# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Ling, Irene' _publ_contact_author_email yatimah70@um.edu.my _publ_section_title ; Incorporating [1-octyl-2,3-dimethylimidazolium i p-sulfonatocalix[4]arene] supermolecules into multi-component bi-layers ; loop_ _publ_author_name I.Ling Y.Alias A.Sobolev C.Raston # Attachment '- Complex I.cif' data_240708g _database_code_depnum_ccdc_archive 'CCDC 749002' #TrackingRef '- Complex I.cif' # 6. CRYSTALLOGRAPHY _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C28 H20 O16 S4, C28 H19 O16 S4, 2(C25 H22 O P), Gd O8 H16, Gd O9 H18, C13 H25 N, 14(H2 O) ; _chemical_formula_sum 'C119 H170 Gd2 N2 O65 P2 S8' _chemical_formula_weight 3301.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 '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/m' _symmetry_space_group_name_Hall '-P 2yb' _symmetry_int_tables_number 11 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 14.2968(2) _cell_length_b 36.8876(3) _cell_length_c 14.6319(2) _cell_angle_alpha 90.0 _cell_angle_beta 110.886(1) _cell_angle_gamma 90.0 _cell_volume 7209.45(15) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 43409 _cell_measurement_theta_min 3.24 _cell_measurement_theta_max 32.3 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method ? _exptl_crystal_F_000 3408 _exptl_absorpt_coefficient_mu 1.146 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8927 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_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 182632 _diffrn_reflns_av_R_equivalents 0.0812 _diffrn_reflns_av_sigmaI/netI 0.0727 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -55 _diffrn_reflns_limit_k_max 55 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 32.38 _reflns_number_total 24970 _reflns_number_gt 16522 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _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^)+(0.1250P)^2^+29.5000P] 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 24970 _refine_ls_number_parameters 871 _refine_ls_number_restraints 33 _refine_ls_R_factor_all 0.1322 _refine_ls_R_factor_gt 0.0909 _refine_ls_wR_factor_ref 0.2425 _refine_ls_wR_factor_gt 0.2241 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _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 0.17534(3) 0.2500 0.68057(3) 0.03006(10) Uani 1 2 d S . . O11W O 0.0419(5) 0.2500 0.7504(5) 0.0377(13) Uani 1 2 d S . . O12W O 0.3320(4) 0.2500 0.8207(4) 0.0388(13) Uani 1 2 d S . . O13W O 0.1557(5) 0.2500 0.5061(5) 0.063(2) Uani 1 2 d S . . O14W O 0.0502(4) 0.2932(2) 0.5919(4) 0.0716(19) Uani 1 1 d . . . O15W O 0.1896(4) 0.30168(13) 0.7891(4) 0.0498(12) Uani 1 1 d . . . O16W O 0.2912(4) 0.29340(15) 0.6476(4) 0.0503(12) Uani 1 1 d . . . Gd2 Gd 0.76850(3) 0.2500 0.01941(3) 0.02848(10) Uani 1 2 d S . . O21W O 0.6095(4) 0.2500 -0.1194(4) 0.0376(13) Uani 1 2 d S . . O22W O 0.6770(8) 0.2978(3) 0.0564(7) 0.049(2) Uiso 0.50 1 d P A -1 O23W O 0.8726(7) 0.2912(2) 0.1448(6) 0.0392(18) Uiso 0.50 1 d P A -1 O24W O 0.7815(7) 0.3032(2) -0.0695(6) 0.0402(19) Uiso 0.50 1 d P A -1 O25W O 0.6557(11) 0.2277(4) 0.0985(11) 0.087(4) Uiso 0.50 1 d P A -1 O26W O 0.9171(14) 0.2209(5) 0.1155(13) 0.108(5) Uiso 0.50 1 d P A -1 O27W O 0.8738(10) 0.2318(3) -0.0648(9) 0.071(3) Uiso 0.50 1 d P A -1 O28W O 0.7197(7) 0.1886(2) -0.0428(6) 0.0396(19) Uiso 0.50 1 d P B -1 O1 O 0.5360(3) 0.46775(10) 0.6619(3) 0.0294(8) Uani 1 1 d . . . C11 C 0.5222(3) 0.43795(12) 0.7108(3) 0.0204(8) Uani 1 1 d . . . C12 C 0.6001(3) 0.42355(12) 0.7895(3) 0.0183(8) Uani 1 1 d . . . C13 C 0.5803(3) 0.39379(12) 0.8376(3) 0.0209(8) Uani 1 1 d . . . H13 H 0.6327 0.3834 0.8911 0.025 Uiso 1 1 calc R . . C14 C 0.4847(4) 0.37888(13) 0.8085(4) 0.0226(9) Uani 1 1 d . . . C15 C 0.4075(3) 0.39347(13) 0.7286(4) 0.0229(9) Uani 1 1 d . . . H15 H 0.3426 0.3830 0.7082 0.027 Uiso 1 1 calc R . . C16 C 0.4249(3) 0.42300(12) 0.6791(3) 0.0197(8) Uani 1 1 d . . . S1 S 0.45984(11) 0.34056(4) 0.86768(12) 0.0386(3) Uani 1 1 d . . . O11 O 0.5351(4) 0.34005(14) 0.9651(4) 0.0540(13) Uani 1 1 d . . . O12 O 0.3588(3) 0.34528(13) 0.8680(4) 0.0486(12) Uani 1 1 d . . . O13 O 0.4673(3) 0.30916(11) 0.8093(4) 0.0519(13) Uani 1 1 d . . . C1 C 0.7053(3) 0.43908(13) 0.8212(3) 0.0219(9) Uani 1 1 d . . . H1A H 0.7420 0.4327 0.8905 0.026 Uiso 1 1 calc R . . H1B H 0.7012 0.4658 0.8164 0.026 Uiso 1 1 calc R . . O2 O 0.7145(3) 0.47583(13) 0.6524(3) 0.0452(11) Uani 1 1 d . . . C21 C 0.7642(3) 0.44345(14) 0.6757(4) 0.0252(9) Uani 1 1 d . . . C22 C 0.8155(3) 0.42966(16) 0.6179(3) 0.0267(10) Uani 1 1 d . . . C23 C 0.8653(4) 0.39723(16) 0.6434(4) 0.0307(11) Uani 1 1 d . . . H23 H 0.9001 0.3875 0.6044 0.037 Uiso 1 1 calc R . . C24 C 0.8651(4) 0.37850(15) 0.7258(4) 0.0303(11) Uani 1 1 d . . . C25 C 0.8142(4) 0.39239(14) 0.7830(4) 0.0262(10) Uani 1 1 d . . . H25 H 0.8142 0.3794 0.8391 0.031 Uiso 1 1 calc R . . C26 C 0.7635(3) 0.42508(13) 0.7590(3) 0.0202(8) Uani 1 1 d . . . S2 S 0.93142(13) 0.33732(4) 0.75824(17) 0.0507(5) Uani 1 1 d . . . O21 O 0.8927(7) 0.3189(2) 0.8225(10) 0.159(5) Uani 1 1 d . . . O22 O 0.9146(4) 0.31851(19) 0.6661(7) 0.100(3) Uani 1 1 d . . . O23 O 1.0368(4) 0.34620(13) 0.8057(4) 0.0498(12) Uani 1 1 d . . . C2 C 0.8155(4) 0.44927(19) 0.5257(4) 0.0364(13) Uani 1 1 d . . . H2A H 0.7996 0.4752 0.5298 0.044 Uiso 1 1 calc R . . H2B H 0.8829 0.4477 0.5214 0.044 Uiso 1 1 calc R . . O3 O 0.6125(3) 0.46808(10) 0.4580(3) 0.0291(7) Uani 1 1 d . . . C31 C 0.6378(4) 0.44200(14) 0.4065(4) 0.0256(10) Uani 1 1 d . . . C32 C 0.5653(4) 0.42471(14) 0.3266(4) 0.0244(9) Uani 1 1 d . . . C33 C 0.5964(4) 0.39914(16) 0.2748(4) 0.0318(11) Uani 1 1 d . . . H33 H 0.5484 0.3874 0.2205 0.038 Uiso 1 1 calc R . . C34 C 0.6964(5) 0.39048(17) 0.3011(4) 0.0371(13) Uani 1 1 d . . . C35 C 0.7679(4) 0.40692(18) 0.3821(4) 0.0373(13) Uani 1 1 d . . . H35 H 0.8364 0.4003 0.4008 0.045 Uiso 1 1 calc R . . C36 C 0.7392(4) 0.43274(16) 0.4349(4) 0.0293(11) Uani 1 1 d . . . S3 S 0.73399(17) 0.35974(6) 0.22983(18) 0.0609(5) Uani 1 1 d . . . O31 O 0.8292(7) 0.3471(2) 0.2844(7) 0.111(3) Uani 1 1 d . . . O32 O 0.6627(7) 0.33020(18) 0.2085(7) 0.110(3) Uani 1 1 d . . . O33 O 0.7302(5) 0.37978(16) 0.1426(4) 0.0653(16) Uani 1 1 d . . . C3 C 0.4544(4) 0.43395(14) 0.2951(3) 0.0245(9) Uani 1 1 d . . . H3A H 0.4471 0.4606 0.2979 0.029 Uiso 1 1 calc R . . H3B H 0.4206 0.4263 0.2262 0.029 Uiso 1 1 calc R . . O4 O 0.4328(3) 0.46830(10) 0.4599(3) 0.0301(8) Uani 1 1 d . . . C41 C 0.3946(3) 0.43447(12) 0.4391(3) 0.0202(8) Uani 1 1 d . . . C42 C 0.3470(3) 0.41818(13) 0.4978(3) 0.0206(8) Uani 1 1 d . . . C43 C 0.3072(4) 0.38411(14) 0.4738(4) 0.0260(9) Uani 1 1 d . . . H43 H 0.2758 0.3727 0.5135 0.031 Uiso 1 1 calc R . . C44 C 0.3121(4) 0.36611(14) 0.3919(4) 0.0283(10) Uani 1 1 d . . . C45 C 0.3592(4) 0.38191(14) 0.3346(4) 0.0253(9) Uani 1 1 d . . . H45 H 0.3625 0.3693 0.2792 0.030 Uiso 1 1 calc R . . C46 C 0.4020(3) 0.41617(13) 0.3575(3) 0.0220(9) Uani 1 1 d . . . S4 S 0.25043(15) 0.32387(4) 0.36165(12) 0.0453(4) Uani 1 1 d . . . O41 O 0.2790(6) 0.30821(15) 0.2860(5) 0.079(2) Uani 1 1 d . . . O42 O 0.2823(5) 0.30237(12) 0.4512(4) 0.0539(13) Uani 1 1 d . . . O43 O 0.1426(4) 0.33195(17) 0.3265(4) 0.0674(16) Uani 1 1 d . . . C4 C 0.3432(3) 0.43712(13) 0.5882(3) 0.0227(9) Uani 1 1 d . . . H4A H 0.2771 0.4330 0.5939 0.027 Uiso 1 1 calc R . . H4B H 0.3517 0.4635 0.5823 0.027 Uiso 1 1 calc R . . P1 P 0.14402(10) 0.48598(4) 0.80956(9) 0.0248(3) Uani 1 1 d . . . O5 O 0.5531(3) 0.54673(11) 0.9338(3) 0.0338(8) Uani 1 1 d . . . C51 C 0.2676(4) 0.50435(14) 0.8481(3) 0.0253(9) Uani 1 1 d . . . C52 C 0.3375(4) 0.49117(13) 0.8110(4) 0.0245(9) Uani 1 1 d . . . H52 H 0.3200 0.4721 0.7643 0.029 Uiso 1 1 calc R . . C53 C 0.4327(4) 0.50572(14) 0.8421(4) 0.0264(10) Uani 1 1 d . . . H53 H 0.4805 0.4965 0.8167 0.032 Uiso 1 1 calc R . . C54 C 0.4595(4) 0.53376(13) 0.9101(3) 0.0231(9) Uani 1 1 d . . . C55 C 0.3908(4) 0.54754(18) 0.9474(4) 0.0369(13) Uani 1 1 d . . . H55 H 0.4085 0.5667 0.9937 0.044 Uiso 1 1 calc R . . C56 C 0.2960(4) 0.53286(19) 0.9160(4) 0.0389(14) Uani 1 1 d . . . H56 H 0.2482 0.5423 0.9412 0.047 Uiso 1 1 calc R . . C57 C 0.5793(5) 0.57835(17) 0.9945(4) 0.0414(14) Uani 1 1 d . . . H57A H 0.6489 0.5850 1.0057 0.062 Uiso 1 1 calc R . . H57B H 0.5719 0.5733 1.0573 0.062 Uiso 1 1 calc R . . H57C H 0.5350 0.5984 0.9619 0.062 Uiso 1 1 calc R . . C61 C 0.1240(4) 0.45537(14) 0.7092(4) 0.0247(9) Uani 1 1 d . . . C62 C 0.0958(4) 0.46983(15) 0.6138(4) 0.0267(10) Uani 1 1 d . . . H62 H 0.0887 0.4953 0.6039 0.032 Uiso 1 1 calc R . . C63 C 0.0786(4) 0.44682(17) 0.5352(4) 0.0311(11) Uani 1 1 d . . . H63 H 0.0608 0.4565 0.4711 0.037 Uiso 1 1 calc R . . C64 C 0.0870(4) 0.40979(17) 0.5490(4) 0.0333(12) Uani 1 1 d . . . H64 H 0.0721 0.3941 0.4942 0.040 Uiso 1 1 calc R . . C65 C 0.1175(5) 0.39529(17) 0.6433(4) 0.0359(12) Uani 1 1 d . . . H65 H 0.1257 0.3698 0.6528 0.043 Uiso 1 1 calc R . . C66 C 0.1356(5) 0.41808(15) 0.7227(4) 0.0344(12) Uani 1 1 d . . . H66 H 0.1560 0.4082 0.7869 0.041 Uiso 1 1 calc R . . C71 C 0.1274(5) 0.46202(16) 0.9089(4) 0.0339(12) Uani 1 1 d . . . C72 C 0.1987(5) 0.4663(2) 1.0048(5) 