# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Colin Raston' _publ_contact_author_email COLIN.RASTON@UWA.EDU.AU _publ_section_title ; Supramolecular architecture containing end capping bis-imidazolium cations ; loop_ _publ_author_name 'Colin Raston' 'Yatimah Alias' 'Lindsay T Byrne' 'Irene Ling' 'Alexandre N. Sobolev' data_080203a _database_code_depnum_ccdc_archive 'CCDC 752169' _publ_section_title_footnote ; ? #<< paper footnote text ; # 4. TEXT _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Barbour, L. J. (2001). J. Supramol. Chem., 1, 189-191. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; # 5. CHEMICAL DATA _publ_section_figure_captions ; ? #<< figure captions ; #============================================================================== # 6. CRYSTALLOGRAPHY _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C28 H19 O16 S4), 4(C44 H38 P2), C22 H32 N4, 32(H2 O)' _chemical_formula_sum 'C254 H286 N4 O64 P8 S8' _chemical_formula_weight 4923.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_int_tables_number 14 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 14.7948(5) _cell_length_b 43.785(2) _cell_length_c 18.951(1) _cell_angle_alpha 90.0 _cell_angle_beta 100.165(4) _cell_angle_gamma 90.0 _cell_volume 12083.6(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10394 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 67.1 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method ? _exptl_crystal_F_000 5196 _exptl_absorpt_coefficient_mu 1.886 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6519 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Oxford Diffraction Gemini-R Ultra, Ruby CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4738 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 176046 _diffrn_reflns_av_R_equivalents 0.1805 _diffrn_reflns_av_sigmaI/netI 0.1197 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -52 _diffrn_reflns_limit_k_max 52 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 67.83 _reflns_number_total 21506 _reflns_number_gt 10310 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'X-Seed 2.0 (Barbour, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1700P)^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 21506 _refine_ls_number_parameters 1517 _refine_ls_number_restraints 90 _refine_ls_R_factor_all 0.1884 _refine_ls_R_factor_gt 0.1152 _refine_ls_wR_factor_ref 0.3115 _refine_ls_wR_factor_gt 0.2746 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.2969(3) 0.29047(11) 0.6424(3) 0.0504(13) Uani 1 1 d . . . H1 H 0.3075 0.2970 0.6853 0.076 Uiso 1 1 calc R . . C11 C 0.2941(4) 0.31443(15) 0.5965(4) 0.0417(17) Uani 1 1 d . . . C12 C 0.3439(4) 0.31286(16) 0.5421(4) 0.0440(18) Uani 1 1 d . . . C13 C 0.3359(5) 0.33626(16) 0.4921(4) 0.0445(17) Uani 1 1 d . . . H13 H 0.3703 0.3353 0.4543 0.053 Uiso 1 1 calc R . . C14 C 0.2787(4) 0.36097(16) 0.4962(4) 0.0465(18) Uani 1 1 d D A . C15 C 0.2305(5) 0.36289(16) 0.5524(4) 0.0469(19) Uani 1 1 d . . . H15 H 0.1921 0.3800 0.5555 0.056 Uiso 1 1 calc R . . C16 C 0.2372(4) 0.34012(16) 0.6044(4) 0.0427(17) Uani 1 1 d . . . S1 S 0.27326(12) 0.39043(4) 0.43105(11) 0.0514(5) Uani 1 1 d D . . O11 O 0.2123(5) 0.41336(17) 0.4518(4) 0.064(2) Uiso 0.67 1 d PD A 1 O12 O 0.3655(4) 0.40168(15) 0.4338(4) 0.0429(17) Uiso 0.67 1 d PD A 1 O13 O 0.2360(5) 0.37725(17) 0.3627(3) 0.0520(19) Uiso 0.67 1 d PD A 1 O14 O 0.1823(7) 0.4027(4) 0.4224(10) 0.120(9) Uiso 0.33 1 d PD A 2 O15 O 0.3437(10) 0.4114(3) 0.4619(8) 0.085(6) Uiso 0.33 1 d PD A 2 O16 O 0.2925(13) 0.3759(4) 0.3675(6) 0.094(7) Uiso 0.33 1 d PD A 2 C1 C 0.4119(4) 0.28697(16) 0.5396(5) 0.0460(18) Uani 1 1 d . . . H1A H 0.4098 0.2805 0.4893 0.055 Uiso 1 1 calc R . . H1B H 0.3948 0.2693 0.5670 0.055 Uiso 1 1 calc R . . O2 O 0.4956(3) 0.27831(11) 0.6853(3) 0.0541(14) Uani 1 1 d . . . H2 H 0.5065 0.2852 0.7279 0.081 Uiso 0.50 1 calc PR B 1 C21 C 0.5439(5) 0.29422(15) 0.6443(4) 0.0441(18) Uani 1 1 d . . . C22 C 0.6306(5) 0.30753(16) 0.6746(5) 0.050(2) Uani 1 1 d . . . C23 C 0.6801(5) 0.32263(17) 0.6299(5) 0.052(2) Uani 1 1 d . . . H23 H 0.7370 0.3319 0.6498 0.062 Uiso 1 1 calc R . . C24 C 0.6485(5) 0.32463(17) 0.5568(5) 0.052(2) Uani 1 1 d . . . C25 C 0.5614(5) 0.31230(17) 0.5277(5) 0.0509(19) Uani 1 1 d . . . H25 H 0.5383 0.3142 0.4778 0.061 Uiso 1 1 calc R . . C26 C 0.5094(4) 0.29746(15) 0.5717(4) 0.0414(17) Uani 1 1 d . . . S2 S 0.71359(13) 0.34238(5) 0.49876(15) 0.0644(6) Uani 1 1 d . . . O21 O 0.7940(4) 0.35490(16) 0.5451(4) 0.083(2) Uani 1 1 d . . . O22 O 0.7351(4) 0.31887(15) 0.4521(4) 0.0679(17) Uani 1 1 d . . . O23 O 0.6560(4) 0.36666(15) 0.4600(5) 0.084(2) Uani 1 1 d . . . C2 C 0.6662(5) 0.30505(18) 0.7549(5) 0.053(2) Uani 1 1 d . . . H2A H 0.6457 0.2853 0.7723 0.063 Uiso 1 1 calc R . . H2B H 0.7342 0.3049 0.7632 0.063 Uiso 1 1 calc R . . O3 O 0.4948(3) 0.30476(10) 0.8057(3) 0.0466(12) Uani 1 1 d . . . H3 H 0.5029 0.2975 0.7657 0.070 Uiso 0.50 1 calc PR C 2 C31 C 0.5497(5) 0.32910(15) 0.8226(4) 0.0431(17) Uani 1 1 d . . . C32 C 0.5214(4) 0.35302(16) 0.8644(4) 0.0436(17) Uani 1 1 d . . . C33 C 0.5799(4) 0.37790(15) 0.8829(4) 0.0437(17) Uani 1 1 d . . . H33 H 0.5627 0.3938 0.9121 0.052 Uiso 1 1 calc R . . C34 C 0.6645(4) 0.37957(15) 0.8583(4) 0.0416(17) Uani 1 1 d . . . C35 C 0.6906(4) 0.35581(16) 0.8189(4) 0.0439(17) Uani 1 1 d . . . H35 H 0.7492 0.3566 0.8051 0.053 Uiso 1 1 calc R . . C36 C 0.6345(4) 0.33069(15) 0.7984(4) 0.0443(18) Uani 1 1 d . . . S3 S 0.74309(11) 0.40948(4) 0.88749(11) 0.0449(5) Uani 1 1 d . . . O31 O 0.6944(3) 0.43329(11) 0.9185(3) 0.0489(13) Uani 1 1 d . . . O32 O 0.8147(4) 0.39525(12) 0.9385(4) 0.0690(18) Uani 1 1 d . . . O33 O 0.7766(4) 0.41923(12) 0.8240(3) 0.0583(15) Uani 1 1 d . . . C3 C 0.4318(4) 0.35148(17) 0.8900(4) 0.0479(18) Uani 1 1 d . . . H3A H 0.4378 0.3628 0.9358 0.057 Uiso 1 1 calc R . . H3B H 0.4191 0.3299 0.9000 0.057 Uiso 1 1 calc R . . O4 O 0.3301(3) 0.31766(11) 0.7702(3) 0.0502(13) Uani 1 1 d . . . H4 H 0.3877 0.3159 0.7840 0.075 Uiso 1 1 calc R . . C41 C 0.3045(5) 0.34707(16) 0.7798(4) 0.0433(16) Uani 1 1 d . . . C42 C 0.2310(4) 0.35990(16) 0.7307(4) 0.0448(17) Uani 1 1 d . . . C43 C 0.2015(5) 0.38908(17) 0.7432(4) 0.0446(17) Uani 1 1 d . . . H43 H 0.1519 0.3979 0.7110 0.053 Uiso 1 1 calc R . . C44 C 0.2439(5) 0.40547(17) 0.8024(4) 0.0479(18) Uani 1 1 d D D . C45 C 0.3188(4) 0.39348(17) 0.8493(4) 0.0443(17) Uani 1 1 d . . . H45 H 0.3485 0.4054 0.8885 0.053 Uiso 1 1 calc R . . C46 C 0.3504(5) 0.36411(16) 0.8391(4) 0.0452(17) Uani 1 1 d . . . S4 S 0.19677(12) 0.44142(4) 0.81937(11) 0.0545(5) Uani 1 1 d D . . O41 O 0.2538(6) 0.4525(2) 0.8854(4) 0.041(3) Uiso 0.50 1 d PD D 1 O42 O 0.2111(7) 0.4600(2) 0.7581(4) 0.056(3) Uiso 0.50 1 d PD D 1 O43 O 0.1031(4) 0.4373(2) 0.8240(5) 0.047(3) Uiso 0.50 1 d PD D 1 O44 O 0.2624(6) 0.4583(2) 0.8680(5) 0.047(3) Uiso 0.50 1 d PD D 2 O45 O 0.1675(9) 0.4557(3) 0.7506(5) 0.093(5) Uiso 0.50 1 d PD D 2 O46 O 0.1162(6) 0.4327(2) 0.8518(6) 0.055(3) Uiso 0.50 1 d PD D 2 C4 C 0.1836(4) 0.34208(17) 0.6643(4) 0.0473(18) Uani 1 1 d . . . H4A H 0.1709 0.3211 0.6793 0.057 Uiso 1 1 calc R . . H4B H 0.1238 0.3519 0.6459 0.057 Uiso 1 1 calc R . . P11 P 0.03753(11) 0.30693(4) 0.33412(11) 0.0412(4) Uani 1 1 d . . . P12 P -0.00246(11) 0.33008(4) -0.04848(11) 0.0417(4) Uani 1 1 d . . . C101 C 0.0338(5) 0.34717(16) 0.3106(4) 0.0467(18) Uani 1 1 d . . . H10A H -0.0190 0.3568 0.3277 0.056 Uiso 1 1 calc R . . H10B H 0.0904 0.3571 0.3358 0.056 Uiso 1 1 calc R . . C102 C 0.0009(5) 0.36528(15) 0.0031(4) 0.0450(17) Uani 1 1 d . . . H10C H 0.0532 0.3778 -0.0064 0.054 Uiso 1 1 calc R . . H10D H -0.0561 0.3769 -0.0142 0.054 Uiso 1 1 calc R . . C111 C 0.0422(4) 0.30298(16) 0.4285(4) 0.0451(18) Uani 1 1 d . . . C112 C -0.0214(5) 0.31948(18) 0.4623(4) 0.0495(19) Uani 1 1 d . . . H112 H -0.0618 0.3339 0.4358 0.059 Uiso 1 1 calc R . . C113 C -0.0238(5) 0.31437(18) 0.5336(4) 0.0517(19) Uani 1 1 d . . . H113 H -0.0675 0.3247 0.5560 0.062 Uiso 1 1 calc R . . C114 C 0.0380(5) 0.29402(18) 0.5729(5) 0.054(2) Uani 1 1 d . . . H114 H 0.0356 0.2902 0.6219 0.064 Uiso 1 1 calc R . . C115 C 0.1026(5) 0.27950(17) 0.5404(5) 0.0503(19) Uani 1 1 d . . . H115 H 0.1467 0.2666 0.5684 0.060 Uiso 1 1 calc R . . C116 C 0.1050(4) 0.28317(15) 0.4694(5) 0.0445(18) Uani 1 1 d . . . H116 H 0.1489 0.2724 0.4479 0.053 Uiso 1 1 calc R . . C121 C -0.0621(5) 0.28817(15) 0.2856(4) 0.0438(17) Uani 1 1 d . . . C122 C -0.1385(5) 0.28311(16) 0.3194(5) 0.0482(18) Uani 1 1 d . . . H122 H -0.1362 0.2880 0.3685 0.058 Uiso 1 1 calc R . . C123 C -0.2194(6) 0.27040(19) 0.2773(5) 0.062(2) Uani 1 1 d . . . H123 H -0.2724 0.2671 0.2981 0.075 Uiso 1 1 calc R . . C124 C -0.2205(7) 0.2632(2) 0.2089(5) 0.065(2) Uani 1 1 d . . . H124 H -0.2740 0.2539 0.1825 0.078 Uiso 1 1 calc R . . C125 C -0.1481(7) 0.2686(2) 0.1755(5) 0.071(3) Uani 1 1 d . . . H125 H -0.1522 0.2639 0.1261 0.086 Uiso 1 1 calc R . . C126 C -0.0683(6) 0.28086(19) 0.2143(5) 0.056(2) Uani 1 1 d . . . H126 H -0.0171 0.2843 0.1914 0.067 Uiso 1 1 calc R . . C131 C 0.1369(5) 0.28927(17) 0.3107(4) 0.0500(19) Uani 1 1 d . . . C132 C 0.2182(5) 0.3049(2) 0.3178(5) 0.055(2) Uani 1 1 d . . . H132 H 0.2217 0.3256 0.3335 0.066 Uiso 1 1 calc R . . C133 C 0.2963(6) 0.2902(2) 0.3017(5) 0.068(2) Uani 1 1 d . . . H133 H 0.3534 0.3007 0.3075 0.081 Uiso 1 1 calc R . . C134 C 0.2897(6) 0.2599(2) 0.2770(6) 0.072(3) Uani 1 1 d . . . H134 H 0.3414 0.2503 0.2631 0.087 Uiso 1 1 calc R . . C135 C 0.2105(7) 0.2445(2) 0.2729(6) 0.079(3) Uani 1 1 d . . . H135 H 0.2081 0.2237 0.2592 0.095 Uiso 1 1 calc R . . C136 C 0.1322(6) 0.2585(2) 0.2883(5) 0.065(2) Uani 1 1 d . . . H136 H 0.0761 0.2475 0.2839 0.078 Uiso 1 1 calc R . . C141 C -0.0256(4) 0.33814(16) -0.1414(4) 0.0438(17) Uani 1 1 d . . . C142 C -0.0100(5) 0.36742(17) -0.1693(4) 0.0470(18) Uani 1 1 d . . . H142 H 0.0126 0.3836 -0.1377 0.056 Uiso 1 1 calc R . . C143 C -0.0274(5) 0.37230(19) -0.2414(5) 0.054(2) Uani 1 1 d . . . H143 H -0.0156 0.3919 -0.2595 0.065 Uiso 1 1 calc R . . C144 C -0.0622(5) 0.3492(2) -0.2891(5) 0.056(2) Uani 1 1 d . . . H144 H -0.0770 0.3531 -0.3391 0.067 Uiso 1 1 calc R . . C145 C -0.0747(5) 0.32028(19) -0.2620(5) 0.0511(19) Uani 1 1 d . . . H145 H -0.0949 0.3040 -0.2941 0.061 Uiso 1 1 calc R . . C146 C -0.0586(4) 0.31505(18) -0.1901(5) 0.0472(18) Uani 1 1 d . . . H146 H -0.0699 0.2953 -0.1727 0.057 Uiso 1 1 calc R . . C151 C 0.1071(5) 0.31132(16) -0.0295(4) 0.0471(18) Uani 1 1 d . . . C152 C 0.1608(5) 0.30843(17) -0.0813(5) 0.053(2) Uani 1 1 d . . . H152 H 0.1375 0.3150 -0.1287 0.064 Uiso 1 1 calc R . . C153 C 0.2490(5) 0.29596(18) -0.0655(5) 0.058(2) Uani 1 1 d . . . H153 H 0.2852 0.2940 -0.1019 0.069 Uiso 1 1 calc R . . C154 C 0.2823(5) 0.28673(18) 0.0026(6) 0.059(2) Uani 1 1 d . . . H154 H 0.3422 0.2782 0.0130 0.071 Uiso 1 1 calc R . . C155 C 0.2326(6) 0.28928(17) 0.0571(5) 0.059(2) Uani 1 1 d . . . H155 H 0.2582 0.2832 0.1045 0.071 Uiso 1 1 calc R . . C156 C 0.1414(5) 0.30136(16) 0.0409(5) 0.053(2) Uani 1 1 d . . . H156 H 0.1046 0.3027 0.0771 0.064 Uiso 1 1 calc R . . C161 C -0.0935(4) 0.30579(16) -0.0318(4) 0.0416(16) Uani 1 1 d . . . C162 C -0.1816(4) 0.31798(16) -0.0402(4) 0.0472(18) Uani 1 1 d . . . H162 H -0.1912 0.3392 -0.0484 0.057 Uiso 1 1 calc R . . C163 C -0.2562(5) 0.29855(17) -0.0365(4) 0.0483(18) Uani 1 1 d . . . H163 H -0.3163 0.3068 -0.0415 0.058 Uiso 1 1 calc R . . C164 C -0.2430(5) 0.26802(16) -0.0257(4) 0.0466(17) Uani 1 1 d . . . H164 H -0.2942 0.2551 -0.0239 0.056 Uiso 1 1 calc R . . C165 C -0.1561(5) 0.25557(17) -0.0173(4) 0.0469(17) Uani 1 1 d . . . H165 H -0.1478 0.2342 -0.0095 0.056 Uiso 1 1 calc R . . C166 C -0.0801(5) 0.27417(16) -0.0202(5) 0.0484(18) Uani 1 1 d . . . H166 H -0.0202 0.2656 -0.0145 0.058 Uiso 1 1 calc R . . C171 C 0.0253(4) 0.35288(15) 0.2321(4) 0.0421(17) Uani 1 1 d . . . C172 C -0.0611(4) 0.35223(16) 0.1859(4) 0.0429(17) Uani 1 1 d . . . H172 H -0.1153 0.3488 0.2051 0.051 Uiso 1 1 calc R . . C173 C -0.0669(4) 0.35639(15) 0.1145(5) 0.0456(19) Uani 1 1 d . . . H173 H -0.1260 0.3562 0.0851 0.055 Uiso 1 1 calc R . . C174 C 0.0099(4) 0.36103(14) 0.0816(4) 0.0407(16) Uani 1 1 d . . . C175 C 0.0946(4) 0.36260(16) 0.1289(4) 0.0431(17) Uani 1 1 d . . . H175 H 0.1483 0.3666 0.1094 0.052 Uiso 1 1 calc R . . C176 C 0.1038(4) 0.35867(15) 0.2007(4) 0.0411(16) Uani 1 1 d . . . H176 H 0.1628 0.3598 0.2300 0.049 Uiso 1 1 calc R . . P21 P 0.24715(12) 0.45662(4) 0.09085(12) 0.0472(5) Uani 1 1 d . . . P22 P 0.73323(13) 0.44276(4) 0.18171(14) 0.0545(5) Uani 1 1 d . . . C201 C 0.3068(5) 0.48031(18) 0.0352(5) 0.0520(19) Uani 1 1 d . . . H20A H 0.2862 0.4747 -0.0157 0.062 Uiso 1 1 calc R . . H20B H 0.2902 0.5020 0.0410 0.062 Uiso 1 1 calc R . . C202 C 0.7026(6) 0.4675(2) 0.1023(6) 0.066(2) Uani 1 1 d . . . H20C H 0.7300 0.4880 0.1127 0.079 Uiso 1 1 calc R . . H20D H 0.7276 0.4587 0.0616 0.079 Uiso 1 1 calc R . . C211 C 0.1265(5) 0.45625(16) 0.0527(5) 0.0513(19) Uani 1 1 d . . . C212 C 0.0940(6) 0.4670(2) -0.0141(5) 0.068(3) Uani 1 1 d . . . H212 H 0.1360 0.4750 -0.0420 0.081 Uiso 1 1 calc R . . C213 C 0.0007(6) 0.4667(3) -0.0427(6) 0.075(3) Uani 1 1 d . . . H213 H -0.0217 0.4757 -0.0881 0.090 Uiso 1 1 calc R . . C214 C -0.0581(6) 0.4531(2) -0.0040(6) 0.071(3) Uani 1 1 d . . . H214 H -0.1215 0.4518 -0.0243 0.085 Uiso 1 1 calc R . . C215 C -0.0283(6) 0.44127(19) 0.0635(7) 0.069(3) Uani 1 1 d . . . H215 H -0.0702 0.4321 0.0897 0.083 Uiso 1 1 calc R . . C216 C 0.0672(5) 0.44315(19) 0.0929(5) 0.058(2) Uani 1 1 d . . . H216 H 0.0898 0.4355 0.1396 0.070 Uiso 1 1 calc R . . C221 C 0.2908(5) 0.41852(17) 0.0882(5) 0.0497(19) Uani 1 1 d . . . C222 C 0.2568(5) 0.40057(17) 0.0281(5) 0.055(2) Uani 1 1 d . . . H222 H 0.2102 0.4080 -0.0089 0.066 Uiso 1 1 calc R . . C223 C 0.2945(6) 0.37096(17) 0.0244(5) 0.058(2) Uani 1 1 d . . . H223 H 0.2714 0.3582 -0.0152 0.070 Uiso 1 1 calc R . . C224 C 0.3624(6) 0.36051(18) 0.0756(6) 0.066(2) Uani 1 1 d . . . H224 H 0.3874 0.3408 0.0710 0.079 Uiso 1 1 calc R . . C225 C 0.3959(7) 0.3782(2) 0.1348(6) 0.073(3) Uani 1 1 d . . . H225 H 0.4427 0.3702 0.1710 0.087 Uiso 1 1 calc R . . C226 C 0.3620(6) 0.40762(18) 0.1420(5) 0.062(2) Uani 1 1 d . . . H226 H 0.3862 0.4200 0.1821 0.074 Uiso 1 1 calc R . . C231 C 0.2620(5) 0.47073(17) 0.1804(5) 0.0500(19) Uani 1 1 d . . . C232 C 0.2721(5) 0.50254(16) 0.1916(5) 0.0465(18) Uani 1 1 d . . . H232 H 0.2724 0.5160 0.1523 0.056 Uiso 1 1 calc R . . C233 C 0.2812(5) 0.51354(18) 0.2589(5) 0.052(2) Uani 1 1 d . . . H233 H 0.2874 0.5350 0.2661 0.063 Uiso 1 1 calc R . . C234 C 0.2820(5) 0.49501(19) 0.3172(5) 0.059(2) Uani 1 1 d . . . H234 H 0.2892 0.5034 0.3641 0.070 Uiso 1 1 calc R . . C235 C 0.2720(5) 0.4635(2) 0.3068(5) 0.055(2) Uani 1 1 d . . . H235 H 0.2720 0.4503 0.3466 0.066 Uiso 1 1 calc R . . C236 C 0.2624(5) 0.45191(18) 0.2395(5) 0.055(2) Uani 1 1 d . . . H236 H 0.2559 0.4305 0.2326 0.065 Uiso 1 1 calc R . . C241 C 0.8527(5) 0.44724(17) 0.2183(5) 0.057(2) Uani 1 1 d . . . C242 C 0.8983(6) 0.4757(2) 0.2129(6) 0.075(3) Uani 1 1 d . . . H242 H 0.8673 0.4922 0.1863 0.090 Uiso 1 1 calc R . . C243 C 0.9887(6) 0.4787(2) 0.2472(6) 0.075(3) Uani 1 1 d . . . H243 H 1.0198 0.4975 0.2434 0.090 Uiso 1 1 calc R . . C244 C 1.0334(6) 0.4559(2) 0.2857(7) 0.081(3) Uani 1 1 d . . . H244 H 1.0942 0.4590 0.3107 0.097 Uiso 1 1 calc R . . C245 C 0.9911(6) 0.4282(2) 0.2890(7) 0.087(3) Uani 1 1 d . . . H245 H 1.0238 0.4118 0.3145 0.104 Uiso 1 1 calc R . . C246 C 0.8994(6) 0.4241(2) 0.2547(7) 0.086(4) Uani 1 1 d . . . H246 H 0.8703 0.4049 0.2573 0.104 Uiso 1 1 calc R . . C251 C 0.6652(5) 0.45573(17) 0.2449(5) 0.056(2) Uani 1 1 d . . . C252 C 0.6995(6) 0.47907(18) 0.2917(5) 0.056(2) Uani 1 1 d . . . H252 H 0.7620 0.4851 0.2968 0.068 Uiso 1 1 calc R . . C253 C 0.6418(6) 0.4934(2) 0.3307(5) 0.061(2) Uani 1 1 d . . . H253 H 0.6653 0.5092 0.3632 0.074 Uiso 1 1 calc R . . C254 C 0.5505(6) 0.4854(2) 0.3238(5) 0.058(2) Uani 1 1 d . . . H254 H 0.5107 0.4963 0.3489 0.070 Uiso 1 1 calc R . . C255 C 0.5179(6) 0.4610(2) 