . . ? C9 C10 C12 122.0(3) . . ? N2 C11 C10 125.2(3) . . ? N2 C11 H11 117.4 . . ? C10 C11 H11 117.4 . . ? N3 C13 C14 119.5(3) . . ? N3 C13 Sn1 121.6(2) . . ? C14 C13 Sn1 118.6(2) . . ? C15 C14 C13 120.7(3) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C16 C15 C14 119.9(3) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C17 C16 C15 116.1(3) . . ? C17 C16 C18 121.4(3) . . ? C15 C16 C18 122.5(3) . . ? N3 C17 C16 125.1(3) . . ? N3 C17 H17 117.5 . . ? C16 C17 H17 117.5 . . ? C20 C19 Ga1 111.7(2) . . ? C20 C19 H19A 109.3 . . ? Ga1 C19 H19A 109.3 . . ? C20 C19 H19B 109.3 . . ? Ga1 C19 H19B 109.3 . . ? H19A C19 H19B 107.9 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 Ga1 116.7(2) . . ? C22 C21 H21A 108.1 . . ? Ga1 C21 H21A 108.1 . . ? C22 C21 H21B 108.1 . . ? Ga1 C21 H21B 108.1 . . ? H21A C21 H21B 107.3 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 Ga1 117.7(2) . . ? C24 C23 H23A 107.9 . . ? Ga1 C23 H23A 107.9 . . ? C24 C23 H23B 107.9 . . ? Ga1 C23 H23B 107.9 . . ? H23A C23 H23B 107.2 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C5 N1 C1 118.7(3) . . ? C5 N1 Eu1 119.9(2) . . ? C1 N1 Eu1 116.8(2) . . ? C11 N2 C7 118.4(3) . . ? C11 N2 Eu1 119.2(2) . . ? C7 N2 Eu1 119.4(2) . . ? C17 N3 C13 118.7(3) . . ? C17 N3 Eu1 120.3(2) . . ? C13 N3 Eu1 118.13(19) . . ? C21 Ga1 C23 114.06(15) . . ? C21 Ga1 C19 109.27(14) . . ? C23 Ga1 C19 117.08(14) . . ? C21 Ga1 Sn1 107.30(11) . . ? C23 Ga1 Sn1 104.01(10) . . ? C19 Ga1 Sn1 104.02(10) . . ? C13 Sn1 C7 104.74(11) . . ? C13 Sn1 C1 97.98(11) . . ? C7 Sn1 C1 98.56(11) . . ? C13 Sn1 Ga1 117.39(8) . . ? C7 Sn1 Ga1 115.82(8) . . ? C1 Sn1 Ga1 119.18(8) . . ? C13 Sn1 Eu1 62.22(8) . . ? C7 Sn1 Eu1 63.23(8) . . ? C1 Sn1 Eu1 62.27(8) . . ? Ga1 Sn1 Eu1 178.510(11) . . ? N3 Eu1 N3 177.27(13) . 2_655 ? N3 Eu1 N2 87.66(8) . 2_655 ? N3 Eu1 N2 93.97(8) 2_655 2_655 ? N3 Eu1 N2 93.97(8) . . ? N3 Eu1 N2 87.66(8) 2_655 . ? N2 Eu1 N2 106.54(12) 2_655 . ? N3 Eu1 N1 86.76(8) . . ? N3 Eu1 N1 91.24(8) 2_655 . ? N2 Eu1 N1 168.15(8) 2_655 . ? N2 Eu1 N1 84.29(8) . . ? N3 Eu1 N1 91.24(8) . 2_655 ? N3 Eu1 N1 86.76(8) 2_655 2_655 ? N2 Eu1 N1 84.29(8) 2_655 2_655 ? N2 Eu1 N1 168.15(8) . 2_655 ? N1 Eu1 N1 85.39(12) . 2_655 ? N3 Eu1 Sn1 53.44(6) . . ? N3 Eu1 Sn1 126.46(6) 2_655 . ? N2 Eu1 Sn1 128.91(6) 2_655 . ? N2 Eu1 Sn1 53.80(6) . . ? N1 Eu1 Sn1 53.85(6) . . ? N1 Eu1 Sn1 122.94(6) 2_655 . ? N3 Eu1 Sn1 126.46(6) . 2_655 ? N3 Eu1 Sn1 53.44(6) 2_655 2_655 ? N2 Eu1 Sn1 53.80(6) 2_655 2_655 ? N2 Eu1 Sn1 128.91(6) . 2_655 ? N1 Eu1 Sn1 122.94(6) . 2_655 ? N1 Eu1 Sn1 53.85(6) 2_655 2_655 ? Sn1 Eu1 Sn1 176.405(9) . 