# Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2003 data_publ # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof. Allan H. White' _publ_contact_author_address ; Chemistry Section, School of Biomedical and Chemical Sciences, University of Western Australia, 35 Stirling Highway, Crawley, 6009, W.A., Australia ; _publ_contact_author_email ahw@crystal.uwa.edu.au _publ_contact_author_fax '+618 9380-1005' _publ_contact_author_phone '+618 9380-3144' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this submission for publication as a New Structure paper . The figures, chemical structure diagram (scheme), Transfer of Copyright Agreement form and structure factor listing will be sent on receipt of your acknowledgement email or letter. ; # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_coden_Cambridge 0177 _journal_name_full Org.Biomol.Chem. _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? # 3. TITLE AND AUTHOR LIST _publ_section_title ; Alkali Metal Ion Complexes of Functionalised Calixarenes - Competition between Pendent Arm and Anion Bonding to Sodium ; loop_ _publ_author_name _publ_author_address 'Rym Abidi' ; Facult\'e des Sciences, Universit\'e de Bizerte, 7021 Zarzouna-Bizerte, Tunisia ; 'Jack M. Harrowfield' ; Chemistry Section, School of Biomedical and Chemical Sciences, University of Western Australia, 35 Stirling Highway, Crawley, 6009, W.A., Australia ; 'Alexandre N. Sobolev' ; Chemistry Section, School of Biomedical and Chemical Sciences, University of Western Australia, 35 Stirling Highway, Crawley, 6009, W.A., Australia ; 'Jacques Vicens' ; Ecole Europ\'eene de Chimie, Polym\`eres, Mat\'eriaux, Universit\'e Louis Pasteur de Strasbourg, 25 rue Becquerel, Cronenbourg 67087, France ; 'Allan H. White' ; Chemistry Section, School of Biomedical and Chemical Sciences, University of Western Australia, 35 Stirling Highway, Crawley, 6009, W.A., Australia ; # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_acknowledgements ; ? ; _publ_section_references ; Bruker (1997). SMART, SAINT, SADABS (version 5.0), SHELXTL (version 5.1) by G.M. Sheldrick, Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G.M. (1990). Acta Cryst. A46, 467-473. Sheldrick, G.M. (1997). SHELXL97. Program for the Refinement of Crystal Structures. University of G\"ottingen, Germany. Streltsov, V.A. and Zavodnik, V.E. (1989). Sov. Phys. Crystallogr., 34, 824-828. ; # 5. CHEMICAL DATA _publ_section_figure_captions ; ? ; # 6. CRYSTALLOGRAPHY data_ra15lt _database_code_CSD 205946 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? #'p-tert-butylcalix[4]arene(1,3-OCH2CH2OCH3)(2,4-OCH2Ph).Na(CF3O3S)' _chemical_melting_point ? _chemical_formula_moiety 'C64 H80 O6, C2 H3 N, Na, C F3 O3 S' _chemical_formula_sum 'C67 H83 F3 N Na O9 S' _chemical_formula_weight 1158.39 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' F F 0.0171 0.0103 '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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 39.501(9) _cell_length_b 13.177(3) _cell_length_c 24.959(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.709(5) _cell_angle_gamma 90.00 _cell_volume 12841(5) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 4134 _cell_measurement_theta_min 2.08 _cell_measurement_theta_max 25.38 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4944 _exptl_absorpt_coefficient_mu 0.121 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9786 _exptl_absorpt_correction_T_max 0.9904 _exptl_absorpt_process_details 'SADABS - Bruker area detector absorption corrections' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 45658 _diffrn_reflns_av_R_equivalents 0.1078 _diffrn_reflns_av_sigmaI/netI 0.1342 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.38 _reflns_number_total 11500 _reflns_number_gt 5550 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL, v. 5.1' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1502P)^2^+30.1242P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_reflns 11500 _refine_ls_number_parameters 739 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1896 _refine_ls_R_factor_gt 0.0965 _refine_ls_wR_factor_ref 0.3137 _refine_ls_wR_factor_gt 0.2410 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _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 Na1 Na 0.09636(5) 0.41497(15) 0.14032(8) 0.0422(5) Uani 1 1 d . . . S1 S 0.04067(5) 0.59625(15) 0.08417(8) 0.0743(6) Uani 1 1 d . . . O1 O 0.07095(13) 0.5615(4) 0.1159(2) 0.0956(17) Uani 1 1 d . . . O2 O 0.01029(14) 0.5584(5) 0.0999(3) 0.126(2) Uani 1 1 d . . . O3 O 0.0402(2) 0.5946(5) 0.0274(2) 0.134(3) Uani 1 1 d . . . C0 C 0.0401(3) 0.7316(9) 0.0964(6) 0.129(4) Uani 1 1 d . . . F1 F 0.01485(17) 0.7782(4) 0.0652(3) 0.154(3) Uani 1 1 d . . . F2 F 0.0679(2) 0.7756(5) 0.0863(4) 0.195(4) Uani 1 1 d . . . F3 F 0.0361(3) 0.7515(8) 0.1446(4) 0.246(5) Uani 1 1 d . . . N01 N 0.21084(16) -0.0134(5) 0.2137(3) 0.0814(18) Uani 1 1 d . . . C01 C 0.19247(16) 0.0531(5) 0.2017(2) 0.0501(14) Uani 1 1 d . . . C02 C 0.16981(14) 0.1369(4) 0.1867(2) 0.0461(14) Uani 1 1 d . . . C1 C 0.09781(12) 0.2872(4) 0.2890(2) 0.0392(12) Uani 1 1 d . . . C11 C 0.07452(12) 0.2021(4) 0.1984(2) 0.0403(13) Uani 1 1 d . . . C12 C 0.08869(12) 0.1947(4) 0.2531(2) 0.0382(12) Uani 1 1 d . . . C13 C 0.09700(13) 0.0986(4) 0.2745(2) 0.0414(13) Uani 1 1 d . . . C14 C 0.09249(13) 0.0110(4) 0.2428(2) 0.0439(13) Uani 1 1 d . . . C141 C 0.09993(15) -0.0955(4) 0.2670(2) 0.0509(15) Uani 1 1 d . . . C142 C 0.12017(17) -0.0900(5) 0.3244(3) 0.0622(17) Uani 1 1 d . . . C143 C 0.12107(17) -0.1564(5) 0.2311(3) 0.0664(18) Uani 1 1 d . . . C144 C 0.06565(16) -0.1482(5) 0.2694(3) 0.0620(17) Uani 1 1 d . . . C15 C 0.08016(14) 0.0226(4) 0.1880(2) 0.0448(13) Uani 1 1 d . . . C16 C 0.07119(12) 0.1171(4) 0.1645(2) 0.0403(13) Uani 1 1 d . . . O11 O 0.06357(8) 0.2969(3) 0.17716(14) 0.0413(9) Uani 1 1 d . . . C111 C 0.02963(14) 0.3265(5) 0.1896(3) 0.0553(16) Uani 1 1 d . . . C112 C 0.00100(16) 0.2655(6) 0.1567(2) 0.0667(19) Uani 1 1 d . . . C113 C -0.00665(17) 0.1692(7) 0.1736(3) 0.074(2) Uani 1 1 d . . . C114 C -0.0309(2) 0.1104(9) 0.1417(4) 0.106(3) Uani 1 1 d . . . C115 C -0.0467(2) 0.1414(10) 0.0955(5) 0.122(4) Uani 1 1 d . . . C116 C -0.0414(2) 0.2396(10) 0.0775(4) 0.105(3) Uani 1 1 d . . . C117 C -0.01615(18) 0.3008(8) 0.1077(3) 0.088(3) Uani 1 1 d . . . C2 C 0.19453(13) 0.4767(4) 0.21830(19) 0.0328(11) Uani 1 1 d . . . C21 C 0.14709(12) 0.3902(3) 0.26037(18) 0.0314(11) Uani 1 1 d . . . C22 C 0.18178(12) 0.4048(3) 0.25821(18) 0.0311(11) Uani 1 1 d . . . C23 C 0.20541(12) 0.3449(4) 0.29092(18) 0.0325(11) Uani 1 1 d . . . C24 C 0.19526(13) 0.2666(4) 0.32342(18) 0.0330(11) Uani 1 1 d . . . C241 C 0.22257(13) 0.2005(4) 0.3577(2) 0.0391(12) Uani 1 1 d . . . C242 C 