0.0484(17) Uani 1 1 d . . . H72 H 0.2547 0.4819 1.0168 0.058 Uiso 1 1 calc R . . C73 C 0.1845(7) 0.4470(3) 1.0812(5) 0.065(2) Uani 1 1 d . . . H73 H 0.2309 0.4494 1.1462 0.078 Uiso 1 1 calc R . . C74 C 0.1009(7) 0.4240(3) 1.0610(6) 0.069(3) Uani 1 1 d . . . H74 H 0.0925 0.4101 1.1121 0.083 Uiso 1 1 calc R . . C75 C 0.0338(7) 0.4217(3) 0.9711(6) 0.073(3) Uani 1 1 d . . . H75 H -0.0243 0.4073 0.9597 0.087 Uiso 1 1 calc R . . C76 C 0.0464(6) 0.4398(2) 0.8935(5) 0.056(2) Uani 1 1 d . . . H76 H -0.0014 0.4369 0.8293 0.068 Uiso 1 1 calc R . . C81 C 0.0543(4) 0.52191(15) 0.7673(4) 0.0276(10) Uani 1 1 d . . . C82 C 0.0838(4) 0.55716(16) 0.7599(4) 0.0344(12) Uani 1 1 d . . . H82 H 0.1528 0.5627 0.7765 0.041 Uiso 1 1 calc R . . C83 C 0.0124(5) 0.58432(18) 0.7282(5) 0.0442(15) Uani 1 1 d . . . H83 H 0.0332 0.6086 0.7257 0.053 Uiso 1 1 calc R . . C84 C -0.0881(5) 0.5766(2) 0.7004(4) 0.0488(18) Uani 1 1 d . . . H84 H -0.1365 0.5953 0.6778 0.059 Uiso 1 1 calc R . . C85 C -0.1176(5) 0.5412(2) 0.7057(6) 0.056(2) Uani 1 1 d . . . H85 H -0.1868 0.5356 0.6861 0.067 Uiso 1 1 calc R . . C86 C -0.0479(5) 0.5139(2) 0.7391(5) 0.0468(16) Uani 1 1 d . . . H86 H -0.0691 0.4898 0.7429 0.056 Uiso 1 1 calc R . . O01W O 0.8334(3) 0.37066(11) 0.0209(3) 0.0371(9) Uani 1 1 d . . . O02W O 0.1217(4) 0.32187(16) 0.0049(4) 0.0591(14) Uani 1 1 d . . . O03W O 0.0215(4) 0.33800(15) 0.1273(4) 0.0498(12) Uani 1 1 d . . . O04W O 0.0618(6) 0.2500 0.9423(6) 0.0583(19) Uani 1 2 d S . . O05W O 0.3198(7) 0.3450(2) 0.0560(8) 0.107(3) Uani 1 1 d . . . O06W O 0.1313(15) 0.2500 0.2025(14) 0.075(3) Uiso 0.50 2 d SP C 1 O06' O 0.2372(15) 0.2500 0.1532(14) 0.075(3) Uiso 0.50 2 d SP D 2 O07W O 1.0195(7) 0.3325(3) 0.4301(7) 0.070(2) Uiso 0.67 1 d P E 1 O07' O 0.9919(12) 0.3131(4) 0.3995(12) 0.051(3) Uiso 0.33 1 d P F 2 O08W O 0.4687(13) 0.1936(5) 0.1724(13) 0.104(5) Uiso 0.50 1 d P . . O09W O 0.0064(14) 0.2500 0.3260(14) 0.073(5) Uiso 0.50 2 d SP . . O10W O 0.4410(13) 0.2500 1.0246(13) 0.067(4) Uiso 0.50 2 d SP . . C1A C 0.5910(19) 0.3385(6) 0.6366(14) 0.1021(19) Uiso 0.50 1 d PD G -1 H1AA H 0.5483 0.3587 0.6023 0.153 Uiso 0.50 1 calc PR G -1 H1AB H 0.6474 0.3478 0.6920 0.153 Uiso 0.50 1 calc PR G -1 H1AC H 0.5518 0.3217 0.6606 0.153 Uiso 0.50 1 calc PR G -1 N1A N 0.6280(11) 0.3199(4) 0.5709(10) 0.1021(19) Uiso 0.50 1 d PGD G -1 C2A C 0.6888(8) 0.2918(3) 0.5959(9) 0.1021(19) Uiso 0.50 1 d PGD G -1 N2A N 0.7305(9) 0.2879(3) 0.5295(8) 0.1021(19) Uiso 0.50 1 d PGD G -1 C3A C 0.6954(11) 0.3135(4) 0.4634(12) 0.1021(19) Uiso 0.50 1 d PGD G -1 H3AA H 0.7127 0.3171 0.4071 0.123 Uiso 0.50 1 calc PR G -1 C4A C 0.6320(12) 0.3333(4) 0.4890(11) 0.1021(19) Uiso 0.50 1 d PGD G -1 H4AA H 0.5956 0.3536 0.4544 0.123 Uiso 0.50 1 calc PR G -1 C5A C 0.8025(11) 0.2602(4) 0.5291(12) 0.1021(19) Uiso 0.50 1 d PD G -1 H5AA H 0.8175 0.2454 0.5890 0.123 Uiso 0.50 1 calc PR G -1 H5AB H 0.8654 0.2723 0.5324 0.123 Uiso 0.50 1 calc PR G -1 C6A C 0.7703(12) 0.2354(5) 0.4424(15) 0.1021(19) Uiso 0.50 1 d PD G -1 H6AA H 0.7888 0.2476 0.3910 0.123 Uiso 0.50 1 calc PR G -1 H6AB H 0.8131 0.2136 0.4619 0.123 Uiso 0.50 1 calc PR G -1 C7A C 0.6661(13) 0.2221(5) 0.3940(12) 0.1021(19) Uiso 0.50 1 d PD G -1 H7AA H 0.6240 0.2441 0.3725 0.123 Uiso 0.50 1 calc PR G -1 H7AB H 0.6648 0.2097 0.3337 0.123 Uiso 0.50 1 calc PR G -1 C8A C 0.6114(13) 0.1981(5) 0.4392(18) 0.1021(19) Uiso 0.50 1 d PD G -1 H8AA H 0.5466 0.1924 0.3871 0.123 Uiso 0.50 1 calc PR G -1 H8AB H 0.5957 0.2130 0.4881 0.123 Uiso 0.50 1 calc PR G -1 C9A C 0.6516(17) 0.1628(5) 0.4887(19) 0.1021(19) Uiso 0.50 1 d PD G -1 H9AA H 0.6613 0.1468 0.4385 0.123 Uiso 0.50 1 calc PR G -1 H9AB H 0.7190 0.1679 0.5372 0.123 Uiso 0.50 1 calc PR G -1 C10A C 0.5971(18) 0.1409(4) 0.5403(16) 0.1021(19) Uiso 0.50 1 d PD G -1 H10A H 0.5443 0.1273 0.4890 0.123 Uiso 0.50 1 calc PR G -1 H10B H 0.6454 0.1227 0.5799 0.123 Uiso 0.50 1 calc PR G -1 C11A C 0.5485(19) 0.1568(5) 0.6052(18) 0.1021(19) Uiso 0.50 1 d PD G -1 H11A H 0.4767 0.1506 0.5754 0.123 Uiso 0.50 1 calc PR G -1 H11B H 0.5748 0.1431 0.6674 0.123 Uiso 0.50 1 calc PR G -1 C12A C 0.552(2) 0.1955(5) 0.6333(18) 0.1021(19) Uiso 0.50 1 d PD G -1 H12A H 0.5119 0.1991 0.6746 0.153 Uiso 0.50 1 calc PR G -1 H12B H 0.5249 0.2104 0.5743 0.153 Uiso 0.50 1 calc PR G -1 H12C H 0.6215 0.2026 0.6695 0.153 Uiso 0.50 1 calc PR G -1 C13A C 0.7073(15) 0.2685(5) 0.6848(13) 0.1021(19) Uiso 0.50 1 d PD G -1 H13A H 0.7556 0.2495 0.6862 0.153 Uiso 1 2 calc SR G -1 H13B H 0.6442 0.2574 0.6825 0.153 Uiso 0.50 1 calc PR G -1 H13C H 0.7342 0.2834 0.7439 0.153 Uiso 0.50 1 calc PR G -1 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 0.02115(17) 0.0424(2) 0.02992(19) 0.000 0.01316(14) 0.000 O11W 0.036(3) 0.039(3) 0.046(3) 0.000 0.023(3) 0.000 O12W 0.026(3) 0.045(3) 0.043(3) 0.000 0.010(2) 0.000 O13W 0.034(3) 0.128(7) 0.028(3) 0.000 0.013(3) 0.000 O14W 0.044(3) 0.121(5) 0.059(3) 0.042(3) 0.030(3) 0.035(3) O15W 0.051(3) 0.050(3) 0.063(3) -0.010(2) 0.039(3) 0.001(2) O16W 0.047(3) 0.067(3) 0.049(3) 0.008(2) 0.032(2) -0.005(2) Gd2 0.0328(2) 0.02068(16) 0.02900(18) 0.000 0.00738(14) 0.000 O21W 0.035(3) 0.026(3) 0.043(3) 0.000 0.004(3) 0.000 O1 0.0193(16) 0.0303(18) 0.037(2) 0.0131(15) 0.0075(15) -0.0002(14) C11 0.018(2) 0.022(2) 0.025(2) -0.0001(16) 0.0125(17) 0.0026(16) C12 0.0162(19) 0.0214(19) 0.0190(19) -0.0063(15) 0.0084(15) -0.0006(15) C13 0.021(2) 0.023(2) 0.020(2) -0.0007(16) 0.0086(16) 0.0036(16) C14 0.023(2) 0.022(2) 0.027(2) 0.0005(17) 0.0133(18) 0.0000(17) C15 0.016(2) 0.025(2) 0.029(2) -0.0029(17) 0.0095(17) -0.0013(16) C16 0.0152(19) 0.022(2) 0.025(2) -0.0011(16) 0.0104(16) 0.0036(15) S1 0.0291(7) 0.0321(7) 0.0518(9) 0.0167(6) 0.0112(6) -0.0021(5) O11 0.045(3) 0.061(3) 0.049(3) 0.029(2) 0.008(2) -0.006(2) O12 0.038(2) 0.048(3) 0.064(3) 0.019(2) 0.024(2) -0.005(2) O13 0.039(2) 0.0219(19) 0.086(4) 0.006(2) 0.012(2) -0.0038(17) C1 0.0159(19) 0.028(2) 0.021(2) -0.0062(17) 0.0052(16) -0.0027(16) O2 0.035(2) 0.057(3) 0.055(3) 0.030(2) 0.029(2) 0.025(2) C21 0.0122(19) 0.037(3) 0.025(2) 0.0047(19) 0.0051(16) -0.0005(18) C22 0.0114(19) 0.049(3) 0.020(2) 0.000(2) 0.0064(16) -0.0073(19) C23 0.023(2) 0.041(3) 0.036(3) -0.010(2) 0.020(2) -0.009(2) C24 0.025(2) 0.031(2) 0.041(3) -0.004(2) 0.020(2) -0.002(2) C25 0.022(2) 0.032(2) 0.030(2) 0.0022(19) 0.0153(19) 0.0003(18) C26 0.0128(18) 0.029(2) 0.0187(19) -0.0045(16) 0.0054(15) -0.0046(16) S2 0.0453(9) 0.0329(7) 0.0964(14) 0.0116(8) 0.0528(10) 0.0091(6) O21 0.172(8) 0.080(5) 0.333(14) 0.120(7) 0.223(10) 0.081(5) O22 0.043(3) 0.081(4) 0.163(7) -0.074(5) 0.020(4) 0.012(3) O23 0.052(3) 0.046(3) 0.050(3) 0.008(2) 0.017(2) 0.021(2) C2 0.018(2) 0.064(4) 0.030(3) 0.009(3) 0.012(2) -0.008(2) O3 0.0240(17) 0.0307(18) 0.0319(19) 0.0005(14) 0.0091(15) -0.0026(14) C31 0.023(2) 0.031(2) 0.025(2) 0.0075(18) 0.0113(18) -0.0022(18) C32 0.022(2) 0.031(2) 0.024(2) 0.0075(18) 0.0127(18) -0.0012(18) C33 0.032(3) 0.039(3) 0.028(2) 0.003(2) 0.015(2) -0.002(2) C34 0.038(3) 0.046(3) 0.038(3) 0.001(2) 0.028(3) 0.004(3) C35 0.025(3) 0.055(4) 0.037(3) 0.010(3) 0.017(2) 0.006(2) C36 0.021(2) 0.045(3) 0.026(2) 0.008(2) 0.0138(19) -0.003(2) S3 0.0680(13) 0.0545(11) 0.0866(15) -0.0108(10) 0.0596(12) 0.0047(9) O31 0.111(6) 0.110(6) 0.133(7) 0.007(5) 0.071(6) 0.064(5) O32 0.153(7) 0.063(4) 0.181(8) -0.052(5) 0.143(7) -0.033(4) O33 0.085(4) 0.069(4) 0.064(3) -0.016(3) 0.053(3) 0.000(3) C3 0.020(2) 0.032(2) 0.020(2) 0.0073(18) 0.0054(17) 0.0007(18) O4 0.0261(18) 0.0238(17) 0.047(2) -0.0042(15) 0.0207(17) -0.0052(14) C41 0.0131(18) 0.023(2) 0.024(2) 0.0055(16) 0.0057(16) 0.0039(15) C42 0.0146(19) 0.026(2) 0.022(2) 0.0035(16) 0.0074(16) 0.0025(16) C43 0.025(2) 0.031(2) 0.025(2) 0.0021(18) 0.0129(19) -0.0048(19) C44 0.030(3) 0.024(2) 0.031(2) 0.0021(19) 0.011(2) -0.0041(19) C45 0.027(2) 0.028(2) 0.022(2) -0.0002(18) 0.0095(18) 0.0014(19) C46 0.016(2) 0.028(2) 0.021(2) 0.0051(17) 0.0052(16) 0.0034(17) S4 0.0673(11) 0.0368(8) 0.0362(8) -0.0067(6) 0.0239(8) -0.0221(7) O41 0.146(6) 0.046(3) 0.068(4) -0.027(3) 0.064(4) -0.037(4) O42 0.089(4) 0.033(2) 0.046(3) -0.0011(19) 0.032(3) -0.016(2) O43 0.055(3) 0.079(4) 0.057(3) -0.006(3) 0.006(3) -0.038(3) C4 0.0156(19) 0.026(2) 0.026(2) 0.0015(17) 0.0075(17) 0.0047(17) P1 0.0238(6) 0.0343(6) 0.0198(5) -0.0025(5) 0.0122(5) -0.0004(5) O5 0.036(2) 0.037(2) 0.0309(19) -0.0090(16) 0.0144(16) -0.0132(17) C51 0.021(2) 0.037(3) 0.017(2) -0.0002(18) 0.0053(17) 0.0036(19) C52 0.030(2) 0.026(2) 0.025(2) -0.0040(17) 0.018(2) -0.0029(18) C53 0.030(2) 0.030(2) 0.028(2) -0.0073(19) 0.021(2) -0.004(2) C54 0.029(2) 0.023(2) 0.019(2) 0.0003(16) 0.0095(18) 0.0003(18) C55 0.026(3) 0.052(3) 0.028(3) -0.018(2) 0.004(2) 0.003(2) C56 0.024(3) 0.060(4) 0.033(3) -0.018(3) 0.011(2) 0.004(2) C57 0.045(3) 0.042(3) 0.032(3) -0.008(2) 0.007(3) -0.012(3) C61 0.023(2) 0.032(2) 0.023(2) -0.0025(18) 0.0124(18) 0.0002(18) C62 0.023(2) 0.038(3) 0.022(2) -0.0008(19) 0.0104(18) 0.008(2) C63 0.020(2) 0.051(3) 0.022(2) -0.006(2) 0.0076(18) 0.007(2) C64 0.018(2) 0.050(3) 0.037(3) -0.017(2) 0.015(2) -0.008(2) C65 0.038(3) 0.036(3) 0.041(3) -0.009(2) 0.023(3) -0.009(2) C66 0.041(3) 0.032(3) 0.037(3) 