# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2006 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Prof Franco Ugozzoli' _publ_contact_author_address ; Chimica Organica e Industriale Universit\`a di Parma Parco Area delle Scienze 17/a Parma N/A I-43100 ITALY ; _publ_contact_author_email FRANCO.UGOZZOLI@UNIPR.IT _publ_section_title ; Organic Guests Recognition by Tungsten-Calix[4]arene Hosts ; loop_ _publ_author_name 'Arturo Arduini' 'Chiara Massera' 'Andrea Pochini' 'Andrea Secchi' 'Franco Ugozzoli' # Attachment '3b_acetone.cif' data_calixw _database_code_depnum_ccdc_archive 'CCDC 299163' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H62 O7 W' _chemical_formula_weight 994.88 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' W W -0.8490 6.8722 '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 14.243(5) _cell_length_b 17.340(5) _cell_length_c 10.360(5) _cell_angle_alpha 90.990(5) _cell_angle_beta 102.510(5) _cell_angle_gamma 98.440(5) _cell_volume 2467.7(16) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 11 _cell_measurement_theta_max 18 _exptl_crystal_description 'thick column' _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1020 _exptl_absorpt_coefficient_mu 2.389 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 1.11 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Philips PW1100' _diffrn_measurement_method 'scintil counter' _diffrn_detector_area_resol_mean 1K _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9219 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.1066 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -2 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 25.11 _reflns_number_total 8695 _reflns_number_gt 5339 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DIPCHIGE software package 2004' _computing_cell_refinement 'DIPCHIGE software package 2004' _computing_data_reduction DIFAU92 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Accelrys DS-ViewerPro 2005' _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^)+(0.1564P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8695 _refine_ls_number_parameters 562 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1250 _refine_ls_R_factor_gt 0.0825 _refine_ls_wR_factor_ref 0.2154 _refine_ls_wR_factor_gt 0.2014 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.913 _refine_ls_shift/su_max 0.015 _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 W1 W 0.23850(3) 0.13242(3) 0.35745(5) 0.0437(2) Uani 1 1 d . . . O1A O 0.1420(5) 0.1929(4) 0.3497(7) 0.0441(17) Uani 1 1 d . . . C1A C 0.0727(7) 0.2370(6) 0.3419(11) 0.042(2) Uani 1 1 d . . . C2A C -0.0185(7) 0.2090(6) 0.2646(11) 0.042(2) Uani 1 1 d . . . C3A C -0.0879(9) 0.2569(7) 0.2547(13) 0.057(3) Uani 1 1 d . . . H3A H -0.1514 0.2391 0.2002 0.062(13) Uiso 1 1 calc R . . C4A C -0.0709(9) 0.3298(7) 0.3197(14) 0.060(3) Uani 1 1 d . A . C5A C 0.0232(8) 0.3555(7) 0.3963(12) 0.055(3) Uani 1 1 d . . . H5A H 0.0371 0.4065 0.4401 0.062(13) Uiso 1 1 calc R . . C6A C 0.0963(8) 0.3100(6) 0.4110(11) 0.044(3) Uani 1 1 d . . . C7A C -0.1544(9) 0.3793(7) 0.3102(15) 0.093(5) Uani 1 1 d D . . C8A C -0.2386(17) 0.3317(13) 0.361(3) 0.113(5) Uiso 0.636(14) 1 d PD A 1 H8A1 H -0.2772 0.3666 0.3898 0.110(17) Uiso 0.636(14) 1 calc PR A 1 H8A2 H -0.2123 0.3019 0.4335 0.110(17) Uiso 0.636(14) 1 calc PR A 1 H8A3 H -0.2786 0.2969 0.2906 0.110(17) Uiso 0.636(14) 1 calc PR A 1 C9A C -0.125(2) 0.4585(10) 0.388(2) 0.113(5) Uiso 0.636(14) 1 d PD A 1 H9A1 H -0.1810 0.4838 0.3822 0.110(17) Uiso 0.636(14) 1 calc PR A 1 H9A2 H -0.0773 0.4906 0.3510 0.110(17) Uiso 0.636(14) 1 calc PR A 1 H9A3 H -0.0974 0.4506 0.4789 0.110(17) Uiso 0.636(14) 1 calc PR A 1 C10A C -0.191(2) 0.3926(15) 0.1620(15) 0.113(5) Uiso 0.636(14) 1 d PD A 1 H0A1 H -0.1840 0.3484 0.1098 0.110(17) Uiso 0.636(14) 1 calc PR A 1 H0A2 H -0.1530 0.4386 0.1386 0.110(17) Uiso 0.636(14) 1 calc PR A 1 H0A3 H -0.2581 0.3992 0.1453 0.110(17) Uiso 0.636(14) 1 calc PR A 1 C11A C -0.162(3) 0.392(3) 0.4555(19) 0.113(5) Uiso 0.364(14) 1 d PD A 2 H1A1 H -0.2134 0.4211 0.4586 0.110(17) Uiso 0.364(14) 1 calc PR A 2 H1A2 H -0.1015 0.4197 0.5057 0.110(17) Uiso 