# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2003 data_CRYSTALS_cif _audit_creation_date 03-06-16 _audit_creation_method CRYSTALS _publ_contact_author ; 'Dr. B. Hasenknopf, Laboratoire de Chimie Inorganique et Materiaux Moleculaires, CNRS UMR7071, Universite Pierre et Marie Curie, case 42, 4 place Jussieu, 75252 Paris cedex 05, France.' ; _publ_contact_author_phone ' 33 1 44 27 30 34' _publ_contact_author_fax ' 33 1 44 27 38 41' _publ_contact_author_email ' hasen@ccr.jussieu.fr ' _publ_requested_journal ' Chem. Comm.' _publ_requested_coeditor_name ' ? ' _publ_contact_letter ; ; _publ_section_title ; Assembly of polyoxometalates into an anisotropic gel ; loop_ _publ_author_name _publ_author_address 'Favette, Sophie' ; 'Laboratoire de Chimie Inorganique et Materiaux Moleculaires, CNRS UMR7071, Universite Pierre et Marie Curie, case 42, 4 place Jussieu, 75252 Paris cedex 05, France.' ; 'Hasenknopf, Bernold' ; 'Laboratoire de Chimie Inorganique et Materiaux Moleculaires, CNRS UMR7071, Universite Pierre et Marie Curie, case 42, 4 place Jussieu, 75252 Paris cedex 05, France.' ; 'Vaissermann, Jacqueline' ; 'Laboratoire de Chimie Inorganique et Materiaux Moleculaires, CNRS UMR7071, Universite Pierre et Marie Curie, case 42, 4 place Jussieu, 75252 Paris cedex 05, France.' ; 'Gouzerh, Pierre' ; 'Laboratoire de Chimie Inorganique et Materiaux Moleculaires, CNRS UMR7071, Universite Pierre et Marie Curie, case 42, 4 place Jussieu, 75252 Paris cedex 05, France.' ; 'Roux, Cecile' ; 'Laboratoire de la Matiere Condensee, CNRS UMR 7574, Universite Pierre et Marie Curie, case 174, 4 place Jussieu, 75252 Paris cedex 05, France. ; #============================================================================== _computing_data_collection 'CAD-4 software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 software (Enraf-Nonius, 1989)' _computing_data_reduction ; RC93 (Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. 1994) ; _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; # _computing_structure_solution 'SHELXS86 (Sheldrick, 1986)' _chemical_melting_point ? _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Enraf-nonius CAD4 ' _refine_ls_matrix_type 'full' _refine_ls_weighting_scheme ; Chebychev polynomial (Carruthers & Watkin, 1979) ; _atom_sites_solution_primary 'Direct_Methods' _atom_sites_solution_hydrogens 'Geometric' _refine_ls_hydrogen_treatment ; H atoms of the polyanion placed geometrically after each