0.000(2) 0.023(2) -0.004(2) C71 0.043(3) 0.043(3) 0.025(2) -0.002(2) 0.024(2) -0.005(2) C72 0.039(3) 0.075(5) 0.034(3) 0.002(3) 0.017(3) -0.010(3) C73 0.058(5) 0.104(7) 0.031(3) 0.001(4) 0.014(3) -0.019(5) C74 0.091(7) 0.090(6) 0.038(4) 0.003(4) 0.034(4) -0.034(5) C75 0.084(6) 0.097(7) 0.043(4) -0.012(4) 0.030(4) -0.056(5) C76 0.058(4) 0.079(5) 0.034(3) -0.007(3) 0.018(3) -0.032(4) C81 0.022(2) 0.039(3) 0.023(2) -0.010(2) 0.0107(18) 0.002(2) C82 0.029(3) 0.041(3) 0.029(3) -0.004(2) 0.006(2) 0.004(2) C83 0.053(4) 0.039(3) 0.034(3) -0.005(2) 0.007(3) 0.011(3) C84 0.050(4) 0.066(4) 0.026(3) -0.012(3) 0.007(3) 0.027(3) C85 0.026(3) 0.080(5) 0.059(4) -0.026(4) 0.010(3) 0.011(3) C86 0.030(3) 0.051(4) 0.064(4) -0.019(3) 0.023(3) -0.002(3) O01W 0.045(2) 0.040(2) 0.0292(19) 0.0003(16) 0.0170(18) -0.0025(18) O02W 0.061(3) 0.073(4) 0.052(3) -0.012(3) 0.031(3) -0.010(3) O03W 0.039(2) 0.067(3) 0.043(3) -0.006(2) 0.014(2) 0.000(2) O04W 0.059(5) 0.070(5) 0.059(4) 0.000 0.037(4) 0.000 O05W 0.100(6) 0.084(5) 0.166(8) -0.015(5) 0.082(6) -0.019(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O14W 2.400(5) . ? Gd1 O14W 2.401(5) 4_565 ? Gd1 O12W 2.439(6) . ? Gd1 O15W 2.443(5) 4_565 ? Gd1 O15W 2.443(5) . ? Gd1 O11W 2.464(6) . ? Gd1 O13W 2.467(6) . ? Gd1 O16W 2.471(5) 4_565 ? Gd1 O16W 2.471(5) . ? Gd2 O26W 2.348(19) 4_565 ? Gd2 O26W 2.348(19) . ? Gd2 O27W 2.358(13) 4_565 ? Gd2 O27W 2.358(13) . ? Gd2 O22W 2.369(10) . ? Gd2 O22W 2.369(10) 4_565 ? Gd2 O24W 2.397(9) 4_565 ? Gd2 O24W 2.397(9) . ? Gd2 O25W 2.438(15) . ? Gd2 O25W 2.438(15) 4_565 ? Gd2 O23W 2.439(9) . ? Gd2 O23W 2.439(9) 4_565 ? O1 C11 1.364(6) . ? C11 C12 1.391(6) . ? C11 C16 1.412(6) . ? C12 C13 1.387(6) . ? C12 C1 1.519(6) . ? C13 C14 1.392(7) . ? C13 H13 0.9500 . ? C14 C15 1.398(7) . ? C14 S1 1.758(5) . ? C15 C16 1.379(7) . ? C15 H15 0.9500 . ? C16 C4 1.516(6) . ? S1 O11 1.448(5) . ? S1 O12 1.456(5) . ? S1 O13 1.465(5) . ? C1 C26 1.524(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? O2 C21 1.369(7) . ? C21 C26 1.398(7) . ? C21 C22 1.399(7) . ? C22 C23 1.374(8) . ? C22 C2 1.530(7) . ? C23 C24 1.391(8) . ? C23 H23 0.9500 . ? C24 C25 1.387(7) . ? C24 S2 1.764(6) . ? C25 C26 1.387(7) . ? C25 H25 0.9500 . ? S2 O21 1.423(6) . ? S2 O23 1.454(6) . ? S2 O22 1.458(7) . ? C2 C36 1.515(8) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? O3 C31 1.350(6) . ? C31 C36 1.400(7) . ? C31 C32 1.409(7) . ? C32 C33 1.378(8) . ? C32 C3 1.524(7) . ? C33 C34 1.380(8) . ? C33 H33 0.9500 . ? C34 C35 1.397(9) . ? C34 S3 1.750(6) . ? C35 C36 1.378(8) . ? C35 H35 0.9500 . ? S3 O31 1.390(8) . ? S3 O32 1.448(7) . ? S3 O33 1.459(6) . ? C3 C46 1.520(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? O4 C41 1.353(6) . ? C41 C42 1.406(6) . ? C41 C46 1.409(7) . ? C42 C43 1.372(7) . ? C42 C4 1.514(7) . ? C43 C44 1.394(7) . ? C43 H43 0.9500 . ? C44 C45 1.377(7) . ? C44 S4 1.767(5) . ? C45 C46 1.392(7) . ? C45 H45 0.9500 . ? S4 O41 1.431(6) . ? S4 O42 1.458(5) . ? S4 O43 1.471(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? P1 C51 1.786(5) . ? P1 C71 1.788(5) . ? P1 C61 1.793(5) . ? P1 C81 1.794(5) . ? O5 C54 1.344(6) . ? O5 C57 1.433(7) . ? C51 C52 1.384(7) . ? C51 C56 1.404(8) . ? C52 C53 1.381(7) . ? C52 H52 0.9500 . ? C53 C54 1.391(7) . ? C53 H53 0.9500 . ? C54 C55 1.380(7) . ? C55 C56 1.378(8) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C61 C66 1.391(8) . ? C61 C62 1.411(7) . ? C62 C63 1.380(7) . ? C62 H62 0.9500 . ? C63 C64 1.380(9) . ? C63 H63 0.9500 . ? C64 C65 1.397(9) . ? C64 H64 0.9500 . ? C65 C66 1.382(8) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C71 C76 1.370(9) . ? C71 C72 1.419(9) . ? C72 C73 1.401(10) . ? C72 H72 0.9500 . ? C73 C74 1.407(12) . ? C73 H73 0.9500 . ? C74 C75 1.326(12) . ? C74 H74 0.9500 . ? C75 C76 1.383(10) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C81 C82 1.384(8) . ? C81 C86 1.400(8) . ? C82 C83 1.388(8) . ? C82 H82 0.9500 . ? C83 C84 1.375(10) . ? C83 H83 0.9500 . ? C84 C85 1.385(12) . ? C84 H84 0.9500 . ? C85 C86 1.376(10) . ? C85 H85 0.9500 . ? C86 H86 0.9500 . ? C1A N1A 1.427(10) . ? C1A H1AA 0.9800 . ? C1A H1AB 0.9800 . ? C1A H1AC 0.9800 . ? N1A C2A 1.317(11) . ? N1A C4A 1.317(11) . ? C2A N2A 1.317(11) . ? C2A C13A 1.503(16) . ? N2A C3A 1.316(11) . ? N2A C5A 1.451(9) . ? C3A C4A 1.317(11) . ? C3A H3AA 0.9500 . ? C4A H4AA 0.9500 . ? C5A C6A 1.498(9) . ? C5A H5AA 0.9900 . ? C5A H5AB 0.9900 . ? C6A C7A 1.486(9) . ? C6A H6AA 0.9900 . ? C6A H6AB 0.9900 . ? C7A C8A 1.483(9) . ? C7A H7AA 0.9900 . ? C7A H7AB 0.9900 . ? C8A C9A 1.500(10) . ? C8A H8AA 0.9900 . ? C8A H8AB 0.9900 . ? C9A C10A 1.500(9) . ? C9A H9AA 0.9900 . ? C9A H9AB 0.9900 . ? C10A C11A 1.483(9) . ? C10A H10A 0.9900 . ? C10A H10B 0.9900 . ? C11A C12A 1.481(10) . ? C11A H11A 0.9900 . ? C11A H11B 0.9900 . ? C12A H12A 0.9800 . ? C12A H12B 0.9800 . ? C12A H12C 0.9800 . ? C13A H13A 0.9800 . ? C13A H13B 0.9800 . ? C13A H13C 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 O14W Gd1 O14W 83.1(4) . 4_565 ? O14W Gd1 O12W 137.61(19) . . ? O14W Gd1 O12W 137.60(19) 4_565 . ? O14W Gd1 O15W 137.93(17) . 4_565 ? O14W Gd1 O15W 73.0(2) 4_565 4_565 ? O12W Gd1 O15W 67.33(15) . 4_565 ? O14W Gd1 O15W 73.0(2) . . ? O14W Gd1 O15W 137.93(17) 4_565 . ? O12W Gd1 O15W 67.33(15) . . ? O15W Gd1 O15W 102.6(2) 4_565 . ? O14W Gd1 O11W 71.73(16) . . ? O14W Gd1 O11W 71.73(16) 4_565 . ? O12W Gd1 O11W 105.4(2) . . ? O15W Gd1 O11W 68.15(14) 4_565 . ? O15W Gd1 O11W 68.15(14) . . ? O14W Gd1 O13W 69.68(18) . . ? O14W Gd1 O13W 69.68(18) 4_565 . ? O12W Gd1 O13W 127.0(2) . . ? O15W Gd1 O13W 128.70(12) 4_565 . ? O15W Gd1 O13W 128.70(12) . . ? O11W Gd1 O13W 127.6(2) . . ? O14W Gd1 O16W 138.27(18) . 4_565 ? O14W Gd1 O16W 83.52(19) 4_565 4_565 ? O12W Gd1 O16W 71.65(16) . 4_565 ? O15W Gd1 O16W 73.44(16) 4_565 4_565 ? O15W Gd1 O16W 136.54(17) . 4_565 ? O11W Gd1 O16W 138.81(13) . 4_565 ? O13W Gd1 O16W 68.60(16) . 4_565 ? O14W Gd1 O16W 83.52(19) . . ? O14W Gd1 O16W 138.27(18) 4_565 . ? O12W Gd1 O16W 71.65(16) . . ? O15W Gd1 O16W 136.54(17) 4_565 . ? O15W Gd1 O16W 73.43(16) . . ? O11W Gd1 O16W 138.81(13) . . ? O13W Gd1 O16W 68.60(16) . . ? O16W Gd1 O16W 80.7(2) 4_565 . ? O26W Gd2 O26W 54.4(9) 4_565 . ? O26W Gd2 O27W 64.7(5) 4_565 4_565 ? O26W Gd2 O27W 80.4(6) . 4_565 ? O26W Gd2 O27W 80.4(6) 4_565 . ? O26W Gd2 O27W 64.7(5) . . ? O27W Gd2 O27W 33.1(6) 4_565 . ? O26W Gd2 O22W 88.8(5) 4_565 . ? O26W Gd2 O22W 131.2(5) . . ? O27W Gd2 O22W 114.5(4) 4_565 . ? O27W Gd2 O22W 147.0(4) . . ? O26W Gd2 O22W 131.2(5) 4_565 4_565 ? O26W Gd2 O22W 88.8(5) . 4_565 ? O27W Gd2 O22W 147.0(4) 4_565 4_565 ? O27W Gd2 O22W 114.5(4) . 4_565 ? O22W Gd2 O22W 96.1(5) . 4_565 ? O26W Gd2 O24W 118.1(5) 4_565 4_565 ? O26W Gd2 O24W 73.9(5) . 4_565 ? O27W Gd2 O24W 76.2(4) 4_565 4_565 ? O27W Gd2 O24W 45.2(4) . 4_565 ? O22W Gd2 O24W 152.7(3) . 4_565 ? O22W Gd2 O24W 70.8(3) 4_565 4_565 ? O26W Gd2 O24W 73.9(5) 4_565 . ? O26W Gd2 O24W 118.1(5) . . ? O27W Gd2 O24W 45.2(4) 4_565 . ? O27W Gd2 O24W 76.2(4) . . ? O22W Gd2 O24W 70.8(3) . . ? O22W Gd2 O24W 152.7(3) 4_565 . ? O24W Gd2 O24W 109.8(4) 4_565 . ? O26W Gd2 O25W 118.7(6) 4_565 . ? O26W Gd2 O25W 99.9(6) . . ? O27W Gd2 O25W 176.0(5) 4_565 . ? O27W Gd2 O25W 143.6(5) . . ? O22W Gd2 O25W 68.3(5) . . ? O22W Gd2 O25W 29.3(4) 4_565 . ? O24W Gd2 O25W 100.0(4) 4_565 . ? O24W Gd2 O25W 136.6(4) . . ? O26W Gd2 O25W 99.9(6) 4_565 4_565 ? O26W Gd2 O25W 118.7(6) . 4_565 ? O27W Gd2 O25W 143.6(5) 4_565 4_565 ? O27W Gd2 O25W 176.0(5) . 4_565 ? O22W Gd2 O25W 29.3(4) . 4_565 ? O22W Gd2 O25W 68.3(5) 4_565 4_565 ? O24W Gd2 O25W 136.6(4) 4_565 4_565 ? O24W Gd2 O25W 100.0(4) . 4_565 ? O25W Gd2 O25W 39.5(7) . 4_565 ? O26W Gd2 O23W 23.8(5) 4_565 . ? O26W Gd2 O23W 69.9(5) . . ? O27W Gd2 O23W 83.3(4) 4_565 . ? O27W Gd2 O23W 103.8(4) . . ? O22W Gd2 O23W 66.6(3) . . ? O22W Gd2 O23W 122.0(3) 4_565 . ? O24W Gd2 O23W 140.7(3) 4_565 . ? O24W Gd2 O23W 75.7(3) . . ? O25W Gd2 O23W 100.5(4) . . ? O25W Gd2 O23W 76.2(4) 4_565 . ? O26W Gd2 O23W 69.9(5) 4_565 4_565 ? O26W Gd2 O23W 23.8(4) . 4_565 ? O27W Gd2 O23W 103.8(4) 4_565 4_565 ? O27W Gd2 O23W 83.3(4) . 4_565 ? O22W Gd2 O23W 122.0(3) . 4_565 ? O22W Gd2 O23W 66.6(3) 4_565 4_565 ? O24W Gd2 O23W 75.7(3) 4_565 4_565 ? O24W Gd2 O23W 140.7(3) . 4_565 ? O25W Gd2 O23W 76.2(4) . 4_565 ? O25W Gd2 O23W 100.5(4) 4_565 4_565 ? O23W Gd2 O23W 77.2(4) . 