data_global # 1. SUBMISSION DETAILS _publ_contact_autor ; A. Monge Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; _publ_contact_author_phone '34 1 334-9025' _publ_contact_author_fax '34 1 372-0623' _publ_contact_author_email amonge@icmm.csic.es _publ_requested_journal 'Chem. Mater. _publ_requested_coeditor_name ? _publ_contact_letter ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Novel 2D and 3D Indium Metal-Organic Frameworks: Topology and Catalytic properties ; loop_ _publ_author_name _publ_author_address 'Angeles Monge' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; 'Natalia Snejko' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; 'Enrique Gutierrez-Puebla' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; 'Caridad Ruiz-Valero' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; 'Marta Iglesias' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; 'Berta Gomez-Lor' ; Instituto de Ciencia de Materiales CSIC Campus de Cantoblanco 28049 MADRID Spain ; #============================================================================== data_in2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C40 H26 In2 N4 O10' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C40 H26 In2 N4 O10' _chemical_formula_weight 952.28 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'In' 'In' -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.1446(6) _cell_length_b 15.4921(8) _cell_length_c 17.2293(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.4690(10) _cell_angle_gamma 90.00 _cell_volume 3450.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1 _cell_measurement_theta_max 30 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.831 _exptl_crystal_density_method ? _exptl_crystal_F_000 1884 _exptl_absorpt_coefficient_mu 1.407 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; The crystal diffracts poorly at higt angles ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22860 _diffrn_reflns_av_R_equivalents 0.0741 _diffrn_reflns_av_sigmaI/netI 0.0901 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.81 _diffrn_reflns_theta_max 31.29 _reflns_number_total 9710 _reflns_number_observed 5954 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens-Bruker SMART' _computing_cell_refinement 'Siemens-Bruker SMART' _computing_data_reduction 'Siemens-Bruker SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or 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 w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9710 _refine_ls_number_parameters 605 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0880 _refine_ls_R_factor_obs 0.0388 _refine_ls_wR_factor_all 0.0885 _refine_ls_wR_factor_obs 0.0745 _refine_ls_goodness_of_fit_all 0.787 _refine_ls_goodness_of_fit_obs 0.861 _refine_ls_restrained_S_all 0.787 _refine_ls_restrained_S_obs 0.861 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group In1 In 0.44020(2) 0.366853(15) 0.097171(13) 0.02054(7) Uani 1 d . . In2 In 0.56010(2) 0.371242(14) -0.107319(13) 0.02024(7) Uani 1 d . . N1 N 0.5944(2) 0.3934(2) 0.1799(2) 0.0291(7) Uani 1 d . . N2 N 0.4135(2) 0.3593(2) 0.2279(2) 0.0268(6) Uani 1 d . . N3 N 0.3953(2) 0.3627(2) -0.1838(2) 0.0285(7) Uani 1 d . . N4 N 0.5679(2) 0.4135(2) -0.2362(2) 0.0280(7) Uani 1 d . . O1 O 0.4946(3) 0.3365(2) -0.0072(2) 0.0298(6) Uani 1 d . . O2 O 0.2760(2) 0.3587(2) 0.0710(2) 0.0375(7) Uani 1 d . . O3 O 0.2548(2) 0.4504(2) -0.0305(2) 0.0429(7) Uani 1 d . . O4 O 0.4579(2) 0.2302(2) 0.1305(2) 0.0323(6) Uani 1 d . . O5 O 0.4011(3) 0.1824(2) 0.0085(2) 0.0558(9) Uani 1 d . . O6 O 0.4662(4) -0.2040(2) 0.2563(2) 0.0746(13) Uani 1 d . . O7 O 0.5715(2) 0.2380(2) -0.1299(2) 0.0404(7) Uani 1 d . . O8 O 0.7233(2) 0.3861(2) -0.0930(2) 0.0423(7) Uani 1 d . . O9 O 0.7371(2) 0.3118(3) 0.0182(2) 0.0637(10) Uani 1 d . . O10 O 0.5519(2) 0.5005(2) -0.0692(2) 0.0354(6) Uani 1 d . . C1 C 0.2198(3) 0.4016(2) 0.0141(2) 0.0286(8) Uani 1 d . . C2 C 0.1053(3) 0.3882(2) 0.0046(2) 0.0294(8) Uani 1 d . . C3 C 0.0424(3) 0.4188(3) -0.0634(2) 0.0334(9) Uani 1 d . . C4 C 0.0600(3) 0.3475(3) 0.0616(2) 0.0330(9) Uani 1 d . . C5 C 0.4266(3) 0.1708(2) 0.0801(2) 0.0277(8) Uani 1 d . . C6 C 0.4267(3) 0.0796(2) 0.1116(2) 0.0260(8) Uani 1 d . . C7 C 0.4078(3) 0.0135(2) 0.0568(2) 0.0341(9) Uani 1 d . . C8 C 0.4128(3) -0.0718(2) 0.0820(2) 0.0348(9) Uani 1 d . . C9 C 0.4347(3) -0.0918(2) 0.1620(2) 0.0253(7) Uani 1 d . . C10 C 0.4498(3) -0.0246(2) 0.2170(2) 0.0297(8) Uani 1 d . . C11 C 0.4467(3) 0.0614(2) 0.1914(2) 0.0306(8) Uani 1 d . . C12 C 0.4460(3) -0.1856(2) 0.1879(2) 0.0288(8) Uani 1 d . . C13 C 0.6809(4) 0.4154(3) 0.1556(3) 0.0453(11) Uani 1 d . . C14 C 0.7741(4) 0.4245(4) 0.2080(4) 0.063(2) Uani 1 d . . C15 C 0.7782(4) 0.4109(4) 0.2863(3) 0.0571(14) Uani 1 d . . C16 C 0.6878(4) 0.3872(3) 0.3138(2) 0.0412(10) Uani 1 d . . C17 C 0.6853(5) 0.3657(3) 0.3947(3) 0.0547(14) Uani 1 d . . C18 C 0.5983(5) 0.3401(3) 0.4170(3) 0.0546(13) Uani 1 d . . C19 C 0.5021(4) 0.3369(3) 0.3621(2) 0.0405(10) Uani 1 d . . C20 C 0.4083(4) 0.3109(3) 0.3824(3) 0.0527(13) Uani 1 d . . C21 C 0.3203(4) 0.3096(3) 0.3262(3) 0.0505(12) Uani 1 d . . C22 C 0.3257(4) 0.3348(3) 0.2493(3) 0.0408(10) Uani 1 d . . C23 C 0.5011(3) 0.3586(2) 0.2829(2) 0.0268(7) Uani 1 d . . C24 C 0.5962(3) 0.3811(2) 0.2576(2) 0.0273(8) Uani 1 d . . C25 C 0.7754(3) 0.3530(3) -0.0299(3) 0.0390(10) Uani 1 d . . C26 C 0.8908(3) 0.3681(3) -0.0171(2) 0.0333(8) Uani 1 d . . C27 C 0.9541(3) 0.3384(3) 0.0515(2) 0.0351(9) Uani 1 d . . C28 C 0.9368(3) 0.4085(3) -0.0734(3) 0.0369(10) Uani 1 d . . C29 C 0.3118(3) 0.3364(3) -0.1576(3) 0.0390(10) Uani 1 d . . C30 C 0.2169(4) 0.3240(3) -0.2076(4) 0.0518(13) Uani 1 d . . C31 C 0.2095(4) 0.3368(3) -0.2861(4) 0.060(2) Uani 1 d . . C32 C 0.2961(4) 0.3634(3) -0.3165(3) 0.0454(11) Uani 1 d . . C33 C 0.2948(5) 0.3783(3) -0.3992(3) 0.063(2) Uani 1 d . . C34 C 0.3785(6) 0.4043(4) -0.4237(3) 0.070(2) Uani 1 d . . C35 C 0.4761(4) 0.4188(3) -0.3709(2) 0.0464(11) Uani 1 d . . C36 C 0.5681(5) 0.4431(4) -0.3946(3) 0.061(2) Uani 1 d . . C37 C 0.6574(5) 0.4534(4) -0.3404(3) 0.0573(14) Uani 1 d . . C38 C 0.6530(4) 0.4369(3) -0.2611(3) 0.0449(11) Uani 1 d . . C39 C 0.4806(3) 0.4038(2) -0.2896(2) 0.0303(8) Uani 1 d . . C40 C 0.3884(3) 0.3764(2) -0.2623(2) 0.0308(8) Uani 1 d . . H4 H 0.0961(30) 0.3255(24) 0.1019(23) 0.024(10) Uiso 1 d . . H11 H 0.4525(27) 0.1027(24) 0.2275(20) 0.019(9) Uiso 1 d . . H10 H 0.4621(27) -0.0386(22) 0.2711(21) 0.021(9) Uiso 1 d . . H18 H 0.5968(31) 0.3182(26) 0.4700(25) 0.042(12) Uiso 1 d . . H8 H 0.4019(31) -0.1169(25) 0.0435(23) 0.034(11) Uiso 1 d . . H3 H 0.0714(31) 0.4524(28) -0.0989(23) 0.038(12) Uiso 1 d . . H28 H 0.9058(35) 0.4239(28) -0.1117(26) 0.039(13) Uiso 1 d . . H15 H 0.8454(42) 0.4194(34) 0.3264(31) 0.073(16) Uiso 1 d . . H14 H 0.8299(37) 0.4323(28) 0.1901(26) 0.047(14) Uiso 1 d . . H10 H 0.6021(58) 0.4966(44) -0.0269(48) 0.129(30) Uiso 1 d . . H21 H 0.2638(38) 0.2888(29) 0.3396(27) 0.053(14) Uiso 1 d . . H22 H 0.2706(32) 0.3284(26) 0.2074(24) 0.036(11) Uiso 1 d . . H100 H 0.4874(40) 0.2983(30) -0.0130(29) 0.048(18) Uiso 1 d . . H17 H 0.7412(53) 0.3671(39) 0.4321(38) 0.102(23) Uiso 1 d . . H38 H 0.7054(34) 0.4493(27) -0.2229(25) 0.037(12) Uiso 1 d . . H37 H 0.7207(38) 0.4747(28) -0.3576(28) 0.052(14) Uiso 1 d . . H29 H 0.3190(32) 0.3212(27) -0.1090(24) 0.039(13) Uiso 1 d . . H13 H 0.6718(34) 0.4243(29) 0.1059(26) 0.045(14) Uiso 1 d . . H20 H 0.4032(38) 0.2992(33) 0.4312(30) 0.068(16) Uiso 1 d . . H31 H 0.1532(40) 0.3241(34) -0.3187(30) 0.065(16) Uiso 1 d . . H7 H 0.3971(31) 0.0248(24) 0.0063(26) 0.032(11) Uiso 1 d . . H27 H 0.9266(31) 0.3061(27) 0.0871(24) 0.040(12) Uiso 1 d . . H30 H 0.1630(40) 0.3076(32) -0.1847(29) 0.065(16) Uiso 1 d . . H34 H 0.3771(44) 0.4200(35) -0.4712(34) 0.074(18) Uiso 1 d . . H36 H 0.5694(46) 0.4441(41) -0.4478(37) 0.097(21) Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 In1 0.02023(14) 0.01805(13) 0.02316(12) 0.00228(10) 0.00347(9) -0.00076(10) In2 0.02198(14) 0.01632(12) 0.02230(12) 0.00025(10) 0.00366(9) -0.00018(10) N1 0.024(2) 0.031(2) 0.032(2) -0.0002(13) 0.0039(13) -0.0034(13) N2 0.026(2) 0.028(2) 0.0284(15) 