cycle. ; #**************************************************************************** _chemical_name_systematic ; # IUPAC name, in full ? ; _cell_length_a 34.272(20) _cell_angle_alpha 90 _cell_length_b 14.094(4) _cell_angle_beta 125.51(5) _cell_length_c 24.568(15) _cell_angle_gamma 90 _cell_volume 961(10) _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'C 1 2/c 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 'x+1/2,y+1/2,z' '-x+1/2,-y+1/2,-z' '-x,y,-z+1/2' 'x,-y,z+1/2' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' 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 ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'N ' 0.0040 0.0030 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International_Tables_Vol_IV_Table_2.2B' 'Mo ' -1.8250 0.6880 3.7025 0.2772 17.2356 1.0958 12.8876 11.0040 3.7429 61.6584 4.3875 'International_Tables_Vol_IV_Table_2.2B' 'Mn ' 0.2950 0.7290 11.2819 5.3409 7.3573 0.3432 3.0193 17.8674 2.2441 83.7543 1.0896 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum ' C76 H140 Mn1 Mo6 N11 O26 ' _chemical_formula_moiety ' C20 H20 Mn1 Mo6 N4 O26 3-, (C16 H36 N1 1+)3, (C2 H3 N1)4 ' _chemical_compound_source ; ? ; _chemical_formula_weight 2254.6 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.8 _cell_measurement_theta_max 15.2 _cell_measurement_temperature 210 _cell_formula_units_Z 4 _exptl_crystal_description 'box' _exptl_crystal_colour 'orange ' _exptl_crystal_size_min 0.5 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_max 0.4 _exptl_crystal_density_diffrn 1.55 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 4632 _exptl_absorpt_coefficient_mu 0.93 _exptl_absorpt_correction_type 'DIFABS' _exptl_absorpt_process_details 'refined from delta-F' _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 1.00 _diffrn_standards_interval_time 3600 _diffrn_standards_interval_count ? _diffrn_standards_number 2 _diffrn_standards_decay_% 16 _diffrn_ambient_temperature 210 _diffrn_reflns_number 9085 _reflns_number_total 8482 _diffrn_reflns_av_R_equivalents 0.02 _reflns_number_observed 6316 _diffrn_reflns_theta_min 1 _diffrn_reflns_theta_max 28 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _reflns_limit_h_min -40 _reflns_limit_h_max 33 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 29 _reflns_observed_criterion >3.00\s(I) _refine_diff_density_min -0.60 _refine_diff_density_max 0.66 _refine_ls_number_reflns 6316 _refine_ls_number_parameters 562 _refine_ls_R_factor_obs 0.0411 _refine_ls_wR_factor_obs 0.0488 _refine_ls_goodness_of_fit_obs 