4_565 ? O1 C11 C12 121.3(4) . . ? O1 C11 C16 116.9(4) . . ? C12 C11 C16 121.8(4) . . ? C13 C12 C11 118.3(4) . . ? C13 C12 C1 120.2(4) . . ? C11 C12 C1 121.4(4) . . ? C12 C13 C14 120.9(4) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C13 C14 C15 120.0(4) . . ? C13 C14 S1 121.0(4) . . ? C15 C14 S1 118.9(4) . . ? C16 C15 C14 120.5(4) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C11 118.5(4) . . ? C15 C16 C4 120.3(4) . . ? C11 C16 C4 121.0(4) . . ? O11 S1 O12 112.9(3) . . ? O11 S1 O13 112.4(3) . . ? O12 S1 O13 112.0(3) . . ? O11 S1 C14 106.6(3) . . ? O12 S1 C14 106.2(2) . . ? O13 S1 C14 106.2(3) . . ? C12 C1 C26 112.4(4) . . ? C12 C1 H1A 109.1 . . ? C26 C1 H1A 109.1 . . ? C12 C1 H1B 109.1 . . ? C26 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? O2 C21 C26 118.4(4) . . ? O2 C21 C22 120.3(5) . . ? C26 C21 C22 121.3(5) . . ? C23 C22 C21 119.0(5) . . ? C23 C22 C2 119.2(5) . . ? C21 C22 C2 121.7(5) . . ? C22 C23 C24 120.4(5) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C25 C24 C23 120.2(5) . . ? C25 C24 S2 120.2(4) . . ? C23 C24 S2 119.6(4) . . ? C26 C25 C24 120.5(5) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C21 118.4(4) . . ? C25 C26 C1 119.4(4) . . ? C21 C26 C1 122.1(4) . . ? O21 S2 O23 111.9(6) . . ? O21 S2 O22 114.1(7) . . ? O23 S2 O22 110.4(3) . . ? O21 S2 C24 106.9(3) . . ? O23 S2 C24 107.5(3) . . ? O22 S2 C24 105.4(4) . . ? C36 C2 C22 110.9(4) . . ? C36 C2 H2A 109.5 . . ? C22 C2 H2A 109.5 . . ? C36 C2 H2B 109.5 . . ? C22 C2 H2B 109.5 . . ? H2A C2 H2B 108.0 . . ? O3 C31 C36 117.6(5) . . ? O3 C31 C32 121.4(4) . . ? C36 C31 C32 120.9(5) . . ? C33 C32 C31 118.6(5) . . ? C33 C32 C3 119.4(5) . . ? C31 C32 C3 121.9(5) . . ? C32 C33 C34 120.7(5) . . ? C32 C33 H33 119.7 . . ? C34 C33 H33 119.7 . . ? C33 C34 C35 120.5(5) . . ? C33 C34 S3 119.5(5) . . ? C35 C34 S3 120.0(5) . . ? C36 C35 C34 120.1(5) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C31 119.1(5) . . ? C35 C36 C2 120.3(5) . . ? C31 C36 C2 120.5(5) . . ? O31 S3 O32 109.9(6) . . ? O31 S3 O33 113.3(5) . . ? O32 S3 O33 112.9(5) . . ? O31 S3 C34 108.7(4) . . ? O32 S3 C34 105.9(3) . . ? O33 S3 C34 105.6(3) . . ? C46 C3 C32 113.8(4) . . ? C46 C3 H3A 108.8 . . ? C32 C3 H3A 108.8 . . ? C46 C3 H3B 108.8 . . ? C32 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? O4 C41 C42 120.1(4) . . ? O4 C41 C46 119.1(4) . . ? C42 C41 C46 120.8(4) . . ? C43 C42 C41 118.8(4) . . ? C43 C42 C4 120.4(4) . . ? C41 C42 C4 120.8(4) . . ? C42 C43 C44 120.8(5) . . ? C42 C43 H43 119.6 . . ? C44 C43 H43 119.6 . . ? C45 C44 C43 120.5(5) . . ? C45 C44 S4 121.9(4) . . ? C43 C44 S4 117.5(4) . . ? C44 C45 C46 120.4(5) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? C45 C46 C41 118.6(4) . . ? C45 C46 C3 121.1(4) . . ? C41 C46 C3 120.3(4) . . ? O41 S4 O42 113.0(4) . . ? O41 S4 O43 111.4(4) . . ? O42 S4 O43 112.2(3) . . ? O41 S4 C44 107.1(3) . . ? O42 S4 C44 106.6(3) . . ? O43 S4 C44 106.0(3) . . ? C42 C4 C16 110.6(4) . . ? C42 C4 H4A 109.5 . . ? C16 C4 H4A 109.5 . . ? C42 C4 H4B 109.5 . . ? C16 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C51 P1 C71 109.5(3) . . ? C51 P1 C61 110.4(2) . . ? C71 P1 C61 109.0(3) . . ? C51 P1 C81 109.5(3) . . ? C71 P1 C81 111.0(3) . . ? C61 P1 C81 107.3(2) . . ? C54 O5 C57 117.8(5) . . ? C52 C51 C56 118.3(5) . . ? C52 C51 P1 120.9(4) . . ? C56 C51 P1 120.7(4) . . ? C53 C52 C51 120.0(5) . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C52 C53 C54 120.8(4) . . ? C52 C53 H53 119.6 . . ? C54 C53 H53 119.6 . . ? O5 C54 C55 123.4(5) . . ? O5 C54 C53 116.4(4) . . ? C55 C54 C53 120.2(5) . . ? C56 C55 C54 118.6(5) . . ? C56 C55 H55 120.7 . . ? C54 C55 H55 120.7 . . ? C55 C56 C51 122.1(5) . . ? C55 C56 H56 118.9 . . ? C51 C56 H56 118.9 . . ? O5 C57 H57A 109.5 . . ? O5 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? O5 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C66 C61 C62 119.5(5) . . ? C66 C61 P1 122.0(4) . . ? C62 C61 P1 118.5(4) . . ? C63 C62 C61 119.7(5) . . ? C63 C62 H62 120.2 . . ? C61 C62 H62 120.2 . . ? C62 C63 C64 120.4(5) . . ? C62 C63 H63 119.8 . . ? C64 C63 H63 119.8 . . ? C63 C64 C65 120.3(5) . . ? C63 C64 H64 119.9 . . ? C65 C64 H64 119.9 . . ? C66 C65 C64 119.8(6) . . ? C66 C65 H65 120.1 . . ? C64 C65 H65 120.1 . . ? C65 C66 C61 120.3(5) . . ? C65 C66 H66 119.9 . . ? C61 C66 H66 119.9 . . ? C76 C71 C72 119.8(6) . . ? C76 C71 P1 120.8(5) . . ? C72 C71 P1 119.4(5) . . ? C73 C72 C71 118.3(6) . . ? C73 C72 H72 120.8 . . ? C71 C72 H72 120.8 . . ? C72 C73 C74 119.6(7) . . ? C72 C73 H73 120.2 . . ? C74 C73 H73 120.2 . . ? C75 C74 C73 120.4(7) . . ? C75 C74 H74 119.8 . . ? C73 C74 H74 119.8 . . ? C74 C75 C76 121.5(7) . . ? C74 C75 H75 119.2 . . ? C76 C75 H75 119.2 . . ? C71 C76 C75 120.2(7) . . ? C71 C76 H76 119.9 . . ? C75 C76 H76 119.9 . . ? C82 C81 C86 119.3(5) . . ? C82 C81 P1 121.3(4) . . ? C86 C81 P1 119.3(5) . . ? C81 C82 C83 119.7(6) . . ? C81 C82 H82 120.1 . . ? C83 C82 H82 120.1 . . ? C84 C83 C82 121.1(7) . . ? C84 C83 H83 119.4 . . ? C82 C83 H83 119.4 . . ? C83 C84 C85 119.0(6) . . ? C83 C84 H84 120.5 . . ? C85 C84 H84 120.5 . . ? C86 C85 C84 120.9(7) . . ? C86 C85 H85 119.6 . . ? C84 C85 H85 119.6 . . ? C85 C86 C81 119.9(7) . . ? C85 C86 H86 120.0 . . ? C81 C86 H86 120.0 . . ? N1A C1A H1AA 109.5 . . ? N1A C1A H1AB 109.5 . . ? H1AA C1A H1AB 109.5 . . ? N1A C1A H1AC 109.5 . . ? H1AA C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? C2A N1A C4A 108.0 . . ? C2A N1A C1A 123.8(5) . . ? C4A N1A C1A 125.4(5) . . ? N1A C2A N2A 108.0 . . ? N1A C2A C13A 125.9(4) . . ? N2A C2A C13A 126.1(4) . . ? C3A N2A C2A 108.0 . . ? C3A N2A C5A 125.9(4) . . ? C2A N2A C5A 126.0(4) . . ? N2A C3A C4A 108.0 . . ? N2A C3A H3AA 126.0 . . ? C4A C3A H3AA 126.0 . . ? N1A C4A C3A 108.0 . . ? N1A C4A H4AA 126.0 . . ? C3A C4A H4AA 126.0 . . ? N2A C5A C6A 115.4(10) . . ? N2A C5A H5AA 108.4 . . ? C6A C5A H5AA 108.4 . . ? N2A C5A H5AB 108.4 . . ? C6A C5A H5AB 108.4 . . ? H5AA C5A H5AB 107.5 . . ? C7A C6A C5A 123.9(10) . . ? C7A C6A H6AA 106.4 . . ? C5A C6A H6AA 106.4 . . ? C7A C6A H6AB 106.4 . . ? C5A C6A H6AB 106.4 . . ? H6AA C6A H6AB 106.4 . . ? C8A C7A C6A 125.6(9) . . ? C8A C7A H7AA 105.9 . . ? C6A C7A H7AA 105.9 . . ? C8A C7A H7AB 105.9 . . ? C6A C7A H7AB 105.9 . . ? H7AA C7A H7AB 106.2 . . ? C7A C8A C9A 124.2(10) . . ? C7A C8A H8AA 106.3 . . ? C9A C8A H8AA 106.3 . . ? C7A C8A H8AB 106.3 . . ? C9A C8A H8AB 106.3 . . ? H8AA C8A H8AB 106.4 . . ? C10A C9A C8A 122.2(10) . . ? C10A C9A H9AA 106.8 . . ? C8A C9A H9AA 106.8 . . ? C10A C9A H9AB 106.8 . . ? C8A C9A H9AB 106.8 . . ? H9AA C9A H9AB 106.6 . . ? C11A C10A C9A 123.7(8) . . ? C11A C10A H10A 106.4 . . ? C9A C10A H10A 106.4 . . ? C11A C10A H10B 106.4 . . ? C9A C10A H10B 106.4 . . ? H10A C10A H10B 106.5 . . ? C12A C11A C10A 125.6(10) . . ? C12A C11A H11A 105.9 . . ? C10A C11A H11A 105.9 . . ? C12A C11A H11B 105.9 . . ? C10A C11A H11B 105.9 . . ? H11A C11A H11B 106.2 . . ? C11A C12A H12A 109.5 . . ? C11A C12A H12B 109.5 . . ? H12A C12A H12B 109.5 . . ? C11A C12A H12C 109.5 . . ? H12A C12A H12C 109.5 . . ? H12B C12A H12C 109.5 . . ? C2A C13A H13A 109.5 . . ? C2A C13A H13B 109.5 . . ? H13A C13A H13B 109.5 . . ? C2A C13A H13C 109.5 . . ? H13A C13A H13C 109.5 . . ? H13B C13A H13C 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 O1 C11 C12 C13 178.3(4) . . . . ? C16 C11 C12 C13 -0.3(7) . . . . ? O1 C11 C12 C1 -3.3(7) . . . . ? C16 C11 C12 C1 178.1(4) . . . . ? C11 C12 C13 C14 -0.6(7) . . . . ? C1 C12 C13 C14 -179.0(4) . . . . ? C12 C13 C14 C15 1.3(7) . . . . ? C12 C13 C14 S1 178.6(3) . . . . ? C13 C14 C15 C16 -1.1(7) . . . . ? S1 C14 C15 C16 -178.5(4) . . . . ? C14 C15 C16 C11 0.3(7) . . . . ? C14 C15 C16 C4 175.7(4) . . . . ? O1 C11 C16 C15 -178.2(4) . . . . ? C12 C11 C16 C15 0.4(7) . . . . ? O1 C11 C16 C4 6.4(6) . . . . ? C12 C11 C16 C4 -175.0(4) . . . . ? C13 C14 S1 O11 24.5(5) . . . . ? C15 C14 S1 O11 -158.1(4) . . . . ? C13 C14 S1 O12 145.1(4) . . . . ? C15 C14 S1 O12 -37.5(5) . . . . ? C13 C14 S1 O13 -95.5(4) . . . . ? C15 C14 S1 O13 81.9(4) . . . . ? C13 C12 C1 C26 96.9(5) . . . . ? C11 C12 C1 C26 -81.4(5) . . . . ? O2 C21 C22 C23 179.5(5) . . . . ? C26 C21 C22 C23 0.6(7) . . . . ? O2 C21 C22 C2 -2.0(7) . . . . ? C26 C21 C22 C2 179.1(4) . . . . ? C21 C22 C23 C24 -0.4(7) . . . . ? C2 C22 C23 C24 -178.8(5) . . . . ? C22 C23 C24 C25 0.1(8) . . . . ? C22 C23 C24 S2 -178.9(4) . . . . ? C23 C24 C25 C26 -0.2(8) . . . . ? S2 C24 C25 C26 178.8(4) . . . . ? C24 C25 C26 C21 0.5(7) . . . . ? C24 C25 C26 C1 177.9(4) . . . . ? O2 C21 C26 C25 -179.6(5) . . . . ? C22 C21 C26 C25 -0.7(7) . . . . ? O2 C21 C26 C1 3.0(7) . . . . ? C22 C21 C26 C1 -178.1(4) . . . . ? C12 C1 C26 C25 -85.3(5) . . . . ? C12 C1 C26 C21 92.1(5) . . . . ? C25 C24 S2 O21 19.6(8) . . . . ? C23 C24 S2 O21 -161.4(7) . . . . ? C25 C24 S2 O23 -100.8(5) . . . . ? C23 C24 S2 O23 78.2(5) . . . . ? C25 C24 S2 O22 141.4(5) . . . . ? C23 C24 S2 O22 -39.6(6) . . . . ? C23 C22 C2 C36 79.7(6) . . . . ? C21 C22 C2 C36 -98.7(6) . . . . ? O3 C31 C32 C33 177.9(5) . . . . ? C36 C31 C32 C33 -1.9(7) . . . . ? O3 C31 C32 C3 -1.1(7) . . . . ? C36 C31 C32 C3 179.2(4) . . . . ? C31 C32 C33 C34 0.4(8) . . . . ? C3 C32 C33 C34 179.4(5) . . . . ? C32 C33 C34 C35 1.4(9) . . . . ? C32 C33 C34 S3 -176.5(4) . . . . ? C33 C34 C35 C36 -1.8(9) . . . . ? S3 C34 C35 C36 176.1(4) . . . . ? C34 C35 C36 C31 0.3(8) . . . . ? C34 C35 C36 C2 176.9(5) . . . . ? O3 C31 C36 C35 -178.3(5) . . . . ? C32 C31 C36 C35 1.5(7) . . . . ? O3 C31 C36 C2 5.2(7) . . . . ? C32 C31 C36 C2 -175.0(5) . . . . ? C22 C2 C36 C35 -95.7(6) . . . . ? C22 C2 C36 C31 80.8(7) . . . . ? C33 C34 S3 O31 -162.2(6) . . . . ? C35 C34 S3 O31 19.9(7) . . . . ? C33 C34 S3 O32 -44.1(7) . . . . ? C35 C34 S3 O32 137.9(7) . . . . ? C33 C34 S3 O33 75.8(6) . . . . ? C35 C34 S3 O33 -102.1(6) . . . . ? C33 C32 C3 C46 101.6(5) . . . . ? C31 C32 C3 C46 -79.5(6) . . . . ? O4 C41 C42 C43 178.7(4) . . . . ? C46 C41 C42 C43 -0.4(7) . . . . ? O4 