0.2794(5) 0.066(2) Uani 1 1 d . . . H255 H 0.4560 0.4545 0.2761 0.079 Uiso 1 1 calc R . . C256 C 0.5755(6) 0.4464(2) 0.2401(6) 0.071(3) Uani 1 1 d . . . H256 H 0.5530 0.4298 0.2096 0.085 Uiso 1 1 calc R . . C261 C 0.7065(5) 0.40379(17) 0.1564(5) 0.053(2) Uani 1 1 d . . . C262 C 0.7089(5) 0.39402(19) 0.0881(6) 0.063(2) Uani 1 1 d . . . H262 H 0.7254 0.4080 0.0541 0.076 Uiso 1 1 calc R . . C263 C 0.6875(5) 0.3641(2) 0.0677(6) 0.065(2) Uani 1 1 d . . . H263 H 0.6879 0.3573 0.0201 0.078 Uiso 1 1 calc R . . C264 C 0.6660(5) 0.3451(2) 0.1185(6) 0.065(2) Uani 1 1 d . . . H264 H 0.6503 0.3246 0.1048 0.078 Uiso 1 1 calc R . . C265 C 0.6652(6) 0.3530(2) 0.1871(7) 0.075(3) Uani 1 1 d . . . H265 H 0.6517 0.3384 0.2209 0.089 Uiso 1 1 calc R . . C266 C 0.6855(6) 0.3842(2) 0.2075(7) 0.073(3) Uani 1 1 d . . . H266 H 0.6844 0.3910 0.2549 0.088 Uiso 1 1 calc R . . C271 C 0.4095(5) 0.47698(17) 0.0536(4) 0.0461(17) Uani 1 1 d . . . C272 C 0.4537(6) 0.4526(2) 0.0246(5) 0.057(2) Uani 1 1 d . . . H272 H 0.4182 0.4379 -0.0050 0.069 Uiso 1 1 calc R . . C273 C 0.5474(5) 0.4500(2) 0.0389(5) 0.057(2) Uani 1 1 d . . . H273 H 0.5763 0.4338 0.0181 0.069 Uiso 1 1 calc R . . C274 C 0.5994(5) 0.4703(2) 0.0825(5) 0.058(2) Uani 1 1 d . . . C275 C 0.5576(5) 0.49531(18) 0.1092(5) 0.059(2) Uani 1 1 d . . . H275 H 0.5941 0.5104 0.1367 0.071 Uiso 1 1 calc R . . C276 C 0.4639(6) 0.49799(18) 0.0957(5) 0.054(2) Uani 1 1 d . . . H276 H 0.4358 0.5146 0.1156 0.065 Uiso 1 1 calc R . . N1 N 0.5669(4) 0.39688(14) 0.6251(4) 0.0504(16) Uani 1 1 d . . . N2 N 0.6007(6) 0.42371(17) 0.5384(4) 0.0659(19) Uani 1 1 d . . . C001 C 0.4887(7) 0.4385(2) 0.7618(5) 0.068(2) Uani 1 1 d . . . H00I H 0.4917 0.4607 0.7691 0.102 Uiso 1 1 calc R . . H00J H 0.5507 0.4305 0.7628 0.102 Uiso 1 1 calc R . . H00K H 0.4619 0.4289 0.8001 0.102 Uiso 1 1 calc R . . C002 C 0.4293(6) 0.4314(2) 0.6898(5) 0.063(2) Uani 1 1 d . . . H00A H 0.3669 0.4396 0.6895 0.076 Uiso 1 1 calc R . . H00B H 0.4552 0.4420 0.6518 0.076 Uiso 1 1 calc R . . C003 C 0.4218(6) 0.3977(2) 0.6723(6) 0.073(3) Uani 1 1 d . . . H00C H 0.3916 0.3875 0.7085 0.088 Uiso 1 1 calc R . . H00D H 0.3812 0.3952 0.6252 0.088 Uiso 1 1 calc R . . C004 C 0.5110(6) 0.38133(18) 0.6696(5) 0.063(2) Uani 1 1 d . . . H00E H 0.5463 0.3795 0.7189 0.075 Uiso 1 1 calc R . . H00F H 0.4973 0.3604 0.6508 0.075 Uiso 1 1 calc R . . C005 C 0.6558(5) 0.40816(19) 0.6478(5) 0.058(2) Uani 1 1 d . . . H005 H 0.6935 0.4047 0.6932 0.070 Uiso 1 1 calc R . . C006 C 0.6774(6) 0.4244(2) 0.5952(5) 0.064(2) Uani 1 1 d . . . H006 H 0.7340 0.4346 0.5950 0.076 Uiso 1 1 calc R . . C007 C 0.5385(6) 0.40639(17) 0.5605(5) 0.055(2) Uani 1 1 d . . . H007 H 0.4804 0.4015 0.5326 0.066 Uiso 1 1 calc R . . C008 C 0.5871(8) 0.4424(2) 0.4742(6) 0.077(3) Uani 1 1 d . . . H00G H 0.5477 0.4313 0.4347 0.092 Uiso 1 1 calc R . . H00H H 0.6470 0.4463 0.4595 0.092 Uiso 1 1 calc R . . C009 C 0.5432(7) 0.4720(2) 0.4867(5) 0.066(2) Uani 1 1 d . . . C010 C 0.5939(8) 0.4991(2) 0.5007(5) 0.075(3) Uani 1 1 d . . . H010 H 0.6583 0.4987 0.5015 0.091 Uiso 1 1 calc R . . C011 C 0.4481(8) 0.4735(2) 0.4866(6) 0.077(3) Uani 1 1 d . . . H011 H 0.4120 0.4555 0.4778 0.092 Uiso 1 1 calc R . . O01W O 0.2092(9) 0.4677(2) 0.5237(7) 0.148(4) Uani 1 1 d . . . H01X H 0.2085 0.4527 0.4951 0.223 Uiso 1 1 d . . . H01Y H 0.2003 0.4840 0.4990 0.223 Uiso 1 1 d . . . O02W O 0.4904(7) 0.3734(3) 0.3464(7) 0.147(4) Uani 1 1 d . . . H02X H 0.4436 0.3778 0.3648 0.220 Uiso 1 1 d . . . H02Y H 0.5363 0.3715 0.3801 0.220 Uiso 1 1 d . . . O03W O 0.9521(9) 0.3944(2) 0.5742(6) 0.142(4) Uani 1 1 d . . . H03X H 0.9041 0.3834 0.5664 0.213 Uiso 1 1 d . . . H03Y H 0.9397 0.4108 0.5946 0.213 Uiso 1 1 d . . . O04W O 0.6021(5) 0.28509(19) 0.3588(4) 0.095(2) Uani 1 1 d . . . H04X H 0.6407 0.2941 0.3906 0.142 Uiso 1 1 d . . . H04Y H 0.5742 0.2717 0.3793 0.142 Uiso 1 1 d . . . O05W O 0.7598(8) 0.4102(2) 0.3794(7) 0.148(4) Uani 1 1 d . . . H05X H 0.7375 0.3999 0.4103 0.222 Uiso 1 1 d . . . H05Y H 0.7974 0.4231 0.4014 0.222 Uiso 1 1 d . . . O06W O 0.9257(4) 0.44949(14) 0.7819(4) 0.0672(16) Uani 1 1 d . . . H06X H 0.8855 0.4390 0.7981 0.101 Uiso 1 1 d . . . H06Y H 0.9785 0.4434 0.8020 0.101 Uiso 1 1 d . . . O07W O 0.1054(6) 0.4797(3) 0.6259(5) 0.117(3) Uani 1 1 d . . . H07X H 0.1327 0.4728 0.6660 0.175 Uiso 1 1 d . . . H07Y H 0.1383 0.4759 0.5945 0.175 Uiso 1 1 d . . . O08W O 0.8253(5) 0.3551(2) 0.3434(5) 0.105(3) Uani 1 1 d . . . H08X H 0.8037 0.3432 0.3716 0.158 Uiso 1 1 d . . . H08Y H 0.8091 0.3733 0.3512 0.158 Uiso 1 1 d . . . O09W O 0.4552(5) 0.28464(14) 0.1502(4) 0.0779(18) Uani 1 1 d . . . H09X H 0.4677 0.2662 0.1619 0.117 Uiso 1 1 d . . . H09Y H 0.4678 0.2957 0.1875 0.117 Uiso 1 1 d . . . O10W O 0.4942(5) 0.32166(16) 0.2677(4) 0.085(2) Uani 1 1 d . . . H10X H 0.4910 0.3382 0.2907 0.128 Uiso 1 1 d . . . H10Y H 0.5279 0.3092 0.2950 0.128 Uiso 1 1 d . . . O11W O 0.5667(6) 0.2751(2) 0.0544(5) 0.114(3) Uani 1 1 d . . . H11X H 0.5260 0.2776 0.0805 0.171 Uiso 1 1 d . . . H11Y H 0.5398 0.2706 0.0123 0.171 Uiso 1 1 d . . . O12W O 0.8163(7) 0.4772(3) 0.5342(7) 0.153(4) Uani 1 1 d . . . H12X H 0.8371 0.4720 0.4969 0.229 Uiso 1 1 d . . . H12Y H 0.8482 0.4684 0.5702 0.229 Uiso 1 1 d . . . O13W O 0.8916(9) 0.4584(3) 0.4228(6) 0.151(4) Uani 1 1 d . . . H13X H 0.9065 0.4755 0.4075 0.227 Uiso 1 1 d . . . H13Y H 0.9379 0.4466 0.4269 0.227 Uiso 1 1 d . . . O14W O 0.9200(11) 0.4485(2) 0.6401(5) 0.163(5) Uani 1 1 d . . . H14X H 0.9191 0.4482 0.6848 0.244 Uiso 1 1 d . . . H14Y H 0.9700 0.4567 0.6338 0.244 Uiso 1 1 d . . . O15W O 0.5020(4) 0.24048(13) 0.4111(4) 0.0695(17) Uani 1 1 d . . . H15X H 0.4985 0.2268 0.3788 0.104 Uiso 1 1 d . . . H15Y H 0.4480 0.2465 0.4134 0.104 Uiso 1 1 d . . . O16W O 1.0141(9) 0.4084(3) 0.4480(8) 0.164(5) Uani 1 1 d . . . H16X H 1.0720 0.4075 0.4505 0.245 Uiso 1 1 d . . . H16Y H 1.0018 0.4038 0.4888 0.245 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.043(3) 0.033(3) 0.072(4) 0.000(2) -0.001(2) -0.005(2) C11 0.030(3) 0.030(3) 0.063(5) -0.004(3) 0.002(3) -0.011(3) C12 0.032(3) 0.033(4) 0.062(5) -0.007(3) -0.005(3) -0.004(3) C13 0.035(3) 0.037(4) 0.060(5) -0.001(3) 0.001(3) -0.005(3) C14 0.032(3) 0.040(4) 0.064(5) -0.009(3) -0.002(3) -0.007(3) C15 0.035(3) 0.034(4) 0.066(5) -0.008(3) -0.005(4) -0.002(3) C16 0.025(3) 0.037(4) 0.061(5) -0.008(3) -0.008(3) -0.009(3) S1 0.0428(9) 0.0389(9) 0.0683(13) 0.0021(9) -0.0022(9) 0.0010(7) C1 0.032(3) 0.035(4) 0.067(5) -0.004(3) 0.000(3) 0.000(3) O2 0.051(3) 0.036(3) 0.069(4) -0.002(2) -0.005(3) -0.004(2) C21 0.035(3) 0.026(3) 0.068(5) -0.005(3) 0.000(4) 0.004(3) C22 0.037(4) 0.031(4) 0.076(6) -0.017(4) -0.003(4) 0.007(3) C23 0.024(3) 0.040(4) 0.091(7) -0.018(4) 0.008(4) 0.003(3) C24 0.033(4) 0.036(4) 0.085(6) -0.017(4) 0.007(4) 0.001(3) C25 0.038(4) 0.038(4) 0.076(6) -0.004(4) 0.005(4) 0.008(3) C26 0.027(3) 0.027(3) 0.067(5) -0.004(3) -0.001(3) -0.002(3) S2 0.0423(10) 0.0482(11) 0.1055(18) -0.0101(11) 0.0201(11) 0.0004(8) O21 0.046(3) 0.077(4) 0.129(6) -0.030(4) 0.025(4) -0.029(3) O22 0.041(3) 0.078(4) 0.087(4) -0.018(3) 0.016(3) -0.013(3) O23 0.061(4) 0.056(4) 0.139(6) 0.018(4) 0.029(4) 0.016(3) C2 0.034(4) 0.041(4) 0.076(6) -0.009(4) -0.006(4) 0.004(3) O3 0.042(2) 0.021(2) 0.070(3) -0.004(2) -0.006(2) -0.0033(18) C31 0.037(4) 0.027(3) 0.059(5) 0.000(3) -0.010(3) 0.001(3) C32 0.032(3) 0.034(4) 0.060(5) 0.002(3) -0.005(3) 0.002(3) C33 0.032(3) 0.029(3) 0.069(5) -0.004(3) 0.005(3) 0.001(3) C34 0.030(3) 0.028(3) 0.063(5) -0.004(3) -0.004(3) 0.002(3) C35 0.027(3) 0.035(4) 0.065(5) -0.004(3) -0.002(3) 0.001(3) C36 0.034(3) 0.024(3) 0.068(5) -0.007(3) -0.009(3) 0.003(3) S3 0.0277(8) 0.0296(8) 0.0728(13) -0.0056(8) -0.0033(8) 0.0028(6) O31 0.040(2) 0.032(2) 0.073(4) -0.013(2) 0.007(2) -0.002(2) O32 0.047(3) 0.038(3) 0.105(5) 0.002(3) -0.032(3) 0.005(2) O33 0.052(3) 0.041(3) 0.080(4) -0.014(3) 0.009(3) -0.007(2) C3 0.034(3) 0.039(4) 0.065(5) -0.008(3) -0.005(3) -0.007(3) O4 0.038(2) 0.032(2) 0.076(4) -0.005(2) -0.003(2) -0.0060(19) C41 0.038(3) 0.037(4) 0.055(5) -0.006(3) 0.008(3) -0.005(3) C42 0.029(3) 0.041(4) 0.064(5) -0.011(3) 0.007(3) -0.007(3) C43 0.030(3) 0.045(4) 0.057(5) -0.002(3) 0.003(3) -0.001(3) C44 0.042(4) 0.046(4) 0.057(5) -0.007(4) 0.014(4) -0.006(3) C45 0.030(3) 0.043(4) 0.057(5) -0.009(3) 0.000(3) -0.006(3) C46 0.038(4) 0.040(4) 0.059(5) -0.008(3) 0.012(3) -0.005(3) S4 0.0463(10) 0.0421(10) 0.0721(14) -0.0125(9) 0.0018(9) 0.0033(8) C4 0.029(3) 0.044(4) 0.064(5) -0.010(4) -0.007(3) -0.004(3) P11 0.0351(8) 0.0335(9) 0.0546(11) -0.0039(8) 0.0071(8) -0.0014(7) P12 0.0323(8) 0.0312(9) 0.0593(12) -0.0038(8) 0.0016(8) 0.0033(7) C101 0.039(4) 0.036(4) 0.064(5) -0.009(3) 0.006(3) -0.006(3) C102 0.036(3) 0.031(3) 0.065(5) -0.005(3) -0.002(3) 0.004(3) C111 0.034(3) 0.034(4) 0.066(5) -0.001(3) 0.003(3) -0.006(3) C112 0.046(4) 0.048(4) 0.053(5) -0.012(4) 0.006(4) 0.007(3) C113 0.046(4) 0.052(5) 0.057(5) -0.012(4) 0.007(4) -0.007(3) C114 0.057(5) 0.045(4) 0.057(5) -0.010(4) 0.003(4) -0.009(4) C115 0.045(4) 0.037(4) 0.063(5) -0.004(4) -0.008(4) -0.009(3) C116 0.031(3) 0.032(4) 0.068(5) -0.009(3) 0.004(3) -0.005(3) C121 0.048(4) 0.028(3) 0.051(5) 0.000(3) -0.002(3) -0.003(3) C122 0.049(4) 0.035(4) 0.061(5) -0.006(3) 0.009(4) -0.012(3) C123 0.057(5) 0.047(5) 0.080(7) 0.003(4) 0.004(4) -0.023(4) C124 0.071(6) 0.050(5) 0.067(6) 0.002(4) -0.008(5) -0.020(4) C125 0.095(7) 0.054(5) 0.060(6) -0.004(4) -0.001(5) -0.026(5) C126 0.060(5) 0.048(5) 0.057(5) 0.001(4) 0.003(4) -0.009(4) C131 0.045(4) 0.043(4) 0.061(5) -0.005(4) 0.005(4) 0.008(3) C132 0.038(4) 0.060(5) 0.066(5) 0.005(4) 0.004(4) 0.003(3) C133 0.039(4) 0.076(6) 0.089(7) 0.006(5) 0.012(4) 0.008(4) C134 0.057(5) 0.065(6) 0.096(7) -0.005(5) 0.018(5) 0.025(5) C135 0.068(6) 0.065(6) 0.109(8) -0.001(6) 0.030(6) 0.014(5) C136 0.060(5) 0.048(5) 0.090(7) -0.008(5) 0.025(5) 0.011(4) C141 0.027(3) 0.038(4) 0.067(5) -0.017(3) 0.010(3) 0.003(3) C142 0.039(4) 0.046(4) 0.054(5) -0.003(3) 0.003(3) 0.004(3) C143 0.053(4) 0.045(4) 0.065(6) -0.004(4) 0.012(4) 0.000(3) C144 0.038(4) 0.076(6) 0.050(5) -0.007(4) 0.001(3) 0.004(4) C145 0.037(4) 0.061(5) 0.057(5) -0.015(4) 0.013(3) -0.004(3) C146 0.029(3) 0.049(4) 0.065(5) -0.010(4) 0.012(3) 0.001(3) C151 0.040(4) 0.034(4) 0.064(5) -0.006(3) -0.002(4) -0.004(3) C152 0.039(4) 0.037(4) 0.082(6) -0.007(4) 0.005(4) -0.001(3) C153 0.041(4) 0.040(4) 0.093(7) 0.000(4) 0.013(4) 0.003(3) C154 0.036(4) 0.039(4) 0.100(7) -0.001(4) 0.002(5) -0.001(3) C155 0.050(4) 0.034(4) 0.084(6) 0.004(4) -0.015(5) -0.001(3) C156 0.046(4) 0.035(4) 0.069(5) -0.001(4) -0.011(4) 0.000(3) C161 0.036(3) 0.037(4) 0.050(4) 0.000(3) 0.004(3) 0.002(3) C162 0.032(3) 0.032(3) 0.073(5) -0.006(3) -0.005(3) 0.001(3) C163 0.029(3) 0.045(4) 0.068(5) -0.006(4) 0.002(3) 0.002(3) C164 0.047(4) 0.037(4) 0.055(5) -0.002(3) 0.005(3) -0.004(3) C165 0.044(4) 0.034(4) 0.063(5) -0.004(3) 0.009(3) 0.004(3) C166 0.042(4) 0.033(4) 0.071(5) -0.005(3) 0.012(4) 0.003(3) C171 0.037(3) 0.025(3) 0.063(5) -0.005(3) 0.005(3) 0.000(3) C172 0.030(3) 0.038(4) 0.060(5) -0.003(3) 0.006(3) 0.000(3) C173 0.026(3) 0.034(4) 0.073(6) -0.008(3) -0.001(3) -0.001(3) C174 0.039(4) 0.022(3) 0.061(5) 0.002(3) 0.008(3) 0.002(3) C175 0.029(3) 0.038(4) 0.059(5) 0.003(3) 0.001(3) -0.008(3) C176 0.032(3) 0.036(4) 0.054(5) 0.000(3) 0.003(3) -0.007(3) P21 0.0417(9) 0.0348(9) 0.0649(13) -0.0079(9) 0.0087(9) 0.0022(7) P22 0.0407(10) 0.0332(9) 0.0923(16) -0.0095(10) 0.0191(10) -0.0011(8) C201 0.047(4) 0.045(4) 0.065(5) 0.005(4) 0.015(4) 0.009(3) C202 0.057(5) 0.054(5) 0.094(7) -0.004(5) 0.033(5) 0.000(4) C211 0.053(4) 0.033(4) 0.067(6) -0.016(4) 0.008(4) 0.003(3) C212 0.049(5) 0.089(7) 0.066(6) -0.012(5) 0.013(4) -0.008(4) C213 0.041(5) 0.092(7) 0.083(7) -0.007(6) -0.008(5) 0.012(5) C214 0.040(4) 0.066(6) 0.099(8) -0.038(6) -0.007(5) 0.007(4) C215 0.043(4) 0.043(5) 0.122(9) -0.021(5) 0.019(5) -0.006(4) C216 0.041(4) 0.046(4) 0.085(6) -0.008(4) 0.009(4) 0.000(3) C221 0.041(4) 0.036(4) 0.074(6) -0.005(4) 0.015(4) 0.000(3) C222 0.046(4) 0.035(4) 0.088(6) -0.011(4) 0.023(4) -0.001(3) C223 0.055(5) 0.034(4) 0.091(7) -0.016(4) 0.027(5) -0.011(3) C224 0.060(5) 0.034(4) 0.104(7) -0.008(5) 0.013(5) 0.003(4) C225 0.070(6) 0.049(5) 0.096(7) -0.002(5) 0.009(5) 0.014(4) C226 0.064(5) 0.037(4) 0.082(6) -0.005(4) 0.009(5) 0.010(4) C231 0.034(3) 0.042(4) 0.073(5) -0.004(4) 0.006(3) 0.003(3) C232 0.036(3) 0.035(4) 0.065(5) -0.005(3) -0.003(3) 0.003(3) C233 0.049(4) 0.037(4) 0.071(6) -0.010(4) 0.011(4) 0.002(3) C234 0.050(4) 0.049(5) 0.076(6) -0.004(4) 0.009(4) 0.003(4) C235 0.046(4) 0.060(5) 0.061(5) 0.003(4) 0.012(4) -0.006(4) C236 0.052(4) 0.040(4) 0.073(6) 0.005(4) 0.014(4) 0.000(3) C241 0.048(4) 0.030(4) 0.096(7) -0.009(4) 0.022(4) -0.004(3) C242 0.065(5) 0.043(5) 0.120(9) -0.016(5) 0.029(6) -0.014(4) C243 0.055(5) 0.052(5) 0.122(9) -0.030(6) 0.029(5) -0.021(4) C244 0.052(5) 0.054(6) 0.136(10) -0.028(6) 0.018(6) -0.011(4) C245 0.057(5) 0.048(5) 0.147(11) -0.014(6) -0.002(6) 0.004(4) C246 0.045(5) 0.038(5) 0.170(12) -0.013(6) 0.004(6) -0.001(4) C251 0.042(4) 0.037(4) 0.089(6) -0.012(4) 0.010(4) 0.000(3) C252 0.051(4) 0.046(4) 0.074(6) -0.002(4) 0.015(4) -0.005(3) C253 0.052(5) 0.051(5) 0.083(6) -0.012(4) 0.017(4) 0.003(4) C254 0.057(5) 0.055(5) 0.061(5) -0.001(4) 0.008(4) 0.008(4) C255 0.047(4) 0.076(6) 0.077(6) -0.002(5) 0.016(4) -0.005(4) C256 0.056(5) 0.055(5) 0.106(8) -0.020(5) 0.028(5) -0.005(4) C261 0.033(4) 0.039(4) 0.086(6) -0.008(4) 0.007(4) -0.002(3) C262 0.043(4) 0.040(4) 0.107(8) -0.010(5) 0.012(4) 0.012(3) C263 0.045(4) 0.056(5) 0.090(7) -0.017(5) 0.003(4) 0.008(4) C264 0.043(4) 0.049(5) 0.102(8) -0.012(5) 0.010(5) -0.004(4) C265 0.061(5) 0.057(6) 0.109(9) 0.000(6) 0.024(5) -0.019(4) C266 0.060(5) 0.053(5) 0.109(8) -0.006(5) 0.020(5) -0.006(4) C271 0.047(4) 0.040(4) 0.054(5) 0.002(3) 0.016(3) 0.003(3) C272 0.053(4) 0.062(5) 0.058(5) -0.009(4) 0.013(4) 0.009(4) C273 0.051(4) 0.058(5) 0.066(5) -0.003(4) 0.016(4) 0.012(4) C274 0.046(4) 0.054(5) 0.075(6) 0.004(4) 0.017(4) 0.008(4) C275 0.050(4) 0.042(4) 0.086(6) -0.011(4) 0.016(4) 0.000(3) C276 0.060(5) 0.041(4) 0.066(5) -0.002(4) 0.023(4) -0.002(4) N1 0.054(4) 0.036(3) 0.057(4) 0.001(3) -0.001(3) 0.003(3) N2 0.084(5) 0.052(4) 0.064(5) -0.007(4) 0.016(4) -0.011(4) C001 0.076(6) 0.051(5) 0.075(6) 0.001(4) 0.009(5) -0.007(4) C002 0.056(5) 0.056(5) 0.077(6) 0.003(4) 0.011(4) 0.011(4) C003 0.057(5) 0.068(6) 0.094(7) 0.007(5) 0.011(5) -0.015(4) C004 0.074(6) 0.035(4) 0.073(6) -0.004(4) -0.003(5) -0.009(4) C005 0.045(4) 0.048(5) 0.075(6) -0.001(4) -0.010(4) 0.002(3) C006 0.050(5) 0.058(5) 0.082(7) -0.017(5) 0.007(5) -0.004(4) C007 0.056(5) 0.038(4) 0.069(6) -0.006(4) 0.002(4) -0.007(3) C008 0.089(7) 0.073(7) 0.069(6) -0.016(5) 0.014(5) -0.018(5) C009 0.095(7) 0.044(5) 0.058(5) -0.006(4) 0.012(5) -0.021(4) C010 0.092(7) 0.066(6) 0.067(6) 0.008(5) 0.011(5) -0.021(5) C011 0.100(8) 0.045(5) 0.082(7) 0.004(5) 0.009(6) -0.016(5) O01W 0.163(10) 0.090(7) 0.194(12) -0.032(7) 0.038(8) -0.024(6) O02W 0.104(7) 0.150(10) 0.187(11) -0.027(8) 0.029(7) 0.014(6) O03W 0.193(11) 0.094(7) 0.142(9) -0.001(6) 0.040(8) -0.030(7) O04W 0.095(5) 0.091(5) 0.096(5) -0.019(4) 0.010(4) -0.037(4) O05W 0.172(10) 0.095(7) 0.197(12) 0.031(7) 0.087(9) 0.024(7) O06W 0.045(3) 0.059(4) 0.096(5) -0.004(3) 0.006(3) -0.008(3) O07W 0.087(5) 0.163(9) 0.097(6) -0.025(6) 0.006(5) 0.011(5) O08W 0.086(5) 0.108(6) 0.128(7) 0.029(5) 0.034(5) 0.015(4) O09W 0.099(5) 0.044(3) 0.089(5) 0.001(3) 0.014(4) 0.004(3) O10W 0.096(5) 0.065(4) 0.092(5) -0.010(4) 0.011(4) -0.001(4) O11W 0.111(6) 0.126(7) 0.107(6) -0.025(5) 0.026(5) -0.053(6) O12W 0.105(7) 0.188(12) 0.165(10) 0.015(9) 0.023(7) 0.014(7) O13W 0.165(10) 0.157(10) 0.123(8) 0.013(7) 0.001(7) 0.063(8) O14W 0.307(17) 0.085(6) 0.085(6) -0.006(5) 0.004(8) 0.017(8) O15W 0.072(4) 0.044(3) 0.089(5) -0.015(3) 0.004(3) 0.007(3) O16W 0.153(10) 0.146(11) 0.207(13) 0.035(9) 0.075(9) 0.046(8) _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 C11 1.359(9) . ? O1 H1 0.8500 . ? C11 C12 1.370(11) . ? C11 C16 1.429(10) . ? C12 C13 1.386(11) . ? C12 C1 1.522(10) . ? C13 C14 1.384(10) . ? C13 H13 0.9500 . ? C14 C15 1.384(11) . ? C14 S1 1.778(8) . ? C15 C16 1.394(11) . ? C15 H15 0.9500 . ? C16 C4 1.497(11) . ? S1 O14 1.431(7) . ? S1 O15 1.432(7) . ? S1 O16 1.436(7) . ? S1 O13 1.436(6) . ? S1 O12 1.443(6) . ? S1 O11 1.449(6) . ? C1 C26 1.534(9) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? O2 C21 1.341(10) . ? O2 H2 0.8500 . ? C21 C26 1.388(11) . ? C21 C22 1.433(10) . ? C22 C23 1.381(12) . ? C22 C2 1.524(12) . ? C23 C24 1.385(13) . ? C23 H23 0.9500 . ? C24 C25 1.417(10) . ? C24 S2 1.764(9) . ? C25 C26 1.391(11) . ? C25 H25 0.9500 . ? S2 O22 1.429(7) . ? S2 O21 1.456(7) . ? S2 O23 1.474(7) . ? C2 C36 1.516(11) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? O3 C31 1.344(8) . ? O3 H3 0.8500 . ? C31 C36 1.411(11) . ? C31 C32 1.420(11) . ? C32 C33 1.397(10) . ? C32 C3 1.492(11) . ? C33 C34 1.413(10) . ? C33 H33 0.9500 . ? C34 C35 1.375(10) . ? C34 S3 1.774(7) . ? C35 C36 1.391(9) . ? C35 H35 0.9500 . ? S3 O32 1.444(5) . ? S3 O33 1.445(7) . ? S3 O31 1.449(5) . ? C3 C46 1.509(10) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? O4 C41 1.363(9) . ? O4 H4 0.8500 . ? C41 C46 1.417(10) . ? C41 C42 1.417(11) . ? C42 C43 1.384(10) . ? C42 C4 1.541(10) . ? C43 C44 1.384(10) . ? C43 H43 0.9500 . ? C44 C45 1.396(10) . ? C44 S4 1.774(8) . ? C45 C46 1.394(10) . ? C45 H45 0.9500 . ? S4 O43 1.416(6) . ? S4 O44 1.422(6) . ? S4 O45 1.441(7) . ? S4 O41 1.463(6) . ? S4 O42 1.463(6) . ? S4 O46 1.484(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? P11 C131 1.785(8) . ? P11 C111 1.786(8) . ? P11 C121 1.793(7) . ? P11 C101 1.816(7) . ? P12 C141 1.769(8) . ? P12 C161 1.788(7) . ? P12 C151 1.796(7) . ? P12 C102 1.821(7) . ? C101 C171 1.491(11) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 C174 1.481(11) . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C111 C116 1.402(10) . ? C111 C112 1.424(11) . ? C112 C113 1.376(12) . ? C112 H112 0.9500 . ? C113 C114 1.394(12) . ? C113 H113 0.9500 . ? C114 C115 1.380(12) . ? C114 H114 0.9500 . ? C115 C116 1.362(12) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C121 C126 1.376(12) . ? C121 C122 1.411(11) . ? C122 C123 1.429(11) . ? C122 H122 0.9500 . ? C123 C124 1.330(14) . ? C123 H123 0.9500 . ? C124 C125 1.357(14) . ? C124 H124 0.9500 . ? C125 C126 1.386(12) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? C131 C132 1.370(11) . ? C131 C136 1.412(12) . ? C132 C133 1.403(12) . ? C132 H132 0.9500 . ? C133 C134 1.403(14) . ? C133 H133 0.9500 . ? C134 C135 1.341(14) . ? C134 H134 0.9500 . ? C135 C136 1.386(13) . ? C135 H135 0.9500 . ? C136 H136 0.9500 . ? C141 C146 1.398(10) . ? C141 C142 1.421(11) . ? C142 C143 1.362(12) . ? C142 H142 0.9500 . ? C143 C144 1.393(12) . ? C143 H143 0.9500 . ? C144 C145 1.391(12) . ? C144 H144 0.9500 . ? C145 C146 1.361(12) . ? C145 H145 0.9500 . ? C146 H146 0.9500 . ? C151 C152 1.373(12) . ? C151 C156 1.410(12) . ? C152 C153 1.397(11) . ? C152 H152 0.9500 . ? C153 C154 1.360(13) . ? C153 H153 0.9500 . ? C154 C155 1.373(14) . ? C154 H154 0.9500 . ? C155 C156 1.431(11) . ? C155 H155 0.9500 . ? C156 H156 0.9500 . ? C161 C162 1.391(10) . ? C161 C166 1.410(10) . ? C162 C163 1.405(10) . ? C162 H162 0.9500 . ? C163 C164 1.361(11) . ? C163 H163 0.9500 . ? C164 C165 1.380(10) . ? C164 H164 0.9500 . ? C165 C166 1.397(10) . ? C165 H165 0.9500 . ? C166 H166 0.9500 . ? C171 C172 1.417(10) . ? C171 C176 1.418(10) . ? C172 C173 1.352(11) . ? C172 H172 0.9500 . ? C173 C174 1.404(10) . ? C173 H173 0.9500 . ? C174 C175 1.409(10) . ? C175 C176 1.353(11) . ? C175 H175 0.9500 . ? C176 H176 0.9500 . ? P21 C231 1.783(9) . ? P21 C221 1.793(7) . ? P21 C211 1.804(8) . ? P21 C201 1.816(8) . ? P22 C251 1.788(9) . ? P22 C241 1.792(8) . ? P22 C261 1.797(8) . ? P22 C202 1.843(10) . ? C201 C271 1.505(10) . ? C201 H20A 0.9900 . ? C201 H20B 0.9900 . ? C202 C274 1.511(12) . ? C202 H20C 0.9900 . ? C202 H20D 0.9900 . ? C211 C212 1.357(13) . ? C211 C216 1.384(12) . ? C212 C213 1.392(12) . ? C212 H212 0.9500 . ? C213 C214 1.368(15) . ? C213 H213 0.9500 . ? C214 C215 1.379(15) . ? C214 H214 0.9500 . ? C215 C216 1.426(12) . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? C221 C222 1.403(12) . ? C221 C226 1.413(12) . ? C222 C223 1.418(11) . ? C222 H222 0.9500 . ? C223 C224 1.348(13) . ? C223 H223 0.9500 . ? C224 C225 1.379(14) . ? C224 H224 0.9500 . ? C225 C226 1.400(12) . ? C225 H225 0.9500 . ? C226 H226 0.9500 . ? C231 C236 1.389(12) . ? C231 C232 1.413(10) . ? C232 C233 1.346(12) . ? C232 H232 0.9500 . ? C233 C234 1.370(13) . ? C233 H233 0.9500 . ? C234 C235 1.397(12) . ? C234 H234 0.9500 . ? C235 C236 1.357(12) . ? C235 H235 0.9500 . ? C236 H236 0.9500 . ? C241 C246 1.346(13) . ? C241 C242 1.429(11) . ? C242 C243 1.387(14) . ? C242 H242 0.9500 . ? C243 C244 1.338(15) . ? C243 H243 0.9500 . ? C244 C245 1.372(14) . ? C244 H244 0.9500 . ? C245 C246 1.410(13) . ? C245 H245 0.9500 . ? C246 H246 0.9500 . ? C251 C256 1.376(12) . ? C251 C252 1.390(12) . ? C252 C253 1.374(12) . ? C252 H252 0.9500 . ? C253 C254 1.378(12) . ? C253 H253 0.9500 . ? C254 C255 1.389(13) . ? C254 H254 0.9500 . ? C255 C256 1.386(13) . ? C255 H255 0.9500 . ? C256 H256 0.9500 . ? C261 C266 1.370(14) . ? C261 C262 1.370(13) . ? C262 C263 1.386(12) . ? C262 H262 0.9500 . ? C263 C264 1.353(14) . ? C263 H263 0.9500 . ? C264 C265 1.348(15) . ? C264 H264 0.9500 . ? C265 C266 1.436(13) . ? C265 H265 0.9500 . ? C266 H266 0.9500 . ? C271 C276 1.379(11) . ? C271 C272 1.413(11) . ? C272 C273 1.368(11) . ? C272 H272 0.9500 . ? C273 C274 1.355(12) . ? C273 H273 0.9500 . ? C274 C275 1.398(12) . ? C275 C276 1.370(12) . ? C275 H275 0.9500 . ? C276 H276 0.9500 . ? N1 C007 1.291(11) . ? N1 C005 1.400(10) . ? N1 C004 1.451(12) . ? N2 C007 1.317(11) . ? N2 C006 1.420(12) . ? N2 C008 1.451(13) . ? C001 C002 1.519(13) . ? C001 H00I 0.9800 . ? C001 H00J 0.9800 . ? C001 H00K 0.9800 . ? C002 C003 1.514(13) . ? C002 H00A 0.9900 . ? C002 H00B 0.9900 . ? C003 C004 1.509(13) . ? C003 H00C 0.9900 . ? C003 H00D 0.9900 . ? C004 H00E 0.9900 . ? C004 H00F 0.9900 . ? C005 C006 1.309(13) . ? C005 H005 0.9500 . ? C006 H006 0.9500 . ? C007 H007 0.9500 . ? C008 C009 1.488(14) . ? C008 H00G 0.9900 . ? C008 H00H 0.9900 . ? C009 C010 1.402(13) . ? C009 C011 1.408(15) . ? C010 C011 1.392(15) 3_666 ? C010 H010 0.9500 . ? C011 C010 1.392(15) 3_666 ? C011 H011 0.9500 . ? O01W H01X 0.8500 . ? O01W H01Y 0.8501 . ? O02W H02X 0.8499 . ? O02W H02Y 0.8500 . ? O03W H03X 0.8500 . ? O03W H03Y 0.8497 . ? O04W H04X 0.8499 . ? O04W H04Y 0.8499 . ? O05W H05X 0.8501 . ? O05W H05Y 0.8499 . ? O06W H06X 0.8500 . ? O06W H06Y 0.8500 . ? O07W H07X 0.8501 . ? O07W H07Y 0.8501 . ? O08W H08X 0.8499 . ? O08W H08Y 0.8501 . ? O09W H09X 0.8501 . ? O09W H09Y 0.8500 . ? O10W H10X 0.8499 . ? O10W H10Y 0.8499 . ? O11W H11X 0.8502 . ? O11W H11Y 0.8499 . ? O12W H12X 0.8501 . ? O12W H12Y 0.8501 . ? O13W H13X 0.8502 . ? O13W H13Y 0.8502 . ? O14W H14X 0.8501 . ? O14W H14Y 0.8501 . ? O15W H15X 0.8500 . ? O15W H15Y 0.8499 . ? O16W H16X 0.8500 . ? O16W H16Y 0.8500 . ? 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 O1 H1 109.5 . . ? O1 C11 C12 118.9(6) . . ? O1 C11 C16 119.5(7) . . ? C12 C11 C16 121.6(7) . . ? C11 C12 C13 119.0(7) . . ? C11 C12 C1 120.4(7) . . ? C13 C12 C1 120.4(7) . . ? C14 C13 C12 121.2(8) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C15 C14 C13 119.6(7) . . ? C15 C14 S1 121.6(5) . . ? C13 C14 S1 118.7(6) . . ? C14 C15 C16 121.2(7) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C15 C16 C11 117.3(7) . . ? C15 C16 C4 120.9(7) . . ? C11 C16 C4 121.7(7) . . ? O14 S1 O15 114.1(6) . . ? O14 S1 O16 113.1(6) . . ? O15 S1 O16 112.9(6) . . ? O14 S1 O13 81.0(8) . . ? O15 S1 O13 139.6(8) . . ? O14 S1 O12 137.7(8) . . ? O16 S1 O12 81.7(7) . . ? O13 S1 O12 112.4(4) . . ? O15 S1 O11 83.6(8) . . ? O16 S1 O11 139.5(8) . . ? O13 S1 O11 111.4(4) . . ? O12 S1 O11 112.5(4) . . ? O14 S1 C14 106.1(7) . . ? O15 S1 C14 103.9(7) . . ? O16 S1 C14 105.6(7) . . ? O13 S1 C14 107.3(4) . . ? O12 S1 C14 107.2(3) . . ? O11 S1 C14 105.5(4) . . ? C12 C1 C26 110.2(6) . . ? C12 C1 H1A 109.6 . . ? C26 C1 H1A 109.6 . . ? C12 C1 H1B 109.6 . . ? C26 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? C21 O2 H2 109.5 . . ? O2 C21 C26 119.2(6) . . ? O2 C21 C22 120.7(7) . . ? C26 C21 C22 120.1(7) . . ? C23 C22 C21 118.9(8) . . ? C23 C22 C2 121.2(7) . . ? C21 C22 C2 119.9(8) . . ? C22 C23 C24 121.5(7) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? C23 C24 C25 119.2(8) . . ? C23 C24 S2 121.8(6) . . ? C25 C24 S2 119.0(7) . . ? C26 C25 C24 120.4(8) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C21 C26 C25 119.8(6) . . ? C21 C26 C1 121.2(7) . . ? C25 C26 C1 118.9(7) . . ? O22 S2 O21 113.4(4) . . ? O22 S2 O23 112.5(5) . . ? O21 S2 O23 111.6(4) . . ? O22 S2 C24 105.9(4) . . ? O21 S2 C24 105.5(4) . . ? O23 S2 C24 107.3(4) . . ? C36 C2 C22 113.9(6) . . ? C36 C2 H2A 108.8 . . ? C22 C2 H2A 108.8 . . ? C36 C2 H2B 108.8 . . ? C22 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? C31 O3 H3 109.5 . . ? O3 C31 C36 119.8(6) . . ? O3 C31 C32 119.5(6) . . ? C36 C31 C32 120.7(6) . . ? C33 C32 C31 119.0(7) . . ? C33 C32 C3 120.0(7) . . ? C31 C32 C3 120.9(6) . . ? C32 C33 C34 120.2(7) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C35 C34 C33 119.3(6) . . ? C35 C34 S3 119.8(5) . . ? C33 C34 S3 120.4(5) . . ? C34 C35 C36 122.6(7) . . ? C34 C35 H35 118.7 . . ? C36 C35 H35 118.7 . . ? C35 C36 C31 118.0(7) . . ? C35 C36 C2 120.7(7) . . ? C31 C36 C2 121.2(6) . . ? O32 S3 O33 111.5(4) . . ? O32 S3 O31 113.4(4) . . ? O33 S3 O31 113.2(3) . . ? O32 S3 C34 104.7(3) . . ? O33 S3 C34 105.1(4) . . ? O31 S3 C34 108.2(3) . . ? C32 C3 C46 115.5(7) . . ? C32 C3 H3A 108.4 . . ? C46 C3 H3A 108.4 . . ? C32 C3 H3B 108.4 . . ? C46 C3 H3B 108.4 . . ? H3A C3 H3B 107.5 . . ? C41 O4 H4 109.5 . . ? O4 C41 C46 119.9(6) . . ? O4 C41 C42 119.0(6) . . ? C46 C41 C42 121.1(6) . . ? C43 C42 C41 118.8(7) . . ? C43 C42 C4 119.7(6) . . ? C41 C42 C4 121.5(6) . . ? C44 C43 C42 120.4(7) . . ? C44 C43 H43 119.8 . . ? C42 C43 H43 119.8 . . ? C43 C44 C45 121.1(7) . . ? C43 C44 S4 118.1(5) . . ? C45 C44 S4 120.8(5) . . ? C46 C45 C44 120.5(7) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C45 C46 C41 118.1(7) . . ? C45 C46 C3 119.9(6) . . ? C41 C46 C3 122.0(6) . . ? O43 S4 O44 126.1(6) . . ? O43 S4 O45 88.3(6) . . ? O44 S4 O45 115.1(5) . . ? O43 S4 O41 114.3(5) . . ? O45 S4 O41 131.6(6) . . ? O43 S4 O42 113.6(5) . . ? O44 S4 O42 92.8(6) . . ? O41 S4 O42 110.6(5) . . ? O44 S4 O46 111.8(5) . . ? O45 S4 O46 110.5(5) . . ? O41 S4 O46 96.6(6) . . ? O42 S4 O46 135.3(5) . . ? O43 S4 C44 108.6(5) . . ? O44 S4 C44 109.4(5) . . ? O45 S4 C44 106.6(6) . . ? O41 S4 C44 105.4(4) . . ? O42 S4 C44 103.4(5) . . ? O46 S4 C44 102.6(5) . . ? C16 C4 C42 115.0(5) . . ? C16 C4 H4A 108.5 . . ? C42 C4 H4A 108.5 . . ? C16 C4 H4B 108.5 . . ? C42 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? C131 P11 C111 108.6(4) . . ? C131 P11 C121 108.2(4) . . ? C111 P11 C121 110.6(3) . . ? C131 P11 C101 110.5(4) . . ? C111 P11 C101 109.5(4) . . ? C121 P11 C101 109.4(3) . . ? C141 P12 C161 106.0(3) . . ? C141 P12 C151 107.5(4) . . ? C161 P12 C151 112.0(3) . . ? C141 P12 C102 110.3(3) . . ? C161 P12 C102 111.0(4) . . ? C151 P12 C102 110.0(3) . . ? C171 C101 P11 113.7(5) . . ? C171 C101 H10A 108.8 . . ? P11 C101 H10A 108.8 . . ? C171 C101 H10B 108.8 . . ? P11 C101 H10B 108.8 . . ? H10A C101 H10B 107.7 . . ? C174 C102 P12 115.0(5) . . ? C174 C102 H10C 108.5 . . ? P12 C102 H10C 108.5 . . ? C174 C102 H10D 108.5 . . ? P12 C102 H10D 108.5 . . ? H10C C102 H10D 107.5 . . ? C116 C111 C112 119.4(7) . . ? C116 C111 P11 121.2(6) . . ? C112 C111 P11 119.3(6) . . ? C113 C112 C111 119.5(7) . . ? C113 C112 H112 120.2 . . ? C111 C112 H112 120.2 . . ? C112 C113 C114 120.0(8) . . ? C112 C113 H113 120.0 . . ? C114 C113 H113 120.0 . . ? C115 C114 C113 119.7(8) . . ? C115 C114 H114 120.1 . . ? C113 C114 H114 120.1 . . ? C116 C115 C114 121.8(7) . . ? C116 C115 H115 119.1 . . ? C114 C115 H115 119.1 . . ? C115 C116 C111 119.3(7) . . ? C115 C116 H116 120.3 . . ? C111 C116 H116 120.3 . . ? C126 C121 C122 119.3(7) . . ? C126 C121 P11 121.1(6) . . ? C122 C121 P11 119.4(6) . . ? C121 C122 C123 117.8(8) . . ? C121 C122 H122 121.1 . . ? C123 C122 H122 121.1 . . ? C124 C123 C122 120.1(9) . . ? C124 C123 H123 120.0 . . ? C122 C123 H123 120.0 . . ? C123 C124 C125 122.6(8) . . ? C123 C124 H124 118.7 . . ? C125 C124 H124 118.7 . . ? C124 C125 C126 119.2(9) . . ? C124 C125 H125 120.4 . . ? C126 C125 H125 120.4 . . ? C121 C126 C125 121.0(9) . . ? C121 C126 H126 119.5 . . ? C125 C126 H126 119.5 . . ? C132 C131 C136 120.2(7) . . ? C132 C131 P11 120.4(6) . . ? C136 C131 P11 119.3(6) . . ? C131 C132 C133 119.4(8) . . ? C131 C132 H132 120.3 . . ? C133 C132 H132 120.3 . . ? C134 C133 C132 119.7(8) . . ? C134 C133 H133 120.2 . . ? C132 C133 H133 120.2 . . ? C135 C134 C133 120.1(8) . . ? C135 C134 H134 119.9 . . ? C133 C134 H134 119.9 . . ? C134 C135 C136 121.4(10) . . ? C134 C135 H135 119.3 . . ? C136 C135 H135 119.3 . . ? C135 C136 C131 119.0(9) . . ? C135 C136 H136 120.5 . . ? C131 C136 H136 120.5 . . ? C146 C141 C142 117.9(7) . . ? C146 C141 P12 119.8(6) . . ? C142 C141 P12 122.3(5) . . ? C143 C142 C141 120.1(7) . . ? C143 C142 H142 120.0 . . ? C141 C142 H142 120.0 . . ? C142 C143 C144 121.3(8) . . ? C142 C143 H143 119.3 . . ? C144 C143 H143 119.3 . . ? C145 C144 C143 118.7(8) . . ? C145 C144 H144 120.7 . . ? C143 C144 H144 120.7 . . ? C146 C145 C144 120.7(7) . . ? C146 C145 H145 119.6 . . ? C144 C145 H145 119.6 . . ? C145 C146 C141 121.3(8) . . ? C145 C146 H146 119.4 . . ? C141 C146 H146 119.4 . . ? C152 C151 C156 119.3(7) . . ? C152 C151 P12 121.0(6) . . ? C156 C151 P12 119.6(6) . . ? C151 C152 C153 121.3(9) . . ? C151 C152 H152 119.3 . . ? C153 C152 H152 119.3 . . ? C154 C153 C152 119.2(9) . . ? C154 C153 H153 120.4 . . ? C152 C153 H153 120.4 . . ? C153 C154 C155 122.5(7) . . ? C153 C154 H154 118.8 . . ? C155 C154 H154 118.8 . . ? C154 C155 C156 118.6(8) . . ? C154 C155 H155 120.7 . . ? C156 C155 H155 120.7 . . ? C151 C156 C155 119.1(9) . . ? C151 C156 H156 120.4 . . ? C155 C156 H156 120.4 . . ? C162 C161 C166 119.9(6) . . ? C162 C161 P12 118.1(5) . . ? C166 C161 P12 121.4(5) . . ? C161 C162 C163 119.3(7) . . ? C161 C162 H162 120.3 . . ? C163 C162 H162 120.3 . . ? C164 C163 C162 120.6(6) . . ? C164 C163 H163 119.7 . . ? C162 C163 H163 119.7 . . ? C163 C164 C165 120.7(7) . . ? C163 C164 H164 119.6 . . ? C165 C164 H164 119.6 . . ? C164 C165 C166 120.3(7) . . ? C164 C165 H165 119.8 . . ? C166 C165 H165 119.8 . . ? C165 C166 C161 119.1(6) . . ? C165 C166 H166 120.5 . . ? C161 C166 H166 120.5 . . ? C172 C171 C176 117.4(7) . . ? C172 C171 C101 121.4(7) . . ? C176 C171 C101 121.2(6) . . ? C173 C172 C171 120.5(7) . . ? C173 C172 H172 119.8 . . ? C171 C172 H172 119.8 . . ? C172 C173 C174 123.3(6) . . ? C172 C173 H173 118.3 . . ? C174 C173 H173 118.3 . . ? C173 C174 C175 115.1(7) . . ? C173 C174 C102 121.8(6) . . ? C175 C174 C102 123.1(6) . . ? C176 C175 C174 123.6(7) . . ? C176 C175 H175 118.2 . . ? C174 C175 H175 118.2 . . ? C175 C176 C171 120.1(6) . . ? C175 C176 H176 120.0 . . ? C171 C176 H176 120.0 . . ? C231 P21 C221 111.4(4) . . ? C231 P21 C211 109.3(4) . . ? C221 P21 C211 108.4(3) . . ? C231 P21 C201 111.4(4) . . ? C221 P21 C201 107.5(4) . . ? C211 P21 C201 108.7(4) . . ? C251 P22 C241 109.9(4) . . ? C251 P22 C261 110.9(4) . . ? C241 P22 C261 111.2(3) . . ? C251 P22 C202 105.9(4) . . ? C241 P22 C202 109.6(4) . . ? C261 P22 C202 109.2(4) . . ? C271 C201 P21 112.6(6) . . ? C271 C201 H20A 109.1 . . ? P21 C201 H20A 109.1 . . ? C271 C201 H20B 109.1 . . ? P21 C201 H20B 109.1 . . ? H20A C201 H20B 107.8 . . ? C274 C202 P22 110.0(6) . . ? C274 C202 H20C 109.7 . . ? P22 C202 H20C 109.7 . . ? C274 C202 H20D 109.7 . . ? P22 C202 H20D 109.7 . . ? H20C C202 H20D 108.2 . . ? C212 C211 C216 120.2(8) . . ? C212 C211 P21 122.2(7) . . ? C216 C211 