1.033 _refine_ls_shift/esd_max 0.150585 _refine_ls_structure_factor_coef 'F' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method 2\q/\w loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type MO1 0.15702(1) 0.15842(3) 0.49211(2) 0.0328 1.0000 Uani MO2 0.23623(1) 0.29412(3) 0.62283(2) 0.0324 1.0000 Uani MO3 0.17169(1) 0.10936(3) 0.37073(2) 0.0316 1.0000 Uani MN1 0.2500 0.2500 0.5000 0.0263 1.0000 Uani O1 0.0869(1) 0.4463(3) 0.3299(2) 0.0535 1.0000 Uani O10 0.1107(1) 0.2152(3) 0.4847(2) 0.0470 1.0000 Uani O11 0.1478(1) 0.0411(2) 0.4973(2) 0.0469 1.0000 Uani O12 0.2084(1) 0.1733(2) 0.5849(1) 0.0338 1.0000 Uani O13 0.1386(1) 0.1698(2) 0.4024(1) 0.0341 1.0000 Uani O20 0.2743(1) 0.2615(3) 0.7046(2) 0.0450 1.0000 Uani O21 0.1904(1) 0.3525(3) 0.6169(2) 0.0462 1.0000 Uani O23 0.2681(1) 0.4016(2) 0.6173(1) 0.0340 1.0000 Uani O30 0.1338(1) 0.1354(3) 0.2878(2) 0.0442 1.0000 Uani O31 0.1625(1) -0.0064(2) 0.3774(2) 0.0463 1.0000 Uani O112 0.1965(1) 0.2989(2) 0.5052(1) 0.0334 1.0000 Uani O113 0.2752(1) 0.3754(2) 0.5103(1) 0.0302 1.0000 Uani O123 0.20878(9) 0.2589(2) 0.4003(1) 0.0309 1.0000 Uani N1 0.1630(1) 0.5040(2) 0.3892(2) 0.0330 1.0000 Uani N2 0.0587(2) 0.7752(4) 0.2363(3) 0.0664 1.0000 Uani C1 0.1893(1) 0.4154(3) 0.4247(2) 0.0304 1.0000 Uani C2 0.1812(2) 0.3442(3) 0.3719(2) 0.0374 1.0000 Uani C3 0.2417(2) 0.4490(3) 0.4693(2) 0.0348 1.0000 Uani C4 0.1717(1) 0.3823(3) 0.4662(2) 0.0339 1.0000 Uani C5 0.1146(2) 0.5109(3) 0.3435(2) 0.0409 1.0000 Uani C6 0.0968(2) 0.6052(4) 0.3079(3) 0.0436 1.0000 Uani C7 0.1230(2) 0.6882(4) 0.3285(3) 0.0550 1.0000 Uani C8 0.1022(2) 0.7705(4) 0.2918(3) 0.0607 1.0000 Uani C9 0.0343(2) 0.6939(6) 0.2168(4) 0.0707 1.0000 Uani C10 0.0509(2) 0.6083(4) 0.2503(3) 0.0574 1.0000 Uani N10 0.6737(2) 0.4752(4) 0.1858(2) 0.0563 1.0000 Uani C11 0.6399(2) 0.4010(5) 0.1337(3) 0.0642 1.0000 Uani C12 0.5942(3) 0.3863(8) 0.1311(4) 0.0880 1.0000 Uani C13 0.5634(4) 0.310(1) 0.0777(6) 0.1116 1.0000 Uani C14 0.5808(7) 0.220(1) 0.100(1) 0.1792 1.0000 Uani C15 0.6910(2) 0.4451(5) 0.2554(3) 0.0598 1.0000 Uani C16 0.7146(4) 0.3481(5) 0.2763(4) 0.0820 1.0000 Uani C17 0.7359(3) 0.3305(6) 0.3496(4) 0.0912 1.0000 Uani C18 0.7817(3) 0.3851(6) 0.3965(5) 0.0958 1.0000 Uani C19 0.7156(2) 0.4834(5) 0.1795(3) 0.0578 1.0000 Uani C20 0.7520(3) 0.5600(6) 0.2245(4) 0.0753 1.0000 Uani C21 0.7965(3) 0.5486(8) 0.2252(5) 0.0844 1.0000 Uani C221 0.8277(5) 0.487(1) 0.2688(6) 0.0631 0.5000 Uani C222 0.8435(8) 0.584(1) 0.281(1) 0.1058 0.5000 Uani C23 0.6496(3) 