0.23403(19) 0.2512(5) 0.4118(3) 0.079(2) Uani 1 1 d . . . C243 C 0.25310(17) 0.1824(5) 0.3286(3) 0.0695(19) Uani 1 1 d . . . C244 C 0.20834(17) 0.0923(5) 0.3666(3) 0.0703(19) Uani 1 1 d . . . C25 C 0.16047(13) 0.2530(4) 0.32314(19) 0.0349(12) Uani 1 1 d . . . C26 C 0.13566(12) 0.3132(4) 0.29164(18) 0.0328(11) Uani 1 1 d . . . O21 O 0.12266(8) 0.4508(2) 0.22875(13) 0.0347(8) Uani 1 1 d . . . C211 C 0.11937(14) 0.5522(4) 0.2509(2) 0.0440(13) Uani 1 1 d . . . C212 C 0.09825(17) 0.5543(5) 0.2972(3) 0.0584(16) Uani 1 1 d . . . O213 O 0.06460(12) 0.5332(3) 0.27617(19) 0.0723(13) Uani 1 1 d . . . C214 C 0.0432(2) 0.5372(7) 0.3177(4) 0.101(3) Uani 1 1 d . . . C3 C 0.15528(12) 0.3185(4) 0.03252(19) 0.0325(11) Uani 1 1 d . . . C31 C 0.17800(12) 0.4074(4) 0.12219(18) 0.0322(11) Uani 1 1 d . . . C32 C 0.18265(13) 0.3409(4) 0.08012(19) 0.0348(12) Uani 1 1 d . . . C33 C 0.21418(12) 0.2894(4) 0.0852(2) 0.0341(11) Uani 1 1 d . . . C34 C 0.23965(12) 0.3006(4) 0.1298(2) 0.0344(11) Uani 1 1 d . . . C341 C 0.27387(13) 0.2449(4) 0.1318(2) 0.0423(13) Uani 1 1 d . . . C342 C 0.29295(16) 0.2897(6) 0.0885(3) 0.074(2) Uani 1 1 d . . . C343 C 0.26744(18) 0.1318(5) 0.1221(4) 0.091(3) Uani 1 1 d . . . C344 C 0.29665(15) 0.2561(6) 0.1866(2) 0.0640(18) Uani 1 1 d . . . C35 C 0.23277(13) 0.3646(4) 0.1716(2) 0.0343(11) Uani 1 1 d . . . C36 C 0.20199(12) 0.4168(3) 0.16895(19) 0.0311(11) Uani 1 1 d . . . O31 O 0.14787(8) 0.4657(2) 0.11646(12) 0.0335(8) Uani 1 1 d . . . C311 C 0.15280(14) 0.5699(4) 0.0984(2) 0.0376(12) Uani 1 1 d . . . C312 C 0.15755(14) 0.5737(4) 0.0400(2) 0.0391(12) Uani 1 1 d . . . C313 C 0.12942(15) 0.5908(4) -0.0001(2) 0.0466(14) Uani 1 1 d . . . C314 C 0.13408(18) 0.5869(4) -0.0547(2) 0.0544(16) Uani 1 1 d . . . C315 C 0.1654(2) 0.5663(4) -0.0687(2) 0.0616(18) Uani 1 1 d . . . C316 C 0.19304(17) 0.5513(4) -0.0293(2) 0.0538(15) Uani 1 1 d . . . C317 C 0.18955(14) 0.5551(4) 0.0250(2) 0.0418(13) Uani 1 1 d . . . C4 C 0.06031(13) 0.1246(4) 0.1036(2) 0.0443(13) Uani 1 1 d . . . C41 C 0.10563(12) 0.2174(4) 0.05972(19) 0.0348(12) Uani 1 1 d . . . C42 C 0.09152(13) 0.1265(4) 0.0750(2) 0.0409(13) Uani 1 1 d . . . C43 C 0.10830(14) 0.0366(4) 0.0662(2) 0.0447(13) Uani 1 1 d . . . C44 C 0.13930(14) 0.0343(4) 0.0450(2) 0.0423(13) Uani 1 1 d . . . C441 C 0.15687(15) -0.0667(4) 0.0346(2) 0.0481(14) Uani 1 1 d . . . C442 C 0.1580(2) -0.1385(5) 0.0833(3) 0.073(2) Uani 1 1 d . . . C443 C 0.19324(15) -0.0519(5) 0.0237(3) 0.0590(17) Uani 1 1 d . . . C444 C 0.13630(18) -0.1167(5) -0.0154(3) 0.074(2) Uani 1 1 d . . . C45 C 0.15319(13) 0.1269(4) 0.0338(2) 0.0375(12) Uani 1 1 d . . . C46 C 0.13713(12) 0.2195(4) 0.04147(19) 0.0349(12) Uani 1 1 d . . . O41 O 0.08826(8) 0.3086(3) 0.06481(13) 0.0393(8) Uani 1 1 d . . . C411 C 0.05874(14) 0.3257(4) 0.0232(2) 0.0495(14) Uani 1 1 d . . . C412 C 0.06697(17) 0.3724(6) -0.0271(3) 0.0692(19) Uani 1 1 d . . . O413 O 0.08752(14) 0.3118(5) -0.0553(2) 0.1006(19) Uani 1 1 d . . . C414 C 0.0699(3) 0.2191(9) -0.0776(4) 0.142(5) Uani 1 1 d . . . H02A H 0.1496 0.1131 0.1622 0.069 Uiso 1 1 calc R . . H02B H 0.1817 0.1888 0.1685 0.069 Uiso 1 1 calc R . . H02C H 0.1626 0.1659 0.2193 0.069 Uiso 1 1 calc R . . H1A H 0.0928 0.2731 0.3260 0.047 Uiso 1 1 calc R . . H1B H 0.0837 0.3457 0.2743 0.047 Uiso 1 1 calc R . . H111A H 0.0259 0.3996 0.1817 0.066 Uiso 1 1 calc R . . H111B H 0.0290 0.3160 0.2287 0.066 Uiso 1 1 calc R . . H113 H 0.0047 0.1435 0.2071 0.089 Uiso 1 1 calc R . . H114 H -0.0360 0.0449 0.1543 0.127 Uiso 1 1 calc R . . H115 H -0.0621 0.0972 0.0738 0.147 Uiso 1 1 calc R . . H116 H -0.0547 0.2648 0.0453 0.127 Uiso 1 1 calc R . . H117 H -0.0109 0.3658 0.0946 0.105 Uiso 1 1 calc R . . H13 H 0.1060 0.0926 0.3119 0.050 Uiso 1 1 calc R . . H142A H 0.1068 -0.0527 0.3480 0.093 Uiso 1 1 calc R . . H142B H 0.1420 -0.0550 0.3234 0.093 Uiso 1 1 calc R . . H142C H 0.1247 -0.1589 0.3385 0.093 Uiso 1 1 calc R . . H143A H 0.1429 -0.1218 0.2298 0.100 Uiso 1 1 calc R . . H143B H 0.1083 -0.1615 0.1943 0.100 Uiso 1 1 calc R . . H143C H 0.1255 -0.2246 0.2462 0.100 Uiso 1 1 calc R . . H144A H 0.0525 -0.1088 0.2924 0.093 Uiso 1 1 calc R . . H144B H 0.0698 -0.2164 0.2846 0.093 Uiso 1 1 calc R . . H144C H 0.0527 -0.1532 0.2328 0.093 Uiso 1 1 calc R . . H15 H 0.0777 -0.0360 0.1655 0.054 Uiso 1 1 calc R . . H2A H 0.2156 0.5111 0.2357 0.039 Uiso 1 1 calc R . . H2B H 0.1770 0.5291 0.2068 0.039 Uiso 1 1 calc R . . H211A H 0.1085 0.5975 0.2216 0.053 Uiso 1 1 calc R . . H211B H 0.1425 0.5792 0.2642 0.053 Uiso 1 1 calc R . . H212A H 0.1070 0.5030 0.3249 0.070 Uiso 1 1 calc R . . H212B H 0.0999 0.6219 0.3147 0.070 Uiso 1 1 calc R . . H214A H 0.0194 0.5234 0.3017 0.151 Uiso 1 1 calc R . . H214B H 0.0447 0.6048 0.3342 0.151 Uiso 1 1 calc R . . H214C H 0.0508 0.4861 0.3454 0.151 Uiso 1 1 calc R . . H23 H 0.2292 0.3572 0.2914 0.039 Uiso 1 1 calc R . . H242A H 0.2429 0.3190 0.4058 0.118 Uiso 1 1 calc R . . H242B H 0.2521 0.2104 0.4329 0.118 Uiso 1 1 calc R . . H242C H 0.2145 0.2570 0.4316 0.118 Uiso 1 1 calc R . . H243A H 0.2635 0.2476 0.3214 0.104 Uiso 1 1 calc R . . H243B H 0.2455 0.1474 0.2942 0.104 Uiso 1 1 calc R . . H243C H 0.2700 0.1405 0.3513 0.104 Uiso 1 1 calc R . . H244A H 0.2013 0.0596 0.3314 0.105 Uiso 1 1 calc R . . H244B H 0.1886 0.0977 0.3860 0.105 Uiso 1 1 calc R . . H244C H 0.2262 0.0515 0.3881 0.105 Uiso 1 1 calc R . . H25 H 0.1531 0.2010 0.3451 0.042 Uiso 1 1 calc R . . H3A H 0.1658 0.3136 -0.0010 0.039 Uiso 1 1 calc R . . H3B H 0.1384 0.3747 0.0279 0.039 Uiso 1 1 calc R . . H311A H 0.1732 0.5996 0.1210 0.045 Uiso 1 1 calc R . . H311B H 0.1326 0.6113 0.1036 0.045 Uiso 1 1 calc R . . H313 H 0.1075 0.6047 0.0094 0.056 Uiso 1 1 calc R . . H314 H 0.1151 0.5989 -0.0823 0.065 Uiso 1 1 calc R . . H315 H 0.1681 0.5623 -0.1059 0.074 Uiso 1 1 calc R . . H316 H 0.2149 0.5381 -0.0393 0.065 Uiso 1 1 calc R . . H317 H 0.2089 0.5450 0.0520 0.050 Uiso 1 1 calc R . . H33 H 0.2183 0.2449 0.0569 0.041 Uiso 1 1 calc R . . H342A H 0.3150 0.2549 0.0895 0.111 Uiso 1 1 calc R . . H342B H 0.2969 0.3622 0.0956 0.111 Uiso 1 1 calc R . . H342C H 0.2792 0.2806 0.0527 0.111 Uiso 1 1 calc R . . H343A H 0.2894 0.0965 0.1234 0.137 Uiso 1 1 calc R . . H343B H 0.2536 0.1218 0.0865 0.137 Uiso 1 1 calc R . . H343C H 0.2552 0.1045 0.1503 0.137 Uiso 1 1 calc R . . H344A H 0.3183 0.2200 0.1859 0.096 Uiso 1 1 calc R . . H344B H 0.2850 0.2275 0.2151 0.096 Uiso 1 1 calc R . . H344C H 0.3014 0.3282 0.1941 0.096 Uiso 1 1 calc R . . H35 H 0.2497 0.3726 0.2027 0.041 Uiso 1 1 calc R . . H4A H 0.0457 0.0658 0.0908 0.053 Uiso 1 1 calc R . . H4B H 0.0467 0.1872 0.0949 0.053 Uiso 1 1 calc R . . H411A H 0.0423 0.3701 0.0384 0.059 Uiso 1 1 calc R . . H411B H 0.0472 0.2599 0.0140 0.059 Uiso 1 1 calc R . . H412A H 0.0453 0.3875 -0.0513 0.083 Uiso 1 1 calc R . . H412B H 0.0789 0.4376 -0.0178 0.083 Uiso 1 1 calc R . . H414A H 0.0853 0.1793 -0.0967 0.213 Uiso 1 1 calc R . . H414B H 0.0494 0.2377 -0.1031 0.213 Uiso 1 1 calc R . . H414C H 0.0632 0.1786 -0.0481 0.213 Uiso 1 1 calc R . . H43 H 0.0984 -0.0258 0.0748 0.054 Uiso 1 1 calc R . . H442A H 0.1347 -0.1496 0.0910 0.109 Uiso 1 1 calc R . . H442B H 0.1720 -0.1080 0.1150 0.109 Uiso 1 1 calc R . . H442C H 0.1680 -0.2035 0.0749 0.109 Uiso 1 1 calc R . . H443A H 0.2033 -0.1180 0.0172 0.089 Uiso 1 1 calc R . . H443B H 0.2069 -0.0195 0.0551 0.089 Uiso 1 1 calc R . . H443C H 0.1931 -0.0087 -0.0083 0.089 Uiso 1 1 calc R . . H444A H 0.1126 -0.1267 -0.0093 0.111 Uiso 1 1 calc R . . H444B H 0.1465 -0.1825 -0.0218 0.111 Uiso 1 1 calc R . . H444C H 0.1366 -0.0728 -0.0470 0.111 Uiso 1 1 calc R . . H45 H 0.1744 0.1278 0.0203 0.045 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 Na1 0.0434(12) 0.0446(12) 0.0392(11) 0.0015(9) 0.0083(9) -0.0007(9) S1 0.0669(12) 0.0754(13) 0.0808(13) 0.0068(10) 0.0120(10) 0.0150(9) O1 0.066(3) 0.092(4) 0.122(4) 0.039(3) -0.007(3) 0.029(3) O2 0.068(4) 0.155(6) 0.160(6) 0.052(5) 0.028(4) -0.023(4) O3 0.223(8) 0.124(5) 0.060(4) -0.009(3) 0.033(4) -0.011(5) C0 0.092(8) 0.128(9) 0.157(11) -0.062(8) -0.019(7) 0.010(7) F1 0.129(5) 0.095(4) 0.228(8) 0.019(4) -0.006(5) 0.043(4) F2 0.140(6) 0.105(5) 0.313(11) 0.040(6) -0.052(7) -0.038(4) F3 0.326(13) 0.258(10) 0.155(7) -0.131(7) 0.037(8) 0.042(9) N01 0.079(4) 0.079(4) 0.082(4) 0.000(3) -0.002(3) 0.017(4) C01 0.049(4) 0.054(4) 0.047(3) -0.003(3) 0.007(3) -0.002(3) C02 0.049(3) 0.048(3) 0.042(3) 0.000(3) 0.007(3) 0.002(3) C1 0.036(3) 0.042(3) 0.042(3) 0.002(2) 0.015(2) 0.004(2) C11 0.028(3) 0.048(3) 0.048(3) 0.008(3) 0.013(2) -0.001(2) C12 0.030(3) 0.040(3) 0.047(3) 0.006(3) 0.016(2) 0.000(2) C13 0.032(3) 0.047(3) 0.046(3) 0.006(3) 0.005(2) -0.001(2) C14 0.034(3) 0.040(3) 0.058(4) 0.006(3) 0.008(3) -0.009(2) C141 0.052(4) 0.038(3) 0.061(4) 0.005(3) 0.005(3) -0.007(3) C142 0.072(4) 0.043(4) 0.066(4) 0.013(3) -0.005(3) -0.005(3) C143 0.064(4) 0.051(4) 0.084(5) 0.012(3) 0.008(4) 0.009(3) C144 0.067(4) 0.049(4) 0.071(4) 0.016(3) 0.013(3) -0.012(3) C15 0.045(3) 0.041(3) 0.048(3) 0.000(3) 0.007(3) -0.013(3) C16 0.029(3) 0.047(3) 0.044(3) 0.008(3) 0.003(2) -0.006(2) O11 0.0319(19) 0.045(2) 0.050(2) 0.0086(17) 0.0147(16) 0.0093(16) C111 0.037(3) 0.068(4) 0.065(4) 0.001(3) 0.020(3) 0.012(3) C112 0.044(4) 0.111(6) 0.046(4) 0.015(4) 0.011(3) 0.024(4) C113 0.044(4) 0.123(7) 0.058(4) 0.006(4) 0.013(3) -0.016(4) C114 0.065(5) 0.162(9) 0.091(6) 0.007(6) 0.017(5) -0.029(6) C115 0.059(6) 0.174(11) 0.127(9) 0.034(8) -0.008(6) -0.013(6) C116 0.046(5) 0.194(11) 0.071(5) 0.008(7) -0.006(4) 0.020(6) C117 0.050(4) 0.147(8) 0.067(5) 0.023(5) 0.012(4) 0.032(5) C2 0.035(3) 0.029(3) 0.034(3) 0.002(2) 0.005(2) 0.002(2) C21 0.038(3) 0.030(3) 0.028(3) -0.005(2) 0.010(2) 0.004(2) C22 0.041(3) 0.029(3) 0.024(2) -0.004(2) 0.008(2) 0.003(2) C23 0.034(3) 0.034(3) 0.030(3) -0.005(2) 0.006(2) 0.002(2) C24 0.041(3) 0.033(3) 0.026(2) -0.002(2) 0.008(2) 0.001(2) C241 0.043(3) 0.039(3) 0.035(3) 0.004(2) 0.005(2) 0.004(2) C242 0.093(5) 0.073(5) 0.059(4) -0.022(4) -0.027(4) 0.039(4) C243 0.068(4) 0.071(5) 0.073(5) 0.021(4) 0.022(4) 0.033(4) C244 0.067(4) 0.056(4) 0.083(5) 0.023(4) -0.005(4) 0.006(3) C25 0.041(3) 0.035(3) 0.031(3) 0.004(2) 0.012(2) 0.002(2) C26 0.034(3) 0.040(3) 0.027(2) -0.001(2) 0.011(2) 0.002(2) O21 0.0379(19) 0.0292(18) 0.0365(19) 0.0008(15) 0.0041(15) 0.0089(15) C211 0.048(3) 0.027(3) 0.057(3) 0.000(2) 0.009(3) 0.008(2) C212 0.071(5) 0.039(3) 0.064(4) -0.009(3) 0.008(3) 0.016(3) O213 0.067(3) 0.071(3) 0.082(3) -0.006(3) 0.023(3) 0.010(2) C214 0.095(6) 0.096(6) 0.130(7) -0.017(5) 0.077(6) -0.006(5) C3 0.036(3) 0.033(3) 0.029(3) 0.002(2) 0.008(2) 0.003(2) C31 0.035(3) 0.035(3) 0.028(3) 0.005(2) 0.010(2) -0.002(2) C32 0.043(3) 0.030(3) 0.033(3) 0.002(2) 0.013(2) -0.004(2) C33 0.038(3) 0.030(3) 0.036(3) -0.001(2) 0.012(2) 0.001(2) C34 0.037(3) 0.031(3) 0.038(3) 0.004(2) 0.012(2) -0.001(2) C341 0.037(3) 0.047(3) 0.044(3) -0.006(3) 0.009(2) 0.003(2) C342 0.049(4) 0.120(6) 0.057(4) 0.013(4) 0.021(3) 0.014(4) C343 0.052(4) 0.055(4) 0.159(8) -0.024(5) -0.008(5) 0.014(3) C344 0.047(4) 0.091(5) 0.054(4) 0.003(3) 0.007(3) 0.027(3) C35 0.036(3) 0.032(3) 0.036(3) 0.004(2) 0.008(2) -0.007(2) C36 0.036(3) 0.027(3) 0.032(3) 0.004(2) 0.011(2) -0.005(2) O31 0.0375(19) 0.0305(18) 0.0330(18) 0.0041(14) 0.0070(15) 0.0053(15) C311 0.045(3) 0.030(3) 0.038(3) 0.003(2) 0.003(2) 0.003(2) C312 0.047(3) 0.030(3) 0.039(3) 0.007(2) 0.003(2) 0.000(2) C313 0.054(4) 0.038(3) 0.047(3) 0.006(3) 0.004(3) -0.002(3) C314 0.074(4) 0.052(4) 0.033(3) 0.009(3) -0.004(3) -0.002(3) C315 0.106(6) 0.047(4) 0.035(3) 0.009(3) 0.019(4) -0.009(4) C316 0.067(4) 0.048(4) 0.052(4) 0.011(3) 0.028(3) -0.002(3) C317 0.049(3) 0.036(3) 0.040(3) 0.003(2) 0.006(3) -0.008(2) C4 0.032(3) 0.051(3) 0.048(3) 0.002(3) 0.003(2) -0.011(3) C41 0.034(3) 0.038(3) 0.031(3) 0.000(2) -0.002(2) -0.001(2) C42 0.038(3) 0.046(3) 0.039(3) -0.004(2) 0.004(2) -0.005(3) C43 0.048(3) 0.038(3) 0.046(3) 0.001(3) 0.000(3) -0.011(3) C44 0.046(3) 0.037(3) 0.042(3) -0.010(2) 0.000(3) -0.006(2) C441 0.063(4) 0.034(3) 0.048(3) -0.009(3) 0.007(3) -0.002(3) C442 0.093(5) 0.046(4) 0.080(5) 0.001(3) 0.016(4) 0.010(4) C443 0.046(4) 0.045(4) 0.084(5) -0.015(3) 0.003(3) 0.008(3) C444 0.070(5) 0.060(4) 0.084(5) -0.026(4) -0.010(4) 0.002(3) C45 0.036(3) 0.037(3) 0.041(3) 0.002(2) 0.008(2) -0.004(2) C46 0.036(3) 0.040(3) 0.027(3) 0.000(2) 0.002(2) -0.002(2) O41 0.0361(19) 0.045(2) 0.0353(19) 0.0021(16) 0.0018(16) 0.0014(16) C411 0.040(3) 0.050(3) 0.054(4) 0.003(3) -0.009(3) 0.003(3) C412 0.054(4) 0.091(5) 0.059(4) 0.004(4) -0.004(3) 0.003(4) O413 0.077(4) 0.160(6) 0.063(3) 0.006(4) 0.004(3) 0.023(4) C414 0.154(10) 0.163(11) 0.100(7) -0.074(7) -0.006(7) 0.040(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Na1 O1 2.219(5) . ? Na1 O11 2.303(4) . ? Na1 O31 2.304(4) . ? Na1 O41 2.332(4) . ? Na1 O21 2.340(4) . ? S1 O1 1.407(5) . ? S1 O2 1.409(6) . ? S1 O3 1.415(6) . ? S1 C0 1.811(12) . ? C0 F3 1.265(14) . ? C0 F2 1.298(14) . ? C0 F1 1.321(12) . ? N01 C01 1.149(7) . ? C01 C02 1.434(8) . ? C1 C12 1.523(7) . ? C1 C26 1.526(7) . ? C11 C16 1.397(7) . ? C11 O11 1.399(6) . ? C11 C12 1.400(7) . ? C12 C13 1.393(7) . ? C13 C14 1.396(7) . ? C14 C15 1.389(8) . ? C14 C141 1.539(8) . ? C141 C144 1.531(8) . ? C141 C143 1.540(9) . ? C141 C142 1.532(8) . ? C15 C16 1.399(7) . ? C16 C4 1.519(7) . ? O11 C111 1.474(6) . ? C111 C112 1.523(9) . ? C112 C117 1.385(9) . ? C112 C113 1.385(10) . ? C113 C114 1.385(11) . ? C114 C115 1.293(12) . ? C115 C116 1.395(13) . ? C116 C117 1.411(12) . ? C2 C22 1.515(6) . ? C2 C36 1.529(6) . ? C21 C26 1.396(7) . ? C21 C22 1.393(7) . ? C21 O21 1.400(6) . ? C22 C23 1.389(7) . ? C23 C24 