P21 117.5(7) . . ? C211 C212 C213 121.6(9) . . ? C211 C212 H212 119.2 . . ? C213 C212 H212 119.2 . . ? C214 C213 C212 118.4(10) . . ? C214 C213 H213 120.8 . . ? C212 C213 H213 120.8 . . ? C213 C214 C215 122.1(8) . . ? C213 C214 H214 119.0 . . ? C215 C214 H214 119.0 . . ? C214 C215 C216 118.3(9) . . ? C214 C215 H215 120.9 . . ? C216 C215 H215 120.9 . . ? C211 C216 C215 119.3(9) . . ? C211 C216 H216 120.4 . . ? C215 C216 H216 120.4 . . ? C222 C221 C226 120.8(7) . . ? C222 C221 P21 117.7(6) . . ? C226 C221 P21 121.4(6) . . ? C221 C222 C223 117.7(8) . . ? C221 C222 H222 121.2 . . ? C223 C222 H222 121.2 . . ? C224 C223 C222 121.6(8) . . ? C224 C223 H223 119.2 . . ? C222 C223 H223 119.2 . . ? C223 C224 C225 120.7(8) . . ? C223 C224 H224 119.6 . . ? C225 C224 H224 119.6 . . ? C224 C225 C226 120.8(9) . . ? C224 C225 H225 119.6 . . ? C226 C225 H225 119.6 . . ? C225 C226 C221 118.4(8) . . ? C225 C226 H226 120.8 . . ? C221 C226 H226 120.8 . . ? C236 C231 C232 118.6(8) . . ? C236 C231 P21 122.9(6) . . ? C232 C231 P21 118.5(7) . . ? C233 C232 C231 119.0(8) . . ? C233 C232 H232 120.5 . . ? C231 C232 H232 120.5 . . ? C232 C233 C234 122.5(8) . . ? C232 C233 H233 118.8 . . ? C234 C233 H233 118.8 . . ? C233 C234 C235 119.0(9) . . ? C233 C234 H234 120.5 . . ? C235 C234 H234 120.5 . . ? C236 C235 C234 119.6(8) . . ? C236 C235 H235 120.2 . . ? C234 C235 H235 120.2 . . ? C235 C236 C231 121.3(8) . . ? C235 C236 H236 119.3 . . ? C231 C236 H236 119.3 . . ? C246 C241 C242 119.2(8) . . ? C246 C241 P22 119.8(6) . . ? C242 C241 P22 120.9(7) . . ? C243 C242 C241 118.5(10) . . ? C243 C242 H242 120.8 . . ? C241 C242 H242 120.8 . . ? C244 C243 C242 121.8(9) . . ? C244 C243 H243 119.1 . . ? C242 C243 H243 119.1 . . ? C243 C244 C245 119.9(9) . . ? C243 C244 H244 120.0 . . ? C245 C244 H244 120.0 . . ? C244 C245 C246 120.1(10) . . ? C244 C245 H245 119.9 . . ? C246 C245 H245 119.9 . . ? C241 C246 C245 120.3(9) . . ? C241 C246 H246 119.9 . . ? C245 C246 H246 119.9 . . ? C256 C251 C252 120.1(8) . . ? C256 C251 P22 120.7(7) . . ? C252 C251 P22 118.4(6) . . ? C253 C252 C251 119.1(8) . . ? C253 C252 H252 120.4 . . ? C251 C252 H252 120.4 . . ? C252 C253 C254 121.6(8) . . ? C252 C253 H253 119.2 . . ? C254 C253 H253 119.2 . . ? C253 C254 C255 118.9(8) . . ? C253 C254 H254 120.6 . . ? C255 C254 H254 120.6 . . ? C256 C255 C254 120.0(8) . . ? C256 C255 H255 120.0 . . ? C254 C255 H255 120.0 . . ? C251 C256 C255 120.2(9) . . ? C251 C256 H256 119.9 . . ? C255 C256 H256 119.9 . . ? C266 C261 C262 121.2(8) . . ? C266 C261 P22 118.3(8) . . ? C262 C261 P22 120.5(7) . . ? C261 C262 C263 121.1(10) . . ? C261 C262 H262 119.5 . . ? C263 C262 H262 119.5 . . ? C264 C263 C262 117.0(10) . . ? C264 C263 H263 121.5 . . ? C262 C263 H263 121.5 . . ? C265 C264 C263 124.9(9) . . ? C265 C264 H264 117.6 . . ? C263 C264 H264 117.6 . . ? C264 C265 C266 117.8(10) . . ? C264 C265 H265 121.1 . . ? C266 C265 H265 121.1 . . ? C261 C266 C265 117.9(10) . . ? C261 C266 H266 121.0 . . ? C265 C266 H266 121.0 . . ? C276 C271 C272 117.8(7) . . ? C276 C271 C201 122.1(7) . . ? C272 C271 C201 120.0(7) . . ? C273 C272 C271 120.5(8) . . ? C273 C272 H272 119.8 . . ? C271 C272 H272 119.8 . . ? C274 C273 C272 120.9(8) . . ? C274 C273 H273 119.6 . . ? C272 C273 H273 119.6 . . ? C273 C274 C275 119.6(7) . . ? C273 C274 C202 122.6(8) . . ? C275 C274 C202 117.7(8) . . ? C276 C275 C274 119.8(8) . . ? C276 C275 H275 120.1 . . ? C274 C275 H275 120.1 . . ? C275 C276 C271 121.3(8) . . ? C275 C276 H276 119.4 . . ? C271 C276 H276 119.4 . . ? C007 N1 C005 108.0(7) . . ? C007 N1 C004 125.4(7) . . ? C005 N1 C004 126.0(7) . . ? C007 N2 C006 106.3(8) . . ? C007 N2 C008 126.2(8) . . ? C006 N2 C008 126.8(8) . . ? C002 C001 H00I 109.5 . . ? C002 C001 H00J 109.5 . . ? H00I C001 H00J 109.5 . . ? C002 C001 H00K 109.5 . . ? H00I C001 H00K 109.5 . . ? H00J C001 H00K 109.5 . . ? C003 C002 C001 113.9(8) . . ? C003 C002 H00A 108.8 . . ? C001 C002 H00A 108.8 . . ? C003 C002 H00B 108.8 . . ? C001 C002 H00B 108.8 . . ? H00A C002 H00B 107.7 . . ? C004 C003 C002 116.1(7) . . ? C004 C003 H00C 108.3 . . ? C002 C003 H00C 108.3 . . ? C004 C003 H00D 108.3 . . ? C002 C003 H00D 108.3 . . ? H00C C003 H00D 107.4 . . ? N1 C004 C003 112.8(7) . . ? N1 C004 H00E 109.0 . . ? C003 C004 H00E 109.0 . . ? N1 C004 H00F 109.0 . . ? C003 C004 H00F 109.0 . . ? H00E C004 H00F 107.8 . . ? C006 C005 N1 107.4(8) . . ? C006 C005 H005 126.3 . . ? N1 C005 H005 126.3 . . ? C005 C006 N2 107.2(8) . . ? C005 C006 H006 126.4 . . ? N2 C006 H006 126.4 . . ? N1 C007 N2 111.0(7) . . ? N1 C007 H007 124.5 . . ? N2 C007 H007 124.5 . . ? N2 C008 C009 111.0(8) . . ? N2 C008 H00G 109.4 . . ? C009 C008 H00G 109.4 . . ? N2 C008 H00H 109.4 . . ? C009 C008 H00H 109.4 . . ? H00G C008 H00H 108.0 . . ? C010 C009 C011 117.5(10) . . ? C010 C009 C008 122.1(10) . . ? C011 C009 C008 120.3(8) . . ? C011 C010 C009 121.4(11) 3_666 . ? C011 C010 H010 119.3 3_666 . ? C009 C010 H010 119.3 . . ? C010 C011 C009 121.1(9) 3_666 . ? C010 C011 H011 119.4 3_666 . ? C009 C011 H011 119.4 . . ? H01X O01W H01Y 108.4 . . ? H02X O02W H02Y 108.4 . . ? H03X O03W H03Y 108.4 . . ? H04X O04W H04Y 108.4 . . ? H05X O05W H05Y 108.4 . . ? H06X O06W H06Y 108.4 . . ? H07X O07W H07Y 108.4 . . ? H08X O08W H08Y 108.4 . . ? H09X O09W H09Y 108.4 . . ? H10X O10W H10Y 108.4 . . ? H11X O11W H11Y 108.4 . . ? H12X O12W H12Y 108.4 . . ? H13X O13W H13Y 108.3 . . ? H14X O14W H14Y 108.4 . . ? H15X O15W H15Y 108.4 . . ? H16X O16W H16Y 108.4 . . ? 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 O1 C11 C12 C13 175.3(6) . . . . ? C16 C11 C12 C13 -2.6(10) . . . . ? O1 C11 C12 C1 -8.9(9) . . . . ? C16 C11 C12 C1 173.2(6) . . . . ? C11 C12 C13 C14 -0.1(10) . . . . ? C1 C12 C13 C14 -175.9(6) . . . . ? C12 C13 C14 C15 1.9(10) . . . . ? C12 C13 C14 S1 179.0(5) . . . . ? C13 C14 C15 C16 -1.1(10) . . . . ? S1 C14 C15 C16 -178.1(5) . . . . ? C14 C15 C16 C11 -1.5(9) . . . . ? C14 C15 C16 C4 -178.9(6) . . . . ? O1 C11 C16 C15 -174.6(6) . . . . ? C12 C11 C16 C15 3.3(9) . . . . ? O1 C11 C16 C4 2.9(9) . . . . ? C12 C11 C16 C4 -179.2(6) . . . . ? C15 C14 S1 O14 -33.5(10) . . . . ? C13 C14 S1 O14 149.4(10) . . . . ? C15 C14 S1 O15 87.1(9) . . . . ? C13 C14 S1 O15 -90.0(9) . . . . ? C15 C14 S1 O16 -153.9(9) . . . . ? C13 C14 S1 O16 29.1(10) . . . . ? C15 C14 S1 O13 -118.9(6) . . . . ? C13 C14 S1 O13 64.0(6) . . . . ? C15 C14 S1 O12 120.1(6) . . . . ? C13 C14 S1 O12 -56.9(6) . . . . ? C15 C14 S1 O11 0.0(7) . . . . ? C13 C14 S1 O11 -177.1(6) . . . . ? C11 C12 C1 C26 -97.5(8) . . . . ? C13 C12 C1 C26 78.3(9) . . . . ? O2 C21 C22 C23 177.3(6) . . . . ? C26 C21 C22 C23 -2.1(10) . . . . ? O2 C21 C22 C2 -3.2(10) . . . . ? C26 C21 C22 C2 177.4(6) . . . . ? C21 C22 C23 C24 -1.3(10) . . . . ? C2 C22 C23 C24 179.2(6) . . . . ? C22 C23 C24 C25 3.4(10) . . . . ? C22 C23 C24 S2 -177.1(5) . . . . ? C23 C24 C25 C26 -2.2(10) . . . . ? S2 C24 C25 C26 178.3(5) . . . . ? O2 C21 C26 C25 -176.1(6) . . . . ? C22 C21 C26 C25 3.3(10) . . . . ? O2 C21 C26 C1 8.3(10) . . . . ? C22 C21 C26 C1 -172.3(6) . . . . ? C24 C25 C26 C21 -1.2(10) . . . . ? C24 C25 C26 C1 174.6(6) . . . . ? C12 C1 C26 C21 89.7(8) . . . . ? C12 C1 C26 C25 -86.0(8) . . . . ? C23 C24 S2 O22 115.9(6) . . . . ? C25 C24 S2 O22 -64.6(6) . . . . ? C23 C24 S2 O21 -4.6(7) . . . . ? C25 C24 S2 O21 174.9(6) . . . . ? C23 C24 S2 O23 -123.7(7) . . . . ? C25 C24 S2 O23 55.8(7) . . . . ? C23 C22 C2 C36 91.2(8) . . . . ? C21 C22 C2 C36 -88.3(8) . . . . ? O3 C31 C32 C33 178.6(6) . . . . ? C36 C31 C32 C33 -1.6(11) . . . . ? O3 C31 C32 C3 0.1(10) . . . . ? C36 C31 C32 C3 179.9(7) . . . . ? C31 C32 C33 C34 2.0(11) . . . . ? C3 C32 C33 C34 -179.5(7) . . . . ? C32 C33 C34 C35 -3.0(11) . . . . ? C32 C33 C34 S3 -174.9(6) . . . . ? C33 C34 C35 C36 3.8(11) . . . . ? S3 C34 C35 C36 175.6(6) . . . . ? C34 C35 C36 C31 -3.3(11) . . . . ? C34 C35 C36 C2 179.9(7) . . . . ? O3 C31 C36 C35 -178.0(6) . . . . ? C32 C31 C36 C35 2.2(10) . . . . ? O3 C31 C36 C2 -1.3(10) . . . . ? C32 C31 C36 C2 178.9(7) . . . . ? C22 C2 C36 C35 -97.3(8) . . . . ? C22 C2 C36 C31 86.1(9) . . . . ? C35 C34 S3 O32 -66.7(7) . . . . ? C33 C34 S3 O32 105.1(6) . . . . ? C35 C34 S3 O33 50.8(7) . . . . ? C33 C34 S3 O33 -137.4(6) . . . . ? C35 C34 S3 O31 172.0(6) . . . . ? C33 C34 S3 O31 -16.2(7) . . . . ? C33 C32 C3 C46 93.5(8) . . . . ? C31 C32 C3 C46 -88.0(8) . . . . ? O4 C41 C42 C43 176.0(7) . . . . ? C46 C41 C42 C43 -2.9(11) . . . . ? O4 C41 C42 C4 -4.0(11) . . . . ? C46 C41 C42 C4 177.1(7) . . . . ? C41 C42 C43 C44 0.6(11) . . . . ? C4 C42 C43 C44 -179.5(7) . . . . ? C42 C43 C44 C45 2.1(11) . . . . ? C42 C43 C44 S4 -174.9(6) . . . . ? C43 C44 C45 C46 -2.5(11) . . . . ? S4 C44 C45 C46 174.4(6) . . . . ? C44 C45 C46 C41 0.2(11) . . . . ? C44 C45 C46 C3 179.7(7) . . . . ? O4 C41 C46 C45 -176.4(7) . . . . ? C42 C41 C46 C45 2.5(11) . . . . ? O4 C41 C46 C3 4.1(11) . . . . ? C42 C41 C46 C3 -177.0(7) . . . . ? C32 C3 C46 C45 -99.4(8) . . . . ? C32 C3 C46 C41 80.0(9) . . . . ? C43 C44 S4 O43 55.5(8) . . . . ? C45 C44 S4 O43 -121.5(7) . . . . ? C43 C44 S4 O44 -163.4(7) . . . . ? C45 C44 S4 O44 19.6(8) . . . . ? C43 C44 S4 O45 -38.4(8) . . . . ? C45 C44 S4 O45 144.6(8) . . . . ? C43 C44 S4 O41 178.4(7) . . . . ? C45 C44 S4 O41 1.4(8) . . . . ? C43 C44 S4 O42 -65.5(7) . . . . ? C45 C44 S4 O42 117.5(7) . . . . ? C43 C44 S4 O46 77.8(7) . . . . ? C45 C44 S4 O46 -99.2(7) . . . . ? C15 C16 C4 C42 -87.3(8) . . . . ? C11 C16 C4 C42 95.3(8) . . . . ? C43 C42 C4 C16 104.6(8) . . . . ? C41 C42 C4 C16 -75.5(9) . . . . ? C131 P11 C101 C171 63.1(6) . . . . ? C111 P11 C101 C171 -177.3(5) . . . . ? C121 P11 C101 C171 -55.9(6) . . . . ? C141 P12 C102 C174 173.8(5) . . . . ? C161 P12 C102 C174 56.6(6) . . . . ? C151 P12 C102 C174 -67.9(6) . . . . ? C131 P11 C111 C116 -12.5(7) . . . . ? C121 P11 C111 C116 106.2(6) . . . . ? C101 P11 C111 C116 -133.2(6) . . . . ? C131 P11 C111 C112 169.7(6) . . . . ? C121 P11 C111 C112 -71.6(6) . . . . ? C101 P11 C111 C112 49.0(6) . . . . ? C116 C111 C112 C113 -3.9(10) . . . . ? P11 C111 C112 C113 174.0(6) . . . . ? C111 C112 C113 C114 2.4(11) . . . . ? C112 C113 C114 C115 1.2(11) . . . . ? C113 C114 C115 C116 -3.6(11) . . . . ? C114 C115 C116 C111 2.1(10) . . . . ? C112 C111 C116 C115 1.6(10) . . . . ? P11 C111 C116 C115 -176.2(5) . . . . ? C131 P11 C121 C126 -43.3(7) . . . . ? C111 P11 C121 C126 -162.2(6) . . . . ? C101 P11 C121 C126 77.1(7) . . . . ? C131 P11 C121 C122 142.0(6) . . . . ? C111 P11 C121 C122 23.1(7) . . . . ? C101 P11 C121 C122 -97.6(6) . . . . ? C126 C121 C122 C123 0.2(11) . . . . ? P11 C121 C122 C123 174.9(6) . . . . ? C121 C122 C123 C124 1.3(12) . . . . ? C122 C123 C124 C125 -2.8(14) . . . . ? C123 C124 C125 C126 2.8(15) . . . . ? C122 C121 C126 C125 -0.2(12) . . . . ? P11 C121 C126 C125 -174.9(7) . . . . ? C124 C125 C126 C121 -1.2(14) . . . . ? C111 P11 C131 C132 -83.7(8) . . . . ? C121 P11 C131 C132 156.2(7) . . . . ? C101 P11 C131 C132 36.5(8) . . . . ? C111 P11 C131 C136 93.0(8) . . . . ? C121 P11 C131 C136 -27.1(8) . . . . ? C101 P11 C131 C136 -146.8(7) . . . . ? C136 C131 C132 C133 0.9(13) . . . . ? P11 C131 C132 C133 177.6(7) . . . . ? C131 C132 C133 C134 1.5(14) . . . . ? C132 C133 C134 C135 -4.0(16) . . . . ? C133 C134 C135 C136 4.2(17) . . . . ? C134 C135 C136 C131 -1.8(16) . . . . ? C132 C131 C136 C135 -0.8(14) . . . . ? P11 C131 C136 C135 -177.5(8) . . . . ? C161 P12 C141 C146 -40.3(6) . . . . ? C151 P12 C141 C146 79.6(6) . . . . ? C102 P12 C141 C146 -160.6(5) . . . . ? C161 P12 C141 C142 141.1(6) . . . . ? C151 P12 C141 C142 -99.0(6) . . . . ? C102 P12 C141 C142 20.9(6) . . . . ? C146 C141 C142 C143 0.2(10) . . . . ? P12 C141 C142 C143 178.8(6) . . . . ? C141 C142 C143 C144 1.2(11) . . . . ? C142 C143 C144 C145 -3.2(11) . . . . ? C143 C144 C145 C146 3.8(11) . . . . ? C144 C145 C146 C141 -2.5(11) . . . . ? C142 C141 C146 C145 0.4(10) . . . . ? P12 C141 C146 C145 -178.2(5) . . . . ? C141 P12 C151 C152 6.6(7) . . . . ? C161 P12 C151 C152 122.6(6) . . . . ? C102 P12 C151 C152 -113.5(6) . . . . ? C141 P12 C151 C156 -178.0(5) . . . . ? C161 P12 C151 C156 -62.0(6) . . . . ? C102 P12 C151 C156 61.9(7) . . . . ? C156 C151 C152 C153 -0.3(11) . . . . ? P12 C151 C152 C153 175.1(6) . . . . ? C151 C152 C153 C154 -0.4(11) . . . . ? C152 C153 C154 C155 -0.3(12) . . . . ? C153 C154 C155 C156 1.7(12) . . . . ? C152 C151 C156 C155 1.8(10) . . . . ? P12 C151 C156 C155 -173.7(5) . . . . ? C154 C155 C156 C151 -2.5(11) . . . . ? C141 P12 C161 C162 -66.8(7) . . . . ? C151 P12 C161 C162 176.3(6) . . . . ? C102 P12 C161 C162 53.0(7) . . . . ? C141 P12 C161 C166 104.4(7) . . . . ? C151 P12 C161 C166 -12.5(8) . . . . ? C102 P12 C161 C166 -135.7(6) . . . . ? C166 C161 C162 C163 0.5(12) . . . . ? P12 C161 C162 C163 171.9(6) . . . . ? C161 C162 C163 C164 -0.9(12) . . . . ? C162 C163 C164 C165 0.8(13) . . . . ? C163 C164 C165 C166 -0.4(12) . . . . ? C164 C165 C166 C161 0.0(12) . . . . ? C162 C161 C166 C165 -0.1(12) . . . . ? P12 C161 C166 C165 -171.2(6) . . . . ? P11 C101 C171 C172 83.3(7) . . . . ? P11 C101 C171 C176 -95.6(7) . . . . ? C176 C171 C172 C173 1.3(10) . . . . ? C101 C171 C172 C173 -177.6(6) . . . . ? C171 C172 C173 C174 1.0(11) . . . . ? C172 C173 C174 C175 -3.0(10) . . . . ? C172 C173 C174 C102 179.5(6) . . . . ? P12 C102 C174 C173 -86.0(7) . . . . ? P12 C102 C174 C175 96.8(7) . . . . ? C173 C174 C175 C176 2.8(10) . . . . ? C102 C174 C175 C176 -179.8(7) . . . . ? C174 C175 C176 C171 -0.6(11) . . . . ? C172 C171 C176 C175 -1.5(10) . . . . ? C101 C171 C176 C175 177.4(6) . . . . ? C231 P21 C201 C271 71.2(6) . . . . ? C221 P21 C201 C271 -51.1(7) . . . . ? C211 P21 C201 C271 -168.3(6) . . . . ? C251 P22 C202 C274 -47.0(7) . . . . ? C241 P22 C202 C274 -165.4(6) . . . . ? C261 P22 C202 C274 72.5(7) . . . . ? C231 P21 C211 C212 134.1(7) . . . . ? C221 P21 C211 C212 -104.3(8) . . . . ? C201 P21 C211 C212 12.3(8) . . . . ? C231 P21 C211 C216 -48.9(7) . . . . ? C221 P21 C211 C216 72.7(7) . . . . ? C201 P21 C211 C216 -170.7(6) . . . . ? C216 C211 C212 C213 3.3(14) . . . . ? P21 C211 C212 C213 -179.8(8) . . . . ? C211 C212 C213 C214 -4.8(15) . . . . ? C212 C213 C214 C215 3.4(15) . . . . ? C213 C214 C215 C216 -0.6(13) . . . . ? C212 C211 C216 C215 -0.4(12) . . . . ? P21 C211 C216 C215 -177.5(6) . . . . ? C214 C215 C216 C211 -0.9(12) . . . . ? C231 P21 C221 C222 158.1(6) . . . . ? C211 P21 C221 C222 37.7(7) . . . . ? C201 P21 C221 C222 -79.7(7) . . . . ? C231 P21 C221 C226 -26.7(8) . . . . ? C211 P21 C221 C226 -147.1(7) . . . . ? C201 P21 C221 C226 95.5(8) . . . . ? C226 C221 C222 C223 1.8(12) . . . . ? P21 C221 C222 C223 177.0(6) . . . . ? C221 C222 C223 C224 -1.8(12) . . . . ? C222 C223 C224 C225 1.7(14) . . . . ? C223 C224 C225 C226 -1.6(16) . . . . ? C224 C225 C226 C221 1.6(15) . . . . ? C222 C221 C226 C225 -1.8(13) . . . . ? P21 C221 C226 C225 -176.8(7) . . . . ? C221 P21 C231 C236 -29.8(7) . . . . ? C211 P21 C231 C236 90.0(7) . . . . ? C201 P21 C231 C236 -149.8(6) . . . . ? C221 P21 C231 C232 151.4(5) . . . . ? C211 P21 C231 C232 -88.7(6) . . . . ? C201 P21 C231 C232 31.4(7) . . . . ? C236 C231 C232 C233 -0.3(10) . . . . ? P21 C231 C232 C233 178.5(5) . . . . ? C231 C232 C233 C234 0.6(11) . . . . ? C232 C233 C234 C235 -0.7(12) . . . . ? C233 C234 C235 C236 0.4(12) . . . . ? C234 C235 C236 C231 -0.2(12) . . . . ? C232 C231 C236 C235 0.2(11) . . . . ? P21 C231 C236 C235 -178.6(6) . . . . ? C251 P22 C241 C246 91.8(9) . . . . ? C261 P22 C241 C246 -31.4(10) . . . . ? C202 P22 C241 C246 -152.3(9) . . . . ? C251 P22 C241 C242 -84.7(9) . . . . ? C261 P22 C241 C242 152.1(8) . . . . ? C202 P22 C241 C242 31.2(9) . . . . ? C246 C241 C242 C243 -1.8(15) . . . . ? P22 C241 C242 C243 174.7(8) . . . . ? C241 C242 C243 C244 -0.9(16) . . . . ? C242 C243 C244 C245 3.2(18) . . . . ? C243 C244 C245 C246 -2.9(19) . . . . ? C242 C241 C246 C245 2.1(17) . . . . ? P22 C241 C246 C245 -174.5(9) . . . . ? C244 C245 C246 C241 0.2(19) . . . . ? C241 P22 C251 C256 -159.7(8) . . . . ? C261 P22 C251 C256 -36.3(9) . . . . ? C202 P22 C251 C256 82.0(9) . . . . ? C241 P22 C251 C252 30.4(8) . . . . ? C261 P22 C251 C252 153.8(7) . . . . ? C202 P22 C251 C252 -87.9(8) . . . . ? C256 C251 C252 C253 -2.6(14) . . . . ? P22 C251 C252 C253 167.4(7) . . . . ? C251 C252 C253 C254 -0.8(14) . . . . ? C252 C253 C254 C255 3.8(14) . . . . ? C253 C254 C255 C256 -3.5(14) . . . . ? C252 C251 C256 C255 2.9(16) . . . . ? P22 C251 C256 C255 -166.8(8) . . . . ? C254 C255 C256 C251 0.2(16) . . . . ? C251 P22 C261 C266 -35.7(8) . . . . ? C241 P22 C261 C266 86.9(7) . . . . ? C202 P22 C261 C266 -152.0(7) . . . . ? C251 P22 C261 C262 145.4(6) . . . . ? C241 P22 C261 C262 -92.0(7) . . . . ? C202 P22 C261 C262 29.0(7) . . . . ? C266 C261 C262 C263 1.8(12) . . . . ? P22 C261 C262 C263 -179.3(6) . . . . ? C261 C262 C263 C264 -1.1(11) . . . . ? C262 C263 C264 C265 -1.0(13) . . . . ? C263 C264 C265 C266 2.3(14) . . . . ? C262 C261 C266 C265 -0.4(13) . . . . ? P22 C261 C266 C265 -179.3(7) . . . . ? C264 C265 C266 C261 -1.5(13) . . . . ? P21 C201 C271 C276 -99.9(8) . . . . ? P21 C201 C271 C272 83.4(9) . . . . ? C276 C271 C272 C273 0.8(13) . . . . ? C201 C271 C272 C273 177.6(8) . . . . ? C271 C272 C273 C274 1.6(14) . . . . ? C272 C273 C274 C275 -4.4(14) . . . . ? C272 C273 C274 C202 177.2(9) . . . . ? P22 C202 C274 C273 -87.1(10) . . . . ? P22 C202 C274 C275 94.5(9) . . . . ? C273 C274 C275 C276 4.8(14) . . . . ? C202 C274 C275 C276 -176.7(8) . . . . ? C274 C275 C276 C271 -2.5(14) . . . . ? C272 C271 C276 C275 -0.3(12) . . . . ? C201 C271 C276 C275 -177.0(8) . . . . ? C001 C002 C003 C004 -59.2(12) . . . . ? C007 N1 C004 C003 -49.7(11) . . . . ? C005 N1 C004 C003 120.1(9) . . . . ? C002 C003 C004 N1 -50.4(12) . . . . ? C007 N1 C005 C006 0.2(10) . . . . ? C004 N1 C005 C006 -171.0(8) . . . . ? N1 C005 C006 N2 0.8(10) . . . . ? C007 N2 C006 C005 -1.5(10) . . . . ? C008 N2 C006 C005 169.0(9) . . . . ? C005 N1 C007 N2 -1.2(9) . . . . ? C004 N1 C007 N2 170.1(7) . . . . ? C006 N2 C007 N1 1.7(10) . . . . ? C008 N2 C007 N1 -168.9(8) . . . . ? C007 N2 C008 C009 81.7(11) . . . . ? C006 N2 C008 C009 -87.0(12) . . . . ? N2 C008 C009 C010 100.0(11) . . . . ? N2 C008 C009 C011 -78.3(12) . . . . ? C011 C009 C010 C011 -0.6(16) . . . 