0.364(14) 1 calc PR A 2 H1A3 H -0.1753 0.3419 0.4923 0.110(17) Uiso 0.364(14) 1 calc PR A 2 C12A C -0.2576(16) 0.358(2) 0.223(3) 0.113(5) Uiso 0.364(14) 1 d PD A 2 H2A1 H -0.3045 0.3664 0.2736 0.110(17) Uiso 0.364(14) 1 calc PR A 2 H2A2 H -0.2681 0.3042 0.1928 0.110(17) Uiso 0.364(14) 1 calc PR A 2 H2A3 H -0.2644 0.3902 0.1481 0.110(17) Uiso 0.364(14) 1 calc PR A 2 C13A C -0.105(3) 0.4567(17) 0.266(4) 0.113(5) Uiso 0.364(14) 1 d PD A 2 H3A1 H -0.1539 0.4883 0.2310 0.110(17) Uiso 0.364(14) 1 calc PR A 2 H3A2 H -0.0712 0.4457 0.1990 0.110(17) Uiso 0.364(14) 1 calc PR A 2 H3A3 H -0.0599 0.4842 0.3406 0.110(17) Uiso 0.364(14) 1 calc PR A 2 C20A C -0.0391(8) 0.1260(6) 0.1990(11) 0.044(3) Uani 1 1 d . . . H20A H -0.0198 0.0900 0.2654 0.040(10) Uiso 1 1 calc R . . H20B H -0.1079 0.1123 0.1647 0.040(10) Uiso 1 1 calc R . . O1B O 0.1447(5) 0.0643(4) 0.2287(7) 0.0415(17) Uani 1 1 d . . . C1B C 0.1000(7) 0.0865(6) 0.1058(11) 0.040(2) Uani 1 1 d . . . C2B C 0.1449(7) 0.0800(6) -0.0018(10) 0.042(2) Uani 1 1 d . . . C3B C 0.0990(8) 0.1014(7) -0.1227(11) 0.049(3) Uani 1 1 d . . . H3B H 0.1295 0.0964 -0.1958 0.062(13) Uiso 1 1 calc R . . C4B C 0.0114(8) 0.1298(6) -0.1468(11) 0.043(2) Uani 1 1 d . . . C5B C -0.0293(8) 0.1369(6) -0.0360(12) 0.047(3) Uani 1 1 d . . . H5B H -0.0898 0.1569 -0.0481 0.062(13) Uiso 1 1 calc R . . C6B C 0.0126(8) 0.1169(6) 0.0885(11) 0.044(3) Uani 1 1 d . . . C7B C -0.0374(9) 0.1539(8) -0.2854(12) 0.060(3) Uani 1 1 d . . . C8B C -0.1457(10) 0.1482(11) -0.3035(15) 0.084(5) Uani 1 1 d . . . H8B1 H -0.1610 0.1964 -0.2732 0.124(15) Uiso 1 1 calc R . . H8B2 H -0.1691 0.1065 -0.2532 0.124(15) Uiso 1 1 calc R . . H8B3 H -0.1761 0.1378 -0.3955 0.124(15) Uiso 1 1 calc R . . C9B C -0.0159(12) 0.1010(11) -0.3918(14) 0.092(6) Uani 1 1 d . . . H9B1 H -0.0337 0.1225 -0.4768 0.124(15) Uiso 1 1 calc R . . H9B2 H -0.0528 0.0499 -0.3927 0.124(15) Uiso 1 1 calc R . . H9B3 H 0.0523 0.0973 -0.3725 0.124(15) Uiso 1 1 calc R . . C10B C 0.0041(14) 0.2375(10) -0.3009(19) 0.113(7) Uani 1 1 d . . . H10A H -0.0240 0.2529 -0.3875 0.124(15) Uiso 1 1 calc R . . H10B H 0.0734 0.2421 -0.2898 0.124(15) Uiso 1 1 calc R . . H10C H -0.0107 0.2706 -0.2352 0.124(15) Uiso 1 1 calc R . . C20B C 0.2392(8) 0.0471(6) 0.0149(12) 0.051(3) Uani 1 1 d . . . H20C H 0.2346 0.0125 -0.0602 0.040(10) Uiso 1 1 calc R . . H20D H 0.2460 0.0166 0.0918 0.040(10) Uiso 1 1 calc R . . O1C O 0.2921(5) 0.1652(4) 0.2137(8) 0.0499(19) Uani 1 1 d . . . C1C C 0.3580(8) 0.1604(6) 0.1361(10) 0.043(3) Uani 1 1 d . . . C2C C 0.4485(7) 0.2088(6) 0.1735(11) 0.042(2) Uani 1 1 d . . . C3C C 0.5097(8) 0.2067(7) 0.0873(12) 0.050(3) Uani 1 1 d . . . H3C H 0.5719 0.2395 0.1084 0.062(13) Uiso 1 1 calc R . . C4C C 0.4855(8) 0.1589(7) -0.0298(12) 0.048(3) Uani 1 1 d . . . C5C C 0.3959(8) 0.1081(6) -0.0544(11) 0.046(3) Uani 1 1 d . . . H5C H 0.3786 0.0731 -0.1314 0.062(13) Uiso 1 1 calc R . . C6C C 0.3325(7) 0.1075(6) 0.0294(10) 0.039(2) Uani 1 1 d . . . C7C C 0.5500(9) 0.1574(7) -0.1271(13) 0.056(3) Uani 1 1 d . . . C8C C 0.6460(11) 0.2140(10) -0.0849(19) 0.100(6) Uani 1 1 d . . . H8C1 H 0.6324 0.2652 -0.0664 0.124(15) Uiso 1 1 calc R . . H8C2 H 0.6805 0.2160 -0.1550 0.124(15) Uiso 1 1 calc R . . H8C3 H 0.6851 0.1963 -0.0069 0.124(15) Uiso 1 1 calc R . . C9C C 0.5000(12) 0.1828(11) -0.2595(16) 0.092(5) Uani 1 1 d . . . H9C1 H 0.4414 0.1469 -0.2939 0.124(15) Uiso 1 1 calc R . . H9C2 H 0.5426 0.1835 -0.3199 0.124(15) Uiso 1 1 calc R . . H9C3 H 0.4842 0.2342 -0.2492 0.124(15) Uiso 1 1 calc R . . C10C C 0.5740(12) 0.0770(8) -0.1445(18) 0.086(5) Uani 1 1 d . . . H10D H 0.6048 0.0600 -0.0603 0.124(15) Uiso 1 1 calc R . . H10E H 0.6173 0.0778 -0.2040 0.124(15) Uiso 1 1 calc R . . H10F H 0.5152 0.0416 -0.1804 0.124(15) Uiso 1 1 calc R . . C20C C 0.4758(8) 0.2556(7) 0.3059(12) 0.054(3) Uani 1 1 d . . . H20E H 0.5401 0.2841 0.3147 0.040(10) Uiso 1 1 calc R . . H20F H 0.4789 0.2193 0.3751 0.040(10) Uiso 1 1 calc R . . O1D O 0.3253(5) 0.2205(4) 0.4549(7) 0.0458(18) Uani 1 1 d . . . C1D C 0.3386(8) 0.2941(7) 0.4006(11) 0.047(3) Uani 1 1 d . . . C2D C 0.2786(8) 0.3478(6) 0.4252(12) 0.046(3) Uani 1 1 d . . . C3D C 0.2979(9) 0.4222(7) 