1.408(7) . ? C24 C25 1.385(7) . ? C24 C241 1.541(7) . ? C241 C242 1.512(8) . ? C241 C243 1.518(8) . ? C241 C244 1.562(8) . ? C25 C26 1.406(7) . ? O21 C211 1.460(6) . ? C211 C212 1.524(8) . ? C212 O213 1.381(7) . ? O213 C214 1.435(8) . ? C3 C32 1.510(7) . ? C3 C46 1.522(7) . ? C31 C36 1.393(7) . ? C31 C32 1.401(7) . ? C31 O31 1.405(6) . ? C32 C33 1.407(7) . ? C33 C34 1.390(7) . ? C34 C35 1.399(7) . ? C34 C341 1.533(7) . ? C341 C342 1.527(8) . ? C341 C343 1.524(8) . ? C341 C344 1.526(8) . ? C35 C36 1.390(7) . ? O31 C311 1.467(6) . ? C311 C312 1.499(7) . ? C312 C317 1.393(7) . ? C312 C313 1.397(7) . ? C313 C314 1.402(8) . ? C314 C315 1.365(9) . ? C315 C316 1.368(9) . ? C316 C317 1.383(8) . ? C4 C42 1.515(7) . ? C41 C46 1.389(7) . ? C41 O41 1.399(6) . ? C41 C42 1.399(7) . ? C42 C43 1.391(7) . ? C43 C44 1.406(8) . ? C44 C45 1.385(7) . ? C44 C441 1.541(8) . ? C441 C443 1.515(8) . ? C441 C444 1.530(8) . ? C441 C442 1.536(8) . ? C45 C46 1.401(7) . ? O41 C411 1.456(6) . ? C411 C412 1.477(9) . ? C412 O413 1.403(8) . ? O413 C414 1.473(12) . ? 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 O1 Na1 O11 116.06(18) . . ? O1 Na1 O31 93.26(18) . . ? O11 Na1 O31 150.60(15) . . ? O1 Na1 O41 107.5(2) . . ? O11 Na1 O41 84.25(14) . . ? O31 Na1 O41 89.08(13) . . ? O1 Na1 O21 101.61(19) . . ? O11 Na1 O21 87.47(14) . . ? O31 Na1 O21 84.38(13) . . ? O41 Na1 O21 150.51(15) . . ? O1 S1 O2 114.5(4) . . ? O1 S1 O3 116.1(5) . . ? O2 S1 O3 113.1(5) . . ? O1 S1 C0 104.8(5) . . ? O2 S1 C0 105.6(6) . . ? O3 S1 C0 100.7(6) . . ? S1 O1 Na1 138.4(4) . . ? F3 C0 F2 108.9(10) . . ? F3 C0 F1 105.7(10) . . ? F2 C0 F1 105.3(12) . . ? F3 C0 S1 111.7(12) . . ? F2 C0 S1 112.0(8) . . ? F1 C0 S1 112.7(7) . . ? N01 C01 C02 179.4(8) . . ? C12 C1 C26 110.4(4) . . ? C16 C11 O11 119.4(5) . . ? C16 C11 C12 121.5(5) . . ? O11 C11 C12 119.1(5) . . ? C13 C12 C11 118.2(5) . . ? C13 C12 C1 118.7(5) . . ? C11 C12 C1 122.9(5) . . ? C12 C13 C14 122.1(5) . . ? C15 C14 C13 117.6(5) . . ? C15 C14 C141 120.4(5) . . ? C13 C14 C141 122.0(5) . . ? C144 C141 C143 110.3(5) . . ? C144 C141 C14 108.2(5) . . ? C143 C141 C14 109.5(5) . . ? C144 C141 C142 108.9(5) . . ? C143 C141 C142 108.5(5) . . ? C14 C141 C142 111.5(5) . . ? C14 C15 C16 122.6(5) . . ? C11 C16 C15 117.7(5) . . ? C11 C16 C4 122.7(5) . . ? C15 C16 C4 119.5(5) . . ? C11 O11 C111 113.3(4) . . ? C11 O11 Na1 126.4(3) . . ? C111 O11 Na1 119.3(3) . . ? O11 C111 C112 111.8(5) . . ? C117 C112 C113 118.5(8) . . ? C117 C112 C111 121.5(7) . . ? C113 C112 C111 119.9(6) . . ? C114 C113 C112 120.1(8) . . ? C115 C114 C113 122.3(10) . . ? C114 C115 C116 120.3(11) . . ? C115 C116 C117 119.2(8) . . ? C112 C117 C116 119.4(9) . . ? C22 C2 C36 109.3(4) . . ? C26 C21 C22 121.6(4) . . ? C26 C21 O21 118.4(4) . . ? C22 C21 O21 119.9(4) . . ? C23 C22 C21 118.5(4) . . ? C23 C22 C2 118.8(4) . . ? C21 C22 C2 122.6(4) . . ? C22 C23 C24 122.0(5) . . ? C25 C24 C23 117.5(4) . . ? C25 C24 C241 122.7(4) . . ? C23 C24 C241 119.8(4) . . ? C242 C241 C243 110.2(5) . . ? C242 C241 C24 109.6(4) . . ? C243 C241 C24 111.3(4) . . ? C242 C241 C244 110.0(5) . . ? C243 C241 C244 104.7(5) . . ? C24 C241 C244 111.0(4) . . ? C24 C25 C26 122.5(4) . . ? C21 C26 C25 117.8(4) . . ? C21 C26 C1 122.5(4) . . ? C25 C26 C1 119.5(4) . . ? C21 O21 C211 113.6(4) . . ? C21 O21 Na1 125.9(3) . . ? C211 O21 Na1 119.3(3) . . ? O21 C211 C212 113.2(4) . . ? O213 C212 C211 108.3(5) . . ? C212 O213 C214 110.9(6) . . ? C32 C3 C46 110.4(4) . . ? C36 C31 C32 122.2(5) . . ? C36 C31 O31 119.7(4) . . ? C32 C31 O31 118.1(4) . . ? C31 C32 C33 116.7(5) . . ? C31 C32 C3 123.5(4) . . ? C33 C32 C3 119.7(4) . . ? C34 C33 C32 123.0(5) . . ? C33 C34 C35 117.5(4) . . ? C33 C34 C341 120.2(4) . . ? C35 C34 C341 122.3(5) . . ? C342 C341 C343 110.7(6) . . ? C342 C341 C344 108.0(5) . . ? C343 C341 C344 107.4(5) . . ? C342 C341 C34 108.6(5) . . ? C343 C341 C34 109.8(4) . . ? C344 C341 C34 112.4(4) . . ? C36 C35 C34 122.0(5) . . ? C35 C36 C31 118.4(4) . . ? C35 C36 C2 119.4(4) . . ? C31 C36 C2 122.1(4) . . ? C31 O31 C311 113.1(4) . . ? C31 O31 Na1 125.6(3) . . ? C311 O31 Na1 121.0(3) . . ? O31 C311 C312 111.9(4) . . ? C317 C312 C313 119.4(5) . . ? C317 C312 C311 120.5(5) . . ? C313 C312 C311 120.0(5) . . ? C314 C313 C312 118.9(6) . . ? C315 C314 C313 121.0(6) . . ? C314 C315 C316 119.9(6) . . ? C315 C316 C317 120.9(6) . . ? C316 C317 C312 119.9(5) . . ? C42 C4 C16 110.2(4) . . ? C46 C41 O41 119.3(4) . . ? C46 C41 C42 121.3(5) . . ? O41 C41 C42 119.3(4) . . ? C43 C42 C41 117.8(5) . . ? C43 C42 C4 120.1(5) . . ? C41 C42 C4 122.0(5) . . ? C42 C43 C44 122.8(5) . . ? C45 C44 C43 116.8(5) . . ? C45 C44 C441 121.7(5) . . ? C43 C44 C441 121.5(5) . . ? C443 C441 C444 108.1(5) . . ? C443 C441 C442 107.9(5) . . ? C444 C441 C442 109.2(5) . . ? C443 C441 C44 112.5(5) . . ? C444 C441 C44 108.2(5) . . ? C442 C441 C44 110.9(5) . . ? C44 C45 C46 122.5(5) . . ? C41 C46 C45 118.4(5) . . ? C41 C46 C3 122.0(4) . . ? C45 C46 C3 119.5(4) . . ? C41 O41 C411 114.8(4) . . ? C41 O41 Na1 125.5(3) . . ? C411 O41 Na1 118.7(3) . . ? O41 C411 C412 114.5(5) . . ? O413 C412 C411 114.2(6) . . ? C412 O413 C414 112.7(7) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 25.38 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.886 _refine_diff_density_min -0.638 _refine_diff_density_rms 0.078 data_ra15-RT _database_code_CSD 207213 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? #'p-tert-butylcalix[4]arene(1,3-OCH2CH2OCH3)(2,4-OCH2Ph).Na(CF3O3S)' _chemical_melting_point ? _chemical_formula_moiety 'C62 H80 O6, C2 H3 N, Na, C F3 O3 S' _chemical_formula_sum 'C67 H83 F3 N Na O9 S' _chemical_formula_weight 1158.39 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' F F 0.0171 0.0103 '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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 40.086(8) _cell_length_b 13.339(3) _cell_length_c 25.135(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.58(3) _cell_angle_gamma 90.00 _cell_volume 13289(5) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 8 _cell_measurement_theta_min 8.31 _cell_measurement_theta_max 9.80 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.158 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4944 _exptl_absorpt_coefficient_mu 0.117 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0 _exptl_absorpt_correction_T_max 0 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Enraf-Nonius CAD-4' _diffrn_measurement_method 2theta/theta _diffrn_standards_number 6 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 3.0 _diffrn_reflns_number 17087 _diffrn_reflns_av_R_equivalents 0.1463 _diffrn_reflns_av_sigmaI/netI 0.2048 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 22.50 _reflns_number_total 8674 _reflns_number_gt 2723 