3_666 ? C008 C009 C010 C011 -179.0(9) . . . 3_666 ? C010 C009 C011 C010 0.6(16) . . . 3_666 ? C008 C009 C011 C010 179.0(9) . . . 3_666 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O4 0.85 1.82 2.665(8) 169.9 . O2 H2 O3 0.85 1.74 2.561(8) 161.6 . O3 H3 O2 0.85 1.73 2.561(8) 166.5 . O4 H4 O3 0.85 1.64 2.477(6) 167.8 . O01W H01X O11 0.85 1.91 2.747(13) 166.1 . O01W H01X O15 0.85 2.85 3.50(2) 134.6 . O01W H01Y O12W 0.85 1.81 2.649(18) 167.2 3_666 O02W H02X O16 0.85 2.25 3.03(2) 152.4 . O02W H02X O12 0.85 2.16 2.962(13) 156.7 . O02W H02Y O23 0.85 2.13 2.977(14) 176.8 . O03W H03X O21 0.85 2.04 2.884(13) 176.2 . O03W H03Y O14W 0.85 1.91 2.756(16) 176.1 . O04W H04X O22 0.85 1.98 2.821(9) 171.1 . O04W H04Y O15W 0.85 1.90 2.740(10) 171.3 . O05W H05X O23 0.85 2.20 3.025(13) 162.2 . O05W H05Y O13W 0.85 2.07 2.892(19) 162.3 . O06W H06X O33 0.85 1.97 2.806(8) 169.7 . O06W H06Y O43 0.85 1.84 2.660(9) 162.7 1_655 O06W H06Y O46 0.85 2.14 2.988(12) 174.3 1_655 O07W H07X O45 0.85 1.76 2.601(12) 168.5 . O07W H07X O42 0.85 2.00 2.843(12) 172.4 . O07W H07Y O01W 0.85 1.88 2.728(16) 179.0 . O08W H08X O22 0.85 2.24 3.086(11) 170.2 . O08W H08Y O05W 0.85 1.89 2.730(14) 169.6 . O09W H09X O2 0.85 2.02 2.873(8) 177.4 4_565 O09W H09Y O10W 0.85 1.88 2.733(10) 177.5 . O10W H10X O02W 0.85 1.87 2.720(14) 175.9 . O10W H10Y O04W 0.85 1.82 2.668(12) 175.2 . O11W H11X O09W 0.85 1.85 2.692(12) 169.7 . O11W H11Y O15W 0.85 1.96 2.800(11) 169.0 4_565 O12W H12X O13W 0.85 1.84 2.685(18) 173.7 . O12W H12Y O14W 0.85 1.77 2.621(16) 175.1 . O13W H13X O07W 0.85 2.06 2.869(17) 159.4 3_666 O13W H13Y O16W 0.85 2.02 2.828(16) 159.1 . O14W H14X O06W 0.85 1.83 2.673(12) 175.2 . O14W H14Y O07W 0.85 2.27 3.118(19) 175.6 1_655 O15W H15X O3 0.85 1.95 2.802(8) 178.1 4_565 O16W H16X O11 0.85 2.09 2.928(14) 169.9 1_655 O16W H16X O14 0.85 1.82 2.629(16) 159.7 1_655 O16W H16Y O03W 0.85 1.93 2.776(18) 170.2 . _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 67.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.298 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.150 # Attachment 'Complex_II.cif' data_080203k _database_code_depnum_ccdc_archive 'CCDC 752170' _publ_section_title_footnote ; ? #<< paper footnote text ; # 4. TEXT _publ_section_synopsis ; ? #<< synopsis if FI,CI,CM,CO papers ; _publ_section_abstract ; ? #<< abstract text ; _publ_section_comment ; ? #<< scientific commentary text ; _publ_section_exptl_prep ; ? #<< material & crystal preparation text ; _publ_section_acknowledgements ; ? #<< acknowledgements text ; _publ_section_references ; Barbour, L. J. (2001). J. Supramol. Chem., 1, 189-191. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; # 5. CHEMICAL DATA _publ_section_figure_captions ; ? #<< figure captions ; #============================================================================== # 6. CRYSTALLOGRAPHY _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H66 Gd2 O45 S8, C22 H32 N4, 0.5(H4 O2), 5(H2 O)' _chemical_formula_sum 'C78 H108 Gd2 N4 O50 S8' _chemical_formula_weight 2472.66 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -8.8380 11.9157 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P 41' _symmetry_space_group_name_Hall 'P 4w' _symmetry_int_tables_number 76 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+1/4' 'y, -x, z+3/4' _cell_length_a 14.1154(2) _cell_length_b 14.1154 _cell_length_c 47.0311(4) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 9370.69(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 54319 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 67.0 _exptl_crystal_description 'tetragonal dipyramid' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.753 _exptl_crystal_density_method ? _exptl_crystal_F_000 5040 _exptl_absorpt_coefficient_mu 11.642 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7192 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Oxford Diffraction Gemini-R Ultra, Ruby CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.4738 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 160747 _diffrn_reflns_av_R_equivalents 0.0724 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -55 _diffrn_reflns_limit_l_max 56 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 67.19 _reflns_number_total 16659 _reflns_number_gt 16339 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'X-Seed 2.0 (Barbour, 2001)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1740P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.002(4) _refine_ls_number_reflns 16659 _refine_ls_number_parameters 1271 _refine_ls_number_restraints 58 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0701 _refine_ls_wR_factor_ref 0.1841 _refine_ls_wR_factor_gt 0.1831 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd -0.02059(6) 0.34255(6) 0.037814(15) 0.02889(18) Uani 1 1 d . . . O01W O 0.1342(9) 0.3735(12) 0.0177(2) 0.060(4) Uani 1 1 d . . . H01X H 0.1461 0.3743 0.0000 0.090 Uiso 1 1 d . . . H01Y H 0.1851 0.3616 0.0266 0.090 Uiso 1 1 d . . . O02W O 0.1144(10) 0.2306(10) 0.0507(3) 0.056(3) Uani 1 1 d . . . H02X H 0.1527 0.2462 0.0638 0.084 Uiso 1 1 d . . . H02Y H 0.1261 0.1737 0.0460 0.084 Uiso 1 1 d . . . O03W O -0.0490(10) 0.1829(8) 0.0215(3) 0.051(3) Uani 1 1 d . . . H03X H 0.0031 0.1554 0.0178 0.076 Uiso 1 1 d . . . H03Y H -0.0786 0.1520 0.0342 0.076 Uiso 1 1 d . . . O04W O -0.1162(8) 0.4409(8) 0.0685(2) 0.042(3) Uani 1 1 d . . . H04X H -0.0809 0.4799 0.0773 0.062 Uiso 1 1 d . . . H04Y H -0.1448 0.4066 0.0806 0.062 Uiso 1 1 d . . . O05W O -0.1845(8) 0.3328(9) 0.0251(2) 0.042(2) Uani 1 1 d . . . H05X H -0.2018 0.3071 0.0096 0.063 Uiso 1 1 d . . . H05Y H -0.2306 0.3301 0.0367 0.063 Uiso 1 1 d . . . O06W O -0.0392(7) 0.5009(7) 0.0177(2) 0.033(2) Uani 1 1 d . . . H06X H -0.0616 0.5136 0.0014 0.050 Uiso 1 1 d . . . H06Y H -0.0460 0.5500 0.0280 0.050 Uiso 1 1 d . . . O07W O -0.0305(10) 0.3337(8) -0.0144(2) 0.050(3) Uani 1 1 d . . . H07X H -0.0099 0.3724 -0.0268 0.075 Uiso 1 1 d . . . H07Y H -0.0853 0.3158 -0.0196 0.075 Uiso 1 1 d . . . Gd2 Gd 0.80328(5) 0.37165(5) 0.156426(14) 0.02074(15) Uani 1 1 d . . . O08W O 0.9532(8) 0.3695(8) 0.1810(3) 0.046(3) Uani 1 1 d . . . H08X H 0.9438 0.3600 0.1986 0.069 Uiso 1 1 d . . . H08Y H 0.9872 0.3248 0.1745 0.069 Uiso 1 1 d . . . O09W O 0.7883(7) 0.5139(6) 0.18243(19) 0.0294(19) Uani 1 1 d . . . H09X H 0.8350 0.5294 0.1929 0.044 Uiso 1 1 d . . . H09Y H 0.7396 0.5415 0.1891 0.044 Uiso 1 1 d . . . O10W O 0.6364(6) 0.4022(6) 0.16590(18) 0.0248(17) Uani 1 1 d . . . H10X H 0.6101 0.3788 0.1512 0.037 Uiso 1 1 d . . . H10Y H 0.6273 0.4617 0.1655 0.037 Uiso 1 1 d . . . O11W O 0.7183(6) 0.2293(6) 0.14548(18) 0.0248(17) Uani 1 1 d . . . H11X H 0.7396 0.1897 0.1334 0.037 Uiso 1 1 d . . . H11Y H 0.6643 0.2099 0.1510 0.037 Uiso 1 1 d . . . O12W O 0.7810(7) 0.2971(7) 0.2008(2) 0.035(2) Uani 1 1 d . . . H12X H 0.8237 0.2698 0.2106 0.052 Uiso 1 1 d . . . H12Y H 0.7290 0.2686 0.2039 0.052 Uiso 1 1 d . . . O13W O 0.9134(7) 0.4834(7) 0.1345(2) 0.039(2) Uani 1 1 d . . . H13X H 0.9714 0.4700 0.1319 0.058 Uiso 1 1 d . . . H13Y H 0.8983 0.5260 0.1226 0.058 Uiso 1 1 d . . . O14W O 0.8849(6) 0.5444(7) -0.0378(2) 0.0310(19) Uani 1 1 d . . . H14X H 0.8434 0.5084 -0.0452 0.037 Uiso 1 1 d . . . H14Y H 0.9207 0.5104 -0.0275 0.037 Uiso 1 1 d . . . O15W O 0.3876(9) 0.3650(11) 0.1314(2) 0.056(3) Uani 1 1 d . . . H15X H 0.4399 0.3601 0.1225 0.084 Uiso 1 1 d . . . H15Y H 0.3431 0.3598 0.1193 0.084 Uiso 1 1 d . . . O16W O 0.7843(9) 0.2574(9) -0.0252(3) 0.053(3) Uani 1 1 d . . . H16X H 0.7369 0.2903 -0.0304 0.079 Uiso 1 1 d . . . H16Y H 0.7639 0.2039 -0.0197 0.079 Uiso 1 1 d . . . O17W O 1.0172(14) 0.4001(10) 0.2306(4) 0.078(5) Uani 1 1 d . . . H17X H 1.0727 0.3871 0.2364 0.117 Uiso 1 1 d . . . H17Y H 1.0067 0.4578 0.2347 0.117 Uiso 1 1 d . . . O18W O 0.850(2) 0.0583(19) 0.0482(6) 0.054(6) Uiso 0.50 1 d P A 1 H18X H 0.8670 0.1112 0.0552 0.080 Uiso 0.50 1 d P B 1 H18Y H 0.8124 0.0694 0.0345 0.080 Uiso 0.50 1 d P C 1 O19W O 0.7884(16) 0.1008(16) 0.0451(5) 0.042(5) Uiso 0.50 1 d P D 2 H19X H 0.8227 0.1464 0.0509 0.063 Uiso 0.50 1 d P E 2 H19Y H 0.7710 0.1137 0.0283 0.051 Uiso 0.50 1 d P F 2 O1A O 0.5177(7) 0.7605(7) 0.05261(19) 0.0302(19) Uani 1 1 d . . . H1A H 0.4589 0.7632 0.0563 0.045 Uiso 1 1 calc R . . C11A C 0.5524(9) 0.6783(9) 0.0616(2) 0.025(2) Uani 1 1 d . . . C12A C 0.5091(8) 0.6340(10) 0.0859(3) 0.026(3) Uani 1 1 d . . . C13A C 0.5456(9) 0.5472(10) 0.0946(2) 0.027(3) Uani 1 1 d . . . H13A H 0.5193 0.5172 0.1109 0.032 Uiso 1 1 calc R . . C14A C 0.6177(9) 0.5040(9) 0.0805(2) 0.024(2) Uani 1 1 d . . . C15A C 0.6617(8) 0.5458(9) 0.0583(2) 0.022(2) Uani 1 1 d . . . H15A H 0.7146 0.5162 0.0495 0.026 Uiso 1 1 calc R . . C16A C 0.6277(9) 0.6344(9) 0.0482(3) 0.026(2) Uani 1 1 d . . . S1A S 0.6556(2) 0.3910(2) 0.09296(6) 0.0263(6) Uani 1 1 d . . . O11A O 0.7386(6) 0.4116(6) 0.11106(17) 0.0240(17) Uani 1 1 d . . . O12A O 0.6813(7) 0.3352(7) 0.0681(2) 0.032(2) Uani 1 1 d . . . O13A O 0.5786(6) 0.3527(7) 0.1092(2) 0.032(2) Uani 1 1 d . . . C1A C 0.4284(9) 0.6782(9) 0.1007(3) 0.025(2) Uani 1 1 d . . . H1AA H 0.4332 0.7481 0.0993 0.030 Uiso 1 1 calc R . . H1AB H 0.4295 0.6606 0.1211 0.030 Uiso 1 1 calc R . . O2A O 0.3287(6) 0.7817(6) 0.05762(19) 0.0273(18) Uani 1 1 d . . . H2A H 0.3307 0.7855 0.0396 0.041 Uiso 1 1 calc R . . C21A C 0.2898(9) 0.6970(9) 0.0653(3) 0.026(3) Uani 1 1 d . . . C22A C 0.2081(9) 0.6639(9) 0.0510(3) 0.029(3) Uani 1 1 d . . . C23A C 0.1700(10) 0.5795(10) 0.0603(3) 0.030(3) Uani 1 1 d . . . H23A H 0.1147 0.5562 0.0512 0.036 Uiso 1 1 calc R . . C24A C 0.2082(11) 0.5276(10) 0.0821(3) 0.037(3) Uani 1 1 d . . . C25A C 0.2926(9) 0.5613(9) 0.0954(3) 0.028(3) Uani 1 1 d . . . H25A H 0.3201 0.5256 0.1104 0.034 Uiso 1 1 calc R . . C26A C 0.3348(9) 0.6443(9) 0.0870(2) 0.023(2) Uani 1 1 d . . . S2A S 0.1475(3) 0.4245(3) 0.09525(8) 0.0390(7) Uani 1 1 d . . . O21A O 0.0758(9) 0.4039(8) 0.0740(2) 0.041(2) Uani 1 1 d . . . O22A O 0.1091(12) 0.4460(10) 0.1232(3) 0.063(4) Uani 1 1 d . . . O23A O 0.2141(9) 0.3504(11) 0.0961(4) 0.070(4) Uani 1 1 d . . . C2A C 0.1677(9) 0.7159(9) 0.0267(3) 0.025(2) Uani 1 1 d . . . H2AA H 0.1838 0.7840 0.0283 0.030 Uiso 1 1 calc R . . H2AB H 0.0979 0.7099 0.0269 0.030 Uiso 1 1 calc R . . O3A O 0.3320(7) 0.7940(7) -0.0016(2) 0.033(2) Uani 1 1 d . . . H3A H 0.3917 0.7876 -0.0028 0.049 Uiso 1 1 calc R . . C31A C 0.2889(8) 0.7182(9) -0.0135(3) 0.023(2) Uani 1 1 d . . . C32A C 0.3277(8) 0.6832(8) -0.0396(2) 0.021(2) Uani 1 1 d . . . C33A C 0.2871(9) 0.6030(9) -0.0513(3) 0.026(3) Uani 1 1 d . . . H33A H 0.3137 0.5764 -0.0681 0.032 Uiso 1 1 calc R . . C34A C 0.2097(9) 0.5617(10) -0.0393(2) 0.026(3) Uani 1 1 d . . . C35A C 0.1683(9) 0.6000(10) -0.0146(3) 0.028(3) Uani 1 1 d . . . H35A H 0.1126 0.5717 -0.0071 0.034 Uiso 1 1 calc R . . C36A C 0.2064(8) 0.6771(9) -0.0012(3) 0.025(3) Uani 1 1 d . . . S3A S 0.1599(2) 0.4576(2) -0.05394(6) 0.0256(6) Uani 1 1 d . . . O31A O 0.1903(7) 0.4517(7) -0.08355(18) 0.033(2) Uani 1 1 d . . . O32A O 0.0592(7) 0.4616(8) -0.05035(19) 0.033(2) Uani 1 1 d . . . O33A O 0.1985(8) 0.3787(7) -0.0371(2) 0.036(2) Uani 1 1 d . . . C3A C 0.4162(9) 0.7265(9) -0.0527(3) 0.026(2) Uani 1 1 d . . . H3AA H 0.4127 0.7213 -0.0736 0.031 Uiso 1 1 calc R . . H3AB H 0.4194 0.7946 -0.0477 0.031 Uiso 1 1 calc R . . O4A O 0.5247(7) 0.7878(6) -0.0036(2) 0.032(2) Uani 1 1 d . . . H4A H 0.5224 0.7794 0.0143 0.048 Uiso 1 1 calc R . . C41A C 0.5530(9) 0.7059(8) -0.0165(3) 0.024(2) Uani 1 1 d . . . C42A C 0.6259(8) 0.6516(9) -0.0058(2) 0.021(2) Uani 1 1 d . . . C43A C 0.6528(8) 0.5708(9) -0.0194(2) 0.022(2) Uani 1 1 d . . . H43A H 0.7030 0.5338 -0.0118 0.027 Uiso 1 1 calc R . . C44A C 0.6078(8) 0.5413(9) -0.0445(2) 0.022(2) Uani 1 1 d U . . C45A C 0.5351(9) 0.5958(9) -0.0552(2) 0.024(2) Uani 1 1 d . . . H45A H 0.5051 0.5758 -0.0723 0.029 Uiso 1 1 calc R . . C46A C 0.5035(8) 0.6781(8) -0.0424(2) 0.020(2) Uani 1 1 d . . . S4A S 0.6406(2) 0.4342(2) -0.06120(6) 0.0249(6) Uani 1 1 d . . . O41A O 0.5879(8) 0.4297(7) -0.08733(19) 0.034(2) Uani 1 1 d . . . O42A O 0.6112(9) 0.3567(7) -0.0421(2) 0.044(3) Uani 1 1 d . . . O43A O 0.7419(7) 0.4355(8) -0.0644(2) 0.040(2) Uani 1 1 d . . . C4A C 0.6752(8) 0.6799(9) 0.0222(2) 0.026(3) Uani 1 1 d . . . H4AA H 0.7424 0.6601 0.0215 0.031 Uiso 1 1 calc R . . H4AB H 0.6734 0.7497 0.0243 0.031 Uiso 1 1 calc R . . O1B O 1.2801(6) 0.0317(6) 0.13011(17) 0.0225(17) Uani 1 1 d . . . H1B H 1.2857 0.0260 0.1480 0.034 Uiso 1 1 calc R . . C11B C 1.1930(8) 0.0679(8) 0.1239(2) 0.021(2) Uani 1 1 d . . . C12B C 1.1392(9) 0.0327(8) 0.1009(2) 0.023(2) Uani 1 1 d . . . C13B C 1.0526(9) 0.0758(8) 0.0958(3) 0.024(2) Uani 1 1 d . . . H13B H 1.0140 0.0532 0.0807 0.029 Uiso 1 1 calc R . . C14B C 1.0213(8) 0.1503(9) 0.1119(2) 0.020(2) Uani 1 1 d . . . C15B C 1.0739(8) 0.1819(9) 0.1345(3) 0.024(2) Uani 1 1 d . . . H15B H 1.0503 0.2319 0.1460 0.029 Uiso 1 1 calc R . . C16B C 1.1609(9) 0.1421(8) 0.1409(2) 0.019(2) Uani 1 1 d . . . S1B S 0.9114(2) 0.2052(2) 0.10489(6) 0.0214(5) Uani 1 1 d . . . O11B O 0.9013(6) 0.2764(6) 0.12699(18) 0.0244(17) Uani 1 1 d . . . O12B O 0.8377(6) 0.1348(6) 0.10618(17) 0.0260(17) Uani 1 1 d . . . O13B O 0.9192(6) 0.2502(7) 0.07651(17) 0.0255(18) Uani 1 1 d . . . C1B C 1.1733(9) -0.0504(9) 0.0840(2) 0.024(2) Uani 1 1 d . . . H1BA H 1.1534 -0.0421 0.0640 0.029 Uiso 1 1 calc R . . H1BB H 1.2434 -0.0512 0.0844 0.029 Uiso 1 1 calc R . . O2B O 1.2679(6) -0.1561(7) 0.12630(17) 0.0238(16) Uani 1 1 d . . . H2B H 1.2641 -0.0960 0.1266 0.036 Uiso 1 1 calc R . . C21B C 1.1826(8) -0.1941(9) 0.1158(3) 0.025(2) Uani 1 1 d . . . C22B C 1.1444(9) -0.2776(9) 0.1269(3) 0.024(2) Uani 1 1 d . . . C23B C 1.0609(10) -0.3114(9) 0.1160(2) 0.026(3) Uani 1 1 d . . . H23B H 1.0332 -0.3671 0.1237 0.032 Uiso 1 1 calc R . . C24B C 