0.5716(5) 0.1741(3) 0.0722 1.0000 Uani C24 0.6298(4) 0.6152(7) 0.1055(5) 0.1058 1.0000 Uani C25 0.5979(7) 0.7012(9) 0.0942(8) 0.1325 1.0000 Uani C261 0.584(1) 0.759(2) 0.043(2) 0.1569 0.5000 Uani C262 0.628(1) 0.774(3) 0.128(2) 0.1499 0.5000 Uani N20 0.0000 0.1771(6) 0.2500 0.0698 1.0000 Uani C27 -0.0358(2) 0.2392(5) 0.2508(4) 0.0733 1.0000 Uani C28 -0.0140(3) 0.3047(6) 0.3110(4) 0.0839 1.0000 Uani C29 -0.0533(3) 0.3464(8) 0.3131(4) 0.0961 1.0000 Uani C30 -0.0329(4) 0.4096(9) 0.3753(5) 0.1239 1.0000 Uani C31 -0.0287(3) 0.1146(6) 0.1868(6) 0.0907 1.0000 Uani C32 0.0027(3) 0.056(1) 0.1735(8) 0.1308 1.0000 Uani C33 -0.0271(4) -0.004(1) 0.1063(9) 0.1314 1.0000 Uani C34 -0.0466(5) -0.080(1) 0.1229(9) 0.1669 1.0000 Uani N100 0.4128(4) 0.1144(9) 0.0587(6) 0.1549 1.0000 Uani C100 0.4115(3) 0.0498(9) 0.0286(5) 0.1055 1.0000 Uani C101 0.4073(3) -0.0305(7) -0.0100(5) 0.1002 1.0000 Uani N200 0.2432(4) 0.3347(7) -0.0513(6) 0.1304 1.0000 Uani C200 0.2866(5) 0.3308(6) -0.0179(6) 0.0977 1.0000 Uani C201 0.3349(3) 0.3259(6) 0.0231(4) 0.0877 1.0000 Uani H21 0.1902 0.3751 0.3437 0.0296 1.0000 Uiso H22 0.1463 0.3270 0.3424 0.0296 1.0000 Uiso H31 0.2446 0.5010 0.4995 0.0296 1.0000 Uiso H32 0.2508 0.4754 0.4401 0.0296 1.0000 Uiso H41 0.1769 0.4348 0.4975 0.0296 1.0000 Uiso H42 0.1366 0.3680 0.4356 0.0296 1.0000 Uiso H71 0.1573 0.6885 0.3694 0.0610 1.0000 Uiso H81 0.1218 0.8312 0.3090 0.0527 1.0000 Uiso H91 0.0010 0.6950 0.1741 0.0556 1.0000 Uiso H101 0.0299 0.5495 0.2331 0.0722 1.0000 Uiso 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 MO1 0.0318(2) 0.0351(2) 0.0343(2) -0.0018(2) 0.0200(2) -0.0057(2) MO2 0.0363(2) 0.0332(2) 0.0316(2) -0.0029(1) 0.0215(2) -0.0015(2) MO3 0.0296(2) 0.0314(2) 0.0315(2) -0.0050(1) 0.0158(2) -0.0027(1) MN1 0.0265(4) 0.0249(4) 0.0268(4) -0.0003(3) 0.0150(3) -0.0004(3) O1 0.041(2) 0.039(2) 0.072(2) 0.009(2) 0.017(2) 0.002(2) O10 0.040(2) 0.059(2) 0.052(2) -0.004(2) 0.030(2) -0.003(2) O11 0.055(2) 0.041(2) 0.053(2) -0.003(2) 0.034(2) -0.009(2) O12 0.040(2) 0.033(2) 0.033(1) 0.000(1) 0.022(1) -0.006(1) O13 0.029(1) 0.038(2) 0.032(1) -0.001(1) 0.015(1) -0.000(1) O20 0.049(2) 0.048(2) 0.035(2) 0.000(1) 0.022(1) 0.002(2) O21 0.047(2) 0.048(2) 0.051(2) -0.003(2) 0.032(2) 0.002(2) O23 0.035(1) 0.032(2) 0.037(2) -0.006(1) 0.021(1) 0.001(1) O30 0.038(2) 0.060(2) 0.034(2) -0.003(1) 0.017(1) 0.007(2) O31 0.048(2) 0.036(2) 0.063(2) -0.009(2) 0.034(2) -0.004(2) O112 0.036(2) 0.030(2) 0.032(1) 0.001(1) 0.018(1) 0.002(1) O113 0.029(1) 0.028(1) 0.033(1) 