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_cell_refinement 'CAD-4 Software (Enraf-Nonius, 1989)' _computing_data_reduction 'PROFIT (Streltsov & Zavodnik, 1989)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL, v. 5.1' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2284P)^2^+10.4322P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00028(16) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8674 _refine_ls_number_parameters 655 _refine_ls_number_restraints 167 _refine_ls_R_factor_all 0.3098 _refine_ls_R_factor_gt 0.1420 _refine_ls_wR_factor_ref 0.4700 _refine_ls_wR_factor_gt 0.3620 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.147 _refine_ls_shift/su_mean 0.007 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 Na1 Na 0.09835(11) 0.4133(3) 0.14468(19) 0.0726(15) Uani 1 1 d . . . S1 S 0.0433(4) 0.5987(10) 0.0969(5) 0.190(4) Uiso 0.50 1 d PD A 1 O1 O 0.0649(6) 0.5316(14) 0.1270(9) 0.207(5) Uiso 0.50 1 d PD A 1 O2 O 0.0096(4) 0.5691(16) 0.0921(10) 0.207(5) Uiso 0.50 1 d PD A 1 O3 O 0.0531(7) 0.6081(18) 0.0442(7) 0.207(5) Uiso 0.50 1 d PD A 1 C0 C 0.0481(5) 0.7242(12) 0.1274(8) 0.25(2) Uiso 0.50 1 d PD A 1 F1 F 0.0365(9) 0.7895(13) 0.0905(12) 0.321(8) Uiso 0.50 1 d PD A 1 F2 F 0.0796(6) 0.7393(18) 0.1441(13) 0.321(8) Uiso 0.50 1 d PD A 1 F3 F 0.0304(8) 0.728(2) 0.1663(12) 0.321(8) Uiso 0.50 1 d PD A 1 S1' S 0.0526(3) 0.6291(11) 0.0970(5) 0.190(4) Uiso 0.50 1 d PD A 2 O1' O 0.0733(5) 0.5540(16) 0.1212(9) 0.207(5) Uiso 0.50 1 d PD A 2 O2' O 0.0311(5) 0.5870(19) 0.0502(7) 0.207(5) Uiso 0.50 1 d PD A 2 O3' O 0.0711(6) 0.7069(15) 0.0768(10) 0.207(5) Uiso 0.50 1 d PD A 2 C0' C 0.0242(5) 0.6769(17) 0.1409(7) 0.25(2) Uiso 0.50 1 d PD A 2 F3' F -0.0046(5) 0.629(2) 0.1303(12) 0.321(8) Uiso 0.50 1 d PD A 2 F2' F 0.0364(7) 0.661(3) 0.1908(6) 0.321(8) Uiso 0.50 1 d PD A 2 F1' F 0.0186(8) 0.7716(17) 0.1316(13) 0.321(8) Uiso 0.50 1 d PD A 2 N01 N 0.2092(4) -0.0130(14) 0.2122(7) 0.155(6) Uiso 1 1 d . . . C01 C 0.1919(5) 0.0518(15) 0.2017(7) 0.122(6) Uiso 1 1 d . . . C02 C 0.1711(3) 0.1332(11) 0.1917(5) 0.094(4) Uiso 1 1 d . . . H01 H 0.1522 0.1159 0.1652 0.141 Uiso 1 1 calc R . . H02 H 0.1833 0.1875 0.1786 0.141 Uiso 1 1 calc R . . H03 H 0.1632 0.1532 0.2244 0.141 Uiso 1 1 calc R . . C1 C 0.1016(3) 0.2927(9) 0.2935(4) 0.063(3) Uani 1 1 d . . . H1A H 0.0881 0.3490 0.2783 0.075 Uiso 1 1 calc R . . H1B H 0.0973 0.2825 0.3300 0.075 Uiso 1 1 calc R . . C11 C 0.0773(3) 0.2086(10) 0.2065(5) 0.063(3) Uani 1 1 d . . . C12 C 0.0918(3) 0.1995(10) 0.2604(5) 0.063(3) Uani 1 1 d . A . C13 C 0.0996(3) 0.1069(9) 0.2823(5) 0.065(3) Uani 1 1 d . . . H13A H 0.1093 0.1018 0.3182 0.078 Uiso 1 1 calc R A . C14 C 0.0931(3) 0.0206(9) 0.2517(6) 0.073(4) Uani 1 1 d D A . C141 C 0.0998(3) -0.0828(9) 0.2776(5) 0.093(5) Uani 1 1 d D . . C142 C 0.1174(4) -0.0778(10) 0.3360(5) 0.136(7) Uani 1 1 d D A . H14A H 0.1038 -0.0400 0.3571 0.205 Uiso 1 1 calc R . . H14B H 0.1390 -0.0459 0.3372 0.205 Uiso 1 1 calc R . . H14C H 0.1205 -0.1445 0.3503 0.205 Uiso 1 1 calc R . . C143 C 0.1221(4) -0.1452(12) 0.2453(6) 0.135(6) Uani 1 1 d D A . H14D H 0.1115 -0.1499 0.2086 0.202 Uiso 1 1 calc R . . H14E H 0.1250 -0.2113 0.2605 0.202 Uiso 1 1 calc R . . H14F H 0.1437 -0.1135 0.2468 0.202 Uiso 1 1 calc R . . C144 C 0.0665(3) -0.1392(11) 0.2769(6) 0.123(6) Uani 1 1 d D A . H14G H 0.0551 -0.1440 0.2405 0.185 Uiso 1 1 calc R . . H14H H 0.0525 -0.1037 0.2983 0.185 Uiso 1 1 calc R . . H14I H 0.0710 -0.2053 0.2913 0.185 Uiso 1 1 calc R . . C15 C 0.0813(3) 0.0297(11) 0.1981(6) 0.082(4) Uani 1 1 d . . . H15A H 0.0787 -0.0278 0.1769 0.098 Uiso 1 1 calc R A . C16 C 0.0731(3) 0.1201(12) 0.1746(5) 0.072(4) Uani 1 1 d . A . O11 O 0.06690(19) 0.3002(6) 0.1841(3) 0.072(2) Uani 1 1 d . A . C111 C 0.0336(3) 0.3306(10) 0.1973(6) 0.087(4) Uani 1 1 d . . . H11A H 0.0320 0.3098 0.2338 0.104 Uiso 1 1 calc R A . H11B H 0.0320 0.4032 0.1961 0.104 Uiso 1 1 calc R . . C112 C 0.0051(3) 0.2886(13) 0.1613(5) 0.099(5) Uani 1 1 d G A . C113 C -0.0068(4) 0.1973(14) 0.1713(6) 0.152(9) Uani 1 1 d G . . H11C H 0.0021 0.1629 0.2023 0.183 Uiso 1 1 calc R A . C114 C -0.0318(4) 0.1560(13) 0.1364(8) 0.26(2) Uani 1 1 d G A . H11D H -0.0401 0.0930 0.1433 0.311 Uiso 1 1 calc R . . C115 C -0.0448(4) 0.2059(17) 0.0915(8) 0.37(4) Uani 1 1 d G . . H11E H -0.0620 0.1774 0.0674 0.443 Uiso 1 1 calc R A . C116 C -0.0328(4) 0.2971(16) 0.0815(6) 0.28(2) Uani 1 1 d G A . H11F H -0.0417 0.3316 0.0505 0.340 Uiso 1 1 calc R . . C117 C -0.0078(4) 0.3385(12) 0.1164(6) 0.157(9) Uani 1 1 d G . . H11G H 0.0005 0.4015 0.1095 0.188 Uiso 1 1 calc R A . C2 C 0.1960(3) 0.4707(8) 0.2160(4) 0.059(3) Uani 1 1 d . . . H2A H 0.1791 0.5215 0.2048 0.071 Uiso 1 1 calc R . . H2B H 0.2166 0.5043 0.2316 0.071 Uiso 1 1 calc R . . C21 C 0.1498(3) 0.3889(8) 0.2613(4) 0.056(3) Uani 1 1 d . . . C22 C 0.1838(3) 0.4040(8) 0.2582(5) 0.058(3) Uani 1 1 d . A . C23 C 0.2071(3) 0.3445(8) 0.2907(4) 0.052(3) Uani 1 1 d . . . H23A H 0.2299 0.3548 0.2896 0.063 Uiso 1 1 calc R A . C24 C 0.1981(3) 0.2718(8) 0.3242(4) 0.057(3) Uani 1 1 d D A . C241 C 0.2242(2) 0.2071(8) 0.3590(4) 0.067(3) Uani 1 1 d D . . C242 C 0.2310(6) 0.2422(17) 0.4162(7) 0.096(9) Uiso 0.50 1 d PD A 1 H24A H 0.2388 0.3104 0.4172 0.144 Uiso 0.50 1 calc PR A 1 H24B H 0.2480 0.2005 0.4361 0.144 Uiso 0.50 1 calc PR A 1 H24C H 0.2107 0.2382 0.4320 0.144 Uiso 0.50 1 calc PR A 1 C243 C 0.2575(5) 0.2058(18) 0.3385(10) 0.101(9) Uiso 0.50 1 d PD A 1 H24D H 0.2663 0.2727 0.3387 0.151 Uiso 0.50 1 calc PR A 1 H24E H 0.2544 0.1799 0.3025 0.151 Uiso 0.50 1 calc PR A 1 H24F H 0.2730 0.1638 0.3613 0.151 Uiso 0.50 1 calc PR A 1 C244 C 0.2131(5) 0.0995(12) 0.3608(9) 0.068(7) Uiso 0.50 1 d PD A 1 H24G H 0.2302 0.0615 0.3830 0.102 Uiso 0.50 1 calc PR A 1 H24H H 0.2098 0.0723 0.3250 0.102 Uiso 0.50 1 calc PR A 1 H24I H 0.1924 0.0960 0.3754 0.102 Uiso 0.50 1 calc PR A 1 C245 C 0.2494(6) 0.2742(18) 0.3918(10) 0.116(11) Uiso 0.50 1 d PD A 2 H24J H 0.2487 0.3396 0.3757 0.174 Uiso 0.50 1 calc PR A 2 H24K H 0.2716 0.2465 0.3929 0.174 Uiso 0.50 1 calc PR A 2 H24L H 0.2442 0.2793 0.4277 0.174 Uiso 0.50 1 calc PR A 2 C246 C 0.2433(7) 0.146(2) 0.3241(10) 0.126(12) Uiso 0.50 1 d PD A 2 H24M H 0.2589 0.1876 0.3089 0.189 Uiso 0.50 1 calc PR A 2 H24N H 0.2279 0.1156 0.2957 0.189 Uiso 0.50 1 calc PR A 2 H24O H 0.2555 0.0938 0.3452 0.189 Uiso 0.50 1 calc PR A 2 C247 C 0.2113(8) 0.137(2) 0.3977(11) 0.178(17) Uiso 0.50 1 d PD A 2 H24P H 0.2079 0.1726 0.4295 0.267 Uiso 0.50 1 calc PR A 2 H24Q H 0.2274 0.0841 0.4071 0.267 Uiso 0.50 1 calc PR A 2 H24R H 0.1903 0.1083 0.3812 0.267 Uiso 0.50 1 calc PR A 2 C25 C 0.1642(3) 0.2595(8) 0.3234(4) 0.059(3) Uani 1 1 d . . . H25A H 0.1574 0.2085 0.3446 0.071 Uiso 1 1 calc R A . C26 C 0.1390(3) 0.3158(9) 0.2939(5) 0.059(3) Uani 1 1 d . A . O21 O 0.12583(19) 0.4487(5) 0.2305(3) 0.063(2) Uani 