1.0173(10) -0.2642(9) 0.0939(3) 0.028(3) Uani 1 1 d . . . C25B C 1.0523(8) -0.1798(10) 0.0836(2) 0.026(3) Uani 1 1 d . . . H25B H 1.0189 -0.1463 0.0692 0.031 Uiso 1 1 calc R . . C26B C 1.1375(8) -0.1436(8) 0.0945(2) 0.020(2) Uani 1 1 d . . . S2B S 0.9119(2) -0.3088(3) 0.07755(7) 0.0313(7) Uani 1 1 d . . . O21B O 0.8768(9) -0.3820(8) 0.0957(3) 0.048(3) Uani 1 1 d . . . O22B O 0.9403(7) -0.3452(9) 0.0501(2) 0.044(3) Uani 1 1 d . . . O23B O 0.8480(7) -0.2282(8) 0.0742(3) 0.042(2) Uani 1 1 d . . . C2B C 1.1950(10) -0.3300(8) 0.1507(2) 0.026(3) Uani 1 1 d . . . H2BA H 1.2641 -0.3205 0.1485 0.031 Uiso 1 1 calc R . . H2BB H 1.1822 -0.3986 0.1487 0.031 Uiso 1 1 calc R . . O3B O 1.2967(7) -0.1923(6) 0.18104(19) 0.0280(18) Uani 1 1 d . . . H3B H 1.2848 -0.1815 0.1636 0.042 Uiso 1 1 calc R . . C31B C 1.2151(9) -0.2253(9) 0.1945(2) 0.024(2) Uani 1 1 d . . . C32B C 1.1828(8) -0.1868(7) 0.2202(2) 0.016(2) Uani 1 1 d . . . C33B C 1.1050(9) -0.2335(9) 0.2333(2) 0.025(2) Uani 1 1 d . . . H33B H 1.0831 -0.2132 0.2514 0.030 Uiso 1 1 calc R . . C34B C 1.0625(11) -0.3063(10) 0.2201(3) 0.036(3) Uani 1 1 d DU G . C35B C 1.0908(10) -0.3382(10) 0.1936(3) 0.030(3) Uani 1 1 d . . . H35B H 1.0572 -0.3881 0.1845 0.036 Uiso 1 1 calc R . . C36B C 1.1657(10) -0.2985(9) 0.1805(2) 0.026(2) Uani 1 1 d . . . S3B S 0.9603(3) -0.3587(3) 0.23636(8) 0.0513(11) Uani 1 1 d D . . O31B O 0.9051(10) -0.4001(10) 0.2146(3) 0.058(3) Uiso 0.729(16) 1 d PD G 1 O32B O 0.9106(11) -0.2814(10) 0.2503(3) 0.058(3) Uiso 0.729(16) 1 d PD G 1 O33B O 0.9939(12) -0.4250(10) 0.2571(3) 0.058(3) Uiso 0.729(16) 1 d PD G 1 O34B O 0.9761(18) -0.366(2) 0.2663(3) 0.058(3) Uiso 0.271(16) 1 d PD G 2 O35B O 0.946(2) -0.4498(13) 0.2236(6) 0.058(3) Uiso 0.271(16) 1 d PD G 2 O36B O 0.8816(13) -0.2967(18) 0.2303(6) 0.058(3) Uiso 0.271(16) 1 d PD G 2 C3B C 1.2287(9) -0.1037(9) 0.2350(2) 0.025(3) Uani 1 1 d . . . H3BA H 1.2215 -0.1113 0.2558 0.030 Uiso 1 1 calc R . . H3BB H 1.2974 -0.1035 0.2306 0.030 Uiso 1 1 calc R . . O4B O 1.2967(6) 0.0013(6) 0.18767(18) 0.0238(17) Uani 1 1 d . . . H4B H 1.2901 -0.0585 0.1868 0.036 Uiso 1 1 calc R . . C41B C 1.2208(8) 0.0402(8) 0.2023(2) 0.020(2) Uani 1 1 d . . . C42B C 1.1820(8) 0.1237(8) 0.1931(3) 0.023(2) Uani 1 1 d . . . C43B C 1.1055(8) 0.1633(8) 0.2084(2) 0.019(2) Uani 1 1 d . . . H43B H 1.0764 0.2206 0.2024 0.023 Uiso 1 1 calc R . . C44B C 1.0740(9) 0.1158(10) 0.2327(2) 0.026(3) Uani 1 1 d . . . C45B C 1.1122(9) 0.0291(9) 0.2415(3) 0.026(3) Uani 1 1 d . . . H45B H 1.0876 -0.0023 0.2578 0.031 Uiso 1 1 calc R . . C46B C 1.1867(8) -0.0103(9) 0.2262(2) 0.023(2) Uani 1 1 d . . . S4B S 0.9817(2) 0.1709(3) 0.25273(7) 0.0336(7) Uani 1 1 d . . . O41B O 0.9438(7) 0.1005(9) 0.2722(2) 0.042(2) Uani 1 1 d . . . O42B O 0.9108(9) 0.2018(12) 0.2333(3) 0.064(4) Uani 1 1 d . . . O43B O 1.0272(7) 0.2471(7) 0.26843(18) 0.0292(19) Uani 1 1 d . . . C4B C 1.2142(10) 0.1771(9) 0.1675(2) 0.027(3) Uani 1 1 d . . . H4BA H 1.2832 0.1680 0.1648 0.032 Uiso 1 1 calc R . . H4BB H 1.2022 0.2456 0.1702 0.032 Uiso 1 1 calc R . . C1 C 0.3969(13) 0.5164(11) 0.0186(4) 0.044(4) Uani 1 1 d . . . H111 H 0.4139 0.5631 0.0331 0.066 Uiso 1 1 calc R . . H112 H 0.3287 0.5036 0.0195 0.066 Uiso 1 1 calc R . . H113 H 0.4129 0.5412 -0.0003 0.066 Uiso 1 1 calc R . . C2 C 0.4510(11) 0.4257(11) 0.0238(3) 0.038(3) Uani 1 1 d . . . H201 H 0.4362 0.4017 0.0431 0.045 Uiso 1 1 calc R . . H202 H 0.5198 0.4387 0.0229 0.045 Uiso 1 1 calc R . . C3 C 0.4248(12) 0.3478(12) 0.0011(3) 0.041(3) Uani 1 1 d . . . H31 H 0.3568 0.3315 0.0030 0.050 Uiso 1 1 calc R . . H32 H 0.4351 0.3734 -0.0182 0.050 Uiso 1 1 calc R . . C4 C 0.4824(13) 0.2613(11) 0.0049(3) 0.040(3) Uani 1 1 d . . . H41 H 0.4749 0.2201 -0.0120 0.048 Uiso 1 1 calc R . . H42 H 0.5501 0.2791 0.0063 0.048 Uiso 1 1 calc R . . N5 N 0.4553(9) 0.2094(11) 0.0301(3) 0.041(3) Uani 1 1 d . . . C6 C 0.4969(10) 0.2108(10) 0.0544(3) 0.033(3) Uani 1 1 d . . . H6 H 0.5527 0.2458 0.0585 0.039 Uiso 1 1 calc R . . N7 N 0.4511(9) 0.1564(10) 0.0730(3) 0.044(3) Uani 1 1 d . . . C8 C 0.3662(16) 0.1244(17) 0.0611(5) 0.069(6) Uani 1 1 d . . . H8 H 0.3154 0.0913 0.0699 0.083 Uiso 1 1 calc R . . C9 C 0.3753(16) 0.1535(16) 0.0331(6) 0.076(8) Uani 1 1 d . . . H9 H 0.3329 0.1374 0.0181 0.091 Uiso 1 1 calc R . . C10 C 0.4796(11) 0.1328(12) 0.1019(3) 0.039(3) Uani 1 1 d . . . H101 H 0.4228 0.1333 0.1142 0.046 Uiso 1 1 calc R . . H102 H 0.5232 0.1824 0.1089 0.046 Uiso 1 1 calc R . . C11 C 0.5278(11) 0.0375(11) 0.1046(3) 0.035(3) Uani 1 1 d . . . C12 C 0.5197(9) -0.0097(10) 0.1295(3) 0.029(3) Uani 1 1 d . . . H12 H 0.4836 0.0164 0.1446 0.035 Uiso 1 1 calc R . . C13 C 0.5643(11) -0.0959(10) 0.1328(3) 0.034(3) Uani 1 1 d . . . H13 H 0.5558 -0.1299 0.1501 0.041 Uiso 1 1 calc R . . C14 C 0.6200(10) -0.1337(9) 0.1122(3) 0.028(3) Uani 1 1 d . . . C15 C 0.6286(12) -0.0827(12) 0.0861(4) 0.045(4) Uani 1 1 d . . . H15 H 0.6644 -0.1081 0.0708 0.054 Uiso 1 1 calc R . . C16 C 0.5851(12) 0.0028(12) 0.0835(3) 0.040(4) Uani 1 1 d . . . H16 H 0.5946 0.0392 0.0668 0.049 Uiso 1 1 calc R . . C17 C 0.6721(11) -0.2263(9) 0.1165(3) 0.034(3) Uani 1 1 d . . . H171 H 0.6306 -0.2720 0.1265 0.041 Uiso 1 1 calc R . . H172 H 0.6896 -0.2537 0.0979 0.041 Uiso 1 1 calc R . . N18 N 0.7567(9) -0.2095(8) 0.1332(2) 0.032(2) Uani 1 1 d . . . C19 C 0.8146(10) -0.1374(10) 0.1310(3) 0.030(3) Uani 1 1 d . . . H19 H 0.8044 -0.0827 0.1196 0.036 Uiso 1 1 calc R . . N20 N 0.8901(7) -0.1529(9) 0.1474(2) 0.029(2) Uani 1 1 d . . . C21 C 0.8775(11) -0.2375(10) 0.1603(3) 0.035(3) Uani 1 1 d . . . H21 H 0.9198 -0.2649 0.1737 0.042 Uiso 1 1 calc R . . C22 C 0.7965(11) -0.2769(9) 0.1514(3) 0.031(3) Uani 1 1 d . . . H22 H 0.7717 -0.3373 0.1563 0.038 Uiso 1 1 calc R . . C23 C 0.9686(11) -0.0850(10) 0.1515(3) 0.034(3) Uani 1 1 d . . . H231 H 0.9572 -0.0275 0.1399 0.040 Uiso 1 1 calc R . . H232 H 1.0289 -0.1139 0.1452 0.040 Uiso 1 1 calc R . . C24 C 0.9756(11) -0.0577(12) 0.1831(3) 0.037(3) Uani 1 1 d . . . H241 H 0.9959 -0.1142 0.1940 0.044 Uiso 1 1 calc R . . H242 H 1.0258 -0.0091 0.1852 0.044 Uiso 1 1 calc R . . C25 C 0.8875(10) -0.0207(10) 0.1959(3) 0.035(3) Uani 1 1 d . . . H251 H 0.9009 -0.0030 0.2159 0.042 Uiso 1 1 calc R . . H252 H 0.8400 -0.0723 0.1963 0.042 Uiso 1 1 calc R . . C26 C 0.8448(13) 0.0632(12) 0.1812(4) 0.046(4) Uani 1 1 d . . . H261 H 0.7863 0.0817 0.1910 0.068 Uiso 1 1 calc R . . H262 H 0.8304 0.0466 0.1615 0.068 Uiso 1 1 calc R . . H263 H 0.8897 0.1161 0.1816 0.068 Uiso 1 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 Gd1 0.0328(4) 0.0340(4) 0.0198(3) -0.0008(3) 0.0015(3) -0.0091(3) O01W 0.046(7) 0.115(12) 0.020(5) -0.004(6) 0.002(4) 0.009(7) O02W 0.060(8) 0.068(8) 0.041(6) 0.002(6) 0.004(6) 0.006(6) O03W 0.077(8) 0.030(5) 0.046(6) 0.003(4) 0.023(6) 0.024(6) O04W 0.041(6) 0.043(6) 0.041(6) -0.014(5) 0.016(5) -0.015(5) O05W 0.040(6) 0.048(6) 0.038(6) -0.009(5) -0.001(4) -0.001(5) O06W 0.041(5) 0.027(5) 0.032(5) -0.011(4) -0.002(4) -0.001(4) O07W 0.085(9) 0.039(6) 0.026(5) -0.003(4) 0.009(5) -0.025(6) Gd2 0.0229(3) 0.0216(3) 0.0178(3) -0.0015(3) -0.0026(3) 0.0036(3) O08W 0.037(5) 0.039(6) 0.062(7) -0.006(5) -0.033(5) 0.007(4) O09W 0.044(5) 0.010(4) 0.034(5) -0.009(3) -0.003(4) -0.002(4) O10W 0.020(4) 0.024(4) 0.030(4) -0.001(3) 0.001(3) 0.001(3) O11W 0.028(4) 0.020(4) 0.026(4) -0.006(3) 0.005(3) -0.005(3) O12W 0.044(6) 0.033(5) 0.027(5) 0.013(4) -0.012(4) 0.002(4) O13W 0.027(5) 0.027(5) 0.063(7) -0.007(4) 0.014(4) -0.021(4) O14W 0.025(4) 0.037(5) 0.031(4) 0.004(4) 0.006(4) -0.007(4) O15W 0.054(7) 0.080(9) 0.034(6) 0.014(6) 0.018(5) 0.028(7) O16W 0.042(6) 0.054(7) 0.062(7) -0.014(6) -0.026(6) 0.010(5) O17W 0.093(12) 0.046(8) 0.094(11) -0.001(7) -0.040(10) 0.010(7) O1A 0.029(5) 0.034(5) 0.028(4) -0.001(4) -0.005(4) 0.006(4) C11A 0.025(6) 0.032(7) 0.018(5) -0.007(5) 0.002(4) -0.001(5) C12A 0.013(5) 0.034(7) 0.030(6) -0.005(5) 0.006(4) -0.002(5) C13A 0.027(6) 0.047(8) 0.006(5) 0.003(5) -0.007(4) 0.002(5) C14A 0.022(6) 0.030(6) 0.020(5) 0.001(5) -0.012(4) 0.006(5) C15A 0.015(5) 0.027(6) 0.023(6) -0.009(4) 0.002(4) 0.000(4) C16A 0.019(5) 0.035(7) 0.023(5) -0.002(5) -0.007(4) -0.003(5) S1A 0.0246(14) 0.0309(15) 0.0233(14) 0.0024(11) -0.0010(11) 0.0018(12) O11A 0.020(4) 0.031(4) 0.021(4) 0.005(3) -0.002(3) -0.001(3) O12A 0.034(5) 0.028(5) 0.035(5) 0.003(4) 0.008(4) -0.006(4) O13A 0.011(4) 0.040(5) 0.046(6) 0.002(4) 0.006(4) -0.009(4) C1A 0.022(6) 0.027(6) 0.025(6) -0.013(5) 0.000(5) 0.004(5) O2A 0.028(4) 0.028(4) 0.026(4) -0.007(3) -0.006(3) 0.004(3) C21A 0.023(6) 0.029(6) 0.028(6) -0.009(5) 0.010(5) 0.000(5) C22A 0.027(6) 0.031(6) 0.029(6) -0.011(5) 0.001(5) 0.010(5) C23A 0.033(7) 0.034(7) 0.023(6) -0.006(5) -0.005(5) 0.009(5) C24A 0.033(7) 0.030(7) 0.049(8) -0.001(6) -0.004(6) 0.008(6) C25A 0.022(6) 0.029(6) 0.033(6) -0.001(5) -0.015(5) -0.003(5) C26A 0.025(6) 0.028(6) 0.017(5) -0.004(4) -0.001(4) 0.005(5) S2A 0.0405(19) 0.0373(18) 0.0391(18) 0.0001(14) -0.0081(15) -0.0042(14) O21A 0.058(7) 0.038(5) 0.026(5) 0.002(4) -0.014(5) -0.007(5) O22A 0.083(10) 0.055(8) 0.051(7) -0.010(6) 0.010(7) -0.015(7) O23A 0.037(6) 0.056(8) 0.117(13) 0.009(8) -0.014(7) 0.002(6) C2A 0.020(5) 0.027(6) 0.028(6) 0.003(5) 0.005(5) 0.009(5) O3A 0.023(4) 0.038(5) 0.036(5) -0.011(4) -0.006(4) 0.009(4) C31A 0.016(5) 0.029(6) 0.024(6) 0.005(5) 0.002(4) 0.015(4) C32A 0.021(6) 0.022(5) 0.020(5) 0.002(4) 0.004(4) 0.010(4) C33A 0.027(6) 0.025(6) 0.026(6) 0.004(5) 0.006(5) 0.012(5) C34A 0.023(6) 0.040(7) 0.014(5) -0.006(5) 0.001(4) 0.012(5) C35A 0.019(6) 0.035(7) 0.031(6) 0.003(5) 0.009(5) 0.009(5) C36A 0.016(5) 0.032(7) 0.029(6) 0.006(5) 0.008(5) 0.019(5) S3A 0.0266(14) 0.0308(15) 0.0193(13) -0.0015(11) 0.0022(11) 0.0050(11) O31A 0.042(5) 0.039(5) 0.018(4) 0.000(4) 0.000(4) 0.001(4) O32A 0.033(5) 0.046(6) 0.020(4) -0.006(4) -0.001(4) 0.002(4) O33A 0.050(6) 0.029(5) 0.028(5) 0.004(4) -0.006(4) 0.000(4) C3A 0.020(6) 0.029(6) 0.028(6) 0.010(5) -0.002(5) -0.002(5) O4A 0.032(5) 0.020(4) 0.044(5) -0.010(4) 0.007(4) -0.002(4) C41A 0.027(6) 0.019(6) 0.026(6) -0.010(5) 0.012(5) -0.012(5) C42A 0.011(5) 0.028(6) 0.024(6) -0.004(5) 0.000(4) -0.002(4) C43A 0.016(5) 0.034(6) 0.017(5) 0.003(5) 0.000(4) -0.001(5) C44A 0.026(5) 0.035(6) 0.005(4) 0.003(4) -0.005(4) -0.008(4) C45A 0.027(6) 0.035(7) 0.009(5) 0.002(4) 0.005(4) 0.000(5) C46A 0.015(5) 0.025(6) 0.019(5) 0.001(4) 0.003(4) -0.002(4) S4A 0.0229(14) 0.0295(15) 0.0223(13) -0.0038(11) 0.0005(11) 0.0013(11) O41A 0.041(5) 0.041(5) 0.020(4) -0.003(4) 0.001(4) -0.002(4) O42A 0.065(7) 0.029(5) 0.038(5) -0.002(4) -0.008(5) -0.003(5) O43A 0.024(5) 0.046(6) 0.051(6) -0.027(5) 0.000(4) 0.000(4) C4A 0.020(5) 0.038(7) 0.020(6) -0.014(5) 0.001(4) -0.016(5) O1B 0.019(4) 0.029(4) 0.019(4) 0.003(3) -0.002(3) 0.005(3) C11B 0.016(5) 0.024(6) 0.021(5) -0.002(4) -0.004(4) 0.002(4) C12B 0.032(6) 0.023(6) 0.014(5) 0.007(4) 0.000(5) -0.006(5) C13B 0.027(6) 0.021(6) 0.025(6) 0.009(5) 0.003(5) -0.003(5) C14B 0.016(5) 0.031(6) 0.014(5) -0.002(4) 0.006(4) 0.001(4) C15B 0.019(5) 0.027(6) 0.027(6) -0.006(5) 0.001(5) 0.003(5) C16B 0.030(6) 0.014(5) 0.012(5) 0.002(4) -0.008(4) 0.004(4) S1B 0.0213(13) 0.0263(14) 0.0166(12) 0.0023(11) 0.0001(10) 0.0024(11) O11B 0.024(4) 0.021(4) 0.028(4) -0.001(3) -0.004(3) 0.010(3) O12B 0.029(4) 0.030(4) 0.019(4) 0.000(3) 0.007(3) -0.001(4) O13B 0.017(4) 0.046(5) 0.013(4) 0.009(3) -0.004(3) -0.001(3) C1B 0.024(6) 0.031(6) 0.018(5) -0.005(5) -0.006(4) -0.006(5) O2B 0.023(4) 0.028(4) 0.020(4) -0.002(3) -0.004(3) -0.002(3) C21B 0.018(6) 0.032(6) 0.025(6) -0.004(5) 0.001(4) 0.001(5) C22B 0.027(6) 0.022(6) 0.023(6) -0.003(5) -0.002(5) 0.000(5) C23B 0.038(7) 0.024(6) 0.017(5) -0.010(5) 0.010(5) -0.004(5) C24B 0.033(7) 0.032(6) 0.020(5) -0.006(5) -0.007(5) -0.003(5) C25B 0.014(5) 0.049(8) 0.014(5) 0.006(5) 0.009(4) 0.004(5) C26B 0.023(6) 0.025(6) 0.012(5) 0.001(4) 0.001(4) 0.006(5) S2B 0.0308(15) 0.0390(17) 0.0239(14) -0.0030(13) -0.0052(11) -0.0103(14) O21B 0.050(6) 0.043(6) 0.051(6) 0.011(5) -0.018(5) -0.030(5) O22B 0.029(5) 0.065(7) 0.039(5) -0.023(5) -0.009(4) -0.008(5) O23B 0.026(5) 0.041(6) 0.060(7) 0.005(5) -0.001(5) 0.008(4) C2B 0.040(7) 0.019(5) 0.019(6) -0.009(4) -0.002(5) 0.010(5) O3B 0.032(4) 0.025(4) 0.027(4) -0.005(3) 0.003(4) -0.004(4) C31B 0.030(6) 0.026(6) 0.017(5) 0.002(5) 0.005(5) 0.007(5) C32B 0.021(5) 0.014(5) 0.014(5) 0.001(4) -0.005(4) 0.007(4) C33B 0.027(6) 0.031(6) 0.017(5) 0.004(5) 0.007(4) -0.003(5) C34B 0.052(7) 0.040(6) 0.017(5) 0.010(5) -0.018(5) -0.010(6) C35B 0.035(7) 0.032(6) 0.023(6) 0.006(5) -0.011(5) 0.001(5) C36B 0.034(6) 0.030(6) 0.014(5) -0.005(4) -0.002(5) -0.008(5) S3B 0.044(2) 0.074(3) 0.0363(19) 0.0226(19) -0.0086(16) -0.023(2) C3B 0.030(6) 0.033(7) 0.011(5) 0.000(4) -0.003(4) 0.010(5) O4B 0.018(4) 0.025(4) 0.028(4) -0.002(3) -0.001(3) 0.006(3) C41B 0.019(5) 0.019(5) 0.024(6) -0.005(4) -0.006(4) 0.010(4) C42B 0.022(6) 0.014(5) 0.031(6) -0.015(5) -0.012(5) 0.000(4) C43B 0.022(5) 0.017(5) 0.018(5) -0.006(4) -0.014(4) 0.000(4) C44B 0.030(6) 0.034(7) 0.014(5) -0.016(5) -0.002(4) 0.017(5) C45B 0.026(6) 0.029(6) 0.023(6) -0.009(5) -0.006(5) 0.008(5) C46B 0.018(5) 0.034(6) 0.019(5) -0.009(5) -0.012(4) 0.009(5) S4B 0.0320(16) 0.0422(18) 0.0267(15) -0.0139(13) -0.0091(12) 0.0172(14) O41B 0.030(5) 0.053(6) 0.044(6) -0.013(5) 0.005(4) -0.005(5) O42B 0.046(7) 0.103(11) 0.043(6) -0.025(7) -0.020(5) 0.054(7) O43B 0.036(5) 0.028(4) 0.023(4) -0.009(3) -0.002(4) 0.004(4) C4B 0.037(7) 0.027(6) 0.017(5) 0.005(4) -0.005(5) -0.009(5) C1 0.052(9) 0.022(7) 0.057(10) -0.004(6) -0.003(7) -0.003(6) C2 0.033(7) 0.044(8) 0.035(7) 0.007(6) -0.010(6) 0.008(6) C3 0.049(9) 0.049(9) 0.027(7) -0.007(6) -0.005(6) -0.004(7) C4 0.057(9) 0.038(8) 0.026(7) -0.008(6) -0.003(6) 0.014(7) N5 0.029(6) 0.059(8) 0.036(7) 0.000(6) 0.000(5) 0.005(6) C6 0.032(7) 0.035(7) 0.031(7) -0.002(5) -0.015(5) -0.011(5) N7 0.026(6) 0.063(8) 0.042(7) 0.029(6) -0.023(5) -0.028(6) C8 0.055(11) 0.073(13) 0.080(14) 0.020(11) -0.029(11) -0.036(11) C9 0.072(13) 0.058(11) 0.097(17) 0.030(12) -0.055(13) -0.035(11) C10 0.043(8) 0.043(8) 0.030(7) 0.014(6) -0.001(6) -0.005(6) C11 0.044(8) 0.034(7) 0.027(6) 0.008(5) -0.007(6) 0.001(6) C12 0.019(6) 0.038(7) 0.030(7) 0.008(5) -0.001(5) -0.002(5) C13 0.043(8) 0.034(7) 0.026(6) 0.002(5) -0.005(6) -0.002(6) C14 0.033(6) 0.029(6) 0.023(6) -0.009(5) -0.015(5) -0.005(5) C15 0.044(8) 0.050(9) 0.041(8) -0.003(7) -0.003(7) -0.006(7) C16 0.054(9) 0.047(9) 0.020(6) 0.010(6) 0.009(6) -0.018(7) C17 0.038(8) 0.024(6) 0.040(7) -0.002(5) -0.003(6) -0.008(5) N18 0.045(7) 0.021(5) 0.031(6) -0.005(4) -0.001(5) -0.001(5) C19 0.037(7) 0.030(7) 0.023(6) -0.002(5) -0.004(5) -0.002(6) N20 0.022(5) 0.043(6) 0.024(5) -0.006(4) 0.003(4) -0.003(5) C21 0.045(8) 0.030(7) 0.031(7) -0.005(5) -0.008(6) -0.001(6) C22 0.042(7) 0.027(6) 0.026(6) 0.006(5) 0.006(5) 0.005(5) C23 0.037(7) 0.035(7) 0.030(7) -0.003(5) -0.005(5) -0.006(6) C24 0.042(8) 0.049(8) 0.020(6) 0.007(6) 0.002(6) 0.001(7) C25 0.037(7) 0.023(6) 0.044(8) -0.003(6) 0.003(6) -0.020(5) C26 0.048(9) 0.038(8) 0.051(9) -0.010(7) -0.005(7) 0.014(7) _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 Gd1 O21A 2.344(10) . ? Gd1 O05W 2.393(11) . ? Gd1 O13B 2.394(8) 1_455 ? Gd1 O03W 2.414(12) . ? Gd1 O04W 2.414(10) . ? Gd1 O01W 2.421(13) . ? Gd1 O06W 2.441(10) . ? Gd1 O07W 2.462(10) . ? Gd1 O02W 2.548(14) . ? O01W H01X 0.8503 . ? O01W H01Y 0.8497 . ? O02W H02X 0.8500 . ? O02W H02Y 0.8501 . ? O03W H03X 0.8498 . ? O03W H03Y 0.8503 . ? O04W H04X 0.8500 . ? O04W H04Y 0.8501 . ? O05W H05X 0.8498 . ? O05W H05Y 0.8499 . ? O06W H06X 0.8500 . ? O06W H06Y 0.8500 . ? O07W H07X 0.8501 . ? O07W H07Y 0.8500 . ? Gd2 O12W 2.358(9) . ? Gd2 O09W 2.360(8) . ? Gd2 O11B 2.374(8) . ? Gd2 O11A 2.388(8) . ? Gd2 O11W 2.396(8) . ? Gd2 O08W 2.410(9) . ? Gd2 O10W 2.436(8) . ? Gd2 O13W 2.442(9) . ? O08W H08X 0.8501 . ? O08W H08Y 0.8501 . ? O09W H09X 0.8499 . ? O09W H09Y 0.8499 . ? O10W H10X 0.8499 . ? O10W H10Y 0.8500 . ? O11W H11X 0.8499 . ? O11W H11Y 0.8501 . ? O12W H12X 0.8498 . ? O12W H12Y 0.8501 . ? O13W H13X 0.8500 . ? O13W