# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1580 data_99150 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'tris-ditertbutylammoniumtrimesate acetone clathrate ' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C36 H69 N3 O7' _chemical_formula_weight 655.94 _chemical_melting_point ? _chemical_compound_source 'D. Plaut, Prof. M. Ward' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 9.7487(6) _cell_length_b 18.492(2) _cell_length_c 23.164(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.641(3) _cell_angle_gamma 90.00 _cell_volume 4090.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4905 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.065 _exptl_crystal_density_method ? _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type 'SADABS, G. Sheldrick (1996)' _exptl_absorpt_correction_T_min 0.882464 _exptl_absorpt_correction_T_max 1.000000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Platform CCD, Siemens' _diffrn_measurement_method 'omega-scans, area detector' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30377 _diffrn_reflns_av_R_equivalents 0.0828 _diffrn_reflns_av_sigmaI/netI 0.1048 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.05 _reflns_number_total 7227 _reflns_number_observed 3305 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART, Siemens' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL-93 (Sheldrick, 1993)' _computing_publication_material ? _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^)+(0.0906P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0069(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7227 _refine_ls_number_parameters 461 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1422 _refine_ls_R_factor_obs 0.0600 _refine_ls_wR_factor_all 0.1752 _refine_ls_wR_factor_obs 0.1478 _refine_ls_goodness_of_fit_all 0.903 _refine_ls_goodness_of_fit_obs 1.166 _refine_ls_restrained_S_all 0.903 _refine_ls_restrained_S_obs 1.166 _refine_ls_shift/esd_max 0.001 _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 O1 O 1.2801(3) 0.65275(13) 0.22128(13) 0.0863(9) Uani 1 d . . O2 O 1.1203(3) 0.70368(14) 0.15625(14) 0.1008(11) Uani 1 d . . O3 O 0.6976(2) 0.56518(11) 0.06675(9) 0.0451(6) Uani 1 d . . O4 O 0.6574(2) 0.45852(12) 0.10521(10) 0.0557(7) Uani 1 d . . O5 O 0.9766(2) 0.36738(11) 0.28333(9) 0.0485(6) Uani 1 d . . O6 O 1.1615(2) 0.43446(11) 0.32413(10) 0.0536(6) Uani 1 d . . N1 N 0.3944(3) 0.42017(12) 0.05172(12) 0.0302(6) Uani 1 d . . H1M H 0.3678(31) 0.4291(16) 0.0078(16) 0.062(10) Uiso 1 d . . H1N H 0.4854(33) 0.4378(15) 0.0654(13) 0.049(9) Uiso 1 d . . N2 N 0.9798(3) 0.22554(14) 0.24201(11) 0.0322(6) Uani 1 d . . H2M H 0.9801(32) 0.2784(19) 0.2594(14) 0.071(11) Uiso 1 d . . H2N H 1.0642(35) 0.2065(17) 0.2598(14) 0.068(11) Uiso 1 d . . N3 N 1.1309(3) 0.84378(15) 0.12336(11) 0.0364(6) Uani 1 d . . H3M H 1.1436(30) 0.7912(18) 0.1387(13) 0.061(10) Uiso 1 d . . H3N H 1.2115(33) 0.8707(17) 0.1447(14) 0.061(10) Uiso 1 d . . C1 C 1.0675(3) 0.59098(14) 0.19242(12) 0.0285(7) Uani 1 d . . C2 C 0.9452(3) 0.58292(14) 0.14999(12) 0.0285(7) Uani 1 d . . H2 H 0.9209(3) 0.61855(14) 0.12013(12) 0.034 Uiso 1 calc R . C3 C 0.8582(3) 0.52377(14) 0.15061(12) 0.0271(7) Uani 1 d . . C4 C 0.8932(3) 0.47272(14) 0.19554(12) 0.0300(7) Uani 1 d . . H4 H 0.8333(3) 0.43243(14) 0.19662(12) 0.036 Uiso 1 calc R . C5 C 1.0139(3) 0.47976(14) 0.23865(12) 0.0298(7) Uani 1 d . . C6 C 1.1002(3) 0.53886(15) 0.23590(12) 0.0314(7) Uani 1 d . . H6 H 1.1842(3) 0.54366(15) 0.26469(12) 0.038 Uiso 1 calc R . C7 C 1.1628(3) 0.6543(2) 0.19033(14) 0.0400(8) Uani 1 d . . C8 C 0.7275(3) 0.5155(2) 0.10364(13) 0.0363(7) Uani 1 d . . C9 C 1.0522(3) 0.4225(2) 0.28539(13) 0.0385(8) Uani 1 d . . C10 C 0.2979(3) 0.4674(2) 0.08042(13) 0.0418(8) Uani 1 d . . C11 C 0.4099(3) 0.33825(15) 0.05667(12) 0.0334(7) Uani 1 d . . C12 C 0.3419(4) 0.4663(2) 0.14737(15) 0.0701(11) Uani 1 d . . H12A H 0.4440(5) 0.4706(13) 0.15868(15) 0.105 Uiso 1 calc R . H12B H 0.3119(22) 0.4207(6) 0.1625(2) 0.105 Uiso 1 calc R . H12C H 0.2980(21) 0.5069(8) 0.1640(2) 0.105 Uiso 1 calc R . C13 C 0.1440(3) 0.4467(2) 0.0600(2) 0.0649(11) Uani 1 d . . H13A H 0.1261(6) 0.4007(6) 0.0782(8) 0.097 Uiso 1 calc R . H13B H 0.1227(7) 0.4416(12) 0.0170(2) 0.097 Uiso 1 calc R . H13C H 0.0846(3) 0.4845(6) 0.0717(9) 0.097 Uiso 1 calc R . C14 C 0.3199(3) 0.5436(2) 0.05772(15) 0.0497(9) Uani 1 d . . H14A H 0.4195(4) 0.5562(4) 0.0682(7) 0.075 Uiso 1 calc R . H14B H 0.2653(16) 0.5785(2) 0.0757(7) 0.075 Uiso 1 calc R . H14C H 0.2890(19) 0.5448(3) 0.0148(2) 0.075 Uiso 1 calc R . C15 C 0.2776(3) 0.2998(2) 0.02585(14) 0.0483(9) Uani 1 d . . H15A H 0.2046(7) 0.3056(9) 0.0490(4) 0.072 Uiso 1 calc R . H15B H 0.2974(6) 0.2483(2) 0.0220(8) 0.072 Uiso 1 calc R . H15C H 0.2454(11) 0.3208(7) -0.0134(3) 0.072 Uiso 1 calc R . C16 C 0.5260(3) 0.3206(2) 0.02344(14) 0.0459(8) Uani 1 d . . H16A H 0.6105(6) 0.3479(7) 0.0406(5) 0.069 Uiso 1 calc R . H16B H 0.4955(8) 0.3340(9) -0.0181(2) 0.069 Uiso 1 calc R . H16C H 0.5464(13) 0.2687(2) 0.0265(7) 0.069 Uiso 1 calc R . C17 C 0.4557(3) 0.3137(2) 0.12023(13) 0.0435(8) Uani 1 d . . H17A H 0.3785(7) 0.3205(9) 0.1410(2) 0.065 Uiso 1 calc R . H17B H 0.5367(12) 0.3422(7) 0.1396(3) 0.065 Uiso 1 calc R . H17C H 0.4814(18) 0.2624(3) 0.12110(13) 0.065 Uiso 1 calc R . C18 C 0.8691(3) 0.1852(2) 0.26789(13) 0.0432(8) Uani 1 d . . C19 C 0.9838(3) 0.2316(2) 0.17663(13) 0.0401(8) Uani 1 d . . C20 C 0.8626(4) 0.1056(2) 0.2501(2) 0.0829(13) Uani 1 d . . H20A H 0.8216(25) 0.1013(2) 0.2080(3) 0.124 Uiso 1 calc R . H20B H 0.8046(23) 0.0791(3) 0.2729(8) 0.124 Uiso 1 calc R . H20C H 0.9574(5) 0.0852(4) 0.2580(11) 0.124 Uiso 1 calc R . C21 C 0.7264(3) 0.2210(2) 0.2505(2) 0.0760(12) Uani 1 d . . H21A H 0.6889(12) 0.2128(11) 0.2085(3) 0.114 Uiso 1 calc R . H21B H 0.7357(5) 0.2731(3) 0.2582(10) 0.114 Uiso 1 calc R . H21C H 0.6625(8) 0.2001(10) 0.2737(8) 0.114 Uiso 1 calc R . C22 C 0.9207(4) 0.1926(2) 0.33424(14) 0.0629(10) Uani 1 d . . H22A H 1.0150(10) 0.1721(10) 0.3454(2) 0.094 Uiso 1 calc R . H22B H 0.8572(13) 0.1667(10) 0.35480(14) 0.094 Uiso 1 calc R . H22C H 0.9233(22) 0.2439(2) 0.3452(2) 0.094 Uiso 1 calc R . C23 C 0.8526(4) 0.2680(2) 0.14179(14) 0.0602(10) Uani 1 d . . H23A H 0.7742(6) 0.2338(4) 0.1363(8) 0.090 Uiso 1 calc R . H23B H 0.8692(8) 0.2831(10) 0.1032(4) 0.090 Uiso 1 calc R . H23C H 0.8300(13) 0.3104(7) 0.1635(5) 0.090 Uiso 1 calc R . C24 C 1.0085(4) 0.1585(2) 0.15000(15) 0.0569(10) Uani 1 d . . H24A H 0.9215(7) 0.1304(5) 0.1431(9) 0.085 Uiso 1 calc R . H24B H 1.0814(16) 0.1321(5) 0.1773(4) 0.085 Uiso 1 calc R . H24C H 1.0385(21) 0.1659(2) 0.1125(5) 0.085 Uiso 1 calc R . C25 C 1.1100(4) 0.2805(2) 0.1767(2) 0.0712(12) Uani 1 d . . H25A H 1.1940(6) 0.2582(6) 0.2004(9) 0.107 Uiso 1 calc R . H25B H 1.0939(11) 0.3276(5) 0.1936(10) 0.107 Uiso 1 calc R . H25C H 1.1231(15) 0.2872(10) 0.1362(2) 0.107 Uiso 1 calc R . C26 C 1.1518(3) 0.8362(2) 0.06017(13) 0.0483(9) Uani 1 d . . C27 C 1.0050(3) 0.8769(2) 0.1433(2) 0.0531(9) Uani 1 d . . C28 C 1.2988(4) 0.8059(2) 0.0677(2) 0.0867(14) Uani 1 d . . H28A H 1.3043(9) 0.7598(8) 0.0889(11) 0.130 Uiso 1 calc R . H28B H 1.3657(5) 0.8402(7) 0.0902(11) 0.130 Uiso 1 calc R . H28C H 1.3217(12) 0.7981(15) 0.0288(2) 0.130 Uiso 1 calc R . C29 C 1.1433(5) 0.9084(2) 0.0292(2) 0.0897(14) Uani 1 d . . H29A H 1.2008(24) 0.9438(5) 0.0548(5) 0.135 Uiso 1 calc R . H29B H 1.0458(6) 0.9248(8) 0.0202(11) 0.135 Uiso 1 calc R . H29C H 1.1778(28) 0.9033(4) -0.0075(7) 0.135 Uiso 1 calc R . C30 C 1.0475(4) 0.7822(2) 0.0261(2) 0.0768(12) Uani 1 d . . H30A H 1.0453(20) 0.7387(6) 0.0501(5) 0.115 Uiso 1 calc R . H30B H 1.0763(15) 0.7692(11) -0.0107(6) 0.115 Uiso 1 calc R . H30C H 0.9541(6) 0.8041(5) 0.0171(10) 0.115 Uiso 1 calc R . C31 C 0.9925(4) 0.9573(2) 0.1311(2) 0.098(2) Uani 1 d . . H31A H 0.9608(31) 0.9653(2) 0.0887(3) 0.148 Uiso 1 calc R . H31B H 1.0840(9) 0.9802(3) 0.1444(13) 0.148 Uiso 1 calc R . H31C H 0.9246(25) 0.9783(4) 0.1522(11) 0.148 Uiso 1 calc R . C32 C 1.0379(4) 0.8653(3) 0.2095(2) 0.099(2) Uani 1 d . . H32A H 1.0473(32) 0.8134(3) 0.2179(2) 0.148 Uiso 1 calc R . H32B H 0.9619(16) 0.8851(15) 0.2266(2) 0.148 Uiso 1 calc R . H32C H 1.1258(18) 0.8898(14) 0.2266(2) 0.148 Uiso 1 calc R . C33 C 0.8689(3) 0.8375(2) 0.1164(2) 0.0700(11) Uani 1 d . . H33A H 0.8831(8) 0.7852(2) 0.1212(9) 0.105 Uiso 1 calc R . H33B H 0.8422(13) 0.8491(10) 0.0744(3) 0.105 Uiso 1 calc R . H33C H 0.7943(7) 0.8528(9) 0.1365(7) 0.105 Uiso 1 calc R . O7 O 0.5934(5) 0.1250(3) 0.0807(2) 0.199(2) Uani 1 d D . C70 C 0.5177(5) 0.0768(3) 0.0910(3) 0.126(2) Uani 1 d D . C71 C 0.3736(5) 0.0884(3) 0.1004(3) 0.144(2) Uani 1 d D . H71A H 0.3355(18) 0.0425(6) 0.1113(20) 0.216 Uiso 1 calc R . H71B H 0.3146(12) 0.1067(23) 0.0640(6) 0.216 Uiso 1 calc R . H71C H 0.3754(8) 0.1237(18) 0.1321(13) 0.216 Uiso 1 calc R . C72 C 0.5713(7) 0.0019(3) 0.0922(4) 0.196(3) Uani 1 d D . H72A H 0.4947(17) -0.0308(6) 0.0752(27) 0.294 Uiso 1 calc R . H72B H 0.6096(63) -0.0123(13) 0.1330(4) 0.294 Uiso 1 calc R . H72C H 0.6451(50) -0.0008(8) 0.0691(25) 0.294 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.051(2) 0.076(2) 0.113(2) 0.030(2) -0.028(2) -0.0350(14) O2 0.089(2) 0.057(2) 0.132(3) 0.051(2) -0.037(2) -0.0393(15) O3 0.0488(13) 0.0476(14) 0.0318(13) 0.0060(11) -0.0085(10) 0.0005(10) O4 0.0453(13) 0.0502(15) 0.060(2) 0.0065(12) -0.0158(11) -0.0159(12) O5 0.0676(15) 0.0275(13) 0.0484(14) 0.0057(11) 0.0074(11) -0.0022(11) O6 0.0512(14) 0.0437(14) 0.056(2) 0.0123(11) -0.0128(12) 0.0090(11) N1 0.0264(14) 0.031(2) 0.031(2) 0.0010(12) 0.0022(11) -0.0011(11) N2 0.0293(14) 0.032(2) 0.035(2) 0.0064(12) 0.0056(12) 0.0003(11) N3 0.041(2) 0.032(2) 0.032(2) -0.0022(13) -0.0015(12) -0.0069(13) C1 0.028(2) 0.023(2) 0.034(2) -0.0015(14) 0.0051(13) 0.0005(12) C2 0.0292(15) 0.027(2) 0.028(2) 0.0013(13) 0.0034(13) 0.0023(13) C3 0.0261(15) 0.028(2) 0.027(2) -0.0020(13) 0.0048(12) 0.0014(12) C4 0.030(2) 0.024(2) 0.035(2) -0.0019(14) 0.0054(14) -0.0043(12) C5 0.030(2) 0.024(2) 0.032(2) -0.0015(13) 0.0011(13) 0.0046(13) C6 0.027(2) 0.031(2) 0.034(2) -0.0003(14) -0.0005(13) 0.0016(13) C7 0.041(2) 0.033(2) 0.044(2) 0.002(2) 0.004(2) -0.0048(15) C8 0.035(2) 0.037(2) 0.034(2) -0.004(2) 0.0002(14) -0.0035(15) C9 0.046(2) 0.030(2) 0.039(2) 0.002(2) 0.006(2) 0.008(2) C10 0.044(2) 0.043(2) 0.041(2) 0.003(2) 0.015(2) 0.009(2) C11 0.034(2) 0.028(2) 0.036(2) 0.0023(14) 0.0030(14) -0.0021(13) C12 0.105(3) 0.068(3) 0.044(2) 0.002(2) 0.031(2) 0.028(2) C13 0.039(2) 0.059(2) 0.103(3) 0.018(2) 0.027(2) 0.012(2) C14 0.061(2) 0.036(2) 0.055(2) 0.001(2) 0.019(2) 0.007(2) C15 0.049(2) 0.041(2) 0.050(2) -0.004(2) -0.001(2) -0.013(2) C16 0.053(2) 0.037(2) 0.049(2) 0.003(2) 0.012(2) 0.007(2) C17 0.046(2) 0.040(2) 0.041(2) 0.011(2) -0.0004(15) -0.0020(15) C18 0.049(2) 0.040(2) 0.043(2) 0.005(2) 0.015(2) -0.009(2) C19 0.046(2) 0.040(2) 0.037(2) 0.005(2) 0.0153(15) 0.0033(15) C20 0.126(4) 0.055(3) 0.082(3) -0.012(2) 