2_655 ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2012-03-30 at 13:09:52 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\software\wingx\files\archive.dat # CIF files read : x1284 x1284m data_x1284 #TrackingRef '- ccdc_887941-887946.cif' _database_code_depnum_ccdc_archive 'CCDC 887945' _audit_creation_date 2012-03-30T13:09:52-00:00 _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 'C48 H66 Eu In2 N6 Sn2' _chemical_formula_sum 'C48 H66 Eu In2 N6 Sn2' _chemical_formula_weight 1346.05 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.7341(4) _cell_length_b 12.5374(3) _cell_length_c 20.1952(4) _cell_angle_alpha 90 _cell_angle_beta 97.908(2) _cell_angle_gamma 90 _cell_volume 5199.85(19) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 9275 _cell_measurement_theta_min 2.8799 _cell_measurement_theta_max 32.3222 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.719 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2628 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.046 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.97269 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.356 _diffrn_orient_matrix_ub_11 0.0262847 _diffrn_orient_matrix_ub_12 -0.0365559 _diffrn_orient_matrix_ub_13 0.0015884 _diffrn_orient_matrix_ub_21 0.0220516 _diffrn_orient_matrix_ub_22 0.0412367 _diffrn_orient_matrix_ub_23 0.0118598 _diffrn_orient_matrix_ub_31 -0.0040218 _diffrn_orient_matrix_ub_32 -0.0128651 _diffrn_orient_matrix_ub_33 0.0333656 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_unetI/netI 0.0329 _diffrn_reflns_number 22444 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 27.88 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 6198 _reflns_number_gt 5334 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0226P)^2^+22.1651P] 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 6198 _refine_ls_number_parameters 293 _refine_ls_number_restraints 77 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0683 _refine_ls_wR_factor_gt 0.0646 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.775 _refine_diff_density_min -2.179 _refine_diff_density_rms 0.108 #----------------------------------------------------------------------------# # 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' N N 0.0061 0.0033 '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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 '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 C1 C 0.63541(18) 0.6149(3) 0.83314(16) 0.0245(7) Uani 1 1 d . . . C2 C 0.6727(2) 0.7027(3) 0.8562(2) 0.0341(9) Uani 1 1 d . . . H2 H 0.7188 0.6963 0.8646 0.041 Uiso 1 1 calc R . . C3 C 0.6437(2) 0.7992(3) 0.8671(2) 0.0420(10) Uani 1 1 d . . . H3 H 0.6698 0.8588 0.8827 0.05 Uiso 1 1 calc R . . C4 C 0.5767(2) 0.8087(3) 0.8552(2) 0.0354(9) Uani 1 1 d . . . C5 C 0.54250(19) 0.7182(3) 0.83349(18) 0.0318(8) Uani 1 1 d . . . H5 H 0.4963 0.7229 0.8257 0.038 Uiso 1 1 calc R . . C6 C 0.5424(2) 0.9125(4) 0.8645(3) 0.0527(12) Uani 1 1 d . . . H6A H 0.4955 0.8995 0.8624 0.079 Uiso 1 1 calc R . . H6B H 0.55 0.9624 0.8291 0.079 Uiso 1 1 calc R . . H6C H 0.5593 0.943 0.9081 0.079 Uiso 1 1 calc R . . C7 C 0.61683(17) 0.3544(3) 0.86034(17) 0.0241(7) Uani 1 1 d . . . C8 C 0.6365(2) 0.3038(3) 0.92066(19) 0.0352(9) Uani 1 1 d . . . H8 H 0.6796 0.314 0.9427 0.042 Uiso 1 1 calc R . . C9 C 0.5939(2) 0.2382(3) 0.9494(2) 0.0403(10) Uani 1 1 d . . . H9 H 0.6075 0.2057 0.9915 0.048 Uiso 1 1 calc R . . C10 C 0.5325(2) 0.2205(3) 0.9171(2) 0.0345(9) Uani 