1 1 d D A . C211 C 0.1239(3) 0.5515(7) 0.2514(5) 0.084(4) Uiso 0.50 1 d PD A 1 H21A H 0.1136 0.5949 0.2225 0.101 Uiso 0.50 1 calc PR A 1 H21G H 0.1465 0.5761 0.2635 0.101 Uiso 0.50 1 calc PR A 1 C212 C 0.1031(4) 0.5568(17) 0.2984(7) 0.101(7) Uiso 0.50 1 d PD A 1 H21B H 0.1121 0.5107 0.3268 0.121 Uiso 0.50 1 calc PR A 1 H21C H 0.1036 0.6241 0.3131 0.121 Uiso 0.50 1 calc PR A 1 O213 O 0.0696(4) 0.5294(17) 0.2757(8) 0.126(6) Uiso 0.50 1 d PD A 1 C214 C 0.0460(5) 0.552(4) 0.3115(14) 0.196(14) Uiso 0.50 1 d PD A 1 H21D H 0.0236 0.5352 0.2944 0.295 Uiso 0.50 1 calc PR A 1 H21E H 0.0471 0.6216 0.3203 0.295 Uiso 0.50 1 calc PR A 1 H21F H 0.0514 0.5127 0.3438 0.295 Uiso 0.50 1 calc PR A 1 C21' C 0.1239(3) 0.5515(7) 0.2514(5) 0.084(4) Uiso 0.50 1 d P A 2 H21H H 0.1273 0.5991 0.2235 0.101 Uiso 0.50 1 calc PR A 2 H21I H 0.1417 0.5614 0.2815 0.101 Uiso 0.50 1 calc PR A 2 C22' C 0.0893(5) 0.5719(14) 0.2699(7) 0.101(7) Uiso 0.50 1 d PD A 2 H22A H 0.0863 0.6432 0.2755 0.121 Uiso 0.50 1 calc PR A 2 H22B H 0.0710 0.5487 0.2430 0.121 Uiso 0.50 1 calc PR A 2 O23' O 0.0893(5) 0.5197(16) 0.3181(7) 0.126(6) Uiso 0.50 1 d PD A 2 C24' C 0.0583(8) 0.537(4) 0.3403(13) 0.196(14) Uiso 0.50 1 d PD A 2 H24S H 0.0596 0.5034 0.3743 0.295 Uiso 0.50 1 calc PR A 2 H24T H 0.0395 0.5114 0.3159 0.295 Uiso 0.50 1 calc PR A 2 H24U H 0.0554 0.6076 0.3453 0.295 Uiso 0.50 1 calc PR A 2 C3 C 0.1538(3) 0.3123(8) 0.0351(4) 0.062(3) Uani 1 1 d . . . H3B H 0.1632 0.3059 0.0018 0.074 Uiso 1 1 calc R . . H3C H 0.1380 0.3678 0.0312 0.074 Uiso 1 1 calc R . . C31 C 0.1781(3) 0.4000(8) 0.1226(5) 0.055(3) Uani 1 1 d . . . C32 C 0.1822(3) 0.3337(9) 0.0815(5) 0.058(3) Uani 1 1 d . A . C33 C 0.2119(3) 0.2815(8) 0.0851(5) 0.061(3) Uani 1 1 d . . . H33A H 0.2146 0.2355 0.0583 0.073 Uiso 1 1 calc R A . C34 C 0.2382(3) 0.2952(9) 0.1278(5) 0.061(3) Uani 1 1 d D A . C341 C 0.2721(3) 0.2410(9) 0.1298(5) 0.081(4) Uani 1 1 d D . . C342 C 0.2937(7) 0.3194(19) 0.1056(11) 0.134(13) Uiso 0.50 1 d PD A 1 H34A H 0.2862 0.3251 0.0676 0.201 Uiso 0.50 1 calc PR A 1 H34B H 0.3170 0.2989 0.1116 0.201 Uiso 0.50 1 calc PR A 1 H34C H 0.2915 0.3832 0.1225 0.201 Uiso 0.50 1 calc PR A 1 C343 C 0.2688(8) 0.1469(17) 0.0938(11) 0.139(13) Uiso 0.50 1 d PD A 1 H34D H 0.2545 0.0989 0.1078 0.209 Uiso 0.50 1 calc PR A 1 H34E H 0.2907 0.1181 0.0935 0.209 Uiso 0.50 1 calc PR A 1 H34F H 0.2592 0.1651 0.0579 0.209 Uiso 0.50 1 calc PR A 1 C344 C 0.2889(8) 0.213(2) 0.1867(8) 0.141(14) Uiso 0.50 1 d PD A 1 H34G H 0.2751 0.1652 0.2018 0.211 Uiso 0.50 1 calc PR A 1 H34H H 0.2915 0.2720 0.2088 0.211 Uiso 0.50 1 calc PR A 1 H34I H 0.3107 0.1842 0.1851 0.211 Uiso 0.50 1 calc PR A 1 C345 C 0.2974(6) 0.2707(19) 0.1798(7) 0.094(9) Uiso 0.50 1 d PD A 2 H34J H 0.2919 0.2354 0.2107 0.142 Uiso 0.50 1 calc PR A 2 H34K H 0.2960 0.3416 0.1857 0.142 Uiso 0.50 1 calc PR A 2 H34L H 0.3198 0.2537 0.1741 0.142 Uiso 0.50 1 calc PR A 2 C346 C 0.2878(7) 0.263(2) 0.0789(8) 0.118(11) Uiso 0.50 1 d PD A 2 H34M H 0.2812 0.2113 0.0526 0.176 Uiso 0.50 1 calc PR A 2 H34N H 0.3119 0.2637 0.0877 0.176 Uiso 0.50 1 calc PR A 2 H34O H 0.2800 0.3266 0.0644 0.176 Uiso 0.50 1 calc PR A 2 C347 C 0.2641(7) 0.1286(13) 0.1327(10) 0.103(10) Uiso 0.50 1 d PD A 2 H34P H 0.2458 0.1194 0.1529 0.154 Uiso 0.50 1 calc PR A 2 H34Q H 0.2836 0.0936 0.1502 0.154 Uiso 0.50 1 calc PR A 2 H34R H 0.2578 0.1027 0.0970 0.154 Uiso 0.50 1 calc PR A 2 C35 C 0.2323(3) 0.3591(9) 0.1682(5) 0.067(3) Uani 1 1 d . . . H35A H 0.2492 0.3682 0.1973 0.080 Uiso 1 1 calc R A . C36 C 0.2025(3) 0.4104(8) 0.1675(5) 0.055(3) Uani 1 1 d . A . O31 O 0.14851(19) 0.4591(5) 0.1177(3) 0.063(2) Uani 1 1 d . A . C311 C 0.1537(3) 0.5619(9) 0.0993(5) 0.074(4) Uani 1 1 d . . . H31A H 0.1731 0.5909 0.1216 0.088 Uiso 1 1 calc R A . H31B H 0.1342 0.6023 0.1035 0.088 Uiso 1 1 calc R . . C312 C 0.1593(3) 0.5649(6) 0.0414(4) 0.076(4) Uani 1 1 d G A . C313 C 0.1323(3) 0.5809(7) 0.0017(6) 0.104(5) Uani 1 1 d G . . H31C H 0.1110 0.5918 0.0108 0.125 Uiso 1 1 calc R A . C314 C 0.1370(4) 0.5809(7) -0.0512(5) 0.118(6) Uani 1 1 d G A . H31D H 0.1187 0.5918 -0.0781 0.142 Uiso 1 1 calc R . . C315 C 0.1685(4) 0.5648(8) -0.0646(4) 0.138(8) Uani 1 1 d G . . H31E H 0.1716 0.5648 -0.1005 0.166 Uiso 1 1 calc R A . C316 C 0.1954(3) 0.5488(7) -0.0249(6) 0.119(6) Uani 1 1 d G A . H31F H 0.2168 0.5379 -0.0340 0.143 Uiso 1 1 calc R . . C317 C 0.1908(3) 0.5488(6) 0.0280(5) 0.090(5) Uani 1 1 d G . . H31G H 0.2090 0.5379 0.0549 0.108 Uiso 1 1 calc R A . C4 C 0.0620(3) 0.1274(10) 0.1148(5) 0.068(3) Uani 1 1 d . . . H4A H 0.0492 0.1886 0.1069 0.081 Uiso 1 1 calc R A . H4B H 0.0473 0.0713 0.1032 0.081 Uiso 1 1 calc R . . C41 C 0.1058(3) 0.2143(9) 0.0663(4) 0.057(3) Uani 1 1 d . . . C42 C 0.0919(3) 0.1271(10) 0.0831(5) 0.065(3) Uani 1 1 d . A . C43 C 0.1077(3) 0.0386(10) 0.0741(5) 0.079(4) Uani 1 1 d . . . H43A H 0.0986 -0.0209 0.0851 0.094 Uiso 1 1 calc R A . C44 C 0.1361(3) 0.0334(9) 0.0497(5) 0.073(4) Uani 1 1 d D A . C441 C 0.1521(3) -0.0673(8) 0.0376(5) 0.086(4) Uani 1 1 d D . . C442 C 0.1586(6) -0.1345(17) 0.0882(8) 0.087(9) Uiso 0.50 1 d PD A 1 H44A H 0.1378 -0.1455 0.1018 0.130 Uiso 0.50 1 calc PR A 1 H44B H 0.1744 -0.1021 0.1152 0.130 Uiso 0.50 1 calc PR A 1 H44C H 0.1677 -0.1977 0.0789 0.130 Uiso 0.50 1 calc PR A 1 C443 C 0.1860(4) -0.0524(19) 0.0164(9) 0.080(9) Uiso 0.50 1 d PD A 1 H44D H 0.2033 -0.0361 0.0458 0.119 Uiso 0.50 1 calc PR A 1 H44E H 0.1839 0.0012 -0.0094 0.119 Uiso 0.50 1 calc PR A 1 H44F H 0.1920 -0.1131 -0.0005 0.119 Uiso 0.50 1 calc PR A 1 C444 C 0.1276(6) -0.122(2) -0.0057(8) 0.105(11) Uiso 0.50 1 d PD A 1 H44G H 0.1065 -0.1323 0.0071 0.158 Uiso 0.50 1 calc PR A 1 H44H H 0.1370 -0.1860 -0.0132 0.158 Uiso 0.50 1 calc PR A 1 H44I H 0.1241 -0.0827 -0.0379 0.158 Uiso 0.50 1 calc PR A 1 C445 C 0.1910(4) -0.065(2) 0.0446(11) 0.110(12) Uiso 0.50 1 d PD A 2 H44J H 0.2000 -0.0876 0.0801 0.165 Uiso 0.50 1 calc PR A 2 H44K H 0.1985 0.0022 0.0395 0.165 Uiso 0.50 1 calc PR A 2 H44L H 0.1987 -0.1084 0.0184 0.165 Uiso 0.50 1 calc PR A 2 C446 C 0.1387(7) -0.093(3) -0.0217(7) 0.148(16) Uiso 0.50 1 d PD A 2 H44M H 0.1150 -0.1076 -0.0253 0.223 Uiso 0.50 1 calc PR A 2 H44N H 0.1505 -0.1499 -0.0326 0.223 Uiso 0.50 1 calc PR A 2 H44O H 0.1421 -0.0365 -0.0441 0.223 Uiso 0.50 1 calc PR A 2 C447 C 0.1411(7) -0.151(2) 0.0734(11) 0.144(16) Uiso 0.50 1 d PD A 2 H44P H 0.1183 -0.1390 0.0793 0.216 Uiso 0.50 1 calc PR A 2 H44Q H 0.1557 -0.1515 0.1073 0.216 Uiso 0.50 1 calc PR A 2 H44R H 0.1423 -0.2145 0.0559 0.216 Uiso 0.50 1 calc PR A 2 C45 C 0.1506(3) 0.1235(10) 0.0366(5) 0.073(4) Uani 1 1 d . . . H45A H 0.1705 0.1225 0.0216 0.088 Uiso 1 1 calc R A . C46 C 0.1354(3) 0.2157(9) 0.0458(4) 0.059(3) Uani 1 1 d . A . O41 O 0.08942(19) 0.3051(6) 0.0703(3) 0.069(2) Uani 1 1 d D A . C411 C 0.0583(4) 0.318(2) 0.0318(7) 0.084(6) Uiso 