Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' # 1. SUBMISSION DETAILS _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jie Zhang' _publ_contact_author_address ; The State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; _publ_contact_author_email zhangjie@fjirsm.ac.cn _publ_contact_author_phone 86-591-83792871 _publ_contact_author_fax 86-591-83710051 _publ_section_title ; [Co5(u3-OH)2(btec)2(bpp)].0.5H2O: A Three-Dimensional Homometallic Molecular Metamagnet Built from the Mixed Hydroxide/Carboxylate-Bridged Ferrimagnetic-like Chains ; _publ_contact_letter ; This CIF will submit for publication as a full paper in 'Dalton Trans.' ; # 2.AUTHOR LIST loop_ _publ_author_name _publ_author_address 'Hong-Peng Jia' ; The State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; 'Wei Li' ; The State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; 'Zhan-Feng Ju' ; The State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; 'Jie Zhang' ; The State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002, P. R. China ; data_1 _database_code_depnum_ccdc_archive 'CCDC 631874' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H20 Co5 N2 O18' _chemical_formula_weight 1027.16 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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.2175(7) _cell_length_b 21.8066(18) _cell_length_c 11.5739(13) _cell_angle_alpha 90.00 _cell_angle_beta 101.632(5) _cell_angle_gamma 90.00 _cell_volume 1784.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4126 _cell_measurement_theta_min 3.0312 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.1200 _exptl_crystal_size_min 0.0800 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.912 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1022 _exptl_absorpt_coefficient_mu 2.361 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6495 _exptl_absorpt_correction_T_max 0.8336 _exptl_absorpt_process_details 'CrystalClear (Rigaku/MSC Inc., 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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_type 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 13936 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4179 _reflns_number_gt 3631 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+3.0777P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4179 _refine_ls_number_parameters 275 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0576 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1122 _refine_ls_wR_factor_gt 0.1063 