1 1 d . . . C11 C 0.5165(2) 0.2710(3) 0.8565(2) 0.0403(10) Uani 1 1 d . . . H11 H 0.4743 0.2584 0.8328 0.048 Uiso 1 1 calc R . . C12 C 0.4838(2) 0.1519(4) 0.9464(3) 0.0487(12) Uani 1 1 d . . . H12A H 0.5067 0.0946 0.973 0.073 Uiso 1 1 calc R . . H12B H 0.4532 0.121 0.9103 0.073 Uiso 1 1 calc R . . H12C H 0.4599 0.1957 0.9751 0.073 Uiso 1 1 calc R . . C13 C 0.65130(17) 0.4412(3) 0.70937(16) 0.0228(7) Uani 1 1 d . . . C14 C 0.6905(2) 0.3876(3) 0.67007(19) 0.0369(9) Uani 1 1 d . . . H14 H 0.7305 0.3575 0.6902 0.044 Uiso 1 1 calc R . . C15 C 0.6721(2) 0.3776(4) 0.6018(2) 0.0412(10) Uani 1 1 d . . . H15 H 0.6988 0.3386 0.5756 0.049 Uiso 1 1 calc R . . C16 C 0.6157(2) 0.4235(3) 0.57183(18) 0.0349(9) Uani 1 1 d . . . C17 C 0.5792(2) 0.4759(4) 0.61383(19) 0.0377(10) Uani 1 1 d . . . H17 H 0.5397 0.5082 0.5942 0.045 Uiso 1 1 calc R . . C18 C 0.5927(3) 0.4172(4) 0.4979(2) 0.0509(12) Uani 1 1 d . . . H18A H 0.5983 0.4868 0.4773 0.076 Uiso 1 1 calc R . . H18B H 0.5466 0.3972 0.4905 0.076 Uiso 1 1 calc R . . H18C H 0.6183 0.3635 0.4776 0.076 Uiso 1 1 calc R . . C19 C 0.8285(2) 0.5204(4) 0.9662(2) 0.0485(11) Uani 1 1 d DU A . H19A H 0.8732 0.5074 0.9891 0.058 Uiso 1 1 calc R . . H19B H 0.8213 0.5985 0.9652 0.058 Uiso 1 1 calc R . . C20 C 0.7808(3) 0.4699(4) 1.0066(2) 0.0544(13) Uani 1 1 d DU . . H20A H 0.7365 0.4922 0.9888 0.082 Uiso 1 1 calc R . . H20B H 0.7907 0.4926 1.0533 0.082 Uiso 1 1 calc R . . H20C H 0.7841 0.3921 1.004 0.082 Uiso 1 1 calc R . . C21 C 0.8521(3) 0.2947(4) 0.8533(3) 0.0673(15) Uani 1 1 d DU A . H21A H 0.8565 0.2801 0.8059 0.081 Uiso 1 1 calc R . . H21B H 0.8954 0.2844 0.8799 0.081 Uiso 1 1 calc R . . C22 C 0.8049(3) 0.2138(5) 0.8763(4) 0.090(2) Uani 1 1 d DU . . H22A H 0.7986 0.2294 0.9225 0.135 Uiso 1 1 calc R . . H22B H 0.8227 0.1418 0.8738 0.135 Uiso 1 1 calc R . . H22C H 0.763 0.2183 0.8474 0.135 Uiso 1 1 calc R . . C23 C 0.8612(4) 0.5818(8) 0.7976(4) 0.060(2) Uani 0.769(15) 1 d PDU A 1 H23A H 0.852 0.6537 0.8144 0.072 Uiso 0.769(15) 1 calc PR A 1 H23B H 0.9091 0.5736 0.8025 0.072 Uiso 0.769(15) 1 calc PR A 1 C24 C 0.8368(6) 0.5778(10) 0.7281(5) 0.110(5) Uani 0.769(15) 1 d PDU A 1 H24A H 0.8366 0.5037 0.7126 0.166 Uiso 0.769(15) 1 calc PR A 1 H24B H 0.8648 0.6208 0.7031 0.166 Uiso 0.769(15) 1 calc PR A 1 H24C H 0.7924 0.6063 0.7208 0.166 Uiso 0.769(15) 1 calc PR A 1 C23F C 0.8658(12) 0.527(3) 0.7769(10) 0.054(5) Uani 0.231(15) 1 d PDU A 2 H23C H 0.9139 0.5241 0.7857 0.065 Uiso 0.231(15) 1 calc PR A 2 H23D H 0.8509 0.4859 0.7357 0.065 Uiso 0.231(15) 1 calc PR A 2 C24F C 0.8405(12) 0.6511(19) 0.7689(13) 0.062(8) Uani 0.231(15) 1 d PDU A 2 H24D H 0.7939 0.6541 0.7729 0.093 Uiso 0.231(15) 1 calc PR A 2 H24E H 0.8477 0.6784 0.7251 0.093 Uiso 0.231(15) 1 calc PR A 2 H24F H 0.8648 0.6948 0.8041 0.093 Uiso 0.231(15) 1 calc PR A 2 N1 N 0.56972(15) 0.6239(3) 0.82252(15) 0.0279(7) Uani 1 1 d . A . N2 N 0.55619(15) 0.3368(3) 0.82854(17) 0.0338(7) Uani 1 1 d . A . N3 N 0.59522(15) 0.4847(3) 0.67996(15) 0.0304(7) Uani 1 1 d . A . In1 In 0.822541(14) 0.46245(3) 0.862462(15) 0.04326(9) Uani 1 1 d DU . . Sn1 Sn 0.684168(11) 0.462193(19) 0.817269(11) 0.02231(7) Uani 1 1 d . A . Eu1 Eu 0.5 0.48366(2) 0.75 0.02264(7) Uani 1 2 d S . . 