Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal of Materials Chemistry' loop_ _publ_author_name 'Feeder, Neil' 'Holmes, A.' 'Kraft, Arno' 'Morrison, John J.' 'Osterod, Frank' 'Peters, Lars' 'Sano, Takeshi' _publ_contact_author_name 'Dr Arno Kraft' _publ_contact_author_address ; Dr Arno Kraft Department of Chemistry Heriot-Watt University Riccarton Edinburgh EH14 4AS UK ; _publ_contact_author_email 'A.Kraft@hw.ac.uk' ############################################## ## CIF for Osterod et al. ## ## Luminescent supramolecular assemblies... ## ## 14b ## ############################################## data_14b _database_code_CSD 153425 _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-4-[2-(3,4,5-trimethoxyphenyl)vinyl]benzoic acid / tris(imidazoline), 3:1 complex / ethanol hydrate ; _chemical_formula_moiety ; C15 H21 N6 3+, (C18 H17 O5 -)3, (C2 H6 O)0.5, (H2 O)4 ; _chemical_formula_sum 'C70 H83 N6 O19.50' _chemical_formula_weight 1320.42 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 14.577(2) _cell_length_b 22.601(4) _cell_length_c 22.184(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.52(3) _cell_angle_gamma 90.00 _cell_volume 7042.1(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12965 _cell_measurement_theta_min 0.93 _cell_measurement_theta_max 22.5 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.245 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2804 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_type 'Sadabs' _exptl_absorpt_correction_T_min 0.9855 _exptl_absorpt_correction_T_max 0.9982 _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.69190 _diffrn_radiation_type 'Synchrotron' _diffrn_radiation_source 'Daresbury SRS Station 9.8' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotaion with narrow frames' _diffrn_reflns_number 27179 _diffrn_reflns_av_R_equivalents 0.1514 _diffrn_reflns_av_sigmaI/netI 0.2245 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 22.49 _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.967 _reflns_number_total 9638 _reflns_number_gt 4163 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 9638 _refine_ls_number_parameters 408 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2761 _refine_ls_R_factor_gt 0.1586 _refine_ls_wR_factor_ref 0.4216 _refine_ls_wR_factor_gt 0.3645 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.140 _refine_ls_shift/su_max 0.026 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.846 _refine_diff_density_min -0.542 _refine_diff_density_rms 0.125 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.0323(6) 0.5475(3) 0.7402(4) 0.046(2) Uiso 1 1 d . . . O2 O 0.0106(6) 0.5813(3) 0.6445(4) 0.043(2) Uiso 1 1 d . . . O3 O -0.8220(5) 0.5501(3) 0.4922(3) 0.0296(18) Uiso 1 1 d . . . O4 O -0.8773(5) 0.4783(3) 0.5718(3) 0.0311(19) Uiso 1 1 d . . . O5 O -0.7551(6) 0.4215(3) 0.6611(4) 0.039(2) Uiso 1 1 d . . . C1 C -0.0195(8) 0.5587(5) 0.6858(6) 0.032(3) Uiso 1 1 d . . . C2 C -0.1220(8) 0.5449(5) 0.6726(5) 0.027(3) Uiso 1 1 d . . . C3 C -0.1872(8) 0.5690(5) 0.6198(5) 0.035(3) Uiso 1 1 d . . . H3 H -0.1662 0.5937 0.5916 0.042 Uiso 1 1 calc R . . C4 C -0.2849(9) 0.5555(5) 0.6098(6) 0.046(3) Uiso 1 1 d . . . H4 H -0.3303 0.5725 0.5752 0.055 Uiso 1 1 calc R . . C5 C -0.3143(9) 0.5191(5) 0.6486(6) 0.040(3) Uiso 1 1 d . . . C6 C -0.2510(9) 0.4955(5) 0.7003(6) 0.045(3) Uiso 1 1 d . . . H6A H -0.2725 0.4703 0.7280 0.054 Uiso 1 1 calc R . . C7 C -0.1571(9) 0.5088(5) 0.7113(6) 0.043(3) Uiso 1 1 d . . . H7A H -0.1137 0.4925 0.7473 0.051 Uiso 1 1 calc R . . C8 C -0.4207(10) 0.5013(6) 0.6411(7) 0.054(4) Uiso 1 1 d . . . H8A H -0.4347 0.4765 0.6720 0.065 Uiso 1 1 calc R . . C9 C -0.4875(10) 0.5180(6) 0.5970(7) 0.052(4) Uiso 1 1 d . . . H9A H -0.4726 0.5420 0.5657 0.062 Uiso 1 1 calc R . . C10 C -0.5892(8) 0.5031(5) 0.5896(5) 0.032(3) Uiso 1 1 d . . . C11 C -0.6556(8) 0.5305(5) 0.5427(5) 0.027(3) Uiso 1 1 d . . . H11A H -0.6356 0.5557 0.5144 0.033 Uiso 1 1 calc R . . C12 C -0.7518(8) 0.5216(4) 0.5362(5) 0.025(3) Uiso 1 1 d . . . C13 C -0.7835(7) 0.4849(4) 0.5752(5) 0.019(2) Uiso 1 1 d . . . C14 C -0.7155(8) 0.4557(4) 0.6241(5) 0.026(3) Uiso 1 1 d . . . C15 C -0.6202(8) 0.4664(5) 0.6319(5) 0.033(3) Uiso 1 1 d . . . H15A H -0.5746 0.4490 0.6660 0.039 Uiso 1 1 calc R . . C16 C -0.7927(9) 0.5830(5) 0.4437(6) 0.045(3) Uiso 1 1 d . . . H16A H -0.8474 0.6047 0.4178 0.067 Uiso 1 1 calc R . . H16B H -0.7688 0.5554 0.4174 0.067 Uiso 1 1 calc R . . H16C H -0.7423 0.6111 0.4634 0.067 Uiso 1 1 calc R . . C17 C -0.9284(8) 0.4424(5) 0.5189(5) 0.035(3) Uiso 1 1 d . . . H17A H -0.9948 0.4380 0.5199 0.053 Uiso 1 1 calc R . . H17B H -0.8986 0.4032 0.5215 0.053 Uiso 1 1 calc R . . H17C H -0.9261 0.4616 0.4798 0.053 Uiso 1 1 calc R . . C18 C -0.6872(9) 0.3890(5) 0.7093(6) 0.047(3) Uiso 1 1 d . . . H18A H -0.7212 0.3663 0.7342 0.070 Uiso 1 1 calc R . . H18B H -0.6434 0.4168 0.7364 0.070 Uiso 1 1 calc R . . H18C H -0.6511 0.3619 0.6898 0.070 Uiso 1 1 calc R . . O6 O 0.5250(6) 0.7242(3) 0.6325(4) 0.043(2) Uiso 1 1 d . . . O7 O 0.4300(7) 0.6797(4) 0.5514(4) 0.054(2) Uiso 1 1 d . . . O8 O 1.1530(6) 0.8238(3) 0.4072(4) 0.043(2) Uiso 1 1 d . . . O9 O 1.1509(6) 0.7386(3) 0.3227(4) 0.036(2) Uiso 1 1 d . . . O10 O 1.0320(5) 0.6479(3) 0.3089(3) 0.035(2) Uiso 1 1 d . . . C19 C 0.5076(9) 0.7041(5) 0.5779(6) 0.040(3) Uiso 1 1 d . . . C20 C 0.5829(8) 0.7072(5) 0.5447(5) 0.032(3) Uiso 1 1 d . . . C21 C 0.6630(9) 0.7384(5) 0.5654(6) 0.040(3) Uiso 1 1 d . . . H21A H 0.6707 0.7606 0.6028 0.048 Uiso 1 1 calc R . . C22 C 0.7346(9) 0.7402(5) 0.5361(6) 0.042(3) Uiso 1 1 d . . . H22A H 0.7899 0.7636 0.5525 0.051 Uiso 1 1 calc R . . C23 C 0.7244(8) 0.7071(4) 0.4817(5) 0.025(3) Uiso 1 1 d . . . C24 C 0.6424(9) 0.6746(6) 0.4584(6) 0.047(3) Uiso 1 1 d . . . H24A H 0.6345 0.6522 0.4211 0.056 Uiso 1 1 calc R . . C25 C 0.5712(9) 0.6747(5) 0.4896(6) 0.042(3) Uiso 1 1 d . . . H25A H 0.5145 0.6526 0.4734 0.051 Uiso 1 1 calc R . . C26 C 0.7999(8) 0.7057(5) 0.4471(5) 0.031(3) Uiso 1 1 d . . . H26A H 0.7895 0.6796 0.4124 0.037 Uiso 1 1 calc R . . C27 C 0.8786(8) 0.7367(4) 0.4600(5) 0.025(3) Uiso 1 1 d . . . H27A H 0.8908 0.7623 0.4952 0.030 Uiso 1 1 calc R . . C28 C 0.9482(8) 0.7345(4) 0.4242(5) 0.025(3) Uiso 1 1 d . . . C29 C 1.0152(8) 0.7806(5) 0.4328(5) 0.027(3) Uiso 1 1 d . . . H29A H 1.0135 0.8116 0.4614 0.033 Uiso 1 1 calc R . . C30 C 1.0830(8) 0.7812(4) 0.4002(5) 0.027(3) Uiso 1 1 d . . . C31 C 1.0850(8) 0.7362(5) 0.3572(5) 0.027(3) Uiso 1 1 d . . . C32 C 1.0203(8) 0.6905(4) 0.3507(5) 0.026(3) Uiso 1 1 d . . . C33 C 0.9523(7) 0.6898(4) 0.3825(5) 0.023(3) Uiso 1 1 d . . . H33A H 0.9074 0.6584 0.3760 0.027 Uiso 1 1 calc R . . C34 C 1.1532(10) 0.8691(6) 0.4526(6) 0.051(4) Uiso 1 1 d . . . H34A H 1.2064 0.8962 0.4547 0.076 Uiso 1 1 calc R . . H34B H 1.1603 0.8509 0.4937 0.076 Uiso 1 1 calc R . . H34C H 1.0931 0.8910 0.4403 0.076 Uiso 1 1 calc R . . C35 C 1.2371(11) 0.7098(6) 0.3494(7) 0.064(4) Uiso 1 1 d . . . H35A H 1.2794 0.7142 0.3220 0.095 Uiso 1 1 calc R . . H35B H 1.2251 0.6677 0.3546 0.095 Uiso 1 1 calc R . . H35C H 1.2672 0.7273 0.3903 0.095 Uiso 1 1 calc R . . C36 C 0.9716(9) 0.5961(5) 0.3024(6) 0.044(3) Uiso 1 1 d . . . H36A H 0.9850 0.5696 0.2709 0.066 Uiso 1 1 calc R . . H36B H 0.9046 0.6083 0.2893 0.066 Uiso 1 1 calc R . . H36C H 0.9842 0.5754 0.3426 0.066 Uiso 1 1 calc R . . O11 O 0.5319(6) 0.4984(3) 0.9071(4) 0.038(2) Uiso 1 1 d . . . O12 O 0.6571(6) 0.4808(4) 0.8711(4) 0.047(2) Uiso 1 1 d . . . O13 O 0.7351(5) 0.1898(3) 1.3475(3) 0.0315(19) Uiso 1 1 d . . . O14 O 0.9204(5) 0.1936(3) 1.3924(3) 0.0297(19) Uiso 1 1 d . . . O15 O 1.0320(5) 0.2572(3) 1.3372(3) 0.0329(19) Uiso 1 1 d . . . C37 C 0.6149(8) 0.4767(5) 0.9113(5) 0.029(3) Uiso 1 1 d . . . C38 C 0.6590(8) 0.4439(4) 0.9710(5) 0.026(3) Uiso 1 1 d . . . C39 C 0.7528(9) 0.4237(5) 0.9821(6) 0.039(3) Uiso 1 1 d . . . H39A H 0.7875 0.4304 0.9521 0.047 Uiso 1 1 calc R . . C40 C 0.7951(9) 0.3935(5) 1.0376(6) 0.042(3) Uiso 1 1 d . . . H40A H 0.8604 0.3827 1.0467 0.050 Uiso 1 1 calc R . . C41 C 0.7431(7) 0.3790(4) 1.0795(5) 0.023(3) Uiso 1 1 d . . . C42 C 0.6512(7) 0.3994(4) 1.0673(5) 0.022(3) Uiso 1 1 d . . . H42A H 0.6147 0.3904 1.0958 0.027 Uiso 1 1 calc R . . C43 C 0.6105(8) 0.4327(4) 1.0149(5) 0.021(2) Uiso 1 1 d . . . H43A H 0.5480 0.4480 1.0091 0.026 Uiso 1 1 calc R . . C44 C 0.7899(8) 0.3475(4) 1.1370(5) 0.030(3) Uiso 1 1 d . . . H44A H 0.8575 0.3458 1.1478 0.036 Uiso 1 1 calc R . . C45 C 0.7484(8) 0.3215(4) 1.1748(5) 0.022(2) Uiso 1 1 d . . . H45A H 0.6809 0.3238 1.1646 0.027 Uiso 1 1 calc R . . C46 C 0.7966(7) 0.2886(4) 1.2327(5) 0.019(2) Uiso 1 1 d . . . C47 C 0.8941(8) 0.2886(4) 1.2551(5) 0.025(3) Uiso 1 1 d . . . H47A H 0.9324 0.3098 1.2339 0.030 Uiso 1 1 calc R . . C48 C 0.9356(8) 0.2574(4) 1.3090(5) 0.025(3) Uiso 1 1 d . . . C49 C 0.8794(8) 0.2246(4) 1.3374(5) 0.026(3) Uiso 1 1 d . . . C50 C 0.7844(8) 0.2239(4) 1.3158(5) 0.025(3) Uiso 1 1 d . . . C51 C 0.7393(7) 0.2569(4) 1.2622(5) 0.020(2) Uiso 1 1 d . . . H51A H 0.6719 0.2574 1.2467 0.024 Uiso 1 1 calc R . . C52 C 0.6352(8) 0.1971(5) 1.3332(5) 0.034(3) Uiso 1 1 d . . . H52A H 0.6101 0.1738 1.3625 0.051 Uiso 1 1 calc R . . H52B H 0.6061 0.1835 1.2903 0.051 Uiso 1 1 calc R . . H52C H 0.6201 0.2390 1.3368 0.051 Uiso 1 1 calc R . . C53 C 0.9829(9) 0.1474(5) 1.3863(6) 0.040(3) Uiso 1 1 d . . . H53A H 0.9808 0.1159 1.4162 0.060 Uiso 1 1 calc R . . H53B H 1.0479 0.1629 1.3947 0.060 Uiso 1 1 calc R . . H53C H 0.9632 0.1315 1.3437 0.060 Uiso 1 1 calc R . . C54 C 1.0911(9) 0.2871(5) 1.3062(6) 0.045(3) Uiso 1 1 d . . . H54A H 1.1578 0.2776 1.3264 0.067 Uiso 1 1 calc R . . H54B H 1.0813 0.3299 1.3083 0.067 Uiso 1 1 calc R . . H54C H 1.0751 0.2746 1.2623 0.067 Uiso 1 1 calc R . . C55 C 0.3025(7) 0.6100(4) 0.6742(4) 0.016(2) Uiso 1 1 d . . . C56 C 0.3984(7) 0.6200(4) 0.6856(5) 0.020(2) Uiso 1 1 d . . . H56A H 0.4222 0.6445 0.6584 0.024 Uiso 1 1 calc R . . C57 C 0.4615(8) 0.5934(4) 0.7384(5) 0.024(3) Uiso 1 1 d . . . C58 C 0.4237(7) 0.5571(4) 0.7776(5) 0.015(2) Uiso 1 1 d . . . H58A H 0.4652 0.5391 0.8133 0.018 Uiso 1 1 calc R . . C59 C 0.3274(7) 0.5476(4) 0.7647(5) 0.019(2) Uiso 1 1 d . . . C60 C 0.2653(8) 0.5740(4) 0.7125(5) 0.021(2) Uiso 1 1 d . . . H60A H 0.1986 0.5675 0.7034 0.025 Uiso 1 1 calc R . . C61 C 0.2362(7) 0.6395(4) 0.6196(4) 0.014(2) Uiso 1 1 d . . . C62 C 0.1009(7) 0.6724(4) 0.5524(5) 0.022(2) Uiso 1 1 d . . . H62A H 0.0538 0.7008 0.5602 0.026 Uiso 1 1 calc R . . H62B H 0.0693 0.6463 0.5170 0.026 Uiso 1 1 calc R . . C63 C 0.1855(7) 0.7043(4) 0.5394(5) 0.022(2) Uiso 1 1 d . . . H63A H 0.1863 0.6999 0.4951 0.026 Uiso 1 1 calc R . . H63B H 0.1854 0.7469 0.5498 0.026 Uiso 1 1 calc R . . C64 C 0.5620(7) 0.6061(4) 0.7520(5) 0.020(2) Uiso 1 1 d . . . C65 C 0.7036(8) 0.6476(5) 0.7480(5) 0.037(3) Uiso 1 1 d . . . H65A H 0.7289 0.6873 0.7624 0.044 Uiso 1 1 calc R . . H65B H 0.7323 0.6340 0.7147 0.044 Uiso 1 1 calc R . . C66 C 0.7222(9) 0.6042(5) 0.8015(6) 0.038(3) Uiso 1 1 d . . . H66A H 0.7702 0.5744 0.7980 0.045 Uiso 1 1 calc R . . H66B H 0.7441 0.6247 0.8423 0.045 Uiso 1 1 calc R . . C67 C 0.2877(7) 0.5122(4) 0.8064(4) 0.016(2) Uiso 1 1 d . . . C68 C 0.2839(8) 0.4524(5) 0.8886(5) 0.031(3) Uiso 1 1 d . . . H68A H 0.2998 0.4670 0.9322 0.037 Uiso 1 1 calc R . . H68B H 0.2925 0.4089 0.8890 0.037 Uiso 1 1 calc R . . C69 C 0.1820(8) 0.4697(5) 0.8529(5) 0.033(3) Uiso 1 1 d . . . H69A H 0.1430 0.4344 0.8365 0.040 Uiso 1 1 calc R . . H69B H 0.1504 0.4927 0.8796 0.040 Uiso 1 1 calc R . . N1 N 0.1443(6) 0.6383(3) 0.6079(4) 0.019(2) Uiso 1 1 d . . . H1A H 0.1126 0.6193 0.6306 0.022 Uiso 1 1 calc R . . N2 N 0.2656(6) 0.6737(3) 0.5812(4) 0.019(2) Uiso 1 1 d . . . H2A H 0.3254 0.6778 0.5807 0.022 Uiso 1 1 calc R . . N3 N 0.6007(6) 0.6481(4) 0.7263(4) 0.025(2) Uiso 1 1 d . . . H3B H 0.5678 0.6737 0.6991 0.031 Uiso 1 1 calc R . . N4 N 0.6299(6) 0.5773(4) 0.7942(4) 0.026(2) Uiso 1 1 d . . . H4B H 0.6197 0.5459 0.8150 0.032 Uiso 1 1 calc R . . N5 N 0.1986(6) 0.5056(3) 0.8028(4) 0.024(2) Uiso 1 1 d . . . H5A H 0.1526 0.5212 0.7730 0.029 Uiso 1 1 calc R . . N6 N 0.3415(6) 0.4809(3) 0.8537(4) 0.023(2) Uiso 1 1 d . . . H6B H 0.4039 0.4780 0.8623 0.028 Uiso 1 1 calc R . . C70 C 0.596(3) 0.3736(15) 0.7513(16) 0.085(11) Uiso 0.50 1 d P . . H70A H 0.6052 0.3452 0.7864 0.102 Uiso 0.50 1 calc PR . . H70B H 0.6603 0.3858 0.7489 0.102 Uiso 0.50 1 calc PR . . C71 C 0.550(2) 0.3411(11) 0.6925(12) 0.051(7) Uiso 0.50 1 d P . . H71A H 0.5893 0.3073 0.6878 0.062 Uiso 0.50 1 calc PR . . H71B H 0.5423 0.3678 0.6567 0.062 Uiso 0.50 1 calc PR . . H71C H 0.4870 0.3270 0.6944 0.062 Uiso 0.50 1 calc PR . . O70 O 0.5549(15) 0.4191(9) 0.7653(10) 0.069(6) Uiso 0.50 1 d P . . H70 H 0.5878 0.4334 0.7991 0.083 Uiso 0.50 1 calc PR . . O100 O 0.6081(7) 0.8300(4) 0.6921(5) 0.069(3) Uiso 1 1 d . . . O101 O -0.0268(9) 0.6026(5) 0.8361(5) 0.088(3) Uiso 1 1 d . . . O102 O 0.8238(13) 0.4439(8) 0.8443(8) 0.056(5) Uiso 0.50 1 d P . . O103 O 0.9087(15) 0.5751(9) 1.0158(10) 0.072(6) Uiso 0.50 1 d P . . O104 O 0.9523(18) 0.5197(10) 0.9187(11) 0.088(7) Uiso 0.50 1 d P A 1 O105 O 0.8571(14) 0.5176(8) 0.8973(9) 0.058(5) Uiso 0.50 1 d P B 2 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.266(13) . ? O2 C1 1.229(12) . ? O3 C12 1.371(12) . ? O3 C16 1.463(13) . ? O4 C13 1.357(12) . ? O4 C17 1.457(13) . ? O5 C14 1.363(12) . ? O5 C18 1.447(14) . ? C1 C2 1.476(15) . ? C2 C7 1.378(15) . ? C2 C3 1.406(15) . ? C3 C4 1.415(16) . ? C3 H3 0.9500 . ? C4 C5 1.342(16) . ? C4 H4 0.9500 . ? C5 C6 1.373(17) . ? C5 C8 1.568(18) . ? C6 C7 1.358(17) . ? C6 H6A 0.9500 . ? C7 H7A 0.9500 . ? C8 C9 1.241(18) . ? C8 H8A 0.9500 . ? C9 C10 1.487(17) . ? C9 H9A 0.9500 . ? C10 C11 1.365(15) . ? C10 C15 1.412(15) . ? C11 C12 1.386(14) . ? C11 H11A 0.9500 . ? C12 C13 1.365(13) . ? C13 C14 1.422(14) . ? C14 