0.001(1) 0.017(1) -0.000(1) O123 0.029(1) 0.028(1) 0.035(1) 0.004(1) 0.017(1) 0.004(1) N1 0.036(2) 0.024(2) 0.039(2) 0.005(1) 0.017(2) 0.009(1) N2 0.071(3) 0.055(3) 0.085(4) 0.031(3) 0.038(3) 0.023(3) C1 0.032(2) 0.026(2) 0.032(2) 0.005(2) 0.016(2) 0.006(2) C2 0.038(2) 0.035(2) 0.038(2) 0.005(2) 0.020(2) 0.006(2) C3 0.034(2) 0.033(2) 0.036(2) 0.005(2) 0.018(2) 0.005(2) C4 0.033(2) 0.031(2) 0.038(2) 0.004(2) 0.021(2) 0.004(2) C5 0.041(2) 0.033(3) 0.043(2) 0.002(2) 0.019(2) 0.008(2) C6 0.043(3) 0.040(3) 0.051(3) 0.009(2) 0.026(2) 0.011(2) C7 0.058(3) 0.040(3) 0.062(3) 0.008(2) 0.026(3) 0.010(2) C8 0.067(4) 0.039(3) 0.079(4) 0.014(3) 0.035(3) 0.010(3) C9 0.062(4) 0.078(5) 0.075(4) 0.034(4) 0.020(3) 0.030(4) C10 0.050(3) 0.052(3) 0.062(3) 0.016(3) 0.019(3) 0.014(3) N10 0.071(3) 0.066(3) 0.062(3) -0.023(2) 0.047(3) -0.009(3) C11 0.072(4) 0.088(5) 0.072(4) -0.037(4) 0.051(3) -0.030(3) C12 0.088(5) 0.154(9) 0.101(6) -0.062(6) 0.070(5) -0.053(6) C13 0.112(8) 0.19(1) 0.141(9) -0.081(9) 0.090(7) -0.086(9) C14 0.24(2) 0.17(1) 0.30(2) -0.13(2) 0.19(2) -0.08(1) C15 0.084(4) 0.065(4) 0.059(3) -0.017(3) 0.050(3) -0.006(3) C16 0.162(8) 0.047(4) 0.087(5) -0.009(4) 0.079(6) -0.005(4) C17 0.110(6) 0.079(5) 0.077(5) 0.000(4) 0.044(5) -0.011(5) C18 0.107(7) 0.053(4) 0.117(7) 0.015(4) 0.028(5) 0.015(4) C19 0.082(4) 0.063(4) 0.078(4) -0.035(3) 0.061(4) -0.021(3) C20 0.094(5) 0.108(6) 0.114(6) -0.070(5) 0.081(5) -0.049(5) C21 0.100(6) 0.143(8) 0.111(6) -0.068(6) 0.084(6) -0.063(6) C221 0.060(7) 0.077(9) 0.056(7) -0.014(6) 0.032(6) 0.000(7) C222 0.12(1) 0.11(1) 0.14(2) -0.03(1) 0.10(1) -0.02(1) C23 0.095(5) 0.075(4) 0.073(4) -0.008(4) 0.057(4) 0.012(4) C24 0.18(1) 0.104(7) 0.085(6) 0.013(5) 0.081(7) 0.053(7) C25 0.22(2) 0.094(8) 0.13(1) 0.023(8) 0.10(1) 0.05(1) C261 0.15(2) 0.15(2) 0.19(3) -0.00(2) 0.11(2) 0.02(2) C262 0.18(3) 0.18(3) 0.19(3) 0.07(3) 0.14(3) 0.06(2) N20 0.028(3) 0.060(5) 0.134(8) 0.0000 0.008(4) 0.0000 C27 0.040(3) 0.067(4) 0.115(6) 0.003(4) 0.026(3) -0.004(3) C28 0.058(4) 0.081(5) 0.095(5) 0.012(4) 0.022(4) -0.006(4) C29 0.073(5) 0.148(8) 0.078(5) 0.012(5) 0.039(4) -0.008(5) C30 0.115(8) 0.16(1) 0.088(6) 0.014(7) 0.047(6) -0.008(7) C31 0.049(4) 0.071(5) 0.166(9) -0.037(6) 0.010(5) 0.005(4) C32 0.063(5) 0.15(1) 0.27(2) -0.11(1) 0.023(8) 0.016(6) C33 0.065(5) 0.13(1) 0.27(2) -0.08(1) 0.049(8) -0.006(6) C34 0.12(1) 0.15(1) 0.19(1) 0.04(1) -0.01(1) 0.017(9) N100 0.17(1) 0.142(9) 0.16(1) -0.041(8) 0.095(8) -0.010(8) C100 0.092(6) 0.120(8) 0.105(7) -0.010(6) 