0.0038(13) 0.0084(12) -0.0019(12) N3 0.027(2) 0.024(2) 0.034(2) -0.0030(13) 0.0041(13) -0.0029(13) N4 0.030(2) 0.023(2) 0.032(2) 0.0016(12) 0.0090(14) 0.0021(12) O1 0.044(2) 0.0182(12) 0.0300(14) 0.0002(12) 0.0144(12) -0.0041(14) O2 0.0191(14) 0.046(2) 0.046(2) 0.0140(13) 0.0002(12) 0.0001(12) O3 0.028(2) 0.057(2) 0.042(2) 0.0127(14) 0.0021(13) -0.0073(13) O4 0.044(2) 0.0183(13) 0.0327(14) 0.0019(10) 0.0023(12) -0.0002(11) O5 0.086(3) 0.031(2) 0.040(2) 0.0115(13) -0.016(2) -0.024(2) O6 0.163(4) 0.025(2) 0.032(2) 0.0059(13) 0.008(2) 0.010(2) O7 0.063(2) 0.0185(13) 0.039(2) -0.0064(11) 0.0058(14) 0.0035(12) O8 0.024(2) 0.047(2) 0.051(2) -0.0034(14) -0.0040(13) 0.0050(12) O9 0.030(2) 0.099(3) 0.063(2) 0.007(2) 0.009(2) -0.015(2) O10 0.059(2) 0.0167(11) 0.0330(15) 0.0012(11) 0.0158(14) 0.0011(14) C1 0.021(2) 0.031(2) 0.033(2) -0.002(2) 0.004(2) 0.001(2) C2 0.023(2) 0.030(2) 0.034(2) -0.002(2) 0.002(2) 0.0013(15) C3 0.031(2) 0.035(2) 0.033(2) 0.004(2) 0.004(2) -0.001(2) C4 0.025(2) 0.043(2) 0.029(2) 0.004(2) 0.000(2) 0.001(2) C5 0.026(2) 0.022(2) 0.033(2) 0.0035(15) 0.002(2) -0.0042(14) C6 0.027(2) 0.019(2) 0.031(2) 0.0041(14) 0.004(2) -0.0021(14) C7 0.047(2) 0.029(2) 0.024(2) 0.004(2) -0.001(2) -0.003(2) C8 0.052(3) 0.018(2) 0.031(2) -0.004(2) -0.003(2) 0.000(2) C9 0.029(2) 0.020(2) 0.027(2) -0.0015(14) 0.0043(15) 0.0003(14) C10 0.044(2) 0.021(2) 0.023(2) -0.0019(14) 0.004(2) 0.0007(15) C11 0.042(2) 0.018(2) 0.031(2) -0.0039(15) 0.003(2) 0.000(2) C12 0.036(2) 0.020(2) 0.030(2) 0.0015(15) 0.007(2) 0.0038(15) C13 0.035(3) 0.061(3) 0.042(3) -0.004(2) 0.013(2) -0.013(2) C14 0.030(3) 0.087(4) 0.075(4) -0.015(3) 0.014(3) -0.017(3) C15 0.024(2) 0.073(4) 0.067(4) -0.013(3) -0.011(2) -0.010(2) C16 0.043(3) 0.038(2) 0.038(2) -0.007(2) -0.006(2) 0.003(2) C17 0.059(4) 0.057(3) 0.039(2) -0.003(2) -0.016(2) 0.002(3) C18 0.081(4) 0.052(3) 0.027(2) 0.007(2) -0.002(2) 0.005(3) C19 0.061(3) 0.031(2) 0.030(2) 0.002(2) 0.007(2) 0.003(2) C20 0.079(4) 0.045(3) 0.041(3) 0.010(2) 0.031(3) -0.003(2) C21 0.052(3) 0.055(3) 0.051(3) 0.007(2) 0.026(3) -0.011(2) C22 0.034(2) 0.045(3) 0.046(3) 0.005(2) 0.014(2) -0.005(2) C23 0.032(2) 0.022(2) 0.026(2) 0.0019(14) 0.0039(14) 0.0007(14) C24 0.031(2) 0.020(2) 0.028(2) -0.0009(14) -0.0018(15) 0.0029(14) C25 0.025(2) 0.043(2) 0.048(2) -0.012(2) 0.004(2) 0.004(2) C26 0.023(2) 0.038(2) 0.039(2) -0.006(2) 0.005(2) 0.003(2) C27 0.026(2) 0.044(2) 0.035(2) 0.002(2) 0.005(2) -0.005(2) C28 0.029(2) 0.042(2) 0.035(2) 0.005(2) -0.006(2) 0.004(2) C29 0.032(2) 0.038(2) 0.048(3) -0.003(2) 0.010(2) -0.005(2) C30 0.025(2) 0.043(3) 0.083(4) -0.002(3) -0.002(2) -0.008(2) C31 0.039(3) 0.045(3) 0.084(4) 0.008(3) -0.025(3) -0.007(2) C32 0.038(3) 