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 C1 0.029(2) 0.0286(19) 0.0165(16) -0.0001(13) 0.0039(13) -0.0050(14) C2 0.026(2) 0.033(2) 0.044(2) -0.0051(17) 0.0061(17) -0.0078(16) C3 0.041(3) 0.029(2) 0.055(3) -0.0074(19) 0.006(2) -0.0114(18) C4 0.042(2) 0.030(2) 0.033(2) -0.0033(16) 0.0045(17) 0.0024(17) C5 0.026(2) 0.036(2) 0.031(2) -0.0064(16) -0.0014(16) 0.0009(16) C6 0.055(3) 0.035(3) 0.067(3) -0.012(2) 0.005(2) 0.009(2) C7 0.0252(19) 0.0221(18) 0.0242(17) 0.0032(13) 0.0009(14) 0.0011(14) C8 0.031(2) 0.042(2) 0.030(2) 0.0067(17) -0.0034(16) -0.0070(17) C9 0.045(3) 0.041(3) 0.034(2) 0.0128(18) 0.0048(19) -0.0032(19) C10 0.032(2) 0.026(2) 0.047(2) 0.0060(17) 0.0103(18) 0.0007(16) C11 0.024(2) 0.035(2) 0.059(3) 0.013(2) -0.0052(19) -0.0051(17) C12 0.048(3) 0.035(2) 0.067(3) 0.014(2) 0.020(2) -0.005(2) C13 0.0214(18) 0.0251(18) 0.0220(16) 0.0009(13) 0.0031(13) -0.0025(13) C14 0.036(2) 0.042(2) 0.032(2) 0.0019(17) 0.0040(17) 0.0164(18) C15 0.051(3) 0.046(3) 0.029(2) -0.0024(17) 0.0124(19) 0.012(2) C16 0.040(2) 0.041(2) 0.0237(18) 0.0006(16) 0.0037(16) -0.0027(18) C17 0.026(2) 0.062(3) 0.0241(18) 0.0017(18) -0.0028(15) 0.0050(18) C18 0.062(3) 0.065(3) 0.024(2) -0.001(2) 0.003(2) 0.001(3) C19 0.047(3) 0.048(3) 0.045(2) 0.007(2) -0.013(2) -0.018(2) C20 0.050(3) 0.063(3) 0.049(3) -0.012(2) 0.003(2) -0.011(2) C21 0.049(3) 0.093(4) 0.059(3) -0.001(3) 0.002(3) 0.031(3) C22 0.061(4) 0.062(4) 0.140(6) -0.024(4) -0.011(4) 0.021(3) C23 0.047(4) 0.082(6) 0.052(4) 0.010(4) 0.007(3) -0.027(5) C24 0.154(10) 0.109(9) 0.065(6) 0.039(6) 0.003(6) -0.061(7) C23F 0.034(11) 0.080(12) 0.049(9) -0.008(10) 0.005(9) -0.002(11) C24F 0.053(14) 0.070(14) 0.061(16) 0.020(12) 0.002(11) -0.002(11) N1 0.0256(17) 0.0302(17) 0.0269(15) -0.0046(12) -0.0004(12) -0.0009(13) N2 0.0245(17) 0.0308(18) 0.0434(19) 0.0100(14) -0.0049(14) -0.0034(13) N3 0.0200(16) 0.048(2) 0.0220(15) -0.0020(13) 0.0004(12) 0.0041(14) In1 0.02163(15) 0.0710(2) 0.03571(16) 0.01452(14) -0.00117(12) -0.00601(13) Sn1 0.01804(12) 0.02694(13) 0.02110(12) 0.00162(9) -0.00037(9) -0.00125(9) Eu1 0.01925(13) 0.02668(13) 0.02108(12) 0 -0.00044(9) 0 #----------------------------------------------------------------------------# # 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 C1 N1 1.354(5) . ? C1 C2 1.388(5) . ? C1 Sn1 2.209(4) . ? C2 C3 1.383(6) . ? C2 H2 0.95 . ? C3 C4 1.383(6) . ? C3 H3 0.95 . ? C4 C5 1.377(6) . ? C4 C6 1.507(6) . ? C5 N1 1.343(5) . ? C5 H5 0.95 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 N2 1.349(5) . ? C7 C8 1.384(5) . ? C7 Sn1 2.206(3) . ? C8 C9 1.391(5) . ? C8 H8 0.95 . ? C9 C10 1.366(6) . ? C9 H9 0.95 . ? C10 C11 1.377(6) . ? C10 C12 1.508(5) . ? C11 N2 1.345(5) . ? C11 H11 0.95 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 N3 1.346(5) . ? C13 C14 1.386(5) . ? C13 Sn1 2.208(3) . ? C14 C15 1.386(6) . ? C14 H14 0.95 . ? C15 C16 1.367(6) . ? C15 H15 0.95 . ? C16 C17 1.378(6) . ? C16 C18 1.506(5) . ? C17 N3 1.336(5) . ? C17 H17 0.95 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 C20 1.506(6) . ? C19 In1 2.204(4) . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 C22 1.526(9) . ? C21 In1 2.206(5) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 C24 1.426(14) . ? C23 In1 2.211(5) . ? C23 H23A 0.99 . ? C23 H23B 0.99 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C23F C24F 1.64(4) . ? C23F In1 2.208(8) . ? C23F H23C 0.99 . ? C23F H23D 0.99 . ? C24F H24D 0.98 . ? C24F H24E 0.98 . ? C24F H24F 0.98 . ? N1 Eu1 2.596(3) . ? N2 Eu1 2.599(3) . ? N3 Eu1 2.582(3) . ? In1 Sn1 2.8886(4) . ? Sn1 Eu1 3.8823(2) . ? Eu1 N3 2.582(3) 2_656 ? Eu1 N1 2.596(3) 2_656 ? Eu1 N2 2.599(3) 2_656 ? Eu1 Sn1 3.8823(3) 2_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 N1 C1 C2 119.3(3) . . ? N1 C1 Sn1 121.3(2) . . ? C2 C1 Sn1 119.4(3) . . ? C3 C2 C1 120.9(4) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C2 C3 C4 119.7(4) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 116.5(4) . . ? C5 C4 C6 121.3(4) . . ? C3 C4 C6 122.2(4) . . ? N1 C5 C4 124.7(4) . . ? N1 C5 H5 117.7 . . ? C4 C5 H5 117.7 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 119.2(3) . . ? N2 C7 Sn1 120.7(2) . . ? C8 C7 Sn1 120.1(3) . . ? C7 C8 C9 120.7(4) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C10 C9 C8 120.0(4) . . ? C10 C9 H9 120 . . ? C8 C9 H9 120 . . ? C9 C10 C11 116.4(4) . . ? C9 C10 C12 122.3(4) . . ? C11 C10 C12 121.2(4) . . ? N2 C11 C10 124.7(4) . . ? N2 C11 H11 117.7 . . ? C10 C11 H11 117.7 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N3 C13 C14 118.9(3) . . ? N3 C13 Sn1 121.2(2) . . ? C14 C13 Sn1 119.8(3) . . ? C15 C14 C13 120.7(4) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C16 C15 C14 120.2(4) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 115.9(3) . . ? C15 C16 C18 123.5(4) . . ? C17 C16 C18 120.6(4) . . ? N3 C17 C16 125.0(4) . . ? N3 C17 H17 117.5 . . ? C16 C17 H17 117.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 In1 114.9(3) . . ? C20 C19 H19A 108.5 . . ? In1 C19 H19A 108.5 . . ? C20 C19 H19B 108.5 . . ? In1 C19 H19B 108.5 . . ? H19A C19 H19B 107.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 In1 114.2(3) . . ? C22 C21 H21A 108.7 . . ? In1 C21 H21A 108.7 . . ? C22 C21 H21B 108.7 . . ? In1 C21 H21B 108.7 . . ? H21A C21 H21B 107.6 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 In1 116.8(6) . . ? C24 C23 H23A 108.1 . . ? In1 C23 H23A 108.1 . . ? C24 C23 H23B 108.1 . . ? In1 C23 H23B 108.1 . . ? H23A C23 H23B 107.3 . . ? C24F C23F In1 105.4(16) . . ? C24F C23F H23C 110.7 . . ? In1 C23F H23C 110.7 . . ? C24F C23F H23D 110.7 . . ? In1 C23F H23D 110.7 . . ? H23C C23F H23D 108.8 . . ? C23F C24F H24D 109.5 . . ? C23F C24F H24E 109.5 . . ? H24D C24F H24E 109.5 . . ? C23F C24F H24F 109.5 . . ? H24D C24F H24F 109.5 . . ? H24E C24F H24F 109.5 . . ? C5 N1 C1 118.9(3) . . ? C5 N1 Eu1 118.4(2) . . ? C1 N1 Eu1 120.2(2) . . ? C11 N2 C7 119.0(3) . . ? C11 N2 Eu1 116.3(3) . . ? C7 N2 Eu1 