C15 1.375(15) . ? C15 H15A 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? O6 C19 1.254(13) . ? O7 C19 1.256(14) . ? O8 C30 1.380(13) . ? O8 C34 1.434(14) . ? O9 C31 1.379(12) . ? O9 C35 1.398(15) . ? O10 C32 1.379(12) . ? O10 C36 1.449(13) . ? C19 C20 1.479(16) . ? C20 C21 1.336(15) . ? C20 C25 1.395(16) . ? C21 C22 1.371(16) . ? C21 H21A 0.9500 . ? C22 C23 1.394(15) . ? C22 H22A 0.9500 . ? C23 C24 1.381(16) . ? C23 C26 1.500(15) . ? C24 C25 1.394(16) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 C27 1.309(14) . ? C26 H26A 0.9500 . ? C27 C28 1.448(14) . ? C27 H27A 0.9500 . ? C28 C33 1.382(14) . ? C28 C29 1.405(14) . ? C29 C30 1.373(14) . ? C29 H29A 0.9500 . ? C30 C31 1.401(14) . ? C31 C32 1.380(14) . ? C32 C33 1.362(14) . ? C33 H33A 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? O11 C37 1.285(12) . ? O12 C37 1.216(12) . ? O13 C50 1.369(12) . ? O13 C52 1.416(13) . ? O14 C49 1.395(12) . ? O14 C53 1.417(13) . ? O15 C48 1.377(12) . ? O15 C54 1.411(13) . ? C37 C38 1.503(15) . ? C38 C43 1.372(14) . ? C38 C39 1.399(15) . ? C39 C40 1.400(16) . ? C39 H39A 0.9500 . ? C40 C41 1.387(15) . ? C40 H40A 0.9500 . ? C41 C42 1.375(14) . ? C41 C44 1.461(15) . ? C42 C43 1.378(14) . ? C42 H42A 0.9500 . ? C43 H43A 0.9500 . ? C44 C45 1.299(14) . ? C44 H44A 0.9500 . ? C45 C46 1.486(14) . ? C45 H45A 0.9500 . ? C46 C47 1.375(14) . ? C46 C51 1.390(13) . ? C47 C48 1.382(14) . ? C47 H47A 0.9500 . ? C48 C49 1.376(14) . ? C49 C50 1.338(15) . ? C50 C51 1.408(14) . ? C51 H51A 0.9500 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.370(13) . ? C55 C60 1.386(13) . ? C55 C61 1.491(13) . ? C56 C57 1.416(14) . ? C56 H56A 0.9500 . ? C57 C58 1.410(13) . ? C57 C64 1.444(14) . ? C58 C59 1.373(13) . ? C58 H58A 0.9500 . ? C59 C60 1.399(14) . ? C59 C67 1.453(13) . ? C60 H60A 0.9500 . ? C61 N1 1.295(12) . ? C61 N2 1.304(11) . ? C62 N1 1.448(12) . ? C62 C63 1.521(13) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 N2 1.456(12) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 N3 1.310(12) . ? C64 N4 1.335(13) . ? C65 N3 1.448(14) . ? C65 C66 1.508(15) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 N4 1.445(14) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 N5 1.289(12) . ? C67 N6 1.333(12) . ? C68 N6 1.438(13) . ? C68 C69 1.535(15) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 N5 1.448(13) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? N1 H1A 0.8800 . ? N2 H2A 0.8800 . ? N3 H3B 0.8800 . ? N4 H4B 0.8800 . ? N5 H5A 0.8800 . ? N6 H6B 0.8800 . ? C70 O70 1.27(3) . ? C70 C71 1.49(4) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? O70 H70 0.8400 . ? 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 C12 O3 C16 117.0(9) . . ? C13 O4 C17 113.3(8) . . ? C14 O5 C18 114.6(9) . . ? O2 C1 O1 123.6(11) . . ? O2 C1 C2 118.9(11) . . ? O1 C1 C2 117.5(10) . . ? C7 C2 C3 117.8(11) . . ? C7 C2 C1 121.7(11) . . ? C3 C2 C1 120.4(10) . . ? C2 C3 C4 118.4(11) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C5 C4 C3 120.8(13) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 121.1(13) . . ? C4 C5 C8 124.4(12) . . ? C6 C5 C8 114.4(11) . . ? C7 C6 C5 118.9(12) . . ? C7 C6 H6A 120.5 . . ? C5 C6 H6A 120.5 . . ? C6 C7 C2 122.9(13) . . ? C6 C7 H7A 118.5 . . ? C2 C7 H7A 118.5 . . ? C9 C8 C5 123.4(13) . . ? C9 C8 H8A 118.3 . . ? C5 C8 H8A 118.3 . . ? C8 C9 C10 124.5(14) . . ? C8 C9 H9A 117.7 . . ? C10 C9 H9A 117.7 . . ? C11 C10 C15 119.0(11) . . ? C11 C10 C9 117.5(11) . . ? C15 C10 C9 123.2(11) . . ? C10 C11 C12 120.3(10) . . ? C10 C11 H11A 119.9 . . ? C12 C11 H11A 119.9 . . ? C13 C12 O3 114.9(9) . . ? C13 C12 C11 121.8(10) . . ? O3 C12 C11 123.3(9) . . ? O4 C13 C12 122.6(9) . . ? O4 C13 C14 118.5(9) . . ? C12 C13 C14 118.7(10) . . ? O5 C14 C15 127.0(10) . . ? O5 C14 C13 113.7(9) . . ? C15 C14 C13 119.2(10) . . ? C14 C15 C10 120.8(11) . . ? C14 C15 H15A 119.6 . . ? C10 C15 H15A 119.6 . . ? O3 C16 H16A 109.5 . . ? O3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O4 C17 H17A 109.5 . . ? O4 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O4 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O5 C18 H18A 109.5 . . ? O5 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O5 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C30 O8 C34 116.0(9) . . ? C31 O9 C35 115.3(9) . . ? C32 O10 C36 116.8(8) . . ? O6 C19 O7 122.4(11) . . ? O6 C19 C20 118.7(11) . . ? O7 C19 C20 118.8(11) . . ? C21 C20 C25 118.1(11) . . ? C21 C20 C19 123.3(11) . . ? C25 C20 C19 118.6(11) . . ? C20 C21 C22 123.9(12) . . ? C20 C21 H21A 118.0 . . ? C22 C21 H21A 118.0 . . ? C21 C22 C23 118.5(12) . . ? C21 C22 H22A 120.8 . . ? C23 C22 H22A 120.8 . . ? C24 C23 C22 119.4(10) . . ? C24 C23 C26 118.5(10) . . ? C22 C23 C26 122.2(10) . . ? C23 C24 C25 119.9(12) . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C24 C25 C20 120.2(12) . . ? C24 C25 H25A 119.9 . . ? C20 C25 H25A 119.9 . . ? C27 C26 C23 126.6(10) . . ? C27 C26 H26A 116.7 . . ? C23 C26 H26A 116.7 . . ? C26 C27 C28 124.4(10) . . ? C26 C27 H27A 117.8 . . ? C28 C27 H27A 117.8 . . ? C33 C28 C29 118.7(9) . . ? C33 C28 C27 123.6(10) . . ? C29 C28 C27 117.6(9) . . ? C30 C29 C28 120.5(10) . . ? C30 C29 H29A 119.7 . . ? C28 C29 H29A 119.7 . . ? C29 C30 O8 124.2(10) . . ? C29 C30 C31 120.1(10) . . ? O8 C30 C31 115.7(9) . . ? O9 C31 C32 122.0(9) . . ? O9 C31 C30 119.6(9) . . ? C32 C31 C30 118.4(10) . . ? C33 C32 O10 125.3(9) . . ? C33 C32 C31 121.8(10) . . ? O10 C32 C31 112.9(9) . . ? C32 C33 C28 120.3(10) . . ? C32 C33 H33A 119.8 . . ? C28 C33 H33A 119.8 . . ? O8 C34 H34A 109.5 . . ? O8 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O8 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O9 C35 H35A 109.5 . . ? O9 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? O9 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O10 C36 H36A 109.5 . . ? O10 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O10 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C50 O13 C52 118.0(8) . . ? C49 O14 C53 114.9(8) . . ? C48 O15 C54 117.3(9) . . ? O12 C37 O11 124.6(11) . . ? O12 C37 C38 120.2(10) . . ? O11 C37 C38 115.2(9) . . ? C43 C38 C39 118.7(10) . . ? C43 C38 C37 122.4(10) . . ? C39 C38 C37 118.9(10) . . ? C38 C39 C40 119.6(11) . . ? C38 C39 H39A 120.2 . . ? C40 C39 H39A 120.2 . . ? C41 C40 C39 120.9(12) . . ? C41 C40 H40A 119.6 . . ? C39 C40 H40A 119.6 . . ? C42 C41 C40 117.9(10) . . ? C42 C41 C44 122.6(9) . . ? C40 C41 C44 119.3(10) . . ? C41 C42 C43 121.8(10) . . ? C41 C42 H42A 119.1 . . ? C43 C42 H42A 119.1 . . ? C38 C43 C42 120.9(10) . . ? C38 C43 H43A 119.6 . . ? C42 C43 H43A 119.6 . . ? C45 C44 C41 126.5(11) . . ? C45 C44 H44A 116.8 . . ? C41 C44 H44A 116.8 . . ? C44 C45 C46 126.1(10) . . ? C44 C45 H45A 117.0 . . ? C46 C45 H45A 117.0 . . ? C47 C46 C51 121.5(9) . . ? C47 C46 C45 121.1(9) . . ? C51 C46 C45 117.4(9) . . ? C46 C47 C48 118.9(10) . . ? C46 C47 H47A 