# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2005 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Adina Lazar' 'A.W. Coleman' 'Oksana Danylyuk' 'Kinga Suwinska' _publ_contact_author_name 'Adina Lazar' _publ_contact_author_address ; CNRS Institute de Biologie et Chimie des Proteines (IBCP) 7, Passage du Vercors Lyon Cedex 7 69367 FRANCE ; _publ_contact_author_email A.LAZAR@IBCP.FR _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Assembly Modes in the Solid State Structure of the Complexes of Melamine with para-Sulphonatocalix[4]arene and Calix[4]arene Dihydroxyphosphonic Acid ; data_para-sulphonato_calix[4]arene.melamine _database_code_depnum_ccdc_archive 'CCDC 278967' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H66 N24 O28.50 S4' _chemical_formula_weight 1467.41 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1991(6) _cell_length_b 15.2930(10) _cell_length_c 19.0080(10) _cell_angle_alpha 75.286(4) _cell_angle_beta 86.453(4) _cell_angle_gamma 82.786(3) _cell_volume 3122.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7527 _cell_measurement_theta_min 2.546 _cell_measurement_theta_max 21.967 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.561 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1532 _exptl_absorpt_coefficient_mu 0.258 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method ; 395 frames via \w rotation (rotation angle 0.9\% and 2*369 s per frame) ; _diffrn_detector_area_resol_mean ; 1242 (horizontal) x 1152 (vertical) pixels, CCD pixel size is 22.5 x 22.5 \mm which gives at the input a pixel of 110 x 110 \mm (with 2 x 2 binning) ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27163 _diffrn_reflns_av_R_equivalents 0.0677 _diffrn_reflns_av_sigmaI/netI 0.0920 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 22.02 _reflns_number_total 7510 _reflns_number_gt 5385 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect data collection software (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Johnson & Burnet, 1996)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+3.4921P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom and difmap' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0022(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7510 _refine_ls_number_parameters 896 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1060 _refine_ls_R_factor_gt 0.0690 _refine_ls_wR_factor_ref 0.1598 _refine_ls_wR_factor_gt 0.1476 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _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 S1A S 0.01836(14) 0.12931(11) 0.29158(8) 0.0258(4) Uani 1 1 d . . . S1B S 0.60677(13) -0.04162(11) 0.27108(8) 0.0244(4) Uani 1 1 d . . . S1D S -0.10847(13) -0.30728(11) 0.26607(8) 0.0265(4) Uani 1 1 d . . . S1C S 0.52298(14) -0.50847(11) 0.28651(8) 0.0255(4) Uani 1 1 d . . . O1A O 0.1619(4) -0.1637(3) 0.5486(2) 0.0283(10) Uani 1 1 d . . . H1A H 0.1254 -0.2097 0.5536 0.043 Uiso 1 1 calc R . . O1C O 0.3190(3) -0.3653(3) 0.5337(2) 0.0279(10) Uani 1 1 d . . . H1C H 0.3691 -0.3406 0.5510 0.042 Uiso 1 1 calc R . . O2A O -0.0999(3) 0.1196(3) 0.2682(2) 0.0304(10) Uani 1 1 d . . . O4D O -0.2374(3) -0.2882(3) 0.2727(2) 0.0323(11) Uani 1 1 d . . . O1B O 0.4243(4) -0.2224(3) 0.5618(2) 0.0257(10) Uani 1 1 d . . . H1B H 0.3779 -0.1878 0.5819 0.039 Uiso 1 1 calc R . . O3C O 0.4225(4) -0.5296(3) 0.2504(2) 0.0335(11) Uani 1 1 d . . . O3B O 0.5613(4) -0.0886(3) 0.2212(2) 0.0275(10) Uani 1 1 d . . . O1D O 0.0649(3) -0.3257(3) 0.5572(2) 0.0248(10) Uani 1 1 d . . . H1D H 0.1172 -0.3697 0.5728 0.037 Uiso 1 1 calc R . . O3D O -0.0524(4) -0.2329(3) 0.2154(2) 0.0346(11) Uani 1 1 d . . . O4B O 0.7354(3) -0.0549(3) 0.2759(2) 0.0310(11) Uani 1 1 d . . . O4A O 0.0254(4) 0.2147(3) 0.3103(2) 0.0355(11) Uani 1 1 d . . . O2B O 0.5610(3) 0.0558(3) 0.2521(2) 0.0287(10) Uani 1 1 d . . . O3A O 0.1125(4) 0.1136(3) 0.2368(2) 0.0331(11) Uani 1 1 d . . . O2C O 0.5893(4) -0.4391(3) 0.2384(2) 0.0318(11) Uani 1 1 d . . . O4C O 0.6025(4) -0.5904(3) 0.3183(2) 0.0345(11) Uani 1 1 d . . . O2D O -0.0707(4) -0.3942(3) 0.2467(2) 0.0310(11) Uani 1 1 d . . . N2X N 0.1473(4) 0.0504(4) -0.0121(3) 0.0293(13) Uani 1 1 d . . . N1X N 0.3491(4) 0.0889(3) -0.0082(3) 0.0250(12) Uani 1 1 d . . . N3X N 0.2517(4) 0.0091(3) 0.0968(3) 0.0298(13) Uani 1 1 d . . . H3X H 0.2535 -0.0179 0.1436 0.036 Uiso 1 1 calc R . . C3B C 0.5474(5) -0.0905(4) 0.3579(3) 0.0246(15) Uani 1 1 d . . . C6D C 0.0360(5) -0.3254(4) 0.4876(3) 0.0242(15) Uani 1 1 d . . . N4X N 0.4455(5) 0.0438(3) 0.1004(3) 0.0323(13) Uani 1 1 d . . . H4X1 H 0.5100 0.0685 0.0799 0.039 Uiso 1 1 calc R . . H4X2 H 0.4444 0.0162 0.1470 0.039 Uiso 1 1 calc R . . C1A C 0.0118(5) -0.0966(4) 0.4585(3) 0.0211(14) Uani 1 1 d . . . C1D C 0.0790(5) -0.3935(4) 0.4518(3) 0.0216(14) Uani 1 1 d . . . N5X N 0.2449(5) 0.1264(4) -0.1135(3) 0.0376(14) Uani 1 1 d . . . H5X1 H 0.3076 0.1514 -0.1365 0.045 Uiso 1 1 calc R . . H5X2 H 0.1801 0.1267 -0.1375 0.045 Uiso 1 1 calc R . . C5D C -0.0424(5) -0.2491(4) 0.4533(3) 0.0221(14) Uani 1 1 d . . . C6A C 0.1213(5) -0.0985(4) 0.4893(3) 0.0224(14) Uani 1 1 d . . . C5A C 0.1965(5) -0.0297(4) 0.4631(3) 0.0211(14) Uani 1 1 d . . . C6B C 0.4573(5) -0.1755(4) 0.4938(3) 0.0223(14) Uani 1 1 d . . . C5B C 0.5361(5) -0.2270(4) 0.4549(3) 0.0249(15) Uani 1 1 d . . . C2A C -0.0201(5) -0.0265(4) 0.3970(3) 0.0233(14) Uani 1 1 d . . . H2A H -0.0931 -0.0255 0.3737 0.028 Uiso 1 1 calc R . . C2D C 0.0336(5) -0.3879(4) 0.3848(3) 0.0254(15) Uani 1 1 d . . . H2D H 0.0601 -0.4343 0.3605 0.030 Uiso 1 1 calc R . . C4B C 0.5799(5) -0.1824(4) 0.3871(3) 0.0230(14) Uani 1 1 d . . . H4B H 0.6336 -0.2157 0.3601 0.028 Uiso 1 1 calc R . . C4D C -0.0859(5) -0.2472(4) 0.3864(3) 0.0244(15) Uani 1 1 d . . . H4D H -0.1416 -0.1975 0.3635 0.029 Uiso 1 1 calc R . . C7A C 0.3163(5) -0.0304(4) 0.4977(3) 0.0231(14) Uani 1 1 d . . . H7A1 H 0.3348 0.0328 0.4911 0.028 Uiso 1 1 calc R . . H7A2 H 0.3101 -0.0587 0.5506 0.028 Uiso 1 1 calc R . . C5C C 0.3021(5) -0.4482(4) 0.4479(3) 0.0222(14) Uani 1 1 d . . . C4A C 0.1626(5) 0.0396(4) 0.4030(3) 0.0226(14) Uani 1 1 d . . . H4A H 0.2134 0.0860 0.3841 0.027 Uiso 1 1 calc R . . C3A C 0.0539(5) 0.0417(4) 0.3698(3) 0.0236(15) Uani 1 1 d . . . C1C C 0.4883(5) -0.3813(4) 0.4497(3) 0.0217(14) Uani 1 1 d . . . C6C C 0.3720(5) -0.3970(4) 0.4764(3) 0.0242(15) Uani 1 1 d . . . C7C C 0.1792(5) -0.4699(4) 0.4813(3) 0.0251(15) Uani 1 1 d . . . H7C1 H 0.1814 -0.4798 0.5348 0.030 Uiso 1 1 calc R . . H7C2 H 0.1607 -0.5269 0.4711 0.030 Uiso 1 1 calc R . . C1B C 0.4168(5) -0.0832(4) 0.4634(3) 0.0220(14) Uani 1 1 d . . . C4C C 0.3484(5) -0.4802(4) 0.3879(3) 0.0256(15) Uani 1 1 d . . . H4C H 0.3019 -0.5145 0.3671 0.031 Uiso 1 1 calc R . . C7B C 0.5657(5) -0.3277(4) 0.4831(3) 0.0235(15) Uani 1 1 d . . . H7B1 H 0.5531 -0.3441 0.5367 0.028 Uiso 1 1 calc R . . H7B2 H 0.6517 -0.3448 0.4721 0.028 Uiso 1 1 calc R . . C1X C 0.3506(5) 0.0484(4) 0.0613(4) 0.0278(15) Uani 1 1 d . . . C2X C 0.2483(6) 0.0882(4) -0.0431(3) 0.0299(16) Uani 1 1 d . . . C3X C 0.1514(5) 0.0126(4) 0.0588(4) 0.0295(16) Uani 1 1 d . . . C3C C 0.4609(5) -0.4623(4) 0.3591(3) 0.0230(15) Uani 1 1 d . . . C3D C -0.0493(5) -0.3169(4) 0.3519(3) 0.0233(14) Uani 1 1 d . . . C7D C -0.0734(5) -0.1685(4) 0.4866(3) 0.0231(14) Uani 1 1 d . . . H7D1 H -0.0688 -0.1897 0.5402 0.028 Uiso 1 1 calc R . . H7D2 H -0.1570 -0.1414 0.4749 0.028 Uiso 1 1 calc R . . C2B C 0.4636(5) -0.0421(4) 0.3951(3) 0.0228(14) Uani 1 1 d . . . H2B H 0.4380 0.0201 0.3736 0.027 Uiso 1 1 calc R . . C2C C 0.5323(5) -0.4143(4) 0.3897(3) 0.0222(14) Uani 1 1 d . . . H2C H 0.6108 -0.4039 0.3699 0.027 Uiso 1 1 calc R . . N6X N 0.0573(5) -0.0238(4) 0.0948(3) 0.0383(15) Uani 1 1 d . . . H6X1 H -0.0087 -0.0230 0.0717 0.046 Uiso 1 1 calc R . . H6X2 H 0.0608 -0.0488 0.1418 0.046 Uiso 1 1 calc R . . N3Y N 0.6560(4) 0.1485(3) 0.0299(3) 0.0256(12) Uani 1 1 d . . . N1Y N 0.8522(4) 0.2007(3) 0.0277(3) 0.0261(12) Uani 1 1 d . . . N2Y N 0.7454(4) 0.2260(3) -0.0794(3) 0.0269(12) Uani 1 1 d . . . H2Y H 0.7418 0.2487 -0.1267 0.032 Uiso 1 1 calc R . . N6Y N 0.5572(4) 0.1811(3) -0.0777(3) 0.0299(13) Uani 1 1 d . . . H6Y1 H 0.4955 0.1543 -0.0551 0.036 Uiso 1 1 calc R . . H6Y2 H 0.5558 0.2055 -0.1249 0.036 Uiso 1 1 calc R . . N5Y N 0.9336(4) 0.2708(3) -0.0832(3) 0.0327(13) Uani 1 1 d . . . H5Y1 H 0.9990 0.2766 -0.0622 0.039 Uiso 1 1 calc R . . H5Y2 H 0.9274 0.2911 -0.1306 0.039 Uiso 1 1 calc R . . N4Y N 0.7568(4) 0.1313(3) 0.1340(3) 0.0304(13) Uani 1 1 d . . . H4Y1 H 0.6962 0.1046 0.1582 0.036 Uiso 1 1 calc R . . H4Y2 H 0.8190 0.1381 0.1576 0.036 Uiso 1 1 calc R . . C2Y C 0.8445(5) 0.2315(4) -0.0434(3) 0.0273(15) Uani 1 1 d . . . C1Y C 0.7546(6) 0.1611(4) 0.0628(3) 0.0276(16) Uani 1 1 d . . . C3Y C 0.6510(5) 0.1845(4) -0.0411(4) 0.0283(16) Uani 1 1 d . . . N1W N 0.8515(4) 0.6962(3) 0.0169(3) 0.0253(12) Uani 1 1 d . . . N2Z N 0.7547(4) 0.4773(3) -0.0959(3) 0.0267(12) Uani 1 1 d . . . H2Z H 0.7561 0.4964 -0.1436 0.032 Uiso 1 1 calc R . . N2W N 0.7332(4) 0.7341(3) -0.0868(3) 0.0261(12) Uani 1 1 d . . . H2W H 0.7239 0.7624 -0.1329 0.031 Uiso 1 1 calc R . . N4Z N 0.7495(4) 0.3846(3) 0.1183(3) 0.0278(13) Uani 1 1 d . . . H4Z1 H 0.6865 0.3600 0.1411 0.033 Uiso 1 1 calc R . . H4Z2 H 0.8116 0.3883 0.1432 0.033 Uiso 1 1 calc R . . N1Z N 0.8510(4) 0.4533(3) 0.0146(3) 0.0254(12) Uani 1 1 d . . . N3W N 0.6547(4) 0.6453(3) 0.0219(3) 0.0241(12) Uani 1 1 d . . . N4W N 0.7684(4) 0.6146(3) 0.1222(3) 0.0276(13) Uani 1 1 d . . . H4W1 H 0.7103 0.5851 0.1468 0.033 Uiso 1 1 calc R . . H4W2 H 0.8338 0.6180 0.1443 0.033 Uiso 1 1 calc R . . N5Z N 0.9435(4) 0.5217(3) -0.0934(3) 0.0297(13) Uani 1 1 d . . . H5Z1 H 1.0070 0.5257 -0.0698 0.036 Uiso 1 1 calc R . . H5Z2 H 0.9422 0.5423 -0.1410 0.036 Uiso 1 1 calc R . . N3Z N 0.6535(4) 0.4086(3) 0.0111(3) 0.0248(12) Uani 1 1 d . . . N6W N 0.5488(5) 0.6827(4) -0.0841(3) 0.0334(14) Uani 1 1 d . . . H6W1 H 0.4893 0.6533 -0.0614 0.040 Uiso 1 1 calc R . . H6W2 H 0.5442 0.7101 -0.1307 0.040 Uiso 1 1 calc R . . N6Z N 0.5658(4) 0.4349(3) -0.0990(3) 0.0292(13) Uani 1 1 d . . . H6Z1 H 0.5015 0.4104 -0.0779 0.035 Uiso 1 1 calc R . . H6Z2 H 0.5697 0.4562 -0.1465 0.035 Uiso 1 1 calc R . . N5W N 0.9198(4) 0.7836(3) -0.0916(3) 0.0296(13) Uani 1 1 d . . . H5W1 H 0.9870 0.7867 -0.0712 0.036 Uiso 1 1 calc R . . H5W2 H 0.9089 0.8110 -0.1378 0.036 Uiso 1 1 calc R . . C1W C 0.7577(5) 0.6532(4) 0.0527(3) 0.0236(15) Uani 1 1 d . . . C3Z C 0.6559(5) 0.4395(4) -0.0595(3) 0.0246(15) Uani 1 1 d . . . C2W C 0.8355(6) 0.7378(4) -0.0531(3) 0.0276(15) Uani 1 1 d . . . C3W C 0.6448(5) 0.6858(4) -0.0484(3) 0.0254(15) Uani 1 1 d . . . C2Z C 0.8505(5) 0.4849(4) -0.0574(3) 0.0222(14) Uani 1 1 d . . . C1Z C 0.7511(5) 0.4163(4) 0.0459(3) 0.0256(15) Uani 1 1 d . . . O2W O 0.2583(4) 0.6774(3) 0.2198(2) 0.0440(12) Uani 1 1 d G . . H2WA H 0.2211 0.6078 0.2386 0.066 Uiso 1 1 d G . . H2WB H 0.3115 0.6988 0.2551 0.066 Uiso 1 1 d G . . O3W O 0.8305(4) 0.4510(3) 0.3320(2) 0.0304(10) Uani 1 1 d G . . H3WA H 0.7220 0.4573 0.3267 0.046 Uiso 1 1 d G . . H3WB H 0.8585 0.5227 0.2962 0.046 Uiso 1 1 d G . . O4W O 0.1573(4) 0.5114(3) 0.2357(2) 0.0320(11) Uani 1 1 d G . . H4WA H 0.1541 0.4499 0.2713 0.048 Uiso 1 1 d G . . H4WB H 0.0799 0.5387 0.2412 0.048 Uiso 1 1 d G . . O5W O 0.9416(4) 0.3795(3) 0.2191(2) 0.0296(10) Uani 1 1 d G . . H5WA H 0.9768 0.3101 0.2540 0.044 Uiso 1 1 d G . . H5WB H 0.9016 0.4062 0.2527 0.044 Uiso 1 1 d G . . O6W O 0.5574(4) 0.3002(3) 0.2149(2) 0.0307(10) Uani 1 1 d G . . H6WA H 0.6075 0.2525 0.2479 0.046 Uiso 1 1 d G . . H6WB H 0.5404 0.3458 0.2521 0.046 Uiso 1 1 d G . . O7W O 0.3382(4) 0.1678(3) 0.2247(2) 0.0325(11) Uani 1 1 d G . . H7WA H 0.4009 0.1224 0.2320 0.049 Uiso 1 1 d G . . H7WB H 0.2803 0.1399 0.2411 0.049 Uiso 1 1 d G . . O8W O -0.3291(3) 0.1612(3) 0.3230(2) 0.0294(10) Uani 1 1 d G . . H8WA H -0.3667 0.1128 0.3024 0.044 Uiso 1 1 d G . . H8WB H -0.2499 0.1546 0.3034 0.044 Uiso 1 1 d G . . O9W O 0.5021(4) 0.2594(3) -0.2249(2) 0.0344(11) Uani 1 1 d G . . H9WA H 0.4632 0.2228 -0.2388 0.052 Uiso 1 1 d G . . H9WB H 0.4640 0.3123 -0.2381 0.052 Uiso 1 1 d G . . O10W O -0.0086(4) -0.0703(3) 0.2393(2) 0.0406(12) Uani 1 1 d G . . H10A H -0.0201 -0.1389 0.2499 0.061 Uiso 1 1 d G . . H10B H -0.0948 -0.0234 0.2486 0.061 Uiso 1 1 d G . . O1WA O 0.2561(4) -0.0505(3) 0.2437(3) 0.0358(12) Uiso 0.90 1 d P . . O1WB O 0.2560(9) -0.1397(7) 0.2976(5) 0.026(2) Uiso 0.40 1 d P . . O1WC O 0.3020(17) -0.2223(13) 0.3076(10) 0.023(5) Uiso 0.20 1 d P . . O2WA O 0.1663(4) 0.3664(3) 0.3558(2) 0.0317(12) Uiso 0.90 1 d P . . O2WB O 0.3499(7) 0.2295(5) 0.3583(4) 0.058(2) Uiso 0.70 1 d P . . O2WC O 0.2685(17) 0.2986(13) 0.3582(10) 0.022(5) Uiso 0.20 1 d P . . 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 S1A 0.0213(9) 0.0321(10) 0.0228(9) -0.0039(7) -0.0046(7) -0.0025(7) S1B 0.0180(9) 0.0279(10) 0.0247(9) -0.0027(7) -0.0034(7) 0.0007(7) S1D 0.0206(9) 0.0319(10) 0.0276(9) -0.0093(8) -0.0055(7) 0.0005(7) S1C 0.0213(9) 0.0316(10) 0.0236(9) -0.0067(7) -0.0042(7) -0.0018(7) O1A 0.025(2) 0.030(3) 0.028(2) -0.002(2) -0.008(2) -0.006(2) O1C 0.022(2) 0.037(3) 0.028(2) -0.012(2) -0.003(2) -0.006(2) O2A 0.018(2) 0.041(3) 0.031(2) -0.007(2) -0.0092(19) -0.0002(19) O4D 0.018(2) 0.039(3) 0.040(3) -0.011(2) -0.011(2) 0.003(2) O1B 0.024(2) 0.029(2) 0.022(2) -0.004(2) 0.0003(19) 0.0018(19) O3C 0.030(3) 0.044(3) 0.031(2) -0.013(2) -0.004(2) -0.010(2) O3B 0.030(2) 0.031(3) 0.022(2) -0.0070(19) -0.0043(19) -0.004(2) O1D 0.022(2) 0.027(3) 0.024(2) -0.0053(19) -0.0051(18) 0.0024(18) O3D 0.038(3) 0.043(3) 0.022(2) -0.007(2) -0.003(2) -0.005(2) O4B 0.018(2) 0.037(3) 0.032(2) -0.001(2) 0.0005(19) -0.001(2) O4A 0.039(3) 0.027(3) 0.040(3) -0.004(2) -0.010(2) -0.005(2) O2B 0.023(2) 0.031(3) 0.030(2) -0.002(2) -0.0056(19) -0.0030(19) O3A 0.023(2) 0.045(3) 0.028(2) -0.004(2) 0.001(2) -0.006(2) O2C 0.027(2) 0.040(3) 0.028(2) -0.006(2) 0.003(2) -0.007(2) O4C 0.033(3) 0.041(3) 0.031(3) -0.014(2) -0.007(2) 0.004(2) O2D 0.029(3) 0.030(3) 0.035(3) -0.014(2) -0.007(2) 0.004(2) N2X 0.020(3) 0.043(3) 0.024(3) -0.007(3) -0.002(2) -0.005(3) N1X 0.018(3) 0.034(3) 0.020(3) -0.002(2) -0.006(2) -0.001(2) N3X 0.022(3) 0.037(3) 0.028(3) -0.004(3) -0.009(3) 0.001(3) C3B 0.020(3) 0.032(4) 0.022(3) -0.004(3) -0.007(3) -0.005(3) C6D 0.017(3) 0.039(4) 0.019(3) -0.009(3) 0.004(3) -0.008(3) N4X 0.023(3) 0.042(4) 0.028(3) -0.003(3) 0.000(3) -0.005(3) C1A 0.015(3) 0.024(4) 0.025(3) -0.008(3) 0.002(3) -0.005(3) C1D 0.014(3) 0.029(4) 0.021(3) -0.003(3) -0.003(3) -0.002(3) N5X 0.019(3) 0.061(4) 0.031(4) -0.005(3) -0.002(2) -0.011(3) C5D 0.015(3) 0.028(4) 0.022(3) -0.004(3) 0.001(3) -0.007(3) C6A 0.025(4) 0.022(4) 0.019(3) -0.004(3) -0.002(3) -0.002(3) C5A 0.019(3) 0.027(4) 0.019(3) -0.013(3) -0.006(3) 0.007(3) C6B 0.012(3) 0.035(4) 0.020(3) -0.004(3) -0.001(3) -0.008(3) C5B 0.020(3) 0.032(4) 0.020(4) -0.003(3) -0.005(3) -0.001(3) C2A 0.016(3) 0.033(4) 0.023(3) -0.013(3) -0.001(3) 0.000(3) C2D 0.018(3) 0.034(4) 0.023(4) -0.007(3) 0.006(3) -0.005(3) C4B 0.015(3) 0.029(4) 0.027(4) -0.013(3) -0.006(3) 0.003(3) C4D 0.015(3) 0.028(4) 0.028(4) -0.002(3) -0.007(3) 0.002(3) C7A 0.016(3) 0.032(4) 0.021(3) -0.004(3) -0.005(3) -0.005(3) C5C 0.016(3) 0.027(4) 0.020(3) 0.001(3) -0.003(3) -0.003(3) C4A 0.015(3) 0.027(4) 0.027(4) -0.009(3) 0.001(3) -0.007(3) C3A 0.021(4) 0.029(4) 0.021(3) -0.007(3) 0.004(3) -0.005(3) C1C 0.014(3) 0.022(3) 0.023(3) 0.005(3) -0.004(3) 0.002(3) C6C 0.028(4) 0.025(4) 0.016(3) -0.001(3) -0.004(3) 0.003(3) C7C 0.025(4) 0.024(4) 0.026(3) -0.006(3) -0.005(3) 0.000(3) C1B 0.016(3) 0.026(4) 0.026(4) -0.009(3) -0.008(3) -0.003(3) C4C 0.025(4) 0.019(3) 0.031(4) -0.002(3) -0.010(3) 0.001(3) C7B 0.013(3) 0.025(4) 0.027(3) 0.001(3) 0.000(3) 0.000(3) C1X 0.010(3) 0.036(4) 0.039(4) -0.015(3) -0.001(3) 0.000(3) C2X 0.030(4) 0.034(4) 0.026(4) -0.009(3) -0.006(3) 0.001(3) C3X 0.017(4) 0.033(4) 0.039(4) -0.011(3) -0.003(3) -0.001(3) C3C 0.021(4) 0.023(4) 0.022(3) 0.000(3) 0.000(3) -0.001(3) C3D 0.015(3) 0.029(4) 0.027(3) -0.008(3) -0.002(3) 0.000(3) C7D 0.019(3) 0.031(4) 0.020(3) -0.006(3) -0.006(3) -0.001(3) C2B 0.021(3) 0.020(3) 0.025(4) 0.001(3) -0.007(3) -0.004(3) C2C 0.018(3) 0.022(3) 0.023(3) 0.001(3) 0.001(3) -0.004(3) N6X 0.020(3) 0.059(4) 0.034(3) -0.004(3) -0.001(3) -0.014(3) N3Y 0.022(3) 0.033(3) 0.020(3) -0.004(2) -0.006(2) -0.002(2) N1Y 0.018(3) 0.031(3) 0.027(3) -0.002(2) -0.002(2) -0.004(2) N2Y 0.021(3) 0.035(3) 0.023(3) -0.003(2) -0.005(2) -0.003(2) N6Y 0.018(3) 0.041(3) 0.028(3) -0.001(3) -0.003(3) -0.008(2) N5Y 0.025(3) 0.046(4) 0.028(3) -0.006(3) -0.005(3) -0.011(3) N4Y 0.023(3) 0.046(4) 0.020(3) 0.000(3) -0.001(2) -0.014(3) C2Y 0.021(4) 0.032(4) 0.029(4) -0.007(3) -0.004(3) -0.004(3) C1Y 0.029(4) 0.025(4) 0.028(4) -0.007(3) -0.007(3) 