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.122 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co -0.39946(7) 0.56167(2) 0.84272(4) 0.01641(14) Uani 1 1 d . . . Co2 Co -0.26195(7) 0.56938(2) 1.14373(4) 0.01499(13) Uani 1 1 d . . . Co3 Co 0.0000 0.5000 1.0000 0.01151(15) Uani 1 2 d S . . N1 N -0.2349(6) 0.62095(16) 1.3008(3) 0.0319(8) Uani 1 1 d . . . O1 O 0.3723(4) 0.50522(12) 0.7783(2) 0.0191(5) Uani 1 1 d . . . O2 O 0.3957(4) 0.58432(14) 0.6671(2) 0.0274(6) Uani 1 1 d . . . O3 O -0.0002(4) 0.48196(12) 0.8177(2) 0.0182(5) Uani 1 1 d . . . O4 O -0.2269(4) 0.54637(14) 0.7336(2) 0.0277(7) Uani 1 1 d . . . O5 O -0.2821(3) 0.51791(11) 0.9875(2) 0.0137(5) Uani 1 1 d . . . H5 H -0.3408 0.4840 0.9847 0.016 Uiso 1 1 d R . . O6 O -0.5205(4) 0.63353(12) 0.8980(2) 0.0262(6) Uani 1 1 d . . . O7 O -0.5347(4) 0.60341(12) 1.0806(2) 0.0217(6) Uani 1 1 d . . . O8 O -0.9378(4) 0.59034(11) 0.9732(2) 0.0215(6) Uani 1 1 d . . . O9 O -1.1225(4) 0.63800(12) 1.0773(3) 0.0282(7) Uani 1 1 d . . . C1 C 0.3118(5) 0.53698(17) 0.6847(3) 0.0176(7) Uani 1 1 d . . . C2 C 0.1471(5) 0.51616(17) 0.5941(3) 0.0168(7) Uani 1 1 d . . . C3 C -0.0343(5) 0.50616(17) 0.6141(3) 0.0166(7) Uani 1 1 d . . . C4 C -0.1779(5) 0.49024(18) 0.5202(3) 0.0194(8) Uani 1 1 d . . . H4 H -0.2988 0.4836 0.5340 0.023 Uiso 1 1 calc R . . C5 C -0.0903(5) 0.51240(17) 0.7311(3) 0.0163(7) Uani 1 1 d . . . C6 C -0.5763(5) 0.63847(16) 0.9935(3) 0.0164(7) Uani 1 1 d . . . C7 C -0.6033(7) 0.7500 0.9940(5) 0.0184(10) Uani 1 2 d S . . H7 H -0.4801 0.7500 0.9813 0.022 Uiso 1 2 calc SR . . C8 C -0.6921(5) 0.69463(16) 1.0031(3) 0.0170(7) Uani 1 1 d . . . C9 C -0.8784(5) 0.69459(16) 1.0213(3) 0.0177(7) Uani 1 1 d . . . C10 C -0.9659(8) 0.7500 1.0317(5) 0.0203(11) Uani 1 2 d S . . H10 H -1.0881 0.7500 1.0461 0.024 Uiso 1 2 calc SR . . C11 C -0.9872(5) 0.63582(15) 1.0236(3) 0.0159(7) Uani 1 1 d . . . C12 C -0.0697(9) 0.6425(3) 1.3565(5) 0.0527(14) Uani 1 1 d . . . H12 H 0.0318 0.6413 1.3182 0.063 Uiso 1 1 calc R . . C13 C -0.0409(12) 0.6668(3) 1.4690(6) 0.075(2) Uani 1 1 d . . . H13 H 0.0790 0.6805 1.5049 0.090 Uiso 1 1 calc R . . C14 C -0.1861(14) 0.6711(3) 1.5284(5) 0.074(2) Uani 1 1 d . . . C15 C -0.3587(13) 0.6502(3) 1.4698(6) 0.074(2) Uani 1 1 d . . . H15 H -0.4627 0.6527 1.5057 0.089 Uiso 1 1 calc R . . C16 C -0.3801(9) 0.6253(3) 1.3577(5) 0.0532(15) Uani 1 1 d . . . H16 H -0.4987 0.6112 1.3204 0.064 Uiso 1 1 calc R . . C17 C -0.1510(15) 0.6921(3) 1.6562(6) 0.095(3) Uani 1 1 d U . . H17A H -0.2558 0.6758 1.6861 0.114 Uiso 1 1 d R . . H17B H -0.0412 0.6705 1.6971 0.114 Uiso 1 1 d R . . C18 C -0.020(3) 0.7500 1.6894(16) 0.068(5) Uani 0.50 2 d SPU . 