0.037(2) 0.051(3) 0.003(2) -0.019(2) 0.000(2) C33 0.070(4) 0.059(4) 0.048(3) 0.008(3) -0.022(3) -0.005(3) C34 0.116(6) 0.057(3) 0.027(3) 0.006(2) -0.012(3) 0.007(3) C35 0.072(3) 0.034(2) 0.032(2) 0.002(2) 0.005(2) 0.007(2) C36 0.095(5) 0.062(3) 0.033(3) 0.011(2) 0.027(3) 0.014(3) C37 0.063(4) 0.064(3) 0.056(3) 0.016(3) 0.037(3) 0.007(3) C38 0.041(3) 0.049(3) 0.049(3) 0.010(2) 0.018(2) 0.001(2) C39 0.040(2) 0.023(2) 0.026(2) 0.0012(14) 0.001(2) 0.005(2) C40 0.034(2) 0.021(2) 0.033(2) 0.000(2) -0.005(2) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag In1 O1 2.105(3) . ? In1 O10 2.118(3) 3_665 ? In1 O2 2.127(3) . ? In1 O4 2.195(2) . ? In1 N1 2.293(3) . ? In1 N2 2.345(3) . ? In2 O7 2.111(3) . ? In2 O10 2.116(3) . ? In2 O8 2.127(3) . ? In2 O1 2.132(3) . ? In2 N3 2.326(3) . ? In2 N4 2.336(3) . ? N1 C13 1.326(5) . ? N1 C24 1.348(4) . ? N2 C22 1.329(5) . ? N2 C23 1.352(5) . ? N3 C29 1.324(5) . ? N3 C40 1.356(5) . ? N4 C38 1.320(5) . ? N4 C39 1.342(5) . ? O2 C1 1.298(4) . ? O3 C1 1.224(4) . ? O4 C5 1.281(4) . ? O5 C5 1.231(4) . ? O6 C12 1.195(4) . ? O7 C12 1.276(4) 3_655 ? O8 C25 1.282(5) . ? O9 C25 1.225(5) . ? O10 In1 2.118(3) 3_665 ? C1 C2 1.499(5) . ? C2 C4 1.388(5) . ? C2 C3 1.390(5) . ? C3 C28 1.376(6) 1_455 ? C4 C27 1.379(5) 1_455 ? C5 C6 1.514(5) . ? C6 C11 1.381(5) . ? C6 C7 1.383(5) . ? C7 C8 1.389(5) . ? C8 C9 1.391(5) . ? C9 C10 1.398(5) . ? C9 C12 1.519(5) . ? C10 C11 1.402(5) . ? C12 O7 1.276(4) 3_655 ? C13 C14 1.390(7) . ? C14 C15 1.357(8) . ? C15 C16 1.406(7) . ? C16 C24 1.405(6) . ? C16 C17 1.440(6) . ? C17 C18 1.330(8) . ? C18 C19 1.436(7) . ? C19 C20 1.400(7) . ? C19 C23 1.403(5) . ? C20 C21 1.368(7) . ? C21 C22 1.395(6) . ? C23 C24 1.440(5) . ? C25 C26 1.510(6) . ? C26 C28 1.383(6) . ? C26 C27 1.394(6) . ? C27 C4 1.379(5) 1_655 ? C28 C3 1.376(6) 1_655 ? C29 C30 1.395(6) . ? C30 C31 1.354(8) . ? C31 C32 1.399(7) . ? C32 C40 1.405(6) . ? C32 C33 1.440(7) . ? C33 C34 1.312(9) . ? C34 C35 1.449(8) . ? C35 C36 1.396(7) . ? C35 C39 1.410(5) . ? C36 C37 1.370(8) . ? C37 C38 1.401(7) . ? C39 C40 1.441(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 In1 O10 89.06(11) . 3_665 ? O1 In1 O2 107.12(12) . . ? O10 In1 O2 95.67(11) 3_665 . ? O1 In1 O4 88.41(10) . . ? O10 In1 O4 171.26(11) 3_665 . ? O2 In1 O4 93.07(10) . . ? O1 In1 N1 99.89(12) . . ? O10 In1 N1 83.88(12) 3_665 . ? O2 In1 N1 152.98(11) . . ? O4 In1 N1 88.32(11) . . ? O1 In1 N2 160.53(11) . . ? O10 In1 N2 106.80(11) 3_665 . ? O2 In1 N2 82.99(11) . . ? O4 In1 N2 74.21(10) . . ? N1 In1 N2 71.43(11) . . ? O7 In2 O10 172.63(10) . . ? O7 In2 O8 91.35(11) . . ? O10 In2 O8 88.20(11) . . ? O7 In2 O1 87.42(11) . . ? O10 In2 O1 86.35(11) . . ? O8 In2 O1 118.75(12) . . ? O7 In2 N3 