0.004(3) C3Y 0.019(4) 0.028(4) 0.037(4) -0.006(3) -0.006(3) -0.005(3) N1W 0.022(3) 0.027(3) 0.025(3) -0.003(2) -0.001(2) -0.004(2) N2Z 0.026(3) 0.033(3) 0.020(3) -0.002(2) -0.006(3) -0.006(2) N2W 0.020(3) 0.037(3) 0.020(3) 0.000(2) -0.003(2) -0.008(2) N4Z 0.016(3) 0.043(3) 0.024(3) -0.006(3) -0.004(2) -0.009(2) N1Z 0.015(3) 0.037(3) 0.024(3) -0.007(2) 0.000(2) -0.003(2) N3W 0.014(3) 0.035(3) 0.021(3) -0.003(2) -0.003(2) -0.004(2) N4W 0.018(3) 0.035(3) 0.030(3) -0.004(3) 0.000(2) -0.010(2) N5Z 0.023(3) 0.048(4) 0.019(3) -0.004(2) -0.003(2) -0.014(3) N3Z 0.019(3) 0.036(3) 0.019(3) -0.004(2) -0.003(2) -0.003(2) N6W 0.028(3) 0.045(4) 0.026(3) -0.003(3) -0.007(3) -0.010(3) N6Z 0.022(3) 0.043(3) 0.022(3) -0.004(3) -0.001(3) -0.012(3) N5W 0.026(3) 0.037(3) 0.023(3) 0.004(2) -0.008(2) -0.014(3) C1W 0.018(4) 0.032(4) 0.017(4) 0.001(3) -0.003(3) 0.002(3) C3Z 0.017(4) 0.030(4) 0.028(4) -0.007(3) -0.004(3) -0.005(3) C2W 0.026(4) 0.027(4) 0.030(4) -0.006(3) -0.004(3) -0.005(3) C3W 0.018(4) 0.027(4) 0.031(4) -0.008(3) 0.003(3) -0.003(3) C2Z 0.022(4) 0.025(4) 0.020(4) -0.008(3) -0.001(3) 0.000(3) C1Z 0.020(4) 0.027(4) 0.028(4) -0.005(3) -0.001(3) 0.001(3) O2W 0.061(3) 0.043(3) 0.026(3) -0.004(2) -0.004(2) -0.009(2) O3W 0.025(2) 0.038(3) 0.027(2) -0.005(2) -0.005(2) -0.003(2) O4W 0.027(2) 0.041(3) 0.027(2) -0.008(2) -0.004(2) 0.002(2) O5W 0.029(3) 0.036(3) 0.022(2) -0.005(2) -0.003(2) 0.001(2) O6W 0.034(3) 0.034(3) 0.025(2) -0.009(2) -0.003(2) -0.004(2) O7W 0.020(2) 0.039(3) 0.035(3) -0.002(2) -0.001(2) -0.002(2) O8W 0.017(2) 0.041(3) 0.030(2) -0.010(2) -0.0009(19) -0.003(2) O9W 0.032(3) 0.034(3) 0.035(3) -0.003(2) -0.011(2) -0.002(2) O10W 0.040(3) 0.041(3) 0.041(3) -0.011(2) -0.002(2) -0.002(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 S1A O4A 1.450(4) . ? S1A O2A 1.459(4) . ? S1A O3A 1.477(4) . ? S1A C3A 1.758(6) . ? S1B O4B 1.435(4) . ? S1B O3B 1.473(4) . ? S1B O2B 1.474(4) . ? S1B C3B 1.757(6) . ? S1D O4D 1.440(4) . ? S1D O3D 1.471(4) . ? S1D O2D 1.473(4) . ? S1D C3D 1.764(6) . ? S1C O4C 1.460(4) . ? S1C O2C 1.461(4) . ? S1C O3C 1.464(4) . ? S1C C3C 1.770(6) . ? O1A C6A 1.360(7) . ? O1A H1A 0.8400 . ? O1C C6C 1.375(7) . ? O1C H1C 0.8400 . ? O1B C6B 1.364(7) . ? O1B H1B 0.8400 . ? O1D C6D 1.380(7) . ? O1D H1D 0.8400 . ? N2X C3X 1.325(8) . ? N2X C2X 1.367(8) . ? N1X C1X 1.309(8) . ? N1X C2X 1.346(8) . ? N3X C3X 1.361(8) . ? N3X C1X 1.384(8) . ? N3X H3X 0.8800 . ? C3B C4B 1.383(8) . ? C3B C2B 1.393(8) . ? C6D C1D 1.404(8) . ? C6D C5D 1.408(8) . ? N4X C1X 1.319(8) . ? N4X H4X1 0.8800 . ? N4X H4X2 0.8800 . ? C1A C6A 1.386(8) . ? C1A C2A 1.400(8) . ? C1A C7D 1.518(8) . ? C1D C2D 1.380(8) . ? C1D C7C 1.535(8) . ? N5X C2X 1.318(8) . ? N5X H5X1 0.8800 . ? N5X H5X2 0.8800 . ? C5D C4D 1.382(8) . ? C5D C7D 1.518(8) . ? C6A C5A 1.404(8) . ? C5A C4A 1.381(8) . ? C5A C7A 1.527(8) . ? C6B C5B 1.409(8) . ? C6B C1B 1.411(8) . ? C5B C4B 1.388(8) . ? C5B C7B 1.498(8) . ? C2A C3A 1.391(8) . ? C2A H2A 0.9500 . ? C2D C3D 1.380(8) . ? C2D H2D 0.9500 . ? C4B H4B 0.9500 . ? C4D C3D 1.394(8) . ? C4D H4D 0.9500 . ? C7A C1B 1.514(8) . ? C7A H7A1 0.9900 . ? C7A H7A2 0.9900 . ? C5C C6C 1.394(8) . ? C5C C4C 1.398(8) . ? C5C C7C 1.518(8) . ? C4A C3A 1.399(8) . ? C4A H4A 0.9500 . ? C1C C6C 1.395(8) . ? C1C C2C 1.399(8) . ? C1C C7B 1.529(8) . ? C7C H7C1 0.9900 . ? C7C H7C2 0.9900 . ? C1B C2B 1.392(8) . ? C4C C3C 1.374(8) . ? C4C H4C 0.9500 . ? C7B H7B1 0.9900 . ? C7B H7B2 0.9900 . ? C3X N6X 1.324(8) . ? C3C C2C 1.394(8) . ? C7D H7D1 0.9900 . ? C7D H7D2 0.9900 . ? C2B H2B 0.9500 . ? C2C H2C 0.9500 . ? N6X H6X1 0.8800 . ? N6X H6X2 0.8800 . ? N3Y C3Y 1.323(8) . ? N3Y C1Y 1.359(8) . ? N1Y C2Y 1.319(8) . ? N1Y C1Y 1.369(8) . ? N2Y C2Y 1.361(8) . ? N2Y C3Y 1.374(8) . ? N2Y H2Y 0.8800 . ? N6Y C3Y 1.309(8) . ? N6Y H6Y1 0.8800 . ? N6Y H6Y2 0.8800 . ? N5Y C2Y 1.324(8) . ? N5Y H5Y1 0.8800 . ? N5Y H5Y2 0.8800 . ? N4Y C1Y 1.316(8) . ? N4Y H4Y1 0.8800 . ? N4Y H4Y2 0.8800 . ? N1W C2W 1.333(8) . ? N1W C1W 1.362(7) . ? N2Z C2Z 1.368(7) . ? N2Z C3Z 1.378(7) . ? N2Z H2Z 0.8800 . ? N2W C2W 1.362(8) . ? N2W C3W 1.371(7) . ? N2W H2W 0.8800 . ? N4Z C1Z 1.337(8) . ? N4Z H4Z1 0.8800 . ? N4Z H4Z2 0.8800 . ? N1Z C2Z 1.331(7) . ? N1Z C1Z 1.353(7) . ? N3W C3W 1.328(8) . ? N3W C1W 1.357(8) . ? N4W C1W 1.310(7) . ? N4W H4W1 0.8800 . ? N4W H4W2 0.8800 . ? N5Z C2Z 1.316(7) . ? N5Z H5Z1 0.8800 . ? N5Z H5Z2 0.8800 . ? N3Z C3Z 1.304(8) . ? N3Z C1Z 1.345(8) . ? N6W C3W 1.319(8) . ? N6W H6W1 0.8800 . ? N6W H6W2 0.8800 . ? N6Z C3Z 1.314(7) . ? N6Z H6Z1 0.8800 . ? N6Z H6Z2 0.8800 . ? N5W C2W 1.318(7) . ? N5W H5W1 0.8800 . ? N5W H5W2 0.8800 . ? O2W H2WA 1.1549 . ? O2W H2WB 1.0587 . ? O3W H3WA 1.2158 . ? O3W H3WB 1.2026 . ? O4W H4WA 1.0123 . ? O4W H4WB 0.9252 . ? O5W H5WA 1.1355 . ? O5W H5WB 0.9101 . ? O6W H6WA 0.9741 . ? O6W H6WB 1.1054 . ? O7W H7WA 0.9146 . ? O7W H7WB 0.8225 . ? O8W H8WA 1.0602 . ? O8W H8WB 0.9439 . ? O9W H9WA 0.8500 . ? O9W H9WB 0.8500 . ? O10W H10A 1.0406 . ? O10W H10B 1.1600 . ? O1WA O1WB 1.483(11) . ? O1WB O1WC 1.27(2) . ? O2WA O2WC 1.439(19) . ? O2WB O2WC 1.307(18) . ? 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 O4A S1A O2A 114.2(3) . . ? O4A S1A O3A 111.3(3) . . ? O2A S1A O3A 110.5(2) . . ? O4A S1A C3A 107.1(3) . . ? O2A S1A C3A 108.5(3) . . ? O3A S1A C3A 104.7(3) . . ? O4B S1B O3B 113.6(2) . . ? O4B S1B O2B 111.5(2) . . ? O3B S1B O2B 110.7(2) . . ? O4B S1B C3B 106.9(3) . . ? O3B S1B C3B 106.0(3) . . ? O2B S1B C3B 107.8(3) . . ? O4D S1D O3D 112.9(3) . . ? O4D S1D O2D 112.8(3) . . ? O3D S1D O2D 110.4(2) . . ? O4D S1D C3D 107.6(3) . . ? O3D S1D C3D 105.8(3) . . ? O2D S1D C3D 106.9(3) . . ? O4C S1C O2C 111.7(3) . . ? O4C S1C O3C 111.5(3) . . ? O2C S1C O3C 112.2(3) . . ? O4C S1C C3C 107.1(3) . . ? O2C S1C C3C 106.8(3) . . ? O3C S1C C3C 107.2(3) . . ? C6A O1A H1A 109.5 . . ? C6C O1C H1C 109.5 . . ? C6B O1B H1B 109.5 . . ? C6D O1D H1D 109.5 . . ? C3X N2X C2X 115.4(5) . . ? C1X N1X C2X 116.7(5) . . ? C3X N3X C1X 119.4(5) . . ? C3X N3X H3X 120.3 . . ? C1X N3X H3X 120.3 . . ? C4B C3B C2B 119.7(5) . . ? C4B C3B S1B 117.7(4) . . ? C2B C3B S1B 122.5(5) . . ? O1D C6D C1D 124.8(5) . . ? O1D C6D C5D 114.2(5) . . ? C1D C6D C5D 121.1(5) . . ? C1X N4X H4X1 120.0 . . ? C1X N4X H4X2 120.0 . . ? H4X1 N4X H4X2 120.0 . . ? C6A C1A C2A 118.3(5) . . ? C6A C1A C7D 123.2(5) . . ? C2A C1A C7D 118.5(5) . . ? C2D C1D C6D 118.0(5) . . ? C2D C1D C7C 118.6(5) . . ? C6D C1D C7C 123.3(5) . . ? C2X N5X H5X1 120.0 . . ? C2X N5X H5X2 120.0 . . ? H5X1 N5X H5X2 120.0 . . ? C4D C5D C6D 118.4(5) . . ? C4D C5D C7D 120.4(5) . . ? C6D C5D C7D 121.2(5) . . ? O1A C6A C1A 123.4(5) . . ? O1A C6A C5A 114.8(5) . . ? C1A C6A C5A 121.7(5) . . ? C4A C5A C6A 119.0(5) . . ? C4A C5A C7A 119.0(5) . . ? C6A C5A C7A 122.0(5) . . ? O1B C6B C5B 114.5(5) . . ? O1B C6B C1B 123.8(5) . . ? C5B C6B C1B 121.7(5) . . ? C4B C5B C6B 117.8(5) . . ? C4B C5B C7B 120.6(5) . . ? C6B C5B C7B 121.4(5) . . ? C3A C2A C1A 120.7(6) . . ? C3A C2A H2A 119.7 . . ? C1A C2A H2A 119.7 . . ? C3D C2D C1D 122.0(6) . . ? C3D C2D H2D 119.0 . . ? C1D C2D H2D 119.0 . . ? C3B C4B C5B 121.7(5) . . ? C3B C4B H4B 119.2 . . ? C5B C4B H4B 119.2 . . ? C5D C4D C3D 121.1(5) . . ? C5D C4D H4D 119.5 . . ? C3D C4D H4D 119.5 . . ? C1B C7A C5A 110.6(5) . . ? C1B C7A H7A1 109.5 . . ? C5A C7A H7A1 109.5 . . ? C1B C7A H7A2 109.5 . . ? C5A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 108.1 . . ? C6C C5C C4C 118.3(5) . . ? C6C C5C C7C 121.1(5) . . ? C4C C5C C7C 120.6(5) . . ? C5A C4A C3A 120.3(6) . . ? C5A C4A H4A 119.8 . . ? C3A C4A H4A 119.8 . . ? C2A C3A C4A 119.9(6) . . ? C2A C3A S1A 121.9(5) . . ? C4A C3A S1A 118.2(4) . . ? C6C C1C C2C 118.2(6) . . ? C6C C1C C7B 121.6(5) . . ? C2C C1C C7B 120.2(5) . . ? O1C C6C C5C 115.1(5) . . ? O1C C6C C1C 122.8(5) . . ? C5C C6C C1C 122.1(5) . . ? C5C C7C C1D 112.3(5) . . ? C5C C7C H7C1 109.1 . . ? C1D C7C H7C1 109.1 . . ? C5C C7C H7C2 109.1 . . ? C1D C7C H7C2 109.1 . . ? H7C1 C7C H7C2 107.9 . . ? C2B C1B C6B 117.8(5) . . ? C2B C1B C7A 118.8(5) . . ? C6B C1B C7A 123.1(5) . . ? C3C C4C C5C 120.3(6) . . ? C3C C4C H4C 119.9 . . ? C5C C4C H4C 119.9 . . ? C5B C7B C1C 112.1(5) . . ? C5B C7B H7B1 109.2 . . ? C1C C7B H7B1 109.2 . . ? C5B C7B H7B2 109.2 . . ? C1C C7B H7B2 109.2 . . ? H7B1 C7B H7B2 107.9 . . ? N1X C1X N4X 121.7(6) . . ? N1X C1X N3X 121.0(6) . . ? N4X C1X N3X 117.3(6) . . ? N5X C2X N1X 118.3(6) . . ? N5X C2X N2X 115.9(6) . . ? N1X C2X