120.5 . . ? C48 C47 H47A 120.5 . . ? C49 C48 O15 116.8(9) . . ? C49 C48 C47 119.7(10) . . ? O15 C48 C47 123.5(9) . . ? C50 C49 C48 121.8(10) . . ? C50 C49 O14 117.9(9) . . ? C48 C49 O14 120.1(10) . . ? C49 C50 O13 117.2(9) . . ? C49 C50 C51 120.1(10) . . ? O13 C50 C51 122.8(10) . . ? C46 C51 C50 117.9(10) . . ? C46 C51 H51A 121.1 . . ? C50 C51 H51A 121.1 . . ? O13 C52 H52A 109.5 . . ? O13 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? O13 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O14 C53 H53A 109.5 . . ? O14 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? O14 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O15 C54 H54A 109.5 . . ? O15 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? O15 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C56 C55 C60 122.0(10) . . ? C56 C55 C61 118.9(8) . . ? C60 C55 C61 119.0(9) . . ? C55 C56 C57 119.2(9) . . ? C55 C56 H56A 120.4 . . ? C57 C56 H56A 120.4 . . ? C58 C57 C56 118.9(10) . . ? C58 C57 C64 122.0(10) . . ? C56 C57 C64 119.1(9) . . ? C59 C58 C57 120.6(10) . . ? C59 C58 H58A 119.7 . . ? C57 C58 H58A 119.7 . . ? C58 C59 C60 120.3(9) . . ? C58 C59 C67 120.8(9) . . ? C60 C59 C67 118.9(9) . . ? C55 C60 C59 119.1(10) . . ? C55 C60 H60A 120.5 . . ? C59 C60 H60A 120.5 . . ? N1 C61 N2 112.7(9) . . ? N1 C61 C55 124.3(8) . . ? N2 C61 C55 122.7(9) . . ? N1 C62 C63 102.8(8) . . ? N1 C62 H62A 111.2 . . ? C63 C62 H62A 111.2 . . ? N1 C62 H62B 111.2 . . ? C63 C62 H62B 111.2 . . ? H62A C62 H62B 109.1 . . ? N2 C63 C62 101.9(8) . . ? N2 C63 H63A 111.4 . . ? C62 C63 H63A 111.4 . . ? N2 C63 H63B 111.4 . . ? C62 C63 H63B 111.4 . . ? H63A C63 H63B 109.2 . . ? N3 C64 N4 109.5(9) . . ? N3 C64 C57 125.8(10) . . ? N4 C64 C57 124.8(9) . . ? N3 C65 C66 102.6(9) . . ? N3 C65 H65A 111.3 . . ? C66 C65 H65A 111.3 . . ? N3 C65 H65B 111.3 . . ? C66 C65 H65B 111.3 . . ? H65A C65 H65B 109.2 . . ? N4 C66 C65 102.7(10) . . ? N4 C66 H66A 111.2 . . ? C65 C66 H66A 111.2 . . ? N4 C66 H66B 111.2 . . ? C65 C66 H66B 111.2 . . ? H66A C66 H66B 109.1 . . ? N5 C67 N6 111.0(9) . . ? N5 C67 C59 126.2(9) . . ? N6 C67 C59 122.8(9) . . ? N6 C68 C69 103.4(9) . . ? N6 C68 H68A 111.1 . . ? C69 C68 H68A 111.1 . . ? N6 C68 H68B 111.1 . . ? C69 C68 H68B 111.1 . . ? H68A C68 H68B 109.0 . . ? N5 C69 C68 101.6(8) . . ? N5 C69 H69A 111.5 . . ? C68 C69 H69A 111.5 . . ? N5 C69 H69B 111.5 . . ? C68 C69 H69B 111.5 . . ? H69A C69 H69B 109.3 . . ? C61 N1 C62 110.5(8) . . ? C61 N1 H1A 124.7 . . ? C62 N1 H1A 124.7 . . ? C61 N2 C63 110.5(8) . . ? C61 N2 H2A 124.8 . . ? C63 N2 H2A 124.8 . . ? C64 N3 C65 112.3(9) . . ? C64 N3 H3B 123.9 . . ? C65 N3 H3B 123.9 . . ? C64 N4 C66 111.6(9) . . ? C64 N4 H4B 124.2 . . ? C66 N4 H4B 124.2 . . ? C67 N5 C69 113.0(9) . . ? C67 N5 H5A 123.5 . . ? C69 N5 H5A 123.5 . . ? C67 N6 C68 110.9(9) . . ? C67 N6 H6B 124.6 . . ? C68 N6 H6B 124.6 . . ? O70 C70 C71 118(3) . . ? O70 C70 H70A 107.7 . . ? C71 C70 H70A 107.7 . . ? O70 C70 H70B 107.7 . . ? C71 C70 H70B 107.7 . . ? H70A C70 H70B 107.1 . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C70 O70 H70 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 O2 C1 C2 C7 166.2(10) . . . . ? O1 C1 C2 C7 -15.3(16) . . . . ? O2 C1 C2 C3 -14.5(16) . . . . ? O1 C1 C2 C3 164.0(10) . . . . ? C7 C2 C3 C4 0.7(16) . . . . ? C1 C2 C3 C4 -178.6(10) . . . . ? C2 C3 C4 C5 -2.1(17) . . . . ? C3 C4 C5 C6 2.4(19) . . . . ? C3 C4 C5 C8 -179.7(11) . . . . ? C4 C5 C6 C7 -1.2(19) . . . . ? C8 C5 C6 C7 -179.3(11) . . . . ? C5 C6 C7 C2 -0.3(18) . . . . ? C3 C2 C7 C6 0.5(17) . . . . ? C1 C2 C7 C6 179.8(11) . . . . ? C4 C5 C8 C9 3(2) . . . . ? C6 C5 C8 C9 -179.4(13) . . . . ? C5 C8 C9 C10 -178.4(11) . . . . ? C8 C9 C10 C11 172.3(13) . . . . ? C8 C9 C10 C15 -2(2) . . . . ? C15 C10 C11 C12 -1.0(16) . . . . ? C9 C10 C11 C12 -175.4(10) . . . . ? C16 O3 C12 C13 -171.3(9) . . . . ? C16 O3 C12 C11 10.8(14) . . . . ? C10 C11 C12 C13 -1.2(16) . . . . ? C10 C11 C12 O3 176.6(9) . . . . ? C17 O4 C13 C12 75.3(12) . . . . ? C17 O4 C13 C14 -109.4(10) . . . . ? O3 C12 C13 O4 -1.8(14) . . . . ? C11 C12 C13 O4 176.1(9) . . . . ? O3 C12 C13 C14 -177.1(8) . . . . ? C11 C12 C13 C14 0.8(15) . . . . ? C18 O5 C14 C15 -6.8(15) . . . . ? C18 O5 C14 C13 177.1(9) . . . . ? O4 C13 C14 O5 2.7(13) . . . . ? C12 C13 C14 O5 178.3(9) . . . . ? O4 C13 C14 C15 -173.7(9) . . . . ? C12 C13 C14 C15 1.8(15) . . . . ? O5 C14 C15 C10 -179.9(10) . . . . ? C13 C14 C15 C10 -3.9(15) . . . . ? C11 C10 C15 C14 3.6(16) . . . . ? C9 C10 C15 C14 177.7(11) . . . . ? O6 C19 C20 C21 -11.0(18) . . . . ? O7 C19 C20 C21 171.5(11) . . . . ? O6 C19 C20 C25 167.4(11) . . . . ? O7 C19 C20 C25 -10.1(17) . . . . ? C25 C20 C21 C22 -0.3(18) . . . . ? C19 C20 C21 C22 178.0(11) . . . . ? C20 C21 C22 C23 -0.8(19) . . . . ? C21 C22 C23 C24 1.3(17) . . . . ? C21 C22 C23 C26 -178.9(11) . . . . ? C22 C23 C24 C25 -0.6(18) . . . . ? C26 C23 C24 C25 179.5(10) . . . . ? C23 C24 C25 C20 -0.5(18) . . . . ? C21 C20 C25 C24 1.0(18) . . . . ? C19 C20 C25 C24 -177.4(11) . . . . ? C24 C23 C26 C27 175.0(11) . . . . ? C22 C23 C26 C27 -4.8(18) . . . . ? C23 C26 C27 C28 -178.5(10) . . . . ? C26 C27 C28 C33 -16.8(17) . . . . ? C26 C27 C28 C29 163.5(11) . . . . ? C33 C28 C29 C30 0.3(16) . . . . ? C27 C28 C29 C30 -180.0(10) . . . . ? C28 C29 C30 O8 -178.0(10) . . . . ? C28 C29 C30 C31 1.0(16) . . . . ? C34 O8 C30 C29 0.9(16) . . . . ? C34 O8 C30 C31 -178.2(10) . . . . ? C35 O9 C31 C32 -88.6(13) . . . . ? C35 O9 C31 C30 91.4(13) . . . . ? C29 C30 C31 O9 177.2(10) . . . . ? O8 C30 C31 O9 -3.7(15) . . . . ? C29 C30 C31 C32 -2.8(16) . . . . ? O8 C30 C31 C32 176.4(9) . . . . ? C36 O10 C32 C33 -5.1(15) . . . . ? C36 O10 C32 C31 175.7(10) . . . . ? O9 C31 C32 C33 -176.6(10) . . . . ? C30 C31 C32 C33 3.3(16) . . . . ? O9 C31 C32 O10 2.6(15) . . . . ? C30 C31 C32 O10 -177.5(9) . . . . ? O10 C32 C33 C28 178.8(10) . . . . ? C31 C32 C33 C28 -2.1(16) . . . . ? C29 C28 C33 C32 0.2(16) . . . . ? C27 C28 C33 C32 -179.5(10) . . . . ? O12 C37 C38 C43 -173.0(10) . . . . ? O11 C37 C38 C43 6.5(15) . . . . ? O12 C37 C38 C39 6.5(16) . . . . ? O11 C37 C38 C39 -174.0(10) . . . . ? C43 C38 C39 C40 -1.0(16) . . . . ? C37 C38 C39 C40 179.6(10) . . . . ? C38 C39 C40 C41 5.3(17) . . . . ? C39 C40 C41 C42 -5.2(16) . . . . ? C39 C40 C41 C44 -179.9(10) . . . . ? C40 C41 C42 C43 0.8(15) . . . . ? C44 C41 C42 C43 175.4(10) . . . . ? C39 C38 C43 C42 -3.4(16) . . . . ? C37 C38 C43 C42 176.1(9) . . . . ? C41 C42 C43 C38 3.5(16) . . . . ? C42 C41 C44 C45 19.1(17) . . . . ? C40 C41 C44 C45 -166.5(11) . . . . ? C41 C44 C45 C46 178.8(9) . . . . ? C44 C45 C46 C47 7.5(16) . . . . ? C44 C45 C46 C51 -171.2(10) . . . . ? C51 C46 C47 C48 -1.4(15) . . . . ? C45 C46 C47 C48 180.0(9) . . . . ? C54 O15 C48 C49 175.5(9) . . . . ? C54 O15 C48 C47 -4.9(14) . . . . ? C46 C47 C48 C49 3.2(15) . . . . ? C46 C47 C48 O15 -176.3(9) . . . . ? O15 C48 C49 C50 176.7(9) . . . . ? C47 C48 