119.1(2) . . ? C17 N3 C13 119.2(3) . . ? C17 N3 Eu1 116.4(2) . . ? C13 N3 Eu1 115.8(2) . . ? C19 In1 C21 114.5(2) . . ? C19 In1 C23F 130.3(9) . . ? C21 In1 C23F 97.8(9) . . ? C19 In1 C23 111.2(3) . . ? C21 In1 C23 117.9(4) . . ? C23F In1 C23 21.3(7) . . ? C19 In1 Sn1 102.95(13) . . ? C21 In1 Sn1 104.33(16) . . ? C23F In1 Sn1 104.2(7) . . ? C23 In1 Sn1 103.8(2) . . ? C7 Sn1 C13 100.94(13) . . ? C7 Sn1 C1 98.45(13) . . ? C13 Sn1 C1 99.29(13) . . ? C7 Sn1 In1 122.07(9) . . ? C13 Sn1 In1 118.06(9) . . ? C1 Sn1 In1 114.06(9) . . ? C7 Sn1 Eu1 62.30(9) . . ? C13 Sn1 Eu1 60.51(9) . . ? C1 Sn1 Eu1 62.81(9) . . ? In1 Sn1 Eu1 175.451(11) . . ? N3 Eu1 N3 179.44(16) 2_656 . ? N3 Eu1 N1 95.51(10) 2_656 . ? N3 Eu1 N1 84.11(10) . . ? N3 Eu1 N1 84.11(10) 2_656 2_656 ? N3 Eu1 N1 95.51(10) . 2_656 ? N1 Eu1 N1 94.79(14) . 2_656 ? N3 Eu1 N2 91.46(10) 2_656 2_656 ? N3 Eu1 N2 88.94(10) . 2_656 ? N1 Eu1 N2 172.69(10) . 2_656 ? N1 Eu1 N2 88.12(10) 2_656 2_656 ? N3 Eu1 N2 88.94(10) 2_656 . ? N3 Eu1 N2 91.46(10) . . ? N1 Eu1 N2 88.12(10) . . ? N1 Eu1 N2 172.69(10) 2_656 . ? N2 Eu1 N2 89.80(15) 2_656 . ? N3 Eu1 Sn1 53.32(7) 2_656 2_656 ? N3 Eu1 Sn1 126.73(7) . 2_656 ? N1 Eu1 Sn1 133.54(7) . 2_656 ? N1 Eu1 Sn1 53.49(7) 2_656 2_656 ? N2 Eu1 Sn1 53.17(7) 2_656 2_656 ? N2 Eu1 Sn1 120.08(7) . 2_656 ? N3 Eu1 Sn1 126.73(7) 2_656 . ? N3 Eu1 Sn1 53.32(7) . . ? N1 Eu1 Sn1 53.49(7) . . ? N1 Eu1 Sn1 133.54(7) 2_656 . ? N2 Eu1 Sn1 120.08(7) 2_656 . ? N2 Eu1 Sn1 53.17(7) . . ? Sn1 Eu1 Sn1 172.048(10) 2_656 . ? #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2012-03-29 at 14:30:46 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\software\wingx\files\archive.dat # CIF files read : x1045 x1045m data_x1045 #TrackingRef '- ccdc_887941-887946.cif' _database_code_depnum_ccdc_archive 'CCDC 887946' _audit_creation_date 2012-03-29T14:30:46-00:00 _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 H54 Al2 N6 Sn2 Yb' _chemical_formula_sum 'C42 H54 Al2 N6 Sn2 Yb' _chemical_formula_weight 1107.29 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 14.5590(3) _cell_length_b 14.5590(3) _cell_length_c 17.5926(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 3229.41(14) _cell_formula_units_Z 3 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 8010 _cell_measurement_theta_min 3.426 _cell_measurement_theta_max 32.2271 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.708 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.383 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.58 (release 29-01-2010 CrysAlis171 .NET) (compiled Jan 29 2010,16:49:25) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.62941 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.356 _diffrn_orient_matrix_ub_11 0.0045798 _diffrn_orient_matrix_ub_12 0.0246662 _diffrn_orient_matrix_ub_13 0.0356552 _diffrn_orient_matrix_ub_21 0.0234564 _diffrn_orient_matrix_ub_22 -0.0283059 _diffrn_orient_matrix_ub_23 0.0156495 _diffrn_orient_matrix_ub_31 0.0509469 _diffrn_orient_matrix_ub_32 0.0419126 _diffrn_orient_matrix_ub_33 -0.0104069 _diffrn_measurement_device_type 'Xcalibur, Sapphire3, Gemini' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_unetI/netI 0.0144 _diffrn_reflns_number 10896 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 30.51 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 2196 _reflns_number_gt 1973 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.58 (release 29-01-2010 CrysAlis171 .NET) (compiled Jan 29 2010,16:49:25) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.58 (release 29-01-2010 CrysAlis171 .NET) (compiled Jan 29 2010,16:49:25) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.58 (release 29-01-2010 CrysAlis171 .NET) (compiled Jan 29 2010,16:49:25) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _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^)+(0.0281P)^2^+0.8307P] 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 2196 _refine_ls_number_parameters 81 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0192 _refine_ls_R_factor_gt 0.0165 _refine_ls_wR_factor_ref 0.0456 _refine_ls_wR_factor_gt 0.0451 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.435 _refine_diff_density_min -0.689 _refine_diff_density_rms 0.08 #----------------------------------------------------------------------------# # 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.385 5.5486 '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 C1 C 0.68204(12) 0.20901(12) 0.18222(9) 0.0166(3) Uani 1 1 d . . . C2 C 0.65527(13) 0.11093(13) 0.14983(10) 0.0199(3) Uani 1 1 d . . . C3 C 0.68746(15) 0.04675(14) 0.18655(11) 0.0263(4) Uani 1 1 d . . . H3 H 0.6718 -0.0193 0.1648 0.032 Uiso 1 1 calc R . . C4 C 0.74195(15) 0.07903(15) 0.25427(11) 0.0269(4) Uani 1 1 d . . . H4 H 0.7666 0.0373 0.2788 0.032 Uiso 1 1 calc R . . C5 C 0.75999(14) 0.17381(14) 0.28586(10) 0.0241(3) Uani 1 1 d . . . H5 H 0.7943 0.1945 0.3338 0.029 Uiso 1 1 calc R . . C6 C 0.59201(15) 0.07157(14) 0.07780(11) 0.0274(4) Uani 1 1 d . . . H6A H 0.5749 0.1246 0.059 0.041 Uiso 1 1 calc R . . H6B H 0.5262 0.005 0.088 0.041 Uiso 1 1 calc R . . H6C H 0.6336 0.0594 0.0395 0.041 Uiso 1 1 calc R . . C7 C 0.51531(14) 0.24322(14) -0.07024(11) 0.0262(4) Uani 1 1 d . . . H7A H 0.4755 0.2779 -0.0545 0.039 Uiso 1 1 calc R . . H7B H 0.4858 0.1741 -0.0452 0.039 Uiso 1 1 calc R . . H7C H 0.5101 0.2333 -0.1255 0.039 Uiso 1 1 calc R . . N1 N 0.73080(11) 0.23754(11) 0.25130(8) 0.0191(3) Uani 1 1 d . . . Al1 Al 0.6667 0.3333 -0.04096(6) 0.01986(18) Uani 1 3 d S . . Sn1 Sn 0.6667 0.3333 0.120000(10) 0.01483(5) Uani 1 3 d S . . Yb1 Yb 0.6667 0.3333 0.3333 0.01593(5) Uani 1 6 d S . . 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 C1 0.0171(7) 0.0194(7) 0.0141(7) 0.0011(6) 0.0020(5) 0.0098(6) C2 0.0210(7) 0.0197(7) 0.0180(8) -0.0004(6) 0.0012(6) 0.0095(6) C3 0.0330(9) 0.0211(8) 0.0279(10) -0.0006(7) -0.0001(7) 0.0158(7) C4 0.0348(9) 0.0278(9) 0.0259(9) 0.0037(7) -0.0014(7) 0.0214(8) C5 0.0295(9) 0.0294(8) 0.0177(8) 0.0016(7) -0.0013(7) 0.0178(7) C6 0.0331(9) 0.0227(8) 0.0242(10) -0.0052(7) -0.0066(7) 0.0124(7) C7 0.0252(8) 0.0287(9) 