# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Shashank Mishra' _publ_contact_author_email MISHRASHASHANK74@REDIFFMAIL.COM _publ_section_title ; Homoleptic gallium(III) and indium(III) aminoalkoxides as precursors for sol-gel routes to metal oxide nanomaterials ; loop_ _publ_author_name 'Shashank Mishra' 'Stephane Daniele' 'Erwan Jeanneau' 'Sarah Petit' 'Marc Rolland' # Attachment 'combindcif_B818974A.cif' data_complex1 _database_code_depnum_ccdc_archive 'CCDC 704500' #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H66 Ga4 N6 O12, 4(C H Cl3)' # Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)' _chemical_formula_structural ? _chemical_formula_sum 'C34 H70 Cl12 Ga4 N6 O12' _chemical_formula_iupac ? _chemical_formula_weight 1459.24 _chemical_compound_source 'see text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 2/c' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,y,1/2-z 3 -x,-y,-z 4 x,-y,1/2+z 5 1/2+x,1/2+y,z 6 1/2-x,1/2+y,1/2-z 7 1/2-x,1/2-y,-z 8 1/2+x,1/2-y,1/2+z _cell_length_a 25.5428(12) _cell_length_b 13.1025(3) _cell_length_c 21.0117(10) _cell_angle_alpha 90 _cell_angle_beta 124.017(7) _cell_angle_gamma 90 _cell_volume 5828.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100 _cell_measurement_reflns_used 9320 _cell_measurement_theta_min 2.5056 _cell_measurement_theta_max 32.4630 _cell_special_details ; ; _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_size_rad ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 2960 _exptl_absorpt_coefficient_mu 2.435 _exptl_crystal_density_meas_temp ? # Permitted for _exptl_absorpt_correction_type : # analytical 'analytical from crystal shape' # Example: de Meulenaer&Tompa: ABST # cylinder 'cylindrical' # gaussian 'Gaussian from crystal shape' # Example: PLATON/ABSG # integration 'integration from crystal shape' # multi-scan 'symmetry-related measurements' # Example: SADABS, MULABS # none 'no absorption corr. applied' # numerical 'numerical from crystal shape' # psi-scan 'psi-scan corrections' # Example: PLATON/ABSP # refdelf 'refined from delta-F' # Example: SHELXA, DIFABS, DELABS # sphere 'spherical' # Example: PLATON/ABSS _exptl_absorpt_correction_type empirical # Example: '(North et al., 1968)' _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.681 _exptl_absorpt_correction_T_max 0.813 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source ? _diffrn_radiation_monochromator ? _diffrn_measurement_device 'Oxford Diffraction XCALIBUR' _diffrn_measurement_device_type Area _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 8.4205 _diffrn_standards_number '2 frames' _diffrn_standards_interval_count '30 frames' _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? # number of measured reflections (redundant set) _diffrn_reflns_number 41086 _diffrn_reflns_av_R_equivalents 0.0744 _diffrn_reflns_av_sigmaI/netI 0.0685 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 6700 # number of observed reflections (> n sig(I)) _reflns_number_gt 4280 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'PLATON (Spek, 2003)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs 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^)+(0.0440P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom # Permitted for _refine_ls_hydrogen_treatment : # refall - refined all H parameters # refxyz - refined H coordinates only # refU - refined H U only # noref - no refinement of H parameters # constr - H parameters constrained # mixed - some constrained, some independent # undef - H-atom parameters not defined _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 6700 _refine_ls_number_parameters 413 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0796 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0951 _refine_ls_wR_factor_gt 0.0767 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.164 _refine_diff_density_min -0.970 _refine_diff_density_rms 0.107 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Ga1 Ga Uani 0.00000 0.16190(4) 0.25000 1.000 0.0162(2) . . Ga2 Ga Uani 0.00000 -0.07574(4) 0.25000 1.000 0.0198(2) . . Ga3 Ga Uani -0.00949(2) 0.27936(3) 0.37199(2) 1.000 0.0167(1) . . O1 O Uani 0.04999(11) 0.04419(17) 0.25870(14) 1.000 0.0215(8) . . O2 O Uani 0.02795(12) -0.1176(2) 0.34927(15) 1.000 0.0281(9) . . O3 O Uani -0.05200(11) 0.25912(18) 0.26151(13) 1.000 0.0201(8) . . O4 O Uani 0.04435(11) 0.18547(18) 0.36081(13) 1.000 0.0194(8) . . O5 O Uani -0.06784(11) 0.20993(18) 0.38353(14) 1.000 0.0234(8) . . O6 O Uani 0.04445(12) 0.39357(17) 0.40576(15) 1.000 0.0251(8) . . N1 N Uani 0.09352(15) -0.1446(2) 0.28493(18) 1.000 0.0248(10) . . N2 N Uani 0.05742(14) 0.2181(2) 0.49517(17) 1.000 0.0233(10) . . N3 N Uani -0.08344(14) 0.4074(2) 0.32056(18) 1.000 0.0245(10) . . C1 C Uani 0.0848(2) -0.1700(4) 0.3929(3) 1.000 0.0336(16) . . C2 C Uani 0.12935(19) -0.1430(3) 0.3691(2) 1.000 0.0305(12) . . C3 C Uani 0.1174(2) -0.0749(3) 0.2521(2) 1.000 0.0262(12) . . C4 C Uani 0.10862(17) 0.0358(3) 0.2669(2) 1.000 0.0230(11) . . C5 C Uani 0.0875(3) -0.2485(3) 0.2554(3) 1.000 0.0385(16) . . C6 C Uani 0.09047(19) 0.1245(3) 0.4229(2) 1.000 0.0277(12) . . C7 C Uani 0.11227(19) 0.1798(3) 0.4972(2) 1.000 0.0277(12) . . C8 C Uani 0.0201(2) 0.1363(3) 0.4983(3) 1.000 0.0329(12) . . C9 C Uani -0.0478(2) 0.1715(4) 0.4560(3) 1.000 0.0373(16) . . C10 C Uani 0.0769(2) 0.2942(4) 0.5560(3) 1.000 0.0377(16) . . C11 C Uani 0.0176(2) 0.4909(3) 0.3935(3) 1.000 0.0402(16) . . C12 C Uani -0.0477(2) 0.4944(3) 0.3198(3) 1.000 0.0384(16) . . C13 C Uani -0.13275(19) 0.3703(3) 0.2433(2) 1.000 0.0299(12) . . C14 C Uani -0.1024(2) 0.3197(3) 0.2065(2) 1.000 0.0300(12) . . C15 C Uani -0.1109(2) 0.4321(4) 0.3644(3) 1.000 0.0393(17) . . Cl1 Cl Uani 0.26430(6) 0.12303(11) 0.50695(10) 1.000 0.0840(6) . . Cl2 Cl Uani 0.31906(9) -0.06600(12) 0.57983(10) 1.000 0.0896(7) . . Cl3 Cl Uani 0.30277(8) -0.01784(15) 