0.50 1 d PD A 1 H41A H 0.0424 0.3569 0.0487 0.101 Uiso 0.50 1 calc PR A 1 H41B H 0.0483 0.2523 0.0234 0.101 Uiso 0.50 1 calc PR A 1 C412 C 0.0633(8) 0.368(2) -0.0196(6) 0.163(11) Uiso 0.50 1 d PD A 1 H41C H 0.0414 0.3761 -0.0416 0.196 Uiso 0.50 1 calc PR A 1 H41D H 0.0725 0.4341 -0.0113 0.196 Uiso 0.50 1 calc PR A 1 O413 O 0.0847(7) 0.316(3) -0.0496(10) 0.198(9) Uiso 0.50 1 d PD A 1 C414 C 0.0693(14) 0.223(3) -0.076(2) 0.29(2) Uiso 0.50 1 d PD A 1 H41E H 0.0853 0.1903 -0.0944 0.440 Uiso 0.50 1 calc PR A 1 H41F H 0.0497 0.2410 -0.1007 0.440 Uiso 0.50 1 calc PR A 1 H41G H 0.0628 0.1794 -0.0487 0.440 Uiso 0.50 1 calc PR A 1 C41' C 0.0673(6) 0.3385(15) 0.0214(7) 0.084(6) Uiso 0.50 1 d PD A 2 H41H H 0.0812 0.3653 -0.0037 0.101 Uiso 0.50 1 calc PR A 2 H41I H 0.0530 0.3924 0.0310 0.101 Uiso 0.50 1 calc PR A 2 C42' C 0.0454(5) 0.258(2) -0.0060(9) 0.163(11) Uiso 0.50 1 d PD A 2 H42A H 0.0383 0.2142 0.0212 0.196 Uiso 0.50 1 calc PR A 2 H42B H 0.0253 0.2883 -0.0257 0.196 Uiso 0.50 1 calc PR A 2 O43' O 0.0613(7) 0.199(2) -0.0421(12) 0.198(9) Uiso 0.50 1 d PD A 2 C44' C 0.0421(13) 0.104(3) -0.057(2) 0.29(2) Uiso 0.50 1 d PD A 2 H44S H 0.0535 0.0656 -0.0811 0.440 Uiso 0.50 1 calc PR A 2 H44T H 0.0198 0.1200 -0.0741 0.440 Uiso 0.50 1 calc PR A 2 H44U H 0.0409 0.0656 -0.0250 0.440 Uiso 0.50 1 calc PR A 2 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 Na1 0.068(3) 0.072(3) 0.078(3) 0.002(3) 0.012(3) 0.002(3) C1 0.060(8) 0.077(9) 0.057(8) 0.001(7) 0.025(6) -0.006(7) C11 0.045(7) 0.069(9) 0.078(10) -0.007(8) 0.020(7) -0.017(7) C12 0.057(8) 0.068(9) 0.067(9) -0.002(8) 0.016(7) -0.005(7) C13 0.062(8) 0.051(8) 0.080(9) 0.002(7) 0.003(7) -0.012(7) C14 0.068(9) 0.083(11) 0.067(10) 0.017(8) 0.006(7) -0.013(7) C141 0.102(12) 0.066(10) 0.115(13) 0.010(9) 0.024(10) -0.012(9) C142 0.21(2) 0.077(11) 0.105(13) 0.037(10) -0.026(13) 0.010(12) C143 0.155(17) 0.089(12) 0.157(17) 0.006(12) 0.012(14) 0.017(12) C144 0.129(14) 0.095(12) 0.154(16) 0.037(11) 0.045(12) -0.026(11) C15 0.103(11) 0.062(9) 0.083(11) 0.005(8) 0.021(9) -0.017(8) C16 0.046(8) 0.093(11) 0.078(10) -0.011(9) 0.013(7) -0.023(7) O11 0.068(6) 0.069(6) 0.080(6) 0.012(5) 0.017(5) 0.003(5) C111 0.071(10) 0.082(10) 0.118(12) 0.001(9) 0.050(9) 0.013(8) C112 0.046(9) 0.171(18) 0.081(12) -0.017(12) 0.010(8) -0.016(11) C113 0.082(13) 0.23(3) 0.155(18) -0.092(17) 0.058(13) -0.064(14) C114 0.16(3) 0.41(5) 0.23(3) -0.21(3) 0.10(2) -0.13(3) C115 0.12(2) 0.72(10) 0.29(5) -0.34(6) 0.10(3) -0.14(4) C116 0.090(18) 0.61(7) 0.14(2) -0.03(3) -0.024(17) 0.11(3) C117 0.085(13) 0.29(3) 0.089(13) 0.025(17) -0.003(11) 0.041(16) C2 0.065(8) 0.044(7) 0.071(8) 0.005(6) 0.018(6) -0.010(6) C21 0.073(9) 0.042(7) 0.049(7) -0.005(6) 0.000(6) 0.022(7) C22 0.047(8) 0.056(8) 0.070(8) -0.002(6) 0.011(6) -0.003(6) C23 0.052(7) 0.056(7) 0.050(7) -0.004(6) 0.010(6) -0.005(6) C24 0.064(9) 0.057(8) 0.054(8) -0.002(6) 0.017(6) 0.007(7) C241 0.047(7) 0.080(9) 0.075(9) 0.001(7) 0.009(6) 0.003(7) C25 0.083(10) 0.048(7) 0.048(7) -0.002(6) 0.013(7) -0.002(7) C26 0.073(9) 0.058(8) 0.048(7) -0.013(7) 0.014(7) -0.003(7) O21 0.077(6) 0.046(5) 0.069(5) -0.006(4) 0.018(4) 0.003(4) C3 0.076(9) 0.064(8) 0.046(7) -0.005(6) 0.013(6) 0.002(7) C31 0.055(8) 0.051(7) 0.065(8) 0.005(7) 0.026(7) 0.003(6) C32 0.059(8) 0.055(7) 0.060(8) 0.007(7) 0.013(7) -0.004(6) C33 0.057(8) 0.059(8) 0.070(9) -0.004(7) 0.020(7) 0.007(7) C34 0.056(8) 0.065(8) 0.067(9) 0.008(7) 0.027(7) 0.005(7) C341 0.077(9) 0.084(10) 0.086(10) -0.011(8) 0.025(8) -0.001(8) C35 0.051(8) 0.064(8) 0.088(10) -0.001(8) 0.022(7) -0.013(7) C36 0.068(8) 0.044(7) 0.054(8) -0.001(6) 0.011(7) -0.010(6) O31 0.076(6) 0.049(5) 0.063(5) 0.001(4) 0.011(4) -0.004(4) C311 0.092(10) 0.053(8) 0.072(9) -0.006(7) 0.001(7) 0.001(7) C312 0.107(12) 0.049(8) 0.067(10) 0.010(7) 0.000(10) -0.015(8) C313 0.149(16) 0.074(10) 0.081(11) 0.005(9) -0.010(12) 0.001(10) C314 0.136(17) 0.098(12) 0.105(16) 0.018(11) -0.033(12) -0.016(12) C315 0.19(2) 0.140(17) 0.082(13) 0.040(12) 0.021(15) -0.001(17) C316 0.159(18) 0.075(11) 0.131(16) 0.012(11) 0.047(15) -0.017(11) C317 0.130(14) 0.073(10) 0.070(11) 0.019(8) 0.030(9) -0.027(9) C4 0.052(8) 0.081(9) 0.069(9) -0.007(7) 0.005(7) -0.010(7) C41 0.049(8) 0.056(8) 0.063(8) -0.012(6) 0.002(6) 0.001(7) C42 0.058(8) 0.071(9) 0.064(8) -0.009(7) -0.001(7) -0.008(8) C43 0.085(10) 0.067(10) 0.088(10) -0.026(8) 0.027(8) -0.018(8) C44 0.089(10) 0.061(9) 0.070(9) -0.017(7) 0.011(8) -0.004(8) C441 0.108(12) 0.066(9) 0.083(10) -0.008(8) 0.006(9) 0.003(8) C45 0.084(10) 0.078(10) 0.061(9) 0.002(7) 0.020(7) 0.013(8) C46 0.067(9) 0.057(8) 0.052(8) -0.003(6) 0.002(6) 0.003(7) O41 0.062(5) 0.074(6) 0.070(6) -0.003(5) 0.002(4) 0.006(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 Na1 O1 2.076(16) . ? Na1 O1' 2.169(17) . ? Na1 O11 2.285(9) . ? Na1 O21 2.320(9) . ? Na1 O31 2.298(9) . ? Na1 O41 2.347(9) . ? S1 O1 1.389(9) . ? S1 O2 1.393(9) . ? S1 O3 1.441(9) . ? S1 C0 1.840(8) . ? C0 F2 1.287(9) . ? C0 F3 1.292(9) . ? C0 F1 1.304(9) . ? S1' O1' 1.382(8) . ? S1' O3' 1.412(9) . ? S1' O2' 1.463(9) . ? S1' C0' 1.816(8) . ? C0' F2' 1.293(9) . ? C0' F1' 1.299(9) . ? C0' F3' 1.311(9) . ? N01 C01 1.12(2) . ? C01 C02 1.37(2) . ? C1 C26 1.527(15) . ? C1 C12 1.515(15) . ? C11 C12 1.398(16) . ? C11 O11 1.383(14) . ? C11 C16 1.424(16) . ? C12 C13 1.369(15) . ? C13 C14 1.389(16) . ? C14 C15 1.365(16) . ? C14 C141 1.532(10) . ? C141 C144 1.531(11) . ? C141 C142 1.532(11) . ? C141 C143 1.537(11) . ? C15 C16 1.361(17) . ? C16 C4 1.504(16) . ? O11 C111 1.480(13) . ? C111 C112 1.458(17) . ? C112 C117 1.346(8) . ? C112 C113 1.346(8) . ? C113 C114 1.346(8) . ? C114 C115 1.346(8) . ? C115 C116 1.346(8) . ? C116 C117 1.346(8) . ? C2 C36 1.517(14) . ? C2 C22 1.518(14) . ? C21 C22 1.395(15) . ? C21 C26 1.384(15) . ? C21 O21 1.391(12) . ? C22 C23 1.391(14) . ? C23 C24 1.368(14) . ? C24 C25 1.366(14) . ? C24 C241 1.527(10) . ? C241 C246 1.496(12) . ? C241 C242 1.498(12) . ? C241 C243 1.501(12) . ? C241 C247 1.498(13) . ? C241 C245 1.502(12) . ? C241 C244 1.505(12) . ? C25 C26 1.383(15) . ? O21 C211 1.475(8) . ? C211 C212 1.544(9) . ? C212 O213 1.427(10) . ? O213 C214 1.431(10) . ? C22' O23' 1.397(10) . ? O23' C24' 1.453(10) . ? C3 C32 1.529(15) . ? C3 C46 1.528(15) . ? C31 C36 1.384(14) . ? C31 C32 1.390(15) . ? C31 O31 1.413(12) . ? C32 C33 1.370(14) . ? C33 C34 1.402(15) . ? C34 C35 1.372(15) . ? C34 C341 1.534(10) . ? C341 C346 1.533(13) . ? C341 C344 1.534(13) . ? C341 C343 1.540(13) . ? C341 C342 1.539(13) . ? C341 C347 1.538(13) . ? C341 C345 1.543(13) . ? C35 C36 1.375(15) . ? O31 C311 1.473(13) . ? C311 C312 1.505(14) . ? C312 C317 1.372(6) . ? C312 C313 1.372(6) . ? C313 C314 1.372(6) . ? C314 C315 1.371(6) . ? C315 C316 1.372(6) . ? C316 C317 1.371(6) . ? C4 C42 1.534(15) . ? C41 C42 1.383(15) . ? C41 C46 1.365(15) . ? C41 O41 1.388(13) . ? C42 C43 1.374(16) . ? C43 C44 1.374(16) . ? C44 C45 1.395(16) . ? C44 C441 1.539(10) . ? C441 C444 1.538(12) . ? C441 C447 1.539(12) . ? C441 C445 1.542(12) . ? C441 C442 1.545(12) . ? C441 C443 1.546(12) . ? C441 C446 1.546(12) . ? C45 C46 1.407(15) . ? O41 C411 1.472(10) . ? O41 C41' 1.474(10) . ? C411 C412 1.492(10) . ? C412 O413 1.406(10) . ? O413 C414 1.486(10) . ? C41' C42' 1.489(10) . ? C42' O43' 1.423(10) . ? O43' C44' 1.501(10) . ? 