0.055(3) -0.041(2) C21 0.038(2) 0.117(3) 0.079(3) 0.015(2) 0.026(2) -0.003(2) C22 0.089(3) 0.060(2) 0.041(2) 0.012(2) 0.016(2) -0.005(2) C23 0.078(3) 0.059(2) 0.040(2) 0.013(2) 0.005(2) 0.024(2) C24 0.073(2) 0.053(2) 0.049(2) -0.001(2) 0.022(2) 0.014(2) C25 0.076(3) 0.067(3) 0.083(3) 0.006(2) 0.046(2) -0.018(2) C26 0.060(2) 0.053(2) 0.030(2) -0.006(2) 0.004(2) -0.015(2) C27 0.048(2) 0.057(2) 0.056(2) -0.014(2) 0.014(2) -0.006(2) C28 0.070(3) 0.109(4) 0.084(3) -0.047(3) 0.022(2) 0.002(2) C29 0.125(4) 0.086(3) 0.057(3) 0.021(2) 0.017(2) -0.026(3) C30 0.092(3) 0.089(3) 0.045(2) -0.026(2) 0.005(2) -0.033(2) C31 0.078(3) 0.050(3) 0.168(5) -0.025(3) 0.027(3) 0.009(2) C32 0.088(3) 0.160(5) 0.055(3) -0.036(3) 0.031(2) -0.030(3) C33 0.045(2) 0.078(3) 0.084(3) -0.005(2) 0.007(2) -0.010(2) O7 0.215(5) 0.172(5) 0.241(6) 0.012(4) 0.117(4) -0.046(4) C70 0.153(6) 0.090(4) 0.156(5) 0.021(4) 0.079(4) -0.037(4) C71 0.138(5) 0.122(5) 0.182(6) 0.040(4) 0.055(5) 0.000(4) C72 0.192(7) 0.144(7) 0.281(10) 0.080(6) 0.116(7) 0.045(5) _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 O1 C7 1.221(3) . ? O2 C7 1.223(3) . ? O3 C8 1.249(3) . ? O4 C8 1.260(3) . ? O5 C9 1.252(3) . ? O6 C9 1.266(3) . ? N1 C11 1.524(3) . ? N1 C10 1.531(3) . ? N1 H1M 1.01(3) . ? N1 H1N 0.94(3) . ? N2 C19 1.527(4) . ? N2 C18 1.530(4) . ? N2 H2M 1.06(3) . ? N2 H2N 0.91(3) . ? N3 C26 1.525(4) . ? N3 C27 1.525(4) . ? N3 H3M 1.03(3) . ? N3 H3N 0.98(3) . ? C1 C6 1.384(4) . ? C1 C2 1.391(3) . ? C1 C7 1.503(4) . ? C2 C3 1.386(3) . ? C2 H2 0.95 . ? C3 C4 1.396(4) . ? C3 C8 1.508(4) . ? C4 C5 1.387(4) . ? C4 H4 0.95 . ? C5 C6 1.389(4) . ? C5 C9 1.507(4) . ? C6 H6 0.95 . ? C10 C12 1.523(4) . ? C10 C13 1.528(4) . ? C10 C14 1.534(4) . ? C11 C15 1.519(4) . ? C11 C17 1.519(4) . ? C11 C16 1.526(4) . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 C21 1.520(4) . ? C18 C22 1.524(4) . ? C18 C20 1.527(4) . ? C19 C23 1.524(4) . ? C19 C24 1.525(4) . ? C19 C25 1.527(4) . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 C29 1.509(5) . ? C26 C28 1.517(5) . ? C26 C30 1.525(4) . ? C27 C31 1.512(5) . ? C27 C32 1.517(5) . ? C27 C33 1.532(4) . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C30 H30A 0.98 . ? C30 H30B 0.98 . ? C30 H30C 0.98 . ? C31 H31A 0.98 . ? C31 H31B 0.98 . ? C31 H31C 0.98 . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? C33 H33A 0.98 . ? C33 H33B 0.98 . ? C33 H33C 0.98 . ? O7 C70 1.2105(10) . ? C70 C72 1.4786(10) . ? C70 C71 1.4796(10) . ? C71 H71A 0.98 . ? C71 H71B 0.98 . ? C71 H71C 0.98 . ? C72 H72A 0.98 . ? C72 H72B 0.98 . ? C72 H72C 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 N1 C10 126.5(2) . . ? C11 N1 H1M 103.8(17) . . ? C10 N1 H1M 106.8(17) . . ? C11 N1 H1N 104.3(17) . . ? C10 N1 H1N 106.1(17) . . ? H1M N1 H1N 108.4(25) . . ? C19 N2 C18 125.8(2) . . ? C19 N2 H2M 108.2(17) . . ? C18 N2 H2M 104.4(17) . . ? C19 N2 H2N 105.9(21) . . ? C18 N2 H2N 106.1(20) . . ? H2M N2 H2N 104.6(26) . . ? C26 N3 C27 126.8(2) . . ? C26 N3 H3M 102.4(16) . . ? C27 N3 H3M 108.8(16) . . ? C26 N3 H3N 106.4(18) . . ? C27 N3 H3N 104.9(18) . . ? H3M N3 H3N 106.1(24) . . ? C6 C1 C2 118.6(2) . . ? C6 C1 C7 120.9(2) . . ? C2 C1 C7 120.5(3) . . ? C3 C2 C1 121.1(2) . . ? C3 C2 H2 119.5(2) . . ? C1 C2 H2 119.5(2) . . ? C2 C3 C4 118.9(2) . . ? C2 C3 C8 120.2(3) . . ? C4 C3 C8 120.9(2) . . ? C5 C4 C3 121.2(2) . . ? C5 C4 H4 119.4(2) . . ? C3 C4 H4 119.4(2) . . ? C4 C5 C6 118.3(3) . . ? C4 C5 C9 120.1(3) . . ? C6 C5 C9 121.5(3) . . ? C1 C6 C5 121.9(2) . . ? C1 C6 H6 119.1(2) . . ? C5 C6 H6 119.1(2) . . ? O1 C7 O2 123.5(3) . . ? O1 C7 C1 118.3(3) . . ? O2 C7 C1 118.1(3) . . ? O3 C8 O4 125.6(3) . . ? O3 C8 C3 117.7(3) . . ? O4 C8 C3 116.7(3) . . ? O5 C9 O6 125.0(3) . . ? O5 C9 C5 119.1(3) . . ? O6 C9 C5 115.9(3) . . ? C12 C10 C13 111.7(3) . . ? C12 C10 N1 111.3(2) . . ? C13 C10 N1 111.9(3) . . ? C12 C10 C14 109.3(3) . . ? C13 C10 C14 108.7(3) . . ? N1 C10 C14 103.6(2) . . ? C15 C11 C17 111.8(2) . . ? C15 C11 N1 111.6(2) . . ? C17 C11 N1 112.1(2) . . ? C15 C11 C16 108.0(2) . . ? C17 C11 C16 108.8(2) . . ? N1 C11 C16 104.3(2) . . ? C10 C12 H12A 109.5(2) . . ? C10 C12 H12B 109.5(2) . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5(2) . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5(2) . . ? C10 C13 H13B 109.5(2) . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5(2) . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C10 C14 H14A 109.5(2) . . ? C10 C14 H14B 109.5(2) . . ? H14A C14 H14B 109.5 . . ? C10 C14 H14C 109.5(2) . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 H15A 109.5(2) . . ? C11 C15 H15B 109.5(2) . . ? H15A C15 H15B 109.5 . . ? C11 C15 H15C 109.5(2) . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C11 C16 H16A 109.5(2) . . ? C11 C16 H16B 109.5(2) . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5(2) . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C11 C17 H17A 109.5(2) . . ? C11 C17 H17B 109.47(15) . . ? H17A C17 H17B 109.5 . . ? C11 C17 H17C 109.5(2) . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C21 C18 C22 109.0(3) . . ? C21 C18 C20 111.2(3) . . ? C22 C18 C20 110.3(3) . . ? C21 C18 N2 111.4(3) . . ? C22 C18 N2 103.6(2) . . ? C20 C18 N2 111.0(3) . . ? C23 C19 C24 111.2(3) . . ? C23 C19 C25 109.2(3) . . ? C24 C19 C25 109.4(3) . . ? C23 C19 N2 111.7(2) . . ? C24 C19 N2 112.0(2) . . ? C25 C19 N2 102.9(2) . . ? C18 C20 H20A 109.5(2) . . ? C18 C20 H20B 109.5(2) . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5(2) . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5(2) . . ? C18 C21 H21B 109.5(2) . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5(2) . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5(2) . . ? C18 C22 H22B 109.5(2) . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5(2) . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 H23A 109.5(2) . . ? C19 C23 H23B 109.5(2) . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5(2) . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C19 C24 H24A 109.5(2) . . ? C19 C24 H24B 109.5(2) . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5(2) . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C19 C25 H25A 109.5(2) . . ? C19 C25 H25B 109.5(2) . . ? H25A C25 H25B 109.5 . . ? C19 C25 H25C 109.5(2) . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C29 C26 C28 110.0(3) . . ? C29 C26 N3 111.7(3) . . ? C28 C26 N3 103.3(3) . . ? C29 C26 C30 111.5(3) . . ? C28 C26 C30 109.5(3) . . ? N3 C26 C30 110.6(3) . . ? C31 C27 C32 108.8(3) . . ? C31 C27 N3 112.2(3) . . ? C32 C27 N3 103.3(3) . . ? C31 C27 C33 111.2(3) . . ? C32 C27 C33 109.4(3) . . ? N3 C27 C33 111.7(3) . . ? C26 C28 H28A 109.5(2) . . ? C26 C28 H28B 109.5(2) . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5(2) . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5(2) . . ? C26 C29 H29B 109.5(2) . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5(2) . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C26 C30 H30A 109.5(2) . . ? C26 C30 H30B 109.5(2) . . ? H30A C30 H30B 109.5 . . ? C26 C30 H30C 109.5(2) . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C27 C31 H31A 109.5(2) . . ? C27 C31 H31B 109.5(2) . . ? H31A C31 H31B 109.5 . . ? C27 C31 H31C 109.5(2) . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 H32A 109.5(2) . . ? C27 C32 H32B 109.5(2) . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5(2) . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C27 C33 H33A 109.5(2) . . ? C27 C33 H33B 109.5(2) . . ? H33A C33 H33B 109.5 . . ? C27 C33 H33C 109.5(2) . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O7 C70 C72 117.8(5) . . ? O7 C70 C71 123.8(5) . . ? C72 C70 C71 118.3(4) . . ? C70 C71 H71A 109.5(3) . . ? C70 C71 H71B 109.5(3) . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.5(3) . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C70 C72 H72A 109.5(4) . . ? C70 C72 H72B 109.5(4) . . ? H72A C72 H72B 109.5 . . ? C70 C72 H72C 109.5(3) . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? 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 C6 C1 C2 C3 -0.6(4) . . . . ? C7 C1 C2 C3 178.4(2) . . . . ? C1 C2 C3 C4 1.5(4) . . . . ? C1 C2 C3 C8 -179.0(2) . . . . ? C2 C3 C4 C5 -1.0(4) . . . . ? C8 C3 C4 C5 179.5(3) . . . . ? C3 C4 C5 C6 -0.4(4) . . . . ? C3 C4 C5 C9 -177.7(2) . . . . ? C2 C1 C6 C5 -0.9(4) . . . . ? C7 C1 C6 C5 -179.9(2) . . . . ? C4 C5 C6 C1 1.4(4) . . . . ? C9 C5 C6 C1 178.6(2) . . . . ? C6 C1 C7 O1 12.2(4) . . . . ? C2 C1 C7 O1 -166.8(3) . . . . ? C6 C1 C7 O2 -170.2(3) . . . . ? C2 C1 C7 O2 10.8(4) . . . . ? C2 C3 C8 O3 -3.7(4) . . . . ? C4 C3 C8 O3 175.8(3) . . . . ? C2 C3 C8 O4 176.4(3) . . . . ? C4 C3 C8 O4 -4.2(4) . . . . ? C4 C5 C9 O5 2.7(4) . . . . ? C6 C5 C9 O5 -174.5(3) . . . . ? C4 C5 C9 O6 -177.7(3) . . . . ? C6 C5 C9 O6 5.1(4) . . . . ? C11 N1 C10 C12 65.6(4) . . . . ? C11 N1 C10 C13 -60.1(4) . . . . ? C11 N1 C10 C14 -177.0(3) . . . . ? C10 N1 C11 C15 67.5(4) . . . . ? C10 N1 C11 C17 -58.7(4) . . . . ? C10 N1 C11 C16 -176.2(3) . . . . ? C19 N2 C18 C21 -66.4(4) . . . . ? C19 N2 C18 C22 176.5(3) . . . . ? C19 N2 C18 C20 58.2(4) . . . . ? C18 N2 C19 C23 59.9(4) . . . . ? C18 N2 C19 C24 -65.5(4) . . . . ? C18 N2 C19 C25 177.0(3) . . . . ? C27 N3 C26 C29 57.1(4) . . . . ? C27 N3 C26 C28 175.3(3) . . . . ? C27 N3 C26 C30 -67.7(4) . . . . ? C26 N3 C27 C31 -66.6(4) . . . . ? C26 N3 C27 C32 176.5(3) . . . . ? C26 N3 C27 C33 59.0(4) . . . . ? _refine_diff_density_max 0.542 _refine_diff_density_min -0.283 _refine_diff_density_rms 0.048 data_99163sq _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'tris-dicyclohexyammoniumtrimesate isopropanol clathrate ' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C54 H96 N3 O9' _chemical_formula_weight 931.34 _chemical_melting_point ? _chemical_compound_source 'D. Plaut, Prof. M. Ward' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5401(6) _cell_length_b 15.815(1) _cell_length_c 18.711(1) _cell_angle_alpha 107.648(1) _cell_angle_beta 105.627(1) _cell_angle_gamma 97.211(1) _cell_volume 2788.