0.43756(9) 1.000 0.0918(7) . . C16 C Uani 0.3194(2) 0.0311(3) 0.5239(3) 1.000 0.0362(14) . . Cl4 Cl Uani 0.20782(7) 0.01877(11) 0.17324(10) 1.000 0.0763(6) . . Cl5 Cl Uani 0.25948(7) 0.18050(16) 0.28212(9) 1.000 0.1012(7) . . Cl6 Cl Uani 0.21978(7) 0.21909(13) 0.12733(11) 1.000 0.0823(7) . . C17 C Uani 0.2046(2) 0.1496(4) 0.1865(3) 1.000 0.0437(16) . . H1 H Uiso 0.1075(17) 0.081(3) 0.227(2) 1.000 0.0270 . . H2 H Uiso 0.1447(18) 0.058(3) 0.320(2) 1.000 0.0270 . . H3 H Uiso 0.1616(19) -0.087(3) 0.270(2) 1.000 0.0320 . . H4 H Uiso 0.0917(18) -0.088(3) 0.195(2) 1.000 0.0320 . . H5 H Uiso 0.056(2) -0.251(4) 0.202(3) 1.000 0.0580 . . H6 H Uiso 0.129(2) -0.277(3) 0.267(3) 1.000 0.0580 . . H7 H Uiso 0.072(2) -0.293(4) 0.277(3) 1.000 0.0580 . . H8 H Uiso 0.1662(19) -0.187(3) 0.393(2) 1.000 0.0360 . . H9 H Uiso 0.1466(19) -0.074(3) 0.390(2) 1.000 0.0360 . . H10 H Uiso 0.079(2) -0.244(3) 0.389(2) 1.000 0.0400 . . H11 H Uiso 0.1038(19) -0.152(3) 0.443(3) 1.000 0.0400 . . H12 H Uiso -0.075(2) 0.111(3) 0.449(2) 1.000 0.0450 . . H13 H Uiso -0.053(2) 0.220(3) 0.485(3) 1.000 0.0450 . . H14 H Uiso 0.0309(19) 0.110(3) 0.544(2) 1.000 0.0390 . . H15 H Uiso 0.0192(19) 0.071(3) 0.469(2) 1.000 0.0390 . . H16 H Uiso 0.097(2) 0.350(4) 0.550(3) 1.000 0.0570 . . H17 H Uiso 0.107(2) 0.263(3) 0.610(3) 1.000 0.0570 . . H18 H Uiso 0.039(2) 0.315(3) 0.553(3) 1.000 0.0570 . . H19 H Uiso 0.1390(18) 0.129(3) 0.542(2) 1.000 0.0330 . . H20 H Uiso 0.1365(19) 0.236(3) 0.505(2) 1.000 0.0330 . . H21 H Uiso 0.1249(19) 0.123(3) 0.421(2) 1.000 0.0340 . . H22 H Uiso 0.0740(19) 0.055(3) 0.424(2) 1.000 0.0340 . . H23 H Uiso -0.129(2) 0.284(3) 0.170(2) 1.000 0.0360 . . H24 H Uiso -0.0875(19) 0.371(3) 0.187(2) 1.000 0.0360 . . H25 H Uiso -0.1604(19) 0.426(3) 0.212(2) 1.000 0.0360 . . H26 H Uiso -0.1582(19) 0.320(3) 0.250(2) 1.000 0.0360 . . H27 H Uiso -0.076(2) 0.456(3) 0.417(3) 1.000 0.0590 . . H28 H Uiso -0.133(2) 0.371(4) 0.364(3) 1.000 0.0590 . . H29 H Uiso -0.144(2) 0.478(4) 0.338(3) 1.000 0.0590 . . H30 H Uiso -0.042(2) 0.487(3) 0.280(3) 1.000 0.0460 . . H31 H Uiso -0.072(2) 0.559(3) 0.315(2) 1.000 0.0460 . . H32 H Uiso 0.043(2) 0.540(3) 0.392(3) 1.000 0.0480 . . H33 H Uiso 0.015(2) 0.510(3) 0.432(3) 1.000 0.0480 . . H34 H Uiso 0.361(2) 0.070(3) 0.551(2) 1.000 0.0430 . . H35 H Uiso 0.167(2) 0.169(3) 0.175(3) 1.000 0.0520 . . 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 0.0166(3) 0.0162(3) 0.0169(3) 0.0000 0.0101(2) 0.0000 Ga2 0.0220(3) 0.0177(3) 0.0218(3) 0.0000 0.0135(3) 0.0000 Ga3 0.0179(2) 0.0167(2) 0.0174(2) 0.0002(2) 0.0110(2) 0.0003(2) O1 0.0205(13) 0.0171(12) 0.0334(15) -0.0007(11) 0.0190(12) -0.0007(10) O2 0.0279(15) 0.0326(15) 0.0262(15) 0.0072(12) 0.0166(13) 0.0065(12) O3 0.0203(13) 0.0229(13) 0.0163(13) 0.0037(10) 0.0097(11) 0.0071(10) O4 0.0200(13) 0.0208(13) 0.0145(13) 0.0016(10) 0.0078(11) 0.0054(10) O5 0.0211(13) 0.0295(14) 0.0225(14) 0.0068(11) 0.0140(12) -0.0004(11) O6 0.0243(14) 0.0164(13) 0.0332(16) 0.0004(11) 0.0153(13) -0.0003(11) N1 0.0333(19) 0.0187(16) 0.0282(18) -0.0006(14) 0.0208(16) 0.0037(14) N2 0.0246(17) 0.0254(17) 0.0186(16) -0.0013(14) 0.0113(14) -0.0020(14) N3 0.0252(17) 0.0246(17) 0.0285(18) 0.0017(14) 0.0179(15) 0.0069(14) C1 0.037(3) 0.037(3) 0.028(2) 0.010(2) 0.019(2) 0.010(2) C2 0.025(2) 0.032(2) 0.028(2) 0.0069(19) 0.0109(19) 0.0043(19) C3 0.027(2) 0.024(2) 0.034(2) 0.0022(18) 0.021(2) 0.0063(18) C4 0.0173(19) 0.023(2) 0.032(2) 0.0038(18) 0.0158(18) 0.0026(16) C5 0.043(3) 0.024(2) 0.050(3) -0.002(2) 0.027(2) 0.008(2) C6 0.022(2) 0.034(2) 0.019(2) 0.0031(18) 0.0065(18) 0.0096(19) C7 0.020(2) 0.035(2) 0.023(2) 0.0035(19) 0.0089(18) 0.0045(18) C8 0.030(2) 0.034(2) 0.029(2) 0.015(2) 0.013(2) -0.0036(19) C9 0.032(2) 0.050(3) 0.034(3) 0.012(2) 0.021(2) -0.002(2) C10 0.038(3) 0.049(3) 0.024(2) -0.010(2) 0.016(2) -0.001(2) C11 0.040(3) 0.020(2) 0.057(3) -0.002(2) 0.025(3) 0.000(2) C12 0.037(3) 0.022(2) 0.055(3) 0.011(2) 0.025(2) 0.007(2) C13 0.025(2) 0.034(2) 0.031(2) 0.005(2) 0.0158(19) 0.0127(19) C14 0.029(2) 0.037(2) 0.023(2) 0.0017(19) 0.0139(19) 0.0103(19) C15 0.043(3) 0.040(3) 0.043(3) -0.003(2) 0.029(2) 0.012(2) Cl1 0.0327(7) 0.0685(9) 0.1165(14) -0.0265(9) 0.0207(8) 0.0101(7) Cl2 0.1143(14) 0.0674(10) 0.0878(12) 0.0169(9) 0.0570(11) -0.0205(10) Cl3 0.0790(11) 0.1504(16) 0.0699(10) -0.0594(11) 0.0564(9) -0.0482(11) C16 0.030(2) 0.035(2) 0.043(3) -0.006(2) 0.020(2) -0.0039(19) Cl4 0.0627(9) 0.0534(9) 0.1195(14) -0.0061(9) 0.0550(10) 0.0074(7) Cl5 0.0489(9) 0.1394(16) 0.0602(10) -0.0261(10) -0.0033(8) 0.0330(10) Cl6 0.0627(9) 0.0916(11) 0.1184(14) 0.0318(10) 0.0665(10) 0.0128(9) C17 0.027(2) 0.050(3) 0.050(3) -0.002(2) 0.019(2) 0.004(2) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 O1 1.945(3) . . yes Ga1 O3 1.951(3) . . yes Ga1 O4 1.962(2) . . yes Ga1 O1 1.945(3) . 2_555 yes Ga1 O3 1.951(3) . 2_555 yes Ga1 O4 1.962(2) . 2_555 yes Ga2 O1 1.968(3) . . yes Ga2 O2 1.870(3) . . yes Ga2 N1 2.258(4) . . yes Ga2 O1 1.968(3) . 2_555 yes Ga2 O2 1.870(3) . 2_555 yes Ga2 N1 2.258(4) . 2_555 yes Ga3 O3 1.954(2) . . yes Ga3 O4 1.955(3) . . yes Ga3 O5 1.874(3) . . yes Ga3 O6 1.883(3) . . yes Ga3 N3 2.295(3) . . yes Cl1 C16 1.731(5) . . yes Cl2 C16 1.735(5) . . yes Cl3 C16 1.738(5) . . yes Cl4 C17 1.746(5) . . yes Cl5 C17 1.736(5) . . yes Cl6 C17 1.751(6) . . yes O1 C4 1.413(6) . . yes O2 C1 1.390(6) . . yes O3 C14 1.399(5) . . yes O4 C6 1.417(5) . . yes O5 C9 1.401(6) . . yes O6 C11 1.402(5) . . yes N1 C3 1.467(6) . . yes N1 C2 1.468(5) . . yes N1 C5 1.468(5) . . yes N2 C10 1.471(6) . . yes N2 C8 1.460(6) . . yes N2 C7 1.466(7) . . yes N3 C15 1.473(7) . . yes N3 C12 1.466(6) . . yes N3 C13 1.473(5) . . yes C1 C2 1.519(8) . . no C3 C4 1.526(6) . . no C6 C7 1.517(5) . . no C8 C9 1.512(8) . . no C11 C12 1.514(8) . . no C13 C14 1.520(7) . . no C1 H11 0.91(5) . . no C1 H10 0.98(4) . . no C2 H9 0.99(4) . . no C2 H8 0.97(5) . . no C3 H4 1.01(4) . . no C3 H3 0.98(5) . . no C4 H2 1.01(4) . . no C4 H1 1.01(4) . . no C5 H7 0.95(6) . . no C5 H5 0.95(5) . . no C5 H6 1.02(6) . . no C6 H21 0.90(5) . . no C6 H22 1.01(4) . . no C7 H20 0.92(5) . . no C7 H19 1.04(4) . . no C8 H14 0.91(4) . . no C8 H15 1.05(4) . . no C9 H12 1.01(5) . . no C9 H13 0.94(5) . . no C10 H18 0.97(6) . . no C10 H17 1.03(5) . . no C10 H16 0.94(6) . . no C11 H33 0.88(5) . . no C11 H32 0.93(5) . . no C12 H30 0.93(6) . . no C12 H31 1.02(4) . . no C13 H25 0.97(4) . . no C13 H26 0.99(5) . . no C14 H24 0.97(5) . . no C14 H23 0.83(4) . . no C15 H29 0.93(6) . . no C15 H27 1.01(5) . . no C15 H28 0.98(5) . . no C16 H34 1.02(5) . . no C17 H35 0.89(6) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ga1 O3 164.40(11) . . . yes O1 Ga1 O4 95.77(11) . . . yes O1 Ga1 O1 75.04(12) . . 