C49 C50 -2.9(16) . . . . ? O15 C48 C49 O14 0.6(14) . . . . ? C47 C48 C49 O14 -178.9(9) . . . . ? C53 O14 C49 C50 119.2(11) . . . . ? C53 O14 C49 C48 -64.7(12) . . . . ? C48 C49 C50 O13 -180.0(9) . . . . ? O14 C49 C50 O13 -3.9(14) . . . . ? C48 C49 C50 C51 0.7(16) . . . . ? O14 C49 C50 C51 176.8(9) . . . . ? C52 O13 C50 C49 168.1(9) . . . . ? C52 O13 C50 C51 -12.5(14) . . . . ? C47 C46 C51 C50 -0.7(14) . . . . ? C45 C46 C51 C50 177.9(9) . . . . ? C49 C50 C51 C46 1.1(15) . . . . ? O13 C50 C51 C46 -178.2(9) . . . . ? C60 C55 C56 C57 -0.7(14) . . . . ? C61 C55 C56 C57 178.2(8) . . . . ? C55 C56 C57 C58 0.3(14) . . . . ? C55 C56 C57 C64 -177.3(9) . . . . ? C56 C57 C58 C59 0.2(14) . . . . ? C64 C57 C58 C59 177.7(9) . . . . ? C57 C58 C59 C60 -0.3(14) . . . . ? C57 C58 C59 C67 -177.4(9) . . . . ? C56 C55 C60 C59 0.6(14) . . . . ? C61 C55 C60 C59 -178.3(8) . . . . ? C58 C59 C60 C55 -0.1(14) . . . . ? C67 C59 C60 C55 177.1(9) . . . . ? C56 C55 C61 N1 -172.6(9) . . . . ? C60 C55 C61 N1 6.3(14) . . . . ? C56 C55 C61 N2 1.4(14) . . . . ? C60 C55 C61 N2 -179.6(9) . . . . ? N1 C62 C63 N2 11.8(9) . . . . ? C58 C57 C64 N3 -165.0(9) . . . . ? C56 C57 C64 N3 12.5(15) . . . . ? C58 C57 C64 N4 13.2(15) . . . . ? C56 C57 C64 N4 -169.3(9) . . . . ? N3 C65 C66 N4 11.6(11) . . . . ? C58 C59 C67 N5 172.0(9) . . . . ? C60 C59 C67 N5 -5.2(15) . . . . ? C58 C59 C67 N6 -9.4(14) . . . . ? C60 C59 C67 N6 173.4(9) . . . . ? N6 C68 C69 N5 0.1(10) . . . . ? N2 C61 N1 C62 4.1(11) . . . . ? C55 C61 N1 C62 178.6(8) . . . . ? C63 C62 N1 C61 -10.2(10) . . . . ? N1 C61 N2 C63 4.6(11) . . . . ? C55 C61 N2 C63 -170.1(8) . . . . ? C62 C63 N2 C61 -10.4(10) . . . . ? N4 C64 N3 C65 4.1(12) . . . . ? C57 C64 N3 C65 -177.4(10) . . . . ? C66 C65 N3 C64 -10.2(12) . . . . ? N3 C64 N4 C66 4.4(12) . . . . ? C57 C64 N4 C66 -174.1(9) . . . . ? C65 C66 N4 C64 -10.4(11) . . . . ? N6 C67 N5 C69 3.9(12) . . . . ? C59 C67 N5 C69 -177.4(9) . . . . ? C68 C69 N5 C67 -2.4(11) . . . . ? N5 C67 N6 C68 -3.8(11) . . . . ? C59 C67 N6 C68 177.5(9) . . . . ? C69 C68 N6 C67 2.1(11) . . . . ? ############################################## ## CIF for Osterod et. al. ## ## Luminescent supramolecular assemblies... ## ## 14f ## ############################################## data_14f _database_code_CSD 153426 _audit_creation_method SHELXL-97 _chemical_name_systematic ; dithieno[3,2-b;2',3'-d]thiophene-2-carboxylic acid / tris(imidazoline), 3:1 complex / ethanol/chloroform solvate ; _chemical_formula_moiety ; C15 H21 N6 3+, (C9 H3 O2 S3 -)3, C2 H6 O, C1 H1 Cl3 ; _chemical_formula_sum 'C45 H37 Cl3 N6 O7 S9' _chemical_formula_weight 1168.70 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.8977(7) _cell_length_b 32.031(2) _cell_length_c 16.2090(10) _cell_angle_alpha 90.00 _cell_angle_beta 107.720(10) _cell_angle_gamma 90.00 _cell_volume 4895.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 21953 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 28.73 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.586 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2400 _exptl_absorpt_coefficient_mu 0.630 _exptl_absorpt_correction_type 'Sadabs' _exptl_absorpt_correction_T_min 0.8897 _exptl_absorpt_correction_T_max 0.9752 _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.68830 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_reflns_number 33111 _diffrn_reflns_av_R_equivalents 0.0625 _diffrn_reflns_av_sigmaI/netI 0.0777 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 28.85 _diffrn_measured_fraction_theta_max 0.880 _diffrn_reflns_theta_full 28.85 _diffrn_measured_fraction_theta_full 0.880 _reflns_number_total 12617 _reflns_number_gt 8525 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'TEXSAN 1.7.1 (MSC, 1996)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1158P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12617 _refine_ls_number_parameters 632 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0905 _refine_ls_R_factor_gt 0.0687 _refine_ls_wR_factor_ref 0.1862 _refine_ls_wR_factor_gt 0.1764 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.969 _refine_ls_shift/su_max 0.157 _refine_ls_shift/su_mean 0.009 _refine_diff_density_max 1.042 _refine_diff_density_min -1.066 _refine_diff_density_rms 0.156 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.3490(2) 0.12368(4) 0.19220(9) 0.0797(5) Uani 1 d . . . Cl2 Cl 0.17598(14) 0.19642(5) 0.16563(12) 0.0835(5) Uani 1 d . . . Cl3 Cl 0.46068(12) 0.20245(4) 0.15619(8) 0.0552(3) Uani 1 d . . . S1 S 0.43310(9) -0.17399(3) 0.39241(5) 0.02716(18) Uani 1 d . . . S2 S 0.40464(13) -0.23891(3) 0.59122(6) 0.0457(3) Uani 1 d . . . S3 S 0.79578(11) -0.23634(3) 0.54196(6) 0.0415(2) Uani 1 d . . . S4 S 0.81255(9) 0.19752(2) 0.11768(5) 0.02449(17) Uani 1 d . . . S5 S 0.90306(9) 0.30967(3) 0.05533(5) 0.02914(19) Uani 1 d . . . S6 S 0.92897(11) 0.28718(3) 0.31285(5) 0.0369(2) Uani 1 d . . . S7 S -0.22879(9) -0.02616(2) -0.24541(5) 0.02856(19) Uani 1 d . . . S8 S -0.57693(12) -0.07794(4) -0.39345(8) 0.0515(3) Uani 1 d . . . S9 S -0.53188(9) 0.05123(3) -0.41122(5) 0.0337(2) Uani 1 d . . . O1 O 0.4124(3) -0.12633(7) 0.23811(14) 0.0319(5) Uani 1 d . . . O2 O 0.6432(3) -0.12274(7) 0.25001(15) 0.0313(5) Uani 1 d . . . O3 O 0.8017(3) 0.10808(8) 0.27963(16) 0.0395(6) Uani 1 d . . . O4 O 0.7503(2) 0.11123(7) 0.13624(15) 0.0289(5) Uani 1 d . . . O5 O 0.0210(2) 0.06897(7) -0.15475(14) 0.0284(5) Uani 1 d . . . O6 O 0.0509(3) 0.00048(8) -0.13780(16) 0.0400(6) Uani 1 d . . . O7 O 1.0016(4) 0.10912(15) 0.4407(2) 0.0880(14) Uani 1 d . . . H100 H 0.9476 0.0985 0.3952 0.106 Uiso 1 calc R . . N1 N 0.1173(3) -0.05936(8) -0.01573(16) 0.0227(5) Uani 1 d . . . H1N H 0.0891 -0.0367 -0.0471 0.027 Uiso 1 calc R . . N2 N 0.2509(3) -0.09886(7) 0.08611(15) 0.0211(5) Uani 1 d . . . H2N H 0.3262 -0.1067 0.1282 0.025 Uiso 1 calc R . . N3 N 0.7483(3) -0.04447(8) 0.26827(15) 0.0217(5) Uani 1 d . . . H3N H 0.7088 -0.0686 0.2486 0.026 Uiso 1 calc R . . N4 N 0.7805(3) 0.02339(8) 0.27511(16) 0.0227(5) Uani 1 d . . . H4N H 0.7607 0.0500 0.2640 0.027 Uiso 1 calc R . . N5 N 0.4902(3) 0.11104(8) 0.01962(16) 0.0239(5) Uani 1 d . . . H5N H 0.5731 0.1099 0.0599 0.029 Uiso 1 calc R . . N6 N 0.2763(3) 0.09245(8) -0.05394(16) 0.0218(5) Uani 1 d . . . H6N H 0.2033 0.0758 -0.0753 0.026 Uiso 1 calc R . . C1 C 0.3409(3) -0.02811(9) 0.07407(17) 0.0178(5) Uani 1 d . . . C2 C 0.4656(3) -0.03415(9) 0.14221(17) 0.0179(5) Uani 1 d . . . H2 H 0.4827 -0.0600 0.1724 0.021 Uiso 1 calc R . . C3 C 0.5651(3) -0.00195(9) 0.16566(16) 0.0171(5) Uani 1 d . . . C4 C 0.5414(3) 0.03555(9) 0.12082(18) 0.0181(5) Uani 1 d . . . H4 H 0.6098 0.0573 0.1366 0.022 Uiso 1 calc R . . C5 C 0.4175(3) 0.04137(8) 0.05278(17) 0.0166(5) Uani 1 d . . . C6 C 0.3168(3) 0.00984(8) 0.02940(17) 0.0178(5) Uani 1 d . . . H6 H 0.2318 0.0140 -0.0168 0.021 Uiso 1 calc R . . C7 C 0.2356(3) -0.06224(9) 