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5026 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.211 _exptl_crystal_size_mid 0.154 _exptl_crystal_size_min 0.116 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.109 _exptl_crystal_density_method ? _exptl_crystal_F_000 1026 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_type 'SADABS, G. Sheldrick (1999)' _exptl_absorpt_correction_T_min 0.703642 _exptl_absorpt_correction_T_max 1.000000 _exptl_special_details ; Data set has been modified for disordered solvent (PLATON, A. Spek). ; _diffrn_ambient_temperature 173(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 'SMART CCD System, Bruker' _diffrn_measurement_method 'area detector, omega-scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22227 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0607 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 25.03 _reflns_number_total 9779 _reflns_number_observed 5851 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL, Siemens' _computing_publication_material ? _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^)+(0.1272P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9779 _refine_ls_number_parameters 620 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0980 _refine_ls_R_factor_obs 0.0642 _refine_ls_wR_factor_all 0.2091 _refine_ls_wR_factor_obs 0.1895 _refine_ls_goodness_of_fit_all 0.973 _refine_ls_goodness_of_fit_obs 1.157 _refine_ls_restrained_S_all 0.974 _refine_ls_restrained_S_obs 1.158 _refine_ls_shift/esd_max 0.043 _refine_ls_shift/esd_mean 0.005 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 O1 O 0.8627(2) 0.63987(11) 0.01292(10) 0.0380(5) Uani 1 d . . O2 O 0.9785(2) 0.62242(13) 0.12432(11) 0.0461(5) Uani 1 d . . O3 O 0.9632(2) 0.81230(13) 0.38276(10) 0.0467(5) Uani 1 d . . O4 O 0.8584(2) 0.92651(12) 0.39066(10) 0.0465(5) Uani 1 d . . O5 O 0.5689(2) 0.95105(13) 0.14349(11) 0.0465(5) Uani 1 d . . O6 O 0.5950(2) 0.87741(13) 0.02876(11) 0.0418(5) Uani 1 d . . N1 N 0.8399(2) 0.47831(13) -0.09900(11) 0.0276(5) Uani 1 d . . H1A H 0.9141(2) 0.45298(13) -0.09700(11) 0.043(8) Uiso 1 calc R . H1B H 0.8642(2) 0.52980(13) -0.05435(11) 0.030(7) Uiso 1 calc R . N2 N 1.08793(15) 0.88870(10) 0.54349(8) 0.0330(5) Uani 1 d . . H2A H 1.03881(15) 0.86918(10) 0.49042(8) 0.062(10) Uiso 1 calc R . H2B H 1.09931(15) 0.95096(10) 0.56327(8) 0.042(8) Uiso 1 calc R . N3 N 0.40135(15) 1.04949(10) 0.08435(8) 0.0286(5) Uani 1 d R . H3A H 0.42054(15) 1.06652(10) 0.04487(8) 0.042(8) Uiso 1 d R . H3B H 0.45446(15) 1.00968(10) 0.09415(8) 0.055(9) Uiso 1 d R . C1 C 0.8569(2) 0.7389(2) 0.13532(14) 0.0245(5) Uani 1 d . . C2 C 0.8978(2) 0.7646(2) 0.21779(14) 0.0273(5) Uani 1 d . . H2A H 0.9580(2) 0.7349(2) 0.24347(14) 0.036(7) Uiso 1 calc R . C3 C 0.8509(2) 0.8334(2) 0.26265(14) 0.0273(5) Uani 1 d . . C4 C 0.7624(2) 0.8758(2) 0.22452(14) 0.0275(6) Uani 1 d . . H4A H 0.7295(2) 0.9223(2) 0.25496(14) 0.033 Uiso 1 calc R . C5 C 0.7211(2) 0.8517(2) 0.14298(14) 0.0252(5) Uani 1 d . . C6 C 0.7695(2) 0.78379(15) 0.09845(14) 0.0249(5) Uani 1 d . . H6A H 0.7429(2) 0.76783(15) 0.04249(14) 0.030 Uiso 1 calc R . C7 C 0.9034(3) 0.6611(2) 0.0867(2) 0.0299(6) Uani 1 d . . C8 C 0.8944(3) 0.8599(2) 0.35184(15) 0.0334(6) Uani 1 d . . C9 C 0.6206(2) 0.8971(2) 0.10173(15) 0.0293(6) Uani 1 d . . C10 C 0.8116(3) 0.5080(2) -0.16949(15) 0.0316(6) Uani 1 d . . H10A H 0.7394(3) 0.5433(2) -0.16810(15) 0.047(8) Uiso 1 calc R . C11 C 0.7631(3) 0.4284(2) -0.2465(2) 0.0514(8) Uani 1 d . . H11A H 0.6780(3) 0.3898(2) -0.2507(2) 0.062 Uiso 1 calc R . H11B H 0.8315(3) 0.3910(2) -0.2483(2) 0.062 Uiso 1 calc R . C12 C 0.7393(4) 0.4630(3) -0.3156(2) 0.0680(10) Uani 1 d . . H12A H 0.6675(4) 0.4978(3) -0.3152(2) 0.085(13) Uiso 1 calc R . H12B H 0.7082(4) 0.4106(3) -0.3662(2) 0.075(11) Uiso 1 calc R . C13 C 0.8696(4) 0.5245(3) -0.3099(2) 0.0651(10) Uani 1 d . . H13A H 0.9396(4) 0.4887(3) -0.3142(2) 0.078 Uiso 1 calc R . H13B H 0.8513(4) 0.5478(3) -0.3543(2) 0.078 Uiso 1 calc R . C14 C 0.9206(3) 0.6036(2) -0.2319(2) 0.0520(8) Uani 1 d . . H14A H 0.8554(3) 0.6435(2) -0.2307(2) 0.053(9) Uiso 1 calc R . H14B H 1.0081(3) 0.6399(2) -0.2272(2) 0.083(12) Uiso 1 calc R . C15 C 0.9392(3) 0.5708(2) -0.1619(2) 0.0401(7) Uani 1 d . . H15A H 1.0137(3) 0.5382(2) -0.1588(2) 0.054(9) Uiso 1 calc R . H15B H 0.9651(3) 0.6240(2) -0.1122(2) 0.064(10) Uiso 1 calc R . C16 C 0.7318(2) 0.4127(2) -0.09334(15) 0.0307(6) Uani 1 d . . H16A H 0.7079(2) 0.3548(2) -0.13988(15) 0.025(6) Uiso 1 calc R . C17 C 0.7896(3) 0.3927(2) -0.0179(2) 0.0345(6) Uani 1 d . . H17A H 0.8684(3) 0.3654(2) -0.0210(2) 0.033(7) Uiso 1 calc R . H17B H 0.8213(3) 0.4504(2) 0.0282(2) 0.035(7) Uiso 1 calc R . C18 C 0.6848(3) 0.3280(2) -0.0059(2) 0.0425(7) Uani 1 d . . H18A H 0.6602(3) 0.2680(2) -0.0491(2) 0.051 Uiso 1 calc R . H18B H 0.7240(3) 0.3190(2) 0.0449(2) 0.051 Uiso 1 calc R . C19 C 0.5589(3) 0.3647(2) -0.0051(2) 0.0444(7) Uani 1 d . . H19A H 0.5817(3) 0.4215(2) 0.0413(2) 0.053 Uiso 1 calc R . H19B H 0.4906(3) 0.3197(2) -0.0002(2) 0.053 Uiso 1 calc R . C20 C 0.5004(3) 0.3839(2) -0.0806(2) 0.0449(7) Uani 1 d . . H20A H 0.4211(3) 0.4107(2) -0.0775(2) 0.061(9) Uiso 1 calc R . H20B H 0.4690(3) 0.3259(2) -0.1264(2) 0.044(8) Uiso 1 calc R . C21 C 0.6044(3) 0.4493(2) -0.0935(2) 0.0379(7) Uani 1 d . . H21A H 0.5649(3) 0.4570(2) -0.1449(2) 0.048(8) Uiso 1 calc R . H21B H 0.6282(3) 0.5096(2) -0.0510(2) 0.045(8) Uiso 1 calc R . C22 C 1.0047(3) 0.8486(2) 0.5838(2) 0.0369(6) Uani 1 d . . H22A H 0.9776(3) 0.7810(2) 0.5558(2) 0.038(7) Uiso 1 calc R . C23 C 1.0829(3) 0.8679(2) 0.6698(2) 0.0451(7) Uani 1 d . . H23A H 1.1142(3) 0.9346(2) 0.6981(2) 0.050(8) Uiso 1 calc R . H23B H 1.1635(3) 0.8413(2) 0.6732(2) 0.041(7) Uiso 1 calc R . C24 C 0.9937(4) 0.8273(3) 0.7093(2) 0.0653(10) Uani 1 d . . H24A H 0.9697(4) 0.7601(3) 0.6841(2) 0.101(14) Uiso 1 calc R . H24B H 1.0450(4) 0.8430(3) 0.7661(2) 0.096(13) Uiso 1 calc R . C25 C 0.8670(4) 0.8624(3) 0.7019(2) 0.0780(12) Uani 1 d . . H25A H 0.8907(4) 0.9287(3) 0.7324(2) 0.091(13) Uiso 1 calc R . H25B H 0.8091(4) 0.8321(3) 0.7249(2) 0.088(12) Uiso 1 calc R . C26 C 0.7897(4) 0.8455(3) 0.6166(3) 0.0816(12) Uani 1 d . . H26A H 0.7103(4) 0.8733(3) 0.6143(3) 0.124(17) Uiso 1 calc R . H26B H 0.7563(4) 0.7791(3) 0.5877(3) 0.076(12) Uiso 1 calc R . C27 C 0.8776(3) 0.8852(3) 0.5759(2) 0.0576(9) Uani 1 d . . H27A H 0.8258(3) 0.8688(3) 0.5190(2) 0.078(11) Uiso 1 calc R . H27B H 0.9023(3) 0.9525(3) 0.6004(2) 0.094(14) Uiso 1 calc R . C28 C 1.2245(3) 0.8681(2) 0.5505(2) 0.0345(6) Uani 1 d . . H28A H 1.2821(3) 0.8948(2) 0.6076(2) 0.040(7) Uiso 1 calc R . C29 C 1.2148(3) 0.7656(2) 0.5212(2) 0.0414(7) Uani 1 d . . H29A H 1.1772(3) 0.7383(2) 0.5543(2) 0.049(8) Uiso 1 calc R . H29B H 1.1527(3) 0.7377(2) 0.4658(2) 0.042(8) Uiso 1 calc R . C30 C 1.3528(3) 0.7455(2) 0.5248(2) 0.0523(8) Uani 1 d . . H30A H 1.4123(3) 0.7686(2) 0.5808(2) 0.056(9) Uiso 1 calc R . H30B H 1.3437(3) 0.6787(2) 0.5035(2) 0.067(10) Uiso 1 calc R . C31 C 1.4166(3) 0.7893(2) 0.4777(2) 0.0568(9) Uani 1 d . . H31A H 1.3616(3) 0.7621(2) 0.4209(2) 0.055(9) Uiso 1 calc R . H31B H 1.5082(3) 0.7776(2) 0.4832(2) 0.075(11) Uiso 1 calc R . C32 C 1.4261(3) 0.8911(2) 0.5067(2) 0.0562(9) Uani 1 d . . H32A H 1.4639(3) 0.9181(2) 0.4735(2) 0.067 Uiso 1 calc R . H32B H 1.4885(3) 0.9189(2) 0.5620(2) 0.067 Uiso 1 calc R . C33 C 1.2889(3) 0.9127(2) 0.5035(2) 0.0458(7) Uani 1 d . . H33A H 1.2292(3) 0.8905(2) 0.4477(2) 0.038(7) Uiso 1 calc R . H33B H 1.2995(3) 0.9795(2) 0.5256(2) 0.037(7) Uiso 1 calc R . C34 C 0.4444(3) 1.1334(2) 0.15821(15) 0.0318(6) Uani 1 d . . H34A H 0.4373(3) 1.1147(2) 0.20372(15) 0.028(6) Uiso 1 calc R . C35 C 0.3561(3) 1.2011(2) 0.1497(2) 0.0453(8) Uani 1 d . . H35A H 0.2617(3) 1.1733(2) 0.1421(2) 0.052(9) Uiso 1 calc R . H35B H 0.3570(3) 1.2170(2) 0.1025(2) 0.056(9) Uiso 1 calc R . C36 C 0.4090(4) 1.2873(2) 0.2241(2) 0.0690(11) Uani 1 d . . H36A H 0.3537(4) 1.3322(2) 0.2172(2) 0.073(10) Uiso 1 calc R . H36B H 0.4003(4) 1.2720(2) 0.2704(2) 0.051(9) Uiso 1 calc R . C37 C 0.5563(4) 1.3290(2) 0.2397(3) 0.0769(12) Uani 1 d . . H37A H 0.5638(4) 1.3491(2) 0.1955(3) 0.092 Uiso 1 calc R . H37B H 0.5889(4) 1.3832(2) 0.2890(3) 0.092 Uiso 1 calc R . C38 C 0.6430(3) 1.2619(2) 0.2477(2) 0.0586(9) Uani 1 d . . H38A H 0.6423(3) 1.2462(2) 0.2950(2) 0.071(11) Uiso 1 calc R . H38B H 0.7374(3) 1.2898(2) 0.2554(2) 0.065(10) Uiso 1 calc R . C39 C 0.5919(3) 1.1756(2) 0.1743(2) 0.0435(7) Uani 1 d . . H39A H 0.6013(3) 1.1903(2) 0.1279(2) 0.052 Uiso 1 calc R . H39B H 0.6476(3) 1.1311(2) 0.1821(2) 0.052 Uiso 1 calc R . C40 C 0.2575(2) 0.9986(2) 0.05249(14) 0.0316(6) Uani 1 d . . H40A H 0.1991(2) 1.0394(2) 0.03661(14) 0.038 Uiso 1 calc R . C41 C 0.2407(3) 0.9173(2) -0.0209(2) 0.0384(7) Uani 1 d . . H41A H 0.3044(3) 0.8795(2) -0.0068(2) 0.032(7) Uiso 1 calc R . H41B H 0.2633(3) 0.9392(2) -0.0612(2) 0.041(8) Uiso 1 calc R . C42 C 0.0966(3) 0.8594(2) -0.0557(2) 0.0494(8) Uani 1 d . . H42A H 0.0344(3) 0.8946(2) -0.0767(2) 0.072(10) Uiso 1 calc R . H42B H 0.0913(3) 0.8045(2) -0.1005(2) 0.056(9) Uiso 1 calc R . C43 C 0.0522(3) 0.8307(2) 0.0057(2) 0.0526(8) Uani 1 d . . H43A H -0.0440(3) 0.7979(2) -0.0177(2) 0.070(10) Uiso 1 calc R . H43B H 0.1063(3) 0.7884(2) 0.0213(2) 0.053(8) Uiso 1 calc R . C44 C 0.0696(3) 0.9118(2) 0.0783(2) 0.0480(8) Uani 1 d . . H44A H 0.0454(3) 0.8905(2) 0.1185(2) 0.092(13) Uiso 1 calc R . H44B H 0.0074(3) 0.9504(2) 0.0639(2) 0.052(8) Uiso 1 calc R . C45 C 0.2152(3) 0.9686(2) 0.1140(2) 0.0408(7) Uani 1 d . . H45A H 0.2221(3) 1.0229(2) 0.1597(2) 0.035(7) Uiso 1 calc R . H45B H 0.2767(3) 0.9321(2) 0.1333(2) 0.047(8) Uiso 1 calc R . O7 O 0.4728(3) 0.9691(2) 0.2736(2) 0.0800(8) Uani 1 d D . H7 H 0.5018(43) 0.9644(7) 0.2352(15) 0.120 Uiso 1 calc R . C70 C 0.3988(3) 0.8820(2) 0.2639(3) 0.105(2) Uani 1 d D . C71 C 0.4905(4) 0.8302(3) 0.3011(2) 0.0797(12) Uani 1 d D . H71A H 0.5467(20) 0.8088(16) 0.2683(9) 0.120 Uiso 1 calc R . H71B H 0.4358(4) 0.7779(11) 0.3049(15) 0.120 Uiso 1 calc R . H71C H 0.5488(19) 0.8704(6) 0.3543(7) 0.120 Uiso 1 calc R . C72 C 0.2724(5) 0.8887(5) 0.2862(4) 0.131(2) Uani 1 d D . H72A H 0.2970(6) 0.9263(25) 0.3424(8) 0.196 Uiso 1 calc R . H72B H 0.2229(23) 0.8276(5) 0.2772(25) 0.196 Uiso 1 calc R . H72C H 0.2150(23) 0.9165(30) 0.2537(20) 0.196 Uiso 1 calc R . O8 O 0.8892(3) 0.6361(2) 0.3763(2) 0.1261(14) Uani 1 d D . H8 H 0.9148(29) 0.6757(33) 0.3587(25) 0.189 Uiso 1 calc R . C80 C 0.7558(3) 0.5855(3) 0.3268(3) 0.128(2) Uani 1 d D . C81 C 0.7530(4) 0.5493(4) 0.2419(3) 0.106(2) Uani 1 d D . H81A H 0.7989(32) 0.5981(7) 0.2293(7) 0.159 Uiso 1 calc R . H81B H 0.6590(4) 0.5275(23) 0.2066(3) 0.159 Uiso 1 calc R . H81C H 0.7995(32) 0.4990(16) 0.2345(6) 0.159 Uiso 1 calc R . C82 C 0.6541(6) 0.6432(5) 0.3378(5) 0.189(3) Uani 1 d D . H82A H 0.6752(43) 0.6778(37) 0.3944(6) 0.283 Uiso 1 calc R . H82B H 0.5632(10) 0.6039(6) 0.3171(39) 0.283 Uiso 1 calc R . H82C H 0.6580(51) 0.6855(33) 0.3091(35) 0.283 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0523(12) 0.0290(10) 0.0325(10) 0.0059(8) 0.0172(9) 0.0133(9) O2 0.0594(13) 0.0487(12) 0.0425(11) 0.0179(9) 0.0230(10) 0.0361(11) O3 0.0598(13) 0.0488(12) 0.0279(10) 0.0119(9) 0.0035(9) 0.0272(10) O4 0.0700(14) 0.0356(11) 0.0309(10) 0.0052(8) 0.0147(10) 0.0215(10) O5 0.0573(13) 0.0519(12) 0.0410(11) 0.0213(10) 0.0163(10) 0.0360(11) O6 0.0522(12) 0.0496(12) 0.0351(11) 0.0260(9) 0.0143(9) 0.0231(10) N1 0.0287(11) 0.0256(11) 0.0284(11) 0.0074(9) 0.0097(9) 0.0102(9) N2 0.0405(13) 0.0320(12) 0.0267(12) 0.0107(9) 0.0088(10) 0.0134(10) N3 0.0328(12) 0.0289(11) 0.0294(11) 0.0140(9) 0.0118(10) 0.0124(9) C1 0.0247(12) 0.0231(12) 0.0276(13) 0.0095(10) 0.0111(11) 0.0047(10) C2 0.0266(13) 0.0246(12) 0.0314(13) 0.0118(10) 0.0074(11) 0.0081(10) C3 0.0297(13) 0.0250(12) 0.0264(13) 0.0092(10) 0.0074(11) 0.0065(10) C4 0.0305(13) 0.0231(12) 0.0292(13) 0.0073(10) 0.0112(11) 0.0092(10) C5 0.0254(13) 0.0220(12) 