0.3737(12) 0.054(3) Uani 1 1 d . . . H3D H 0.2588 0.4606 0.3888 0.062(13) Uiso 1 1 calc R . . C4D C 0.3690(9) 0.4436(7) 0.3030(13) 0.056(3) Uani 1 1 d . B . C5D C 0.4244(9) 0.3875(7) 0.2826(12) 0.057(3) Uani 1 1 d . . . H5D H 0.4747 0.4005 0.2347 0.062(13) Uiso 1 1 calc R . . C6D C 0.4099(8) 0.3126(7) 0.3293(12) 0.048(3) Uani 1 1 d . . . C7D C 0.3897(10) 0.5269(6) 0.2555(13) 0.078(4) Uani 1 1 d D . . C8D C 0.2918(13) 0.5500(18) 0.181(3) 0.110(5) Uiso 0.567(15) 1 d PD B 3 H8D1 H 0.2545 0.5612 0.2444 0.110(17) Uiso 0.567(15) 1 calc PR B 3 H8D2 H 0.2559 0.5076 0.1217 0.110(17) Uiso 0.567(15) 1 calc PR B 3 H8D3 H 0.3043 0.5953 0.1324 0.110(17) Uiso 0.567(15) 1 calc PR B 3 C9D C 0.430(2) 0.5828(16) 0.3785(19) 0.110(5) Uiso 0.567(15) 1 d PD B 3 H9D1 H 0.4424 0.6353 0.3512 0.110(17) Uiso 0.567(15) 1 calc PR B 3 H9D2 H 0.4897 0.5683 0.4276 0.110(17) Uiso 0.567(15) 1 calc PR B 3 H9D3 H 0.3834 0.5797 0.4333 0.110(17) Uiso 0.567(15) 1 calc PR B 3 C10D C 0.4611(17) 0.5359(18) 0.163(2) 0.110(5) Uiso 0.567(15) 1 d PD B 3 H0D1 H 0.4686 0.5885 0.1348 0.110(17) Uiso 0.567(15) 1 calc PR B 3 H0D2 H 0.4362 0.5005 0.0867 0.110(17) Uiso 0.567(15) 1 calc PR B 3 H0D3 H 0.5231 0.5242 0.2088 0.110(17) Uiso 0.567(15) 1 calc PR B 3 C11D C 0.4971(13) 0.556(2) 0.326(3) 0.110(5) Uiso 0.433(15) 1 d PD B 4 H1D1 H 0.5074 0.6115 0.3393 0.110(17) Uiso 0.433(15) 1 calc PR B 4 H1D2 H 0.5394 0.5409 0.2724 0.110(17) Uiso 0.433(15) 1 calc PR B 4 H1D3 H 0.5112 0.5325 0.4102 0.110(17) Uiso 0.433(15) 1 calc PR B 4 C12D C 0.383(3) 0.525(2) 0.1049(15) 0.110(5) Uiso 0.433(15) 1 d PD B 4 H2D1 H 0.3169 0.5069 0.0593 0.110(17) Uiso 0.433(15) 1 calc PR B 4 H2D2 H 0.4243 0.4901 0.0828 0.110(17) Uiso 0.433(15) 1 calc PR B 4 H2D3 H 0.4034 0.5764 0.0787 0.110(17) Uiso 0.433(15) 1 calc PR B 4 C13D C 0.326(2) 0.5841(19) 0.292(3) 0.110(5) Uiso 0.433(15) 1 d PD B 4 H3D1 H 0.3237 0.6254 0.2312 0.110(17) Uiso 0.433(15) 1 calc PR B 4 H3D2 H 0.3529 0.6056 0.3803 0.110(17) Uiso 0.433(15) 1 calc PR B 4 H3D3 H 0.2613 0.5570 0.2864 0.110(17) Uiso 0.433(15) 1 calc PR B 4 C20D C 0.1979(8) 0.3325(7) 0.4960(12) 0.050(3) Uani 1 1 d . . . H20G H 0.1987 0.3785 0.5494 0.040(10) Uiso 1 1 calc R . . H20H H 0.2111 0.2914 0.5550 0.040(10) Uiso 1 1 calc R . . O1* O 0.2081(5) 0.0780(4) 0.5101(7) 0.0420(17) Uani 1 1 d . . . C1* C 0.2584(8) 0.0228(6) 0.5542(11) 0.043(3) Uani 1 1 d . . . C2* C 0.2395(10) -0.0247(8) 0.6571(12) 0.062(4) Uani 1 1 d . . . H2* H 0.1884 -0.0180 0.7012 0.059(17) Uiso 1 1 calc R . . C3* C 0.2978(11) -0.0816(8) 0.6920(15) 0.068(4) Uani 1 1 d . . . H3* H 0.2892 -0.1138 0.7642 0.059(17) Uiso 1 1 calc R . . C4* C 0.3676(11) -0.0920(8) 0.6242(16) 0.072(4) Uani 1 1 d . . . H4* H 0.4065 -0.1323 0.6491 0.059(17) Uiso 1 1 calc R . . C5* C 0.3840(9) -0.0464(7) 0.5212(14) 0.060(3) Uani 1 1 d . . . H5* H 0.4332 -0.0543 0.4742 0.059(17) Uiso 1 1 calc R . . C6* C 0.3285(8) 0.0093(6) 0.4893(11) 0.045(3) Uani 1 1 d . . . O2* O 0.3329(5) 0.0610(4) 0.3867(8) 0.0445(18) Uani 1 1 d . . . C1G C 0.229(3) 0.3476(18) -0.081(4) 0.173(15) Uani 1 1 d . . . C2G C 0.183(2) 0.3178(18) 0.025(3) 0.181(14) Uani 1 1 d . . . H2G1 H 0.1297 0.3454 0.0298 0.27(7) Uiso 1 1 calc R . . H2G2 H 0.2295 0.3253 0.1083 0.27(7) Uiso 1 1 calc R . . H2G3 H 0.1584 0.2631 0.0076 0.27(7) Uiso 1 1 calc R . . O3G O 0.200(2) 0.4027(12) -0.138(2) 0.263(16) Uani 1 1 d . . . C4G C 0.303(3) 0.306(2) -0.122(4) 0.24(2) Uani 1 1 d . . . H4G1 H 0.2702 0.2603 -0.1764 0.27(7) Uiso 1 1 calc R . . H4G2 H 0.3454 0.2908 -0.0449 0.27(7) Uiso 1 1 calc R . . H4G3 H 0.3396 0.3399 -0.1713 0.27(7) 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 W1 0.0369(3) 0.0472(3) 0.0451(3) -0.00438(18) 0.01073(18) -0.00138(17) O1A 0.042(4) 0.042(4) 0.043(4) 0.001(3) 0.006(3) -0.003(3) C1A 0.034(5) 0.047(6) 0.048(7) 0.006(5) 0.015(5) 0.006(5) C2A 0.037(6) 0.043(6) 0.045(6) -0.007(5) 0.016(5) -0.007(5) C3A 0.039(6) 0.066(8) 0.061(8) -0.016(6) 0.004(6) 0.002(6) C4A 0.050(7) 0.054(7) 0.070(9) -0.009(6) -0.001(6) 0.011(6) C5A 0.047(7) 0.051(7) 0.063(8) -0.022(6) 0.008(6) 0.002(5) C6A 0.043(6) 0.045(6) 0.039(6) -0.010(5) 0.004(5) -0.003(5) C7A 0.063(9) 0.075(10) 0.134(15) -0.035(10) 0.009(10) 