N2X 125.8(6) . . ? N6X C3X N2X 120.6(6) . . ? N6X C3X N3X 117.8(6) . . ? N2X C3X N3X 121.6(6) . . ? C4C C3C C2C 121.1(5) . . ? C4C C3C S1C 120.2(5) . . ? C2C C3C S1C 118.5(4) . . ? C2D C3D C4D 119.2(6) . . ? C2D C3D S1D 123.2(5) . . ? C4D C3D S1D 117.6(4) . . ? C5D C7D C1A 111.5(5) . . ? C5D C7D H7D1 109.3 . . ? C1A C7D H7D1 109.3 . . ? C5D C7D H7D2 109.3 . . ? C1A C7D H7D2 109.3 . . ? H7D1 C7D H7D2 108.0 . . ? C1B C2B C3B 121.1(5) . . ? C1B C2B H2B 119.4 . . ? C3B C2B H2B 119.4 . . ? C3C C2C C1C 119.9(5) . . ? C3C C2C H2C 120.1 . . ? C1C C2C H2C 120.1 . . ? C3X N6X H6X1 120.0 . . ? C3X N6X H6X2 120.0 . . ? H6X1 N6X H6X2 120.0 . . ? C3Y N3Y C1Y 116.3(5) . . ? C2Y N1Y C1Y 115.4(5) . . ? C2Y N2Y C3Y 119.4(5) . . ? C2Y N2Y H2Y 120.3 . . ? C3Y N2Y H2Y 120.3 . . ? C3Y N6Y H6Y1 120.0 . . ? C3Y N6Y H6Y2 120.0 . . ? H6Y1 N6Y H6Y2 120.0 . . ? C2Y N5Y H5Y1 120.0 . . ? C2Y N5Y H5Y2 120.0 . . ? H5Y1 N5Y H5Y2 120.0 . . ? C1Y N4Y H4Y1 120.0 . . ? C1Y N4Y H4Y2 120.0 . . ? H4Y1 N4Y H4Y2 120.0 . . ? N1Y C2Y N5Y 120.9(6) . . ? N1Y C2Y N2Y 122.3(6) . . ? N5Y C2Y N2Y 116.8(6) . . ? N4Y C1Y N3Y 117.0(6) . . ? N4Y C1Y N1Y 117.7(6) . . ? N3Y C1Y N1Y 125.3(5) . . ? N6Y C3Y N3Y 121.5(6) . . ? N6Y C3Y N2Y 117.4(6) . . ? N3Y C3Y N2Y 121.0(6) . . ? C2W N1W C1W 115.9(5) . . ? C2Z N2Z C3Z 119.6(5) . . ? C2Z N2Z H2Z 120.2 . . ? C3Z N2Z H2Z 120.2 . . ? C2W N2W C3W 119.5(5) . . ? C2W N2W H2W 120.2 . . ? C3W N2W H2W 120.2 . . ? C1Z N4Z H4Z1 120.0 . . ? C1Z N4Z H4Z2 120.0 . . ? H4Z1 N4Z H4Z2 120.0 . . ? C2Z N1Z C1Z 115.8(5) . . ? C3W N3W C1W 116.2(5) . . ? C1W N4W H4W1 120.0 . . ? C1W N4W H4W2 120.0 . . ? H4W1 N4W H4W2 120.0 . . ? C2Z N5Z H5Z1 120.0 . . ? C2Z N5Z H5Z2 120.0 . . ? H5Z1 N5Z H5Z2 120.0 . . ? C3Z N3Z C1Z 116.7(5) . . ? C3W N6W H6W1 120.0 . . ? C3W N6W H6W2 120.0 . . ? H6W1 N6W H6W2 120.0 . . ? C3Z N6Z H6Z1 120.0 . . ? C3Z N6Z H6Z2 120.0 . . ? H6Z1 N6Z H6Z2 120.0 . . ? C2W N5W H5W1 120.0 . . ? C2W N5W H5W2 120.0 . . ? H5W1 N5W H5W2 120.0 . . ? N4W C1W N3W 117.0(5) . . ? N4W C1W N1W 117.5(5) . . ? N3W C1W N1W 125.4(5) . . ? N3Z C3Z N6Z 121.8(6) . . ? N3Z C3Z N2Z 121.0(6) . . ? N6Z C3Z N2Z 117.2(5) . . ? N5W C2W N1W 120.3(6) . . ? N5W C2W N2W 118.2(6) . . ? N1W C2W N2W 121.5(6) . . ? N6W C3W N3W 121.6(5) . . ? N6W C3W N2W 117.0(6) . . ? N3W C3W N2W 121.4(6) . . ? N5Z C2Z N1Z 120.8(5) . . ? N5Z C2Z N2Z 118.5(5) . . ? N1Z C2Z N2Z 120.7(5) . . ? N4Z C1Z N3Z 117.2(5) . . ? N4Z C1Z N1Z 116.8(5) . . ? N3Z C1Z N1Z 126.1(5) . . ? H2WA O2W H2WB 119.9 . . ? H3WA O3W H3WB 104.4 . . ? H4WA O4W H4WB 101.2 . . ? H5WA O5W H5WB 101.9 . . ? H6WA O6W H6WB 95.7 . . ? H7WA O7W H7WB 102.2 . . ? H8WA O8W H8WB 99.4 . . ? H9WA O9W H9WB 107.7 . . ? H10A O10W H10B 114.5 . . ? O1WC O1WB O1WA 140.9(11) . . ? O2WB O2WC O2WA 171.4(16) . . ? 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 O4B S1B C3B C4B -59.4(5) . . . . ? O3B S1B C3B C4B 62.1(5) . . . . ? O2B S1B C3B C4B -179.3(4) . . . . ? O4B S1B C3B C2B 125.1(5) . . . . ? O3B S1B C3B C2B -113.4(5) . . . . ? O2B S1B C3B C2B 5.2(6) . . . . ? O1D C6D C1D C2D 174.3(5) . . . . ? C5D C6D C1D C2D -5.9(8) . . . . ? O1D C6D C1D C7C -9.7(9) . . . . ? C5D C6D C1D C7C 170.1(5) . . . . ? O1D C6D C5D C4D -173.7(5) . . . . ? C1D C6D C5D C4D 6.4(8) . . . . ? O1D C6D C5D C7D 9.6(8) . . . . ? C1D C6D C5D C7D -170.2(5) . . . . ? C2A C1A C6A O1A -179.5(5) . . . . ? C7D C1A C6A O1A -1.5(9) . . . . ? C2A C1A C6A C5A 3.6(8) . . . . ? C7D C1A C6A C5A -178.3(5) . . . . ? O1A C6A C5A C4A -179.9(5) . . . . ? C1A C6A C5A C4A -2.8(8) . . . . ? O1A C6A C5A C7A 1.8(8) . . . . ? C1A C6A C5A C7A 178.9(5) . . . . ? O1B C6B C5B C4B -175.9(5) . . . . ? C1B C6B C5B C4B 4.5(9) . . . . ? O1B C6B C5B C7B 8.0(8) . . . . ? C1B C6B C5B C7B -171.6(5) . . . . ? C6A C1A C2A C3A -2.8(8) . . . . ? C7D C1A C2A C3A 179.0(5) . . . . ? C6D C1D C2D C3D 1.7(8) . . . . ? C7C C1D C2D C3D -174.5(5) . . . . ? C2B C3B C4B C5B -3.5(9) . . . . ? S1B C3B C4B C5B -179.1(5) . . . . ? C6B C5B C4B C3B -0.5(9) . . . . ? C7B C5B C4B C3B 175.6(5) . . . . ? C6D C5D C4D C3D -2.8(8) . . . . ? C7D C5D C4D C3D 173.9(5) . . . . ? C4A C5A C7A C1B -89.9(6) . . . . ? C6A C5A C7A C1B 88.3(6) . . . . ? C6A C5A C4A C3A 1.2(8) . . . . ? C7A C5A C4A C3A 179.5(5) . . . . ? C1A C2A C3A C4A 1.3(8) . . . . ? C1A C2A C3A S1A 178.5(4) . . . . ? C5A C4A C3A C2A -0.4(8) . . . . ? C5A C4A C3A S1A -177.8(4) . . . . ? O4A S1A C3A C2A 128.3(5) . . . . ? O2A S1A C3A C2A 4.6(5) . . . . ? O3A S1A C3A C2A -113.4(5) . . . . ? O4A S1A C3A C4A -54.4(5) . . . . ? O2A S1A C3A C4A -178.1(4) . . . . ? O3A S1A C3A C4A 63.9(5) . . . . ? C4C C5C C6C O1C 177.9(5) . . . . ? C7C C5C C6C O1C -2.8(8) . . . . ? C4C C5C C6C C1C -3.6(8) . . . . ? C7C C5C C6C C1C 175.7(5) . . . . ? C2C C1C C6C O1C -178.1(5) . . . . ? C7B C1C C6C O1C 0.4(8) . . . . ? C2C C1C C6C C5C 3.6(8) . . . . ? C7B C1C C6C C5C -177.9(5) . . . . ? C6C C5C C7C C1D 85.2(7) . . . . ? C4C C5C C7C C1D -95.5(6) . . . . ? C2D C1D C7C C5C 79.7(7) . . . . ? C6D C1D C7C C5C -96.3(7) . . . . ? O1B C6B C1B C2B 176.0(5) . . . . ? C5B C6B C1B C2B -4.4(8) . . . . ? O1B C6B C1B C7A -10.6(9) . . . . ? C5B C6B C1B C7A 169.0(5) . . . . ? C5A C7A C1B C2B 77.1(7) . . . . ? C5A C7A C1B C6B -96.2(6) . . . . ? C6C C5C C4C C3C 1.0(8) . . . . ? C7C C5C C4C C3C -178.4(5) . . . . ? C4B C5B C7B C1C -78.9(7) . . . . ? C6B C5B C7B C1C 97.0(6) . . . . ? C6C C1C C7B C5B -82.2(7) . . . . ? C2C C1C C7B C5B 96.4(6) . . . . ? C2X N1X C1X N4X 178.9(5) . . . . ? C2X N1X C1X N3X -1.7(8) . . . . ? C3X N3X C1X N1X 0.2(8) . . . . ? C3X N3X C1X N4X 179.6(5) . . . . ? C1X N1X C2X N5X -178.2(6) . . . . ? C1X N1X C2X N2X 1.2(9) . . . . ? C3X N2X C2X N5X -179.7(6) . . . . ? C3X N2X C2X N1X 0.8(9) . . . . ? C2X N2X C3X N6X 178.1(6) . . . . ? C2X N2X C3X N3X -2.3(8) . . . . ? C1X N3X C3X N6X -178.4(5) . . . . ? C1X N3X C3X N2X 2.0(9) . . . . ? C5C C4C C3C C2C 1.7(9) . . . . ? C5C C4C C3C S1C 176.3(4) . . . . ? O4C S1C C3C C4C -97.5(5) . . . . ? O2C S1C C3C C4C 142.8(5) . . . . ? O3C S1C C3C C4C 22.3(5) . . . . ? O4C S1C C3C C2C 77.3(5) . . . . ? O2C S1C C3C C2C -42.4(5) . . . . ? O3C S1C C3C C2C -162.9(4) . . . . ? C1D C2D C3D C4D 1.8(9) . . . . ? C1D C2D C3D S1D 179.6(4) . . . . ? C5D C4D C3D C2D -1.3(9) . . . . ? C5D C4D C3D S1D -179.2(4) . . . . ? O4D S1D C3D C2D 131.7(5) . . . . ? O3D S1D C3D C2D -107.4(5) . . . . ? O2D S1D C3D C2D 10.3(6) . . . . ? O4D S1D C3D C4D -50.5(5) . . . . ? O3D S1D C3D C4D 70.4(5) . . . . ? O2D S1D C3D C4D -171.9(4) . . . . ? C4D C5D C7D C1A -84.7(7) . . . . ? C6D C5D C7D C1A 91.9(6) . . . . ? C6A C1A C7D C5D -86.3(7) . . . . ? C2A C1A C7D C5D 91.7(6) . . . . ? C6B C1B C2B C3B 0.3(8) . . . . ? C7A C1B C2B C3B -173.4(5) . . . . ? C4B C3B C2B C1B 3.6(9) . . . . ? S1B C3B C2B C1B 179.0(5) . . . . ? C4C C3C C2C C1C -1.8(9) . . . . ? S1C C3C C2C C1C -176.5(4) . . . . ? C6C C1C C2C C3C -0.8(8) . . . . ? C7B C1C C2C C3C -179.4(5) . . . . ? C1Y N1Y C2Y N5Y -179.7(5) . . . . ? C1Y N1Y C2Y N2Y 1.2(8) . . . . ? C3Y N2Y C2Y N1Y -2.0(9) . . . . ? C3Y N2Y C2Y N5Y 178.9(5) . . . . ? C3Y N3Y C1Y N4Y 175.3(5) . . . . ? C3Y N3Y C1Y N1Y -5.9(9) . . . . ? C2Y N1Y C1Y N4Y -178.3(5) . . . . ? C2Y N1Y C1Y N3Y 2.8(8) . . . . ? C1Y N3Y C3Y N6Y -176.1(5) . . . . ? C1Y N3Y C3Y N2Y 4.9(8) . . . . ? C2Y N2Y C3Y N6Y 179.6(5) . . . . ? C2Y N2Y C3Y N3Y -1.3(9) . . . . ? C3W N3W C1W N4W 179.2(5) . . . . ? C3W N3W C1W N1W -2.3(8) . . . . ? C2W N1W C1W N4W -177.4(5) . . . . ? C2W N1W C1W N3W 4.1(8) . . . . ? C1Z N3Z C3Z N6Z 179.5(5) . . . . ? C1Z N3Z C3Z N2Z 0.6(8) . . . . ? C2Z N2Z C3Z N3Z -1.8(8) . . . . ? C2Z N2Z C3Z N6Z 179.2(5) . . . . ? C1W N1W C2W N5W 177.9(5) . . . . ? C1W N1W C2W N2W -2.5(8) . . . . ? C3W N2W C2W N5W 179.0(5) . . . . ? C3W N2W C2W N1W -0.6(9) . . . . ? C1W N3W C3W N6W 179.9(5) . . . . ? C1W N3W C3W N2W -1.2(8) . . . . ? C2W N2W C3W N6W -178.5(5) . . . . ? C2W N2W C3W N3W 2.6(8) . . . . ? C1Z N1Z C2Z N5Z -179.6(5) . . . . ? C1Z N1Z C2Z N2Z -1.5(8) . . . . ? C3Z N2Z C2Z N5Z -179.6(5) . . . . ? C3Z N2Z C2Z N1Z 2.3(8) . . . . ? C3Z N3Z C1Z N4Z -179.8(5) . . . . ? C3Z N3Z C1Z N1Z 0.2(9) . . . . ? C2Z N1Z C1Z N4Z -179.7(5) . . . . ? C2Z N1Z C1Z N3Z 0.3(8) . . . . ? 