0.055(5) -0.014(6) C101 0.086(5) 0.107(7) 0.116(7) -0.026(6) 0.058(5) -0.019(5) N200 0.134(8) 0.092(6) 0.21(1) -0.077(7) 0.003(8) 0.035(6) C200 0.15(1) 0.054(5) 0.120(8) -0.025(5) 0.041(7) 0.027(6) C201 0.099(6) 0.065(5) 0.091(5) 0.003(4) 0.045(5) 0.003(4) _refine_ls_extinction_coef 88 _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' 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 MO1 . O10 . 1.692(3) yes MO1 . O11 . 1.703(3) yes MO1 . O12 . 1.919(3) yes MO1 . O13 . 1.913(3) yes MO1 . O112 . 2.312(3) yes MO1 . O113 4_556 2.405(3) yes MO2 . O12 . 1.909(3) yes MO2 . O20 . 1.704(3) yes MO2 . O21 . 1.702(3) yes MO2 . O23 . 1.917(3) yes MO2 . O112 . 2.375(3) yes MO2 . O123 4_556 2.384(3) yes MO3 . O13 . 1.911(3) yes MO3 . O23 4_556 1.915(3) yes MO3 . O30 . 1.702(3) yes MO3 . O31 . 1.688(3) yes MO3 . O113 4_556 2.393(3) yes MO3 . O123 . 2.348(3) yes MN1 . O112 . 2.031(3) yes MN1 . O112 4_556 2.031(3) yes MN1 . O113 . 1.919(3) yes MN1 . O113 4_556 1.919(3) yes MN1 . O123 . 1.997(3) yes MN1 . O123 4_556 1.997(3) yes O1 . C5 . 1.214(6) yes O112 . C4 . 1.441(5) yes O113 . C3 . 1.436(5) yes O123 . C2 . 1.434(5) yes N1 . C1 . 1.489(5) yes N1 . C5 . 1.364(6) yes N2 . C8 . 1.313(8) yes N2 . C9 . 1.333(9) yes C1 . C2 . 1.533(6) yes C1 . C3 . 1.537(6) yes C1 . C4 . 1.528(6) yes C2 . H21 . 1.005 no C2 . H22 . 1.005 no C3 . H31 . 1.007 no C3 . H32 . 1.005 no C4 . H41 . 1.005 no C4 . H42 . 1.002 no C5 . C6 . 1.511(7) yes C6 . C7 . 1.379(8) yes C6 . C10 . 1.377(7) yes C7 . C8 . 1.386(8) yes C7 . H71 . 1.010 no C8 . H81 . 1.016 no C9 . C10 . 1.382(9) yes C9 . H91 . 1.008 no C10 . H101 . 1.015 no N10 . C11 . 1.533(7) yes N10 . C15 . 1.508(8) yes N10 . C19 . 1.534(7) yes N10 . C23 . 1.529(9) yes C11 . C12 . 1.542(9) yes C12 . C13 . 1.54(1) yes C13 . C14 . 1.38(2) yes C15 . C16 . 1.52(1) yes C16 . C17 . 1.52(1) yes C17 . C18 . 1.51(1) yes C19 . C20 . 1.530(9) yes C20 . C21 . 1.52(1) yes C21 . C221 . 1.31(2) yes C21 . C222 . 1.47(2) yes C221 . C222 . 1.44(2) yes C23 . C24 . 1.53(1) yes C24 . C25 . 1.55(2) yes C25 . C261 . 1.33(3) yes C25 . C262 . 1.35(4) yes N20 . C27 . 1.517(9) yes N20 . C27 5_555 1.517(9) yes N20 . C31 . 1.54(1) yes N20 . C31 5_555 1.54(1) yes C27 . C28 . 1.52(1) yes C28 . C29 . 1.50(1) yes C29 . C30 . 1.54(1) yes C31 . C32 . 1.53(2) yes C32 . C33 . 1.60(2) yes C33 . C34 . 1.44(2) yes N100 . C100 . 1.16(1) yes C100 . C101 . 1.43(1) yes N200 . C200 . 1.21(1) yes C200 . C201 . 1.35(1) yes 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 O10 . MO1 . O11 . 