C41 C42 C4 -3.8(6) . . . . ? C46 C41 C42 C4 177.2(4) . . . . ? C41 C42 C43 C44 -1.1(7) . . . . ? C4 C42 C43 C44 -178.6(4) . . . . ? C42 C43 C44 C45 1.4(8) . . . . ? C42 C43 C44 S4 -175.2(4) . . . . ? C43 C44 C45 C46 -0.3(8) . . . . ? S4 C44 C45 C46 176.2(4) . . . . ? C44 C45 C46 C41 -1.0(7) . . . . ? C44 C45 C46 C3 179.9(5) . . . . ? O4 C41 C46 C45 -177.7(4) . . . . ? C42 C41 C46 C45 1.4(6) . . . . ? O4 C41 C46 C3 1.4(6) . . . . ? C42 C41 C46 C3 -179.5(4) . . . . ? C32 C3 C46 C45 -88.7(6) . . . . ? C32 C3 C46 C41 92.3(5) . . . . ? C45 C44 S4 O41 12.4(6) . . . . ? C43 C44 S4 O41 -171.0(5) . . . . ? C45 C44 S4 O42 133.7(5) . . . . ? C43 C44 S4 O42 -49.7(5) . . . . ? C45 C44 S4 O43 -106.6(5) . . . . ? C43 C44 S4 O43 70.0(5) . . . . ? C43 C42 C4 C16 79.4(5) . . . . ? C41 C42 C4 C16 -98.1(5) . . . . ? C15 C16 C4 C42 -89.0(5) . . . . ? C11 C16 C4 C42 86.3(5) . . . . ? C71 P1 C51 C52 111.6(4) . . . . ? C61 P1 C51 C52 -8.5(5) . . . . ? C81 P1 C51 C52 -126.5(4) . . . . ? C71 P1 C51 C56 -69.2(5) . . . . ? C61 P1 C51 C56 170.7(5) . . . . ? C81 P1 C51 C56 52.8(5) . . . . ? C56 C51 C52 C53 0.9(8) . . . . ? P1 C51 C52 C53 -179.8(4) . . . . ? C51 C52 C53 C54 -0.4(8) . . . . ? C57 O5 C54 C55 -5.4(8) . . . . ? C57 O5 C54 C53 172.7(5) . . . . ? C52 C53 C54 O5 -178.3(5) . . . . ? C52 C53 C54 C55 -0.2(8) . . . . ? O5 C54 C55 C56 178.2(5) . . . . ? C53 C54 C55 C56 0.2(9) . . . . ? C54 C55 C56 C51 0.4(10) . . . . ? C52 C51 C56 C55 -0.9(9) . . . . ? P1 C51 C56 C55 179.8(5) . . . . ? C51 P1 C61 C66 96.6(5) . . . . ? C71 P1 C61 C66 -23.8(5) . . . . ? C81 P1 C61 C66 -144.1(5) . . . . ? C51 P1 C61 C62 -83.3(4) . . . . ? C71 P1 C61 C62 156.3(4) . . . . ? C81 P1 C61 C62 36.0(5) . . . . ? C66 C61 C62 C63 1.0(8) . . . . ? P1 C61 C62 C63 -179.1(4) . . . . ? C61 C62 C63 C64 1.1(8) . . . . ? C62 C63 C64 C65 -2.9(8) . . . . ? C63 C64 C65 C66 2.4(8) . . . . ? C64 C65 C66 C61 -0.3(9) . . . . ? C62 C61 C66 C65 -1.4(8) . . . . ? P1 C61 C66 C65 178.7(4) . . . . ? C51 P1 C71 C76 -167.7(6) . . . . ? C61 P1 C71 C76 -46.8(7) . . . . ? C81 P1 C71 C76 71.3(7) . . . . ? C51 P1 C71 C72 12.8(6) . . . . ? C61 P1 C71 C72 133.7(5) . . . . ? C81 P1 C71 C72 -108.3(6) . . . . ? C76 C71 C72 C73 1.0(11) . . . . ? P1 C71 C72 C73 -179.4(6) . . . . ? C71 C72 C73 C74 0.1(13) . . . . ? C72 C73 C74 C75 -2.6(16) . . . . ? C73 C74 C75 C76 3.9(17) . . . . ? C72 C71 C76 C75 0.2(13) . . . . ? P1 C71 C76 C75 -179.4(7) . . . . ? C74 C75 C76 C71 -2.7(16) . . . . ? C51 P1 C81 C82 5.5(5) . . . . ? C71 P1 C81 C82 126.5(5) . . . . ? C61 P1 C81 C82 -114.4(4) . . . . ? C51 P1 C81 C86 -176.1(5) . . . . ? C71 P1 C81 C86 -55.0(5) . . . . ? C61 P1 C81 C86 64.0(5) . . . . ? C86 C81 C82 C83 2.4(8) . . . . ? P1 C81 C82 C83 -179.1(4) . . . . ? C81 C82 C83 C84 -2.5(9) . . . . ? C82 C83 C84 C85 1.0(10) . . . . ? C83 C84 C85 C86 0.5(11) . . . . ? C84 C85 C86 C81 -0.5(11) . . . . ? C82 C81 C86 C85 -1.0(9) . . . . ? P1 C81 C86 C85 -179.4(5) . . . . ? C4A N1A C2A N2A 0.0 . . . . ? C1A N1A C2A N2A -162.2(18) . . . . ? C4A N1A C2A C13A 179.99(14) . . . . ? C1A N1A C2A C13A 17.8(18) . . . . ? N1A C2A N2A C3A 0.0 . . . . ? C13A C2A N2A C3A -179.99(14) . . . . ? N1A C2A N2A C5A -180.0(4) . . . . ? C13A C2A N2A C5A 0.0(4) . . . . ? C2A N2A C3A C4A 0.0 . . . . ? C5A N2A C3A C4A 180.0(4) . . . . ? C2A N1A C4A C3A 0.0 . . . . ? C1A N1A C4A C3A 161.8(18) . . . . ? N2A C3A C4A N1A 0.0 . . . . ? C3A N2A C5A C6A -60.7(13) . . . . ? C2A N2A C5A C6A 119.2(13) . . . . ? N2A C5A C6A C7A -37(2) . . . . ? C5A C6A C7A C8A -65(3) . . . . ? C6A C7A C8A C9A -52(3) . . . . ? C7A C8A C9A C10A 175(2) . . . . ? C8A C9A C10A C11A -43(4) . . . . ? C9A C10A C11A C12A -4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.340 _refine_diff_density_min -3.057 _refine_diff_density_rms 0.166 # Attachment '- Complex II.cif' data_160808p _database_code_depnum_ccdc_archive 'CCDC 749003' #TrackingRef '- Complex II.cif' # 6. CRYSTALLOGRAPHY _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H20 O16 S, C13 H25 N, Gd H16 O8, 5(H2 O)' _chemical_formula_sum 'C41 H71 Gd N2 O29 S4' _chemical_formula_weight 1341.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.2450(2) _cell_length_b 14.6552(3) _cell_length_c 15.3003(3) _cell_angle_alpha 103.867(2) _cell_angle_beta 100.692(1) _cell_angle_gamma 98.878(1) _cell_volume 2771.10(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 39248 _cell_measurement_theta_min 2.87 _cell_measurement_theta_max 37.1 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method ? _exptl_crystal_F_000 1382 _exptl_absorpt_coefficient_mu 1.438 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.91927 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur-S, Sapphire CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.0009 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63423 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 37.23 _reflns_number_total 27437 _reflns_number_gt 22954 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) ; _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^)+(0.0480P)^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 27437 _refine_ls_number_parameters 701 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0836 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.002 _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 1.027800(5) 0.463821(5) 0.243910(5) 0.01195(2) Uani 1 1 d . . . O01W O 1.14750(10) 0.60513(9) 0.35310(9) 0.0244(3) Uani 1 1 d . . . H01A H 1.1276 0.6469 0.3914 0.037 Uiso 1 1 d . . . H01B H 1.2131 0.6100 0.3721 0.037 Uiso 1 1 d . . . O02W O 1.20431(8) 0.46396(8) 0.21788(8) 0.01454(19) Uani 1 1 d . . . H02A H 1.2557 0.5113 0.2433 0.022 Uiso 1 1 d . . . H02B H 1.2164 0.4316 0.1683 0.022 Uiso 1 1 d . . . O03W O 1.12031(9) 0.39665(9) 0.35510(8) 0.0191(2) Uani 1 1 d . . . H03A H 1.1834 0.4198 0.3856 0.029 Uiso 1 1 d . . . H03B H 1.0853 0.3763 0.3904 0.029 Uiso 1 1 d . . . O04W O 0.93902(10) 0.51435(10) 0.35979(9) 0.0288(3) Uani 1 1 d . . . H04A H 0.9531 0.5626 0.4071 0.043 Uiso 1 1 d . . . H04B H 0.8794 0.4808 0.3567 0.043 Uiso 1 1 d . . . O05W O 1.04764(11) 0.56898(14) 0.15123(14) 0.0504(5) Uani 1 1 d . . . H05A H 1.0032 0.5890 0.1168 0.076 Uiso 1 1 d . . . H05B H 1.1087 0.5999 0.1547 0.076 Uiso 1 1 d . . . O06W O 1.01084(9) 0.34185(8) 0.10596(8) 0.0175(2) Uani 1 1 d . . . H06A H 1.0388 0.3502 0.0620 0.026 Uiso 1 1 d . . . H06B H 0.9548 0.2989 0.0833 0.026 Uiso 1 1 d . . . O07W O 0.90982(8) 0.32241(8) 0.24859(8) 0.0158(2) Uani 1 1 d . . . H07A H 0.9206 0.2869 0.2845 0.024 Uiso 1 1 d . . . H07B H 0.8506 0.2981 0.2109 0.024 Uiso 1 1 d . . . O08W O 0.85462(8) 0.46832(8) 0.15943(8) 0.01572(19) Uani 1 1 d . . . H08A H 0.8300 0.5150 0.1465 0.024 Uiso 1 1 d . . . H08B H 0.8220 0.4170 0.1182 0.024 Uiso 1 1 d . . . O09W O 0.32389(10) 0.46688(9) 0.48206(9) 0.0223(2) Uani 1 1 d . . . H09A H 0.3444 0.5223 0.4757 0.033 Uiso 1 1 d . . . H09B H 0.3756 0.4517 0.5133 0.033 Uiso 1 1 d . . . O10W O 0.23824(10) 0.67088(11) 0.15943(10) 0.0287(3) Uani 1 1 d . . . H10A H 0.2860 0.6534 0.1931 0.043 Uiso 1 1 d . . . H10B H 0.2546 0.6697 0.1081 0.043 Uiso 1 1 d . . . O11W O 0.74999(10) 0.42295(10) 0.36725(10) 0.0268(3) Uani 1 1 d . . . H11A H 0.7307 0.4604 0.4098 0.040 Uiso 1 1 d . . . H11B H 0.7315 0.3657 0.3698 0.040 Uiso 1 1 d . . . O12W O 0.32253(11) 0.76389(10) 0.60800(9) 0.0272(3) Uani 1 1 d . . . H12A H 0.3317 0.7310 0.5573 0.041 Uiso 1 1 d . . . H12B H 0.2849 0.8034 0.5962 0.041 Uiso 1 1 d . . . O13W O 0.1429(5) 0.7904(5) 0.2650(5) 0.0589(16) Uiso 0.33 1 d P A 1 H13A H 0.1672 0.7441 0.2374 0.088 Uiso 0.33 1 d P B 1 H13B H 0.1190 0.8186 0.2256 0.088 Uiso 0.33 1 d P C 1 O14W O 0.1017(5) 0.8870(4) 0.1262(4) 0.0508(14) Uiso 0.33 1 d P D 2 H14A H 0.1220 0.8648 0.1714 0.076 Uiso 0.33 1 d P E 2 H14B H 0.1245 0.8584 0.0810 0.076 Uiso 0.33 1 d P F 2 O15W O 0.1416(5) 0.8324(5) 0.2148(4) 0.0522(14) Uiso 0.33 1 d P G 3 H15A H 0.1686 0.7851 0.1942 0.078 Uiso 0.33 1 d P H 3 H15B H 0.1235 0.8565 0.1705 0.078 Uiso 0.33 1 d P I 3 O1 O 0.63352(9) 1.06044(8) 0.43930(8) 0.0160(2) Uani 1 1 d . . . H1 H 0.6107 1.0807 0.3934 0.024 Uiso 1 1 calc R . . C11 C 0.58193(11) 0.96800(10) 0.42490(10) 0.0121(2) Uani 1 1 d . . . C12 C 0.63281(10) 0.91470(10) 0.47747(9) 0.0117(2) Uani 1 1 d . . . C13 C 0.58537(11) 0.81992(10) 0.46651(10) 0.0122(2) Uani 1 1 d . . . H13 H 0.6186 0.7834 0.5023 0.018 Uiso 1 1 calc R . . C14 C 0.48941(11) 0.77801(10) 0.40343(10) 0.0118(2) Uani 1 1 d . . . C15 C 0.43967(11) 0.83180(11) 0.35213(10) 0.0131(2) Uani 1 1 d . . . H15 H 0.3737 0.8031 0.3100 0.020 Uiso 1 1 calc R . . C16 C 0.48487(11) 0.92697(11) 0.36148(10) 0.0124(2) Uani 1 1 d . . . S1 S 0.43619(3) 0.65510(3) 0.38690(2) 0.01276(6) Uani 1 1 d . . . O11 O 0.35967(10) 0.64963(9) 0.44451(9) 0.0216(2) Uani 1 1 d . . . O12 O 0.38427(9) 0.61595(8) 0.28902(8) 0.0174(2) Uani 1 1 d . . . O13 O 0.52342(10) 0.61212(9) 0.41567(9) 0.0217(2) Uani 1 1 d . . . C1 C 0.74182(11) 0.95616(11) 0.53951(10) 0.0127(2) Uani 1 1 d . . . H11 H 0.7453 0.9378 0.5980 0.015 Uiso 1 1 calc R . . H12 H 0.7548 1.0272 0.5549 0.015 Uiso 1 1 calc R . . O2 O 0.81062(8) 1.01843(8) 0.38696(8) 0.01527(19) Uani 