0.011(8) C20A 0.034(5) 0.049(6) 0.047(7) 0.001(5) 0.012(5) -0.003(5) O1B 0.038(4) 0.048(4) 0.036(4) 0.000(3) 0.008(3) -0.001(3) C1B 0.038(6) 0.035(5) 0.044(6) -0.008(5) 0.012(5) -0.010(4) C2B 0.033(5) 0.047(6) 0.039(6) -0.009(5) 0.003(5) -0.007(4) C3B 0.037(6) 0.060(7) 0.044(7) -0.013(5) 0.018(5) -0.019(5) C4B 0.038(6) 0.049(6) 0.038(6) -0.002(5) 0.009(5) -0.002(5) C5B 0.030(5) 0.050(7) 0.058(8) -0.008(5) 0.009(5) -0.006(5) C6B 0.037(6) 0.047(6) 0.042(7) -0.015(5) 0.007(5) -0.009(5) C7B 0.049(7) 0.078(9) 0.048(7) 0.002(6) 0.011(6) -0.002(6) C8B 0.051(8) 0.135(14) 0.066(10) 0.006(9) 0.005(7) 0.023(9) C9B 0.079(11) 0.163(17) 0.044(8) 0.000(9) 0.020(8) 0.044(11) C10B 0.109(14) 0.101(13) 0.100(14) 0.040(11) -0.015(11) -0.024(11) C20B 0.046(6) 0.046(6) 0.055(7) -0.015(5) 0.009(6) -0.005(5) O1C 0.039(4) 0.063(5) 0.051(5) -0.008(4) 0.033(4) -0.012(3) C1C 0.042(6) 0.049(6) 0.037(6) 0.003(5) 0.011(5) -0.003(5) C2C 0.030(5) 0.046(6) 0.049(7) -0.007(5) 0.009(5) -0.003(4) C3C 0.035(6) 0.054(7) 0.056(7) -0.008(6) 0.009(5) -0.002(5) C4C 0.032(6) 0.051(6) 0.059(8) -0.001(6) 0.014(5) -0.004(5) C5C 0.040(6) 0.045(6) 0.049(7) -0.009(5) 0.008(5) 0.003(5) C6C 0.032(5) 0.045(6) 0.039(6) -0.001(5) 0.010(5) 0.001(4) C7C 0.045(7) 0.060(7) 0.063(8) -0.010(6) 0.020(6) 0.000(6) C8C 0.060(9) 0.113(13) 0.126(15) -0.045(11) 0.049(10) -0.029(9) C9C 0.078(11) 0.127(15) 0.086(12) 0.022(11) 0.041(10) 0.029(10) C10C 0.089(11) 0.071(9) 0.118(14) 0.005(9) 0.063(10) 0.016(8) C20C 0.036(6) 0.066(8) 0.054(7) -0.011(6) 0.005(5) -0.001(5) O1D 0.039(4) 0.054(5) 0.043(4) -0.010(4) 0.010(3) 0.000(3) C1D 0.043(6) 0.051(7) 0.037(6) -0.006(5) -0.002(5) -0.005(5) C2D 0.036(6) 0.040(6) 0.056(7) -0.015(5) 0.003(5) 0.001(5) C3D 0.054(7) 0.044(7) 0.058(8) -0.013(6) 0.009(6) -0.001(5) C4D 0.058(7) 0.046(7) 0.058(8) -0.010(6) 0.009(6) -0.010(6) C5D 0.047(7) 0.060(8) 0.058(8) -0.020(6) 0.017(6) -0.013(6) C6D 0.032(5) 0.052(7) 0.053(7) -0.016(5) 0.009(5) -0.007(5) C7D 0.085(11) 0.049(8) 0.095(11) 0.005(7) 0.023(9) -0.009(7) C20D 0.040(6) 0.047(6) 0.060(7) -0.016(6) 0.010(5) 0.001(5) O1* 0.029(4) 0.045(4) 0.051(5) 0.014(3) 0.015(3) -0.009(3) C1* 0.041(6) 0.039(6) 0.048(7) -0.014(5) 0.014(5) -0.004(5) C2* 0.058(8) 0.080(9) 0.039(7) -0.008(6) 0.013(6) -0.019(7) C3* 0.076(10) 0.055(8) 0.073(10) 0.016(7) 0.013(8) 0.011(7) C4* 0.066(9) 0.060(8) 0.089(11) 0.012(8) 0.005(8) 0.021(7) C5* 0.047(7) 0.056(7) 0.076(9) -0.001(7) 0.017(7) 0.003(6) C6* 0.034(6) 0.041(6) 0.054(7) 0.004(5) 0.000(5) 0.000(5) O2* 0.033(4) 0.047(4) 0.058(5) -0.007(4) 0.020(3) 0.004(3) C1G 0.21(4) 0.10(2) 0.15(3) -0.007(19) -0.05(3) -0.04(2) C2G 0.18(3) 0.15(3) 0.15(3) -0.06(2) -0.05(2) -0.03(2) O3G 0.41(4) 0.117(15) 0.21(2) 0.074(16) -0.04(2) 0.04(2) C4G 0.19(3) 0.19(3) 0.34(5) -0.02(3) -0.01(3) 0.11(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O1A 1.837(7) . ? W1 O1C 1.875(7) . ? W1 O1B 1.915(7) . ? W1 O2* 1.939(7) . ? W1 O1D 1.932(7) . ? W1 O1* 1.951(7) . ? O1A C1A 1.324(12) . ? C1A C2A 1.384(14) . ? C1A C6A 1.403(14) . ? C2A C3A 1.372(15) . ? C2A C20A 1.540(14) . ? C3A C4A 1.385(16) . ? C3A H3A 0.9600 . ? C4A C5A 1.406(16) . ? C4A C7A 1.553(16) . ? C5A C6A 1.380(16) . ? C5A H5A 0.9600 . ? C6A C20D 1.514(15) . ? C7A C12A 1.538(8) . ? C7A C9A 1.535(8) . ? C7A C10A 1.544(8) . ? C7A C8A 1.546(8) . ? C7A C13A 1.545(8) . ? C7A C11A 1.545(8) . ? C8A H8A1 0.9599 . ? C8A H8A2 0.9599 . ? C8A H8A3 0.9599 . ? C9A H9A1 0.9599 . ? C9A H9A2 0.9599 . ? C9A H9A3 0.9599 . ? C10A H0A1 0.9599 . ? C10A H0A2 0.9599 . ? C10A H0A3 0.9599 . ? C11A H1A1 0.9599 . ? C11A H1A2 0.9599 . ? C11A H1A3 0.9599 . ? C12A H2A1 0.9599 . ? C12A H2A2 0.9599 . ? C12A H2A3 0.9599 . ? C13A H3A1 0.9599 . ? C13A H3A2 0.9599 . ? C13A H3A3 0.9599 . ? C20A C6B 1.507(15) . ? C20A H20A 0.9600 . ? C20A H20B 0.9600 . ? O1B C1B 1.383(13) . ? C1B C2B 1.411(15) . ? C1B C6B 1.400(15) . ? C2B C3B 1.367(16) . ? C2B C20B 1.512(15) . ? C3B C4B 1.381(15) . ? C3B H3B 0.9600 . ? C4B C5B 1.404(16) . ? C4B C7B 1.548(17) . ? C5B C6B 1.372(16) . ? C5B H5B 0.9600 . ? C7B C10B 1.51(2) . ? C7B C8B 1.500(18) . ? C7B C9B 1.532(19) . ? C8B H8B1 0.9599 . ? C8B H8B2 0.9599 . ? C8B H8B3 0.9599 . ? C9B H9B1 