0.0326(13) 0.0139(10) 0.0106(11) 0.0065(10) C6 0.0264(13) 0.0246(12) 0.0244(12) 0.0096(10) 0.0094(10) 0.0035(10) C7 0.0324(14) 0.0261(13) 0.0355(15) 0.0112(11) 0.0165(12) 0.0085(11) C8 0.040(2) 0.0271(13) 0.0299(14) 0.0071(11) 0.0086(12) 0.0082(12) C9 0.0327(14) 0.0273(13) 0.0333(14) 0.0175(11) 0.0104(12) 0.0092(11) C10 0.0332(14) 0.0304(13) 0.0325(14) 0.0127(11) 0.0090(12) 0.0116(11) C11 0.067(2) 0.042(2) 0.035(2) 0.0104(13) 0.0061(15) 0.010(2) C12 0.094(3) 0.065(2) 0.031(2) 0.016(2) 0.003(2) 0.009(2) C13 0.085(3) 0.089(3) 0.038(2) 0.035(2) 0.025(2) 0.037(2) C14 0.051(2) 0.071(2) 0.050(2) 0.036(2) 0.022(2) 0.017(2) C15 0.040(2) 0.046(2) 0.038(2) 0.0190(14) 0.0143(13) 0.0091(13) C16 0.0301(14) 0.0247(13) 0.0358(14) 0.0098(11) 0.0099(12) 0.0047(11) C17 0.0344(15) 0.0350(15) 0.0393(15) 0.0177(12) 0.0129(12) 0.0118(12) C18 0.046(2) 0.038(2) 0.049(2) 0.0224(13) 0.0155(14) 0.0080(13) C19 0.036(2) 0.047(2) 0.051(2) 0.0194(14) 0.0169(14) 0.0020(13) C20 0.033(2) 0.049(2) 0.053(2) 0.0188(15) 0.0140(14) 0.0057(13) C21 0.0305(14) 0.041(2) 0.047(2) 0.0207(13) 0.0122(13) 0.0095(12) C22 0.042(2) 0.0357(15) 0.0366(15) 0.0146(12) 0.0155(13) 0.0116(12) C23 0.053(2) 0.051(2) 0.033(2) 0.0164(14) 0.0150(14) 0.0121(15) C24 0.082(3) 0.076(3) 0.054(2) 0.034(2) 0.033(2) 0.017(2) C25 0.085(3) 0.091(3) 0.077(3) 0.031(2) 0.056(2) 0.019(2) C26 0.051(2) 0.110(4) 0.092(3) 0.036(3) 0.036(2) 0.015(2) C27 0.045(2) 0.080(3) 0.054(2) 0.026(2) 0.019(2) 0.021(2) C28 0.040(2) 0.0348(14) 0.0296(14) 0.0113(11) 0.0106(12) 0.0137(12) C29 0.055(2) 0.0331(15) 0.045(2) 0.0189(13) 0.021(2) 0.0196(14) C30 0.065(2) 0.051(2) 0.052(2) 0.020(2) 0.026(2) 0.030(2) C31 0.056(2) 0.061(2) 0.058(2) 0.015(2) 0.026(2) 0.026(2) C32 0.051(2) 0.056(2) 0.065(2) 0.016(2) 0.031(2) 0.010(2) C33 0.055(2) 0.035(2) 0.048(2) 0.0134(14) 0.019(2) 0.0096(14) C34 0.0357(15) 0.0311(14) 0.0277(13) 0.0079(11) 0.0102(12) 0.0112(11) C35 0.043(2) 0.035(2) 0.054(2) 0.0090(14) 0.0140(15) 0.0177(13) C36 0.066(2) 0.042(2) 0.081(3) -0.003(2) 0.021(2) 0.019(2) C37 0.076(3) 0.034(2) 0.093(3) -0.003(2) 0.017(2) 0.001(2) C38 0.047(2) 0.051(2) 0.057(2) 0.001(2) 0.012(2) -0.002(2) C39 0.041(2) 0.047(2) 0.042(2) 0.0135(14) 0.0149(14) 0.0115(14) C40 0.0316(14) 0.0306(14) 0.0341(14) 0.0134(11) 0.0091(12) 0.0106(11) C41 0.049(2) 0.0314(14) 0.037(2) 0.0125(12) 0.0168(14) 0.0117(13) C42 0.055(2) 0.034(2) 0.048(2) 0.0081(14) 0.008(2) 0.0047(14) C43 0.046(2) 0.040(2) 0.073(2) 0.024(2) 0.018(2) 0.0070(15) C44 0.042(2) 0.051(2) 0.056(2) 0.025(2) 0.020(2) 0.0093(14) C45 0.039(2) 0.048(2) 0.040(2) 0.0204(14) 0.0157(13) 0.0083(13) O7 0.096(2) 0.070(2) 0.072(2) 0.0280(14) 0.025(2) 0.0114(15) C70 0.086(3) 0.096(3) 0.141(4) 0.084(3) 0.016(3) -0.008(3) C71 0.080(3) 0.074(3) 0.092(3) 0.027(2) 0.044(2) 0.010(2) C72 0.107(4) 0.226(7) 0.143(5) 0.142(5) 0.068(4) 0.070(4) O8 0.096(2) 0.085(2) 0.152(3) 0.054(2) -0.030(2) -0.012(2) C80 0.082(4) 0.110(4) 0.140(5) 0.037(4) -0.018(4) -0.021(3) C81 0.067(3) 0.127(4) 0.126(4) 0.074(4) 0.010(3) 0.003(3) C82 0.089(4) 0.280(10) 0.209(8) 0.097(7) 0.052(5) 0.049(6) _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 O1 C7 1.252(3) . ? O2 C7 1.256(3) . ? O3 C8 1.267(3) . ? O4 C8 1.251(3) . ? O5 C9 1.256(3) . ? O6 C9 1.248(3) . ? N1 C16 1.491(3) . ? N1 C10 1.499(3) . ? N1 H1A 0.92 . ? N1 H1B 0.92 . ? N2 C28 1.495(3) . ? N2 C22 1.499(3) . ? N2 H2A 0.92 . ? N2 H2B 0.92 . ? N3 C40 1.489(3) . ? N3 C34 1.509(3) . ? N3 H3A 0.92 . ? N3 H3B 0.92 . ? C1 C6 1.395(3) . ? C1 C2 1.396(3) . ? C1 C7 1.515(3) . ? C2 C3 1.391(3) . ? C2 H2A 0.95 . ? C3 C4 1.385(3) . ? C3 C8 1.512(3) . ? C4 C5 1.382(3) . ? C4 H4A 0.95 . ? C5 C6 1.389(3) . ? C5 C9 1.524(3) . ? C6 H6A 0.95 . ? C10 C11 1.505(4) . ? C10 C15 1.514(4) . ? C10 H10A 1.00 . ? C11 C12 1.523(4) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 C13 1.539(5) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C13 C14 1.512(4) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 C15 1.523(4) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C16 C17 1.522(4) . ? C16 C21 1.526(3) . ? C16 H16A 1.00 . ? C17 C18 1.519(4) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? C18 C19 1.515(4) . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C19 C20 1.518(4) . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? C20 C21 1.530(4) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 C23 1.512(4) . ? C22 C27 1.514(4) . ? C22 H22A 1.00 . ? C23 C24 1.534(4) . ? C23 H23A 0.99 . ? C23 H23B 0.99 . ? C24 C25 1.498(5) . ? C24 H24A 0.99 . ? C24 H24B 0.99 . ? C25 C26 1.506(6) . ? C25 H25A 0.99 . ? C25 H25B 0.99 . ? C26 C27 1.537(5) . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? C27 H27A 0.99 . ? C27 H27B 0.99 . ? C28 C33 1.519(4) . ? C28 C29 1.527(4) . ? C28 H28A 1.00 . ? C29 C30 1.516(4) . ? C29 H29A 0.99 . ? C29 H29B 0.99 . ? C30 C31 1.511(5) . ? C30 H30A 0.99 . ? C30 H30B 0.99 . ? C31 C32 1.515(4) . ? C31 H31A 0.99 . ? C31 H31B 0.99 . ? C32 C33 1.517(4) . ? C32 H32A 0.99 . ? C32 H32B 0.99 . ? C33 H33A 0.99 . ? C33 H33B 0.99 . ? C34 C35 1.520(3) . ? C34 C39 1.522(4) . ? C34 H34A 1.00 . ? C35 C36 1.533(4) . ? C35 H35A 0.99 . ? C35 H35B 0.99 . ? C36 C37 1.520(5) . ? C36 H36A 0.99 . ? C36 H36B 0.99 . ? C37 C38 1.501(5) . ? C37 H37A 0.99 . ? C37 H37B 0.99 . ? C38 C39 1.523(4) . ? C38 H38A 0.99 . ? C38 H38B 0.99 . ? C39 H39A 0.99 . ? C39 H39B 0.99 . ? C40 C45 1.517(4) . ? C40 C41 1.520(3) . ? C40 H40A 1.00 . ? C41 C42 1.525(4) . ? C41 H41A 0.99 . ? C41 H41B 0.99 . ? C42 C43 1.517(4) . ? C42 H42A 0.99 . ? C42 H42B 0.99 . ? C43 C44 1.508(4) . ? C43 H43A 0.99 . ? C43 H43B 0.99 . ? C44 C45 1.531(4) . ? C44 H44A 0.99 . ? C44 H44B 0.99 . ? C45 H45A 0.99 . ? C45 H45B 0.99 . ? O7 C70 1.4282(10) . ? O7 H7 0.84 . ? C70 C71 1.5072(10) . ? C70 C72 1.5073(10) . ? C71 H71A 0.98 . ? C71 H71B 0.98 . ? C71 H71C 0.98 . ? C72 H72A 0.98 . ? C72 H72B 0.98 . ? C72 H72C 0.98 . ? O8 C80 1.4291(10) . ? O8 H8 0.84 . ? C80 C81 1.5081(10) . ? C80 C82 1.5084(10) . ? C81 H81A 0.98 . ? C81 H81B 0.98 . ? C81 H81C 0.98 . ? C82 H82A 0.98 . ? C82 H82B 0.98 . ? C82 H82C 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C16 N1 C10 119.1(2) . . ? C16 N1 H1A 107.55(11) . . ? C10 N1 H1A 107.55(12) . . ? C16 N1 H1B 107.55(12) . . ? C10 N1 H1B 107.55(12) . . ? H1A N1 H1B 107.0 . . ? C28 N2 C22 117.6(2) . . ? C28 N2 H2A 107.89(11) . . ? C22 N2 H2A 107.89(12) . . ? C28 N2 H2B 107.89(11) . . ? C22 N2 H2B 107.90(11) . . ? H2A N2 H2B 107.2 . . ? C40 N3 C34 118.4(2) . . ? C40 N3 H3A 107.50(11) . . ? C34 N3 H3A 107.65(12) . . ? C40 N3 H3B 107.81(11) . . ? C34 N3 H3B 107.88(11) . . ? H3A N3 H3B 107.1 . . ? C6 C1 C2 119.1(2) . . ? C6 C1 C7 120.7(2) . . ? C2 C1 C7 120.1(2) . . ? C3 C2 C1 120.5(2) . . ? C3 C2 H2A 119.75(14) . . ? C1 C2 H2A 119.75(13) . . ? C4 C3 C2 119.2(2) . . ? C4 C3 C8 120.6(2) . . ? C2 C3 C8 120.1(2) . . ? C5 C4 C3 121.2(2) . . ? C5 C4 H4A 119.40(13) . . ? C3 C4 H4A 119.40(13) . . ? C4 C5 C6 119.4(2) . . ? C4 C5 C9 120.6(2) . . ? C6 C5 C9 120.0(2) . . ? C5 C6 C1 120.5(2) . . ? C5 C6 H6A 119.76(14) . . ? C1 C6 H6A 119.76(13) . . ? O1 C7 O2 125.5(2) . . ? O1 C7 C1 117.7(2) . . ? O2 C7 C1 116.7(2) . . ? O4 C8 O3 123.8(2) . . ? O4 C8 C3 118.3(2) . . ? O3 C8 C3 117.9(2) . . ? O6 C9 O5 124.8(2) . . ? O6 C9 C5 117.5(2) . . ? O5 C9 C5 117.7(2) . . ? N1 C10 C11 112.2(2) . . ? N1 C10 C15 108.0(2) . . ? C11 C10 C15 111.5(2) . . ? N1 C10 H10A 108.34(11) . . ? C11 C10 H10A 108.3(2) . . ? C15 C10 H10A 108.34(14) . . ? C10 C11 C12 109.6(3) . . ? C10 C11 H11A 109.7(2) . . ? C12 C11 H11A 109.7(2) . . ? C10 C11 H11B 109.7(2) . . ? C12 C11 H11B 109.7(2) . . ? H11A C11 H11B 108.2 . . ? C11 C12 C13 110.9(3) . . ? C11 C12 H12A 109.5(2) . . ? C13 C12 H12A 109.5(2) . . ? C11 C12 H12B 109.5(2) . . ? C13 C12 H12B 109.5(2) . . ? H12A C12 H12B 108.0 . . ? C14 C13 C12 110.2(3) . . ? C14 C13 H13A 109.6(2) . . ? C12 C13 H13A 109.6(2) . . ? C14 C13 H13B 109.6(2) . . ? C12 C13 H13B 109.6(2) . . ? H13A C13 H13B 108.1 . . ? C13 C14 C15 111.4(3) . . ? C13 C14 H14A 109.4(2) . . ? C15 C14 H14A 109.4(2) . . ? C13 C14 H14B 109.4(2) . . ? C15 C14 H14B 109.4(2) . . ? H14A C14 H14B 108.0 . . ? C10 C15 C14 111.8(2) . . ? C10 C15 H15A 109.25(14) . . ? C14 C15 H15A 109.3(2) . . ? C10 C15 H15B 109.25(14) . . ? C14 C15 H15B 109.3(2) . . ? H15A C15 H15B 107.9 . . ? N1 C16 C17 107.6(2) . . ? N1 C16 C21 112.0(2) . . ? C17 C16 C21 111.2(2) . . ? N1 C16 H16A 108.63(12) . . ? C17 C16 H16A 108.63(13) . . ? C21 C16 H16A 108.63(14) . . ? C18 C17 C16 111.4(2) . . ? C18 C17 H17A 109.34(14) . . ? C16 C17 H17A 109.34(13) . . ? C18 C17 H17B 109.34(15) . . ? C16 C17 H17B 109.34(13) . . ? H17A C17 H17B 108.0 . . ? C19 C18 C17 111.2(2) . . ? C19 C18 H18A 109.4(2) . . ? C17 C18 H18A 109.38(15) . . ? C19 C18 H18B 109.4(2) . . ? C17 C18 H18B 109.38(15) . . ? H18A C18 H18B 108.0 . . ? C18 C19 C20 110.7(2) . . ? C18 C19 H19A 109.5(2) . . ? C20 C19 H19A 109.5(2) . . ? C18 C19 H19B 109.5(2) . . ? C20 C19 H19B 109.49(15) . . ? H19A C19 H19B 108.1 . . ? C19 C20 C21 111.7(2) . . ? C19 C20 H20A 109.27(15) . . ? C21 C20 H20A 109.27(14) . . ? C19 C20 H20B 109.3(2) . . ? C21 C20 H20B 109.3(2) . . ? H20A C20 H20B 107.9 . . ? C16 C21 C20 110.6(2) . . ? C16 C21 H21A 109.53(14) . . ? C20 C21 H21A 109.5(2) . . ? C16 C21 H21B 109.53(14) . . ? C20 C21 H21B 109.5(2) . . ? H21A C21 H21B 108.1 . . ? N2 C22 C23 112.0(2) . . ? N2 C22 C27 108.7(2) . . ? C23 C22 C27 111.3(2) . . ? N2 C22 H22A 108.27(11) . . ? C23 C22 H22A 108.3(2) . . ? C27 C22 H22A 108.3(2) . . ? C22 C23 C24 110.4(3) . . ? C22 C23 H23A 109.6(2) . . ? C24 C23 H23A 109.6(2) . . ? C22 C23 H23B 109.57(14) . . ? C24 C23 H23B 109.6(2) . . ? H23A C23 H23B 108.1 . . ? C25 C24 C23 111.3(3) . . ? C25 C24 H24A 109.4(2) . . ? C23 C24 H24A 109.4(2) . . ? C25 C24 H24B 109.4(2) . . ? C23 C24 H24B 109.4(2) . . ? H24A C24 H24B 108.0 . . ? C24 C25 C26 111.4(3) . . ? C24 C25 H25A 109.3(2) . . ? C26 C25 H25A 109.3(3) . . ? C24 C25 H25B 109.3(2) . . ? C26 C25 H25B 109.3(2) . . ? H25A C25 H25B 108.0 . . ? C25 C26 C27 111.9(3) . . ? C25 C26 H26A 109.2(2) . . ? C27 C26 H26A 109.2(2) . . ? C25 C26 H26B 109.2(3) . . ? C27 C26 H26B 109.2(2) . . ? H26A C26 H26B 107.9 . . ? C22 C27 C26 110.1(3) . . ? C22 C27 H27A 109.6(2) . . ? C26 C27 H27A 109.6(2) . . ? C22 C27 H27B 109.6(2) . . ? C26 C27 H27B 109.6(2) . . ? H27A C27 H27B 108.1 . . ? N2 C28 C33 108.9(2) . . ? N2 C28 C29 111.2(2) . . ? C33 C28 C29 110.7(2) . . ? N2 C28 H28A 108.66(11) . . ? C33 C28 H28A 108.7(2) . . ? C29 C28 H28A 108.66(15) . . ? C30 C29 C28 110.7(2) . . ? C30 C29 H29A 109.5(2) . . ? C28 C29 H29A 109.49(15) . . ? C30 C29 H29B 109.5(2) . . ? C28 C29 H29B 109.50(15) . . ? H29A C29 H29B 108.1 . . ? C31 C30 C29 111.3(3) . . ? C31 C30 H30A 109.4(2) . . ? C29 C30 H30A 109.4(2) . . ? C31 C30 H30B 109.4(2) . . ? C29 C30 H30B 109.4(2) . . ? H30A C30 H30B 108.0 . . ? C30 C31 C32 110.5(2) . . ? C30 C31 H31A 109.5(2) . . ? C32 C31 H31A 109.5(2) . . ? C30 C31 H31B 109.5(2) . . ? C32 C31 H31B 109.5(2) . . ? H31A