1 1 d . . . H2 H 0.7594 1.0291 0.4113 0.023 Uiso 1 1 calc R . . C21 C 0.85662(10) 0.95439(10) 0.42211(10) 0.0119(2) Uani 1 1 d . . . C22 C 0.93759(10) 0.92409(10) 0.38229(9) 0.0117(2) Uani 1 1 d . . . C23 C 0.99054(11) 0.86069(11) 0.41697(10) 0.0125(2) Uani 1 1 d . . . H23 H 1.0460 0.8399 0.3916 0.015 Uiso 1 1 calc R . . C24 C 0.96222(11) 0.82786(10) 0.48871(10) 0.0121(2) Uani 1 1 d . . . C25 C 0.88012(11) 0.85681(10) 0.52624(10) 0.0123(2) Uani 1 1 d . . . H25 H 0.8604 0.8320 0.5739 0.015 Uiso 1 1 calc R . . C26 C 0.82722(10) 0.92136(10) 0.49461(9) 0.0116(2) Uani 1 1 d . . . S2 S 1.03313(3) 0.75327(3) 0.53725(2) 0.01216(6) Uani 1 1 d . . . O21 O 1.12359(9) 0.74943(9) 0.49588(8) 0.0173(2) Uani 1 1 d . . . O22 O 1.06118(9) 0.79610(8) 0.63716(7) 0.01468(19) Uani 1 1 d . . . O23 O 0.96273(9) 0.65870(8) 0.51283(8) 0.0175(2) Uani 1 1 d . . . C2 C 0.96753(10) 0.96123(11) 0.30429(9) 0.0122(2) Uani 1 1 d . . . H21 H 1.0369 0.9478 0.2969 0.015 Uiso 1 1 calc R . . H22 H 0.9736 1.0317 0.3203 0.015 Uiso 1 1 calc R . . O3 O 0.81264(8) 1.05735(8) 0.21414(7) 0.01407(18) Uani 1 1 d . . . H3 H 0.8563 1.0781 0.2663 0.021 Uiso 1 1 calc R . . C31 C 0.81364(10) 0.96307(10) 0.17599(9) 0.0114(2) Uani 1 1 d . . . C32 C 0.73576(10) 0.91589(10) 0.09517(9) 0.0112(2) Uani 1 1 d . . . C33 C 0.73305(11) 0.82082(10) 0.05074(9) 0.0118(2) Uani 1 1 d . . . H33 H 0.6807 0.7883 -0.0041 0.014 Uiso 1 1 calc R . . C34 C 0.80680(10) 0.77284(10) 0.08613(9) 0.0109(2) Uani 1 1 d . . . C35 C 0.88251(11) 0.81960(10) 0.16701(10) 0.0120(2) Uani 1 1 d . . . H35 H 0.9321 0.7861 0.1910 0.014 Uiso 1 1 calc R . . C36 C 0.88693(10) 0.91485(10) 0.21356(9) 0.0111(2) Uani 1 1 d . . . S3 S 0.79948(3) 0.64971(3) 0.03408(2) 0.01135(6) Uani 1 1 d . . . O31 O 0.73933(9) 0.62886(8) -0.06066(8) 0.0167(2) Uani 1 1 d . . . O32 O 0.90853(8) 0.63812(8) 0.03912(8) 0.01531(19) Uani 1 1 d . . . O33 O 0.74913(9) 0.59682(8) 0.08903(8) 0.0171(2) Uani 1 1 d . . . C3 C 0.65289(11) 0.96770(10) 0.05933(10) 0.0124(2) Uani 1 1 d . . . H31 H 0.6797 1.0379 0.0844 0.015 Uiso 1 1 calc R . . H32 H 0.6400 0.9519 -0.0090 0.015 Uiso 1 1 calc R . . O4 O 0.61388(9) 1.03874(8) 0.24568(8) 0.0170(2) Uani 1 1 d . . . H4 H 0.6688 1.0506 0.2257 0.026 Uiso 1 1 calc R . . C41 C 0.53705(11) 0.97652(10) 0.17651(10) 0.0125(2) Uani 1 1 d . . . C42 C 0.44221(11) 0.94864(10) 0.20122(10) 0.0124(2) Uani 1 1 d . . . C43 C 0.35924(11) 0.88579(11) 0.13407(10) 0.0144(2) Uani 1 1 d . . . H43 H 0.2941 0.8672 0.1492 0.017 Uiso 1 1 calc R . . C44 C 0.37130(11) 0.84992(10) 0.04464(10) 0.0127(2) Uani 1 1 d . . . C45 C 0.46585(11) 0.87627(10) 0.02095(10) 0.0124(2) Uani 1 1 d . . . H45 H 0.4730 0.8503 -0.0402 0.015 Uiso 1 1 calc R . . C46 C 0.55010(10) 0.94044(10) 0.08626(10) 0.0113(2) Uani 1 1 d . . . S4 S 0.26600(3) 0.76633(3) -0.03687(3) 0.01433(6) Uani 1 1 d . . . O41 O 0.28497(9) 0.76162(9) -0.12815(8) 0.0215(2) Uani 1 1 d . . . O42 O 0.26914(10) 0.67467(9) -0.01398(9) 0.0230(2) Uani 1 1 d . . . O43 O 0.17065(9) 0.79939(10) -0.02311(10) 0.0256(3) Uani 1 1 d . . . C4 C 0.43103(11) 0.98159(11) 0.30040(10) 0.0142(2) Uani 1 1 d . . . H41 H 0.4620 1.0511 0.3259 0.017 Uiso 1 1 calc R . . H42 H 0.3555 0.9720 0.3009 0.017 Uiso 1 1 calc R . . N1A N 0.58153(10) 0.68153(10) 0.19431(10) 0.0162(2) Uani 1 1 d . . . N2A N 0.53778(11) 0.52651(10) 0.15597(10) 0.0189(2) Uani 1 1 d . . . C1A C 0.63985(13) 0.77956(12) 0.24011(12) 0.0198(3) Uani 1 1 d . . . H1AA H 0.6985 0.7789 0.2894 0.030 Uiso 1 1 calc R . . H1AB H 0.5931 0.8181 0.2668 0.030 Uiso 1 1 calc R . . H1AC H 0.6672 0.8075 0.1949 0.030 Uiso 1 1 calc R . . C2A C 0.60720(12) 0.60264(12) 0.21347(11) 0.0162(3) Uani 1 1 d . . . C3A C 0.46612(13) 0.55799(13) 0.09839(12) 0.0214(3) Uani 1 1 d . . . H3A H 0.4080 0.5188 0.0512 0.026 Uiso 1 1 calc R . . C4A C 0.49402(13) 0.65433(13) 0.12156(12) 0.0205(3) Uani 1 1 d . . . H4A H 0.4599 0.6959 0.0932 0.025 Uiso 1 1 calc R . . C5A C 0.69880(13) 0.60271(14) 0.28620(12) 0.0218(3) Uani 1 1 d . . . H5A1 H 0.7360 0.6690 0.3178 0.033 Uiso 1 1 calc R . . H5A2 H 0.7465 0.5668 0.2576 0.033 Uiso 1 1 calc R . . H5A3 H 0.6743 0.5723 0.3311 0.033 Uiso 1 1 calc R . . C6A C 0.53517(15) 0.42528(12) 0.15446(14) 0.0241(3) Uani 1 1 d . . . H6A1 H 0.6078 0.4142 0.1637 0.029 Uiso 1 1 calc R . . H6A2 H 0.4950 0.3835 0.0930 0.029 Uiso 1 1 calc R . . C7A C 0.48512(13) 0.39763(12) 0.22908(12) 0.0181(3) Uani 1 1 d . . . H7A1 H 0.5251 0.4392 0.2907 0.022 Uiso 1 1 calc R . . H7A2 H 0.4123 0.4082 0.2199 0.022 Uiso 1 1 calc R . . C8A C 0.48379(14) 0.29281(12) 0.22593(13) 0.0222(3) Uani 1 1 d . . . H8A1 H 0.5566 0.2823 0.2329 0.027 Uiso 1 1 calc R . . H8A2 H 0.4424 0.2517 0.1646 0.027 Uiso 1 1 calc R . . C9A C 0.43694(15) 0.26193(15) 0.30146(14) 0.0277(4) Uani 1 1 d . . . H9A1 H 0.4537 0.1991 0.3047 0.033 Uiso 1 1 calc R . . H9A2 H 0.4716 0.3092 0.3618 0.033 Uiso 1 1 calc R . . C10A C 0.31857(15) 0.25300(15) 0.28757(13) 0.0267(4) Uani 1 1 d . . . H101 H 0.2978 0.2415 0.3436 0.032 Uiso 1 1 calc R . . H102 H 0.3013 0.3149 0.2815 0.032 Uiso 1 1 calc R . . C11A C 0.25395(17) 0.1735(2) 0.20387(17) 0.0414(5) Uani 1 1 d . . . H111 H 0.2762 0.1126 0.2067 0.050 Uiso 1 1 calc R . . H112 H 0.2693 0.1884 0.1473 0.050 Uiso 1 1 calc R . . C12A C 0.13622(18) 0.1589(2) 0.19597(17) 0.0423(6) Uani 1 1 d . . . H121 H 0.1206 0.1385 0.2500 0.051 Uiso 1 1 calc R . . H122 H 0.1154 0.2215 0.1991 0.051 Uiso 1 1 calc R . . C13A C 0.0699(3) 0.0864(4) 0.1092(3) 0.0963(17) Uani 1 1 d . . . H131 H -0.0046 0.0826 0.1095 0.144 Uiso 1 1 calc R . . H132 H 0.0873 0.0233 0.1066 0.144 Uiso 1 1 calc R . . H133 H 0.0838 0.1062 0.0550 0.144 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 0.01017(3) 0.01439(3) 0.01010(3) 0.00310(2) 0.00161(2) 0.00038(2) O01W 0.0201(5) 0.0202(6) 0.0258(6) -0.0060(5) 0.0078(5) 0.0000(4) O02W 0.0124(4) 0.0139(5) 0.0146(5) 0.0001(4) 0.0038(4) -0.0001(3) O03W 0.0135(4) 0.0273(6) 0.0182(5) 0.0117(5) 0.0026(4) 0.0019(4) O04W 0.0188(5) 0.0283(7) 0.0266(7) -0.0138(5) 0.0111(5) -0.0064(5) O05W 0.0152(6) 0.0655(12) 0.0803(13) 0.0633(11) -0.0088(7) -0.0068(6) O06W 0.0153(4) 0.0187(5) 0.0156(5) 0.0007(4) 0.0052(4) -0.0008(4) O07W 0.0150(4) 0.0164(5) 0.0135(5) 0.0065(4) -0.0016(4) -0.0021(4) O08W 0.0142(4) 0.0117(5) 0.0185(5) 0.0028(4) -0.0008(4) 0.0022(4) O09W 0.0204(5) 0.0205(6) 0.0265(6) 0.0108(5) 0.0022(5) 0.0024(4) O10W 0.0205(6) 0.0357(8) 0.0308(7) 0.0209(6) 0.0006(5) -0.0036(5) O11W 0.0246(6) 0.0226(6) 0.0352(7) 0.0077(6) 0.0126(5) 0.0041(5) O12W 0.0313(7) 0.0240(6) 0.0228(6) 0.0020(5) -0.0001(5) 0.0105(5) O1 0.0193(5) 0.0097(4) 0.0171(5) 0.0019(4) 0.0035(4) 0.0009(4) C11 0.0139(5) 0.0102(5) 0.0112(6) 0.0007(4) 0.0035(4) 0.0026(4) C12 0.0111(5) 0.0131(6) 0.0094(5) 0.0012(4) 0.0022(4) 0.0012(4) C13 0.0121(5) 0.0131(6) 0.0110(5) 0.0033(5) 0.0025(4) 0.0019(4) C14 0.0117(5) 0.0120(6) 0.0108(5) 0.0021(4) 0.0026(4) 0.0011(4) C15 0.0120(5) 0.0144(6) 0.0119(6) 0.0022(5) 0.0027(4) 0.0023(4) C16 0.0131(5) 0.0133(6) 0.0107(5) 0.0017(5) 0.0032(4) 0.0042(4) S1 0.01309(13) 0.01202(14) 0.01184(14) 0.00273(12) 0.00268(11) -0.00022(11) O11 0.0236(5) 0.0206(6) 0.0200(6) 0.0036(5) 0.0120(5) -0.0021(4) O12 0.0195(5) 0.0156(5) 0.0124(5) 0.0009(4) 0.0010(4) -0.0019(4) O13 0.0212(5) 0.0149(5) 0.0268(6) 0.0063(5) -0.0006(5) 0.0043(4) C1 0.0123(5) 0.0139(6) 0.0093(5) 0.0010(5) 0.0014(4) 0.0001(4) O2 0.0148(4) 0.0173(5) 0.0157(5) 0.0080(4) 0.0036(4) 0.0037(4) C21 0.0109(5) 0.0117(6) 0.0105(5) 0.0025(4) -0.0006(4) -0.0008(4) C22 0.0108(5) 0.0136(6) 0.0082(5) 0.0019(4) -0.0003(4) -0.0008(4) C23 0.0117(5) 0.0147(6) 0.0097(5) 0.0025(5) 0.0011(4) 0.0013(4) C24 0.0131(5) 0.0124(6) 0.0092(5) 0.0024(4) 0.0010(4) 0.0006(4) C25 0.0126(5) 0.0130(6) 0.0094(5) 0.0024(5) 0.0011(4) 0.0000(4) C26 0.0113(5) 0.0128(6) 0.0081(5) 0.0009(4) 0.0004(4) -0.0001(4) S2 0.01537(14) 0.01044(14) 0.00988(14) 0.00225(11) 0.00234(11) 0.00199(11) O21 0.0177(5) 0.0198(5) 0.0174(5) 0.0062(4) 0.0069(4) 0.0074(4) O22 0.0206(5) 0.0117(5) 0.0094(4) 0.0019(4) -0.0001(4) 0.0022(4) O23 0.0246(5) 0.0112(5) 0.0138(5) 0.0012(4) 0.0046(4) -0.0011(4) C2 0.0102(5) 0.0138(6) 0.0100(5) 0.0032(5) -0.0003(4) -0.0013(4) O3 0.0165(4) 0.0099(4) 0.0122(5) 0.0016(4) -0.0015(4) 0.0000(4) C31 0.0119(5) 0.0108(5) 0.0098(5) 0.0026(4) 0.0009(4) -0.0002(4) C32 0.0112(5) 0.0114(6) 0.0103(5) 0.0037(4) 0.0009(4) 0.0015(4) C33 0.0119(5) 0.0128(6) 0.0090(5) 0.0022(4) 0.0006(4) 0.0017(4) C34 0.0110(5) 0.0122(6) 0.0090(5) 0.0024(4) 0.0022(4) 0.0020(4) C35 0.0117(5) 0.0136(6) 0.0101(5) 0.0036(5) 0.0014(4) 0.0018(4) C36 0.0105(5) 0.0128(6) 0.0084(5) 0.0029(4) 0.0005(4) -0.0006(4) S3 0.01142(13) 0.01182(14) 0.01043(14) 0.00167(11) 0.00261(10) 0.00344(11) O31 0.0171(5) 0.0181(5) 0.0109(5) -0.0013(4) -0.0014(4) 0.0061(4) O32 0.0133(4) 0.0202(5) 0.0144(5) 0.0050(4) 0.0046(4) 0.0073(4) O33 0.0194(5) 0.0141(5) 0.0210(5) 0.0063(4) 0.0096(4) 0.0046(4) C3 0.0127(5) 0.0122(6) 0.0114(6) 0.0041(5) -0.0001(4) 0.0018(4) O4 0.0153(4) 0.0173(5) 0.0125(5) -0.0017(4) 0.0004(4) -0.0014(4) C41 0.0138(5) 0.0103(6) 0.0116(6) 0.0019(5) -0.0002(4) 0.0027(4) C42 0.0137(5) 0.0122(6) 0.0118(6) 0.0033(5) 0.0020(4) 0.0052(4) C43 0.0139(5) 0.0141(6) 0.0148(6) 