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 O1D 0.84 1.96 2.792(6) 170.1 . O1C H1C O1B 0.84 2.04 2.786(6) 147.2 . O1C H1C O4C 0.84 2.46 2.887(6) 112.2 2_646 O1B H1B O8W 0.84 1.98 2.704(5) 143.6 2_556 O1B H1B O1A 0.84 2.50 2.969(6) 116.5 . O1D H1D O3W 0.84 1.99 2.678(6) 138.4 2_656 O1D H1D O1C 0.84 2.34 2.865(5) 121.2 . N3X H3X O1WA 0.88 1.84 2.709(7) 168.3 . N4X H4X1 N3Y 0.88 2.19 3.063(7) 171.7 . N4X H4X2 O3B 0.88 2.20 2.899(6) 136.5 . N5X H5X1 O3B 0.88 2.41 2.995(6) 124.2 2_655 N5X H5X2 O3D 0.88 2.31 3.015(7) 137.2 2 N6X H6X1 N2X 0.88 2.12 2.982(7) 166.5 2 N6X H6X2 O10W 0.88 1.93 2.736(7) 151.7 . N2Y H2Y O2W 0.88 1.84 2.702(6) 165.6 2_665 N6Y H6Y1 N1X 0.88 2.06 2.943(7) 176.2 . N6Y H6Y2 O9W 0.88 1.97 2.823(7) 163.3 . N5Y H5Y1 N1W 0.88 2.06 2.939(7) 174.3 2_765 N5Y H5Y2 O3D 0.88 2.34 2.925(6) 123.8 2_655 N4Y H4Y1 O2B 0.88 2.30 3.145(6) 159.9 . N4Y H4Y2 O2A 0.88 2.28 3.051(6) 146.3 1_655 N2Z H2Z O4W 0.88 1.97 2.747(6) 146.5 2_665 N2W H2W O7W 0.88 1.92 2.779(6) 165.1 2_665 N4Z H4Z1 O6W 0.88 2.08 2.945(6) 167.6 . N4Z H4Z2 O5W 0.88 2.08 2.948(6) 168.5 . N4W H4W1 O2C 0.88 2.12 2.919(6) 150.0 1_565 N4W H4W2 O2D 0.88 2.23 3.027(6) 150.1 1_665 N5Z H5Z1 N1Z 0.88 2.06 2.936(7) 174.8 2_765 N5Z H5Z2 O5W 0.88 2.14 2.816(6) 133.1 2_765 N5Z H5Z2 O4W 0.88 2.53 3.172(7) 130.8 2_665 N6W H6W1 N3Z 0.88 2.02 2.904(7) 177.1 2_665 N6W H6W2 O6W 0.88 2.07 2.760(7) 134.8 2_665 N6W H6W2 O7W 0.88 2.65 3.342(7) 135.9 2_665 N6Z H6Z1 N3W 0.88 2.14 3.024(7) 176.8 2_665 N6Z H6Z2 O3C 0.88 2.01 2.878(6) 168.3 2_655 N6Z H6Z2 O2C 0.88 2.65 3.240(7) 125.4 2_655 N5W H5W1 N1Y 0.88 2.08 2.956(7) 177.0 2_765 N5W H5W2 O3A 0.88 1.95 2.828(6) 172.5 2_665 O2W H2WA O4W 1.15 1.73 2.848(7) 160.6 . O2W H2WB O1WC 1.06 1.74 2.639(19) 139.8 1_565 O2W H2WB O9W 1.06 2.26 2.979(7) 123.7 2_665 O3W H3WA O4C 1.22 1.64 2.749(6) 148.7 1_565 O3W H3WA O2C 1.22 2.43 3.350(6) 130.6 1_565 O3W H3WB O2D 1.20 1.64 2.819(6) 165.7 1_665 O4W H4WA O2WA 1.01 1.78 2.746(6) 157.9 . O4W H4WB O2D 0.93 1.87 2.795(6) 173.9 1_565 O5W H5WA O4A 1.14 1.63 2.761(6) 174.8 1_655 O5W H5WB O3W 0.91 1.90 2.805(5) 172.6 . O6W H6WA O8W 0.97 1.83 2.790(6) 167.1 1_655 O6W H6WB O4C 1.11 1.98 2.988(6) 149.6 1_565 O6W H6WB O3C 1.11 2.17 3.048(6) 134.3 1_565 O7W H7WA O2B 0.91 1.96 2.840(6) 162.1 . O7W H7WB O3A 0.82 1.98 2.736(6) 152.2 . O8W H8WA O2B 1.06 1.74 2.781(6) 166.4 1_455 O8W H8WB O2A 0.94 1.84 2.770(5) 169.4 . O9W H9WA O3B 0.85 2.05 2.775(6) 143.4 2_655 O9W H9WA O4D 0.85 2.66 3.100(6) 114.0 2 O9W H9WB O2C 0.85 1.96 2.764(6) 158.4 2_655 O10W H10A O3D 1.04 1.81 2.745(6) 148.0 . O10W H10B O4B 1.16 2.02 2.902(6) 129.4 1_455 O10W H10B O2A 1.16 2.30 3.127(6) 125.7 . _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 22.02 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.542 _refine_diff_density_min -0.319 _refine_diff_density_rms 0.072 data_calix[4]arene_dihydrophosphonic_acid.melamine _database_code_depnum_ccdc_archive 'CCDC 278968' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H68 N18 O20 P2' _chemical_formula_weight 1171.05 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' O O 0.0106 0.0060 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.1727(9) _cell_length_b 12.4313(7) _cell_length_c 19.5080(10) _cell_angle_alpha 90.00 _cell_angle_beta 103.281(3) _cell_angle_gamma 90.00 _cell_volume 5233.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6715 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 21.967 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2472 _exptl_absorpt_coefficient_mu 0.177 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9522 _exptl_absorpt_correction_T_max 0.9947 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method ; 241 frames via \f rotation and 52 frames via \w rotation (rotation angle 1.5\% and 2*300 s per frame) ; _diffrn_detector_area_resol_mean ; 1242 (horizontal) x 1152 (vertical) pixels, CCD pixel size is 22.5 x 22.5 \mm which gives at the input a pixel of 110 x 110 \mm (with 2 x 2 binning) ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55429 _diffrn_reflns_av_R_equivalents 0.0643 _diffrn_reflns_av_sigmaI/netI 0.1185 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 21.98 _reflns_number_total 6336 _reflns_number_gt 4206 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect data collection software (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Johnson & Burnet, 1996)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0245P)^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 and difmap' _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00187(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6336 _refine_ls_number_parameters 751 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1013 _refine_ls_R_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.1104 _refine_ls_wR_factor_gt 0.0978 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.143 _refine_ls_shift/su_mean 0.004 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 C1A C 0.14961(18) 0.6682(4) 0.7066(2) 0.0233(11) Uani 1 1 d . . . C2A C 0.12185(18) 0.7664(4) 0.7096(3) 0.0303(13) Uani 1 1 d . . . H2A H 0.1158 0.7916 0.7536 0.036 Uiso 1 1 calc R . . C3A C 0.10249(19) 0.8293(4) 0.6501(3) 0.0348(13) Uani 1 1 d . . . H3A H 0.0841 0.8975 0.6533 0.042 Uiso 1 1 calc R . . C4A C 0.11022(18) 0.7919(4) 0.5863(3) 0.0297(12) Uani 1 1 d . . . H4A H 0.0969 0.8354 0.5456 0.036 Uiso 1 1 calc R . . C5A C 0.13695(18) 0.6923(4) 0.5795(2) 0.0250(12) Uani 1 1 d . . . C6A C 0.15663(18) 0.6332(4) 0.6413(3) 0.0263(12) Uani 1 1 d . . . C7A C 0.14557(17) 0.6542(4) 0.5086(2) 0.0270(12) Uani 1 1 d . . . H7A1 H 0.1894 0.6329 0.5140 0.032 Uiso 1 1 calc R . . H7A2 H 0.1376 0.7157 0.4755 0.032 Uiso 1 1 calc R . . O1A O 0.18657(12) 0.5353(2) 0.64187(15) 0.0308(8) Uani 1 1 d . . . H1A H 0.1889 0.5194 0.6007 0.046 Uiso 1 1 calc R . . C1B C 0.1047(2) 0.5608(4) 0.4759(2) 0.0270(12) Uani 1 1 d . . . C2B C 0.0436(2) 0.5784(4) 0.4388(2) 0.0310(13) Uani 1 1 d . . . H2B H 0.0279 0.6498 0.4345 0.037 Uiso 1 1 calc R . . C3B C 0.0055(2) 0.4961(4) 0.4086(2) 0.0323(13) Uani 1 1 d . . . H3B H -0.0356 0.5106 0.3832 0.039 Uiso 1 1 calc R . . C4B C 0.0279(2) 0.3905(4) 0.4155(2) 0.0318(13) Uani 1 1 d . . . H4B H 0.0015 0.3335 0.3944 0.038 Uiso 1 1 calc R . . C5B C 0.08781(19) 0.3672(4) 0.4525(2) 0.0250(12) Uani 1 1 d . . . C6B C 0.12503(19) 0.4551(4) 0.4799(2) 0.0267(12) Uani 1 1 d . . . C7B C 0.11048(18) 0.2522(3) 0.4648(2) 0.0254(12) Uani 1 1 d . . . H7B1 H 0.1562 0.2510 0.4723 0.030 Uiso 1 1 calc R . . H7B2 H 0.0930 0.2089 0.4223 0.030 Uiso 1 1 calc R . . O1B O 0.18624(11) 0.4325(2) 0.51840(15) 0.0243(8) Uani 1 1 d . . . O2B O 0.22332(12) 0.3882(2) 0.40719(14) 0.0297(8) Uani 1 1 d G . . O3B O 0.28509(11) 0.3379(2) 0.53080(14) 0.0248(8) Uani 1 1 d . . . O4B O 0.27763(12) 0.5318(2) 0.49050(15) 0.0264(8) Uani 1 1 d . . . P1B P 0.24701(5) 0.42188(10) 0.48309(7) 0.0261(4) Uani 1 1 d . . . C1C C 0.09213(19) 0.2014(3) 0.5281(2) 0.0241(12) Uani 1 1 d . . . C2C C 0.03668(19) 0.1447(3) 0.5176(2) 0.0276(12) Uani 1 1 d . . . H2C H 0.0125 0.1356 0.4710 0.033 Uiso 1 1 calc R . . C3C C 0.0159(2) 0.1011(4) 0.5733(3) 0.0317(13) Uani 1 1 d . . . H3C H -0.0217 0.0614 0.5650 0.038 Uiso 1 1 calc R . . C4C C 0.05062(19) 0.1161(3) 0.6415(3) 0.0280(13) Uani 1 1 d . . . H4C H 0.0360 0.0870 0.6797 0.034 Uiso 1 1 calc R . . C5C C 0.10622(19) 0.1725(3) 0.6553(2) 0.0244(12) Uani 1 1 d . . . C6C C 0.12605(18) 0.2129(3) 0.5967(3) 0.0250(12) Uani 1 1 d . . . C7C C 0.13964(19) 0.1971(3) 0.7302(2) 0.0271(12) Uani 1 1 d . . . H7C1 H 0.1849 0.1987 0.7339 0.033 Uiso 1 1 calc R . . H7C2 H 0.1307 0.1405 0.7621 0.033 Uiso 1 1 calc R . . O1C O 0.18333(12) 0.2646(2) 0.61304(15) 0.0303(8) Uani 1 1 d . . . H1C H 0.1922 0.2862 0.5758 0.046 Uiso 1 1 calc R . . C1D C 0.11795(19) 0.3057(4) 0.7512(2) 0.0227(12) Uani 1 1 d . . . C2D C 0.05724(19) 0.3191(4) 0.7572(2) 0.0293(12) Uani 1 1 d . . . H2D H 0.0305 0.2585 0.7523 0.035 Uiso 1 1 calc R . . C3D C 0.0352(2) 0.4190(4) 0.7702(2) 0.0312(13) Uani 1 1 d . . . H3D H -0.0060 0.4263 0.7761 0.037 Uiso 1 1 calc R . . C4D C 0.07257(18) 0.5080(4) 0.7746(2) 0.0286(13) Uani 1 1 d . . . H4D H 0.0562 0.5771 0.7806 0.034 Uiso 1 1 calc R . . C5D C 0.13393(19) 0.4980(4) 0.7705(2) 0.0240(12) Uani 1 1 d . . . C6D C 0.15629(19) 0.3959(4) 0.7616(2) 0.0239(12) Uani 1 1 d . . . C7D C 0.17338(18) 0.5990(3) 0.7710(2) 0.0284(12) Uani 1 1 d . . . H7D1 H 0.1732 0.6415 0.8139 0.034 Uiso 1 1 calc R . . H7D2 H 0.2167 0.5776 0.7726 0.034 Uiso 1 1 calc R . . O1D O 0.21980(11) 0.3819(2) 0.76233(14) 0.0225(8) Uani 1 1 d . . . O2D O 0.23356(12) 0.3122(2) 0.88679(15) 