105.3(2) no O10 . MO1 . O12 . 103.5(1) no O11 . MO1 . O12 . 95.7(1) no O10 . MO1 . O13 . 100.0(1) no O11 . MO1 . O13 . 102.5(1) no O12 . MO1 . O13 . 145.2(1) no O10 . MO1 . O112 . 92.7(1) no O11 . MO1 . O112 . 160.1(1) no O12 . MO1 . O112 . 71.5(1) no O13 . MO1 . O112 . 82.2(1) no O10 . MO1 . O113 4_556 162.0(1) no O11 . MO1 . O113 4_556 91.9(1) no O12 . MO1 . O113 4_556 79.5(1) no O13 . MO1 . O113 4_556 70.6(1) no O112 . MO1 . O113 4_556 71.2(1) no O12 . MO2 . O20 . 99.1(1) no O12 . MO2 . O21 . 102.4(1) no O20 . MO2 . O21 . 105.5(2) no O12 . MO2 . O23 . 144.5(1) no O20 . MO2 . O23 . 102.7(1) no O21 . MO2 . O23 . 98.4(1) no O12 . MO2 . O112 . 70.1(1) no O20 . MO2 . O112 . 161.3(1) no O21 . MO2 . O112 . 91.9(1) no O23 . MO2 . O112 . 80.8(1) no O12 . MO2 . O123 4_556 81.0(1) no O20 . MO2 . O123 4_556 91.5(1) no O21 . MO2 . O123 4_556 161.6(1) no O23 . MO2 . O123 4_556 70.7(1) no O112 . MO2 . O123 4_556 72.1(1) no O13 . MO3 . O23 4_556 144.7(1) no O13 . MO3 . O30 . 99.9(1) no O23 4_556 MO3 . O30 . 101.9(1) no O13 . MO3 . O31 . 101.7(1) no O23 4_556 MO3 . O31 . 98.8(1) no O30 . MO3 . O31 . 105.6(2) no O13 . MO3 . O113 4_556 70.9(1) no O23 4_556 MO3 . O113 4_556 80.4(1) no O30 . MO3 . O113 4_556 162.4(1) no O31 . MO3 . O113 4_556 91.1(1) no O13 . MO3 . O123 . 79.4(1) no O23 4_556 MO3 . O123 . 71.5(1) no O30 . MO3 . O123 . 94.4(1) no O31 . MO3 . O123 . 159.3(1) no O113 4_556 MO3 . O123 . 69.5(1) no O112 . MN1 . O112 4_556 179.99 no O112 . MN1 . O113 . 91.9(1) no O112 4_556 MN1 . O113 . 88.1(1) no O112 . MN1 . O113 4_556 88.1(1) no O112 4_556 MN1 . O113 4_556 91.9(1) no O113 . MN1 . O113 4_556 179.99 no O112 . MN1 . O123 . 91.9(1) no O112 4_556 MN1 . O123 . 88.1(1) no O113 . MN1 . O123 . 92.7(1) no O113 4_556 MN1 . O123 . 87.3(1) no O112 . MN1 . O123 4_556 88.1(1) no O112 4_556 MN1 . O123 4_556 91.9(1) no O113 . MN1 . O123 4_556 87.3(1) no O113 4_556 MN1 . O123 4_556 92.7(1) no O123 . MN1 . O123 4_556 179.99 no MO1 . O12 . MO2 . 122.1(2) no MO1 . O13 . MO3 . 123.7(1) no MO2 . O23 . MO3 4_556 122.2(2) no MO1 . O112 . MO2 . 91.2(1) no MO1 . O112 . MN1 . 100.2(1) no MO2 . O112 . MN1 . 99.6(1) no MO1 . O112 . C4 . 122.4(2) no MO2 . O112 . C4 . 122.1(2) no MN1 . O112 . C4 . 116.1(2) no MO1 4_556 O113 . MO3 4_556 89.29(9) no MO1 4_556 O113 . MN1 . 100.5(1) no MO3 4_556 O113 . MN1 . 102.0(1) no MO1 4_556 O113 . C3 . 121.1(2) no MO3 4_556 O113 . C3 . 121.5(2) no MN1 . O113 . C3 . 117.2(2) no MO2 4_556 O123 . MO3 . 90.3(1) no MO2 4_556 O123 . MN1 . 