0.04814(17) 0.0183(5) Uani 1 d . . . C8 C 0.0381(3) -0.09860(9) -0.02826(19) 0.0245(6) Uani 1 d . . . H8A H 0.0345 -0.1118 -0.0841 0.029 Uiso 1 calc R . . H8B H -0.0598 -0.0943 -0.0261 0.029 Uiso 1 calc R . . C9 C 0.1260(3) -0.12495(9) 0.04917(19) 0.0249(6) Uani 1 d . . . H9A H 0.0734 -0.1297 0.0914 0.030 Uiso 1 calc R . . H9B H 0.1524 -0.1522 0.0298 0.030 Uiso 1 calc R . . C10 C 0.6983(3) -0.00767(9) 0.23727(17) 0.0182(6) Uani 1 d . . . C11 C 0.8795(3) -0.03948(10) 0.34025(19) 0.0255(6) Uani 1 d . . . H11A H 0.9575 -0.0563 0.3308 0.031 Uiso 1 calc R . . H11B H 0.8656 -0.0477 0.3960 0.031 Uiso 1 calc R . . C12 C 0.9102(3) 0.00756(10) 0.33854(19) 0.0240(6) Uani 1 d . . . H12A H 0.9249 0.0204 0.3962 0.029 Uiso 1 calc R . . H12B H 0.9947 0.0128 0.3194 0.029 Uiso 1 calc R . . C13 C 0.3942(3) 0.08177(9) 0.00542(17) 0.0184(6) Uani 1 d . . . C14 C 0.4420(3) 0.14609(9) -0.0402(2) 0.0258(7) Uani 1 d . . . H14A H 0.4912 0.1466 -0.0850 0.031 Uiso 1 calc R . . H14B H 0.4568 0.1731 -0.0091 0.031 Uiso 1 calc R . . C15 C 0.2839(3) 0.13635(9) -0.0796(2) 0.0242(6) Uani 1 d . . . H15A H 0.2250 0.1546 -0.0552 0.029 Uiso 1 calc R . . H15B H 0.2534 0.1394 -0.1434 0.029 Uiso 1 calc R . . C16 C 0.5408(3) -0.13499(9) 0.27258(19) 0.0228(6) Uani 1 d . . . C17 C 0.5707(3) -0.16311(9) 0.34981(18) 0.0225(6) Uani 1 d . . . C18 C 0.6949(4) -0.18217(10) 0.3924(2) 0.0272(7) Uani 1 d . . . H18 H 0.7802 -0.1799 0.3773 0.033 Uiso 1 calc R . . C19 C 0.6791(4) -0.20598(10) 0.4628(2) 0.0295(7) Uani 1 d . . . C20 C 0.6617(4) -0.24616(10) 0.5884(2) 0.0364(9) Uani 1 d . . . C21 C 0.6545(6) -0.26959(11) 0.6624(2) 0.0447(11) Uani 1 d . . . H21 H 0.7322 -0.2841 0.7007 0.054 Uiso 1 calc R . . C22 C 0.5241(6) -0.26822(12) 0.6703(2) 0.0520(13) Uani 1 d . . . H22 H 0.4991 -0.2821 0.7153 0.062 Uiso 1 calc R . . C23 C 0.5344(4) -0.22771(10) 0.5443(2) 0.0334(8) Uani 1 d . . . C24 C 0.5457(4) -0.20423(10) 0.47155(19) 0.0278(7) Uani 1 d . . . C25 C 0.7872(3) 0.12715(10) 0.2102(2) 0.0244(6) Uani 1 d . . . C26 C 0.8206(3) 0.17275(10) 0.2146(2) 0.0242(6) Uani 1 d . . . C27 C 0.8558(4) 0.19942(10) 0.2827(2) 0.0297(7) Uani 1 d . . . H27 H 0.8643 0.1914 0.3405 0.036 Uiso 1 calc R . . C28 C 0.8783(4) 0.24012(9) 0.2583(2) 0.0267(7) Uani 1 d . . . C29 C 0.9332(3) 0.31138(9) 0.2179(2) 0.0267(7) Uani 1 d . . . C30 C 0.9682(4) 0.35239(10) 0.1978(2) 0.0321(8) Uani 1 d . . . H30 H 0.9957 0.3746 0.2384 0.039 Uiso 1 calc R . . C31 C 0.9566(4) 0.35543(10) 0.1123(2) 0.0317(7) Uani 1 d . . . H31 H 0.9761 0.3804 0.0863 0.038 Uiso 1 calc R . . C32 C 0.8968(3) 0.28452(9) 0.1479(2) 0.0236(6) Uani 1 d . . . C33 C 0.8620(3) 0.24401(9) 0.17007(19) 0.0231(6) Uani 1 d . . . C34 C -0.0204(3) 0.03211(10) -0.16918(18) 0.0239(6) Uani 1 d . . . C35 C -0.1634(3) 0.02497(9) -0.23122(18) 0.0212(6) Uani 1 d . . . C36 C -0.2552(3) 0.05292(10) -0.28235(18) 0.0215(6) Uani 1 d . . . H36 H -0.2375 0.0820 -0.2835 0.026 Uiso 1 calc R . . C37 C -0.3801(3) 0.03310(10) -0.33350(19) 0.0256(6) Uani 1 d . . . C38 C -0.5967(4) 0.00058(13) -0.4279(2) 0.0372(9) Uani 1 d . . . C39 C -0.7223(4) -0.01823(16) -0.4845(3) 0.0505(11) Uani 1 d . . . H39 H -0.7951 -0.0033 -0.5258 0.061 Uiso 1 calc R . . C40 C -0.7240(5) -0.05939(17) -0.4719(3) 0.0613(14) Uani 1 d . . . H40 H -0.7997 -0.0769 -0.5034 0.074 Uiso 1 calc R . . C41 C -0.5071(4) -0.02870(12) -0.3752(2) 0.0357(8) Uani 1 d . . . C42 C -0.3821(4) -0.00944(10) -0.3209(2) 0.0281(7) Uani 1 d . . . C43 C 0.3473(4) 0.17776(12) 0.2065(3) 0.0402(9) Uani 1 d . . . H43 H 0.3822 0.1839 0.2700 0.048 Uiso 1 calc R . . C44 C 1.1428(8) 0.1046(2) 0.4416(4) 0.095(2) Uani 1 d . . . H44A H 1.1637 0.0743 0.4420 0.114 Uiso 1 calc R . . H44B H 1.2044 0.1163 0.4967 0.114 Uiso 1 calc R . . C45 C 1.1827(6) 0.12320(17) 0.3725(4) 0.0712(15) Uani 1 d . . . H45A H 1.2821 0.1166 0.3791 0.085 Uiso 1 calc R . . H45B H 1.1709 0.1535 0.3740 0.085 Uiso 1 calc R . . H45C H 1.1224 0.1122 0.3171 0.085 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 Cl1 0.1495(15) 0.0458(7) 0.0586(8) -0.0010(6) 0.0536(9) 0.0020(8) Cl2 0.0426(7) 0.1095(12) 0.0948(12) -0.0005(9) 0.0157(7) 0.0098(7) Cl3 0.0566(6) 0.0693(7) 0.0468(6) -0.0104(5) 0.0264(5) -0.0090(5) S1 0.0313(4) 0.0333(4) 0.0149(3) 0.0108(3) 0.0041(3) 0.0031(3) S2 0.0758(7) 0.0432(5) 0.0206(4) 0.0110(4) 0.0185(5) -0.0002(5) S3 0.0516(6) 0.0378(5) 0.0220(4) 0.0079(3) -0.0085(4) 0.0126(4) S4 0.0337(4) 0.0228(4) 0.0164(3) -0.0054(3) 0.0067(3) -0.0039(3) S5 0.0380(5) 0.0266(4) 0.0226(4) -0.0017(3) 0.0088(3) -0.0032(3) S6 0.0647(6) 0.0227(4) 0.0145(4) -0.0040(3) -0.0013(4) 0.0052(4) S7 0.0420(5) 0.0251(4) 0.0210(4) -0.0014(3) 0.0131(3) -0.0052(3) S8 0.0568(6) 0.0578(7) 0.0488(6) -0.0263(5) 0.0295(5) -0.0313(5) S9 0.0267(4) 0.0546(6) 0.0183(4) -0.0057(4) 0.0047(3) 0.0006(4) O1 0.0417(14) 0.0342(13) 0.0178(11) 0.0130(9) 0.0063(10) 0.0104(10) O2 0.0493(14) 0.0234(11) 0.0250(12) 0.0022(9) 0.0167(11) -0.0031(10) O3 0.0626(17) 0.0294(13) 0.0256(13) 0.0010(10) 0.0123(12) -0.0061(11) O4 0.0340(12) 0.0270(11) 0.0244(12) -0.0060(9) 0.0070(10) -0.0073(9) O5 0.0293(12) 0.0306(12) 0.0214(11) -0.0003(9) 0.0021(9) -0.0005(9) O6 0.0529(16) 0.0333(13) 0.0229(12) 0.0085(10) -0.0046(11) 0.0093(11) O7 0.066(2) 0.172(4) 0.0300(17) -0.017(2) 0.0204(17) -0.038(3) N1 0.0273(13) 0.0227(13) 0.0135(11) 0.0022(9) -0.0004(10) -0.0032(10) N2 0.0295(13) 0.0197(12) 0.0124(11) 0.0038(9) 0.0038(10) -0.0026(10) N3 0.0282(13) 0.0211(12) 0.0111(11) 0.0015(9) -0.0013(10) -0.0002(10) N4 0.0261(13) 0.0241(13) 0.0143(12) 0.0017(9) 0.0009(10) -0.0007(10) N5 0.0301(13) 0.0227(13) 0.0155(12) 0.0051(10) 0.0020(10) -0.0027(10) N6 0.0279(13) 0.0193(12) 0.0154(12) 0.0055(9) 0.0024(10) -0.0016(10) C1 0.0263(14) 0.0206(14) 0.0073(11) 0.0014(10) 0.0061(10) -0.0011(11) C2 0.0246(14) 0.0208(14) 0.0084(12) 0.0030(10) 0.0052(11) 0.0011(10) C3 0.0221(14) 0.0245(14) 0.0054(11) 0.0014(10) 0.0050(10) 0.0017(11) C4 0.0253(14) 0.0179(13) 0.0125(12) 0.0002(10) 0.0077(11) -0.0022(10) C5 0.0260(14) 0.0180(13) 0.0076(11) 0.0015(9) 0.0076(10) 0.0019(10) C6 0.0253(14) 0.0201(13) 0.0077(11) 0.0026(10) 0.0046(11) 0.0008(10) C7 0.0260(14) 0.0199(14) 0.0094(12) 0.0001(10) 0.0063(11) 0.0014(11) C8 0.0299(16) 0.0270(16) 0.0146(14) 0.0006(11) 0.0038(12) -0.0060(12) C9 0.0357(17) 0.0211(15) 0.0176(14) -0.0011(11) 0.0077(13) -0.0055(12) C10 0.0244(14) 0.0220(14) 0.0084(12) 0.0019(10) 0.0054(11) 0.0000(10) C11 0.0259(15) 0.0307(16) 0.0151(14) 0.0038(12) -0.0008(12) 0.0027(12) C12 0.0264(15) 0.0304(16) 0.0125(13) 0.0011(11) 0.0017(12) -0.0002(12) C13 0.0288(15) 0.0186(13) 0.0094(12) 0.0011(10) 0.0085(11) 0.0005(11) C14 0.0370(17) 0.0208(14) 0.0172(14) 0.0056(11) 0.0046(13) -0.0019(12) C15 0.0351(17) 0.0185(14) 0.0185(14) 0.0059(11) 0.0072(13) 0.0001(12) C16 0.0367(17) 0.0171(14) 0.0138(13) -0.0009(10) 0.0067(12) 0.0017(12) C17 0.0293(16) 0.0227(14) 0.0131(13) 0.0025(11) 0.0029(12) -0.0029(11) C18 0.0313(17) 0.0278(16) 