0.9599 . ? C9B H9B2 0.9599 . ? C9B H9B3 0.9599 . ? C10B H10A 0.9599 . ? C10B H10B 0.9599 . ? C10B H10C 0.9599 . ? C20B C6C 1.543(14) . ? C20B H20C 0.9600 . ? C20B H20D 0.9600 . ? O1C C1C 1.373(12) . ? C1C C6C 1.375(14) . ? C1C C2C 1.403(14) . ? C2C C3C 1.379(15) . ? C2C C20C 1.527(15) . ? C3C C4C 1.407(16) . ? C3C H3C 0.9600 . ? C4C C5C 1.410(14) . ? C4C C7C 1.507(16) . ? C5C C6C 1.380(15) . ? C5C H5C 0.9600 . ? C7C C9C 1.51(2) . ? C7C C10C 1.501(18) . ? C7C C8C 1.535(17) . ? C8C H8C1 0.9599 . ? C8C H8C2 0.9599 . ? C8C H8C3 0.9599 . ? C9C H9C1 0.9599 . ? C9C H9C2 0.9599 . ? C9C H9C3 0.9599 . ? C10C H10D 0.9599 . ? C10C H10E 0.9599 . ? C10C H10F 0.9599 . ? C20C C6D 1.510(15) . ? C20C H20E 0.9600 . ? C20C H20F 0.9600 . ? O1D C1D 1.407(13) . ? C1D C6D 1.384(16) . ? C1D C2D 1.408(15) . ? C2D C3D 1.416(17) . ? C2D C20D 1.487(16) . ? C3D C4D 1.385(17) . ? C3D H3D 0.9600 . ? C4D C5D 1.379(17) . ? C4D C7D 1.543(16) . ? C5D C6D 1.397(17) . ? C5D H5D 0.9600 . ? C7D C13D 1.533(8) . ? C7D C10D 1.537(8) . ? C7D C12D 1.542(8) . ? C7D C9D 1.539(8) . ? C7D C11D 1.550(8) . ? C7D C8D 1.551(8) . ? C8D H8D1 0.9599 . ? C8D H8D2 0.9599 . ? C8D H8D3 0.9599 . ? C9D H9D1 0.9599 . ? C9D H9D2 0.9599 . ? C9D H9D3 0.9599 . ? C10D H0D1 0.9599 . ? C10D H0D2 0.9599 . ? C10D H0D3 0.9599 . ? C11D H1D1 0.9599 . ? C11D H1D2 0.9599 . ? C11D H1D3 0.9599 . ? C12D H2D1 0.9599 . ? C12D H2D2 0.9599 . ? C12D H2D3 0.9599 . ? C13D H3D1 0.9599 . ? C13D H3D2 0.9599 . ? C13D H3D3 0.9599 . ? C20D H20G 0.9600 . ? C20D H20H 0.9600 . ? O1* C1* 1.309(13) . ? C1* C6* 1.362(15) . ? C1* C2* 1.406(17) . ? C2* C3* 1.383(19) . ? C2* H2* 0.9600 . ? C3* C4* 1.36(2) . ? C3* H3* 0.9600 . ? C4* C5* 1.379(19) . ? C4* H4* 0.9600 . ? C5* C6* 1.337(16) . ? C5* H5* 0.9600 . ? C6* O2* 1.408(13) . ? C1G O3G 1.21(3) . ? C1G C4G 1.48(5) . ? C1G C2G 1.46(4) . ? C2G H2G1 0.9599 . ? C2G H2G2 0.9599 . ? C2G H2G3 0.9599 . ? C4G H4G1 0.9599 . ? C4G H4G2 0.9599 . ? C4G H4G3 0.9599 . ? 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 O1A W1 O1C 102.4(3) . . ? O1A W1 O1B 85.5(3) . . ? O1C W1 O1B 85.0(3) . . ? O1A W1 O2* 171.5(3) . . ? O1C W1 O2* 86.1(3) . . ? O1B W1 O2* 94.5(3) . . ? O1A W1 O1D 86.0(3) . . ? O1C W1 O1D 85.3(3) . . ? O1B W1 O1D 165.5(3) . . ? O2* W1 O1D 95.6(3) . . ? O1A W1 O1* 93.4(3) . . ? O1C W1 O1* 164.2(3) . . ? O1B W1 O1* 95.1(3) . . ? O2* W1 O1* 78.1(3) . . ? O1D W1 O1* 97.1(3) . . ? C1A O1A W1 178.9(7) . . ? O1A C1A C2A 118.2(9) . . ? O1A C1A C6A 118.1(9) . . ? C2A C1A C6A 123.7(10) . . ? C3A C2A C1A 116.9(10) . . ? C3A C2A C20A 123.1(10) . . ? C1A C2A C20A 119.9(10) . . ? C2A C3A C4A 123.1(11) . . ? C2A C3A H3A 118.4 . . ? C4A C3A H3A 118.4 . . ? C3A C4A C5A 117.4(11) . . ? C3A C4A C7A 120.5(11) . . ? C5A C4A C7A 122.1(11) . . ? C6A C5A C4A 122.4(10) . . ? C6A C5A H5A 118.8 . . ? C4A C5A H5A 118.8 . . ? C5A C6A C1A 116.4(10) . . ? C5A C6A C20D 125.3(10) . . ? C1A C6A C20D 118.4(10) . . ? C12A C7A C9A 120(2) . . ? C12A C7A C10A 51.1(15) . . ? C9A C7A C10A 109.3(7) . . ? C12A C7A C8A 57.7(15) . . ? C9A C7A C8A 108.9(7) . . ? C10A C7A C8A 108.6(7) . . ? C12A C7A C13A 109.0(8) . . ? C9A C7A C13A 52.0(16) . . ? C10A C7A C13A 66.6(15) . . ? C8A C7A C13A 151(2) . . ? C12A C7A C11A 109.0(8) . . ? C9A C7A C11A 56.5(16) . . ? C10A C7A C11A 149.4(19) . . ? C8A C7A C11A 60.2(15) . . ? C13A C7A C11A 108.3(8) . . ? C12A C7A C4A 125.6(19) . . ? C9A C7A C4A 114.5(14) . . ? C10A C7A C4A 106.6(14) . . ? C8A C7A C4A 108.8(14) . . ? C13A C7A C4A 100(2) . . ? C11A C7A C4A 103.9(19) . . ? C7A C8A H8A1 109.5 . . ? C7A C8A H8A2 109.5 . . ? C7A C8A H8A3 109.5 . . ? C7A C9A H9A1 109.5 . . ? C7A C9A H9A2 109.5 . . ? C7A C9A H9A3 109.5 . . ? C7A C10A H0A1 109.5 . . ? C7A C10A H0A2 109.5 . . ? C7A C10A H0A3 109.5 . . ? C7A C11A H1A1 109.5 . . ? C7A C11A H1A2 109.5 . . ? H1A1 C11A H1A2 109.5 . . ? C7A C11A H1A3 109.5 . . ? H1A1 C11A H1A3 109.5 . . ? H1A2 C11A H1A3 109.5 . . ? C7A C12A H2A1 109.5 . . ? C7A C12A H2A2 109.5 . . ? H2A1 C12A H2A2 109.5 . . ? C7A C12A H2A3 109.5 . . ? H2A1 C12A H2A3 109.5 . . ? H2A2 C12A H2A3 109.5 . . ? C7A C13A H3A1 109.5 . . ? C7A C13A H3A2 109.5 . . ? H3A1 C13A H3A2 109.5 . . ? C7A C13A H3A3 109.5 . . ? H3A1 C13A H3A3 109.5 . . ? H3A2 C13A H3A3 109.5 . . ? C6B C20A C2A 114.0(9) . . ? C6B C20A H20A 108.8 . . ? C2A C20A H20A 108.8 . . ? C6B C20A H20B 108.8 . . ? C2A C20A H20B 108.8 . . ? H20A C20A H20B 107.7 . . ? C1B O1B W1 124.3(6) . . ? O1B C1B C2B 119.1(9) . . ? O1B C1B C6B 120.7(9) . . ? C2B C1B C6B 120.1(10) . . ? C3B C2B C1B 118.2(10) . . ? C3B C2B C20B 120.9(10) . . ? C1B C2B C20B 120.9(10) . . ? C2B C3B C4B 124.3(10) . . ? C2B C3B H3B 117.8 . . ? C4B C3B H3B 117.8 . . ? C3B C4B C5B 115.4(10) . . ? C3B C4B C7B 122.4(10) . . ? C5B C4B C7B 122.2(10) . . ? C6B C5B C4B 123.7(10) . . ? C6B C5B H5B 118.1 . . ? C4B C5B H5B 118.1 . . ? C5B C6B C1B 118.2(10) . . ? C5B C6B C20A 118.8(10) . . ? C1B C6B C20A 123.0(10) . . ? C10B C7B C8B 108.4(13) . . ? C10B C7B C4B 108.3(11) . . ? C8B C7B C4B 112.2(11) . . ? C10B C7B C9B 109.8(14) . . ? C8B C7B C9B 108.8(12) . . ? C4B C7B C9B 109.4(11) . . ? C7B C8B H8B1 109.5 . . ? C7B C8B H8B2 109.5 . . ? H8B1 C8B H8B2 109.5 . . ? C7B C8B H8B3 109.5 . . ? H8B1 C8B H8B3 109.5 . . ? H8B2 C8B H8B3 109.5 . . ? C7B C9B H9B1 109.5 . . ? C7B C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? C7B C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? C7B C10B H10A 109.5 . . ? C7B C10B H10B 109.5 . . ? H10A C10B H10B 109.5 . . ? C7B C10B H10C 109.5 . . ? H10A C10B H10C 109.5 . . ? H10B C10B H10C 109.5 . . ? C2B C20B C6C 116.0(9) . . ? C2B C20B H20C 108.3 . . ? C6C C20B H20C 108.3 . . ? C2B C20B H20D 108.3 . . ? C6C C20B H20D 108.3 . . ? H20C C20B H20D 107.4 . . ? C1C O1C W1 150.5(8) . . ? O1C C1C C6C 118.3(9) . . ? O1C C1C C2C 117.4(9) . . ? C6C C1C C2C 124.3(10) . . ? C3C C2C C1C 115.6(10) . . ? C3C C2C C20C 124.3(9) . . ? C1C C2C C20C 120.0(10) . . ? C2C C3C C4C 123.3(10) . . ? C2C C3C H3C 118.3 . . ? C4C C3C H3C 118.3 . . ? C3C C4C C5C 117.0(10) . . ? C3C C4C C7C 124.1(10) . . ? C5C C4C C7C 118.8(10) . . ? C6C C5C C4C 121.8(10) . . ? C6C C5C H5C 119.1 . . ? C4C C5C H5C 119.1 . . ? C1C C6C C5C 117.5(9) . . ? C1C C6C C20B 118.8(9) . . ? C5C C6C C20B 123.5(9) . . ? C4C C7C C9C 110.1(11) . . ? C4C C7C C10C 110.9(11) . . ? C9C C7C C10C 109.0(13) . . ? C4C C7C C8C 112.7(11) . . ? C9C C7C C8C 105.9(13) . . ? C10C C7C C8C 108.1(12) . . ? C7C C8C H8C1 109.5 . . ? C7C C8C H8C2 109.5 . . ? H8C1 C8C H8C2 109.5 . . ? C7C C8C H8C3 109.5 . . ? H8C1 C8C H8C3 109.5 . . ? H8C2 C8C H8C3 109.5 . . ? C7C C9C H9C1 109.5 . . ? C7C C9C H9C2 109.5 . . ? H9C1 C9C H9C2 109.5 . . ? C7C C9C H9C3 109.5 . . ? H9C1 C9C H9C3 109.5 . . ? H9C2 C9C H9C3 109.5 . . ? C7C C10C H10D 109.5 . . ? C7C C10C H10E 109.5 . . ? H10D C10C H10E 109.5 . . ? C7C C10C H10F 109.5 . . ? H10D C10C H10F 109.5 . . ? H10E C10C H10F 109.5 . . ? C2C C20C C6D 117.3(9) . . ? C2C C20C H20E 108.0 . . ? C6D C20C H20E 108.0 . . ? C2C C20C H20F 108.0 . . ? C6D C20C H20F 108.0 . . ? H20E C20C H20F 107.2 . . ? C1D O1D W1 122.1(6) . . ? C6D C1D C2D 122.2(11) . . ? C6D C1D O1D 120.6(10) . . ? C2D C1D O1D 117.2(10) . . ? C1D C2D C3D 115.0(11) . . ? C1D C2D C20D 126.1(11) . . ? C3D C2D C20D 118.9(10) . . ? C4D C3D C2D 124.9(11) . . ? C4D C3D H3D 117.6 . . ? C2D C3D H3D 117.6 . . ? C5D C4D C3D 116.6(12) . . ? C5D C4D C7D 121.1(12) . . ? C3D C4D C7D 122.3(11) . . ? C6D C5D C4D 122.4(11) . . ? C6D C5D H5D 118.8 . . ? C4D C5D H5D 118.8 . . ? C5D C6D C1D 119.0(11) . . ? C5D C6D C20C 118.8(10) . . ? C1D C6D C20C 122.1(11) . . ? C13D C7D C10D 130.0(19) . . ? C13D C7D C12D 109.7(8) . . ? C10D C7D C12D 43.1(13) . . ? C13D C7D C9D 61.1(13) . . ? C10D C7D C9D 109.6(7) . . ? C12D C7D C9D 139.8(19) . . ? C13D C7D C4D 115.2(17) . . ? C10D C7D C4D 114.2(15) . . ? C12D C7D C4D 110.6(17) . . ? C9D C7D C4D 108.0(14) . . ? C13D C7D C11D 109.0(7) . . ? C10D C7D C11D 65.6(14) . . ? C12D C7D C11D 108.2(7) . . ? C9D C7D C11D 51.1(13) . . ? C4D C7D C11D 103.8(17) . . ? C13D C7D C8D 47.5(13) . . ? C10D C7D C8D 108.6(7) . . ? C12D C7D C8D 69.5(13) . . ? C9D C7D C8D 108.1(7) . . ? C4D C7D C8D 108.1(14) . . ? C11D C7D C8D 146.6(18) . . ? C7D C8D H8D1 109.5 . . ? C7D C8D H8D2 109.5 . . ? C7D C8D H8D3 109.5 . . ? C7D C9D H9D1 109.5 . . ? C7D C9D H9D2 109.5 . . ? C7D C9D H9D3 109.5 . . ? C7D C10D H0D1 109.5 . . ? C7D C10D