0.0203(9) -0.0010(7) -0.0005(7) 0.0101(7) N1 0.0246(7) 0.0228(7) 0.0136(6) 0.0003(5) 0.0003(5) 0.0146(6) Al1 0.0237(3) 0.0237(3) 0.0121(4) 0 0 0.01186(13) Sn1 0.01744(7) 0.01744(7) 0.00961(10) 0 0 0.00872(3) Yb1 0.01849(6) 0.01849(6) 0.01082(8) 0 0 0.00924(3) #----------------------------------------------------------------------------# # 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 C1 N1 1.363(2) . ? C1 C2 1.400(2) . ? C1 Sn1 2.2203(16) . ? C2 C3 1.396(2) . ? C2 C6 1.501(2) . ? C3 C4 1.377(3) . ? C3 H3 0.95 . ? C4 C5 1.385(2) . ? C4 H4 0.95 . ? C5 N1 1.344(2) . ? C5 H5 0.95 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 Al1 1.9878(17) . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? N1 Yb1 2.4904(13) . ? Al1 C7 1.9878(17) 2_655 ? Al1 C7 1.9878(17) 3_665 ? Al1 Sn1 2.8317(10) . ? Sn1 C1 2.2203(16) 2_655 ? Sn1 C1 2.2203(16) 3_665 ? Sn1 Yb1 3.7531(2) . ? Yb1 N1 2.4903(13) 16_655 ? Yb1 N1 2.4903(14) 17 ? Yb1 N1 2.4904(13) 3_665 ? Yb1 N1 2.4904(14) 2_655 ? Yb1 N1 2.4904(14) 18_545 ? Yb1 Sn1 3.7531(2) 16_655 ? 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 C1 C2 120.71(14) . . ? N1 C1 Sn1 116.13(11) . . ? C2 C1 Sn1 122.74(12) . . ? C3 C2 C1 118.63(16) . . ? C3 C2 C6 118.84(15) . . ? C1 C2 C6 122.53(15) . . ? C4 C3 C2 120.07(16) . . ? C4 C3 H3 120 . . ? C2 C3 H3 120 . . ? C3 C4 C5 118.48(16) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? N1 C5 C4 122.57(17) . . ? N1 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Al1 C7 H7A 109.5 . . ? Al1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Al1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 N1 C1 119.29(14) . . ? C5 N1 Yb1 117.46(11) . . ? C1 N1 Yb1 113.78(10) . . ? C7 Al1 C7 113.53(5) 2_655 . ? C7 Al1 C7 113.53(5) 2_655 3_665 ? C7 Al1 C7 113.53(5) . 3_665 ? C7 Al1 Sn1 105.02(6) 2_655 . ? C7 Al1 Sn1 105.02(6) . . ? C7 Al1 Sn1 105.02(6) 3_665 . ? C1 Sn1 C1 97.78(5) . 2_655 ? C1 Sn1 C1 97.78(5) . 3_665 ? C1 Sn1 C1 97.78(5) 2_655 3_665 ? C1 Sn1 Al1 119.54(4) . . ? C1 Sn1 Al1 119.54(4) 2_655 . ? C1 Sn1 Al1 119.54(4) 3_665 . ? C1 Sn1 Yb1 60.46(4) . . ? C1 Sn1 Yb1 60.46(4) 2_655 . ? C1 Sn1 Yb1 60.46(4) 3_665 . ? Al1 Sn1 Yb1 180 . . ? N1 Yb1 N1 180.00(5) 16_655 . ? N1 Yb1 N1 89.79(5) 16_655 17 ? N1 Yb1 N1 90.21(5) . 17 ? N1 Yb1 N1 90.21(5) 16_655 3_665 ? N1 Yb1 N1 89.79(5) . 3_665 ? N1 Yb1 N1 90.21(5) 17 3_665 ? N1 Yb1 N1 90.21(5) 16_655 2_655 ? N1 Yb1 N1 89.79(5) . 2_655 ? N1 Yb1 N1 180 17 2_655 ? N1 Yb1 N1 89.79(5) 3_665 2_655 ? N1 Yb1 N1 89.79(5) 16_655 18_545 ? N1 Yb1 N1 90.21(5) . 18_545 ? N1 Yb1 N1 89.79(5) 17 18_545 ? N1 Yb1 N1 180 3_665 18_545 ? N1 Yb1 N1 90.21(5) 2_655 18_545 ? N1 Yb1 Sn1 54.59(3) 16_655 16_655 ? N1 Yb1 Sn1 125.41(3) . 16_655 ? N1 Yb1 Sn1 54.59(3) 17 16_655 ? N1 Yb1 Sn1 125.42(3) 3_665 16_655 ? N1 Yb1 Sn1 125.42(3) 2_655 16_655 ? N1 Yb1 Sn1 54.59(3) 18_545 16_655 ? N1 Yb1 Sn1 125.42(3) 16_655 . ? N1 Yb1 Sn1 54.58(3) . . ? N1 Yb1 Sn1 125.41(3) 17 . ? N1 Yb1 Sn1 54.58(3) 3_665 . ? N1 Yb1 Sn1 54.58(3) 2_655 . ? N1 Yb1 Sn1 125.41(3) 18_545 . ? Sn1 Yb1 Sn1 180 16_655 . ? #===END