C31 H31B 108.1 . . ? C31 C32 C33 111.6(3) . . ? C31 C32 H32A 109.3(2) . . ? C33 C32 H32A 109.3(2) . . ? C31 C32 H32B 109.3(2) . . ? C33 C32 H32B 109.3(2) . . ? H32A C32 H32B 108.0 . . ? C32 C33 C28 110.8(2) . . ? C32 C33 H33A 109.5(2) . . ? C28 C33 H33A 109.5(2) . . ? C32 C33 H33B 109.5(2) . . ? C28 C33 H33B 109.48(14) . . ? H33A C33 H33B 108.1 . . ? N3 C34 C35 111.8(2) . . ? N3 C34 C39 107.6(2) . . ? C35 C34 C39 111.2(2) . . ? N3 C34 H34A 108.70(12) . . ? C35 C34 H34A 108.7(2) . . ? C39 C34 H34A 108.71(15) . . ? C34 C35 C36 109.8(2) . . ? C34 C35 H35A 109.7(2) . . ? C36 C35 H35A 109.7(2) . . ? C34 C35 H35B 109.7(2) . . ? C36 C35 H35B 109.7(2) . . ? H35A C35 H35B 108.2 . . ? C37 C36 C35 111.0(3) . . ? C37 C36 H36A 109.4(2) . . ? C35 C36 H36A 109.4(2) . . ? C37 C36 H36B 109.4(2) . . ? C35 C36 H36B 109.4(2) . . ? H36A C36 H36B 108.0 . . ? C38 C37 C36 111.1(3) . . ? C38 C37 H37A 109.4(2) . . ? C36 C37 H37A 109.4(2) . . ? C38 C37 H37B 109.4(2) . . ? C36 C37 H37B 109.4(2) . . ? H37A C37 H37B 108.0 . . ? C37 C38 C39 110.9(3) . . ? C37 C38 H38A 109.5(2) . . ? C39 C38 H38A 109.5(2) . . ? C37 C38 H38B 109.5(2) . . ? C39 C38 H38B 109.5(2) . . ? H38A C38 H38B 108.0 . . ? C34 C39 C38 110.9(2) . . ? C34 C39 H39A 109.46(15) . . ? C38 C39 H39A 109.5(2) . . ? C34 C39 H39B 109.45(14) . . ? C38 C39 H39B 109.5(2) . . ? H39A C39 H39B 108.0 . . ? N3 C40 C45 111.6(2) . . ? N3 C40 C41 108.1(2) . . ? C45 C40 C41 111.2(2) . . ? N3 C40 H40A 108.66(11) . . ? C45 C40 H40A 108.66(14) . . ? C41 C40 H40A 108.66(14) . . ? C40 C41 C42 111.5(2) . . ? C40 C41 H41A 109.34(14) . . ? C42 C41 H41A 109.34(15) . . ? C40 C41 H41B 109.33(14) . . ? C42 C41 H41B 109.3(2) . . ? H41A C41 H41B 108.0 . . ? C43 C42 C41 111.7(2) . . ? C43 C42 H42A 109.3(2) . . ? C41 C42 H42A 109.3(2) . . ? C43 C42 H42B 109.3(2) . . ? C41 C42 H42B 109.29(15) . . ? H42A C42 H42B 107.9 . . ? C44 C43 C42 111.3(2) . . ? C44 C43 H43A 109.4(2) . . ? C42 C43 H43A 109.4(2) . . ? C44 C43 H43B 109.4(2) . . ? C42 C43 H43B 109.4(2) . . ? H43A C43 H43B 108.0 . . ? C43 C44 C45 111.6(2) . . ? C43 C44 H44A 109.3(2) . . ? C45 C44 H44A 109.3(2) . . ? C43 C44 H44B 109.3(2) . . ? C45 C44 H44B 109.3(2) . . ? H44A C44 H44B 108.0 . . ? C40 C45 C44 110.5(2) . . ? C40 C45 H45A 109.54(14) . . ? C44 C45 H45A 109.5(2) . . ? C40 C45 H45B 109.54(14) . . ? C44 C45 H45B 109.5(2) . . ? H45A C45 H45B 108.1 . . ? C70 O7 H7 109.5(2) . . ? O7 C70 C71 111.1(3) . . ? O7 C70 C72 111.8(4) . . ? C71 C70 C72 116.4(3) . . ? C70 C71 H71A 109.5(2) . . ? C70 C71 H71B 109.5(2) . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.5(2) . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C70 C72 H72A 109.5(3) . . ? C70 C72 H72B 109.5(3) . . ? H72A C72 H72B 109.5 . . ? C70 C72 H72C 109.5(2) . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C80 O8 H8 109.5(3) . . ? O8 C80 C81 109.2(4) . . ? O8 C80 C82 110.5(4) . . ? C81 C80 C82 112.6(5) . . ? C80 C81 H81A 109.5(3) . . ? C80 C81 H81B 109.5(2) . . ? H81A C81 H81B 109.5 . . ? C80 C81 H81C 109.5(3) . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C80 C82 H82A 109.5(4) . . ? C80 C82 H82B 109.5(3) . . ? H82A C82 H82B 109.47(5) . . ? C80 C82 H82C 109.5(4) . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? 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 C6 C1 C2 C3 0.7(4) . . . . ? C7 C1 C2 C3 -177.2(2) . . . . ? C1 C2 C3 C4 0.4(4) . . . . ? C1 C2 C3 C8 179.3(2) . . . . ? C2 C3 C4 C5 -0.7(4) . . . . ? C8 C3 C4 C5 -179.5(2) . . . . ? C3 C4 C5 C6 -0.2(4) . . . . ? C3 C4 C5 C9 178.2(2) . . . . ? C4 C5 C6 C1 1.3(4) . . . . ? C9 C5 C6 C1 -177.1(2) . . . . ? C2 C1 C6 C5 -1.6(3) . . . . ? C7 C1 C6 C5 176.4(2) . . . . ? C6 C1 C7 O1 1.2(4) . . . . ? C2 C1 C7 O1 179.1(2) . . . . ? C6 C1 C7 O2 -177.8(2) . . . . ? C2 C1 C7 O2 0.1(4) . . . . ? C4 C3 C8 O4 -6.4(4) . . . . ? C2 C3 C8 O4 174.7(2) . . . . ? C4 C3 C8 O3 172.3(2) . . . . ? C2 C3 C8 O3 -6.5(4) . . . . ? C4 C5 C9 O6 174.8(2) . . . . ? C6 C5 C9 O6 -6.8(3) . . . . ? C4 C5 C9 O5 -5.7(4) . . . . ? C6 C5 C9 O5 172.7(2) . . . . ? C16 N1 C10 C11 -54.3(3) . . . . ? C16 N1 C10 C15 -177.6(2) . . . . ? N1 C10 C11 C12 -178.7(3) . . . . ? C15 C10 C11 C12 -57.4(3) . . . . ? C10 C11 C12 C13 58.6(4) . . . . ? C11 C12 C13 C14 -57.5(4) . . . . ? C12 C13 C14 C15 54.7(4) . . . . ? N1 C10 C15 C14 179.3(2) . . . . ? C11 C10 C15 C14 55.6(3) . . . . ? C13 C14 C15 C10 -54.1(3) . . . . ? C10 N1 C16 C17 178.2(2) . . . . ? C10 N1 C16 C21 -59.2(3) . . . . ? N1 C16 C17 C18 178.5(2) . . . . ? C21 C16 C17 C18 55.4(3) . . . . ? C16 C17 C18 C19 -56.0(3) . . . . ? C17 C18 C19 C20 56.1(3) . . . . ? C18 C19 C20 C21 -56.1(3) . . . . ? N1 C16 C21 C20 -175.2(2) . . . . ? C17 C16 C21 C20 -54.7(3) . . . . ? C19 C20 C21 C16 55.4(3) . . . . ? C28 N2 C22 C23 51.3(3) . . . . ? C28 N2 C22 C27 174.6(2) . . . . ? N2 C22 C23 C24 179.0(2) . . . . ? C27 C22 C23 C24 57.1(3) . . . . ? C22 C23 C24 C25 -56.4(4) . . . . ? C23 C24 C25 C26 55.4(5) . . . . ? C24 C25 C26 C27 -55.0(5) . . . . ? N2 C22 C27 C26 -180.0(3) . . . . ? C23 C22 C27 C26 -56.2(4) . . . . ? C25 C26 C27 C22 55.0(4) . . . . ? C22 N2 C28 C33 178.2(2) . . . . ? C22 N2 C28 C29 56.0(3) . . . . ? N2 C28 C29 C30 177.3(2) . . . . ? C33 C28 C29 C30 56.1(3) . . . . ? C28 C29 C30 C31 -56.7(3) . . . . ? C29 C30 C31 C32 56.5(4) . . . . ? C30 C31 C32 C33 -56.2(4) . . . . ? C31 C32 C33 C28 56.0(3) . . . . ? N2 C28 C33 C32 -178.2(2) . . . . ? C29 C28 C33 C32 -55.6(3) . . . . ? C40 N3 C34 C35 -53.7(3) . . . . ? C40 N3 C34 C39 -176.1(2) . . . . ? N3 C34 C35 C36 -176.7(3) . . . . ? C39 C34 C35 C36 -56.3(3) . . . . ? C34 C35 C36 C37 56.5(4) . . . . ? C35 C36 C37 C38 -57.1(4) . . . . ? C36 C37 C38 C39 56.5(4) . . . . ? N3 C34 C39 C38 179.2(2) . . . . ? C35 C34 C39 C38 56.4(3) . . . . ? C37 C38 C39 C34 -56.1(4) . . . . ? C34 N3 C40 C45 -57.0(3) . . . . ? C34 N3 C40 C41 -179.5(2) . . . . ? N3 C40 C41 C42 178.0(2) . . . . ? C45 C40 C41 C42 55.3(3) . . . . ? C40 C41 C42 C43 -54.2(3) . . . . ? C41 C42 C43 C44 54.2(3) . . . . ? C42 C43 C44 C45 -55.4(3) . . . . ? N3 C40 C45 C44 -176.7(2) . . . . ? C41 C40 C45 C44 -56.0(3) . . . . ? C43 C44 C45 C40 56.4(3) . . . . ? _refine_diff_density_max 0.648 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.056 data_99033sq _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'tris-dicyclohexyammoniumtrimesate methanol-acetone clathrate' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C45 H75 N3 O6' _chemical_formula_weight 754.08 _chemical_melting_point ? _chemical_compound_source 'D. Plaut, Prof. M. Ward' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.9805(3) _cell_length_b 19.5242(4) _cell_length_c 20.0428(4) _cell_angle_alpha 116.268(1) _cell_angle_beta 111.491(1) _cell_angle_gamma 95.189(1) _cell_volume 5284.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 20573 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'irregular block' _exptl_crystal_colour colorless _exptl_crystal_size_max 1.0 _exptl_crystal_size_mid 0.8 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.948 _exptl_crystal_density_method ? _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 0.062 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.900245 _exptl_absorpt_correction_T_max 1.000000 _exptl_special_details ; Data set has been modified for disordered solvent (PLATON, A. Spek). ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'SMART CCD System, Siemens' _diffrn_measurement_method 'area detector, omega-scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35303 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0431 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 25.05 _reflns_number_total 17825 _reflns_number_observed 13363 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART, Siemens' _computing_cell_refinement 'SAINT, Siemens' _computing_data_reduction 'SAINT, Siemens' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL, Siemens' _computing_publication_material ? _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^)+(0.0613P)^2^+2.1815P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17825 _refine_ls_number_parameters 1058 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_obs 0.0563 _refine_ls_wR_factor_all 0.1478 _refine_ls_wR_factor_obs 0.1379 _refine_ls_goodness_of_fit_all 1.061 _refine_ls_goodness_of_fit_obs 1.153 _refine_ls_restrained_S_all 1.061 _refine_ls_restrained_S_obs 1.153 _refine_ls_shift/esd_max 0.012 _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 O1 O 0.42687(10) 0.37465(9) 0.49971(9) 0.0408(4) Uani 1 d . . O2 O 0.48206(13) 0.48827(9) 0.62294(10) 0.0533(4) Uani 1 d . . O3 O 0.45710(10) 0.45506(9) 0.85153(9) 0.0399(4) Uani 1 d . . O4 O 0.54525(10) 0.38537(9) 0.88645(8) 0.0419(4) Uani 1 d . . O5 O 0.49784(10) 0.12675(8) 0.62735(9) 0.0396(4) Uani 1 d . . O6 O 0.45595(10) 0.12589(8) 0.50720(9) 0.0426(4) Uani 1 d . . O7 O 1.00691(10) 0.86918(8) 0.36967(9) 0.0392(4) Uani 1 d . . O8 O 1.02714(10) 0.86673(8) 0.48519(9) 0.0378(3) Uani 1 d . . O9 O 1.06006(11) 0.62404(10) 0.49782(9) 0.0446(4) Uani 1 d . . O10 O 1.02906(12) 0.50933(9) 0.38088(10) 0.0487(4) Uani 1 d . . O11 O 0.97413(9) 0.51198(8) 0.12054(8) 0.0345(3) Uani 1 d . . O12 O 0.97538(11) 0.62705(9) 0.12190(9) 0.0436(4) Uani 1 d . . N1 N 0.50646(11) 0.61357(9) 0.60326(10) 0.0339(4) Uani 1 d . . H1A H 0.52980(11) 0.61016(9) 0.56748(10) 0.038(6) Uiso 1 calc R . H1B H 0.49832(11) 0.56496(9) 0.60046(10) 0.053(7) Uiso 1 calc R . N2 N 0.63335(10) 0.50289(9) 1.05690(10) 0.0291(4) Uani 1 d . . H2A H 0.59324(10) 0.51708(9) 1.07732(10) 0.050(7) Uiso 1 calc R . H2B H 0.60118(10) 0.46708(9) 1.00040(10) 0.043(6) Uiso 1 calc R . N3 N 0.39699(10) -0.02863(9) 0.38200(10) 0.0285(4) Uani 1 d . . H3A H 0.41938(10) 0.02175(9) 0.42881(10) 0.043(6) Uiso 1 calc R . H3B H 0.43947(10) -0.05425(9) 0.38967(10) 0.033(6) Uiso 1 calc R . N4 N 0.95633(11) 0.97164(9) 0.57025(10) 0.0312(4) Uani 1 d . . H4A H 0.98626(11) 0.94712(9) 0.54094(10) 0.037(6) Uiso 1 calc R . H4B H 0.97182(11) 1.02478(9) 0.58588(10) 0.054(7) Uiso 1 calc R . N5 N 1.04868(11) 0.40448(10) 0.43565(10) 0.0354(4) Uiso 1 d . . H5A H 1.01016(11) 0.40237(10) 0.45765(10) 0.034(5) Uiso 1 calc R . H5B H 1.04526(11) 0.44529(10) 0.42442(10) 0.104(11) Uiso 1 calc R . N6 N 0.95484(10) 0.58543(9) -0.03017(9) 0.0265(3) Uani 1 d . . H6A H 0.96597(10) 0.59359(9) 0.02172(9) 0.054(7) Uiso 1 calc R . H6B H 0.98419(10) 0.55030(9) -0.05034(9) 0.040(6) Uiso 1 calc R . C1 C 0.46840(12) 0.36737(10) 0.62353(11) 0.0239(4) Uani 1 d . . C2 C 0.46872(12) 0.28811(11) 0.58480(11) 0.0251(4) Uani 1 d . . H2A H 0.45854(12) 0.26149(11) 0.52828(11) 0.022(5) Uiso 1 calc R . C3 C 0.48393(11) 0.24748(10) 0.62856(11) 0.0240(4) Uani 1 d . . C4 C 0.49849(11) 0.28693(11) 0.71107(11) 0.0247(4) Uani 1 d . . H4A H 0.51267(11) 0.26075(11) 0.74219(11) 0.026(5) Uiso 1 calc R . C5 C 0.49255(11) 0.36458(11) 0.74889(11) 0.0248(4) Uani 1 d . . C6 C 0.47841(12) 0.40451(11) 0.70486(11) 0.0255(4) Uani 1 d . . H6A H 0.47553(12) 0.45777(11) 