85.98(11) . . ? O10 In2 N3 97.77(11) . . ? O8 In2 N3 152.60(11) . . ? O1 In2 N3 88.41(11) . . ? O7 In2 N4 94.70(11) . . ? O10 In2 N4 92.52(11) . . ? O8 In2 N4 82.07(11) . . ? O1 In2 N4 159.07(12) . . ? N3 In2 N4 71.01(11) . . ? C13 N1 C24 119.2(4) . . ? C13 N1 In1 124.2(3) . . ? C24 N1 In1 116.5(2) . . ? C22 N2 C23 118.4(3) . . ? C22 N2 In1 124.7(3) . . ? C23 N2 In1 114.6(2) . . ? C29 N3 C40 118.6(4) . . ? C29 N3 In2 124.7(3) . . ? C40 N3 In2 116.2(2) . . ? C38 N4 C39 118.5(4) . . ? C38 N4 In2 124.9(3) . . ? C39 N4 In2 116.1(2) . . ? In1 O1 In2 152.2(2) . . ? C1 O2 In1 123.1(2) . . ? C5 O4 In1 120.6(2) . . ? C12 O7 In2 139.3(3) 3_655 . ? C25 O8 In2 115.2(3) . . ? In2 O10 In1 147.13(15) . 3_665 ? O3 C1 O2 124.2(3) . . ? O3 C1 C2 120.1(3) . . ? O2 C1 C2 115.7(3) . . ? C4 C2 C3 119.0(4) . . ? C4 C2 C1 122.5(3) . . ? C3 C2 C1 118.5(3) . . ? C28 C3 C2 119.8(4) 1_455 . ? C27 C4 C2 120.7(4) 1_455 . ? O5 C5 O4 124.8(3) . . ? O5 C5 C6 118.6(3) . . ? O4 C5 C6 116.6(3) . . ? C11 C6 C7 120.4(3) . . ? C11 C6 C5 122.3(3) . . ? C7 C6 C5 117.2(3) . . ? C6 C7 C8 119.9(4) . . ? C7 C8 C9 120.7(3) . . ? C8 C9 C10 119.0(3) . . ? C8 C9 C12 119.7(3) . . ? C10 C9 C12 121.2(3) . . ? C9 C10 C11 120.2(3) . . ? C6 C11 C10 119.7(3) . . ? O6 C12 O7 126.6(3) . 3_655 ? O6 C12 C9 120.7(3) . . ? O7 C12 C9 112.6(3) 3_655 . ? N1 C13 C14 121.8(5) . . ? C15 C14 C13 120.1(5) . . ? C14 C15 C16 119.5(4) . . ? C24 C16 C15 117.2(4) . . ? C24 C16 C17 119.0(4) . . ? C15 C16 C17 123.8(4) . . ? C18 C17 C16 121.4(5) . . ? C17 C18 C19 121.4(4) . . ? C20 C19 C23 117.4(4) . . ? C20 C19 C18 123.7(4) . . ? C23 C19 C18 118.9(4) . . ? C21 C20 C19 119.8(4) . . ? C20 C21 C22 119.1(4) . . ? N2 C22 C21 122.7(4) . . ? N2 C23 C19 122.6(3) . . ? N2 C23 C24 117.5(3) . . ? C19 C23 C24 119.9(4) . . ? N1 C24 C16 122.2(4) . . ? N1 C24 C23 118.4(3) . . ? C16 C24 C23 119.3(3) . . ? O9 C25 O8 124.2(4) . . ? O9 C25 C26 120.4(4) . . ? O8 C25 C26 115.4(4) . . ? C28 C26 C27 118.3(4) . . ? C28 C26 C25 121.5(4) . . ? C27 C26 C25 120.1(4) . . ? C4 C27 C26 120.4(4) 1_655 . ? C3 C28 C26 121.7(4) 1_655 . ? N3 C29 C30 122.4(5) . . ? C31 C30 C29 119.4(5) . . ? C30 C31 C32 120.1(5) . . ? C31 C32 C40 117.2(4) . . ? C31 C32 C33 123.5(5) . . ? C40 C32 C33 119.3(5) . . ? C34 C33 C32 120.5(5) . . ? C33 C34 C35 123.0(5) . . ? C36 C35 C39 117.0(5) . . ? C36 C35 C34 124.9(5) . . ? C39 C35 C34 118.0(5) . . ? C37 C36 C35 120.8(4) . . ? C36 C37 C38 117.5(5) . . ? N4 C38 C37 123.6(5) . . ? N4 C39 C35 122.5(4) . . ? N4 C39 C40 118.3(3) . . ? C35 C39 C40 119.2(4) . . ? N3 C40 C32 122.2(4) . . ? N3 C40 C39 117.7(3) . . ? C32 C40 C39 120.0(4) . . ? _refine_diff_density_max 0.596 _refine_diff_density_min -1.040 _refine_diff_density_rms 0.122