0.0256(8) Uani 1 1 d G . . H2DO H 0.2317 0.2232 0.8891 0.026 Uiso 1 1 d G . . O3D O 0.29753(12) 0.4659(2) 0.86514(15) 0.0264(8) Uani 1 1 d . . . O4D O 0.31660(11) 0.2835(2) 0.81702(14) 0.0241(8) Uani 1 1 d G . . P1D P 0.27030(5) 0.36044(10) 0.83540(6) 0.0240(3) Uani 1 1 d . . . C3X C 0.4552(2) -0.0523(4) 0.2342(2) 0.0213(11) Uani 1 1 d . . . C1X C 0.4574(2) 0.1361(4) 0.2328(2) 0.0213(11) Uani 1 1 d . . . C2X C 0.5458(2) 0.0400(4) 0.2685(2) 0.0217(11) Uani 1 1 d . . . N1X N 0.42517(15) 0.0431(3) 0.21954(18) 0.0225(9) Uani 1 1 d . . . H1X H 0.3850 0.0445 0.2016 0.027 Uiso 1 1 calc R . . N2X N 0.51857(15) 0.1384(3) 0.25712(17) 0.0201(9) Uani 1 1 d . . . N3X N 0.51629(15) -0.0562(3) 0.26030(18) 0.0217(9) Uani 1 1 d . . . N6X N 0.42197(14) -0.1416(3) 0.22073(18) 0.0254(10) Uani 1 1 d . . . H6X1 H 0.4402 -0.2047 0.2291 0.030 Uiso 1 1 calc R . . H6X2 H 0.3817 -0.1378 0.2035 0.030 Uiso 1 1 calc R . . N4X N 0.42585(15) 0.2275(3) 0.21932(17) 0.0244(9) Uani 1 1 d . . . H4X1 H 0.4454 0.2896 0.2265 0.029 Uiso 1 1 calc R . . H4X2 H 0.3854 0.2260 0.2032 0.029 Uiso 1 1 calc R . . N5X N 0.60703(15) 0.0381(3) 0.29011(18) 0.0261(10) Uani 1 1 d . . . H5X1 H 0.6266 -0.0238 0.2984 0.031 Uiso 1 1 calc R . . H5X2 H 0.6281 0.0988 0.2961 0.031 Uiso 1 1 calc R . . C3Y C 0.4417(2) 0.2325(4) 0.5630(2) 0.0208(11) Uani 1 1 d . . . C1Y C 0.4401(2) 0.4215(4) 0.5575(2) 0.0202(11) Uani 1 1 d . . . C2Y C 0.5308(2) 0.3291(4) 0.5915(2) 0.0227(11) Uani 1 1 d . . . N1Y N 0.40895(14) 0.3259(3) 0.54921(17) 0.0211(9) Uani 1 1 d . . . H1Y H 0.3683 0.3246 0.5351 0.025 Uiso 1 1 calc R . . N2Y N 0.50105(15) 0.4256(3) 0.58019(18) 0.0230(9) Uani 1 1 d . . . N3Y N 0.50324(15) 0.2308(3) 0.58314(18) 0.0231(9) Uani 1 1 d . . . N6Y N 0.41072(15) 0.1407(3) 0.55576(17) 0.0265(10) Uani 1 1 d . . . H6Y1 H 0.4308 0.0793 0.5642 0.032 Uiso 1 1 calc R . . H6Y2 H 0.3700 0.1410 0.5425 0.032 Uiso 1 1 calc R . . N4Y N 0.40762(15) 0.5115(3) 0.54414(18) 0.0253(10) Uani 1 1 d . . . H4Y1 H 0.4266 0.5741 0.5503 0.030 Uiso 1 1 calc R . . H4Y2 H 0.3671 0.5086 0.5291 0.030 Uiso 1 1 calc R . . N5Y N 0.59127(14) 0.3313(3) 0.61190(17) 0.0269(10) Uani 1 1 d . . . H5Y1 H 0.6123 0.2708 0.6196 0.032 Uiso 1 1 calc R . . H5Y2 H 0.6109 0.3934 0.6179 0.032 Uiso 1 1 calc R . . C2Z C 0.4449(2) 0.8286(4) 0.5657(2) 0.0216(11) Uani 1 1 d . . . C1Z C 0.5362(2) 0.9194(4) 0.5956(2) 0.0213(11) Uani 1 1 d . . . C3Z C 0.5328(2) 0.7300(4) 0.6009(2) 0.0194(11) Uani 1 1 d . . . N3Z N 0.47152(15) 0.7299(3) 0.57772(18) 0.0220(9) Uani 1 1 d . . . N2Z N 0.47533(16) 0.9249(3) 0.57165(18) 0.0209(9) Uani 1 1 d . . . N1Z N 0.56636(14) 0.8231(3) 0.61212(17) 0.0201(9) Uani 1 1 d . . . H1Z H 0.6066 0.8214 0.6297 0.024 Uiso 1 1 calc R . . N6Z N 0.56410(14) 0.6392(3) 0.61453(17) 0.0244(10) Uani 1 1 d . . . H6Z1 H 0.5444 0.5772 0.6083 0.029 Uiso 1 1 calc R . . H6Z2 H 0.6046 0.6406 0.6298 0.029 Uiso 1 1 calc R . . N5Z N 0.38406(14) 0.8314(3) 0.54565(17) 0.0281(10) Uani 1 1 d . . . H5Z1 H 0.3627 0.7711 0.5407 0.034 Uiso 1 1 calc R . . H5Z2 H 0.3648 0.8935 0.5372 0.034 Uiso 1 1 calc R . . N4Z N 0.57057(15) 1.0077(3) 0.60588(18) 0.0253(10) Uani 1 1 d . . . H4Z1 H 0.5530 1.0712 0.5968 0.030 Uiso 1 1 calc R . . H4Z2 H 0.6110 1.0029 0.6218 0.030 Uiso 1 1 calc R . . C1S C 0.1912(2) -0.0274(4) 0.4799(3) 0.0437(15) Uani 1 1 d . . . H1S1 H 0.1850 0.0036 0.4326 0.066 Uiso 1 1 calc R . . H1S2 H 0.1534 -0.0178 0.4973 0.066 Uiso 1 1 calc R . . H1S3 H 0.2004 -0.1043 0.4780 0.066 Uiso 1 1 calc R . . C2S C 0.24455(19) 0.0286(4) 0.5288(2) 0.0363(14) Uani 1 1 d . . . H2S1 H 0.2352 0.1064 0.5301 0.044 Uiso 1 1 calc R . . H2S2 H 0.2491 -0.0002 0.5770 0.044 Uiso 1 1 calc R . . O1S O 0.30199(12) 0.0151(2) 0.50768(15) 0.0310(8) Uani 1 1 d . . . H1S H 0.2989 0.0419 0.4675 0.046 Uiso 1 1 calc R . . O1W O 0.30670(12) 0.0982(3) 0.16775(15) 0.0296(8) Uani 1 1 d G . . H1W1 H 0.2932 0.1145 0.1246 0.044 Uiso 1 1 d G . . H1W2 H 0.2672 0.0812 0.1833 0.044 Uiso 1 1 d G . . O2W O 0.29741(14) 0.3483(2) 0.20023(17) 0.0337(8) Uani 1 1 d G . . H2W1 H 0.3005 0.3106 0.2372 0.051 Uiso 1 1 d G . . H2W2 H 0.2715 0.3175 0.1671 0.051 Uiso 1 1 d G . . O3W O 0.32339(13) 0.4858(3) 0.34912(18) 0.0424(10) Uani 1 1 d G . . H3W1 H 0.2899 0.4715 0.3795 0.064 Uiso 1 1 d G . . H3W2 H 0.2993 0.4995 0.3059 0.064 Uiso 1 1 d G . . O4W O 0.23305(18) 0.5312(3) 0.2274(3) 0.0776(13) Uani 1 1 d G . . H4W1 H 0.2461 0.4692 0.2193 0.116 Uiso 1 1 d G . . H4W2 H 0.1962 0.5242 0.2324 0.116 Uiso 1 1 d G . . O5W O 0.14223(15) 0.5313(3) 0.32336(18) 0.0554(11) Uani 1 1 d G . . H5W1 H 0.0907 0.5377 0.3409 0.083 Uiso 1 1 d G . . H5W2 H 0.1771 0.4642 0.3522 0.083 Uiso 1 1 d G . . O6W O 0.29870(14) 0.7111(3) 0.21122(18) 0.0392(9) Uani 1 1 d G . . H6W1 H 0.2704 0.6639 0.2074 0.059 Uiso 1 1 d G . . H6W2 H 0.2954 0.7535 0.2444 0.059 Uiso 1 1 d G . . O7W O 0.23436(14) 0.6881(3) 0.38846(18) 0.0451(9) Uani 1 1 d G . . H7W1 H 0.2549 0.6311 0.4376 0.068 Uiso 1 1 d G . . H7W2 H 0.2018 0.6410 0.3484 0.068 Uiso 1 1 d G . . O8W O 0.31783(12) 0.6662(3) 0.60239(18) 0.0338(8) Uani 1 1 d G . . H8W1 H 0.2950 0.6211 0.5756 0.051 Uiso 1 1 d G . . H8W2 H 0.2957 0.6972 0.6268 0.051 Uiso 1 1 d G . . O9W O 0.31364(12) 0.8187(2) 0.34134(16) 0.0304(8) Uani 1 1 d G . . H9W1 H 0.2847 0.7821 0.3519 0.046 Uiso 1 1 d G . . H9W2 H 0.3040 0.9044 0.3465 0.046 Uiso 1 1 d G . . 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 C1A 0.017(2) 0.020(3) 0.032(3) -0.002(3) 0.004(2) 0.001(2) C2A 0.031(3) 0.021(3) 0.038(4) -0.003(3) 0.007(3) 0.000(2) C3A 0.031(3) 0.026(3) 0.050(4) -0.002(3) 0.015(3) 0.006(3) C4A 0.026(3) 0.019(3) 0.042(4) 0.007(3) 0.005(3) 0.001(2) C5A 0.022(3) 0.013(3) 0.039(4) 0.004(3) 0.005(2) -0.003(2) C6A 0.022(3) 0.011(3) 0.045(4) -0.003(3) 0.006(3) 0.000(2) C7A 0.025(3) 0.023(3) 0.033(3) 0.005(3) 0.008(2) 0.002(2) O1A 0.0388(19) 0.023(2) 0.030(2) 0.0009(16) 0.0059(16) 0.0066(16) C1B 0.027(3) 0.021(3) 0.031(3) 0.001(3) 0.006(3) -0.003(3) C2B 0.037(3) 0.016(3) 0.042(3) 0.005(3) 0.012(3) 0.001(3) C3B 0.026(3) 0.029(4) 0.040(4) 0.003(3) 0.005(3) -0.001(3) C4B 0.034(3) 0.030(4) 0.030(3) 0.001(3) 0.004(3) -0.004(3) C5B 0.027(3) 0.017(3) 0.033(3) 0.002(3) 0.009(3) -0.002(2) C6B 0.019(3) 0.028(4) 0.033(3) 0.000(3) 0.007(2) 0.001(3) C7B 0.023(3) 0.020(3) 0.030(3) -0.002(2) 0.002(2) -0.004(2) O1B 0.0187(17) 0.023(2) 0.031(2) -0.0001(16) 0.0047(15) 0.0008(14) O2B 0.047(2) 0.019(2) 0.022(2) -0.0023(16) 0.0048(16) 0.0053(15) O3B 0.0245(17) 0.022(2) 0.026(2) 0.0025(16) 0.0024(15) 0.0063(15) O4B 0.0274(17) 0.016(2) 0.036(2) 0.0037(16) 0.0081(15) -0.0021(15) P1B 0.0277(7) 0.0219(9) 0.0292(9) 0.0016(7) 0.0078(6) 0.0030(6) C1C 0.025(3) 0.013(3) 0.034(3) -0.004(2) 0.007(3) 0.000(2) C2C 0.027(3) 0.020(3) 0.036(3) -0.001(3) 0.006(3) 0.000(2) C3C 0.029(3) 0.020(3) 0.044(4) -0.005(3) 0.005(3) 0.001(2) C4C 0.030(3) 0.012(3) 0.047(4) 0.002(3) 0.020(3) 0.006(2) C5C 0.023(3) 0.017(3) 0.035(3) 0.001(3) 0.011(3) -0.001(2) C6C 0.021(3) 0.014(3) 0.039(4) -0.005(3) 0.006(3) -0.004(2) C7C 0.032(3) 0.021(3) 0.029(3) 0.002(2) 0.008(2) -0.001(2) O1C 0.0313(18) 0.031(2) 0.030(2) -0.0019(17) 0.0102(16) -0.0091(16) C1D 0.028(3) 0.016(3) 0.023(3) -0.002(2) 0.004(2) 0.005(2) C2D 0.026(3) 0.030(4) 0.034(3) -0.005(3) 0.011(2) -0.007(2) C3D 0.023(3) 0.029(4) 0.044(3) -0.010(3) 0.011(3) -0.003(3) C4D 0.021(3) 0.025(3) 0.040(3) -0.002(3) 0.009(2) 0.006(2) C5D 0.029(3) 0.019(3) 0.023(3) -0.003(2) 0.002(2) 0.000(2) C6D 0.026(3) 0.024(3) 0.023(3) -0.002(2) 0.007(2) 0.000(3) C7D 0.031(3) 0.021(3) 0.035(3) -0.003(3) 0.009(3) 0.002(2) O1D 0.0173(16) 0.020(2) 0.031(2) 0.0007(15) 0.0058(15) 0.0021(14) O2D 0.0303(17) 0.0155(19) 0.034(2) 0.0006(16) 0.0134(16) -0.0004(15) O3D 0.0289(17) 0.0156(19) 0.033(2) -0.0016(16) 0.0041(15) -0.0039(15) O4D 0.0241(16) 0.0182(19) 0.031(2) 0.0006(15) 0.0085(15) 0.0010(14) P1D 0.0259(7) 0.0184(8) 0.0279(8) 0.0018(7) 0.0070(6) 0.0012(6) C3X 0.030(3) 0.018(3) 0.018(3) 0.001(2) 0.011(2) 0.002(3) C1X 0.030(3) 0.017(3) 0.018(3) 0.000(2) 0.009(2) 0.005(3) C2X 0.026(3) 0.019(3) 0.021(3) 0.001(2) 0.005(2) 0.003(3) N1X 0.022(2) 0.013(3) 0.031(3) -0.001(2) 0.0025(19) -0.002(2) N2X 0.023(2) 0.017(3) 0.021(2) -0.0007(19) 0.0057(19) -0.0011(19) N3X 0.024(2) 0.013(3) 0.028(3) -0.0006(19) 0.005(2) 0.0018(19) N6X 0.023(2) 0.011(2) 0.043(3) -0.002(2) 0.0097(19) 0.0009(19) N4X 0.023(2) 0.017(3) 0.031(3) -0.002(2) 0.0037(18) -0.0035(19) N5X 0.024(2) 0.015(2) 0.037(3) 0.0001(19) 