0.73054(11) 0.032(5) Uiso 1 calc R . C7 C 0.45799(13) 0.41353(12) 0.57843(13) 0.0320(4) Uani 1 d . . C8 C 0.47915(13) 0.15990(11) 0.58428(13) 0.0300(4) Uani 1 d . . C9 C 0.49907(13) 0.40482(11) 0.83595(12) 0.0303(4) Uani 1 d . . C10 C 1.01114(11) 0.74681(10) 0.36727(11) 0.0234(4) Uani 1 d . . C11 C 1.02311(12) 0.70555(11) 0.41008(11) 0.0263(4) Uani 1 d . . H11A H 1.03174(12) 0.73210(11) 0.46613(11) 0.031(5) Uiso 1 calc R . C12 C 1.02261(12) 0.62601(11) 0.37198(12) 0.0275(4) Uani 1 d . . C13 C 1.00760(12) 0.58684(11) 0.28891(12) 0.0260(4) Uani 1 d . . H13A H 1.00613(12) 0.53229(11) 0.26213(12) 0.031(5) Uiso 1 calc R . C14 C 0.99476(11) 0.62691(10) 0.24490(11) 0.0229(4) Uani 1 d . . C15 C 0.99749(11) 0.70718(10) 0.28483(11) 0.0240(4) Uani 1 d . . H15A H 0.98995(11) 0.73509(10) 0.25542(11) 0.021(5) Uiso 1 calc R . C16 C 1.01512(12) 0.83444(11) 0.41054(12) 0.0282(4) Uani 1 d . . C17 C 1.03856(14) 0.58290(13) 0.42026(14) 0.0355(5) Uani 1 d . . C18 C 0.98016(12) 0.58513(11) 0.15533(11) 0.0260(4) Uani 1 d . . C19 C 0.41676(14) 0.62467(12) 0.57058(13) 0.0366(5) Uani 1 d . . H19A H 0.38944(14) 0.62539(12) 0.60731(13) 0.041(6) Uiso 1 calc R . C20 C 0.4232(2) 0.70361(13) 0.5716(2) 0.0441(5) Uani 1 d . . H20A H 0.4559(2) 0.70656(13) 0.5404(2) 0.048(7) Uiso 1 calc R . H20B H 0.4567(2) 0.74898(13) 0.6299(2) 0.040(6) Uiso 1 calc R . C21 C 0.3304(2) 0.7101(2) 0.5316(2) 0.0575(7) Uani 1 d . . H21A H 0.3007(2) 0.7136(2) 0.5668(2) 0.082(10) Uiso 1 calc R . H21B H 0.3358(2) 0.7599(2) 0.5294(2) 0.081(9) Uiso 1 calc R . C22 C 0.2741(2) 0.6391(2) 0.4443(2) 0.0584(7) Uani 1 d . . H22A H 0.3007(2) 0.6384(2) 0.4076(2) 0.051(7) Uiso 1 calc R . H22B H 0.2139(2) 0.6442(2) 0.4216(2) 0.083(9) Uiso 1 calc R . C23 C 0.2672(2) 0.5608(2) 0.4447(2) 0.0569(7) Uani 1 d . . H23A H 0.2355(2) 0.5594(2) 0.4770(2) 0.064(8) Uiso 1 calc R . H23B H 0.2325(2) 0.5150(2) 0.3867(2) 0.057(7) Uiso 1 calc R . C24 C 0.35887(15) 0.55284(13) 0.48302(14) 0.0434(5) Uani 1 d . . H24A H 0.38789(15) 0.54829(13) 0.44710(14) 0.042(6) Uiso 1 calc R . H24B H 0.35287(15) 0.50331(13) 0.48567(14) 0.041(6) Uiso 1 calc R . C25 C 0.5749(2) 0.67594(12) 0.69054(13) 0.0399(5) Uani 1 d . . H25A H 0.5873(2) 0.72843(12) 0.69329(13) 0.046(6) Uiso 1 calc R . C26 C 0.6604(2) 0.65236(14) 0.70864(15) 0.0488(6) Uani 1 d . . H26A H 0.6814(2) 0.64880(14) 0.66753(15) 0.061(8) Uiso 1 calc R . H26B H 0.6487(2) 0.59910(14) 0.70326(15) 0.048(6) Uiso 1 calc R . C27 C 0.7323(2) 0.7150(2) 0.7976(2) 0.0718(9) Uani 1 d . . H27A H 0.7865(2) 0.6979(2) 0.8095(2) 0.097(11) Uiso 1 calc R . H27B H 0.7477(2) 0.7670(2) 0.8010(2) 0.091(10) Uiso 1 calc R . C28 C 0.7016(2) 0.7257(2) 0.8625(2) 0.0757(9) Uani 1 d . . H28A H 0.7480(2) 0.7688(2) 0.9184(2) 0.098(11) Uiso 1 calc R . H28B H 0.6927(2) 0.6755(2) 0.8636(2) 0.086(10) Uiso 1 calc R . C29 C 0.6154(2) 0.7472(2) 0.8435(2) 0.0735(9) Uani 1 d . . H29A H 0.6263(2) 0.8007(2) 0.8493(2) 0.070(8) Uiso 1 calc R . H29B H 0.5946(2) 0.7500(2) 0.8845(2) 0.096(11) Uiso 1 calc R . C30 C 0.5428(2) 0.6855(2) 0.75491(15) 0.0542(7) Uani 1 d . . H30A H 0.5268(2) 0.6332(2) 0.75071(15) 0.056(7) Uiso 1 calc R . H30B H 0.4891(2) 0.7033(2) 0.74339(15) 0.056(7) Uiso 1 calc R . C31 C 0.68711(13) 0.57704(12) 1.06879(12) 0.0333(5) Uani 1 d . . H31A H 0.72582(13) 0.56130(12) 1.04063(12) 0.038(6) Uiso 1 calc R . C32 C 0.74587(14) 0.63933(13) 1.16114(13) 0.0408(5) Uani 1 d . . H32A H 0.78964(14) 0.61716(13) 1.18683(13) 0.055(7) Uiso 1 calc R . H32B H 0.70888(14) 0.65275(13) 1.19074(13) 0.047(6) Uiso 1 calc R . C33 C 0.7946(2) 0.71531(14) 1.1698(2) 0.0502(6) Uani 1 d . . H33A H 0.8303(2) 0.75621(14) 1.2298(2) 0.057(7) Uiso 1 calc R . H33B H 0.8358(2) 0.70245(14) 1.1448(2) 0.053(7) Uiso 1 calc R . C34 C 0.7307(2) 0.74968(15) 1.1272(2) 0.0586(7) Uani 1 d . . H34A H 0.7647(2) 0.79658(15) 1.1314(2) 0.061(7) Uiso 1 calc R . H34B H 0.6935(2) 0.76794(15) 1.1558(2) 0.061(8) Uiso 1 calc R . C35 C 0.6712(2) 0.6866(2) 1.0353(2) 0.0584(7) Uani 1 d . . H35A H 0.6274(2) 0.7087(2) 1.0096(2) 0.068(8) Uiso 1 calc R . H35B H 0.7078(2) 0.6729(2) 1.0054(2) 0.075(9) Uiso 1 calc R . C36 C 0.62238(15) 0.61105(13) 1.02640(14) 0.0420(5) Uani 1 d . . H36A H 0.58141(15) 0.62386(13) 1.05166(14) 0.046(6) Uiso 1 calc R . H36B H 0.58650(15) 0.57023(13) 0.96638(14) 0.049(7) Uiso 1 calc R . C37 C 0.68256(13) 0.45971(12) 1.09635(12) 0.0320(4) Uani 1 d . . H37A H 0.71017(13) 0.49553(12) 1.15842(12) 0.037(6) Uiso 1 calc R . C38 C 0.61446(14) 0.38515(13) 1.07138(14) 0.0381(5) Uani 1 d . . H38A H 0.58205(14) 0.35165(13) 1.00969(14) 0.039(6) Uiso 1 calc R . H38B H 0.57079(14) 0.40154(13) 1.09229(14) 0.058(7) Uiso 1 calc R . C39 C 0.6590(2) 0.3356(2) 1.1068(2) 0.0538(6) Uani 1 d . . H39A H 0.6829(2) 0.3658(2) 1.1684(2) 0.060(8) Uiso 1 calc R . H39B H 0.6141(2) 0.2849(2) 1.0844(2) 0.066(8) Uiso 1 calc R . C40 C 0.7338(2) 0.3166(2) 1.0844(2) 0.0612(7) Uani 1 d . . H40A H 0.7088(2) 0.2804(2) 1.0232(2) 0.062(8) Uiso 1 calc R . H40B H 0.7641(2) 0.2885(2) 1.1118(2) 0.071(8) Uiso 1 calc R . C41 C 0.8008(2) 0.3926(2) 1.1118(2) 0.0553(7) Uani 1 d . . H41A H 0.8479(2) 0.3785(2) 1.0952(2) 0.060(7) Uiso 1 calc R . H41B H 0.8290(2) 0.4271(2) 1.1734(2) 0.063(8) Uiso 1 calc R . C42 C 0.75593(15) 0.43862(14) 1.07214(15) 0.0428(5) Uani 1 d . . H42A H 0.80031(15) 0.48826(14) 1.09140(15) 0.049(7) Uiso 1 calc R . H42B H 0.73053(15) 0.40541(14) 1.01058(15) 0.047(6) Uiso 1 calc R . C43 C 0.38537(14) -0.01898(12) 0.30889(12) 0.0362(5) Uani 1 d . . H43A H 0.36892(14) -0.07315(12) 0.25913(12) 0.030(5) Uiso 1 calc R . C44 C 0.4747(2) 0.03127(14) 0.33015(14) 0.0442(6) Uani 1 d . . H44A H 0.5198(2) 0.00344(14) 0.34013(14) 0.052(7) Uiso 1 calc R . H44B H 0.4942(2) 0.08358(14) 0.38201(14) 0.052(7) Uiso 1 calc R . C45 C 0.4676(2) 0.0450(2) 0.2587(2) 0.0615(8) Uani 1 d . . H45A H 0.5248(2) 0.0810(2) 0.2755(2) 0.069(8) Uiso 1 calc R . H45B H 0.4553(2) -0.0068(2) 0.2088(2) 0.077(9) Uiso 1 calc R . C46 C 0.3942(2) 0.0819(2) 0.2370(2) 0.0712(9) Uani 1 d . . H46A H 0.4100(2) 0.1364(2) 0.2848(2) 0.066(8) Uiso 1 calc R . H46B H 0.3887(2) 0.0869(2) 0.1885(2) 0.091(10) Uiso 1 calc R . C47 C 0.3058(2) 0.0318(2) 0.2163(2) 0.0688(8) Uani 1 d . . H47A H 0.2869(2) -0.0208(2) 0.1649(2) 0.079(9) Uiso 1 calc R . H47B H 0.2604(2) 0.0590(2) 0.2053(2) 0.093(11) Uiso 1 calc R . C48 C 0.3123(2) 0.01884(15) 0.2882(2) 0.0516(6) Uani 1 d . . H48A H 0.3253(2) 0.07088(15) 0.3381(2) 0.057(7) Uiso 1 calc R . H48B H 0.2548(2) -0.01657(15) 0.2718(2) 0.061(8) Uiso 1 calc R . C49 C 0.31680(13) -0.07333(11) 0.37814(12) 0.0320(4) Uani 1 d . . H49A H 0.27116(13) -0.04454(11) 0.37250(12) 0.030(5) Uiso 1 calc R . C50 C 0.34580(14) -0.07090(12) 0.46069(13) 0.0339(5) Uani 1 d . . H50A H 0.36569(14) -0.01460(12) 0.50670(13) 0.039(6) Uiso 1 calc R . H50B H 0.39670(14) -0.09255(12) 0.47072(13) 0.027(5) Uiso 1 calc R . C51 C 0.26981(15) -0.12000(13) 0.46079(15) 0.0430(5) Uani 1 d . . H51A H 0.29171(15) -0.12029(13) 0.51371(15) 0.038(6) Uiso 1 calc R . H51B H 0.22141(15) -0.09495(13) 0.45705(15) 0.060(7) Uiso 1 calc R . C52 C 0.23405(15) -0.20607(13) 0.38691(14) 0.0425(5) Uani 1 d . . H52A H 0.28144(15) -0.23223(13) 0.39256(14) 0.045(6) Uiso 1 calc R . H52B H 0.18427(15) -0.23673(13) 0.38686(14) 0.046(6) Uiso 1 calc R . C53 C 0.20197(15) -0.20670(14) 0.30483(15) 0.0462(6) Uani 1 d . . H53A H 0.17967(15) -0.26271(14) 0.25770(15) 0.049(7) Uiso 1 calc R . H53B H 0.15224(15) -0.18335(14) 0.29781(15) 0.053(7) Uiso 1 calc R . C54 C 0.27635(14) -0.15912(12) 0.30297(13) 0.0387(5) Uani 1 d . . H54A H 0.25274(14) -0.15765(12) 0.25070(13) 0.051(7) Uiso 1 calc R . H54B H 0.32310(14) -0.18601(12) 0.30352(13) 0.039(6) Uiso 1 calc R . C55 C 0.98993(15) 0.96744(12) 0.64829(13) 0.0373(5) Uani 1 d . . H55A H 0.97986(15) 0.90982(12) 0.63193(13) 0.038(6) Uiso 1 calc R . C56 C 1.0896(2) 1.00981(14) 0.69803(14) 0.0437(5) Uani 1 d . . H56A H 1.1010(2) 1.06629(14) 0.71201(14) 0.042(6) Uiso 1 calc R . H56B H 1.1192(2) 0.98361(14) 0.66353(14) 0.042(6) Uiso 1 calc R . C57 C 1.1286(2) 1.0072(2) 0.7786(2) 0.0609(7) Uani 1 d . . H57A H 1.1232(2) 0.9511(2) 0.7646(2) 0.055(7) Uiso 1 calc R . H57B H 1.1925(2) 1.0381(2) 0.8115(2) 0.066(8) Uiso 1 calc R . C58 C 1.0805(2) 1.0423(2) 0.8306(2) 0.0671(8) Uani 1 d . . H58A H 1.1042(2) 1.0369(2) 0.8805(2) 0.081(9) Uiso 1 calc R . H58B H 1.0915(2) 1.1001(2) 0.8499(2) 0.086(10) Uiso 1 calc R . C59 C 0.9812(2) 0.9999(2) 0.7803(2) 0.0584(7) Uani 1 d . . H59A H 0.9514(2) 1.0253(2) 0.8149(2) 0.067(8) Uiso 1 calc R . H59B H 0.9700(2) 0.9432(2) 0.7654(2) 0.063(8) Uiso 1 calc R . C60 C 0.9422(2) 1.00370(14) 0.70058(14) 0.0439(5) Uani 1 d . . H60A H 0.8780(2) 0.97377(14) 0.66787(14) 0.046(6) Uiso 1 calc R . H60B H 0.9489(2) 1.06015(14) 0.71523(14) 0.051(7) Uiso 1 calc R . C61 C 0.85869(14) 0.93553(12) 0.51130(13) 0.0354(5) Uani 1 d . . H61A H 0.82598(14) 0.96599(12) 0.54077(13) 0.033(5) Uiso 1 calc R . C62 C 0.8251(2) 0.84734(13) 0.4840(2) 0.0487(6) Uani 1 d . . H62A H 0.8600(2) 0.81666(13) 0.4588(2) 0.059(7) Uiso 1 calc R . H62B H 0.8326(2) 0.84285(13) 0.5331(2) 0.050(7) Uiso 1 calc R . C63 C 0.7270(2) 0.81310(15) 0.4202(2) 0.0591(7) Uani 1 d . . H63A H 0.7057(2) 0.75575(15) 0.4014(2) 0.075(9) Uiso 1 calc R . H63B H 0.6921(2) 0.84155(15) 0.4472(2) 0.049(7) Uiso 1 calc R . C64 C 0.7119(2) 0.8214(2) 0.3449(2) 0.0635(8) Uani 1 d . . H64A H 0.6478(2) 0.7991(2) 0.3052(2) 0.060(7) Uiso 1 calc R . H64B H 0.7442(2) 0.7907(2) 0.3159(2) 0.069(8) Uiso 1 calc R . C65 C 0.7445(2) 0.9092(2) 0.3723(2) 0.0522(6) Uani 1 d . . H65A H 0.7083(2) 0.9388(2) 0.3963(2) 0.068(8) Uiso 1 calc R . H65B H 0.7373(2) 0.9136(2) 0.3232(2) 0.065(8) Uiso 1 calc R . C66 C 0.84233(14) 0.94635(13) 0.43752(13) 0.0397(5) Uani 1 d . . H66A H 0.87911(14) 0.92113(13) 0.41109(13) 0.040(6) Uiso 1 calc R . H66B H 0.86084(14) 1.00427(13) 0.45756(13) 0.041(6) Uiso 1 calc R . C67 C 1.14143(14) 0.42623(12) 0.50170(13) 0.0365(5) Uiso 1 d . . H67A H 1.18364(14) 0.42759(12) 0.47791(13) 0.046(6) Uiso 1 calc R . C68 C 1.16339(15) 0.51013(13) 0.57479(14) 0.0436(5) Uiso 1 d . . H68A H 1.15954(15) 0.54881(13) 0.55525(14) 0.066(8) Uiso 1 calc R . H68B H 1.11961(15) 0.51067(13) 0.59663(14) 0.032(5) Uiso 1 calc R . C69 C 1.2566(2) 0.5352(2) 0.6443(2) 0.0557(6) Uiso 1 d . . H69A H 1.3006(2) 0.5378(2) 0.6234(2) 0.059(7) Uiso 1 calc R . H69B H 1.2695(2) 0.5893(2) 0.6916(2) 0.095(10) Uiso 1 calc R . C70 C 1.2649(2) 0.47579(15) 0.6746(2) 0.0544(6) Uiso 1 d . . H70A H 1.2241(2) 0.47625(15) 0.6996(2) 0.060(7) Uiso 1 calc R . H70B H 1.3262(2) 0.49192(15) 0.7183(2) 0.074(8) Uiso 1 calc R . C71 C 1.2422(2) 0.3915(2) 0.6021(2) 0.0564(7) Uiso 1 d . . H71A H 1.2877(2) 0.3899(2) 0.5820(2) 0.075(9) Uiso 1 calc R . H71B H 1.2441(2) 0.3533(2) 0.6223(2) 0.072(8) Uiso 1 calc R . C72 C 1.15087(15) 0.36514(14) 0.52973(14) 0.0431(5) Uiso 1 d . . H72A H 1.10460(15) 0.35849(14) 0.54719(14) 0.048(6) Uiso 1 calc R . H72B H 1.14171(15) 0.31264(14) 0.48222(14) 0.036(5) Uiso 1 calc R . C73 C 1.01633(14) 0.32695(13) 0.35405(14) 