H13Y 0.8499 . ? O14W H14X 0.8501 . ? O14W H14Y 0.8500 . ? O15W H15X 0.8499 . ? O15W H15Y 0.8498 . ? O16W H16X 0.8502 . ? O16W H16Y 0.8498 . ? O17W H17X 0.8497 . ? O17W H17Y 0.8503 . ? O18W H18X 0.8497 . ? O18W H18Y 0.8507 . ? O18W H19X 1.3084 . ? O19W H18X 1.2144 . ? O19W H18Y 0.7510 . ? O19W H19X 0.8495 . ? O19W H19Y 0.8505 . ? O1A C11A 1.328(17) . ? O1A H1A 0.8500 . ? C11A C16A 1.382(18) . ? C11A C12A 1.440(17) . ? C12A C13A 1.391(19) . ? C12A C1A 1.473(16) . ? C13A C14A 1.359(19) . ? C13A H13A 0.9500 . ? C14A C15A 1.352(18) . ? C14A S1A 1.781(12) . ? C15A C16A 1.421(18) . ? C15A H15A 0.9500 . ? C16A C4A 1.534(17) . ? S1A O13A 1.435(9) . ? S1A O12A 1.456(10) . ? S1A O11A 1.477(9) . ? C1A C26A 1.546(16) . ? C1A H1AA 0.9900 . ? C1A H1AB 0.9900 . ? O2A C21A 1.365(16) . ? O2A H2A 0.8500 . ? C21A C26A 1.413(19) . ? C21A C22A 1.414(19) . ? C22A C23A 1.38(2) . ? C22A C2A 1.475(18) . ? C23A C24A 1.37(2) . ? C23A H23A 0.9500 . ? C24A C25A 1.428(19) . ? C24A S2A 1.799(16) . ? C25A C26A 1.372(19) . ? C25A H25A 0.9500 . ? S2A O23A 1.408(15) . ? S2A O22A 1.451(14) . ? S2A O21A 1.452(11) . ? C2A C36A 1.520(17) . ? C2A H2AA 0.9900 . ? C2A H2AB 0.9900 . ? O3A C31A 1.352(17) . ? O3A H3A 0.8500 . ? C31A C36A 1.423(18) . ? C31A C32A 1.433(16) . ? C32A C33A 1.383(19) . ? C32A C3A 1.521(16) . ? C33A C34A 1.361(19) . ? C33A H33A 0.9500 . ? C34A C35A 1.410(17) . ? C34A S3A 1.768(14) . ? C35A C36A 1.37(2) . ? C35A H35A 0.9500 . ? S3A O32A 1.432(10) . ? S3A O31A 1.459(9) . ? S3A O33A 1.471(10) . ? C3A C46A 1.490(16) . ? C3A H3AA 0.9900 . ? C3A H3AB 0.9900 . ? O4A C41A 1.364(15) . ? O4A H4A 0.8500 . ? C41A C42A 1.380(19) . ? C41A C46A 1.456(17) . ? C42A C43A 1.362(18) . ? C42A C4A 1.542(15) . ? C43A C44A 1.403(16) . ? C43A H43A 0.9500 . ? C44A C45A 1.378(18) . ? C44A S4A 1.766(13) . ? C45A C46A 1.383(18) . ? C45A H45A 0.9500 . ? S4A O43A 1.438(10) . ? S4A O41A 1.438(10) . ? S4A O42A 1.476(12) . ? C4A H4AA 0.9900 . ? C4A H4AB 0.9900 . ? O1B C11B 1.364(14) . ? O1B H1B 0.8500 . ? C11B C16B 1.393(16) . ? C11B C12B 1.411(17) . ? C12B C13B 1.386(19) . ? C12B C1B 1.495(17) . ? C13B C14B 1.371(17) . ? C13B H13B 0.9500 . ? C14B C15B 1.369(17) . ? C14B S1B 1.766(12) . ? C15B C16B 1.383(17) . ? C15B H15B 0.9500 . ? C16B C4B 1.542(15) . ? S1B O12B 1.440(9) . ? S1B O11B 1.453(9) . ? S1B O13B 1.482(8) . ? O13B Gd1 2.394(8) 1_655 ? C1B C26B 1.492(17) . ? C1B H1BA 0.9900 . ? C1B H1BB 0.9900 . ? O2B C21B 1.408(15) . ? O2B H2B 0.8500 . ? C21B C26B 1.384(17) . ? C21B C22B 1.398(18) . ? C22B C23B 1.370(19) . ? C22B C2B 1.519(17) . ? C23B C24B 1.380(19) . ? C23B H23B 0.9500 . ? C24B C25B 1.378(19) . ? C24B S2B 1.789(13) . ? C25B C26B 1.403(18) . ? C25B H25B 0.9500 . ? S2B O21B 1.428(11) . ? S2B O22B 1.446(11) . ? S2B O23B 1.459(11) . ? C2B C36B 1.531(16) . ? C2B H2BA 0.9900 . ? C2B H2BB 0.9900 . ? O3B C31B 1.393(16) . ? O3B H3B 0.8500 . ? C31B C32B 1.405(16) . ? C31B C36B 1.408(18) . ? C32B C33B 1.421(17) . ? C32B C3B 1.510(17) . ? C33B C34B 1.344(19) . ? C33B H33B 0.9500 . ? C34B C35B 1.39(2) . ? C34B S3B 1.792(16) . ? C35B C36B 1.34(2) . ? C35B H35B 0.9500 . ? S3B O31B 1.412(12) . ? S3B O34B 1.428(12) . ? S3B O33B 1.431(12) . ? S3B O35B 1.434(12) . ? S3B O36B 1.442(12) . ? S3B O32B 1.453(12) . ? C3B C46B 1.504(17) . ? C3B H3BA 0.9900 . ? C3B H3BB 0.9900 . ? O4B C41B 1.387(14) . ? O4B H4B 0.8500 . ? C41B C42B 1.371(17) . ? C41B C46B 1.414(18) . ? C42B C43B 1.413(17) . ? C42B C4B 1.491(18) . ? C43B C44B 1.397(18) . ? C43B H43B 0.9500 . ? C44B C45B 1.400(19) . ? C44B S4B 1.786(12) . ? C45B C46B 1.391(17) . ? C45B H45B 0.9500 . ? S4B O42B 1.424(11) . ? S4B O41B 1.452(13) . ? S4B O43B 1.455(10) . ? C4B H4BA 0.9900 . ? C4B H4BB 0.9900 . ? C1 C2 1.51(2) . ? C1 H111 0.9800 . ? C1 H112 0.9800 . ? C1 H113 0.9800 . ? C2 C3 1.57(2) . ? C2 H201 0.9900 . ? C2 H202 0.9900 . ? C3 C4 1.48(2) . ? C3 H31 0.9900 . ? C3 H32 0.9900 . ? C4 N5 1.44(2) . ? C4 H41 0.9900 . ? C4 H42 0.9900 . ? N5 C6 1.287(19) . ? N5 C9 1.38(2) . ? C6 N7 1.333(19) . ? C6 H6 0.9500 . ? N7 C8 1.40(2) . ? N7 C10 1.454(18) . ? C8 C9 1.38(3) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.51(2) . ? C10 H101 0.9900 . ? C10 H102 0.9900 . ? C11 C12 1.354(19) . ? C11 C16 1.37(2) . ? C12 C13 1.38(2) . ? C12 H12 0.9500 . ? C13 C14 1.36(2) . ? C13 H13 0.9500 . ? C14 C15 1.42(2) . ? C14 C17 1.51(2) . ? C15 C16 1.36(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 N18 1.447(19) . ? C17 H171 0.9900 . ? C17 H172 0.9900 . ? N18 C19 1.310(19) . ? N18 C22 1.397(18) . ? C19 N20 1.331(18) . ? C19 H19 0.9500 . ? N20 C21 1.351(19) . ? N20 C23 1.478(18) . ? C21 C22 1.34(2) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.538(18) . ? C23 H231 0.9900 . ? C23 H232 0.9900 . ? C24 C25 1.48(2) . ? C24 H241 0.9900 . ? C24 H242 0.9900 . ? C25 C26 1.50(2) . ? C25 H251 0.9900 . ? C25 H252 0.9900 . ? C26 H261 0.9800 . ? C26 H262 0.9800 . ? C26 H263 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 O21A Gd1 O05W 139.8(4) . . ? O21A Gd1 O13B 81.7(3) . 1_455 ? O05W Gd1 O13B 79.3(3) . 1_455 ? O21A Gd1 O03W 132.2(4) . . ? O05W Gd1 O03W 72.9(4) . . ? O13B Gd1 O03W 71.0(4) 1_455 . ? O21A Gd1 O04W 71.3(4) . . ? O05W Gd1 O04W 69.0(4) . . ? O13B Gd1 O04W 70.2(4) 1_455 . ? O03W Gd1 O04W 129.3(4) . . ? O21A Gd1 O01W 72.1(4) . . ? O05W Gd1 O01W 141.8(4) . . ? O13B Gd1 O01W 135.7(4) 1_455 . ? O03W Gd1 O01W 101.2(5) . . ? O04W Gd1 O01W 129.4(4) . . ? O21A Gd1 O06W 90.3(3) . . ? O05W Gd1 O06W 81.5(4) . . ? O13B Gd1 O06W 139.0(3) 1_455 . ? O03W Gd1 O06W 135.5(4) . . ? O04W Gd1 O06W 69.2(4) . . ? O01W Gd1 O06W 77.3(5) . . ? O21A Gd1 O07W 140.8(4) . . ? O05W Gd1 O07W 72.1(4) . . ? O13B Gd1 O07W 135.2(3) 1_455 . ? O03W Gd1 O07W 68.0(4) . . ? O04W Gd1 O07W 126.3(5) . . ? O01W Gd1 O07W 70.8(4) . . ? O06W Gd1 O07W 69.8(3) . . ? O21A Gd1 O02W 67.8(4) . . ? O05W Gd1 O02W 138.3(4) . . ? O13B Gd1 O02W 75.4(4) 1_455 . ? O03W Gd1 O02W 67.7(5) . . ? O04W Gd1 O02W 129.3(4) . . ? O01W Gd1 O02W 62.0(5) . . ? O06W Gd1 O02W 137.7(4) . . ? O07W Gd1 O02W 104.4(4) . . ? Gd1 O01W H01X 124.3 . . ? Gd1 O01W H01Y 122.3 . . ? H01X O01W H01Y 108.7 . . ? Gd1 O02W H02X 119.2 . . ? Gd1 O02W H02Y 132.1 . . ? H02X O02W H02Y 108.0 . . ? Gd1 O03W H03X 110.3 . . ? Gd1 O03W H03Y 109.6 . . ? H03X O03W H03Y 109.5 . . ? Gd1 O04W H04X 109.6 . . ? Gd1 O04W H04Y 109.7 . . ? H04X O04W H04Y 108.6 . . ? Gd1 O05W H05X 121.1 . . ? Gd1 O05W H05Y 125.7 . . ? H05X O05W H05Y 108.1 . . ? Gd1 O06W H06X 125.6 . . ? Gd1 O06W H06Y 122.5 . . ? H06X O06W H06Y 107.6 . . ? Gd1 O07W H07X 129.1 . . ? Gd1 O07W H07Y 110.8 . . ? H07X O07W H07Y 107.8 . . ? O12W Gd2 O09W 84.8(3) . . ? O12W Gd2 O11B 110.0(3) . . ? O09W Gd2 O11B 146.7(3) . . ? O12W Gd2 O11A 147.7(3) . . ? O09W Gd2 O11A 103.2(3) . . ? O11B Gd2 O11A 80.5(3) . . ? O12W Gd2 O11W 75.5(3) . . ? O09W Gd2 O11W 141.3(3) . . ? O11B Gd2 O11W 72.1(3) . . ? O11A Gd2 O11W 79.3(3) . . ? O12W Gd2 O08W 71.8(4) . . ? O09W Gd2 O08W 80.9(4) . . ? O11B Gd2 O08W 76.1(4) . . ? O11A Gd2 O08W 140.0(4) . . ? O11W Gd2 O08W 122.1(3) . . ? O12W Gd2 O10W 77.8(3) . . ? O09W Gd2 O10W 70.6(3) . . ? O11B Gd2 O10W 140.4(3) . . ? O11A Gd2 O10W 75.6(3) . . ? O11W Gd2 O10W 72.8(3) . . ? O08W Gd2 O10W 139.8(4) . . ? O12W Gd2 O13W 138.2(4) . . ? O09W Gd2 O13W 74.1(3) . . ? O11B Gd2 O13W 75.5(3) . . ? O11A Gd2 O13W 73.4(4) . . ? O11W Gd2 O13W 140.3(3) . . ? O08W Gd2 O13W 69.6(4) . . ? O10W Gd2 O13W 125.3(3) . . ? Gd2 O08W H08X 109.4 . . ? Gd2 O08W H08Y 109.4 . . ? H08X O08W H08Y 108.8 . . ? Gd2 O09W H09X 116.7 . . ? Gd2 O09W H09Y 130.7 . . ? H09X O09W H09Y 107.3 . . ? Gd2 O10W H10X 101.8 . . ? Gd2 O10W H10Y 108.4 . . ? H10X O10W H10Y 107.7 . . ? Gd2 O11W H11X 121.2 . . ? Gd2 O11W H11Y 130.8 . . ? H11X O11W H11Y 107.9 . . ? Gd2 O12W H12X 125.9 . . ? Gd2 O12W H12Y 118.6 . . ? H12X O12W H12Y 107.7 . . ? Gd2 O13W H13X 122.0 . . ? Gd2 O13W H13Y 125.1 . . ? H13X O13W H13Y 107.7 . . ? H14X O14W H14Y 107.9 . . ? H15X O15W H15Y 107.9 . . ? H16X O16W H16Y 107.9 . . ? H17X O17W H17Y 107.1 . . ? H18X O18W H18Y 108.0 . . ? H19X O19W H19Y 107.5 . . ? C11A O1A H1A 109.5 . . ? O1A C11A C16A 122.0(11) . . ? O1A C11A C12A 118.4(11) . . ? C16A C11A C12A 119.6(12) . . ? C13A C12A C11A 117.3(11) . . ? C13A C12A C1A 121.4(11) . . ? C11A C12A C1A 121.3(12) . . ? C14A C13A C12A 122.0(12) . . ? C14A C13A H13A 119.0 . . ? C12A C13A H13A 119.0 . . ? C15A C14A C13A 121.7(12) . . ? C15A C14A S1A 120.4(10) . . ? C13A C14A S1A 117.9(10) . . ? C14A C15A C16A 119.1(11) . . ? C14A C15A H15A 120.4 . . ? C16A C15A H15A 120.4 . . ? C11A C16A C15A 120.2(12) . . ? C11A C16A C4A 120.7(12) . . ? C15A C16A C4A 119.1(11) . . ? O13A S1A O12A 114.4(6) . . ? O13A S1A O11A 111.6(5) . . ? O12A S1A O11A 111.9(6) . . ? O13A S1A C14A 106.5(6) . . ? O12A S1A C14A 107.2(6) . . ? O11A S1A C14A 104.5(5) . . ? S1A O11A Gd2 140.5(5) . . ? C12A C1A C26A 109.5(9) . . ? C12A C1A H1AA 109.8 . . ? C26A C1A H1AA 109.8 . . ? C12A C1A H1AB 109.8 . . ? C26A C1A H1AB 109.8 . . ? H1AA C1A H1AB 108.2 . . ? C21A O2A H2A 109.5 . . ? O2A C21A C26A 118.1(11) . . ? O2A C21A C22A 119.5(12) . . ? C26A C21A C22A 122.4(12) . . ? C23A C22A C21A 116.9(12) . . ? C23A C22A C2A 121.7(12) . . ? C21A C22A C2A 121.3(13) . . ? C24A C23A C22A 123.1(13) . . ? C24A C23A H23A 118.4 . . ? C22A C23A H23A 118.4 . . ? C23A C24A C25A 118.5(14) . . ? C23A C24A S2A 120.2(12) . . ? C25A C24A S2A 121.1(11) . . ? C26A C25A C24A 121.4(12) . . ? C26A C25A H25A 119.3 . . ? C24A C25A H25A 119.3 . . ? C25A C26A C21A 117.4(11) . . ? C25A C26A C1A 121.1(11) . . ? C21A C26A C1A 121.5(11) . . ? O23A S2A O22A 112.2(11) . . ? O23A S2A O21A 109.6(9) . . ? O22A S2A O21A 113.9(8) . . ? O23A S2A C24A 107.0(8) . . ? O22A S2A C24A 108.7(8) . . ? O21A S2A C24A 104.9(7) . . ? S2A O21A Gd1 168.1(8) . . ? C22A C2A C36A 110.6(9) . . ? C22A C2A H2AA 109.5 . . ? C36A C2A H2AA 109.5 . . ? C22A C2A H2AB 109.5 . . ? C36A C2A H2AB 109.5 . . ? H2AA C2A H2AB 108.1 . . ? C31A O3A H3A 109.5 . . ? O3A C31A C36A 121.5(11) . . ? O3A C31A C32A 117.1(11) . . ? C36A C31A C32A 121.4(12) . . ? C33A C32A C31A 117.8(11) . . ? C33A C32A C3A 120.5(11) . . ? C31A C32A C3A 121.5(11) . . ? C34A C33A C32A 121.1(11) . . ? C34A C33A H33A 119.4 . . ? C32A C33A H33A 119.4 . . ? C33A C34A C35A 120.7(12) . . ? C33A C34A S3A 121.0(9) . . ? C35A C34A S3A 118.3(10) . . ? C36A C35A C34A 121.6(12) . . ? C36A C35A H35A 119.2 . . ? C34A C35A H35A 119.2 . . ? C35A C36A C31A 117.2(11) . . ? C35A C36A C2A 122.9(11) . . ? C31A C36A C2A 119.8(12) . . ? O32A S3A O31A 114.0(6) . . ? O32A S3A O33A 109.5(6) . . ? O31A S3A O33A 111.1(6) . . ? O32A S3A C34A 108.4(6) . . ? O31A S3A C34A 107.5(6) . . ? O33A S3A C34A 105.8(6) . . ? C46A C3A C32A 111.4(9) . . ? C46A C3A H3AA 109.4 . . ? C32A C3A H3AA 109.4 . . ? C46A C3A H3AB 109.4 . . ? C32A C3A H3AB 109.4 . . ? H3AA C3A H3AB 108.0 . . ? C41A O4A H4A 109.5 . . ? O4A C41A C42A 121.7(11) . . ? O4A C41A C46A 117.4(12) . . ? C42A C41A C46A 120.9(11) . . ? C43A C42A C41A 120.0(11) . . ? C43A C42A C4A 119.6(11) . . ? C41A C42A C4A 120.3(11) . . ? C42A C43A C44A 121.2(11) . . ? C42A C43A H43A 119.4 . . ? C44A C43A H43A 119.4 . . ? C45A C44A C43A 118.6(12) . . ? C45A C44A S4A 120.7(9) . . ? C43A C44A S4A 120.7(10) . . ? C44A C45A C46A 123.3(11) . . ? C44A C45A H45A 118.4 . . ? C46A C45A H45A 118.4 . . ? C45A C46A C41A 115.9(11) . . ? C45A C46A C3A 120.6(11) . . ? C41A C46A C3A 123.0(11) . . ? O43A S4A O41A 115.3(6) . . ? O43A S4A O42A 110.7(7) . . ? O41A S4A O42A 110.0(6) . . ? O43A S4A C44A 107.2(6) . . ? O41A S4A C44A 106.4(6) . . ? O42A S4A C44A 106.8(6) . . ? C16A C4A C42A 112.0(9) . . ? C16A C4A H4AA 109.2 . . ? C42A C4A H4AA 109.2 . . ? C16A C4A H4AB 109.2 . . ? C42A C4A H4AB 109.2 . . ? H4AA C4A H4AB 107.9 . . ? C11B O1B H1B 109.5 . . ? O1B C11B C16B 116.8(10) . . ? O1B C11B C12B 121.3(10) . . ? C16B C11B C12B 122.0(11) . . ? C13B C12B C11B 116.9(11) . . ? C13B C12B C1B 122.5(11) . . ? C11B C12B C1B 120.6(11) . . ? C14B C13B C12B 121.7(12) . . ? C14B C13B H13B 119.1 . . ? C12B C13B H13B 119.1 . . ? C15B C14B C13B 120.3(11) . . ? C15B C14B S1B 118.7(9) . . ? C13B C14B S1B 121.0(9) . . ? C14B C15B C16B 121.1(11) . . ? C14B C15B H15B 119.4 . . ? C16B C15B H15B 119.4 . . ? C15B C16B C11B 118.0(10) . . ? C15B C16B C4B 118.6(10) . . ? C11B C16B C4B 123.3(10) . . ? O12B S1B O11B 112.1(5) . . ? O12B S1B O13B 112.8(5) . . ? O11B S1B O13B 110.8(6) . . ? O12B S1B C14B 108.9(6) . . ? O11B S1B C14B 104.8(5) . . ? O13B S1B C14B 107.0(5) . . ? S1B O11B Gd2 149.9(6) . . ? S1B O13B Gd1 160.8(5) . 1_655 ? C26B C1B C12B 114.1(10) . . ? C26B C1B H1BA 108.7 . . ? C12B C1B H1BA 108.7 . . ? C26B C1B H1BB 108.7 . . ? C12B C1B H1BB 108.7 . . ? H1BA C1B H1BB 107.6 . . ? C21B O2B H2B 109.5 . . ? C26B C21B C22B 121.9(11) . . ? C26B C21B O2B 116.8(11) . . ? C22B C21B O2B 121.2(11) . . ? C23B C22B C21B 119.1(12) . . ? C23B C22B C2B 120.6(12) . . ? C21B C22B C2B 120.3(11) . . ? C22B C23B C24B 119.8(12) . . ? C22B C23B H23B 120.1 . . ? C24B C23B H23B 120.1 . . ? C25B C24B C23B 121.5(12) . . ? C25B C24B S2B 116.8(10) . . ? C23B C24B S2B 121.7(10) . . ? C24B C25B C26B 119.7(11) . . ? C24B C25B H25B 120.2 . . ? C26B C25B H25B 120.2 . . ? C21B C26B C25B 118.0(11) . . ? C21B C26B C1B 122.5(11) . . ? C25B C26B C1B 119.5(10) . . ? O21B S2B O22B 111.8(8) . . ? O21B S2B O23B 114.4(8) . . ? O22B S2B O23B 110.7(7) . . ? O21B S2B C24B 106.6(6) . . ? O22B S2B C24B 106.1(6) . . ? O23B S2B C24B 106.6(7) . . ? C22B C2B C36B 114.0(10) . . ? C22B C2B H2BA 108.7 . . ? C36B C2B H2BA 108.7 . . ? C22B C2B H2BB 108.7 . . ? C36B C2B H2BB 108.7 . . ? H2BA C2B H2BB 107.6 . . ? C31B O3B H3B 109.5 . . ? O3B C31B C32B 122.0(11) . . ? O3B C31B C36B 116.4(10) . . ? C32B C31B C36B 121.6(11) . . ? C31B C32B C33B 116.5(11) . . ? C31B C32B C3B 123.9(11) . . ? C33B C32B C3B 119.5(10) . . ? C34B C33B C32B 119.9(11) . . ? C34B C33B H33B 120.0 . . ? C32B C33B H33B 120.0 . . ? C33B C34B C35B 122.5(14) . . ? C33B C34B S3B 118.5(11) . . ? C35B C34B S3B 118.9(10) . . ? C36B C35B C34B 120.2(13) . . ? C36B C35B H35B 119.9 . . ? C34B C35B H35B 119.9 . . ? C35B C36B C31B 118.9(11) . . ? C35B C36B C2B 120.7(12) . . ? C31B C36B C2B 120.4(11) . . ? O31B S3B O33B 113.9(6) . . ? O34B S3B O35B 111.8(8) . . ? O34B S3B O36B 110.9(8) . . ? O35B S3B O36B 110.7(8) . . ? O31B S3B O32B 111.8(6) . . ? O33B S3B O32B 110.1(6) . . ? O31B S3B C34B 107.8(7) . . ? O34B S3B C34B 108.9(9) . . ? O33B S3B C34B 107.0(7) . . ? O35B S3B C34B 107.7(9) . . ? O36B S3B C34B 106.6(9) . . ? O32B S3B C34B 105.8(7) . . ? C46B C3B C32B 112.6(9) . . ? C46B C3B H3BA 109.1 . . ? C32B C3B H3BA 109.1 . . ? C46B C3B H3BB 109.1 . . ? C32B C3B H3BB 109.1 . . ? H3BA C3B H3BB 107.8 . . ? C41B O4B H4B 109.5 . . ? C42B C41B O4B 119.4(11) . . ? C42B C41B C46B 123.3(11) . . ? O4B C41B C46B 117.3(10) . . ? C41B C42B C43B 118.9(12) . . ? C41B C42B C4B 124.7(11) . . ? C43B C42B C4B 116.4(11) . . ? C44B C43B C42B 118.1(11) . . ? C44B C43B H43B 121.0 . . ? C42B C43B H43B 121.0 . . ? C43B C44B C45B 122.7(11) . . ? C43B C44B S4B 117.0(9) . . ? C45B C44B S4B 120.3(10) . . ? C46B C45B C44B 119.1(12) . . ? C46B C45B H45B 120.5 . . ? C44B C45B H45B 120.5 . . ? C45B C46B C41B 117.9(11) . . ? C45B C46B C3B 120.4(12) . . ? C41B C46B C3B 121.7(10) . . ? O42B S4B O41B 110.8(9) . . ? O42B S4B O43B 114.2(8) . . ? O41B S4B O43B 110.4(6) . . ? O42B S4B C44B 107.9(6) . . ? O41B S4B C44B 107.6(7) . . ? O43B S4B C44B 105.6(6) . . ? C42B C4B C16B 110.2(10) . . ? C42B C4B H4BA 109.6 . . ? C16B C4B H4BA 109.6 . . ? C42B C4B H4BB 109.6 . . ? C16B C4B H4BB 109.6 . . ? H4BA C4B H4BB 108.1 . . ? C2 C1 H111 109.5 . . ? C2 C1 H112 109.5 . . ? H111 C1 H112 109.5 . . ? C2 C1 H113 109.5 . . ? H111 C1 H113 109.5 . . ? H112 C1 H113 109.5 . . ? C1 C2 C3 111.3(13) . . ? C1 C2 H201 109.4 . . ? C3 C2 H201 109.4 . . ? C1 C2 H202 109.4 . . ? C3 C2 H202 109.4 . . ? H201 C2 H202 108.0 . . ? C4 C3 C2 111.5(12) . . ? C4 C3 H31 109.3 . . ? C2 C3 H31 109.3 . . ? C4 C3 H32 109.3 . . ? C2 C3 H32 109.3 . . ? H31 C3 H32 108.0 . . ? N5 C4 C3 111.8(13) . . ? N5 C4 H41 109.3 . . ? C3 C4 H41 109.3 . . ? N5 