1 H18A H 0.0812 0.7500 1.6455 0.082 Uiso 0.50 2 calc SPR . 1 H18B H 0.0356 0.7500 1.7730 0.082 Uiso 0.50 2 calc SPR . 1 C18' C -0.263(4) 0.7500 1.6772(18) 0.080(6) Uani 0.50 2 d SPU . 2 H18C H -0.3850 0.7500 1.6239 0.096 Uiso 0.50 2 calc SPR . 2 H18D H -0.2835 0.7500 1.7574 0.096 Uiso 0.50 2 calc SPR . 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 Co1 0.0144(3) 0.0202(3) 0.0150(2) -0.00123(18) 0.00364(19) 0.00211(19) Co2 0.0139(3) 0.0151(2) 0.0168(3) -0.00021(18) 0.00506(19) 0.00025(18) Co3 0.0112(3) 0.0110(3) 0.0128(3) -0.0002(2) 0.0036(2) 0.0003(2) N1 0.042(2) 0.0241(18) 0.030(2) -0.0055(14) 0.0071(17) 0.0014(16) O1 0.0144(13) 0.0258(14) 0.0144(12) 0.0047(10) -0.0032(10) -0.0042(11) O2 0.0251(16) 0.0315(16) 0.0234(15) 0.0063(12) -0.0003(12) -0.0056(12) O3 0.0179(13) 0.0236(13) 0.0137(12) 0.0008(10) 0.0046(10) 0.0066(11) O4 0.0237(15) 0.0430(17) 0.0190(14) 0.0077(12) 0.0106(11) 0.0161(13) O5 0.0114(12) 0.0149(12) 0.0144(12) -0.0012(9) 0.0014(9) -0.0003(9) O6 0.0376(17) 0.0203(14) 0.0225(14) 0.0003(11) 0.0105(12) 0.0109(12) O7 0.0188(14) 0.0192(13) 0.0296(15) 0.0069(11) 0.0105(11) 0.0059(11) O8 0.0272(15) 0.0122(12) 0.0286(15) -0.0020(10) 0.0138(12) -0.0013(11) O9 0.0259(15) 0.0150(13) 0.0498(18) -0.0009(12) 0.0223(14) -0.0014(11) C1 0.0148(18) 0.0236(19) 0.0155(17) -0.0003(14) 0.0058(14) -0.0004(14) C2 0.0129(17) 0.0232(18) 0.0138(17) 0.0009(13) 0.0015(13) 0.0011(14) C3 0.0143(17) 0.0228(18) 0.0135(17) 0.0008(13) 0.0043(13) 0.0016(14) C4 0.0118(17) 0.032(2) 0.0136(17) 0.0019(14) 0.0015(13) -0.0012(15) C5 0.0150(17) 0.0212(18) 0.0136(17) 0.0022(13) 0.0050(13) 0.0016(14) C6 0.0137(17) 0.0118(16) 0.0235(19) -0.0020(13) 0.0031(14) -0.0002(13) C7 0.010(2) 0.017(2) 0.030(3) 0.000 0.006(2) 0.000 C8 0.0192(19) 0.0131(17) 0.0183(18) 0.0003(13) 0.0030(14) 0.0005(14) C9 0.0182(18) 0.0113(16) 0.0239(19) -0.0010(13) 0.0050(15) -0.0031(14) C10 0.019(3) 0.017(3) 0.027(3) 0.000 0.010(2) 0.000 C11 0.0125(17) 0.0106(16) 0.0250(19) 0.0034(13) 0.0047(14) 0.0004(13) C12 0.059(4) 0.046(3) 0.049(3) -0.015(3) 0.002(3) -0.010(3) C13 0.116(6) 0.048(4) 0.050(4) -0.020(3) -0.010(4) -0.013(4) C14 0.155(8) 0.032(3) 0.033(3) -0.004(2) 0.016(4) 0.000(4) C15 0.129(7) 0.056(4) 0.052(4) -0.011(3) 0.051(4) 0.007(4) C16 0.071(4) 0.048(3) 0.048(3) -0.010(2) 0.031(3) 0.005(3) C17 0.178(7) 0.054(4) 0.049(4) -0.009(3) 0.015(4) 0.000(5) C18 0.096(10) 0.054(8) 0.046(7) 0.000 -0.004(7) 0.000 C18' 0.117(11) 0.074(9) 0.057(8) 0.000 0.036(8) 0.000 _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 