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 O1 Na1 O1' 13.0(11) . . ? O1 Na1 O11 102.3(8) . . ? O1' Na1 O11 115.2(7) . . ? O1 Na1 O21 104.3(7) . . ? O1' Na1 O21 102.4(7) . . ? O11 Na1 O21 87.0(3) . . ? O1 Na1 O31 107.5(8) . . ? O1' Na1 O31 94.6(7) . . ? O11 Na1 O31 150.1(4) . . ? O21 Na1 O31 84.6(3) . . ? O1 Na1 O41 106.3(7) . . ? O1' Na1 O41 107.8(7) . . ? O11 Na1 O41 84.9(3) . . ? O21 Na1 O41 149.4(3) . . ? O31 Na1 O41 88.0(3) . . ? O1 S1 O2 112.4(8) . . ? O1 S1 O3 108.9(8) . . ? O2 S1 O3 109.8(8) . . ? O1 S1 C0 110.0(7) . . ? O2 S1 C0 109.5(7) . . ? O3 S1 C0 106.1(7) . . ? S1 O1 Na1 159.6(16) . . ? F2 C0 F3 111.6(10) . . ? F2 C0 F1 110.8(9) . . ? F3 C0 F1 109.5(9) . . ? F2 C0 S1 108.4(8) . . ? F3 C0 S1 108.6(8) . . ? F1 C0 S1 107.9(8) . . ? O1' S1' O3' 112.3(8) . . ? O1' S1' O2' 108.5(8) . . ? O3' S1' O2' 105.7(8) . . ? O1' S1' C0' 112.1(7) . . ? O3' S1' C0' 111.8(7) . . ? O2' S1' C0' 106.0(7) . . ? S1' O1' Na1 166.0(16) . . ? F2' C0' F1' 111.4(9) . . ? F2' C0' F3' 108.2(9) . . ? F1' C0' F3' 108.4(9) . . ? F2' C0' S1' 110.6(8) . . ? F1' C0' S1' 109.7(8) . . ? F3' C0' S1' 108.5(8) . . ? N01 C01 C02 177(2) . . ? C26 C1 C12 110.1(9) . . ? C12 C11 O11 121.9(12) . . ? C12 C11 C16 118.1(13) . . ? O11 C11 C16 120.1(12) . . ? C13 C12 C11 120.4(12) . . ? C13 C12 C1 119.6(11) . . ? C11 C12 C1 119.8(12) . . ? C12 C13 C14 120.8(12) . . ? C13 C14 C15 118.8(12) . . ? C13 C14 C141 120.3(11) . . ? C15 C14 C141 120.9(13) . . ? C144 C141 C142 108.0(7) . . ? C144 C141 C143 107.6(7) . . ? C142 C141 C143 107.9(7) . . ? C144 C141 C14 109.9(10) . . ? C142 C141 C14 113.3(10) . . ? C143 C141 C14 110.0(11) . . ? C16 C15 C14 122.2(13) . . ? C15 C16 C11 119.3(13) . . ? C15 C16 C4 120.5(13) . . ? C11 C16 C4 120.1(13) . . ? C11 O11 C111 112.2(9) . . ? C11 O11 Na1 127.4(7) . . ? C111 O11 Na1 119.4(7) . . ? C112 C111 O11 113.8(10) . . ? C117 C112 C113 120.0 . . ? C117 C112 C111 119.9(14) . . ? C113 C112 C111 119.9(14) . . ? C114 C113 C112 120.0 . . ? C113 C114 C115 120.0 . . ? C116 C115 C114 120.0 . . ? C117 C116 C115 120.0 . . ? C116 C117 C112 120.0 . . ? C36 C2 C22 111.3(9) . . ? C22 C21 C26 122.1(11) . . ? C22 C21 O21 119.1(11) . . ? C26 C21 O21 118.9(11) . . ? C23 C22 C21 117.4(11) . . ? C23 C22 C2 119.2(10) . . ? C21 C22 C2 122.9(11) . . ? C22 C23 C24 123.5(11) . . ? C23 C24 C25 115.4(10) . . ? C23 C24 C241 122.2(11) . . ? C25 C24 C241 122.4(10) . . ? C246 C241 C242 134.3(17) . . ? C246 C241 C243 39.8(11) . . ? C242 C241 C243 106.7(8) . . ? C246 C241 C247 107.1(9) . . ? C242 C241 C247 66.7(11) . . ? C243 C241 C247 129(2) . . ? C246 C241 C245 106.6(9) . . ? C242 C241 C245 43.6(10) . . ? C243 C241 C245 68.5(11) . . ? C247 C241 C245 106.7(9) . . ? C246 C241 C244 70.9(11) . . ? C242 C241 C244 106.4(8) . . ? C243 C241 C244 106.2(8) . . ? C247 C241 C244 41.5(11) . . ? C245 C241 C244 136.8(16) . . ? C246 C241 C24 110.0(14) . . ? C242 C241 C24 112.7(13) . . ? C243 C241 C24 112.3(13) . . ? C247 C241 C24 116.9(16) . . ? C245 C241 C24 109.0(14) . . ? C244 C241 C24 112.1(12) . . ? C26 C25 C24 126.1(11) . . ? C25 C26 C21 115.6(11) . . ? C25 C26 C1 122.1(11) . . ? C21 C26 C1 122.1(11) . . ? C21 O21 C211 113.8(8) . . ? C21 O21 Na1 126.5(6) . . ? C211 O21 Na1 118.5(7) . . ? O21 C211 C212 112.2(8) . . ? O213 C212 C211 105.4(9) . . ? C212 O213 C214 111.6(10) . . ? C22' O23' C24' 111.3(10) . . ? C32 C3 C46 110.3(9) . . ? C36 C31 C32 121.4(11) . . ? C36 C31 O31 119.8(11) . . ? C32 C31 O31 118.7(11) . . ? C33 C32 C31 118.2(11) . . ? C33 C32 C3 119.7(11) . . ? C31 C32 C3 121.9(11) . . ? C32 C33 C34 122.2(11) . . ? C35 C34 C33 117.0(10) . . ? C35 C34 C341 121.3(11) . . ? C33 C34 C341 121.7(11) . . ? C346 C341 C344 130.4(19) . . ? C346 C341 C343 71.0(12) . . ? C344 C341 C343 109.6(8) . . ? C346 C341 C342 38.7(11) . . ? C344 C341 C342 109.9(8) . . ? C343 C341 C342 109.1(8) . . ? C346 C341 C347 109.8(8) . . ? C344 C341 C347 77.4(12) . . ? C343 C341 C347 40.0(11) . . ? C342 C341 C347 144.7(16) . . ? C346 C341 C34 110.8(14) . . ? C344 C341 C34 114.0(15) . . ? C343 C341 C34 111.5(15) . . ? C342 C341 C34 102.5(15) . . ? C347 C341 C34 105.6(13) . . ? C346 C341 C345 109.4(8) . . ? C344 C341 C345 32.8(11) . . ? C343 C341 C345 132.5(18) . . ? C342 C341 C345 79.0(12) . . ? C347 C341 C345 109.1(8) . . ? C34 C341 C345 112.0(13) . . ? C34 C35 C36 123.1(12) . . ? C31 C36 C35 117.9(11) . . ? C31 C36 C2 121.5(11) . . ? C35 C36 C2 120.5(11) . . ? C31 O31 C311 112.9(9) . . ? C31 O31 Na1 125.8(6) . . ? C311 O31 Na1 120.8(7) . . ? O31 C311 C312 112.1(8) . . ? C317 C312 C313 120.0 . . ? C317 C312 C311 120.4(11) . . ? C313 C312 C311 119.5(11) . . ? C314 C313 C312 120.0 . . ? C315 C314 C313 120.0 . . ? C314 C315 C316 120.0 . . ? C317 C316 C315 120.0 . . ? C316 C317 C312 120.0 . . ? C16 C4 C42 112.5(9) . . ? C42 C41 C46 122.7(12) . . ? C42 C41 O41 119.7(11) . . ? C46 C41 O41 117.6(11) . . ? C43 C42 C41 117.1(12) . . ? C43 C42 C4 120.1(12) . . ? C41 C42 C4 122.5(12) . . ? C42 C43 C44 123.3(13) . . ? C43 C44 C45 117.8(11) . . ? C43 C44 C441 122.0(12) . . ? C45 C44 C441 120.2(12) . . ? C44 C441 C444 108.4(14) . . ? C44 C441 C447 110.6(16) . . ? C444 C441 C447 81.9(13) . . ? C44 C441 C445 113.9(14) . . ? C444 C441 C445 128.1(18) . . ? C447 C441 C445 108.8(8) . . ? C44 C441 C442 111.6(13) . . ? C444 C441 C442 108.4(8) . . ? C447 C441 C442 29.2(12) . . ? C445 C441 C442 82.8(12) . . ? C44 C441 C443 111.7(14) . . ? C444 C441 C443 108.6(8) . . ? C447 C441 C443 129.8(18) . . ? C445 C441 C443 27.2(12) . . ? C442 C441 C443 108.0(8) . . ? C44 C441 C446 106.7(16) . . ? C444 C441 C446 28.3(12) . . ? C447 C441 C446 108.4(8) . . ? C445 C441 C446 108.3(8) . . ? C442 C441 C446 131.1(18) . . ? C443 C441 C446 83.9(13) . . ? C46 C45 C44 120.5(12) . . ? C41 C46 C45 118.2(12) . . ? C41 C46 C3 123.2(11) . . ? C45 C46 C3 118.5(11) . . ? C41 O41 C411 114.7(13) . . ? C41 O41 C41' 115.9(11) . . ? C411 O41 C41' 21.5(13) . . ? C41 O41 Na1 125.2(6) . . ? C411 O41 Na1 117.8(11) . . ? C41' O41 Na1 118.7(10) . . ? O41 C411 C412 114.2(10) . . ? O413 C412 C411 114.5(10) . . ? C412 O413 C414 113.5(11) . . ? O41 C41' C42' 114.0(10) . . ? O43' C42' C41' 113.7(11) . . ? C42' O43' C44' 111.2(11) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.651 _refine_diff_density_min -0.605 _refine_diff_density_rms 0.077