100.3(1) no MO3 . O123 . MN1 . 101.1(1) no MO2 4_556 O123 . C2 . 122.3(2) no MO3 . O123 . C2 . 121.1(2) no MN1 . O123 . C2 . 116.5(2) no C1 . N1 . C5 . 125.2(4) no C8 . N2 . C9 . 115.3(5) no N1 . C1 . C2 . 107.6(3) no N1 . C1 . C3 . 102.7(3) no C2 . C1 . C3 . 111.5(3) no N1 . C1 . C4 . 107.9(3) no C2 . C1 . C4 . 114.6(4) no C3 . C1 . C4 . 111.6(3) no O123 . C2 . C1 . 113.1(3) no O123 . C2 . H21 . 108.7 no C1 . C2 . H21 . 108.7 no O123 . C2 . H22 . 108.7 no C1 . C2 . H22 . 108.8 no H21 . C2 . H22 . 108.7 no O113 . C3 . C1 . 113.9(3) no O113 . C3 . H31 . 108.3 no C1 . C3 . H31 . 108.8 no O113 . C3 . H32 . 108.4 no C1 . C3 . H32 . 108.8 no H31 . C3 . H32 . 108.5 no O112 . C4 . C1 . 112.6(3) no O112 . C4 . H41 . 108.5 no C1 . C4 . H41 . 108.9 no O112 . C4 . H42 . 108.8 no C1 . C4 . H42 . 109.1 no H41 . C4 . H42 . 108.9 no O1 . C5 . N1 . 123.7(4) no O1 . C5 . C6 . 120.9(4) no N1 . C5 . C6 . 115.3(4) no C5 . C6 . C7 . 125.2(4) no C5 . C6 . C10 . 117.3(5) no C7 . C6 . C10 . 117.5(5) no C6 . C7 . C8 . 119.5(5) no C6 . C7 . H71 . 120.2 no C8 . C7 . H71 . 120.4 no N2 . C8 . C7 . 124.2(6) no N2 . C8 . H81 . 117.9 no C7 . C8 . H81 . 117.9 no N2 . C9 . C10 . 125.5(6) no N2 . C9 . H91 . 117.1 no C10 . C9 . H91 . 117.4 no C6 . C10 . C9 . 118.0(6) no C6 . C10 . H101 . 120.9 no C9 . C10 . H101 . 121.1 no C11 . N10 . C15 . 111.3(5) no C11 . N10 . C19 . 105.4(4) no C15 . N10 . C19 . 111.1(5) no C11 . N10 . C23 . 112.7(5) no C15 . N10 . C23 . 106.0(4) no C19 . N10 . C23 . 110.5(5) no N10 . C11 . C12 . 112.6(5) no C11 . C12 . C13 . 107.9(6) no C12 . C13 . C14 . 112.2(13) no N10 . C15 . C16 . 114.8(5) no C15 . C16 . C17 . 110.0(6) no C16 . C17 . C18 . 113.0(8) no N10 . C19 . C20 . 113.5(4) no C19 . C20 . C21 . 108.9(5) no C20 . C21 . C221 . 114.5(10) no C20 . C21 . C222 . 121.2(9) no C221 . C21 . C222 . 62.1(11) no C21 . C221 . C222 . 64.3(12) no C21 . C222 . C221 . 53.6(9) no N10 . C23 . C24 . 114.0(5) no C23 . C24 . C25 . 109.0(8) no C24 . C25 . C261 . 118.6(16) no C24 . C25 . C262 . 105.6(19) no C261 . C25 . C262 . 81.1(20) no C27 . N20 . C27 5_555 109.5(7) no C27 . N20 . C31 . 107.1(4) no C27 5_555 N20 . C31 . 111.4(6) no C27 . N20 . C31 5_555 111.4(6) no C27 5_555 N20 . C31 5_555 107.1(4) no C31 . N20 . C31 5_555 110.4(9) no N20 . C27 . C28 . 114.6(5) no C27 . C28 . C29 . 109.1(6) no C28 . C29 . C30 . 111.2(7) no N20 . C31 . C32 . 113.8(6) no C31 . C32 . C33 . 113.6(8) no C32 . C33 . C34 . 103.1(17) no N100 . C100 . C101 . 177.1(12) no N200 . C200 . C201 . 176.1(15) no