Co1 O6 1.963(3) . ? Co1 O5 1.965(2) . ? Co1 O4 1.973(3) . ? Co1 O1 2.071(3) 1_455 ? Co1 O2 2.313(3) 1_455 ? Co2 O9 2.039(3) 1_655 ? Co2 O7 2.093(3) . ? Co2 O1 2.094(2) 3_567 ? Co2 O5 2.108(2) . ? Co2 N1 2.113(4) . ? Co2 O3 2.166(2) 3_567 ? Co3 O5 2.050(2) . ? Co3 O5 2.050(2) 3_567 ? Co3 O8 2.058(2) 3_467 ? Co3 O8 2.058(2) 1_655 ? Co3 O3 2.145(2) 3_567 ? Co3 O3 2.145(2) . ? N1 C12 1.322(7) . ? N1 C16 1.349(6) . ? O1 C1 1.285(4) . ? O2 C1 1.234(5) . ? O3 C5 1.268(4) . ? O4 C5 1.238(4) . ? O5 H5 0.8499 . ? O6 C6 1.255(4) . ? O7 C6 1.253(4) . ? O8 C11 1.239(4) . ? O9 C11 1.260(4) . ? C1 C2 1.489(5) . ? C2 C4 1.391(5) 3_566 ? C2 C3 1.392(5) . ? C3 C4 1.386(5) . ? C3 C5 1.495(4) . ? C4 C2 1.391(5) 3_566 ? C4 H4 0.9300 . ? C6 C8 1.499(5) . ? C7 C8 1.381(4) . ? C7 C8 1.381(4) 4_575 ? C7 H7 0.9300 . ? C8 C9 1.402(5) . ? C9 C10 1.380(4) . ? C9 C11 1.506(5) . ? C10 C9 1.380(4) 4_575 ? C10 H10 0.9300 . ? C12 C13 1.382(8) . ? C12 H12 0.9300 . ? C13 C14 1.367(11) . ? C13 H13 0.9300 . ? C14 C15 1.371(11) . ? C14 C17 1.520(8) . ? C15 C16 1.386(8) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18' 1.544(15) . ? C17 C18 1.579(15) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C18 C17 1.579(15) 4_575 ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18' C17 1.544(15) 4_575 ? C18' H18C 0.9700 . ? C18' H18D 0.9700 . ? 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 O6 Co1 O5 104.67(10) . . ? O6 Co1 O4 136.35(12) . . ? O5 Co1 O4 104.16(11) . . ? O6 Co1 O1 102.60(12) . 1_455 ? O5 Co1 O1 101.14(10) . 1_455 ? O4 Co1 O1 103.16(12) . 1_455 ? O6 Co1 O2 82.44(11) . 1_455 ? O5 Co1 O2 160.40(10) . 1_455 ? O4 Co1 O2 81.23(11) . 1_455 ? O1 Co1 O2 59.30(10) 1_455 1_455 ? O9 Co2 O7 96.27(11) 1_655 . ? O9 Co2 O1 172.95(11) 1_655 3_567 ? O7 Co2 O1 90.75(10) . 3_567 ? O9 Co2 O5 91.21(11) 1_655 . ? O7 Co2 O5 89.53(10) . . ? O1 Co2 O5 89.41(10) 3_567 . ? O9 Co2 N1 88.11(13) 1_655 . ? O7 Co2 N1 91.65(13) . . ? O1 Co2 N1 91.12(12) 3_567 . ? O5 Co2 N1 178.70(13) . . ? O9 Co2 O3 88.83(11) 1_655 3_567 ? O7 Co2 O3 167.49(10) . 3_567 ? O1 Co2 O3 84.39(10) 3_567 3_567 ? O5 Co2 O3 78.93(9) . 3_567 ? N1 Co2 O3 99.94(13) . 3_567 ? O5 Co3 O5 180.000(1) . 3_567 ? O5 Co3 O8 87.09(10) . 3_467 ? O5 Co3 O8 92.91(10) 3_567 3_467 ? O5 Co3 O8 92.91(10) . 1_655 ? O5 Co3 O8 87.09(10) 3_567 1_655 ? O8 Co3 O8 180.000(1) 3_467 1_655 ? O5 Co3 O3 80.70(9) . 