H0D2 109.5 . . ? C7D C10D H0D3 109.5 . . ? C7D C11D H1D1 109.5 . . ? C7D C11D H1D2 109.5 . . ? C7D C11D H1D3 109.5 . . ? C7D C12D H2D1 109.5 . . ? C7D C12D H2D2 109.5 . . ? C7D C12D H2D3 109.5 . . ? C7D C13D H3D1 109.5 . . ? C7D C13D H3D2 109.5 . . ? C7D C13D H3D3 109.5 . . ? C2D C20D C6A 116.7(10) . . ? C2D C20D H20G 108.1 . . ? C6A C20D H20G 108.1 . . ? C2D C20D H20H 108.1 . . ? C6A C20D H20H 108.1 . . ? H20G C20D H20H 107.3 . . ? C1* O1* W1 117.7(6) . . ? O1* C1* C6* 116.4(10) . . ? O1* C1* C2* 123.6(10) . . ? C6* C1* C2* 119.9(11) . . ? C3* C2* C1* 117.2(12) . . ? C3* C2* H2* 121.4 . . ? C1* C2* H2* 121.4 . . ? C2* C3* C4* 120.3(13) . . ? C2* C3* H3* 119.9 . . ? C4* C3* H3* 119.9 . . ? C5* C4* C3* 122.2(13) . . ? C5* C4* H4* 118.9 . . ? C3* C4* H4* 118.9 . . ? C6* C5* C4* 117.3(12) . . ? C6* C5* H5* 121.3 . . ? C4* C5* H5* 121.3 . . ? C5* C6* C1* 123.1(12) . . ? C5* C6* O2* 126.0(11) . . ? C1* C6* O2* 110.9(9) . . ? C6* O2* W1 116.9(6) . . ? O3G C1G C4G 122(4) . . ? O3G C1G C2G 118(5) . . ? C4G C1G C2G 120(3) . . ? C1G C2G H2G1 109.5 . . ? C1G C2G H2G2 109.5 . . ? H2G1 C2G H2G2 109.5 . . ? C1G C2G H2G3 109.5 . . ? H2G1 C2G H2G3 109.5 . . ? H2G2 C2G H2G3 109.5 . . ? C1G C4G H4G1 109.5 . . ? C1G C4G H4G2 109.5 . . ? H4G1 C4G H4G2 109.5 . . ? C1G C4G H4G3 109.5 . . ? H4G1 C4G H4G3 109.5 . . ? H4G2 C4G H4G3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.11 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 4.153 _refine_diff_density_min -4.082 _refine_diff_density_rms 0.213 # Attachment '4a_DMF.cif' data_calixw3 _database_code_depnum_ccdc_archive 'CCDC 299164' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H27 N O6 W' _chemical_formula_weight 693.39 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' 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' W W -0.8490 6.8722 '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/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.789(5) _cell_length_b 17.600(5) _cell_length_c 16.397(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.940(5) _cell_angle_gamma 90.00 _cell_volume 2527.0(18) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 26 _cell_measurement_theta_min 15 _cell_measurement_theta_max 20 _exptl_crystal_description 'thick column' _exptl_crystal_colour orange _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.823 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 4.620 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 1.12 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Philips PW1100' _diffrn_measurement_method 'scintil counter' _diffrn_detector_area_resol_mean 1K _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11417 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0727 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 34.99 _reflns_number_total 11083 _reflns_number_gt 5990 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DIPCHIGE software package, 2004' _computing_cell_refinement 'DIPCHIGE software package, 2004' _computing_data_reduction 'DIFAU92, 1992' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Accelrys DS-ViewerPro 2005' _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^)+(0.1168P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11083 _refine_ls_number_parameters 357 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1169 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.1801 _refine_ls_wR_factor_gt 0.1629 _refine_ls_goodness_of_fit_ref 0.857 _refine_ls_restrained_S_all 0.857 _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 W1 W 0.28553(2) 0.417335(13) 0.255172(16) 0.03681(9) Uani 1 1 d . . . O1A O 0.2401(4) 0.3427(2) 0.1707(3) 0.0425(10) Uani 1 1 d . . . C1A C 0.3348(6) 0.2880(3) 0.1440(4) 0.0385(13) Uani 1 1 d . . . C2A C 0.3396(7) 0.2172(3) 0.1818(4) 0.0422(14) Uani 1 1 d . . . C3A C 0.4434(7) 0.1634(4) 0.1568(4) 0.0462(15) Uani 1 1 d . . . H3A H 0.4499 0.1145 0.1828 0.063(7) Uiso 1 1 calc R . . C4A C 0.5359(8) 0.1793(4) 0.0955(4) 0.0502(16) Uani 1 1 d . . . H4A H 0.6077 0.1420 0.0799 0.063(7) Uiso 1 1 calc R . . C5A C 0.5259(8) 0.2496(4) 0.0560(4) 0.0469(14) Uani 1 1 d . . . H5A H 0.5888 0.2598 