0.0182(15) 0.0011(12) 0.0010(13) -0.0013(12) C19 0.0398(19) 0.0248(16) 0.0148(14) 0.0051(12) -0.0053(13) 0.0034(13) C20 0.064(2) 0.0229(16) 0.0114(14) 0.0033(12) -0.0039(15) 0.0048(15) C21 0.092(3) 0.0235(17) 0.0113(15) 0.0023(12) 0.0057(18) 0.0085(18) C22 0.112(4) 0.0276(19) 0.0127(16) 0.0068(13) 0.013(2) 0.001(2) C23 0.057(2) 0.0261(16) 0.0134(14) 0.0044(12) 0.0054(14) -0.0023(15) C24 0.0432(19) 0.0244(16) 0.0099(13) 0.0066(11) -0.0006(13) 0.0003(13) C25 0.0273(16) 0.0252(15) 0.0210(15) 0.0013(12) 0.0078(12) 0.0009(12) C26 0.0284(16) 0.0254(15) 0.0178(14) -0.0017(11) 0.0055(12) 0.0010(12) C27 0.0426(19) 0.0263(16) 0.0184(15) -0.0015(12) 0.0066(14) 0.0031(13) C28 0.0388(18) 0.0211(15) 0.0162(14) -0.0025(11) 0.0024(13) 0.0040(12) C29 0.0339(17) 0.0203(14) 0.0191(15) -0.0021(11) -0.0018(13) 0.0034(12) C30 0.0400(19) 0.0197(15) 0.0272(17) -0.0022(12) -0.0037(14) 0.0028(13) C31 0.0350(18) 0.0229(16) 0.0329(18) 0.0005(13) 0.0039(15) -0.0010(13) C32 0.0268(15) 0.0209(14) 0.0192(14) -0.0037(11) 0.0011(12) 0.0022(11) C33 0.0287(15) 0.0215(14) 0.0160(14) -0.0038(11) 0.0023(12) 0.0022(11) C34 0.0321(16) 0.0306(16) 0.0096(13) 0.0009(11) 0.0071(12) 0.0010(12) C35 0.0292(15) 0.0229(14) 0.0130(13) -0.0018(11) 0.0084(11) -0.0018(11) C36 0.0283(15) 0.0255(15) 0.0122(13) -0.0008(11) 0.0085(11) -0.0010(12) C37 0.0251(15) 0.0380(18) 0.0141(14) -0.0046(12) 0.0068(12) -0.0022(12) C38 0.0288(18) 0.063(2) 0.0227(17) -0.0171(16) 0.0121(14) -0.0101(16) C39 0.033(2) 0.087(3) 0.034(2) -0.023(2) 0.0137(17) -0.015(2) C40 0.049(3) 0.089(4) 0.054(3) -0.040(3) 0.026(2) -0.036(2) C41 0.0361(18) 0.051(2) 0.0268(17) -0.0196(16) 0.0205(15) -0.0164(16) C42 0.0343(17) 0.0352(18) 0.0182(15) -0.0084(13) 0.0130(13) -0.0075(13) C43 0.046(2) 0.046(2) 0.0297(19) -0.0065(16) 0.0126(17) 0.0000(17) C44 0.123(6) 0.097(5) 0.046(3) 0.010(3) -0.001(3) -0.047(4) C45 0.077(4) 0.072(4) 0.069(4) -0.024(3) 0.029(3) -0.004(3) _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 Cl1 C43 1.748(4) . ? Cl2 C43 1.728(4) . ? Cl3 C43 1.763(4) . ? S1 C24 1.719(3) . ? S1 C17 1.739(3) . ? S2 C23 1.718(4) . ? S2 C22 1.732(4) . ? S3 C19 1.739(3) . ? S3 C20 1.742(4) . ? S4 C33 1.710(3) . ? S4 C26 1.741(3) . ? S5 C32 1.721(3) . ? S5 C31 1.727(3) . ? S6 C29 1.734(3) . ? S6 C28 1.743(3) . ? S7 C42 1.719(4) . ? S7 C35 1.750(3) . ? S8 C41 1.711(4) . ? S8 C40 1.721(5) . ? S9 C38 1.735(4) . ? S9 C37 1.740(3) . ? O1 C16 1.254(4) . ? O2 C16 1.241(4) . ? O3 C25 1.250(4) . ? O4 C25 1.251(4) . ? O5 C34 1.248(4) . ? O6 C34 1.251(4) . ? O7 C44 1.401(9) . ? O7 H100 0.8400 . ? N1 C7 1.309(4) . ? N1 C8 1.462(4) . ? N1 H1N 0.8800 . ? N2 C7 1.312(4) . ? N2 C9 1.461(4) . ? N2 H2N 0.8800 . ? N3 C10 1.318(4) . ? N3 C11 1.466(4) . ? N3 H3N 0.8800 . ? N4 C10 1.313(4) . ? N4 C12 1.469(4) . ? N4 H4N 0.8800 . ? N5 C13 1.305(4) . ? N5 C14 1.465(4) . ? N5 H5N 0.8800 . ? N6 C13 1.312(4) . ? N6 C15 1.475(4) . ? N6 H6N 0.8800 . ? C1 C2 1.397(4) . ? C1 C6 1.398(4) . ? C1 C7 1.480(4) . ? C2 C3 1.396(4) . ? C2 H2 0.9500 . ? C3 C4 1.387(4) . ? C3 C10 1.479(4) . ? C4 C5 1.390(4) . ? C4 H4 0.9500 . ? C5 C6 1.389(4) . ? C5 C13 1.486(4) . ? C6 H6 0.9500 . ? C8 C9 1.543(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C11 C12 1.539(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C14 C15 1.532(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.497(4) . ? C17 C18 1.358(4) . ? C18 C19 1.420(5) . ? C18 H18 0.9500 . ? C19 C24 1.372(5) . ? C20 C23 1.378(5) . ? C20 C21 1.435(5) . ? C21 C22 1.336(7) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.431(4) . ? C25 C26 1.495(4) . ? C26 C27 1.354(4) . ? C27 C28 1.400(4) . ? C27 H27 0.9500 . ? C28 C33 1.394(4) . ? C29 C32 1.382(4) . ? C29 C30 1.422(4) . ? C30 C31 1.359(5) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.417(4) . ? C34 C35 1.484(4) . ? C35 C36 1.362(4) . ? C36 C37 1.413(4) . ? C36 H36 0.9500 . ? C37 C42 1.379(5) . ? C38 C41 1.391(6) . ? C38 C39 1.434(5) . ? C39 C40 1.335(7) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.422(4) . ? C43 H43 1.0000 . ? C44 C45 1.426(8) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? 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 C24 S1 C17 90.07(16) . . ? C23 S2 C22 90.4(2) . . ? C19 S3 C20 89.86(17) . . ? C33 S4 C26 91.20(15) . . ? C32 S5 C31 91.02(16) . . ? C29 S6 C28 90.97(15) . . ? C42 S7 C35 90.74(15) . . ? C41 S8 C40 90.9(2) . . ? C38 S9 C37 89.85(17) . . ? C44 O7 H100 109.5 . . ? C7 N1 C8 111.2(2) . . ? C7 N1 H1N 124.4 . . ? C8 N1 H1N 124.4 . . ? C7 N2 C9 110.9(2) . . ? C7 N2 H2N 124.5 . . ? C9 N2 H2N 124.5 . . ? C10 N3 C11 110.2(2) . . ? C10 N3 H3N 124.9 . . ? C11 N3 H3N 124.9 . . ? C10 N4 C12 110.5(2) . . ? C10 N4 H4N 124.7 . . ? C12 N4 H4N 124.7 . . ? C13 N5 C14 111.2(2) . . ? C13 N5 H5N 124.4 . . ? C14 N5 H5N 124.4 . . ? C13 N6 C15 110.2(2) . . ? C13 N6 H6N 124.9 . . ? C15 N6 H6N 124.9 . . ? C2 C1 C6 120.0(3) . . ? C2 C1 C7 119.9(2) . . ? C6 C1 C7 120.0(2) . . ? C3 C2 C1 119.5(3) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C4 C3 C2 120.3(2) . . ? C4 C3 C10 119.1(3) . . ? C2 C3 C10 120.6(2) . . ? C3 C4 C5 120.0(3) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 120.4(2) . . ? C6 C5 C13 120.4(2) . . ? C4 C5 C13 119.2(3) . . ? C5 C6 C1 119.7(2) . . ? C5 C6 H6 120.1 . . ? C1 C6 H6 120.1 . . ? N1 C7 N2 112.4(3) . . ? N1 C7 C1 123.8(3) . . ? N2 C7 C1 123.8(2) . . ? N1 C8 C9 102.2(2) . . ? N1 C8 H8A 111.3 . . ? C9 C8 H8A 111.3 . . ? N1 C8 H8B 111.3 . . ? C9 C8 H8B 111.3 . . ? H8A C8 H8B 109.2 . . ? N2 C9 C8 102.6(2) . . ? N2 C9 H9A 111.3 . . ? C8 C9 H9A 111.3 . . ? N2 C9 H9B 111.3 . . ? C8 C9 H9B 111.3 . . ? H9A C9 H9B 109.2 . . ? N4 C10 N3 113.1(2) . . ? N4 C10 C3 123.4(3) . . ? N3 C10 C3 123.5(3) . . ? N3 C11 C12 103.0(2) . . ? N3 C11 H11A 111.2 . . ? C12 C11 H11A 111.2 . . ? N3 C11 H11B 111.2 . . ? C12 C11 H11B 111.2 . . ? H11A C11 H11B 109.1 . . ? N4 C12 C11 102.4(2) . . ? N4 C12 H12A 111.3 . . ? C11 C12 H12A 111.3 . . ? N4 C12 H12B 111.3 . . ? C11 C12 H12B 111.3 . . ? H12A C12 H12B 109.2 . . ? N5 C13 N6 112.3(2) . . ? N5 C13 C5 123.0(3) . . ? N6 C13 C5 124.7(3) . . ? N5 C14 C15 101.9(2) . . ? N5 C14 H14A 111.4 . . ? C15 C14 H14A 111.4 . . ? N5 C14 H14B 111.4 . . ? C15 C14 H14B 111.4 . . ? H14A C14 H14B 109.3 . . ? N6 C15 C14 102.1(2) . . ? N6 C15 H15A 111.4 . . ? C14 C15 H15A 111.3 . . ? N6 C15 H15B 111.3 . . ? C14 C15 H15B 111.3 . . ? H15A C15 H15B 109.2 . . ? O2 C16 O1 127.4(3) . . ? O2 C16 C17 117.7(3) . . ? O1 C16 C17 114.9(3) . . ? C18 C17 C16 127.8(3) . . ? C18 C17 S1 113.9(2) . . ? C16 C17 S1 118.3(2) . . ? C17 C18 C19 110.2(3) . . ? C17 C18 H18 124.9 . . ? C19 C18 H18 124.9 . . ? C24 C19 C18 114.0(3) . . ? C24 C19 S3 113.0(2) . . ? C18 C19 S3 133.0(3) . . ? C23 C20 C21 112.8(4) . . ? C23 C20 S3 113.3(3) . . ? C21 C20 S3 133.9(3) . . ? C22 C21 C20 111.0(4) . . ? C22 C21 H21 124.5 . . ? C20 C21 H21 124.5 . . ? C21 C22 S2 114.1(3) . . ? C21 