2_555 yes O1 Ga1 O3 94.17(12) . . 2_555 yes O1 Ga1 O4 98.58(11) . . 2_555 yes O3 Ga1 O4 74.41(11) . . . yes O1 Ga1 O3 94.17(12) 2_555 . . yes O3 Ga1 O3 98.46(12) . . 2_555 yes O3 Ga1 O4 93.62(11) . . 2_555 yes O1 Ga1 O4 98.58(11) 2_555 . . yes O3 Ga1 O4 93.62(11) 2_555 . . yes O4 Ga1 O4 161.89(10) . . 2_555 yes O1 Ga1 O3 164.40(11) 2_555 . 2_555 yes O1 Ga1 O4 95.77(11) 2_555 . 2_555 yes O3 Ga1 O4 74.41(11) 2_555 . 2_555 yes O1 Ga2 O2 107.92(12) . . . yes O1 Ga2 N1 77.02(11) . . . yes O1 Ga2 O1 74.01(12) . . 2_555 yes O1 Ga2 O2 99.26(12) . . 2_555 yes O1 Ga2 N1 149.65(11) . . 2_555 yes O2 Ga2 N1 81.13(13) . . . yes O1 Ga2 O2 99.26(12) 2_555 . . yes O2 Ga2 O2 145.88(12) . . 2_555 yes O2 Ga2 N1 85.39(13) . . 2_555 yes O1 Ga2 N1 149.65(11) 2_555 . . yes O2 Ga2 N1 85.39(13) 2_555 . . yes N1 Ga2 N1 132.89(11) . . 2_555 yes O1 Ga2 O2 107.92(12) 2_555 . 2_555 yes O1 Ga2 N1 77.02(11) 2_555 . 2_555 yes O2 Ga2 N1 81.13(13) 2_555 . 2_555 yes O3 Ga3 O4 74.49(11) . . . yes O3 Ga3 O5 97.72(12) . . . yes O3 Ga3 O6 111.01(12) . . . yes O3 Ga3 N3 77.05(11) . . . yes O4 Ga3 O5 111.96(11) . . . yes O4 Ga3 O6 97.45(13) . . . yes O4 Ga3 N3 148.49(11) . . . yes O5 Ga3 O6 143.52(12) . . . yes O5 Ga3 N3 84.90(12) . . . yes O6 Ga3 N3 80.36(12) . . . yes Ga1 O1 Ga2 105.47(15) . . . yes Ga1 O1 C4 132.0(2) . . . yes Ga2 O1 C4 122.5(2) . . . yes Ga2 O2 C1 119.1(3) . . . yes Ga1 O3 Ga3 105.76(12) . . . yes Ga1 O3 C14 130.1(2) . . . yes Ga3 O3 C14 123.2(2) . . . yes Ga1 O4 Ga3 105.29(12) . . . yes Ga1 O4 C6 129.4(2) . . . yes Ga3 O4 C6 121.5(2) . . . yes Ga3 O5 C9 118.8(3) . . . yes Ga3 O6 C11 118.3(3) . . . yes Ga2 N1 C2 102.7(3) . . . yes Ga2 N1 C3 103.9(2) . . . yes Ga2 N1 C5 113.1(4) . . . yes C2 N1 C3 114.5(3) . . . yes C2 N1 C5 111.7(3) . . . yes C3 N1 C5 110.6(4) . . . yes C7 N2 C8 112.6(3) . . . yes C7 N2 C10 110.7(4) . . . yes C8 N2 C10 111.7(4) . . . yes Ga3 N3 C12 102.7(3) . . . yes Ga3 N3 C13 104.4(2) . . . yes Ga3 N3 C15 114.9(3) . . . yes C12 N3 C13 113.5(3) . . . yes C12 N3 C15 110.7(3) . . . yes C13 N3 C15 110.4(4) . . . yes O2 C1 C2 111.5(4) . . . yes N1 C2 C1 108.4(4) . . . yes N1 C3 C4 110.4(4) . . . yes O1 C4 C3 108.4(4) . . . yes O4 C6 C7 108.4(3) . . . yes N2 C7 C6 109.8(4) . . . yes N2 C8 C9 108.2(4) . . . yes O5 C9 C8 110.5(5) . . . yes O6 C11 C12 111.2(4) . . . yes N3 C12 C11 107.6(4) . . . yes N3 C13 C14 109.9(4) . . . yes O3 C14 C13 108.8(3) . . . yes O2 C1 H10 112(3) . . . no O2 C1 H11 109(3) . . . no C2 C1 H10 108(3) . . . no C2 C1 H11 108(4) . . . no H10 C1 H11 108(3) . . . no N1 C2 H8 113(2) . . . no N1 C2 H9 112(2) . . . no C1 C2 H8 112(3) . . . no C1 C2 H9 107(3) . . . no H8 C2 H9 105(4) . . . no N1 C3 H3 114(2) . . . no N1 C3 H4 107(3) . . . no C4 C3 H3 110(2) . . . no C4 C3 H4 109(2) . . . no H3 C3 H4 106(4) . . . no O1 C4 H1 108(3) . . . no O1 C4 H2 111(3) . . . no C3 C4 H1 109(2) . . . no C3 C4 H2 111(2) . . . no H1 C4 H2 109(3) . . . no N1 C5 H5 111(3) . . . no N1 C5 H6 113(3) . . . no N1 C5 H7 110(3) . . . no H5 C5 H6 111(5) . . . no H5 C5 H7 104(5) . . . no H6 C5 H7 109(4) . . . no O4 C6 H21 108(2) . . . no O4 C6 H22 113(2) . . . no C7 C6 H21 105(2) . . . no C7 C6 H22 109(2) . . . no H21 C6 H22 114(4) . . . no N2 C7 H19 112(3) . . . no N2 C7 H20 106(3) . . . no C6 C7 H19 108(2) . . . no C6 C7 H20 113(2) . . . no H19 C7 H20 109(3) . . . no N2 C8 H14 121(3) . . . no N2 C8 H15 112(3) . . . no C9 C8 H14 108(3) . . . no C9 C8 H15 105(3) . . . no H14 C8 H15 102(3) . . . no O5 C9 H12 109(2) . . . no O5 C9 H13 111(3) . . . no C8 C9 H12 108(3) . . . no C8 C9 H13 111(4) . . . no H12 C9 H13 107(4) . . . no N2 C10 H16 111(3) . . . no N2 C10 H17 112(2) . . . no N2 C10 H18 107(3) . . . no H16 C10 H17 109(4) . . . no H16 C10 H18 112(4) . . . no H17 C10 H18 107(5) . . . no O6 C11 H32 111(3) . . . no O6 C11 H33 112(3) . . . no C12 C11 H32 110(3) . . . no C12 C11 H33 109(4) . . . no H32 C11 H33 104(5) . . . no N3 C12 H30 110(3) . . . no N3 C12 H31 107(3) . . . no C11 C12 H30 106(4) . . . no C11 C12 H31 113(2) . . . no H30 C12 H31 113(4) . . . no N3 C13 H25 110(2) . . . no N3 C13 H26 107(2) . . . no C14 C13 H25 112(3) . . . no C14 C13 H26 110(3) . . . no H25 C13 H26 108(4) . . . no O3 C14 H23 110(3) . . . no O3 C14 H24 110(3) . . . no C13 C14 H23 109(4) . . . no C13 C14 H24 110(3) . . . no H23 C14 H24 108(4) . . . no N3 C15 H27 108(3) . . . no N3 C15 H28 107(3) . . . no N3 C15 H29 111(4) . . . no H27 C15 H28 115(4) . . . no H27 C15 H29 114(4) . . . no H28 C15 H29 101(5) . . . no Cl1 C16 Cl2 109.8(3) . . . yes Cl1 C16 Cl3 110.3(3) . . . yes Cl2 C16 Cl3 110.2(2) . . . yes Cl1 C16 H34 104(2) . . . no Cl2 C16 H34 113(2) . . . no Cl3 C16 H34 110(2) . . . no Cl4 C17 Cl5 109.5(3) . . . yes Cl4 C17 Cl6 110.4(3) . . . yes Cl5 C17 Cl6 110.1(3) . . . yes Cl4 C17 H35 112(3) . . . no Cl5 C17 H35 107(3) . . . no Cl6 C17 H35 107(3) . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Ga1 O1 Ga2 97.37(13) . . . . no O4 Ga1 O1 C4 -84.7(3) . . . . no O1 Ga1 O1 Ga2 0.00(11) 2_555 . . . no O1 Ga1 O1 C4 178.0(3) 2_555 . . . no O3 Ga1 O1 Ga2 -168.55(11) 2_555 . . . no O3 Ga1 O1 C4 9.4(3) 2_555 . . . no O4 Ga1 O1 Ga2 -93.72(13) 2_555 . . . no O4 Ga1 O1 C4 84.2(3) 2_555 . . . no O4 Ga1 O3 Ga3 -1.85(12) . . . . no O4 Ga1 O3 C14 166.7(4) . . . . no O1 Ga1 O3 Ga3 95.91(13) 2_555 . . . no O1 Ga1 O3 C14 -95.5(3) 2_555 . . . no O3 Ga1 O3 Ga3 -93.28(13) 2_555 . . . no O3 Ga1 O3 C14 75.3(3) 2_555 . . . no O4 Ga1 O3 Ga3 -168.03(13) 2_555 . . . no O4 Ga1 O3 C14 0.6(3) 2_555 . . . no O1 Ga1 O4 Ga3 -165.81(13) . . . . no O1 Ga1 O4 C6 -8.1(4) . . . . no O3 Ga1 O4 Ga3 1.85(12) . . . . no O3 Ga1 O4 C6 159.6(4) . . . . no O1 Ga1 O4 Ga3 -90.12(13) 2_555 . . . no O1 Ga1 O4 C6 67.6(4) 2_555 . . . no O3 Ga1 O4 Ga3 99.62(13) 2_555 . . . no O3 Ga1 O4 C6 -102.7(4) 2_555 . . . no O1 Ga1 O1 Ga2 0.00(11) . . 2_555 . no O3 Ga1 O1 Ga2 -168.55(11) . . 2_555 . no O4 Ga1 O1 Ga2 -93.72(13) . . 2_555 . no O2 Ga2 O1 Ga1 -94.77(14) . . . . no O2 Ga2 O1 C4 87.0(3) . . . . no N1 Ga2 O1 Ga1 -170.84(14) . . . . no N1 Ga2 O1 C4 11.0(2) . . . . no O1 Ga2 O1 Ga1 0.00(10) 2_555 . . . no O1 Ga2 O1 C4 -178.2(3) 2_555 . . . no O2 Ga2 O1 Ga1 106.12(14) 2_555 . . . no O2 Ga2 O1 C4 -72.1(3) 2_555 . . . no N1 Ga2 O1 Ga1 17.9(3) 2_555 . . . no N1 Ga2 O1 C4 -160.3(2) 2_555 . . . no O1 Ga2 O2 C1 -76.0(3) . . . . no N1 Ga2 O2 C1 -2.8(3) . . . . no O1 Ga2 O2 C1 -152.1(3) 2_555 . . . no O2 Ga2 O2 C1 65.1(4) 2_555 . . . no N1 Ga2 O2 C1 131.9(3) 2_555 . . . no O1 Ga2 N1 C2 89.5(2) . . . . no O1 Ga2 N1 C3 -30.1(2) . . . . no O1 Ga2 N1 C5 -150.1(3) . . . . no O2 Ga2 N1 C2 -21.4(2) . . . . no O2 Ga2 N1 C3 -140.9(2) . . . . no O2 Ga2 N1 C5 99.1(3) . . . . no O1 Ga2 N1 C2 71.8(3) 2_555 . . . no O1 Ga2 N1 C3 -47.7(3) 2_555 . . . no O1 Ga2 N1 C5 -167.7(3) 2_555 . . . no O2 Ga2 N1 C2 -169.9(2) 2_555 . . . no O2 Ga2 N1 C3 70.5(2) 2_555 . . . no O2 Ga2 N1 C5 -49.4(3) 2_555 . . . no N1 Ga2 N1 C2 -96.5(2) 2_555 . . . no N1 Ga2 N1 C3 143.9(2) 2_555 . . . no N1 Ga2 N1 C5 24.0(4) 2_555 . . . no O1 Ga2 O1 Ga1 0.00(11) . . 2_555 . no O2 Ga2 O1 Ga1 106.12(14) . . 2_555 . no N1 Ga2 O1 Ga1 17.9(3) . . 2_555 . no O4 Ga3 O3 Ga1 1.86(12) . . . . no O4 Ga3 O3 C14 -167.7(3) . . . . no O5 Ga3 O3 Ga1 -108.88(14) . . . . no O5 Ga3 O3 C14 81.5(3) . . . . no O6 Ga3 O3 Ga1 94.01(14) . . . . no O6 Ga3 O3 C14 -75.6(3) . . . . no N3 Ga3 O3 Ga1 168.20(16) . . . . no N3 Ga3 O3 C14 -1.4(3) . . . . no O3 Ga3 O4 Ga1 -1.84(12) . . . . no O3 Ga3 O4 C6 -161.7(3) . . . . no O5 Ga3 O4 Ga1 90.35(13) . . . . no O5 Ga3 O4 C6 -69.5(3) . . . . no O6 Ga3 O4 Ga1 -111.66(13) . . . . no O6 Ga3 O4 C6 88.5(3) . . . . no N3 Ga3 O4 Ga1 -28.0(3) . . . . no N3 Ga3 O4 C6 172.1(3) . . . . no O3 Ga3 O5 C9 157.2(3) . . . . no O4 Ga3 O5 C9 80.8(3) . . . . no O6 Ga3 O5 C9 -60.5(4) . . . . no N3 Ga3 O5 C9 -126.7(3) . . . . no O3 Ga3 O6 C11 79.2(3) . . . . no O4 Ga3 O6 C11 155.4(3) . . . . no O5 Ga3 O6 C11 -60.4(4) . . . . no N3 Ga3 O6 C11 7.2(3) . . . . no O3 Ga3 N3 C12 -94.7(3) . . . . no O3 Ga3 N3 C13 24.0(3) . . . . no O3 Ga3 N3 C15 145.1(3) . . . . no O4 Ga3 N3 C12 -68.9(3) . . . . no O4 Ga3 N3 C13 49.8(4) . . . . no O4 Ga3 N3 C15 170.9(3) . . . . no O5 Ga3 N3 C12 166.2(3) . . . . no O5 Ga3 N3 C13 -75.2(3) . . . . no O5 Ga3 N3 C15 45.9(3) . . . . no O6 Ga3 N3 C12 19.7(3) . . . . no O6 Ga3 N3 C13 138.3(3) . . . . no O6 Ga3 N3 C15 -100.6(3) . . . . no Ga1 O1 C4 C3 -166.9(2) . . . . no Ga2 O1 C4 C3 10.7(4) . . . . no Ga2 O2 C1 C2 26.8(5) . . . . no Ga1 O3 C14 C13 171.8(3) . . . . no Ga3 O3 C14 C13 -21.4(5) . . . . no Ga1 O4 C6 C7 177.0(3) . . . . no Ga3 O4 C6 C7 -28.4(5) . . . . no Ga3 O5 C9 C8 -34.3(5) . . . . no Ga3 O6 C11 C12 -33.1(5) . . . . no Ga2 N1 C2 C1 38.9(3) . . . . no C3 N1 C2 C1 150.8(4) . . . . no C5 N1 C2 C1 -82.5(5) . . . . no Ga2 N1 C3 C4 44.7(3) . . . . no C2 N1 C3 C4 -66.5(5) . . . . no C5 N1 C3 C4 166.3(4) . . . . no C8 N2 C7 C6 69.2(4) . . . . no C10 N2 C7 C6 -164.9(3) . . . . no C7 N2 C8 C9 -150.7(4) . . . . no C10 N2 C8 C9 84.0(5) . . . . no Ga3 N3 C12 C11 -39.7(4) . . . . no C13 N3 C12 C11 -151.8(4) . . . . no C15 N3 C12 C11 83.4(5) . . . . no Ga3 N3 C13 C14 -41.4(3) . . . . no C12 N3 C13 C14 69.7(4) . . . . no C15 N3 C13 C14 -165.4(3) . . . . no O2 C1 C2 N1 -45.3(5) . . . . no N1 C3 C4 O1 -38.6(4) . . . . no O4 C6 C7 N2 46.4(5) . . . . no N2 C8 C9 O5 50.0(5) . . . . no O6 C11 C12 N3 49.7(6) . . . . no N3 C13 C14 O3 42.5(4) . . . . no loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Ga3 N2 2.305(3) . . no Ga3 C10 3.211(5) . . no Ga3 H15 3.24(4) . . no Ga3 H16 3.30(5) . . no Ga3 H18 3.31(5) . . no Ga3 H20 3.22(4) . . no Ga3 H1 3.39(4) . 2_555 no Cl1 Cl1 3.384(2) . 7_556 no Cl3 C15 3.384(6) . 5_545 no Cl3 Cl6 3.632(3) . 6_545 no Cl5 C10 3.639(6) . 7_556 no Cl6 Cl3 3.632(3) . 6_555 no Cl1 H21 2.96(5) . . no Cl2 H25 3.12(4) . 8_555 no Cl3 H29 3.07(6) . 5_545 no Cl4 H19 3.00(4) . 4_554 no Cl4 H12 3.13(4) . 2_555 no Cl5 H26 2.92(5) . 2_555 no Cl5 H17 2.94(6) . 7_556 no Cl6 H28 3.06(6) . 2_555 no O1 O4 2.898(4) . . no O1 O2 3.103(4) . . no O1 N1 2.641(4) . . no O1 O2 2.924(4) . 2_555 no O1 O3 2.853(3) . 2_555 no O1 O4 2.961(3) . 2_555 no O1 C3 2.385(6) . . no O1 C6 3.176(4) . . no O1 C2 3.201(5) . . no O1 O1 2.369(5) . 2_555 no O2 C2 2.405(6) . . no O2 C3 3.128(6) . 2_555 no O2 N1 2.700(5) . . no O2 C5 3.036(7) . 2_555 no O2 N1 2.813(5) . 2_555 no O2 O1 2.924(4) . 2_555 no O2 O1 3.103(4) . . no O3 O4 2.853(4) . 2_555 no O3 O1 2.853(3) . 2_555 no O3 O5 2.883(4) . . no O3 C13 2.375(6) . . no O3 C12 3.296(5) . . no O3 O3 2.954(5) . 2_555 no O3 C4 3.169(5) . 2_555 no O3 O4 2.366(4) . . no O3 N3 2.660(4) . . no O3 O6 3.163(3) . . no O4 O5 3.174(5) . . no O4 O1 2.898(4) . . no O4 O3 2.853(4) . 2_555 no O4 O1 2.961(3) . 2_555 no O4 O3 2.366(4) . . no O4 C14 3.105(6) . 2_555 no O4 O6 2.885(3) . . no O4 C8 3.339(6) . . no O4 N2 2.685(4) . . no O5 N3 2.831(4) . . no O5 O3 2.883(4) . . no O5 C13 3.222(4) . . no O5 C15 3.058(6) . . no O5 O4 3.174(5) . . no O5 N2 2.712(5) . . no O5 C17 3.040(7) . 