0.0409(5) Uiso 1 d . . H73A H 1.02154(14) 0.28243(13) 0.36585(14) 0.058(7) Uiso 1 calc R . C74 C 1.0714(2) 0.3286(2) 0.3093(2) 0.0545(6) Uiso 1 d . . H74A H 1.1339(2) 0.3358(2) 0.3443(2) 0.066(8) Uiso 1 calc R . H74B H 1.0697(2) 0.3742(2) 0.2998(2) 0.026(5) Uiso 1 calc R . C75 C 1.0341(2) 0.2497(2) 0.2251(2) 0.0735(8) Uiso 1 d . . H75A H 1.0680(2) 0.2526(2) 0.1949(2) 0.083(9) Uiso 1 calc R . H75B H 1.0423(2) 0.2051(2) 0.2354(2) 0.062(7) Uiso 1 calc R . C76 C 0.9366(2) 0.2324(2) 0.1711(2) 0.0677(8) Uiso 1 d . . H76A H 0.9288(2) 0.2736(2) 0.1553(2) 0.055(7) Uiso 1 calc R . H76B H 0.9146(2) 0.1796(2) 0.1192(2) 0.145(15) Uiso 1 calc R . C77 C 0.8834(2) 0.2321(2) 0.2169(2) 0.0596(7) Uiso 1 d . . H77A H 0.8868(2) 0.1876(2) 0.2281(2) 0.091(10) Uiso 1 calc R . H77B H 0.8204(2) 0.2231(2) 0.1815(2) 0.062(7) Uiso 1 calc R . C78 C 0.9187(2) 0.31198(14) 0.29992(15) 0.0484(6) Uiso 1 d . . H78A H 0.9120(2) 0.35627(14) 0.28879(15) 0.067(8) Uiso 1 calc R . H78B H 0.8839(2) 0.31019(14) 0.32970(15) 0.067(8) Uiso 1 calc R . C79 C 0.99570(13) 0.66378(11) -0.01849(12) 0.0300(4) Uani 1 d . . H79A H 0.99033(13) 0.65412(11) -0.07354(12) 0.024(5) Uiso 1 calc R . C80 C 1.09417(14) 0.69359(12) 0.04262(13) 0.0355(5) Uani 1 d . . H80A H 1.12282(14) 0.65275(12) 0.02091(13) 0.045(6) Uiso 1 calc R . H80B H 1.10094(14) 0.70167(12) 0.09704(13) 0.037(6) Uiso 1 calc R . C81 C 1.1401(2) 0.77272(13) 0.05507(15) 0.0458(6) Uani 1 d . . H81A H 1.2030(2) 0.79263(13) 0.09741(15) 0.058(7) Uiso 1 calc R . H81B H 1.1389(2) 0.76329(13) 0.00190(15) 0.053(7) Uiso 1 calc R . C82 C 1.0946(2) 0.83530(13) 0.0833(2) 0.0505(6) Uani 1 d . . H82A H 1.1227(2) 0.88428(13) 0.0868(2) 0.054(7) Uiso 1 calc R . H82B H 1.1022(2) 0.84958(13) 0.1397(2) 0.061(8) Uiso 1 calc R . C83 C 0.9957(2) 0.80464(12) 0.02290(15) 0.0464(6) Uani 1 d . . H83A H 0.9881(2) 0.79579(12) -0.03198(15) 0.047(6) Uiso 1 calc R . H83B H 0.9672(2) 0.84568(12) 0.04451(15) 0.051(7) Uiso 1 calc R . C84 C 0.94978(14) 0.72607(12) 0.01152(13) 0.0363(5) Uani 1 d . . H84A H 0.95267(14) 0.73553(12) 0.06525(13) 0.036(6) Uiso 1 calc R . H84B H 0.88649(14) 0.70630(12) -0.02985(13) 0.031(5) Uiso 1 calc R . C85 C 0.85692(12) 0.54479(11) -0.08647(12) 0.0287(4) Uani 1 d . . H85A H 0.82389(12) 0.57798(11) -0.05973(12) 0.034(5) Uiso 1 calc R . C86 C 0.83546(13) 0.46387(12) -0.09238(13) 0.0337(5) Uani 1 d . . H86A H 0.84856(13) 0.47295(12) -0.03623(13) 0.058(7) Uiso 1 calc R . H86B H 0.87394(13) 0.43339(12) -0.11150(13) 0.028(5) Uiso 1 calc R . C87 C 0.73801(14) 0.41441(14) -0.15281(14) 0.0410(5) Uani 1 d . . H87A H 0.72793(14) 0.36092(14) -0.15857(14) 0.058(7) Uiso 1 calc R . H87B H 0.69957(14) 0.44132(14) -0.12995(14) 0.057(7) Uiso 1 calc R . C88 C 0.71317(14) 0.40473(13) -0.23817(13) 0.0393(5) Uani 1 d . . H88A H 0.64955(14) 0.37410(13) -0.27573(13) 0.039(6) Uiso 1 calc R . H88B H 0.74850(14) 0.37438(13) -0.26297(13) 0.041(6) Uiso 1 calc R . C89 C 0.73088(14) 0.48705(13) -0.22996(14) 0.0421(5) Uani 1 d . . H89A H 0.69400(14) 0.51660(13) -0.20688(14) 0.044(6) Uiso 1 calc R . H89B H 0.71403(14) 0.48017(13) -0.28586(14) 0.039(6) Uiso 1 calc R . C90 C 0.82952(14) 0.53564(12) -0.17230(12) 0.0344(5) Uani 1 d . . H90A H 0.86627(14) 0.50798(12) -0.19718(12) 0.040(6) Uiso 1 calc R . H90B H 0.83956(14) 0.58922(12) -0.16635(12) 0.043(6) Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0538(9) 0.0444(8) 0.0308(8) 0.0254(7) 0.0184(7) 0.0133(7) O2 0.0926(13) 0.0282(8) 0.0486(10) 0.0258(8) 0.0333(9) 0.0198(8) O3 0.0478(9) 0.0421(8) 0.0309(8) 0.0139(7) 0.0239(7) 0.0185(7) O4 0.0539(9) 0.0456(9) 0.0234(7) 0.0169(7) 0.0156(7) 0.0163(7) O5 0.0529(9) 0.0288(7) 0.0522(9) 0.0254(7) 0.0305(8) 0.0218(7) O6 0.0590(10) 0.0250(7) 0.0371(9) 0.0089(7) 0.0239(8) 0.0137(7) O7 0.0587(10) 0.0215(7) 0.0363(8) 0.0132(6) 0.0222(7) 0.0137(6) O8 0.0509(9) 0.0275(7) 0.0312(8) 0.0077(6) 0.0240(7) 0.0123(6) O9 0.0611(10) 0.0596(10) 0.0401(9) 0.0370(8) 0.0318(8) 0.0320(8) O10 0.0764(12) 0.0417(9) 0.0537(10) 0.0365(8) 0.0370(9) 0.0284(8) O11 0.0430(8) 0.0253(7) 0.0288(7) 0.0069(6) 0.0190(6) 0.0095(6) O12 0.0756(11) 0.0369(8) 0.0266(8) 0.0190(7) 0.0273(8) 0.0201(8) N1 0.0489(10) 0.0255(9) 0.0339(9) 0.0191(8) 0.0203(8) 0.0129(8) N2 0.0307(9) 0.0323(9) 0.0214(8) 0.0116(7) 0.0114(7) 0.0106(7) N3 0.0354(9) 0.0210(8) 0.0268(9) 0.0113(7) 0.0129(7) 0.0100(7) N4 0.0416(10) 0.0206(8) 0.0368(9) 0.0131(7) 0.0247(8) 0.0111(7) N6 0.0345(9) 0.0233(8) 0.0213(8) 0.0110(7) 0.0125(7) 0.0103(7) C1 0.0249(9) 0.0239(9) 0.0250(9) 0.0134(8) 0.0121(8) 0.0087(7) C2 0.0245(9) 0.0255(9) 0.0216(9) 0.0096(8) 0.0107(8) 0.0045(7) C3 0.0218(9) 0.0204(9) 0.0280(10) 0.0112(8) 0.0113(8) 0.0061(7) C4 0.0242(9) 0.0251(9) 0.0267(10) 0.0156(8) 0.0105(8) 0.0067(7) C5 0.0221(9) 0.0260(9) 0.0210(9) 0.0096(8) 0.0083(7) 0.0044(7) C6 0.0269(10) 0.0194(9) 0.0273(10) 0.0099(8) 0.0121(8) 0.0073(7) C7 0.0367(11) 0.0322(11) 0.0343(12) 0.0216(9) 0.0170(9) 0.0127(9) C8 0.0301(10) 0.0235(10) 0.0408(12) 0.0159(9) 0.0205(9) 0.0108(8) C9 0.0319(10) 0.0301(10) 0.0230(10) 0.0105(8) 0.0122(8) 0.0034(8) C10 0.0240(9) 0.0216(9) 0.0234(9) 0.0100(8) 0.0118(8) 0.0062(7) C11 0.0294(10) 0.0294(10) 0.0218(9) 0.0119(8) 0.0146(8) 0.0096(8) C12 0.0307(10) 0.0309(10) 0.0286(10) 0.0184(9) 0.0167(8) 0.0112(8) C13 0.0303(10) 0.0218(9) 0.0296(10) 0.0139(8) 0.0158(8) 0.0100(8) C14 0.0230(9) 0.0218(9) 0.0228(9) 0.0104(8) 0.0108(7) 0.0062(7) C15 0.0242(9) 0.0240(9) 0.0245(9) 0.0137(8) 0.0105(8) 0.0063(7) C16 0.0293(10) 0.0218(9) 0.0282(10) 0.0084(8) 0.0137(8) 0.0061(8) C17 0.0425(12) 0.0418(12) 0.0428(13) 0.0303(11) 0.0265(10) 0.0211(10) C18 0.0266(10) 0.0254(10) 0.0225(9) 0.0088(8) 0.0122(8) 0.0075(8) C19 0.0468(12) 0.0352(11) 0.0376(12) 0.0223(10) 0.0234(10) 0.0158(10) C20 0.0561(14) 0.0360(12) 0.0470(14) 0.0253(11) 0.0234(12) 0.0202(11) C21 0.065(2) 0.062(2) 0.067(2) 0.0433(15) 0.0341(15) 0.0372(14) C22 0.0455(14) 0.071(2) 0.070(2) 0.049(2) 0.0200(13) 0.0211(13) C23 0.0481(14) 0.065(2) 0.060(2) 0.0430(15) 0.0161(13) 0.0059(12) C24 0.0498(13) 0.0360(12) 0.0436(13) 0.0239(10) 0.0177(11) 0.0065(10) C25 0.0544(14) 0.0271(10) 0.0326(11) 0.0160(9) 0.0135(10) 0.0118(10) C26 0.0551(15) 0.0470(14) 0.0471(14) 0.0306(12) 0.0179(12) 0.0158(11) C27 0.066(2) 0.069(2) 0.061(2) 0.041(2) 0.0029(15) 0.0099(15) C28 0.096(2) 0.059(2) 0.045(2) 0.0282(14) 0.004(2) 0.023(2) C29 0.114(3) 0.055(2) 0.0363(14) 0.0192(13) 0.022(2) 0.035(2) C30 0.079(2) 0.0523(15) 0.0374(13) 0.0230(12) 0.0298(13) 0.0312(14) C31 0.0336(11) 0.0336(11) 0.0300(11) 0.0147(9) 0.0144(9) 0.0080(9) C32 0.0363(12) 0.0369(12) 0.0353(12) 0.0138(10) 0.0091(10) 0.0097(9) C33 0.0389(13) 0.0370(12) 0.0508(15) 0.0154(11) 0.0082(11) 0.0033(10) C34 0.0526(15) 0.0398(13) 0.067(2) 0.0285(13) 0.0126(14) 0.0044(12) C35 0.057(2) 0.0516(15) 0.060(2) 0.0372(14) 0.0118(14) 0.0071(12) C36 0.0399(12) 0.0385(12) 0.0355(12) 0.0193(10) 0.0065(10) 0.0053(10) C37 0.0330(11) 0.0363(11) 0.0258(10) 0.0153(9) 0.0126(9) 0.0136(9) C38 0.0389(12) 0.0416(12) 0.0369(12) 0.0224(10) 0.0168(10) 0.0143(10) C39 0.062(2) 0.0502(15) 0.055(2) 0.0357(13) 0.0213(13) 0.0176(13) C40 0.066(2) 0.056(2) 0.068(2) 0.0369(15) 0.0266(15) 0.0345(14) C41 0.0477(14) 0.061(2) 0.065(2) 0.0362(14) 0.0259(13) 0.0295(13) C42 0.0395(12) 0.0466(13) 0.0455(14) 0.0233(11) 0.0216(11) 0.0187(10) C43 0.0515(13) 0.0251(10) 0.0258(10) 0.0131(9) 0.0126(9) 0.0063(9) C44 0.0542(14) 0.0416(13) 0.0369(12) 0.0231(11) 0.0187(11) 0.0070(11) C45 0.083(2) 0.051(2) 0.047(2) 0.0293(13) 0.0261(14) -0.0005(14) C46 0.103(2) 0.051(2) 0.050(2) 0.0365(14) 0.016(2) 0.003(2) C47 0.080(2) 0.061(2) 0.056(2) 0.042(2) 0.0084(15) 0.011(2) C48 0.0537(15) 0.0452(14) 0.0492(15) 0.0315(12) 0.0086(12) 0.0116(12) C49 0.0305(10) 0.0271(10) 0.0365(11) 0.0161(9) 0.0134(9) 0.0099(8) C50 0.0382(11) 0.0294(10) 0.0325(11) 0.0139(9) 0.0174(9) 0.0091(9) C51 0.0447(13) 0.0456(13) 0.0500(14) 0.0273(11) 0.0283(11) 0.0181(11) C52 0.0351(12) 0.0405(12) 0.0540(14) 0.0282(11) 0.0180(11) 0.0082(10) C53 0.0365(12) 0.0399(13) 0.0491(14) 0.0247(11) 0.0068(11) 0.0008(10) C54 0.0396(12) 0.0319(11) 0.0310(11) 0.0140(9) 0.0073(9) 0.0038(9) C55 0.0529(13) 0.0285(11) 0.0432(12) 0.0211(10) 0.0293(11) 0.0181(10) C56 0.0514(14) 0.0451(13) 0.0463(13) 0.0271(11) 0.0274(11) 0.0211(11) C57 0.068(2) 0.073(2) 0.056(2) 0.0419(15) 0.0288(14) 0.0285(15) C58 0.086(2) 0.081(2) 0.046(2) 0.038(2) 0.034(2) 0.029(2) C59 0.084(2) 0.059(2) 0.053(2) 0.0324(13) 0.046(2) 0.0257(15) C60 0.0583(15) 0.0416(13) 0.0455(13) 0.0240(11) 0.0339(12) 0.0190(11) C61 0.0376(11) 0.0263(10) 0.0454(12) 0.0156(9) 0.0251(10) 0.0110(9) C62 0.0454(13) 0.0301(11) 0.074(2) 0.0233(12) 0.0345(13) 0.0106(10) C63 0.0407(14) 0.0365(13) 0.093(2) 0.0272(14) 0.0333(14) 0.0038(11) C64 0.0389(14) 0.053(2) 0.062(2) 0.0071(14) 0.0206(13) -0.0072(12) C65 0.0428(13) 0.0559(15) 0.0459(14) 0.0200(12) 0.0187(11) 0.0031(11) C66 0.0391(12) 0.0318(11) 0.0397(12) 0.0121(10) 0.0194(10) 0.0031(9) C79 0.0402(11) 0.0263(10) 0.0240(10) 0.0134(8) 0.0144(9) 0.0106(8) C80 0.0405(12) 0.0324(11) 0.0294(11) 0.0156(9) 0.0129(9) 0.0084(9) C81 0.0478(14) 0.0369(12) 0.0429(13) 0.0199(11) 0.0139(11) 0.0045(10) C82 0.063(2) 0.0283(11) 0.0464(14) 0.0154(10) 0.0186(12) 0.0057(11) C83 0.065(2) 0.0275(11) 0.0445(14) 0.0176(10) 0.0229(12) 0.0181(11) C84 0.0433(12) 0.0308(11) 0.0321(11) 0.0150(9) 0.0155(10) 0.0133(9) C85 0.0305(10) 0.0278(10) 0.0253(10) 0.0124(8) 0.0117(8) 0.0102(8) C86 0.0366(11) 0.0349(11) 0.0315(11) 0.0189(9) 0.0156(9) 0.0088(9) C87 0.0384(12) 0.0417(12) 0.0420(13) 0.0219(10) 0.0181(10) 0.0064(10) C88 0.0312(11) 0.0389(12) 0.0336(11) 0.0145(10) 0.0072(9) 0.0054(9) C89 0.0396(12) 0.0436(12) 0.0319(12) 0.0191(10) 0.0062(10) 0.0113(10) C90 0.0412(12) 0.0297(10) 0.0264(10) 0.0158(9) 0.0085(9) 0.0084(9) _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 O1 C7 1.265(2) . ? O2 C7 1.251(2) . ? O3 C9 1.259(2) . ? O4 C9 1.263(2) . ? O5 C8 1.263(2) . ? O6 C8 1.258(2) . ? O7 C16 1.255(2) . ? O8 C16 1.263(2) . ? O9 C17 1.273(3) . ? O10 C17 1.255(3) . ? O11 C18 1.255(2) . ? O12 C18 1.258(2) . ? N1 C19 1.500(3) . ? N1 C25 1.504(3) . ? N2 C37 1.506(2) . ? N2 C31 1.511(3) . ? N3 C43 1.504(2) . ? N3 C49 1.507(2) . ? N4 C55 1.499(3) . ? N4 C61 1.503(3) . ? N5 C73 1.506(3) . ? N5 C67 1.506(3) . ? N6 C79 1.499(2) . ? N6 C85 1.504(2) . ? C1 C2 1.392(3) . ? C1 C6 1.393(3) . ? C1 C7 1.514(3) . ? C2 C3 1.397(3) . ? C3 C4 1.388(3) . ? C3 C8 1.516(3) . ? C4 C5 1.396(3) . ? C5 C6 1.390(3) . ? C5 C9 1.518(3) . ? C10 C15 1.392(3) . ? C10 C11 1.393(3) . ? C10 C16 1.519(2) . ? C11 C12 1.392(3) . ? C12 C13 1.396(3) . ? C12 C17 1.513(3) . ? C13 C14 1.392(3) . ? C14 C15 1.396(2) . ? C14 C18 1.513(3) . ? C19 C24 1.524(3) . ? C19 C20 1.526(3) . ? C20 C21 1.531(3) . ? C21 C22 1.512(4) . ? C22 C23 1.526(4) . ? C23 C24 1.520(3) . ? C25 C30 1.522(3) . ? C25 C26 1.527(3) . ? C26 C27 1.540(4) . ? C27 C28 1.512(5) . ? C28 C29 1.520(4) . ? C29 C30 1.534(4) . ? C31 C36 1.523(3) . ? C31 C32 1.528(3) . ? C32 C33 1.536(3) . ? C33 C34 1.522(3) . ? C34 C35 1.527(4) . ? C35 C36 1.527(3) . ? C37 C42 1.522(3) . ? C37 C38 1.528(3) . ? C38 C39 1.537(3) . ? C39 C40 1.520(4) . ? C40 C41 1.522(4) . ? C41 C42 1.526(3) . ? C43 C48 1.523(3) . ? C43 C44 1.527(3) . ? C44 C45 1.535(3) . ? C45 C46 1.518(4) . ? C46 C47 1.516(4) . ? C47 C48 1.538(4) . ? C49 C50 1.520(3) . ? C49 C54 1.532(3) . ? C50 C51 1.537(3) . ? C51 C52 1.529(3) . ? C52 C53 1.526(3) . ? C53 C54 1.521(3) . ? C55 C56 1.524(3) . ? C55 C60 1.525(3) . ? C56 C57 1.531(3) . ? C57 C58 1.521(4) . ? C58 C59 1.519(4) . ? C59 C60 1.529(3) . ? C61 C66 1.515(3) . ? C61 C62 1.533(3) . ? C62 C63 1.529(3) . ? C63 C64 1.521(4) . ? C64 C65 1.522(4) . ? C65 C66 1.532(3) . ? C67 C72 1.525(3) . ? C67 C68 1.528(3) . ? C68 C69 1.525(3) . ? C69 C70 1.525(4) . ? C70 C71 1.526(4) . ? C71 C72 1.524(3) . ? C73 C74 1.521(3) . ? C73 C78 1.525(3) . ? C74 C75 1.536(4) . ? C75 C76 1.514(4) . ? C76 C77 1.506(4) . ? C77 C78 1.538(4) . ? C79 C84 1.522(3) . ? C79 C80 1.525(3) . ? C80 C81 1.535(3) . ? C81 C82 1.513(3) . ? C82 C83 1.527(3) . ? C83 C84 1.535(3) . ? C85 C90 1.528(3) . ? C85 C86 1.530(3) . ? C86 C87 1.531(3) . ? C87 C88 1.520(3) . ? C88 C89 1.531(3) . ? C89 C90 1.538(3) . ? 