0.002(2) 0.0016(18) C3Y 0.034(3) 0.009(3) 0.021(3) -0.001(2) 0.010(2) 0.001(3) C1Y 0.028(3) 0.013(3) 0.021(3) -0.002(2) 0.009(2) -0.004(3) C2Y 0.025(3) 0.020(3) 0.024(3) 0.001(2) 0.009(2) 0.001(3) N1Y 0.019(2) 0.015(3) 0.028(2) -0.0002(19) 0.0024(18) 0.000(2) N2Y 0.021(2) 0.019(3) 0.028(2) -0.002(2) 0.0039(19) 0.0011(19) N3Y 0.021(2) 0.019(3) 0.031(3) 0.000(2) 0.0095(19) -0.0005(19) N6Y 0.026(2) 0.018(3) 0.035(3) 0.003(2) 0.0075(19) 0.0051(19) N4Y 0.024(2) 0.014(3) 0.038(3) 0.000(2) 0.0069(19) 0.0010(19) N5Y 0.025(2) 0.012(2) 0.042(3) 0.002(2) 0.004(2) 0.0019(18) C2Z 0.027(3) 0.021(3) 0.018(3) 0.003(2) 0.007(2) 0.003(3) C1Z 0.034(3) 0.013(3) 0.018(3) -0.002(2) 0.008(2) -0.002(3) C3Z 0.029(3) 0.012(3) 0.018(3) -0.002(2) 0.006(2) -0.002(3) N3Z 0.022(2) 0.018(3) 0.026(2) -0.0009(19) 0.0051(18) 0.0021(19) N2Z 0.021(2) 0.015(3) 0.026(2) 0.0011(19) 0.0043(19) 0.0005(19) N1Z 0.019(2) 0.015(3) 0.026(2) 0.001(2) 0.0040(18) -0.004(2) N6Z 0.021(2) 0.012(3) 0.039(3) -0.001(2) 0.0041(19) -0.0039(19) N5Z 0.022(2) 0.014(2) 0.045(3) 0.002(2) 0.002(2) 0.0019(18) N4Z 0.023(2) 0.014(2) 0.038(3) 0.003(2) 0.0051(19) 0.0014(19) C1S 0.042(3) 0.035(4) 0.054(4) 0.004(3) 0.012(3) -0.011(3) C2S 0.037(3) 0.038(4) 0.036(3) 0.005(3) 0.015(3) 0.007(3) O1S 0.0289(18) 0.030(2) 0.035(2) 0.0087(16) 0.0083(16) 0.0054(15) O1W 0.0248(17) 0.035(2) 0.028(2) 0.0023(18) 0.0032(15) 0.0025(16) O2W 0.039(2) 0.030(2) 0.033(2) 0.0034(18) 0.0100(17) -0.0025(17) O3W 0.043(2) 0.028(2) 0.065(3) 0.010(2) 0.0292(19) 0.0019(18) O4W 0.070(3) 0.063(3) 0.101(4) -0.001(3) 0.022(3) -0.003(2) O5W 0.062(2) 0.051(3) 0.051(3) 0.003(2) 0.009(2) 0.003(2) O6W 0.047(2) 0.030(2) 0.044(3) 0.0007(18) 0.0163(19) 0.0057(17) O7W 0.047(2) 0.037(2) 0.047(2) 0.016(2) 0.0027(19) -0.0093(18) O8W 0.0363(19) 0.027(2) 0.038(2) -0.0052(17) 0.0079(17) -0.0010(16) O9W 0.0262(18) 0.015(2) 0.048(2) 0.0032(17) 0.0029(17) -0.0009(15) _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 C1A C2A 1.374(6) . ? C1A C6A 1.389(6) . ? C1A C7D 1.514(6) . ? C2A C3A 1.384(6) . ? C2A H2A 0.9500 . ? C3A C4A 1.377(6) . ? C3A H3A 0.9500 . ? C4A C5A 1.392(6) . ? C4A H4A 0.9500 . ? C5A C6A 1.392(6) . ? C5A C7A 1.515(6) . ? C6A O1A 1.386(5) . ? C7A C1B 1.521(6) . ? C7A H7A1 0.9900 . ? C7A H7A2 0.9900 . ? O1A H1A 0.8400 . ? C1B C6B 1.386(6) . ? C1B C2B 1.399(5) . ? C2B C3B 1.370(6) . ? C2B H2B 0.9500 . ? C3B C4B 1.399(6) . ? C3B H3B 0.9500 . ? C4B C5B 1.389(5) . ? C4B H4B 0.9500 . ? C5B C6B 1.399(6) . ? C5B C7B 1.517(6) . ? C6B O1B 1.420(5) . ? C7B C1C 1.524(5) . ? C7B H7B1 0.9900 . ? C7B H7B2 0.9900 . ? O1B P1B 1.654(3) . ? O2B P1B 1.512(3) . ? O3B P1B 1.519(3) . ? O4B P1B 1.518(3) . ? C1C C6C 1.384(6) . ? C1C C2C 1.391(5) . ? C2C C3C 1.385(5) . ? C2C H2C 0.9500 . ? C3C C4C 1.387(6) . ? C3C H3C 0.9500 . ? C4C C5C 1.389(5) . ? C4C H4C 0.9500 . ? C5C C6C 1.407(6) . ? C5C C7C 1.510(6) . ? C6C O1C 1.394(4) . ? C7C C1D 1.521(5) . ? C7C H7C1 0.9900 . ? C7C H7C2 0.9900 . ? O1C H1C 0.8400 . ? C1D C2D 1.388(5) . ? C1D C6D 1.393(6) . ? C2D C3D 1.380(6) . ? C2D H2D 0.9500 . ? C3D C4D 1.373(5) . ? C3D H3D 0.9500 . ? C4D C5D 1.387(5) . ? C4D H4D 0.9500 . ? C5D C6D 1.388(6) . ? C5D C7D 1.529(5) . ? C6D O1D 1.416(4) . ? C7D H7D1 0.9900 . ? C7D H7D2 0.9900 . ? O1D P1D 1.620(3) . ? O2D P1D 1.550(3) . ? O2D H2DO 1.1088 . ? O3D P1D 1.503(3) . ? O4D P1D 1.505(3) . ? C3X N6X 1.325(5) . ? C3X N3X 1.334(5) . ? C3X N1X 1.358(5) . ? C1X N4X 1.329(5) . ? C1X N2X 1.330(5) . ? C1X N1X 1.353(5) . ? C2X N5X 1.326(5) . ? C2X N3X 1.355(5) . ? C2X N2X 1.360(5) . ? N1X H1X 0.8800 . ? N6X H6X1 0.8800 . ? N6X H6X2 0.8800 . ? N4X H4X1 0.8800 . ? N4X H4X2 0.8800 . ? N5X H5X1 0.8800 . ? N5X H5X2 0.8800 . ? C3Y N6Y 1.322(5) . ? C3Y N3Y 1.331(5) . ? C3Y N1Y 1.363(5) . ? C1Y N2Y 1.323(5) . ? C1Y N4Y 1.323(5) . ? C1Y N1Y 1.366(5) . ? C2Y N5Y 1.309(5) . ? C2Y N3Y 1.359(5) . ? C2Y N2Y 1.362(5) . ? N1Y H1Y 0.8800 . ? N6Y H6Y1 0.8800 . ? N6Y H6Y2 0.8800 . ? N4Y H4Y1 0.8800 . ? N4Y H4Y2 0.8800 . ? N5Y H5Y1 0.8800 . ? N5Y H5Y2 0.8800 . ? C2Z N5Z 1.316(4) . ? C2Z N3Z 1.358(5) . ? C2Z N2Z 1.366(5) . ? C1Z N4Z 1.324(5) . ? C1Z N2Z 1.325(5) . ? C1Z N1Z 1.372(5) . ? C3Z N6Z 1.320(5) . ? C3Z N3Z 1.329(5) . ? C3Z N1Z 1.367(5) . ? N1Z H1Z 0.8800 . ? N6Z H6Z1 0.8800 . ? N6Z H6Z2 0.8800 . ? N5Z H5Z1 0.8800 . ? N5Z H5Z2 0.8800 . ? N4Z H4Z1 0.8800 . ? N4Z H4Z2 0.8800 . ? C1S C2S 1.509(6) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C2S O1S 1.436(4) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? O1S H1S 0.8400 . ? O1W H1W1 0.8499 . ? O1W H1W2 1.0119 . ? O2W H2W1 0.8500 . ? O2W H2W2 0.8501 . ? O3W H3W1 1.0646 . ? O3W H3W2 0.9043 . ? O4W H4W1 0.8501 . ? O4W H4W2 0.8501 . ? O5W H5W1 1.2684 . ? O5W H5W2 1.1883 . ? O6W H6W1 0.8500 . ? O6W H6W2 0.8502 . ? O7W H7W1 1.1951 . ? O7W H7W2 1.1028 . ? O8W H8W1 0.8500 . ? O8W H8W2 0.8500 . ? O9W H9W1 0.8501 . ? O9W H9W2 1.0958 . ? 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 C2A C1A C6A 117.6(4) . . ? C2A C1A C7D 122.9(4) . . ? C6A C1A C7D 119.5(4) . . ? C1A C2A C3A 121.4(4) . . ? C1A C2A H2A 119.3 . . ? C3A C2A H2A 119.3 . . ? C4A C3A C2A 119.3(4) . . ? C4A C3A H3A 120.3 . . ? C2A C3A H3A 120.4 . . ? C3A C4A C5A 122.0(5) . . ? C3A C4A H4A 119.0 . . ? C5A C4A H4A 119.0 . . ? C4A C5A C6A 116.3(4) . . ? C4A C5A C7A 120.7(4) . . ? C6A C5A C7A 123.0(4) . . ? O1A C6A C1A 115.0(4) . . ? O1A C6A C5A 121.7(4) . . ? C1A C6A C5A 123.3(4) . . ? C5A C7A C1B 115.8(3) . . ? C5A C7A H7A1 108.3 . . ? C1B C7A H7A1 108.3 . . ? C5A C7A H7A2 108.3 . . ? C1B C7A H7A2 108.3 . . ? H7A1 C7A H7A2 107.4 . . ? C6A O1A H1A 109.5 . . ? C6B C1B C2B 116.2(4) . . ? C6B C1B C7A 123.1(4) . . ? C2B C1B C7A 120.7(4) . . ? C3B C2B C1B 122.3(4) . . ? C3B C2B H2B 118.9 . . ? C1B C2B H2B 118.9 . . ? C2B C3B C4B 119.3(4) . . ? C2B C3B H3B 120.4 . . ? C4B C3B H3B 120.4 . . ? C5B C4B C3B 121.4(4) . . ? C5B C4B H4B 119.3 . . ? C3B C4B H4B 119.3 . . ? C4B C5B C6B 116.5(4) . . ? C4B C5B C7B 121.4(4) . . ? C6B C5B C7B 122.0(4) . . ? C1B C6B C5B 124.3(4) . . ? C1B C6B O1B 118.4(4) . . ? C5B C6B O1B 117.2(4) . . ? C5B C7B C1C 112.3(3) . . ? C5B C7B H7B1 109.2 . . ? C1C C7B H7B1 109.2 . . ? C5B C7B H7B2 109.2 . . ? C1C C7B H7B2 109.2 . . ? H7B1 C7B H7B2 107.9 . . ? C6B O1B P1B 124.5(3) . . ? O2B P1B O4B 112.92(17) . . ? O2B P1B O3B 115.43(17) . . ? O4B P1B O3B 112.75(17) . . ? O2B P1B O1B 107.28(16) . . ? O4B P1B O1B 106.13(15) . . ? O3B P1B O1B 101.01(15) . . ? C6C C1C C2C 117.4(4) . . ? C6C C1C C7B 123.7(4) . . ? C2C C1C C7B 118.8(4) . . ? C3C C2C C1C 121.7(4) . . ? C3C C2C H2C 119.2 . . ? C1C C2C H2C 119.2 . . ? C2C C3C C4C 119.2(4) . . ? C2C C3C H3C 120.4 . . ? C4C C3C H3C 120.4 . . ? C3C C4C C5C 121.7(4) . . ? C3C C4C H4C 119.1 . . ? C5C C4C H4C 119.1 . . ? C4C C5C C6C 116.9(4) . . ? C4C C5C C7C 120.4(4) . . ? C6C C5C C7C 122.5(4) . . ? C1C C6C O1C 122.2(4) . . ? C1C C6C C5C 123.1(4) . . ? O1C C6C C5C 114.7(4) . . ? C5C C7C C1D 109.0(4) . . ? C5C C7C H7C1 109.9 . . ? C1D C7C H7C1 109.9 . . ? C5C C7C H7C2 109.9 . . ? C1D C7C H7C2 109.9 . . ? H7C1 C7C H7C2 108.3 . . ? C6C O1C H1C 109.5 . . ? C2D C1D C6D 117.6(4) . . ? C2D C1D C7C 120.1(4) . . ? C6D C1D C7C 122.2(4) . . ? C3D C2D C1D 121.0(4) . . ? C3D C2D H2D 119.5 . . ? C1D C2D H2D 119.5 . . ? C4D C3D C2D 120.2(4) . . ? C4D C3D H3D 119.9 . . ? C2D C3D H3D 119.9 . . ? C3D C4D C5D 120.7(4) . . ? C3D C4D H4D 119.7 . . ? C5D C4D H4D 119.7 . . ? C4D C5D C6D 118.2(4) . . ? C4D C5D C7D 119.6(4) . . ? C6D C5D C7D 122.1(4) . . ? C5D C6D C1D 122.0(4) . . ? C5D C6D O1D 119.6(4) . . ? C1D C6D O1D 118.3(4) . . ? C1A C7D C5D 111.9(4) . . ? C1A C7D H7D1 109.2 . . ? C5D C7D H7D1 109.2 . . ? C1A C7D H7D2 109.2 . . ? C5D C7D H7D2 109.2 . . ? H7D1 C7D H7D2 107.9 . . ? C6D O1D P1D 120.9(2) . . ? P1D O2D H2DO 116.3 . . ? O3D P1D O4D 114.23(15) . . ? O3D P1D O2D 108.17(16) . . ? O4D P1D O2D 113.39(16) . . ? O3D P1D O1D 109.34(16) . . ? O4D P1D O1D 105.46(15) . . ? O2D P1D O1D 105.85(15) . . ? N6X C3X N3X 121.0(4) . . ? N6X C3X N1X 117.8(4) . . ? N3X C3X N1X 121.2(4) . . ? N4X C1X N2X 120.0(4) . . ? N4X C1X N1X 117.5(4) . . ? N2X C1X N1X 122.5(4) . . ? N5X C2X N3X 117.0(4) . . ? N5X C2X N2X 116.8(4) . . ? N3X C2X N2X 126.2(4) . . ? C1X N1X C3X 119.6(4) . . ? C1X N1X H1X 120.2 . . ? C3X N1X H1X 120.2 . . ? C1X N2X C2X 114.6(4) . . ? C3X N3X C2X 115.7(4) . . ? C3X N6X H6X1 120.0 . . ? C3X N6X H6X2 120.0 . . ? H6X1 N6X H6X2 120.0 . . ? C1X N4X H4X1 120.0 . . ? C1X N4X H4X2 120.0 . . ? H4X1 N4X H4X2 120.0 . . ? C2X N5X H5X1 120.0 . . ? C2X N5X H5X2 120.0 . . ? H5X1 N5X H5X2 120.0 . . ? N6Y C3Y N3Y 119.4(4) . . ? N6Y C3Y N1Y 118.3(4) . . ? N3Y C3Y N1Y 122.3(4) . . ? N2Y C1Y N4Y 120.1(4) . . ? N2Y C1Y N1Y 121.5(4) . . ? N4Y C1Y N1Y 118.3(4) . . ? N5Y C2Y N3Y 117.2(4) . . ? N5Y C2Y N2Y 117.0(4) . . ? N3Y C2Y N2Y 125.8(4) . . ? C3Y N1Y C1Y 119.1(4) . . ? C3Y N1Y H1Y 120.4 . . ? C1Y N1Y H1Y 120.4 . . ? C1Y N2Y C2Y 116.1(4) . . ? C3Y N3Y C2Y 115.1(4) . . ? C3Y N6Y H6Y1 120.0 . . ? C3Y N6Y H6Y2 120.0 . . ? H6Y1 N6Y H6Y2 120.0 . . ? C1Y N4Y H4Y1 120.0 . . ? C1Y N4Y H4Y2 120.0 . . ? H4Y1 N4Y H4Y2 120.0 . . ? C2Y N5Y H5Y1 120.0 . . ? C2Y N5Y H5Y2 120.0 . . ? H5Y1 N5Y H5Y2 120.0 . . ? N5Z C2Z N3Z 116.7(4) . . ? N5Z C2Z N2Z 117.0(4) . . ? N3Z C2Z N2Z 126.2(4) . . ? N4Z C1Z N2Z 121.0(4) . . ? N4Z C1Z N1Z 117.1(4) . . ? N2Z C1Z N1Z 121.9(4) . . ? N6Z C3Z N3Z 121.1(4) . . ? N6Z C3Z N1Z 116.8(4) . . ? N3Z C3Z N1Z 122.1(4) . . ? C3Z N3Z C2Z 115.3(4) . . ? C1Z N2Z C2Z 115.3(4) . . ? C3Z N1Z C1Z 118.9(4) . . ? C3Z N1Z H1Z 120.5 . . ? C1Z N1Z H1Z 120.5 . . ? C3Z N6Z H6Z1 120.0 . . ? C3Z N6Z H6Z2 120.0 . . ? H6Z1 N6Z H6Z2 120.0 . . ? C2Z N5Z H5Z1 120.0 . . ? C2Z N5Z H5Z2 120.0 . . ? H5Z1 N5Z H5Z2 120.0 . . ? C1Z N4Z H4Z1 120.0 . . ? C1Z N4Z H4Z2 120.0 . . ? H4Z1 N4Z H4Z2 120.0 . . ? C2S C1S H1S1 109.5 . . ? C2S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? C2S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? O1S C2S C1S 112.5(4) . . ? O1S C2S H2S1 109.1 . . ? C1S C2S H2S1 109.1 . . ? O1S C2S H2S2 109.1 . . ? C1S C2S H2S2 109.1 . . ? H2S1 C2S H2S2 107.8 . . ? C2S O1S H1S 109.5 . . ? H1W1 O1W H1W2 102.4 . . ? H2W1 O2W H2W2 107.7 . . ? H3W1 O3W H3W2 102.2 . . ? H4W1 O4W H4W2 107.7 . . ? H5W1 O5W H5W2 116.4 . . ? H6W1 O6W H6W2 107.7 . . ? H7W1 O7W H7W2 108.7 . . ? H8W1 O8W H8W2 107.7 . . ? H9W1 O9W H9W2 109.0 . . ? 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 C6A C1A C2A C3A -1.1(6) . . . . ? C7D C1A C2A C3A 177.8(4) . . . . ? C1A C2A C3A C4A 1.2(7) . . . . ? C2A C3A C4A C5A 0.1(7) . . . . ? C3A C4A C5A C6A -1.2(6) . . . . ? C3A C4A C5A C7A -179.2(4) . . . . ? C2A C1A C6A O1A 178.2(3) . . . . ? C7D C1A C6A O1A -0.8(6) . . . . ? C2A C1A C6A C5A -0.1(6) . . . . ? C7D C1A C6A C5A -179.1(4) . . . . ? C4A C5A C6A O1A -176.9(3) . . . . ? C7A C5A C6A O1A 1.0(6) . . . . ? C4A C5A C6A C1A 1.2(6) . . . . ? C7A C5A C6A C1A 179.1(4) . . . . ? C4A C5A C7A C1B -110.6(5) . . . . ? C6A C5A C7A C1B 71.6(5) . . . . ? C5A C7A C1B C6B -98.7(5) . . . . ? C5A C7A C1B C2B 81.8(5) . . . . ? C6B C1B C2B C3B 0.5(6) . . . . ? C7A C1B C2B C3B 180.0(4) . . . . ? C1B C2B C3B C4B 0.9(7) . . . . ? C2B C3B C4B C5B 0.2(7) . . . . ? C3B C4B C5B C6B -2.4(6) . . . . ? C3B C4B C5B C7B 175.2(4) . . . . ? C2B C1B C6B C5B -2.9(7) . . . . ? C7A C1B C6B C5B 177.6(4) . . . . ? C2B C1B C6B O1B -178.5(4) . . . . ? C7A C1B C6B O1B 2.0(6) . . . . ? C4B C5B C6B C1B 3.9(7) . . . . ? C7B C5B C6B C1B -173.7(4) . . . . ? C4B C5B C6B O1B 179.5(3) . . . . ? C7B C5B C6B O1B 1.9(6) . . . . ? C4B C5B C7B C1C -83.4(5) . . . . ? C6B C5B C7B C1C 94.1(5) . . . . ? C1B C6B O1B P1B -95.3(4) . . . . ? C5B C6B O1B P1B 88.8(4) . . . . ? C6B O1B P1B O2B -26.1(4) . . . . ? C6B O1B P1B O4B 94.9(3) . . . . ? C6B O1B P1B O3B -147.3(3) . . . . ? C5B C7B C1C C6C -85.0(5) . . . . ? C5B C7B C1C C2C 91.6(5) . . . . ? C6C C1C C2C C3C -0.1(6) . . . . ? C7B C1C C2C C3C -176.8(4) . . . . ? C1C C2C C3C C4C 1.2(6) . . . . ? C2C C3C C4C C5C -0.9(6) . . . . ? C3C C4C C5C C6C -0.6(6) . . . . ? C3C C4C C5C C7C 173.8(4) . . . . ? C2C C1C C6C O1C 177.5(4) . . . . ? C7B C1C C6C O1C -5.9(6) . . . . ? C2C C1C C6C C5C -1.5(6) . . . . ? C7B C1C C6C C5C 175.0(4) . . . . ? C4C C5C C6C C1C 1.9(6) . . . . ? C7C C5C C6C C1C -172.4(4) . . . . ? C4C C5C C6C O1C -177.3(3) . . . . ? C7C C5C C6C O1C 8.5(6) . . . . ? C4C C5C C7C C1D -90.9(5) . . . . ? C6C C5C C7C C1D 83.1(5) . . . . ? C5C C7C C1D C2D 66.4(5) . . . . ? C5C C7C C1D C6D -110.3(5) . . . . ? C6D C1D C2D C3D 2.6(6) . . . . ? C7C C1D C2D C3D -174.3(4) . . . . ? C1D C2D C3D C4D 2.6(7) . . . . ? C2D C3D C4D C5D -4.0(7) . . . . ? C3D C4D C5D C6D 0.2(6) . . . . ? C3D C4D C5D C7D 176.2(4) . . . . ? C4D C5D C6D C1D 5.2(6) . . . . ? C7D C5D C6D C1D -170.7(4) . . . . ? C4D C5D C6D O1D -175.5(4) . . . . ? C7D C5D C6D O1D 8.6(6) . . . . ? C2D C1D C6D C5D -6.5(6) . . . . ? C7C C1D C6D C5D 170.3(4) . . . . ? C2D C1D C6D O1D 174.1(4) . . . . ? C7C C1D C6D O1D -9.1(6) . . . . ? C2A C1A C7D C5D 109.9(5) . . . . ? C6A C1A C7D C5D -71.1(5) . . . . ? C4D C5D C7D C1A -64.6(5) . . . . ? C6D C5D C7D C1A 111.2(5) . . . . ? C5D C6D O1D P1D 88.6(4) . . . . ? C1D C6D O1D P1D -92.0(4) . . . . ? C6D O1D P1D O3D -92.6(3) . . . . ? C6D O1D P1D O4D 144.1(3) . . . . ? C6D O1D P1D O2D 23.7(3) . . . . ? N4X C1X N1X C3X -178.3(4) . . . . ? N2X C1X N1X C3X 2.9(6) . . . . ? N6X C3X N1X C1X 179.7(4) . . . . ? N3X C3X N1X C1X -1.2(6) . . . . ? N4X C1X N2X C2X -179.6(4) . . . . ? N1X C1X N2X C2X -0.9(6) . . . . ? N5X C2X N2X C1X 177.4(3) . . . . ? N3X C2X N2X C1X -3.1(6) . . . . ? N6X C3X N3X C2X 176.8(4) . . . . ? N1X C3X N3X C2X -2.3(6) . . . . ? N5X C2X N3X C3X -175.8(4) . . . . ? N2X C2X N3X C3X 4.7(6) . . . . ? N6Y C3Y N1Y C1Y 179.0(4) . . . . ? N3Y C3Y N1Y C1Y -1.3(6) . . . . ? N2Y C1Y N1Y C3Y -1.6(6) . . . . ? N4Y C1Y N1Y C3Y -179.8(4) . . . . ? N4Y C1Y N2Y C2Y -179.0(4) . . . . ? N1Y C1Y N2Y C2Y 2.9(6) . . . . ? N5Y C2Y N2Y C1Y 178.0(3) . . . . ? N3Y C2Y N2Y C1Y -1.6(6) . . . . ? N6Y C3Y N3Y C2Y -177.8(4) . . . . ? N1Y C3Y N3Y C2Y 2.4(6) . . . . ? N5Y C2Y N3Y C3Y 179.4(4) . . . . ? N2Y C2Y N3Y C3Y -1.0(6) . . . . ? N6Z C3Z N3Z C2Z -179.9(4) . . . . ? N1Z C3Z N3Z C2Z 0.4(6) . . . . ? N5Z C2Z N3Z C3Z -177.1(3) . . . . ? N2Z C2Z N3Z C3Z 3.6(6) . . . . ? N4Z C1Z N2Z C2Z -177.7(4) . . . . ? N1Z C1Z N2Z C2Z 0.9(6) . . . . ? N5Z C2Z N2Z C1Z 176.5(3) . . . . ? N3Z C2Z N2Z C1Z -4.2(6) . . . . ? N6Z C3Z N1Z C1Z 177.0(4) . . . . ? N3Z C3Z N1Z C1Z -3.3(6) . . . . ? N4Z C1Z N1Z C3Z -178.7(3) . . . . ? N2Z C1Z N1Z C3Z 2.7(6) . . . . ? 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 O1B 0.84 1.92 2.725(4) 158.9 . O2D H2DO O2B 1.11 1.45 2.542(4) 166.0 4_566 O1C H1C O1B 0.84 2.12 2.797(4) 136.9 . O1C H1C O3B 0.84 2.50 3.187(3) 139.7 . N1X H1X O1W 0.88 1.83 2.677(4) 159.7 . N6X H6X1 N2X 0.88 2.14 3.023(5) 176.4 2_645 N6X H6X2 O8W 0.88 2.18 2.882(5) 136.8 4_565 N6X H6X2 O6W 0.88 2.66 3.259(4) 126.5 1_545 N4X H4X1 N3X 0.88 2.09 2.966(5) 174.6 2_655 N4X H4X2 O1W 0.88 2.34 3.059(4) 138.5 . N4X H4X2 O2W 0.88 2.46 3.165(5) 137.0 . N5X H5X1 O2W 0.88 2.31 3.148(4) 158.6 2_645 N5X H5X2 O6W 0.88 2.17 3.003(5) 157.5 2_645 N1Y H1Y O3B 0.88 1.84 2.691(4) 163.7 . N6Y H6Y1 N2Z 0.88 2.15 3.023(5) 173.0 1_545 N6Y H6Y2 O1S 0.88 2.17 2.844(4) 132.9 . N4Y H4Y1 N3Z 0.88 2.19 3.063(5) 173.4 . N4Y H4Y2 O4B 0.88 1.97 2.843(4) 168.9 . N5Y H5Y1 O9W 0.88 1.98 2.806(4) 154.7 3_666 N5Y H5Y2 O3W 0.88 2.09 2.944(5) 163.7 3_666 N1Z H1Z O4D 0.88 1.84 2.691(4) 161.8 2_656 N6Z H6Z1 N2Y 0.88 2.13 3.003(5) 172.2 . N6Z H6Z2 O3W 0.88 2.21 2.885(4) 133.3 3_666 N6Z H6Z2 O4D 0.88 2.54 3.222(4) 134.9 2_656 N5Z H5Z2 O1S 0.88 2.05 2.908(4) 166.2 1_565 N5Z H5Z1 O8W 0.88 2.16 2.888(4) 139.1 . N4Z H4Z1 N3Y 0.88 2.26 3.133(5) 174.0 1_565 N4Z H4Z2 O3D 0.88 2.04 2.895(4) 164.3 2_656 O1S H1S O3D 0.84 1.99 2.770(4) 153.6 4_565 O1S H1S O2D 0.84 2.61 3.291(4) 138.9 4_565 O1W H1W1 O3B 0.85 1.89 2.722(4) 165.0 4_565 O1W H1W2 O1D 1.01 2.11 2.968(4) 141.7 4_565 O1W H1W2 O1A 1.01 2.30 3.079(4) 133.1 4_565 O2W H2W1 O4D 0.85 1.91 2.759(4) 172.4 4_565 O2W H2W2 O1C 0.85 2.24 3.048(4) 157.8 4_565 O3W H3W1 O2B 1.06 1.98 2.972(4) 154.0 . O3W H3W1 O4B 1.06 2.37 3.201(4) 134.2 . O3W H3W2 O4W 0.90 1.90 2.791(6) 166.0 . O4W H4W1 O2W 0.85 1.97 2.799(5) 164.0 . O4W H4W2 O5W 0.85 2.36 3.049(5) 138.6 . O5W H5W2 O2B 1.19 1.61 2.779(4) 166.9 . O6W H6W1 O4W 0.85 1.93 2.726(5) 156.4 . O6W H6W2 O9W 0.85 2.01 2.821(4) 158.7 . O7W H7W1 O4B 1.20 1.61 2.790(4) 166.5 . O7W H7W2 O5W 1.10 1.88 2.897(5) 150.9 . O8W H8W2 O6W 0.85 1.99 2.725(4) 143.9 4_576 O8W H8W1 O4B 0.85 1.96 2.731(4) 150.2 . O9W H9W1 O7W 0.85 1.87 2.704(4) 168.2 . O9W H9W2 O3D 1.10 1.67 2.755(4) 171.6 4_575 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 21.98 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.239 _refine_diff_density_min -0.318 _refine_diff_density_rms 0.054