2_555 no O6 C12 2.407(6) . . no O6 C7 3.288(5) . . no O6 C10 3.069(6) . . no O6 N2 2.869(4) . . no O6 C16 3.083(7) . 7_556 no O6 N3 2.714(5) . . no O6 O4 2.885(3) . . no O6 O3 3.163(3) . . no O1 H9 2.91(4) . . no O2 H22 2.63(4) . . no O2 H5 2.50(6) . 2_555 no O2 H4 2.68(5) . 2_555 no O3 H1 2.81(4) . 2_555 no O4 H23 2.89(5) . 2_555 no O5 H28 2.58(6) . . no O5 H26 2.83(4) . . no O5 H1 2.58(4) . 2_555 no O5 H35 2.18(6) . 2_555 no O6 H24 2.74(5) . 2_555 no O6 H16 2.60(5) . . no O6 H34 2.11(5) . 7_556 no N1 O2 2.700(5) . . no N1 O1 2.641(4) . . no N1 O2 2.813(5) . 2_555 no N1 C4 2.458(5) . . no N1 C1 2.423(7) . . no N2 O4 2.685(4) . . no N2 O6 2.869(4) . . no N2 O5 2.712(5) . . no N2 Ga3 2.305(3) . . no N3 C11 2.404(7) . . no N3 C14 2.450(5) . . no N3 O6 2.714(5) . . no N3 O5 2.831(4) . . no N3 O3 2.660(4) . . no C7 O6 3.288(5) . . no C8 O4 3.339(6) . . no C9 C17 3.416(8) . 2_555 no C10 Ga3 3.211(5) . . no C10 O6 3.069(6) . . no C10 Cl5 3.639(6) . 7_556 no C11 C16 3.514(9) . 7_556 no C15 Cl3 3.384(6) . 5_455 no C16 O6 3.083(7) . 7_556 no C16 C11 3.514(9) . 7_556 no C17 O5 3.040(7) . 2_555 no C17 C9 3.416(8) . 2_555 no C1 H22 3.07(4) . . no C1 H7 2.78(5) . . no C2 H2 2.93(4) . . no C4 H9 2.63(4) . . no C5 H31 2.84(4) . 2_545 no C5 H10 2.94(4) . . no C6 H15 2.59(5) . . no C8 H22 2.81(5) . . no C9 H35 2.73(6) . 2_555 no C9 H18 2.75(5) . . no C10 H13 2.94(6) . . no C11 H34 2.75(5) . 7_556 no C11 H27 2.74(6) . . no C12 H24 2.87(4) . . no C14 H30 2.63(5) . . no C15 H33 2.88(6) . . no C16 H32 3.07(6) . 7_556 no C17 H12 2.96(4) . 2_555 no H1 H35 2.59(7) . . no H1 O5 2.58(4) . 2_555 no H1 Ga3 3.39(4) . 2_555 no H1 O3 2.81(4) . 2_555 no H2 H21 2.59(6) . . no H2 H9 2.25(6) . . no H2 C2 2.93(4) . . no H4 H5 2.36(7) . . no H4 O2 2.68(5) . 2_555 no H5 O2 2.50(6) . 2_555 no H5 H4 2.36(7) . . no H5 H31 2.58(7) . 2_545 no H6 H8 2.55(6) . . no H7 H10 2.35(7) . . no H7 C1 2.78(5) . . no H8 H6 2.55(6) . . no H9 C4 2.63(4) . . no H9 H2 2.25(6) . . no H9 O1 2.91(4) . . no H10 H7 2.35(7) . . no H10 C5 2.94(4) . . no H12 H35 2.46(7) . 2_555 no H12 Cl4 3.13(5) . 2_555 no H12 C17 2.96(4) . 2_555 no H13 H18 2.31(8) . . no H13 C10 2.94(6) . . no H14 H17 2.59(6) . . no H15 C6 2.59(5) . . no H15 Ga3 3.24(4) . . no H15 H22 2.09(7) . . no H16 Ga3 3.30(5) . . no H16 O6 2.60(5) . . no H16 H20 2.28(7) . . no H17 H14 2.59(6) . . no H17 Cl5 2.94(6) . 7_556 no H18 Ga3 3.31(5) . . no H18 H13 2.31(8) . . no H18 C9 2.75(5) . . no H19 Cl4 3.00(4) . 4_555 no H20 Ga3 3.22(4) . . no H20 H16 2.28(7) . . no H21 H2 2.59(6) . . no H21 Cl1 2.96(5) . . no H22 C8 2.81(5) . . no H22 H15 2.09(7) . . no H22 O2 2.63(4) . . no H22 C1 3.07(4) . . no H23 O4 2.89(5) . 2_555 no H24 H34 2.51(5) . 8_454 no H24 O6 2.74(5) . 2_555 no H24 C12 2.87(4) . . no H24 H30 2.22(6) . . no H25 Cl2 3.12(4) . 8_454 no H25 H29 2.53(7) . . no H26 Cl5 2.92(5) . 2_555 no H26 H28 2.21(7) . . no H26 O5 2.83(4) . . no H27 C11 2.74(6) . . no H27 H31 2.58(7) . . no H27 H33 2.28(9) . . no H28 O5 2.58(6) . . no H28 H26 2.21(7) . . no H28 Cl6 3.06(6) . 2_555 no H29 H25 2.53(7) . . no H29 Cl3 3.07(6) . 5_455 no H29 H31 2.40(8) . . no H30 C14 2.63(5) . . no H30 H24 2.22(6) . . no H31 C5 2.84(4) . 2_565 no H31 H5 2.58(7) . 2_565 no H31 H27 2.58(7) . . no H31 H29 2.40(8) . . no H32 H34 2.50(7) . 7_556 no H32 C16 3.07(6) . 7_556 no H33 C15 2.88(6) . . no H33 H27 2.28(9) . . no H34 O6 2.11(5) . 7_556 no H34 C11 2.75(5) . 7_556 no H34 H32 2.50(7) . 7_556 no H34 H24 2.51(5) . 8_555 no H35 H1 2.59(7) . . no H35 O5 2.18(6) . 2_555 no H35 C9 2.73(6) . 2_555 no H35 H12 2.46(7) . 2_555 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # C4 H1 O5 1.01(4) 2.58(4) 3.549(4) 161(4) 2_555 yes C5 H5 O2 0.95(5) 2.50(6) 3.036(7) 116(4) 2_555 yes C15 H28 O5 0.98(5) 2.58(6) 3.058(6) 111(4) . yes C16 H34 O6 1.02(5) 2.11(5) 3.083(7) 160(4) 7_556 yes C17 H35 O5 0.89(6) 2.18(6) 3.040(7) 165(5) 2_555 yes # Loop Mechanism for Extra Tables(s) #loop_ #_publ_manuscript_incl_extra_item #'_geom_extra_tableA_col_1' #===END data_complex2 _database_code_depnum_ccdc_archive 'CCDC 704501' _audit_creation_date 08-02-25 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title 'scale in P -1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 11.33520(29) _cell_length_b 11.43510(29) _cell_length_c 14.60850(40) _cell_angle_alpha 74.8165(17) _cell_angle_beta 89.7859(16) _cell_angle_gamma 70.8371(17) _cell_volume 1719.143(83) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' In -0.7276 1.3100 19.1624 0.5476 18.5596 6.3776 4.2948 25.8499 2.0396 92.8029 4.9391 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 1 # Given Formula = C25 H55 Cl5 In5 N4 O10 # Dc = 2.56 Fooo = 928.00 Mu = 37.54 M = 1323.10 # Found Formula = C18 H36 Cl9 In2 N3 O6 # Dc = 1.81 FOOO = 928.00 Mu = 20.76 M = 939.21 _chemical_formula_sum 'C36 H72 Cl18 In4 N6 O12' _chemical_formula_moiety 'C30 H66 In4 N6 O12, 6(C H Cl3)' _chemical_compound_source ? _chemical_formula_weight 1878.47 _cell_measurement_reflns_used 31144 _cell_measurement_theta_min 0.730 _cell_measurement_theta_max 27.878 _cell_measurement_temperature 150 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_min 0.14 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_max 0.44 _exptl_crystal_density_diffrn 1.814 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 2.076 # Sheldrick geometric approximatio 0.68 0.75 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_absorpt_correction_T_min 0.47 _exptl_absorpt_correction_T_max 0.75 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 15429 _reflns_number_total 8216 _diffrn_reflns_av_R_equivalents 0.031 # Number of reflections with Friedels Law is 8216 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 8227 _diffrn_reflns_theta_min 1.450 _diffrn_reflns_theta_max 27.908 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.908 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min -14 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.74 _refine_diff_density_max 1.18 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 5411 _refine_ls_number_restraints 0 _refine_ls_number_parameters 370 _oxford_refine_ls_R_factor_ref 0.0322 _refine_ls_wR_factor_ref 0.0327 _refine_ls_goodness_of_fit_ref 1.1267 _refine_ls_shift/su_max 0.001196 # The values computed from all data _oxford_reflns_number_all 8187 _refine_ls_R_factor_all 0.0582 _refine_ls_wR_factor_all 0.0610 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 5818 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_gt 0.0345 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.187 0.284E-01 0.112E-01 ; 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Cl1 Cl 0.63978(15) 0.79808(13) 0.28680(9) 0.0503 1.0000 Uani . . . . . . . Cl2 Cl 0.72813(16) 0.63536(14) 0.47668(10) 0.0577 1.0000 Uani . . . . . . . Cl3 Cl 0.59829(14) 0.90855(16) 0.44504(14) 0.0648 1.0000 Uani . . . . . . . Cl4 Cl 0.59006(14) 0.90151(15) 0.84726(11) 0.0595 1.0000 Uani . . . . . . . Cl5 Cl 0.66924(13) 0.64441(13) 0.97406(13) 0.0576 1.0000 Uani . . . . . . . Cl6 Cl 0.66377(16) 0.85555(17) 1.04634(12) 0.0621 1.0000 Uani . . . . . . . Cl7 Cl 0.58605(16) 0.45384(15) 0.81109(10) 0.0635 1.0000 Uani . . . . . . . Cl8 Cl 0.54322(13) 0.71043(15) 0.69163(11) 0.0539 1.0000 Uani . . . . . . . Cl9 Cl 0.48891(12) 0.52167(13) 0.61506(9) 0.0448 1.0000 Uani . . . . . . . N1 N 0.7938(3) 1.2216(3) 0.0766(2) 0.0270 1.0000 Uani . . . . . . . N2 N 1.0052(3) 1.3985(3) 0.2320(2) 0.0244 1.0000 Uani . . . . . . . N3 N 1.1925(3) 0.8319(3) 0.3675(3) 0.0302 1.0000 Uani . . . . . . . C1 C 0.8017(5) 1.0375(4) 0.2124(3) 0.0332 1.0000 Uani . . . . . . . C2 C 0.8058(5) 1.0839(5) 0.1055(3) 0.0373 1.0000 Uani . . . . . . . C3 C 0.6614(4) 1.3018(5) 0.0650(4) 0.0398 1.0000 Uani . . . . . . . C4 C 0.8533(5) 1.2545(5) -0.0121(3) 0.0365 1.0000 Uani . . . . . . . C5 C 0.9966(5) 1.2030(5) 0.0082(4) 0.0405 1.0000 Uani . . . . . . . C6 C 0.7791(4) 1.4850(5) 0.2485(4) 0.0388 1.0000 Uani . . . . . . . C7 C 0.8935(7) 1.5176(7) 0.2123(6) 0.0327 0.611 Uani . . . 1 1 . . C8 C 1.1086(7) 1.4263(7) 0.1785(5) 0.0320 0.611 Uani . . . 1 1 . . In2 In 0.92558(3) 1.24670(3) 0.195065(19) 0.0209 1.0000 Uani . . . . . . . C13 C 1.1247(4) 1.2018(4) 0.3571(3) 0.0314 1.0000 Uani . . . . . . . C21 C 0.4906(4) 0.5780(4) 0.7164(3) 0.0340 1.0000 Uani . . . . . . . O1 O 0.8929(3) 1.0686(3) 0.2564(2) 0.0322 1.0000 Uani . . . . . . . O2 O 1.0352(3) 1.2438(3) 0.0817(2) 0.0321 1.0000 Uani . . . . . . . C14 C 1.0402(5) 0.7202(4) 0.3680(4) 0.0392 1.0000 Uani . . . . . . . C15 C 1.1747(4) 0.7053(4) 0.3952(4) 0.0380 1.0000 Uani . . . . . . . C16 C 1.2259(5) 0.8630(5) 0.2689(4) 0.0453 1.0000 Uani . . . . . . . C17 C 1.2877(4) 0.8398(4) 0.4331(4) 0.0339 1.0000 Uani . . . . . . . C18 C 0.7601(4) 1.1545(4) 0.4706(3) 0.0309 1.0000 Uani . . . . . . . C19 C 0.7016(4) 0.7906(4) 0.3993(3) 0.0344 1.0000 Uani . . . . . . . C20 C 0.6923(4) 0.7943(4) 0.9463(4) 0.0355 1.0000 Uani . . . . . . . O5 O 0.8803(3) 1.0591(3) 0.4830(2) 0.0278 1.0000 Uani . . . . . . . O6 O 0.9551(3) 0.8120(3) 0.4051(2) 0.0303 1.0000 Uani . . . . . . . In1 In 1.00276(3) 0.97680(3) 0.38944(2) 0.0226 1.0000 Uani . . . . . . . O3 O 0.7665(3) 1.3783(3) 0.2244(3) 0.0367 1.0000 Uani . . . . . . . O4 O 1.0593(3) 1.1372(3) 0.3180(2) 0.0276 1.0000 Uani . . . . . . . C12 C 1.1298(11) 1.3169(11) 0.2842(8) 0.0297 0.389 Uani . . . 1 2 . . C11 C 0.9124(12) 1.4555(12) 0.2927(11) 0.0405 0.389 Uani . . . 1 2 . . C9 C 1.0473(7) 1.3457(7) 0.3358(5) 0.0310 0.611 Uani . . . 1 1 . . C10 C 1.0175(13) 1.4956(11) 0.1470(9) 0.0366 0.389 Uani . . . 1 2 . . H11 H 0.7192 1.0796 0.2310 0.0411 1.0000 Uiso . . . . . . . H12 H 0.8200 0.9446 0.2325 0.0412 1.0000 Uiso . . . . . . . H21 H 0.8862 1.0345 0.0893 0.0451 1.0000 Uiso . . . . . . . H22 H 0.7384 1.0712 0.0734 0.0450 1.0000 Uiso . . . . . . . H31 H 0.6564 1.3898 0.0534 0.0578 1.0000 Uiso . . . . . . . H32 H 0.6233 1.2775 0.1228 0.0577 1.0000 Uiso . . . . . . . H33 H 0.6181 1.2916 0.0129 0.0578 1.0000 Uiso . . . . . . . H41 H 0.8253 1.3473 -0.0372 0.0458 1.0000 Uiso . . . . . . . H42 H 0.8285 1.2179 -0.0584 0.0461 1.0000 Uiso . . . . . . . H51 H 1.0324 1.2356 -0.0496 0.0520 1.0000 Uiso . . . . . . . H52 H 1.0258 1.1092 0.0255 0.0517 1.0000 Uiso . . . . . . . H71 H 0.9084 1.5766 0.2444 0.0380 0.611 Uiso . . . 1 1 . . H72 H 0.8791 1.5583 0.1441 0.0379 0.611 Uiso . . . 1 1 . . H81 H 1.1805 1.3484 0.1914 0.0479 0.611 Uiso . . . 1 1 . . H82 H 1.1303 1.4922 0.1978 0.0480 0.611 Uiso . . . 1 1 . . H83 H 1.0829 1.4554 0.1113 0.0479 0.611 Uiso . . . 1 1 . . H211 H 0.4055 0.6041 0.7348 0.0378 1.0000 Uiso . . . . . . . H141 H 1.0248 0.7450 0.2990 0.0470 1.0000 Uiso . . . . . . . H142 H 1.0284 0.6378 0.3932 0.0468 1.0000 Uiso . . . . . . . H151 H 1.1921 0.6701 0.4634 0.0438 1.0000 Uiso . . . . . . . H152 H 1.2307 0.6474 0.3636 0.0445 1.0000 Uiso . . . . . . . H161 H 1.2280 0.9495 0.2507 0.0670 1.0000 Uiso . . . . . . . H162 H 1.3074 0.8046 0.2640 0.0667 1.0000 Uiso . . . . . . . H163 H 1.1649 0.8574 0.2263 0.0668 1.0000 Uiso . . . . . . . H171 H 1.3035 0.9202 0.4058 0.0397 1.0000 Uiso . . . . . . . H172 H 1.3648 0.7664 0.4403 0.0402 1.0000 Uiso . . . . . . . H181 H 0.7657 1.2381 0.4359 0.0332 1.0000 Uiso . . . . . . . H182 H 0.7020 1.1342 0.4338 0.0331 1.0000 Uiso . . . . . . . H191 H 0.7817 0.8064 0.3929 0.0418 1.0000 Uiso . . . . . . . H201 H 0.7789 0.7833 0.9312 0.0441 1.0000 Uiso . . . . . . . H121 H 1.1603 1.3682 0.3148 0.0419 0.389 Uiso . . . 1 2 . . H122 H 1.1870 1.2890 0.2381 0.0421 0.389 Uiso . . . 1 2 . . H111 H 0.9223 1.5344 0.2985 0.0560 0.389 Uiso . . . 1 2 . . H112 H 0.9249 1.3946 0.3551 0.0560 0.389 Uiso . . . 1 2 . . H91 H 1.0979 1.3917 0.3532 0.0390 0.611 Uiso . . . 1 1 . . H92 H 0.9749 1.3564 0.3718 0.0391 0.611 Uiso . . . 1 1 . . H101 H 0.9353 1.5470 0.1146 0.0550 0.389 Uiso . . . 1 2 . . H102 H 1.0553 1.5507 0.1653 0.0549 0.389 Uiso . . . 