C22 H22 122.9 . . ? S2 C22 H22 122.9 . . ? C20 C23 C24 111.4(4) . . ? C20 C23 S2 111.7(3) . . ? C24 C23 S2 137.0(3) . . ? C19 C24 C23 112.5(3) . . ? C19 C24 S1 111.8(2) . . ? C23 C24 S1 135.7(3) . . ? O3 C25 O4 125.7(3) . . ? O3 C25 C26 118.1(3) . . ? O4 C25 C26 116.1(3) . . ? C27 C26 C25 130.9(3) . . ? C27 C26 S4 112.2(2) . . ? C25 C26 S4 117.0(2) . . ? C26 C27 C28 112.4(3) . . ? C26 C27 H27 123.8 . . ? C28 C27 H27 123.8 . . ? C33 C28 C27 113.2(3) . . ? C33 C28 S6 111.7(2) . . ? C27 C28 S6 135.1(3) . . ? C32 C29 C30 114.0(3) . . ? C32 C29 S6 112.3(2) . . ? C30 C29 S6 133.6(2) . . ? C31 C30 C29 110.5(3) . . ? C31 C30 H30 124.8 . . ? C29 C30 H30 124.8 . . ? C30 C31 S5 113.7(3) . . ? C30 C31 H31 123.2 . . ? S5 C31 H31 123.2 . . ? C29 C32 C33 112.6(3) . . ? C29 C32 S5 110.8(2) . . ? C33 C32 S5 136.6(2) . . ? C28 C33 C32 112.4(3) . . ? C28 C33 S4 111.0(2) . . ? C32 C33 S4 136.6(2) . . ? O5 C34 O6 125.3(3) . . ? O5 C34 C35 117.6(3) . . ? O6 C34 C35 117.0(3) . . ? C36 C35 C34 129.3(3) . . ? C36 C35 S7 112.6(2) . . ? C34 C35 S7 118.1(2) . . ? C35 C36 C37 111.4(3) . . ? C35 C36 H36 124.3 . . ? C37 C36 H36 124.3 . . ? C42 C37 C36 114.0(3) . . ? C42 C37 S9 112.9(2) . . ? C36 C37 S9 133.1(3) . . ? C41 C38 C39 112.1(4) . . ? C41 C38 S9 113.5(3) . . ? C39 C38 S9 134.4(4) . . ? C40 C39 C38 111.4(4) . . ? C40 C39 H39 124.3 . . ? C38 C39 H39 124.3 . . ? C39 C40 S8 114.0(3) . . ? C39 C40 H40 123.0 . . ? S8 C40 H40 123.0 . . ? C38 C41 C42 111.1(3) . . ? C38 C41 S8 111.5(3) . . ? C42 C41 S8 137.4(3) . . ? C37 C42 C41 112.7(3) . . ? C37 C42 S7 111.3(2) . . ? C41 C42 S7 135.9(3) . . ? Cl2 C43 Cl1 109.9(2) . . ? Cl2 C43 Cl3 110.8(2) . . ? Cl1 C43 Cl3 110.5(2) . . ? Cl2 C43 H43 108.5 . . ? Cl1 C43 H43 108.5 . . ? Cl3 C43 H43 108.5 . . ? O7 C44 C45 117.5(5) . . ? O7 C44 H44A 107.9 . . ? C45 C44 H44A 107.9 . . ? O7 C44 H44B 107.9 . . ? C45 C44 H44B 107.9 . . ? H44A C44 H44B 107.2 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 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 0.5(4) . . . . ? C7 C1 C2 C3 179.3(3) . . . . ? C1 C2 C3 C4 -1.0(4) . . . . ? C1 C2 C3 C10 -179.7(3) . . . . ? C2 C3 C4 C5 0.7(4) . . . . ? C10 C3 C4 C5 179.4(3) . . . . ? C3 C4 C5 C6 0.2(4) . . . . ? C3 C4 C5 C13 -179.9(3) . . . . ? C4 C5 C6 C1 -0.7(4) . . . . ? C13 C5 C6 C1 179.4(3) . . . . ? C2 C1 C6 C5 0.3(4) . . . . ? C7 C1 C6 C5 -178.5(3) . . . . ? C8 N1 C7 N2 -2.0(4) . . . . ? C8 N1 C7 C1 177.5(3) . . . . ? C9 N2 C7 N1 -3.6(4) . . . . ? C9 N2 C7 C1 176.8(3) . . . . ? C2 C1 C7 N1 -178.9(3) . . . . ? C6 C1 C7 N1 -0.1(4) . . . . ? C2 C1 C7 N2 0.5(4) . . . . ? C6 C1 C7 N2 179.4(3) . . . . ? C7 N1 C8 C9 6.2(3) . . . . ? C7 N2 C9 C8 7.2(3) . . . . ? N1 C8 C9 N2 -7.6(3) . . . . ? C12 N4 C10 N3 3.2(4) . . . . ? C12 N4 C10 C3 -175.3(3) . . . . ? C11 N3 C10 N4 3.1(4) . . . . ? C11 N3 C10 C3 -178.4(3) . . . . ? C4 C3 C10 N4 16.9(4) . . . . ? C2 C3 C10 N4 -164.4(3) . . . . ? C4 C3 C10 N3 -161.4(3) . . . . ? C2 C3 C10 N3 17.3(4) . . . . ? C10 N3 C11 C12 -7.6(3) . . . . ? C10 N4 C12 C11 -7.6(3) . . . . ? N3 C11 C12 N4 8.7(3) . . . . ? C14 N5 C13 N6 -4.6(4) . . . . ? C14 N5 C13 C5 176.1(3) . . . . ? C15 N6 C13 N5 -6.1(4) . . . . ? C15 N6 C13 C5 173.2(3) . . . . ? C6 C5 C13 N5 -173.9(3) . . . . ? C4 C5 C13 N5 6.1(4) . . . . ? C6 C5 C13 N6 6.9(4) . . . . ? C4 C5 C13 N6 -173.0(3) . . . . ? C13 N5 C14 C15 12.5(3) . . . . ? C13 N6 C15 C14 13.3(3) . . . . ? N5 C14 C15 N6 -14.5(3) . . . . ? O2 C16 C17 C18 -10.2(5) . . . . ? O1 C16 C17 C18 170.1(3) . . . . ? O2 C16 C17 S1 170.2(2) . . . . ? O1 C16 C17 S1 -9.4(4) . . . . ? C24 S1 C17 C18 1.3(3) . . . . ? C24 S1 C17 C16 -179.1(2) . . . . ? C16 C17 C18 C19 179.6(3) . . . . ? S1 C17 C18 C19 -0.9(3) . . . . ? C17 C18 C19 C24 -0.2(4) . . . . ? C17 C18 C19 S3 -178.7(3) . . . . ? C20 S3 C19 C24 -0.8(3) . . . . ? C20 S3 C19 C18 177.8(3) . . . . ? C19 S3 C20 C23 1.1(3) . . . . ? C19 S3 C20 C21 -179.5(4) . . . . ? C23 C20 C21 C22 0.7(4) . . . . ? S3 C20 C21 C22 -178.8(3) . . . . ? C20 C21 C22 S2 -0.5(4) . . . . ? C23 S2 C22 C21 0.1(3) . . . . ? C21 C20 C23 C24 179.3(3) . . . . ? S3 C20 C23 C24 -1.1(4) . . . . ? C21 C20 C23 S2 -0.6(4) . . . . ? S3 C20 C23 S2 179.00(17) . . . . ? C22 S2 C23 C20 0.3(3) . . . . ? C22 S2 C23 C24 -179.6(4) . . . . ? C18 C19 C24 C23 -178.6(3) . . . . ? S3 C19 C24 C23 0.3(4) . . . . ? C18 C19 C24 S1 1.1(4) . . . . ? S3 C19 C24 S1 179.97(16) . . . . ? C20 C23 C24 C19 0.5(4) . . . . ? S2 C23 C24 C19 -179.6(3) . . . . ? C20 C23 C24 S1 -179.1(3) . . . . ? S2 C23 C24 S1 0.8(6) . . . . ? C17 S1 C24 C19 -1.3(3) . . . . ? C17 S1 C24 C23 178.3(4) . . . . ? O3 C25 C26 C27 -5.7(5) . . . . ? O4 C25 C26 C27 176.2(3) . . . . ? O3 C25 C26 S4 175.2(3) . . . . ? O4 C25 C26 S4 -3.0(4) . . . . ? C33 S4 C26 C27 1.6(3) . . . . ? C33 S4 C26 C25 -179.1(3) . . . . ? C25 C26 C27 C28 -179.8(3) . . . . ? S4 C26 C27 C28 -0.6(4) . . . . ? C26 C27 C28 C33 -1.1(4) . . . . ? C26 C27 C28 S6 -178.0(3) . . . . ? C29 S6 C28 C33 -1.7(3) . . . . ? C29 S6 C28 C27 175.3(4) . . . . ? C28 S6 C29 C32 0.2(3) . . . . ? C28 S6 C29 C30 -178.5(4) . . . . ? C32 C29 C30 C31 0.2(4) . . . . ? S6 C29 C30 C31 179.0(3) . . . . ? C29 C30 C31 S5 0.4(4) . . . . ? C32 S5 C31 C30 -0.7(3) . . . . ? C30 C29 C32 C33 -179.7(3) . . . . ? S6 C29 C32 C33 1.3(4) . . . . ? C30 C29 C32 S5 -0.7(4) . . . . ? S6 C29 C32 S5 -179.74(17) . . . . ? C31 S5 C32 C29 0.8(3) . . . . ? C31 S5 C32 C33 179.4(4) . . . . ? C27 C28 C33 C32 -175.0(3) . . . . ? S6 C28 C33 C32 2.7(4) . . . . ? C27 C28 C33 S4 2.2(4) . . . . ? S6 C28 C33 S4 179.90(17) . . . . ? C29 C32 C33 C28 -2.6(4) . . . . ? S5 C32 C33 C28 178.8(3) . . . . ? C29 C32 C33 S4 -178.8(3) . . . . ? S5 C32 C33 S4 2.6(6) . . . . ? C26 S4 C33 C28 -2.1(3) . . . . ? C26 S4 C33 C32 174.1(4) . . . . ? O5 C34 C35 C36 6.5(5) . . . . ? O6 C34 C35 C36 -171.1(3) . . . . ? O5 C34 C35 S7 -174.8(2) . . . . ? O6 C34 C35 S7 7.5(4) . . . . ? C42 S7 C35 C36 -0.2(2) . . . . ? C42 S7 C35 C34 -179.1(2) . . . . ? C34 C35 C36 C37 178.9(3) . . . . ? S7 C35 C36 C37 0.2(3) . . . . ? C35 C36 C37 C42 -0.1(4) . . . . ? C35 C36 C37 S9 -178.6(3) . . . . ? C38 S9 C37 C42 -1.0(3) . . . . ? C38 S9 C37 C36 177.6(3) . . . . ? C37 S9 C38 C41 1.0(3) . . . . ? C37 S9 C38 C39 -178.5(4) . . . . ? C41 C38 C39 C40 1.1(5) . . . . ? S9 C38 C39 C40 -179.4(3) . . . . ? C38 C39 C40 S8 -0.6(5) . . . . ? C41 S8 C40 C39 0.0(4) . . . . ? C39 C38 C41 C42 178.9(3) . . . . ? S9 C38 C41 C42 -0.8(4) . . . . ? C39 C38 C41 S8 -1.1(4) . . . . ? S9 C38 C41 S8 179.28(18) . . . . ? C40 S8 C41 C38 0.6(3) . . . . ? C40 S8 C41 C42 -179.3(4) . . . . ? C36 C37 C42 C41 -178.1(3) . . . . ? S9 C37 C42 C41 0.7(4) . . . . ? C36 C37 C42 S7 -0.1(4) . . . . ? S9 C37 C42 S7 178.72(17) . . . . ? C38 C41 C42 C37 0.0(4) . . . . ? S8 C41 C42 C37 179.9(3) . . . . ? C38 C41 C42 S7 -177.3(3) . . . . ? S8 C41 C42 S7 2.6(6) . . . . ? C35 S7 C42 C37 0.2(3) . . . . ? C35 S7 C42 C41 177.5(4) . . . . ?