C4 H42 109.3 . . ? C3 C4 H42 109.3 . . ? H41 C4 H42 107.9 . . ? C6 N5 C9 106.9(15) . . ? C6 N5 C4 126.8(14) . . ? C9 N5 C4 126.2(15) . . ? N5 C6 N7 110.8(12) . . ? N5 C6 H6 124.6 . . ? N7 C6 H6 124.6 . . ? C6 N7 C8 109.7(13) . . ? C6 N7 C10 127.8(11) . . ? C8 N7 C10 122.5(14) . . ? C9 C8 N7 101.9(16) . . ? C9 C8 H8 129.0 . . ? N7 C8 H8 129.0 . . ? C8 C9 N5 110.1(16) . . ? C8 C9 H9 125.0 . . ? N5 C9 H9 125.0 . . ? N7 C10 C11 114.0(14) . . ? N7 C10 H101 108.8 . . ? C11 C10 H101 108.8 . . ? N7 C10 H102 108.8 . . ? C11 C10 H102 108.8 . . ? H101 C10 H102 107.7 . . ? C12 C11 C16 120.0(14) . . ? C12 C11 C10 118.2(14) . . ? C16 C11 C10 121.5(13) . . ? C11 C12 C13 119.6(13) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C14 C13 C12 122.0(13) . . ? C14 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? C13 C14 C15 117.7(14) . . ? C13 C14 C17 121.5(13) . . ? C15 C14 C17 120.8(13) . . ? C16 C15 C14 119.2(15) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C15 C16 C11 121.2(13) . . ? C15 C16 H16 119.4 . . ? C11 C16 H16 119.4 . . ? N18 C17 C14 109.5(10) . . ? N18 C17 H171 109.8 . . ? C14 C17 H171 109.8 . . ? N18 C17 H172 109.8 . . ? C14 C17 H172 109.8 . . ? H171 C17 H172 108.2 . . ? C19 N18 C22 109.0(12) . . ? C19 N18 C17 126.9(12) . . ? C22 N18 C17 123.5(12) . . ? N18 C19 N20 109.1(12) . . ? N18 C19 H19 125.4 . . ? N20 C19 H19 125.4 . . ? C19 N20 C21 107.4(12) . . ? C19 N20 C23 124.6(13) . . ? C21 N20 C23 127.8(12) . . ? C22 C21 N20 109.8(12) . . ? C22 C21 H21 125.1 . . ? N20 C21 H21 125.1 . . ? C21 C22 N18 104.6(12) . . ? C21 C22 H22 127.7 . . ? N18 C22 H22 127.7 . . ? N20 C23 C24 109.7(12) . . ? N20 C23 H231 109.7 . . ? C24 C23 H231 109.7 . . ? N20 C23 H232 109.7 . . ? C24 C23 H232 109.7 . . ? H231 C23 H232 108.2 . . ? C25 C24 C23 115.4(13) . . ? C25 C24 H241 108.4 . . ? C23 C24 H241 108.4 . . ? C25 C24 H242 108.4 . . ? C23 C24 H242 108.4 . . ? H241 C24 H242 107.5 . . ? C24 C25 C26 115.4(13) . . ? C24 C25 H251 108.4 . . ? C26 C25 H251 108.4 . . ? C24 C25 H252 108.4 . . ? C26 C25 H252 108.4 . . ? H251 C25 H252 107.5 . . ? C25 C26 H261 109.5 . . ? C25 C26 H262 109.5 . . ? H261 C26 H262 109.5 . . ? C25 C26 H263 109.5 . . ? H261 C26 H263 109.5 . . ? H262 C26 H263 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 O1A C11A C12A C13A 178.9(11) . . . . ? C16A C11A C12A C13A -0.6(17) . . . . ? O1A C11A C12A C1A -0.2(18) . . . . ? C16A C11A C12A C1A -179.6(11) . . . . ? C11A C12A C13A C14A -1.5(18) . . . . ? C1A C12A C13A C14A 177.6(12) . . . . ? C12A C13A C14A C15A 3.9(19) . . . . ? C12A C13A C14A S1A -177.8(10) . . . . ? C13A C14A C15A C16A -4.0(18) . . . . ? S1A C14A C15A C16A 177.8(9) . . . . ? O1A C11A C16A C15A -179.1(11) . . . . ? C12A C11A C16A C15A 0.4(17) . . . . ? O1A C11A C16A C4A 0.5(18) . . . . ? C12A C11A C16A C4A 180.0(10) . . . . ? C14A C15A C16A C11A 1.9(17) . . . . ? C14A C15A C16A C4A -177.7(10) . . . . ? C15A C14A S1A O13A -160.7(10) . . . . ? C13A C14A S1A O13A 21.0(11) . . . . ? C15A C14A S1A O12A -37.8(11) . . . . ? C13A C14A S1A O12A 143.9(10) . . . . ? C15A C14A S1A O11A 81.0(10) . . . . ? C13A C14A S1A O11A -97.3(10) . . . . ? O13A S1A O11A Gd2 18.9(11) . . . . ? O12A S1A O11A Gd2 -110.6(8) . . . . ? C14A S1A O11A Gd2 133.7(8) . . . . ? O12W Gd2 O11A S1A -9.5(13) . . . . ? O09W Gd2 O11A S1A -110.7(9) . . . . ? O11B Gd2 O11A S1A 103.1(9) . . . . ? O11W Gd2 O11A S1A 29.7(8) . . . . ? O08W Gd2 O11A S1A 157.8(7) . . . . ? O10W Gd2 O11A S1A -45.0(8) . . . . ? O13W Gd2 O11A S1A -179.4(9) . . . . ? C13A C12A C1A C26A -89.5(14) . . . . ? C11A C12A C1A C26A 89.5(14) . . . . ? O2A C21A C22A C23A -178.0(11) . . . . ? C26A C21A C22A C23A 3.7(17) . . . . ? O2A C21A C22A C2A 4.2(17) . . . . ? C26A C21A C22A C2A -174.2(11) . . . . ? C21A C22A C23A C24A -0.7(19) . . . . ? C2A C22A C23A C24A 177.2(12) . . . . ? C22A C23A C24A C25A -1(2) . . . . ? C22A C23A C24A S2A 173.6(10) . . . . ? C23A C24A C25A C26A 1(2) . . . . ? S2A C24A C25A C26A -174.3(11) . . . . ? C24A C25A C26A C21A 2.1(19) . . . . ? C24A C25A C26A C1A -177.4(12) . . . . ? O2A C21A C26A C25A 177.2(11) . . . . ? C22A C21A C26A C25A -4.4(18) . . . . ? O2A C21A C26A C1A -3.2(16) . . . . ? C22A C21A C26A C1A 175.1(11) . . . . ? C12A C1A C26A C25A 85.6(14) . . . . ? C12A C1A C26A C21A -94.0(14) . . . . ? C23A C24A S2A O23A 130.3(13) . . . . ? C25A C24A S2A O23A -54.7(15) . . . . ? C23A C24A S2A O22A -108.2(14) . . . . ? C25A C24A S2A O22A 66.7(15) . . . . ? C23A C24A S2A O21A 13.9(14) . . . . ? C25A C24A S2A O21A -171.1(12) . . . . ? O23A S2A O21A Gd1 -3(4) . . . . ? O22A S2A O21A Gd1 -130(3) . . . . ? C24A S2A O21A Gd1 112(3) . . . . ? O05W Gd1 O21A S2A 145(3) . . . . ? O13B Gd1 O21A S2A 83(4) 1_455 . . . ? O03W Gd1 O21A S2A 28(4) . . . . ? O04W Gd1 O21A S2A 155(4) . . . . ? O01W Gd1 O21A S2A -61(4) . . . . ? O06W Gd1 O21A S2A -138(4) . . . . ? O07W Gd1 O21A S2A -80(4) . . . . ? O02W Gd1 O21A S2A 5(3) . . . . ? C23A C22A C2A C36A -84.0(15) . . . . ? C21A C22A C2A C36A 93.8(14) . . . . ? O3A C31A C32A C33A 177.1(10) . . . . ? C36A C31A C32A C33A -5.2(16) . . . . ? O3A C31A C32A C3A 2.8(16) . . . . ? C36A C31A C32A C3A -179.5(10) . . . . ? C31A C32A C33A C34A 3.5(17) . . . . ? C3A C32A C33A C34A 177.8(11) . . . . ? C32A C33A C34A C35A 0.4(19) . . . . ? C32A C33A C34A S3A -178.4(9) . . . . ? C33A C34A C35A C36A -3(2) . . . . ? S3A C34A C35A C36A 176.1(10) . . . . ? C34A C35A C36A C31A 1.1(18) . . . . ? C34A C35A C36A C2A -175.5(11) . . . . ? O3A C31A C36A C35A -179.4(11) . . . . ? C32A C31A C36A C35A 3.0(17) . . . . ? O3A C31A C36A C2A -2.8(16) . . . . ? C32A C31A C36A C2A 179.6(10) . . . . ? C22A C2A C36A C35A 84.5(15) . . . . ? C22A C2A C36A C31A -92.0(13) . . . . ? C33A C34A S3A O32A -144.9(10) . . . . ? C35A C34A S3A O32A 36.2(12) . . . . ? C33A C34A S3A O31A -21.2(12) . . . . ? C35A C34A S3A O31A 159.9(10) . . . . ? C33A C34A S3A O33A 97.7(11) . . . . ? C35A C34A S3A O33A -81.2(11) . . . . ? C33A C32A C3A C46A -83.7(14) . . . . ? C31A C32A C3A C46A 90.4(14) . . . . ? O4A C41A C42A C43A -179.3(11) . . . . ? C46A C41A C42A C43A 0.2(17) . . . . ? O4A C41A C42A C4A 2.8(17) . . . . ? C46A C41A C42A C4A -177.7(10) . . . . ? C41A C42A C43A C44A 0.2(17) . . . . ? C4A C42A C43A C44A 178.2(11) . . . . ? C42A C43A C44A C45A -0.1(17) . . . . ? C42A C43A C44A S4A -177.7(9) . . . . ? C43A C44A C45A C46A -0.5(18) . . . . ? S4A C44A C45A C46A 177.1(9) . . . . ? C44A C45A C46A C41A 0.8(17) . . . . ? C44A C45A C46A C3A -171.4(11) . . . . ? O4A C41A C46A C45A 178.8(10) . . . . ? C42A C41A C46A C45A -0.7(16) . . . . ? O4A C41A C46A C3A -9.2(16) . . . . ? C42A C41A C46A C3A 171.3(11) . . . . ? C32A C3A C46A C45A 84.1(14) . . . . ? C32A C3A C46A C41A -87.6(14) . . . . ? C45A C44A S4A O43A 131.6(11) . . . . ? C43A C44A S4A O43A -50.9(11) . . . . ? C45A C44A S4A O41A 7.7(11) . . . . ? C43A C44A S4A O41A -174.8(10) . . . . ? C45A C44A S4A O42A -109.8(11) . . . . ? C43A C44A S4A O42A 67.7(11) . . . . ? C11A C16A C4A C42A -87.7(14) . . . . ? C15A C16A C4A C42A 91.9(13) . . . . ? C43A C42A C4A C16A -87.3(13) . . . . ? C41A C42A C4A C16A 90.7(14) . . . . ? O1B C11B C12B C13B -178.3(10) . . . . ? C16B C11B C12B C13B 0.3(17) . . . . ? O1B C11B C12B C1B 4.7(17) . . . . ? C16B C11B C12B C1B -176.7(11) . . . . ? C11B C12B C13B C14B 1.2(17) . . . . ? C1B C12B C13B C14B 178.1(11) . . . . ? C12B C13B C14B C15B -2.6(18) . . . . ? C12B C13B C14B S1B 179.3(9) . . . . ? C13B C14B C15B C16B 2.4(18) . . . . ? S1B C14B C15B C16B -179.4(9) . . . . ? C14B C15B C16B C11B -0.9(18) . . . . ? C14B C15B C16B C4B -176.7(11) . . . . ? O1B C11B C16B C15B 178.2(11) . . . . ? C12B C11B C16B C15B -0.4(18) . . . . ? O1B C11B C16B C4B -6.2(17) . . . . ? C12B C11B C16B C4B 175.1(11) . . . . ? C15B C14B S1B O12B -121.1(10) . . . . ? C13B C14B S1B O12B 57.1(11) . . . . ? C15B C14B S1B O11B -0.9(11) . . . . ? C13B C14B S1B O11B 177.3(9) . . . . ? C15B C14B S1B O13B 116.7(10) . . . . ? C13B C14B S1B O13B -65.1(11) . . . . ? O12B S1B O11B Gd2 -34.7(12) . . . . ? O13B S1B O11B Gd2 92.3(11) . . . . ? C14B S1B O11B Gd2 -152.7(10) . . . . ? O12W Gd2 O11B S1B 95.1(11) . . . . ? O09W Gd2 O11B S1B -152.8(9) . . . . ? O11A Gd2 O11B S1B -53.2(10) . . . . ? O11W Gd2 O11B S1B 28.6(10) . . . . ? O08W Gd2 O11B S1B 159.5(11) . . . . ? O10W Gd2 O11B S1B 0.2(13) . . . . ? O13W Gd2 O11B S1B -128.3(11) . . . . ? O12B S1B O13B Gd1 -168.9(17) . . . 1_655 ? O11B S1B O13B Gd1 64.4(19) . . . 1_655 ? C14B S1B O13B Gd1 -49(2) . . . 1_655 ? C13B C12B C1B C26B -84.5(14) . . . . ? C11B C12B C1B C26B 92.3(13) . . . . ? C26B C21B C22B C23B 1.3(18) . . . . ? O2B C21B C22B C23B 179.6(11) . . . . ? C26B C21B C22B C2B -178.7(11) . . . . ? O2B C21B C22B C2B -0.4(17) . . . . ? C21B C22B C23B C24B 1.7(18) . . . . ? C2B C22B C23B C24B -178.3(11) . . . . ? C22B C23B C24B C25B -4.5(19) . . . . ? C22B C23B C24B S2B 176.4(10) . . . . ? C23B C24B C25B C26B 4.2(19) . . . . ? S2B C24B C25B C26B -176.6(9) . . . . ? C22B C21B C26B C25B -1.6(18) . . . . ? O2B C21B C26B C25B -179.9(10) . . . . ? C22B C21B C26B C1B 174.9(11) . . . . ? O2B C21B C26B C1B -3.4(17) . . . . ? C24B C25B C26B C21B -1.2(17) . . . . ? C24B C25B C26B C1B -177.8(11) . . . . ? C12B C1B C26B C21B -86.3(14) . . . . ? C12B C1B C26B C25B 90.2(13) . . . . ? C25B C24B S2B O21B -166.3(11) . . . . ? C23B C24B S2B O21B 12.9(13) . . . . ? C25B C24B S2B O22B 74.4(12) . . . . ? C23B C24B S2B O22B -106.5(12) . . . . ? C25B C24B S2B O23B -43.6(12) . . . . ? C23B C24B S2B O23B 135.5(11) . . . . ? C23B C22B C2B C36B -90.3(14) . . . . ? C21B C22B C2B C36B 89.8(15) . . . . ? O3B C31B C32B C33B -173.2(11) . . . . ? C36B C31B C32B C33B 7.8(17) . . . . ? O3B C31B C32B C3B 3.6(17) . . . . ? C36B C31B C32B C3B -175.4(11) . . . . ? C31B C32B C33B C34B -4.3(17) . . . . ? C3B C32B C33B C34B 178.7(11) . . . . ? C32B C33B C34B C35B -1(2) . . . . ? C32B C33B C34B S3B -176.3(9) . . . . ? C33B C34B C35B C36B 3(2) . . . . ? S3B C34B C35B C36B 178.3(11) . . . . ? C34B C35B C36B C31B 1(2) . . . . ? C34B C35B C36B C2B -177.3(12) . . . . ? O3B C31B C36B C35B 174.8(12) . . . . ? C32B C31B C36B C35B -6.1(19) . . . . ? O3B C31B C36B C2B -7.2(17) . . . . ? C32B C31B C36B C2B 171.9(11) . . . . ? C22B C2B C36B C35B 87.1(16) . . . . ? C22B C2B C36B C31B -90.8(15) . . . . ? C33B C34B S3B O31B 154.1(12) . . . . ? C35B C34B S3B O31B -21.6(13) . . . . ? C33B C34B S3B O34B -41.1(18) . . . . ? C35B C34B S3B O34B 143.2(17) . . . . ? C33B C34B S3B O33B -83.0(12) . . . . ? C35B C34B S3B O33B 101.3(12) . . . . ? C33B C34B S3B O35B -162.5(17) . . . . ? C35B C34B S3B O35B 21.8(17) . . . . ? C33B C34B S3B O36B 78.6(17) . . . . ? C35B C34B S3B O36B -97.1(17) . . . . ? C33B C34B S3B O32B 34.4(13) . . . . ? C35B C34B S3B O32B -141.4(12) . . . . ? C31B C32B C3B C46B 91.1(14) . . . . ? C33B C32B C3B C46B -92.2(13) . . . . ? O4B C41B C42B C43B -179.2(9) . . . . ? C46B C41B C42B C43B 1.6(17) . . . . ? O4B C41B C42B C4B 1.3(17) . . . . ? C46B C41B C42B C4B -177.9(11) . . . . ? C41B C42B C43B C44B 1.0(15) . . . . ? C4B C42B C43B C44B -179.4(10) . . . . ? C42B C43B C44B C45B -2.9(17) . . . . ? C42B C43B C44B S4B 176.5(8) . . . . ? C43B C44B C45B C46B 2.1(18) . . . . ? S4B C44B C45B C46B -177.3(9) . . . . ? C44B C45B C46B C41B 0.5(17) . . . . ? C44B C45B C46B C3B -179.5(11) . . . . ? C42B C41B C46B C45B -2.4(17) . . . . ? O4B C41B C46B C45B 178.4(10) . . . . ? C42B C41B C46B C3B 177.6(11) . . . . ? O4B C41B C46B C3B -1.6(16) . . . . ? C32B C3B C46B C45B 92.2(13) . . . . ? C32B C3B C46B C41B -87.9(13) . . . . ? C43B C44B S4B O42B 46.2(13) . . . . ? C45B C44B S4B O42B -134.4(12) . . . . ? C43B C44B S4B O41B 165.8(9) . . . . ? C45B C44B S4B O41B -14.8(12) . . . . ? C43B C44B S4B O43B -76.3(10) . . . . ? C45B C44B S4B O43B 103.2(11) . . . . ? C41B C42B C4B C16B 88.5(14) . . . . ? C43B C42B C4B C16B -91.0(12) . . . . ? C15B C16B C4B C42B 86.1(13) . . . . ? C11B C16B C4B C42B -89.5(15) . . . . ? C1 C2 C3 C4 176.0(14) . . . . ? C2 C3 C4 N5 71.6(18) . . . . ? C3 C4 N5 C6 -99.5(19) . . . . ? C3 C4 N5 C9 76(2) . . . . ? C9 N5 C6 N7 2(2) . . . . ? C4 N5 C6 N7 178.2(15) . . . . ? N5 C6 N7 C8 -7(2) . . . . ? N5 C6 N7 C10 174.3(17) . . . . ? C6 N7 C8 C9 9(3) . . . . ? C10 N7 C8 C9 -173(2) . . . . ? N7 C8 C9 N5 -7(3) . . . . ? C6 N5 C9 C8 3(3) . . . . ? C4 N5 C9 C8 -172.5(18) . . . . ? C6 N7 C10 C11 -98(2) . . . . ? C8 N7 C10 C11 84(2) . . . . ? N7 C10 C11 C12 -151.3(13) . . . . ? N7 C10 C11 C16 34(2) . . . . ? C16 C11 C12 C13 -4(2) . . . . ? C10 C11 C12 C13 -178.8(13) . . . . ? C11 C12 C13 C14 3(2) . . . . ? C12 C13 C14 C15 -2(2) . . . . ? C12 C13 C14 C17 177.2(13) . . . . ? C13 C14 C15 C16 3(2) . . . . ? C17 C14 C15 C16 -176.3(13) . . . . ? C14 C15 C16 C11 -5(2) . . . . ? C12 C11 C16 C15 5(2) . . . . ? C10 C11 C16 C15 179.6(15) . . . . ? C13 C14 C17 N18 -79.3(16) . . . . ? C15 C14 C17 N18 100.0(15) . . . . ? C14 C17 N18 C19 -40.0(19) . . . . ? C14 C17 N18 C22 150.3(13) . . . . ? C22 N18 C19 N20 -1.3(15) . . . . ? C17 N18 C19 N20 -172.2(13) . . . . ? N18 C19 N20 C21 -0.6(15) . . . . ? N18 C19 N20 C23 -176.9(12) . . . . ? C19 N20 C21 C22 2.3(16) . . . . ? C23 N20 C21 C22 178.5(13) . . . . ? N20 C21 C22 N18 -3.0(15) . . . . ? C19 N18 C22 C21 2.6(15) . . . . ? C17 N18 C22 C21 173.9(13) . . . . ? C19 N20 C23 C24 119.1(14) . . . . ? C21 N20 C23 C24 -56.5(19) . . . . ? N20 C23 C24 C25 -54.6(17) . . . . ? C23 C24 C25 C26 -55.8(18) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1A H1A O2A 0.85 1.86 2.695(13) 168.7 . O2A H2A O3A 0.85 1.94 2.790(13) 178.7 . O3A H3A O4A 0.85 1.88 2.724(13) 173.2 . O4A H4A O1A 0.85 1.82 2.674(14) 179.5 . O1B H1B O4B 0.85 1.90 2.751(12) 174.9 . O2B H2B O1B 0.85 1.83 2.663(13) 168.6 . O3B H3B O2B 0.85 1.81 2.656(12) 176.1 . O4B H4B O3B 0.85 1.91 2.750(12) 169.6 . O01W H01X O33A 0.85 1.89 2.733(15) 168.3 . O02W H02X O23A 0.85 2.29 3.07(2) 153.0 . O02W H02Y O41B 0.85 2.03 2.811(18) 151.6 4_564 O03W H03X O41B 0.85 1.97 2.767(16) 155.0 4_564 O03W H03Y O18W 0.85 1.79 2.59(3) 156.2 1_455 O03W H03Y O19W 0.85 2.08 2.80(3) 142.9 1_455 O04W H04X O21B 0.85 2.21 2.809(17) 127.0 1_465 O04W H04Y O11A 0.85 2.18 2.895(13) 141.2 1_455 O05W H05X O16W 0.85 1.79 2.633(16) 169.1 1_455 O05W H05Y O12A 0.85 1.93 2.770(14) 169.0 1_455 O06W H06X O14W 0.85 2.04 2.888(14) 179.7 1_455 O06W H06Y O22B 0.85 1.82 2.669(14) 179.7 1_465 O07W H07X O32A 0.85 1.94 2.780(15) 168.8 . O07W H07Y O16W 0.85 2.03 2.873(18) 169.0 1_455 O08W H08X O17W 0.85 1.91 2.54(2) 129.5 . O09W H09X O31B 0.85 1.74 2.546(15) 158.3 1_565 O09W H09X O35B 0.85 2.15 2.99(3) 170.8 1_565 O09W H09Y O42A 0.85 1.90 2.741(14) 171.4 3_655 O10W H10X O13A 0.85 2.06 2.874(13) 160.5 . O10W H10Y O41A 0.85 1.96 2.786(13) 164.1 3_655 O11W H11X O12B 0.85 2.04 2.835(12) 155.2 . O11W H11Y O31A 0.85 1.81 2.652(13) 168.7 3_655 O12W H12X O42B 0.85 1.89 2.739(15) 175.2 . O12W H12Y O33A 0.85 1.86 2.710(15) 174.7 3_655 O13W H13X O22A 0.85 2.02 2.86(2) 175.3 1_655 O13W H13Y O21B 0.85 1.84 2.687(16) 174.8 1_565 O14W H14X O43A 0.85 1.98 2.827(14) 174.5 . O14W H14Y O06W 0.85 2.20 2.888(14) 137.7 1_655 O14W H14Y O32A 0.85 2.34 2.787(14) 113.6 1_655 O14W H14Y O07W 0.85 2.66 3.388(16) 144.6 1_655 O15W H15X O13A 0.85 2.06 2.895(15) 168.3 . O15W H15Y O23A 0.85 2.13 2.96(2) 168.7 . O16W H16X O42A 0.85 2.08 2.926(17) 173.2 . O16W H16X O43A 0.85 2.60 3.172(19) 125.9 . O16W H16Y O36B 0.85 1.48 2.286(19) 157.0 4_664 O16W H16Y O32B 0.85 1.98 2.82(2) 169.6 4_664 O17W H17X O3A 0.85 2.11 2.96(2) 170.7 3_755 O17W H17Y O35B 0.85 1.65 2.37(3) 140.8 1_565 O17W H17Y O33B 0.85 1.97 2.78(2) 160.7 1_565 O17W H17Y O31B 0.85 2.64 3.32(2) 137.6 1_565 O18W H18X O13B 0.85 2.32 3.17(3) 176.2 . O18W H18X O12B 0.85 2.46 2.94(3) 116.8 . O18W H18Y O32B 0.85 2.10 2.95(3) 177.1 4_664 O19W H19X O03W 0.85 2.34 2.80(3) 114.8 1_655 O19W H19X O13B 0.85 2.34 3.17(2) 166.5 . O19W H19Y O36B 0.85 2.45 3.29(4) 167.7 4_664 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 67.19 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 4.017 _refine_diff_density_min -1.059 _refine_diff_density_rms 0.163