1 2 . . H103 H 1.0686 1.4532 0.1044 0.0549 0.389 Uiso . . . 1 2 . . H61 H 0.7607 1.5569 0.1916 0.0521 0.389 Uiso . . . 1 2 . . H62 H 0.7202 1.5078 0.2945 0.0519 0.389 Uiso . . . 1 2 . . H63 H 0.7855 1.4661 0.3173 0.0519 0.611 Uiso . . . 1 1 . . H64 H 0.7049 1.5599 0.2222 0.0519 0.611 Uiso . . . 1 1 . . H131 H 1.2047 1.1915 0.3303 0.0390 0.611 Uiso . . . 1 1 . . H132 H 1.1397 1.1652 0.4257 0.0388 0.611 Uiso . . . 1 1 . . H133 H 1.2097 1.1438 0.3797 0.0390 0.389 Uiso . . . 1 2 . . H134 H 1.0827 1.2277 0.4101 0.0390 0.389 Uiso . . . 1 2 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0715(9) 0.0440(7) 0.0386(7) -0.0102(5) -0.0072(6) -0.0245(7) Cl2 0.0824(11) 0.0483(8) 0.0442(8) 0.0009(6) -0.0034(7) -0.0349(8) Cl3 0.0458(8) 0.0707(10) 0.0944(12) -0.0583(10) 0.0179(8) -0.0138(7) Cl4 0.0506(8) 0.0573(9) 0.0548(9) -0.0026(7) -0.0035(7) -0.0079(7) Cl5 0.0419(7) 0.0368(7) 0.0952(12) -0.0175(7) 0.0028(7) -0.0154(6) Cl6 0.0725(10) 0.0728(10) 0.0585(9) -0.0406(8) 0.0195(8) -0.0302(8) Cl7 0.0736(10) 0.0515(8) 0.0408(7) -0.0034(6) -0.0144(7) 0.0037(7) Cl8 0.0485(8) 0.0593(8) 0.0593(9) -0.0109(7) 0.0010(6) -0.0295(7) Cl9 0.0369(6) 0.0526(7) 0.0399(7) -0.0198(6) -0.0005(5) -0.0033(5) N1 0.0256(18) 0.0307(18) 0.0231(17) -0.0026(14) -0.0008(14) -0.0112(15) N2 0.0256(17) 0.0246(17) 0.0235(17) -0.0057(14) 0.0028(13) -0.0098(14) N3 0.0293(19) 0.0263(18) 0.032(2) -0.0078(15) 0.0058(15) -0.0063(15) C1 0.043(3) 0.030(2) 0.030(2) -0.0025(18) -0.007(2) -0.021(2) C2 0.051(3) 0.032(2) 0.032(2) -0.0079(19) -0.006(2) -0.019(2) C3 0.030(2) 0.050(3) 0.037(3) -0.004(2) -0.005(2) -0.017(2) C4 0.044(3) 0.050(3) 0.022(2) -0.010(2) 0.0017(19) -0.024(2) C5 0.039(3) 0.060(3) 0.034(3) -0.025(2) 0.011(2) -0.022(2) C6 0.031(2) 0.031(2) 0.062(3) -0.027(2) 0.014(2) -0.0102(19) C7 0.031(4) 0.020(3) 0.045(5) -0.013(3) 0.002(3) -0.003(3) C8 0.036(4) 0.029(4) 0.032(4) -0.006(3) 0.001(3) -0.014(3) In2 0.02239(14) 0.01931(14) 0.02056(14) -0.00493(11) 0.00094(11) -0.00687(11) C13 0.034(2) 0.033(2) 0.029(2) -0.0023(18) -0.0083(19) -0.0191(19) C21 0.024(2) 0.036(2) 0.037(2) -0.0089(19) 0.0000(18) -0.0040(18) O1 0.0402(18) 0.0265(15) 0.0304(16) 0.0018(12) -0.0112(14) -0.0192(13) O2 0.0273(15) 0.0460(19) 0.0281(16) -0.0156(14) 0.0057(13) -0.0149(14) C14 0.038(3) 0.028(2) 0.053(3) -0.015(2) 0.004(2) -0.010(2) C15 0.034(2) 0.024(2) 0.053(3) -0.013(2) 0.005(2) -0.0041(18) C16 0.044(3) 0.055(3) 0.037(3) -0.019(2) 0.014(2) -0.011(2) C17 0.023(2) 0.033(2) 0.046(3) -0.012(2) 0.0031(19) -0.0079(18) C18 0.021(2) 0.029(2) 0.032(2) -0.0053(18) -0.0055(17) 0.0029(17) C19 0.037(2) 0.034(2) 0.034(2) -0.0118(19) 0.002(2) -0.013(2) C20 0.033(2) 0.034(2) 0.042(3) -0.016(2) 0.004(2) -0.0111(19) O5 0.0168(13) 0.0290(15) 0.0301(16) -0.0078(12) -0.0012(11) 0.0017(11) O6 0.0257(15) 0.0221(14) 0.0419(18) -0.0072(13) 0.0025(13) -0.0077(12) In1 0.02344(15) 0.01854(14) 0.02282(15) -0.00331(11) -0.00106(12) -0.00518(11) O3 0.0255(16) 0.0338(17) 0.061(2) -0.0275(16) 0.0116(15) -0.0112(13) O4 0.0320(16) 0.0274(15) 0.0225(14) 0.0019(11) -0.0082(12) -0.0156(13) C12 0.030(6) 0.038(6) 0.028(6) -0.010(5) -0.004(5) -0.020(5) C11 0.040(7) 0.039(7) 0.060(9) -0.029(7) 0.018(6) -0.026(6) C9 0.039(4) 0.032(4) 0.029(4) -0.012(3) 0.001(3) -0.018(3) C10 0.053(8) 0.025(6) 0.034(6) 0.007(5) 0.000(6) -0.028(6) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.12790(11) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cl1 . C19 . 1.759(5) yes Cl2 . C19 . 1.766(5) yes Cl3 . C19 . 1.752(5) yes Cl4 . C20 . 1.757(5) yes Cl5 . C20 . 1.761(5) yes Cl6 . C20 . 1.765(5) yes Cl7 . C21 . 1.753(5) yes Cl8 . C21 . 1.756(5) yes Cl9 . C21 . 1.765(5) yes N1 . C2 . 1.478(6) yes N1 . C3 . 1.463(6) yes N1 . C4 . 1.476(6) yes N1 . In2 . 2.424(3) yes N2 . C7 . 1.485(7) yes N2 . C8 . 1.481(8) yes N2 . In2 . 2.375(3) yes N2 . C9 . 1.492(8) yes N2 . In2 . 2.375(3) yes N2 . C12 . 1.489(12) yes N2 . C11 . 1.470(13) yes N2 . C10 . 1.474(11) yes N3 . C15 . 1.478(6) yes N3 . C16 . 1.469(6) yes N3 . C17 . 1.486(6) yes N3 . In1 . 2.325(4) yes C1 . C2 . 1.518(6) yes C1 . O1 . 1.405(5) yes C1 . H11 . 0.975 no C1 . H12 . 0.975 no C2 . H21 . 0.968 no C2 . H22 . 0.967 no C3 . H31 . 0.958 no C3 . H32 . 0.964 no C3 . H33 . 0.959 no C4 . C5 . 1.535(7) yes C4 . H41 . 0.968 no C4 . H42 . 0.969 no C5 . O2 . 1.401(5) yes C5 . H51 . 0.974 no C5 . H52 . 0.974 no C6 . C7 . 1.519(9) yes C6 . O3 . 1.405(5) yes C6 . H63 . 0.969 no C6 . H64 . 0.973 no C6 . O3 . 1.405(5) yes C6 . C11 . 1.540(14) yes C6 . H61 . 0.970 no C6 . H62 . 0.970 no C7 . H71 . 0.973 no C7 . H72 . 0.972 no C8 . H81 . 0.965 no C8 . H82 . 0.970 no C8 . H83 . 0.963 no In2 . O1 . 2.150(3) yes In2 . O2 . 2.068(3) yes In2 . O3 . 2.061(3) yes In2 . O4 . 2.164(3) yes C13 . O4 . 1.417(5) yes C13 . C9 . 1.536(9) yes C13 . H131 . 0.970 no C13 . H132 . 0.971 no C13 . O4 . 1.417(5) yes C13 . C12 . 1.478(12) yes C13 . H133 . 0.972 no C13 . H134 . 0.969 no C21 . H211 . 0.971 no O1 . In1 . 2.127(3) yes C14 . C15 . 1.520(7) yes C14 . O6 . 1.399(6) yes C14 . H141 . 0.973 no C14 . H142 . 0.971 no C15 . H151 . 0.965 no C15 . H152 . 0.968 no C16 . H161 . 0.963 no C16 . H162 . 0.961 no C16 . H163 . 0.962 no C17 . C18 2_776 1.514(7) yes C17 . H171 . 0.976 no C17 . H172 . 0.976 no C18 . O5 . 1.415(5) yes C18 . H181 . 0.980 no C18 . H182 . 0.972 no C19 . H191 . 0.982 no C20 . H201 . 0.980 no O5 . In1 2_776 2.158(3) yes O5 . In1 . 2.117(3) yes O6 . In1 . 2.083(3) yes In1 . O4 . 2.152(3) yes C12 . H121 . 0.968 no C12 . H122 . 0.974 no C11 . H111 . 0.970 no C11 . H112 . 0.969 no C9 . H91 . 0.969 no C9 . H92 . 0.964 no C10 . H101 . 0.967 no C10 . H102 . 0.959 no C10 . H103 . 0.963 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 . N1 . C3 . 109.9(4) yes C2 . N1 . C4 . 111.6(4) yes C3 . N1 . C4 . 110.4(4) yes C2 . N1 . In2 . 105.5(2) yes C3 . N1 . In2 . 116.3(3) yes C4 . N1 . In2 . 103.0(2) yes C7 . N2 . C8 . 