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 C19 N1 C25 118.2(2) . . ? C37 N2 C31 117.89(15) . . ? C43 N3 C49 118.2(2) . . ? C55 N4 C61 118.4(2) . . ? C73 N5 C67 117.1(2) . . ? C79 N6 C85 118.51(14) . . ? C2 C1 C6 119.4(2) . . ? C2 C1 C7 120.7(2) . . ? C6 C1 C7 119.9(2) . . ? C1 C2 C3 120.4(2) . . ? C4 C3 C2 119.3(2) . . ? C4 C3 C8 120.8(2) . . ? C2 C3 C8 119.8(2) . . ? C3 C4 C5 120.8(2) . . ? C6 C5 C4 119.0(2) . . ? C6 C5 C9 119.9(2) . . ? C4 C5 C9 121.1(2) . . ? C5 C6 C1 120.8(2) . . ? O2 C7 O1 124.9(2) . . ? O2 C7 C1 116.6(2) . . ? O1 C7 C1 118.5(2) . . ? O6 C8 O5 125.3(2) . . ? O6 C8 C3 117.1(2) . . ? O5 C8 C3 117.6(2) . . ? O3 C9 O4 125.4(2) . . ? O3 C9 C5 116.6(2) . . ? O4 C9 C5 118.0(2) . . ? C15 C10 C11 119.1(2) . . ? C15 C10 C16 120.4(2) . . ? C11 C10 C16 120.5(2) . . ? C12 C11 C10 121.0(2) . . ? C11 C12 C13 119.1(2) . . ? C11 C12 C17 120.3(2) . . ? C13 C12 C17 120.6(2) . . ? C14 C13 C12 120.7(2) . . ? C13 C14 C15 119.3(2) . . ? C13 C14 C18 120.8(2) . . ? C15 C14 C18 119.8(2) . . ? C10 C15 C14 120.8(2) . . ? O7 C16 O8 125.2(2) . . ? O7 C16 C10 117.6(2) . . ? O8 C16 C10 117.2(2) . . ? O10 C17 O9 124.9(2) . . ? O10 C17 C12 117.7(2) . . ? O9 C17 C12 117.4(2) . . ? O11 C18 O12 125.3(2) . . ? O11 C18 C14 117.8(2) . . ? O12 C18 C14 116.9(2) . . ? N1 C19 C24 108.2(2) . . ? N1 C19 C20 111.7(2) . . ? C24 C19 C20 111.9(2) . . ? C19 C20 C21 110.4(2) . . ? C22 C21 C20 111.8(2) . . ? C21 C22 C23 110.8(2) . . ? C24 C23 C22 110.8(2) . . ? C23 C24 C19 111.4(2) . . ? N1 C25 C30 111.8(2) . . ? N1 C25 C26 108.4(2) . . ? C30 C25 C26 111.1(2) . . ? C25 C26 C27 110.0(2) . . ? C28 C27 C26 111.7(3) . . ? C27 C28 C29 111.0(2) . . ? C28 C29 C30 111.8(2) . . ? C25 C30 C29 110.6(2) . . ? N2 C31 C36 107.7(2) . . ? N2 C31 C32 111.9(2) . . ? C36 C31 C32 110.9(2) . . ? C31 C32 C33 109.7(2) . . ? C34 C33 C32 112.1(2) . . ? C33 C34 C35 110.5(2) . . ? C36 C35 C34 110.9(2) . . ? C31 C36 C35 111.3(2) . . ? N2 C37 C42 112.6(2) . . ? N2 C37 C38 107.7(2) . . ? C42 C37 C38 111.7(2) . . ? C37 C38 C39 111.5(2) . . ? C40 C39 C38 111.4(2) . . ? C39 C40 C41 111.2(2) . . ? C40 C41 C42 110.9(2) . . ? C37 C42 C41 109.8(2) . . ? N3 C43 C48 111.6(2) . . ? N3 C43 C44 107.7(2) . . ? C48 C43 C44 111.7(2) . . ? C43 C44 C45 110.7(2) . . ? C46 C45 C44 111.2(2) . . ? C47 C46 C45 111.6(2) . . ? C46 C47 C48 111.3(2) . . ? C43 C48 C47 110.0(2) . . ? N3 C49 C50 107.4(2) . . ? N3 C49 C54 111.4(2) . . ? C50 C49 C54 112.4(2) . . ? C49 C50 C51 111.4(2) . . ? C52 C51 C50 110.3(2) . . ? C53 C52 C51 110.3(2) . . ? C54 C53 C52 111.2(2) . . ? C53 C54 C49 111.1(2) . . ? N4 C55 C56 108.2(2) . . ? N4 C55 C60 112.4(2) . . ? C56 C55 C60 111.2(2) . . ? C55 C56 C57 111.0(2) . . ? C58 C57 C56 110.8(2) . . ? C59 C58 C57 111.1(2) . . ? C58 C59 C60 111.3(2) . . ? C55 C60 C59 109.8(2) . . ? N4 C61 C66 108.0(2) . . ? N4 C61 C62 111.9(2) . . ? C66 C61 C62 112.0(2) . . ? C63 C62 C61 109.2(2) . . ? C64 C63 C62 111.7(2) . . ? C63 C64 C65 110.2(2) . . ? C64 C65 C66 110.6(2) . . ? C61 C66 C65 112.0(2) . . ? N5 C67 C72 111.6(2) . . ? N5 C67 C68 108.1(2) . . ? C72 C67 C68 111.4(2) . . ? C69 C68 C67 110.5(2) . . ? C70 C69 C68 110.7(2) . . ? C69 C70 C71 110.4(2) . . ? C72 C71 C70 112.3(2) . . ? C71 C72 C67 111.3(2) . . ? N5 C73 C74 111.4(2) . . ? N5 C73 C78 108.7(2) . . ? C74 C73 C78 111.0(2) . . ? C73 C74 C75 109.7(2) . . ? C76 C75 C74 112.3(3) . . ? C77 C76 C75 110.7(3) . . ? C76 C77 C78 110.9(2) . . ? C73 C78 C77 109.7(2) . . ? N6 C79 C84 112.5(2) . . ? N6 C79 C80 108.48(15) . . ? C84 C79 C80 111.1(2) . . ? C79 C80 C81 110.8(2) . . ? C82 C81 C80 111.1(2) . . ? C81 C82 C83 111.2(2) . . ? C82 C83 C84 111.5(2) . . ? C79 C84 C83 109.5(2) . . ? N6 C85 C90 112.1(2) . . ? N6 C85 C86 107.09(15) . . ? C90 C85 C86 112.1(2) . . ? C85 C86 C87 111.9(2) . . ? C88 C87 C86 110.9(2) . . ? C87 C88 C89 110.1(2) . . ? C88 C89 C90 110.6(2) . . ? C85 C90 C89 110.0(2) . . ? 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 C6 C1 C2 C3 -3.6(3) . . . . ? C7 C1 C2 C3 176.0(2) . . . . ? C1 C2 C3 C4 0.2(3) . . . . ? C1 C2 C3 C8 176.7(2) . . . . ? C2 C3 C4 C5 4.1(3) . . . . ? C8 C3 C4 C5 -172.4(2) . . . . ? C3 C4 C5 C6 -4.8(3) . . . . ? C3 C4 C5 C9 173.7(2) . . . . ? C4 C5 C6 C1 1.3(3) . . . . ? C9 C5 C6 C1 -177.2(2) . . . . ? C2 C1 C6 C5 2.8(3) . . . . ? C7 C1 C6 C5 -176.7(2) . . . . ? C2 C1 C7 O2 -161.1(2) . . . . ? C6 C1 C7 O2 18.4(3) . . . . ? C2 C1 C7 O1 18.2(3) . . . . ? C6 C1 C7 O1 -162.2(2) . . . . ? C4 C3 C8 O6 172.2(2) . . . . ? C2 C3 C8 O6 -4.2(3) . . . . ? C4 C3 C8 O5 -7.1(3) . . . . ? C2 C3 C8 O5 176.4(2) . . . . ? C6 C5 C9 O3 28.4(3) . . . . ? C4 C5 C9 O3 -150.1(2) . . . . ? C6 C5 C9 O4 -151.9(2) . . . . ? C4 C5 C9 O4 29.6(3) . . . . ? C15 C10 C11 C12 0.8(3) . . . . ? C16 C10 C11 C12 -177.8(2) . . . . ? C10 C11 C12 C13 -1.6(3) . . . . ? C10 C11 C12 C17 178.1(2) . . . . ? C11 C12 C13 C14 1.1(3) . . . . ? C17 C12 C13 C14 -178.6(2) . . . . ? C12 C13 C14 C15 0.3(3) . . . . ? C12 C13 C14 C18 178.9(2) . . . . ? C11 C10 C15 C14 0.7(3) . . . . ? C16 C10 C15 C14 179.3(2) . . . . ? C13 C14 C15 C10 -1.3(3) . . . . ? C18 C14 C15 C10 -179.8(2) . . . . ? C15 C10 C16 O7 -0.9(3) . . . . ? C11 C10 C16 O7 177.6(2) . . . . ? C15 C10 C16 O8 179.6(2) . . . . ? C11 C10 C16 O8 -1.9(3) . . . . ? C11 C12 C17 O10 173.4(2) . . . . ? C13 C12 C17 O10 -6.9(3) . . . . ? C11 C12 C17 O9 -6.2(3) . . . . ? C13 C12 C17 O9 173.5(2) . . . . ? C13 C14 C18 O11 4.6(3) . . . . ? C15 C14 C18 O11 -176.8(2) . . . . ? C13 C14 C18 O12 -175.1(2) . . . . ? C15 C14 C18 O12 3.4(3) . . . . ? C25 N1 C19 C24 -178.0(2) . . . . ? C25 N1 C19 C20 58.4(2) . . . . ? N1 C19 C20 C21 175.6(2) . . . . ? C24 C19 C20 C21 54.1(3) . . . . ? C19 C20 C21 C22 -55.2(3) . . . . ? C20 C21 C22 C23 56.6(3) . . . . ? C21 C22 C23 C24 -56.5(3) . . . . ? C22 C23 C24 C19 55.7(3) . . . . ? N1 C19 C24 C23 -178.5(2) . . . . ? C20 C19 C24 C23 -55.0(3) . . . . ? C19 N1 C25 C30 58.2(2) . . . . ? C19 N1 C25 C26 -178.9(2) . . . . ? N1 C25 C26 C27 179.9(2) . . . . ? C30 C25 C26 C27 -56.8(3) . . . . ? C25 C26 C27 C28 56.5(3) . . . . ? C26 C27 C28 C29 -55.5(3) . . . . ? C27 C28 C29 C30 54.9(4) . . . . ? N1 C25 C30 C29 177.9(2) . . . . ? C26 C25 C30 C29 56.6(3) . . . . ? C28 C29 C30 C25 -55.5(3) . . . . ? C37 N2 C31 C36 -177.7(2) . . . . ? C37 N2 C31 C32 -55.6(2) . . . . ? N2 C31 C32 C33 -176.6(2) . . . . ? C36 C31 C32 C33 -56.3(2) . . . . ? C31 C32 C33 C34 56.3(3) . . . . ? C32 C33 C34 C35 -56.0(3) . . . . ? C33 C34 C35 C36 55.3(3) . . . . ? N2 C31 C36 C35 180.0(2) . . . . ? C32 C31 C36 C35 57.2(3) . . . . ? C34 C35 C36 C31 -56.4(3) . . . . ? C31 N2 C37 C42 -53.4(2) . . . . ? C31 N2 C37 C38 -177.0(2) . . . . ? N2 C37 C38 C39 178.4(2) . . . . ? C42 C37 C38 C39 54.3(2) . . . . ? C37 C38 C39 C40 -52.8(3) . . . . ? C38 C39 C40 C41 54.6(3) . . . . ? C39 C40 C41 C42 -57.8(3) . . . . ? N2 C37 C42 C41 -178.1(2) . . . . ? C38 C37 C42 C41 -56.8(2) . . . . ? C40 C41 C42 C37 58.4(3) . . . . ? C49 N3 C43 C48 54.4(2) . . . . ? C49 N3 C43 C44 177.4(2) . . . . ? N3 C43 C44 C45 -178.9(2) . . . . ? C48 C43 C44 C45 -56.0(3) . . . . ? C43 C44 C45 C46 54.9(3) . . . . ? C44 C45 C46 C47 -55.4(3) . . . . ? C45 C46 C47 C48 56.2(3) . . . . ? N3 C43 C48 C47 177.0(2) . . . . ? C44 C43 C48 C47 56.3(3) . . . . ? C46 C47 C48 C43 -56.0(3) . . . . ? C43 N3 C49 C50 -177.4(2) . . . . ? C43 N3 C49 C54 59.2(2) . . . . ? N3 C49 C50 C51 -176.2(2) . . . . ? C54 C49 C50 C51 -53.3(2) . . . . ? C49 C50 C51 C52 55.5(2) . . . . ? C50 C51 C52 C53 -57.9(2) . . . . ? C51 C52 C53 C54 58.4(3) . . . . ? C52 C53 C54 C49 -55.5(3) . . . . ? N3 C49 C54 C53 173.7(2) . . . . ? C50 C49 C54 C53 53.1(2) . . . . ? C61 N4 C55 C56 -178.5(2) . . . . ? C61 N4 C55 C60 -55.4(2) . . . . ? N4 C55 C56 C57 -179.6(2) . . . . ? C60 C55 C56 C57 56.6(2) . . . . ? C55 C56 C57 C58 -55.5(3) . . . . ? C56 C57 C58 C59 55.6(3) . . . . ? C57 C58 C59 C60 -56.8(3) . . . . ? N4 C55 C60 C59 -178.3(2) . . . . ? C56 C55 C60 C59 -56.9(2) . . . . ? C58 C59 C60 C55 57.0(3) . . . . ? C55 N4 C61 C66 -179.1(2) . . . . ? C55 N4 C61 C62 -55.4(2) . . . . ? N4 C61 C62 C63 -176.6(2) . . . . ? C66 C61 C62 C63 -55.1(3) . . . . ? C61 C62 C63 C64 57.5(3) . . . . ? C62 C63 C64 C65 -58.8(3) . . . . ? C63 C64 C65 C66 56.1(3) . . . . ? N4 C61 C66 C65 178.4(2) . . . . ? C62 C61 C66 C65 54.7(2) . . . . ? C64 C65 C66 C61 -54.7(3) . . . . ? C73 N5 C67 C72 -62.8(2) . . . . ? C73 N5 C67 C68 174.3(2) . . . . ? N5 C67 C68 C69 179.4(2) . . . . ? C72 C67 C68 C69 56.5(2) . . . . ? C67 C68 C69 C70 -58.3(3) . . . . ? C68 C69 C70 C71 57.3(3) . . . . ? C69 C70 C71 C72 -55.1(3) . . . . ? C70 C71 C72 C67 53.4(3) . . . . ? N5 C67 C72 C71 -174.7(2) . . . . ? C68 C67 C72 C71 -53.8(3) . . . . ? C67 N5 C73 C74 -63.3(2) . . . . ? C67 N5 C73 C78 174.1(2) . . . . ? N5 C73 C74 C75 -178.0(2) . . . . ? C78 C73 C74 C75 -56.7(3) . . . . ? C73 C74 C75 C76 55.4(3) . . . . ? C74 C75 C76 C77 -55.7(3) . . . . ? C75 C76 C77 C78 56.6(3) . . . . ? N5 C73 C78 C77 -178.8(2) . . . . ? C74 C73 C78 C77 58.4(3) . . . . ? C76 C77 C78 C73 -58.0(3) . . . . ? C85 N6 C79 C84 55.2(2) . . . . ? C85 N6 C79 C80 178.5(2) . . . . ? N6 C79 C80 C81 178.4(2) . . . . ? C84 C79 C80 C81 -57.5(2) . . . . ? C79 C80 C81 C82 55.7(2) . . . . ? C80 C81 C82 C83 -54.9(3) . . . . ? C81 C82 C83 C84 56.0(3) . . . . ? N6 C79 C84 C83 179.4(2) . . . . ? C80 C79 C84 C83 57.6(2) . . . . ? C82 C83 C84 C79 -56.8(2) . . . . ? C79 N6 C85 C90 52.0(2) . . . . ? C79 N6 C85 C86 175.3(2) . . . . ? N6 C85 C86 C87 -176.4(2) . . . . ? C90 C85 C86 C87 -53.2(2) . . . . ? C85 C86 C87 C88 54.4(2) . . . . ? C86 C87 C88 C89 -57.5(2) . . . . ? C87 C88 C89 C90 59.7(2) . . . . ? N6 C85 C90 C89 174.8(2) . . . . ? C86 C85 C90 C89 54.4(2) . . . . ? C88 C89 C90 C85 -57.7(2) . . . . ? _refine_diff_density_max 0.459 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.047