0.0047(5) 0.0015(5) 0.0024(5) C44 0.0130(5) 0.0105(6) 0.0130(6) 0.0035(5) -0.0005(4) 0.0012(4) C45 0.0138(5) 0.0112(6) 0.0105(5) 0.0029(4) -0.0004(4) 0.0022(4) C46 0.0116(5) 0.0092(5) 0.0117(6) 0.0026(4) -0.0004(4) 0.0027(4) S4 0.01327(14) 0.01278(15) 0.01368(15) 0.00348(12) -0.00179(11) -0.00073(11) O41 0.0202(5) 0.0249(6) 0.0131(5) 0.0040(4) -0.0023(4) -0.0046(4) O42 0.0289(6) 0.0132(5) 0.0204(6) 0.0057(4) -0.0052(5) -0.0033(4) O43 0.0129(5) 0.0246(6) 0.0315(7) -0.0003(5) -0.0009(5) 0.0007(4) C4 0.0162(6) 0.0142(6) 0.0126(6) 0.0026(5) 0.0029(5) 0.0065(5) N1A 0.0169(5) 0.0157(6) 0.0180(6) 0.0060(5) 0.0066(5) 0.0039(4) N2A 0.0222(6) 0.0165(6) 0.0195(6) 0.0050(5) 0.0088(5) 0.0036(5) C1A 0.0238(7) 0.0147(7) 0.0227(8) 0.0048(6) 0.0116(6) 0.0027(5) C2A 0.0181(6) 0.0172(7) 0.0172(7) 0.0068(5) 0.0091(5) 0.0057(5) C3A 0.0188(7) 0.0272(8) 0.0178(7) 0.0066(6) 0.0047(5) 0.0030(6) C4A 0.0187(6) 0.0272(8) 0.0191(7) 0.0099(6) 0.0055(5) 0.0078(6) C5A 0.0194(7) 0.0290(9) 0.0202(7) 0.0100(7) 0.0054(6) 0.0082(6) C6A 0.0326(8) 0.0138(7) 0.0292(9) 0.0045(6) 0.0175(7) 0.0042(6) C7A 0.0194(6) 0.0152(7) 0.0213(7) 0.0060(6) 0.0066(5) 0.0044(5) C8A 0.0223(7) 0.0161(7) 0.0276(8) 0.0058(6) 0.0050(6) 0.0035(6) C9A 0.0278(8) 0.0250(9) 0.0288(9) 0.0133(7) -0.0008(7) 0.0005(7) C10A 0.0297(9) 0.0269(9) 0.0235(8) 0.0109(7) 0.0046(7) 0.0020(7) C11A 0.0282(10) 0.0467(14) 0.0373(12) -0.0020(10) 0.0041(9) -0.0022(9) C12A 0.0313(10) 0.0542(15) 0.0355(12) 0.0105(11) 0.0064(9) -0.0042(10) C13A 0.0423(16) 0.148(4) 0.053(2) -0.021(2) 0.0061(14) -0.034(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Gd1 O04W 2.3425(12) . ? Gd1 O05W 2.3486(14) . ? Gd1 O06W 2.3648(11) . ? Gd1 O03W 2.4013(12) . ? Gd1 O07W 2.4197(11) . ? Gd1 O08W 2.4339(11) . ? Gd1 O01W 2.4369(12) . ? Gd1 O02W 2.4431(10) . ? O01W H01A 0.8500 . ? O01W H01B 0.8500 . ? O02W H02A 0.8500 . ? O02W H02B 0.8500 . ? O03W H03A 0.8500 . ? O03W H03B 0.8500 . ? O04W H04A 0.8500 . ? O04W H04B 0.8501 . ? O05W H05A 0.8500 . ? O05W H05B 0.8500 . ? O06W H06A 0.8500 . ? O06W H06B 0.8500 . ? O07W H07A 0.8500 . ? O07W H07B 0.8500 . ? O08W H08A 0.8500 . ? O08W H08B 0.8500 . ? O09W H09A 0.8499 . ? O09W H09B 0.8501 . ? O10W H10A 0.8500 . ? O10W H10B 0.8500 . ? O11W H11A 0.8500 . ? O11W H11B 0.8500 . ? O12W H12A 0.8500 . ? O12W H12B 0.8500 . ? O13W H13A 0.8500 . ? O13W H13B 0.8501 . ? O13W H15A 1.1830 . ? O14W H14A 0.8499 . ? O14W H14B 0.8499 . ? O14W H15B 0.9249 . ? O15W H13B 0.4160 . ? O15W H14A 0.9272 . ? O15W H15A 0.8499 . ? O15W H15B 0.8500 . ? O1 C11 1.3661(18) . ? O1 H1 0.8501 . ? C11 C12 1.405(2) . ? C11 C16 1.405(2) . ? C12 C13 1.390(2) . ? C12 C1 1.5162(19) . ? C13 C14 1.3942(19) . ? C13 H13 0.9500 . ? C14 C15 1.392(2) . ? C14 S1 1.7690(15) . ? C15 C16 1.392(2) . ? C15 H15 0.9500 . ? C16 C4 1.520(2) . ? S1 O13 1.4471(13) . ? S1 O12 1.4591(12) . ? S1 O11 1.4666(12) . ? C1 C26 1.5199(19) . ? C1 H11 0.9900 . ? C1 H12 0.9900 . ? O2 C21 1.3556(18) . ? O2 H2 0.8501 . ? C21 C26 1.406(2) . ? C21 C22 1.406(2) . ? C22 C23 1.391(2) . ? C22 C2 1.516(2) . ? C23 C24 1.388(2) . ? C23 H23 0.9500 . ? C24 C25 1.3962(19) . ? C24 S2 1.7539(15) . ? C25 C26 1.385(2) . ? C25 H25 0.9500 . ? S2 O21 1.4576(11) . ? S2 O22 1.4580(11) . ? S2 O23 1.4675(12) . ? C2 C36 1.5175(19) . ? C2 H21 0.9900 . ? C2 H22 0.9900 . ? O3 C31 1.3681(17) . ? O3 H3 0.8501 . ? C31 C32 1.4028(19) . ? C31 C36 1.404(2) . ? C32 C33 1.388(2) . ? C32 C3 1.5216(19) . ? C33 C34 1.3929(19) . ? C33 H33 0.9500 . ? C34 C35 1.3883(19) . ? C34 S3 1.7686(14) . ? C35 C36 1.394(2) . ? C35 H35 0.9500 . ? S3 O31 1.4536(11) . ? S3 O33 1.4537(12) . ? S3 O32 1.4703(11) . ? C3 C46 1.5172(19) . ? C3 H31 0.9900 . ? C3 H32 0.9900 . ? O4 C41 1.3559(18) . ? O4 H4 0.8501 . ? C41 C42 1.407(2) . ? C41 C46 1.408(2) . ? C42 C43 1.388(2) . ? C42 C4 1.521(2) . ? C43 C44 1.392(2) . ? C43 H43 0.9500 . ? C44 C45 1.391(2) . ? C44 S4 1.7596(14) . ? C45 C46 1.393(2) . ? C45 H45 0.9500 . ? S4 O41 1.4518(13) . ? S4 O43 1.4536(13) . ? S4 O42 1.4718(13) . ? C4 H41 0.9900 . ? C4 H42 0.9900 . ? N1A C2A 1.336(2) . ? N1A C4A 1.381(2) . ? N1A C1A 1.458(2) . ? N2A C2A 1.333(2) . ? N2A C3A 1.382(2) . ? N2A C6A 1.473(2) . ? C1A H1AA 0.9800 . ? C1A H1AB 0.9800 . ? C1A H1AC 0.9800 . ? C2A C5A 1.486(2) . ? C3A C4A 1.344(3) . ? C3A H3A 0.9500 . ? C4A H4A 0.9500 . ? C5A H5A1 0.9800 . ? C5A H5A2 0.9800 . ? C5A H5A3 0.9800 . ? C6A C7A 1.525(2) . ? C6A H6A1 0.9900 . ? C6A H6A2 0.9900 . ? C7A C8A 1.523(2) . ? C7A H7A1 0.9900 . ? C7A H7A2 0.9900 . ? C8A C9A 1.535(3) . ? C8A H8A1 0.9900 . ? C8A H8A2 0.9900 . ? C9A C10A 1.523(3) . ? C9A H9A1 0.9900 . ? C9A H9A2 0.9900 . ? C10A C11A 1.516(3) . ? C10A H101 0.9900 . ? C10A H102 0.9900 . ? C11A C12A 1.519(3) . ? C11A H111 0.9900 . ? C11A H112 0.9900 . ? C12A C13A 1.505(4) . ? C12A H121 0.9900 . ? C12A H122 0.9900 . ? C13A H131 0.9800 . ? C13A H132 0.9800 . ? C13A H133 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 O04W Gd1 O05W 113.93(7) . . ? O04W Gd1 O06W 141.79(4) . . ? O05W Gd1 O06W 84.62(6) . . ? O04W Gd1 O03W 83.75(5) . . ? O05W Gd1 O03W 144.35(4) . . ? O06W Gd1 O03W 100.35(4) . . ? O04W Gd1 O07W 73.29(4) . . ? O05W Gd1 O07W 140.67(5) . . ? O06W Gd1 O07W 71.93(4) . . ? O03W Gd1 O07W 72.57(4) . . ? O04W Gd1 O08W 75.76(5) . . ? O05W Gd1 O08W 71.28(4) . . ? O06W Gd1 O08W 79.77(4) . . ? O03W Gd1 O08W 144.36(4) . . ? O07W Gd1 O08W 73.73(4) . . ? O04W Gd1 O01W 74.84(4) . . ? O05W Gd1 O01W 77.89(6) . . ? O06W Gd1 O01W 143.31(4) . . ? O03W Gd1 O01W 77.52(5) . . ? O07W Gd1 O01W 138.05(4) . . ? O08W Gd1 O01W 123.06(4) . . ? O04W Gd1 O02W 141.95(4) . . ? O05W Gd1 O02W 75.79(5) . . ? O06W Gd1 O02W 73.03(4) . . ? O03W Gd1 O02W 72.15(4) . . ? O07W Gd1 O02W 123.73(4) . . ? O08W Gd1 O02W 138.78(4) . . ? O01W Gd1 O02W 71.52(4) . . ? Gd1 O01W H01A 123.3 . . ? Gd1 O01W H01B 125.0 . . ? H01A O01W H01B 108.4 . . ? Gd1 O02W H02A 123.1 . . ? Gd1 O02W H02B 123.4 . . ? H02A O02W H02B 108.4 . . ? Gd1 O03W H03A 124.3 . . ? Gd1 O03W H03B 116.2 . . ? H03A O03W H03B 108.4 . . ? Gd1 O04W H04A 133.2 . . ? Gd1 O04W H04B 118.4 . . ? H04A O04W H04B 108.4 . . ? Gd1 O05W H05A 132.1 . . ? Gd1 O05W H05B 119.1 . . ? H05A O05W H05B 108.4 . . ? Gd1 O06W H06A 123.7 . . ? Gd1 O06W H06B 120.7 . . ? H06A O06W H06B 108.4 . . ? Gd1 O07W H07A 127.5 . . ? Gd1 O07W H07B 124.0 . . ? H07A O07W H07B 108.4 . . ? Gd1 O08W H08A 130.6 . . ? Gd1 O08W H08B 115.7 . . ? H08A O08W H08B 108.4 . . ? H09A O09W H09B 108.4 . . ? H10A O10W H10B 108.4 . . ? H11A O11W H11B 108.4 . . ? H12A O12W H12B 108.4 . . ? H13A O13W H13B 108.3 . . ? H13A O13W H15A 55.7 . . ? H13B O13W H15A 56.4 . . ? H14A O14W H14B 107.6 . . ? H14A O14W H15B 6.4 . . ? H14B O14W H15B 102.0 . . ? H13B O15W H14A 120.1 . . ? H13B O15W H15A 99.1 . . ? H14A O15W H15A 113.3 . . ? H13B O15W H15B 120.5 . . ? H14A O15W H15B 6.3 . . ? H15A O15W H15B 107.4 . . ? C11 O1 H1 109.5 . . ? O1 C11 C12 115.57(12) . . ? O1 C11 C16 123.24(13) . . ? C12 C11 C16 121.19(13) . . ? C13 C12 C11 118.99(13) . . ? C13 C12 C1 119.76(13) . . ? C11 C12 C1 121.07(13) . . ? C12 C13 C14 120.50(13) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C15 C14 C13 119.88(13) . . ? C15 C14 S1 121.30(11) . . ? C13 C14 S1 118.76(11) . . ? C14 C15 C16 121.12(13) . . ? C14 C15 H15 119.4 . . ? C16 C15 H15 119.4 . . ? C15 C16 C11 118.31(13) . . ? C15 C16 C4 119.52(13) . . ? C11 C16 C4 122.11(13) . . ? O13 S1 O12 113.60(7) . . ? O13 S1 O11 111.60(8) . . ? O12 S1 O11 110.57(7) . . ? O13 S1 C14 106.46(7) . . ? O12 S1 C14 106.52(7) . . ? O11 S1 C14 107.69(7) . . ? C12 C1 C26 112.44(11) . . ? C12 C1 H11 109.1 . . ? C26 C1 H11 109.1 . . ? C12 C1 H12 109.1 . . ? C26 C1 H12 109.1 . . ? H11 C1 H12 107.8 . . ? C21 O2 H2 109.5 . . ? O2 C21 C26 122.65(13) . . ? O2 C21 C22 115.53(12) . . ? C26 C21 C22 121.81(13) . . ? C23 C22 C21 118.64(13) . . ? C23 C22 C2 120.84(12) . . ? C21 C22 C2 120.51(13) . . ? C24 C23 C22 119.95(13) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 120.85(13) . . ? C23 C24 S2 120.32(11) . . ? C25 C24 S2 118.77(11) . . ? C26 C25 C24 120.66(13) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C21 118.06(13) . . ? C25 C26 C1 120.05(12) . . ? C21 C26 C1 121.87(13) . . ? O21 S2 O22 113.60(7) . . ? O21 S2 O23 111.85(7) . . ? O22 S2 O23 110.91(7) . . ? O21 S2 C24 106.27(7) . . ? O22 S2 C24 106.85(7) . . ? O23 S2 C24 106.89(7) . . ? C22 C2 C36 111.61(11) . . ? C22 C2 H21 109.3 . . ? C36 C2 H21 109.3 . . ? C22 C2 H22 109.3 . . ? C36 C2 H22 109.3 . . ? H21 C2 H22 108.0 . . ? C31 O3 H3 109.5 . . ? O3 C31 C32 115.63(12) . . ? O3 C31 C36 123.39(12) . . ? C32 C31 C36 120.98(13) . . ? C33 C32 C31 119.26(13) . . ? C33 C32 C3 120.73(12) . . ? C31 C32 C3 119.97(12) . . ? C32 C33 C34 120.31(13) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C35 C34 C33 120.03(13) . . ? C35 C34 S3 119.08(11) . . ? C33 C34 S3 120.71(10) . . ? C34 C35 C36 121.04(13) . . ? C34 C35 H35 119.5 . . ? C36 C35 H35 119.5 . . ? C35 C36 C31 118.35(12) . . ? C35 C36 C2 119.06(12) . . ? C31 C36 C2 122.54(13) . . ? O31 S3 O33 113.42(7) . . ? O31 S3 O32 112.47(6) . . ? O33 S3 O32 111.35(7) . . ? O31 S3 C34 106.45(7) . . ? O33 S3 C34 106.46(6) . . ? O32 S3 C34 106.08(7) . . ? C46 