109.5(5) yes C7 . N2 . In2 . 103.2(3) yes C8 . N2 . In2 . 117.8(3) yes C7 . N2 . C9 . 111.8(5) yes C8 . N2 . C9 . 109.7(5) yes In2 . N2 . C9 . 104.8(3) yes In2 . N2 . C12 . 103.3(5) yes In2 . N2 . C11 . 102.4(5) yes C12 . N2 . C11 . 113.7(8) yes In2 . N2 . C10 . 113.2(5) yes C12 . N2 . C10 . 111.2(7) yes C11 . N2 . C10 . 112.4(8) yes C15 . N3 . C16 . 111.4(4) yes C15 . N3 . C17 . 112.2(4) yes C16 . N3 . C17 . 110.1(4) yes C15 . N3 . In1 . 104.7(3) yes C16 . N3 . In1 . 112.6(3) yes C17 . N3 . In1 . 105.5(3) yes C2 . C1 . O1 . 107.6(4) yes C2 . C1 . H11 . 110.7 no O1 . C1 . H11 . 109.6 no C2 . C1 . H12 . 110.6 no O1 . C1 . H12 . 109.6 no H11 . C1 . H12 . 108.8 no C1 . C2 . N1 . 110.5(4) yes C1 . C2 . H21 . 108.1 no N1 . C2 . H21 . 108.5 no C1 . C2 . H22 . 109.2 no N1 . C2 . H22 . 110.1 no H21 . C2 . H22 . 110.5 no N1 . C3 . H31 . 108.3 no N1 . C3 . H32 . 109.4 no H31 . C3 . H32 . 109.0 no N1 . C3 . H33 . 110.6 no H31 . C3 . H33 . 110.1 no H32 . C3 . H33 . 109.5 no N1 . C4 . C5 . 110.2(4) yes N1 . C4 . H41 . 108.8 no C5 . C4 . H41 . 109.1 no N1 . C4 . H42 . 109.4 no C5 . C4 . H42 . 110.1 no H41 . C4 . H42 . 109.1 no C4 . C5 . O2 . 111.7(4) yes C4 . C5 . H51 . 108.1 no O2 . C5 . H51 . 108.7 no C4 . C5 . H52 . 109.1 no O2 . C5 . H52 . 109.5 no H51 . C5 . H52 . 109.7 no C7 . C6 . O3 . 113.7(4) yes C7 . C6 . H63 . 108.6 no O3 . C6 . H63 . 108.1 no C7 . C6 . H64 . 108.2 no O3 . C6 . H64 . 109.1 no H63 . C6 . H64 . 109.1 no O3 . C6 . C11 . 111.7(5) yes O3 . C6 . H61 . 109.1 no C11 . C6 . H61 . 109.2 no O3 . C6 . H62 . 109.0 no C11 . C6 . H62 . 108.4 no H61 . C6 . H62 . 109.4 no C6 . C7 . N2 . 110.0(5) yes C6 . C7 . H71 . 109.1 no N2 . C7 . H71 . 109.4 no C6 . C7 . H72 . 109.9 no N2 . C7 . H72 . 109.3 no H71 . C7 . H72 . 109.2 no N2 . C8 . H81 . 109.0 no N2 . C8 . H82 . 110.1 no H81 . C8 . H82 . 109.7 no N2 . C8 . H83 . 109.5 no H81 . C8 . H83 . 108.9 no H82 . C8 . H83 . 109.6 no N1 . In2 . N2 . 142.30(12) yes N1 . In2 . O1 . 73.56(12) yes N2 . In2 . O1 . 142.99(11) yes N1 . In2 . O2 . 77.77(12) yes N2 . In2 . O2 . 88.77(12) yes O1 . In2 . O2 . 114.18(13) yes N1 . In2 . O3 . 87.17(13) yes N2 . In2 . O3 . 77.74(12) yes O1 . In2 . O3 . 101.34(13) yes O2 . In2 . O3 . 134.92(14) yes N1 . In2 . O4 . 141.92(11) yes N2 . In2 . O4 . 75.30(12) yes O1 . In2 . O4 . 71.38(11) yes O2 . In2 . O4 . 103.58(12) yes O3 . In2 . O4 . 113.80(13) yes O4 . C13 . C9 . 110.4(4) yes O4 . C13 . H131 . 109.6 no C9 . C13 . H131 . 109.7 no O4 . C13 . H132 . 109.7 no C9 . C13 . H132 . 108.6 no H131 . C13 . H132 . 108.9 no O4 . C13 . C12 . 110.3(5) yes O4 . C13 . H133 . 109.2 no C12 . C13 . H133 . 109.1 no O4 . C13 . H134 . 109.6 no C12 . C13 . H134 . 109.5 no H133 . C13 . H134 . 109.2 no Cl9 . C21 . Cl8 . 111.1(3) yes Cl9 . C21 . Cl7 . 110.1(3) yes Cl8 . C21 . Cl7 . 110.2(3) yes Cl9 . C21 . H211 . 107.9 no Cl8 . C21 . H211 . 109.2 no Cl7 . C21 . H211 . 108.3 no C1 . O1 . In2 . 120.3(2) yes C1 . O1 . In1 . 131.2(3) yes In2 . O1 . In1 . 108.24(12) yes C5 . O2 . In2 . 116.1(3) yes C15 . C14 . O6 . 111.2(4) yes C15 . C14 . H141 . 109.6 no O6 . C14 . H141 . 109.9 no C15 . C14 . H142 . 108.8 no O6 . C14 . H142 . 109.0 no H141 . C14 . H142 . 108.3 no C14 . C15 . N3 . 110.3(4) yes C14 . C15 . H151 . 108.7 no N3 . C15 . H151 . 108.8 no C14 . C15 . H152 . 109.0 no N3 . C15 . H152 . 110.1 no H151 . C15 . H152 . 109.8 no N3 . C16 . H161 . 109.5 no N3 . C16 . H162 . 109.9 no H161 . C16 . H162 . 108.8 no N3 . C16 . H163 . 110.3 no H161 . C16 . H163 . 108.6 no H162 . C16 . H163 . 109.7 no C18 2_776 C17 . N3 . 111.7(4) yes C18 2_776 C17 . H171 . 106.7 no N3 . C17 . H171 . 107.9 no C18 2_776 C17 . H172 . 110.4 no N3 . C17 . H172 . 109.9 no H171 . C17 . H172 . 110.3 no C17 2_776 C18 . O5 . 109.8(3) yes C17 2_776 C18 . H181 . 110.1 no O5 . C18 . H181 . 109.1 no C17 2_776 C18 . H182 . 109.3 no O5 . C18 . H182 . 109.9 no H181 . C18 . H182 . 108.6 no Cl2 . C19 . Cl1 . 109.1(3) yes Cl2 . C19 . Cl3 . 110.6(3) yes Cl1 . C19 . Cl3 . 110.2(3) yes Cl2 . C19 . H191 . 109.0 no Cl1 . C19 . H191 . 109.3 no Cl3 . C19 . H191 . 108.6 no Cl6 . C20 . Cl5 . 108.5(3) yes Cl6 . C20 . Cl4 . 110.4(3) yes Cl5 . C20 . Cl4 . 110.0(3) yes Cl6 . C20 . H201 . 109.3 no Cl5 . C20 . H201 . 109.8 no Cl4 . C20 . H201 . 108.9 no C18 . O5 . In1 2_776 117.1(2) yes C18 . O5 . In1 . 134.4(3) yes In1 2_776 O5 . In1 . 105.58(12) yes C14 . O6 . In1 . 112.8(3) yes N3 . In1 . O5 2_776 76.63(12) yes N3 . In1 . O1 . 109.31(13) yes O5 2_776 In1 . O1 . 162.46(11) yes N3 . In1 . O5 . 149.08(12) yes O5 2_776 In1 . O5 . 74.42(12) yes O1 . In1 . O5 . 101.54(12) yes N3 . In1 . O6 . 79.14(13) yes O5 2_776 In1 . O6 . 105.60(12) yes O1 . In1 . O6 . 91.83(12) yes O5 . In1 . O6 . 98.38(12) yes N3 . In1 . O4 . 91.04(13) yes O5 2_776 In1 . O4 . 91.64(11) yes O1 . In1 . O4 . 72.07(11) yes O5 . In1 . O4 . 100.34(12) yes O6 . In1 . O4 . 157.37(12) yes C6 . O3 . In2 . 117.8(3) yes C13 . O4 . In2 . 118.4(2) yes C13 . O4 . In1 . 128.7(2) yes In2 . O4 . In1 . 106.83(12) yes N2 . C12 . C13 . 112.7(7) yes N2 . C12 . H121 . 108.5 no C13 . C12 . H121 . 108.9 no N2 . C12 . H122 . 108.2 no C13 . C12 . H122 . 108.8 no H121 . C12 . H122 . 109.6 no C6 . C11 . N2 . 109.7(9) yes C6 . C11 . H111 . 109.6 no N2 . C11 . H111 . 109.7 no C6 . C11 . H112 . 108.9 no N2 . C11 . H112 . 109.1 no H111 . C11 . H112 . 109.8 no C13 . C9 . N2 . 109.3(5) yes C13 . C9 . H91 . 109.9 no N2 . C9 . H91 . 109.5 no C13 . C9 . H92 . 109.5 no N2 . C9 . H92 . 109.3 no H91 . C9 . H92 . 109.3 no N2 . C10 . H101 . 109.4 no N2 . C10 . H102 . 110.0 no H101 . C10 . H102 . 109.1 no N2 . C10 . H103 . 109.7 no H101 . C10 . H103 . 109.2 no H102 . C10 . H103 . 109.5 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C21 . H211 . C6 2_676 137 0.97 2.60 3.372(10) yes C21 . H211 . O3 2_676 169 0.97 2.00 2.957(10) yes C19 . H191 . O6 . 169 0.98 2.00 2.966(10) yes C20 . H201 . O2 2_776 172 0.98 2.04 3.017(10) yes #===END