3_567 ? O5 Co3 O3 99.30(9) 3_567 3_567 ? O8 Co3 O3 89.10(10) 3_467 3_567 ? O8 Co3 O3 90.90(10) 1_655 3_567 ? O5 Co3 O3 99.30(9) . . ? O5 Co3 O3 80.70(9) 3_567 . ? O8 Co3 O3 90.90(10) 3_467 . ? O8 Co3 O3 89.10(10) 1_655 . ? O3 Co3 O3 180.000(1) 3_567 . ? C12 N1 C16 116.7(5) . . ? C12 N1 Co2 121.8(4) . . ? C16 N1 Co2 120.8(4) . . ? C1 O1 Co1 95.4(2) . 1_655 ? C1 O1 Co2 133.4(2) . 3_567 ? Co1 O1 Co2 130.58(12) 1_655 3_567 ? C1 O2 Co1 85.6(2) . 1_655 ? C5 O3 Co3 125.5(2) . . ? C5 O3 Co2 136.1(2) . 3_567 ? Co3 O3 Co2 93.72(10) . 3_567 ? C5 O4 Co1 136.4(2) . . ? Co1 O5 Co3 113.82(11) . . ? Co1 O5 Co2 114.59(11) . . ? Co3 O5 Co2 98.34(10) . . ? Co1 O5 H5 105.3 . . ? Co3 O5 H5 108.5 . . ? Co2 O5 H5 116.4 . . ? C6 O6 Co1 126.8(2) . . ? C6 O7 Co2 123.6(2) . . ? C11 O8 Co3 127.1(2) . 1_455 ? C11 O9 Co2 130.5(2) . 1_455 ? O2 C1 O1 119.7(3) . . ? O2 C1 C2 119.1(3) . . ? O1 C1 C2 121.1(3) . . ? C4 C2 C3 118.6(3) 3_566 . ? C4 C2 C1 116.3(3) 3_566 . ? C3 C2 C1 125.1(3) . . ? C4 C3 C2 119.2(3) . . ? C4 C3 C5 115.9(3) . . ? C2 C3 C5 124.9(3) . . ? C3 C4 C2 122.2(3) . 3_566 ? C3 C4 H4 118.9 . . ? C2 C4 H4 118.9 3_566 . ? O4 C5 O3 125.3(3) . . ? O4 C5 C3 116.0(3) . . ? O3 C5 C3 118.7(3) . . ? O7 C6 O6 126.1(3) . . ? O7 C6 C8 119.0(3) . . ? O6 C6 C8 114.7(3) . . ? C8 C7 C8 122.0(5) . 4_575 ? C8 C7 H7 119.0 . . ? C8 C7 H7 119.0 4_575 . ? C7 C8 C9 119.1(3) . . ? C7 C8 C6 115.8(3) . . ? C9 C8 C6 125.2(3) . . ? C10 C9 C8 118.8(3) . . ? C10 C9 C11 119.6(3) . . ? C8 C9 C11 121.5(3) . . ? C9 C10 C9 122.2(5) 4_575 . ? C9 C10 H10 118.9 4_575 . ? C9 C10 H10 118.9 . . ? O8 C11 O9 126.0(3) . . ? O8 C11 C9 118.2(3) . . ? O9 C11 C9 115.8(3) . . ? N1 C12 C13 123.0(6) . . ? N1 C12 H12 118.5 . . ? C13 C12 H12 118.5 . . ? C14 C13 C12 121.0(7) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C15 116.2(6) . . ? C13 C14 C17 121.0(8) . . ? C15 C14 C17 122.5(8) . . ? C14 C15 C16 120.8(7) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? N1 C16 C15 122.3(6) . . ? N1 C16 H16 118.9 . . ? C15 C16 H16 118.9 . . ? C14 C17 C18' 114.2(10) . . ? C14 C17 C18 116.9(9) . . ? C18' C17 C18 67.2(11) . . ? C14 C17 H17A 104.5 . . ? C18' C17 H17A 76.8 . . ? C18 C17 H17A 133.2 . . ? C14 C17 H17B 106.9 . . ? C18' C17 H17B 136.7 . . ? C18 C17 H17B 82.9 . . ? H17A C17 H17B 105.9 . . ? C17 C18 C17 106.3(14) . 4_575 ? C17 C18 H18A 110.5 . . ? C17 C18 H18A 110.5 4_575 . ? C17 C18 H18B 110.5 . . ? C17 C18 H18B 110.5 4_575 . ? H18A C18 H18B 108.7 . . ? C17 C18' C17 109.8(16) 4_575 . ? C17 C18' H18C 109.7 4_575 . ? C17 C18' H18C 109.7 . . ? C17 C18' H18D 109.7 4_575 . ? C17 C18' H18D 109.7 . . ? H18C C18' H18D 108.2 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.201 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.111