C3 C32 112.27(11) . . ? C46 C3 H31 109.2 . . ? C32 C3 H31 109.2 . . ? C46 C3 H32 109.2 . . ? C32 C3 H32 109.2 . . ? H31 C3 H32 107.9 . . ? C41 O4 H4 109.5 . . ? O4 C41 C42 115.24(13) . . ? O4 C41 C46 123.23(13) . . ? C42 C41 C46 121.53(13) . . ? C43 C42 C41 118.81(13) . . ? C43 C42 C4 119.68(13) . . ? C41 C42 C4 121.43(13) . . ? C42 C43 C44 120.07(13) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C45 C44 C43 120.92(13) . . ? C45 C44 S4 120.51(11) . . ? C43 C44 S4 118.51(11) . . ? C44 C45 C46 120.46(13) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? C45 C46 C41 118.19(13) . . ? C45 C46 C3 119.70(13) . . ? C41 C46 C3 122.11(12) . . ? O41 S4 O43 113.71(8) . . ? O41 S4 O42 111.50(8) . . ? O43 S4 O42 111.59(8) . . ? O41 S4 C44 107.65(7) . . ? O43 S4 C44 106.81(7) . . ? O42 S4 C44 105.02(7) . . ? C16 C4 C42 111.90(11) . . ? C16 C4 H41 109.2 . . ? C42 C4 H41 109.2 . . ? C16 C4 H42 109.2 . . ? C42 C4 H42 109.2 . . ? H41 C4 H42 107.9 . . ? C2A N1A C4A 108.74(14) . . ? C2A N1A C1A 125.22(14) . . ? C4A N1A C1A 125.98(14) . . ? C2A N2A C3A 108.73(14) . . ? C2A N2A C6A 126.29(15) . . ? C3A N2A C6A 124.96(15) . . ? N1A C1A H1AA 109.5 . . ? N1A C1A H1AB 109.5 . . ? H1AA C1A H1AB 109.5 . . ? N1A C1A H1AC 109.5 . . ? H1AA C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? N2A C2A N1A 108.12(14) . . ? N2A C2A C5A 127.32(15) . . ? N1A C2A C5A 124.55(15) . . ? C4A C3A N2A 107.25(15) . . ? C4A C3A H3A 126.4 . . ? N2A C3A H3A 126.4 . . ? C3A C4A N1A 107.15(15) . . ? C3A C4A H4A 126.4 . . ? N1A C4A H4A 126.4 . . ? C2A C5A H5A1 109.5 . . ? C2A C5A H5A2 109.5 . . ? H5A1 C5A H5A2 109.5 . . ? C2A C5A H5A3 109.5 . . ? H5A1 C5A H5A3 109.5 . . ? H5A2 C5A H5A3 109.5 . . ? N2A C6A C7A 112.28(13) . . ? N2A C6A H6A1 109.1 . . ? C7A C6A H6A1 109.1 . . ? N2A C6A H6A2 109.1 . . ? C7A C6A H6A2 109.1 . . ? H6A1 C6A H6A2 107.9 . . ? C8A C7A C6A 111.06(14) . . ? C8A C7A H7A1 109.4 . . ? C6A C7A H7A1 109.4 . . ? C8A C7A H7A2 109.4 . . ? C6A C7A H7A2 109.4 . . ? H7A1 C7A H7A2 108.0 . . ? C7A C8A C9A 113.21(15) . . ? C7A C8A H8A1 108.9 . . ? C9A C8A H8A1 108.9 . . ? C7A C8A H8A2 108.9 . . ? C9A C8A H8A2 108.9 . . ? H8A1 C8A H8A2 107.8 . . ? C10A C9A C8A 115.04(15) . . ? C10A C9A H9A1 108.5 . . ? C8A C9A H9A1 108.5 . . ? C10A C9A H9A2 108.5 . . ? C8A C9A H9A2 108.5 . . ? H9A1 C9A H9A2 107.5 . . ? C11A C10A C9A 114.61(18) . . ? C11A C10A H101 108.6 . . ? C9A C10A H101 108.6 . . ? C11A C10A H102 108.6 . . ? C9A C10A H102 108.6 . . ? H101 C10A H102 107.6 . . ? C10A C11A C12A 114.1(2) . . ? C10A C11A H111 108.7 . . ? C12A C11A H111 108.7 . . ? C10A C11A H112 108.7 . . ? C12A C11A H112 108.7 . . ? H111 C11A H112 107.6 . . ? C13A C12A C11A 115.1(2) . . ? C13A C12A H121 108.5 . . ? C11A C12A H121 108.5 . . ? C13A C12A H122 108.5 . . ? C11A C12A H122 108.5 . . ? H121 C12A H122 107.5 . . ? C12A C13A H131 109.5 . . ? C12A C13A H132 109.5 . . ? H131 C13A H132 109.5 . . ? C12A C13A H133 109.5 . . ? H131 C13A H133 109.5 . . ? H132 C13A H133 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 O1 C11 C12 C13 -179.83(12) . . . . ? C16 C11 C12 C13 -0.4(2) . . . . ? O1 C11 C12 C1 -4.88(19) . . . . ? C16 C11 C12 C1 174.54(13) . . . . ? C11 C12 C13 C14 0.8(2) . . . . ? C1 C12 C13 C14 -174.19(13) . . . . ? C12 C13 C14 C15 -1.1(2) . . . . ? C12 C13 C14 S1 176.17(11) . . . . ? C13 C14 C15 C16 1.0(2) . . . . ? S1 C14 C15 C16 -176.21(11) . . . . ? C14 C15 C16 C11 -0.6(2) . . . . ? C14 C15 C16 C4 176.64(12) . . . . ? O1 C11 C16 C15 179.67(13) . . . . ? C12 C11 C16 C15 0.3(2) . . . . ? O1 C11 C16 C4 2.5(2) . . . . ? C12 C11 C16 C4 -176.87(12) . . . . ? C15 C14 S1 O13 154.63(12) . . . . ? C13 C14 S1 O13 -22.64(13) . . . . ? C15 C14 S1 O12 33.09(13) . . . . ? C13 C14 S1 O12 -144.18(11) . . . . ? C15 C14 S1 O11 -85.55(13) . . . . ? C13 C14 S1 O11 97.18(12) . . . . ? C13 C12 C1 C26 75.94(16) . . . . ? C11 C12 C1 C26 -98.98(16) . . . . ? O2 C21 C22 C23 178.01(12) . . . . ? C26 C21 C22 C23 -0.9(2) . . . . ? O2 C21 C22 C2 -0.97(19) . . . . ? C26 C21 C22 C2 -179.88(13) . . . . ? C21 C22 C23 C24 0.7(2) . . . . ? C2 C22 C23 C24 179.71(13) . . . . ? C22 C23 C24 C25 0.7(2) . . . . ? C22 C23 C24 S2 -176.44(11) . . . . ? C23 C24 C25 C26 -2.0(2) . . . . ? S2 C24 C25 C26 175.16(11) . . . . ? C24 C25 C26 C21 1.8(2) . . . . ? C24 C25 C26 C1 -176.84(13) . . . . ? O2 C21 C26 C25 -179.21(13) . . . . ? C22 C21 C26 C25 -0.4(2) . . . . ? O2 C21 C26 C1 -0.6(2) . . . . ? C22 C21 C26 C1 178.26(13) . . . . ? C12 C1 C26 C25 -108.45(15) . . . . ? C12 C1 C26 C21 72.95(17) . . . . ? C23 C24 S2 O21 7.11(14) . . . . ? C25 C24 S2 O21 -170.10(11) . . . . ? C23 C24 S2 O22 128.72(12) . . . . ? C25 C24 S2 O22 -48.49(13) . . . . ? C23 C24 S2 O23 -112.48(12) . . . . ? C25 C24 S2 O23 70.31(13) . . . . ? C23 C22 C2 C36 106.24(15) . . . . ? C21 C22 C2 C36 -74.79(17) . . . . ? O3 C31 C32 C33 178.29(12) . . . . ? C36 C31 C32 C33 -1.6(2) . . . . ? O3 C31 C32 C3 -4.12(18) . . . . ? C36 C31 C32 C3 176.00(12) . . . . ? C31 C32 C33 C34 0.1(2) . . . . ? C3 C32 C33 C34 -177.47(13) . . . . ? C32 C33 C34 C35 1.0(2) . . . . ? C32 C33 C34 S3 176.23(10) . . . . ? C33 C34 C35 C36 -0.6(2) . . . . ? S3 C34 C35 C36 -175.92(10) . . . . ? C34 C35 C36 C31 -0.8(2) . . . . ? C34 C35 C36 C2 176.88(12) . . . . ? O3 C31 C36 C35 -177.93(12) . . . . ? C32 C31 C36 C35 1.9(2) . . . . ? O3 C31 C36 C2 4.4(2) . . . . ? C32 C31 C36 C2 -175.69(12) . . . . ? C22 C2 C36 C35 -73.50(16) . . . . ? C22 C2 C36 C31 104.12(15) . . . . ? C35 C34 S3 O31 -162.30(11) . . . . ? C33 C34 S3 O31 22.43(13) . . . . ? C35 C34 S3 O33 76.40(12) . . . . ? C33 C34 S3 O33 -98.87(12) . . . . ? C35 C34 S3 O32 -42.31(12) . . . . ? C33 C34 S3 O32 142.42(11) . . . . ? C33 C32 C3 C46 78.24(16) . . . . ? C31 C32 C3 C46 -99.30(15) . . . . ? O4 C41 C42 C43 179.37(13) . . . . ? C46 C41 C42 C43 -1.5(2) . . . . ? O4 C41 C42 C4 -3.9(2) . . . . ? C46 C41 C42 C4 175.22(13) . . . . ? C41 C42 C43 C44 1.3(2) . . . . ? C4 C42 C43 C44 -175.45(13) . . . . ? C42 C43 C44 C45 -0.1(2) . . . . ? C42 C43 C44 S4 177.22(11) . . . . ? C43 C44 C45 C46 -1.0(2) . . . . ? S4 C44 C45 C46 -178.24(11) . . . . ? C44 C45 C46 C41 0.8(2) . . . . ? C44 C45 C46 C3 179.50(13) . . . . ? O4 C41 C46 C45 179.51(13) . . . . ? C42 C41 C46 C45 0.4(2) . . . . ? O4 C41 C46 C3 0.8(2) . . . . ? C42 C41 C46 C3 -178.25(13) . . . . ? C32 C3 C46 C45 -102.66(15) . . . . ? C32 C3 C46 C41 76.01(17) . . . . ? C45 C44 S4 O41 -18.95(14) . . . . ? C43 C44 S4 O41 163.70(12) . . . . ? C45 C44 S4 O43 -141.42(13) . . . . ? C43 C44 S4 O43 41.23(14) . . . . ? C45 C44 S4 O42 99.97(13) . . . . ? C43 C44 S4 O42 -77.38(13) . . . . ? C15 C16 C4 C42 -73.35(16) . . . . ? C11 C16 C4 C42 103.80(16) . . . . ? C43 C42 C4 C16 100.69(16) . . . . ? C41 C42 C4 C16 -75.99(17) . . . . ? C3A N2A C2A N1A 0.20(17) . . . . ? C6A N2A C2A N1A -178.48(14) . . . . ? C3A N2A C2A C5A -179.11(15) . . . . ? C6A N2A C2A C5A 2.2(3) . . . . ? C4A N1A C2A N2A -0.86(17) . . . . ? C1A N1A C2A N2A -178.14(14) . . . . ? C4A N1A C2A C5A 178.47(14) . . . . ? C1A N1A C2A C5A 1.2(2) . . . . ? C2A N2A C3A C4A 0.55(18) . . . . ? C6A N2A C3A C4A 179.25(15) . . . . ? N2A C3A C4A N1A -1.05(18) . . . . ? C2A N1A C4A C3A 1.20(18) . . . . ? C1A N1A C4A C3A 178.45(14) . . . . ? C2A N2A C6A C7A 80.0(2) . . . . ? C3A N2A C6A C7A -98.52(19) . . . . ? N2A C6A C7A C8A -179.87(15) . . . . ? C6A C7A C8A C9A 178.39(15) . . . . ? C7A C8A C9A C10A 71.5(2) . . . . ? C8A C9A C10A C11A 65.9(2) . . . . ? C9A C10A C11A C12A 174.3(2) . . . . ? C10A C11A C12A C13A 174.9(3) . . . . ? 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 2.21 2.8604(16) 133.8 . O1 H1 O12W 0.85 2.32 2.8422(18) 120.1 2_676 O2 H2 O1 0.85 1.89 2.7256(16) 166.4 . O3 H3 O22 0.85 2.06 2.7787(15) 141.7 2_776 O3 H3 O2 0.85 2.36 2.8395(15) 116.3 . O4 H4 O3 0.85 1.93 2.7479(16) 159.6 . O01W H01A O21 0.85 1.93 2.7556(17) 163.9 . O01W H01B O11 0.85 1.97 2.7960(18) 163.9 1_655 O02W H02A O12 0.85 1.99 2.8398(15) 172.5 1_655 O02W H02B O31 0.85 1.91 2.7578(15) 172.4 2_765 O03W H03A O09W 0.85 2.05 2.8888(17) 167.5 1_655 O03W H03B O23 0.85 1.86 2.6993(16) 167.2 2_766 O04W H04A O23 0.85 1.84 2.6841(16) 170.6 . O04W H04B O11W 0.85 1.84 2.6871(18) 170.7 . O05W H05A O32 0.85 1.91 2.7568(18) 177.5 . O05W H05B O10W 0.85 1.84 2.6922(19) 177.3 1_655 O06W H06A O32 0.85 1.84 2.6926(15) 175.9 2_765 O06W H06B O43 0.85 1.93 2.7831(16) 176.0 2_665 O07W H07A O22 0.85 1.91 2.7626(15) 177.6 2_766 O07W H07B O41 0.85 1.93 2.7814(16) 177.4 2_665 O08W H08A O33 0.85 1.98 2.8080(16) 165.2 . O08W H08B O42 0.85 1.89 2.7170(16) 164.9 2_665 O09W H09A O11 0.85 2.02 2.8592(18) 167.2 . O09W H09B O13 0.85 2.04 2.8802(17) 167.4 2_666 O10W H10A O12 0.85 2.01 2.8537(18) 170.2 . O10W H10B O42 0.85 1.93 2.7707(19) 169.9 . O11W H11A O09W 0.85 2.06 2.9019(19) 171.6 2_666 O11W H11B O12W 0.85 2.05 2.895(2) 171.5 2_666 O12W H12A O11 0.85 1.98 2.8296(18) 175.7 . O12W H12B O21 0.85 2.29 2.8119(18) 120.3 1_455 O12W H12B O1 0.85 2.35 2.8422(18) 117.5 2_676 _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 35.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.419 _refine_diff_density_min -0.800 _refine_diff_density_rms 0.119