0.0122 0.063(7) Uiso 1 1 calc R . . C6A C 0.4246(7) 0.3056(4) 0.0798(4) 0.0423(14) Uani 1 1 d . . . C20A C 0.2387(7) 0.1994(4) 0.2521(4) 0.0448(15) Uani 1 1 d . . . H20A H 0.1490 0.2307 0.2454 0.041(7) Uiso 1 1 calc R . . H20B H 0.2062 0.1474 0.2472 0.041(7) Uiso 1 1 calc R . . O1B O 0.2360(4) 0.3428(2) 0.3349(3) 0.0433(10) Uani 1 1 d . . . C1B C 0.3150(6) 0.2852(3) 0.3750(4) 0.0414(13) Uani 1 1 d . . . C2B C 0.3953(7) 0.2993(3) 0.4503(4) 0.0422(14) Uani 1 1 d . . . C3B C 0.4731(8) 0.2403(4) 0.4905(4) 0.0506(16) Uani 1 1 d . . . H3B H 0.5281 0.2492 0.5428 0.063(7) Uiso 1 1 calc R . . C4B C 0.4726(9) 0.1681(4) 0.4564(5) 0.0584(19) Uani 1 1 d . . . H4B H 0.5259 0.1271 0.4850 0.063(7) Uiso 1 1 calc R . . C5B C 0.3941(8) 0.1559(4) 0.3805(5) 0.0493(16) Uani 1 1 d . . . H5B H 0.3956 0.1060 0.3570 0.063(7) Uiso 1 1 calc R . . C6B C 0.3151(6) 0.2117(3) 0.3378(4) 0.0418(14) Uani 1 1 d . . . C20B C 0.4129(8) 0.3795(4) 0.4845(4) 0.0493(16) Uani 1 1 d . . . H20C H 0.4296 0.3773 0.5431 0.041(7) Uiso 1 1 calc R . . H20D H 0.3205 0.4076 0.4708 0.041(7) Uiso 1 1 calc R . . O1C O 0.3859(4) 0.4759(2) 0.3430(3) 0.0423(10) Uani 1 1 d . . . C1C C 0.5299(6) 0.4662(3) 0.3819(4) 0.0377(12) Uani 1 1 d . . . C2C C 0.6537(7) 0.5021(3) 0.3459(4) 0.0381(12) Uani 1 1 d . . . C3C C 0.8000(7) 0.4875(3) 0.3842(4) 0.0457(15) Uani 1 1 d . . . H3C H 0.8874 0.5101 0.3625 0.063(7) Uiso 1 1 calc R . . C4C C 0.8209(8) 0.4413(4) 0.4524(5) 0.0502(16) Uani 1 1 d . . . H4C H 0.9223 0.4310 0.4765 0.063(7) Uiso 1 1 calc R . . C5C C 0.6970(9) 0.4101(4) 0.4860(4) 0.0514(17) Uani 1 1 d . . . H5C H 0.7127 0.3803 0.5351 0.063(7) Uiso 1 1 calc R . . C6C C 0.5484(8) 0.4210(3) 0.4496(4) 0.0422(13) Uani 1 1 d . . . C20C C 0.6278(7) 0.5541(3) 0.2730(4) 0.0422(13) Uani 1 1 d . . . H20E H 0.5260 0.5741 0.2718 0.041(7) Uiso 1 1 calc R . . H20F H 0.6972 0.5961 0.2804 0.041(7) Uiso 1 1 calc R . . O1D O 0.3869(4) 0.4760(2) 0.1797(3) 0.0413(9) Uani 1 1 d . . . C1D C 0.5279(6) 0.4758(3) 0.1488(4) 0.0376(12) Uani 1 1 d . . . C2D C 0.5457(8) 0.4355(4) 0.0782(4) 0.0435(14) Uani 1 1 d . . . C3D C 0.6887(9) 0.4403(4) 0.0445(4) 0.0476(15) Uani 1 1 d . . . H3D H 0.7042 0.4143 -0.0055 0.063(7) Uiso 1 1 calc R . . C4D C 0.8056(8) 0.4824(4) 0.0839(5) 0.0583(19) Uani 1 1 d . . . H4D H 0.9017 0.4859 0.0604 0.063(7) Uiso 1 1 calc R . . C5D C 0.7865(7) 0.5194(4) 0.1558(4) 0.0462(15) Uani 1 1 d . . . H5D H 0.8707 0.5471 0.1825 0.063(7) Uiso 1 1 calc R . . C6D C 0.6480(6) 0.5177(3) 0.1915(4) 0.0387(12) Uani 1 1 d . . . C20D C 0.4205(8) 0.3829(4) 0.0405(4) 0.0474(15) Uani 1 1 d . . . H20G H 0.3228 0.4058 0.0462 0.041(7) Uiso 1 1 calc R . . H20H H 0.4317 0.3773 -0.0169 0.041(7) Uiso 1 1 calc R . . O1 O 0.1150(4) 0.4642(3) 0.2469(3) 0.0551(13) Uani 1 1 d . . . O1G O 0.5180(4) 0.3555(2) 0.2604(2) 0.0342(8) Uani 1 1 d . . . C1G C 0.6129(6) 0.3164(3) 0.3029(4) 0.0349(11) Uani 1 1 d . . . H1G H 0.5825 0.2976 0.3540 0.093(12) Uiso 1 1 calc R . . N1G N 0.7499(5) 0.2987(3) 0.2840(3) 0.0325(9) Uani 1 1 d . . . C2G C 0.8126(8) 0.3231(5) 0.2084(5) 0.061(2) Uani 1 1 d . . . H2G1 H 0.7307 0.3379 0.1691 0.093(12) Uiso 1 1 calc R . . H2G2 H 0.8681 0.2818 0.1867 0.093(12) Uiso 1 1 calc R . . H2G3 H 0.8800 0.3654 0.2198 0.093(12) Uiso 1 1 calc R . . C3G C 0.8521(8) 0.2535(5) 0.3420(5) 0.062(2) Uani 1 1 d . . . H3G1 H 0.8003 0.2419 0.3897 0.093(12) Uiso 1 1 calc R . . H3G2 H 0.9427 0.2823 0.3578 0.093(12) Uiso 1 1 calc R . . H3G3 H 0.8795 0.2072 0.3161 0.093(12) 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 W1 0.01398(9) 0.02888(12) 0.06717(19) -0.00353(10) 0.00116(8) 0.00603(7) O1A 0.0235(17) 0.033(2) 0.069(3) -0.0052(19) -0.0078(18) 0.0039(15) C1A 0.023(2) 0.034(3) 0.055(3) -0.009(2) -0.010(2) 0.001(2) C2A 0.028(2) 0.030(3) 0.067(4) -0.009(3) -0.006(3) -0.003(2) C3A 0.037(3) 0.037(3) 0.064(4) -0.010(3) -0.005(3) 0.003(3) C4A 0.041(3) 0.042(3) 0.067(4) -0.014(3) 0.002(3) 0.007(3) C5A 0.043(3) 0.048(4) 0.049(4) -0.006(3) 0.001(3) 0.003(3) C6A 0.036(3) 0.039(3) 0.049(3) -0.009(3) -0.012(3) 0.000(2) C20A 0.028(2) 0.027(3) 0.080(5) -0.010(3) 0.006(3) -0.009(2) O1B 0.0208(16) 0.033(2) 0.077(3) -0.001(2) 0.0122(18) 0.0013(15) C1B 0.022(2) 0.038(3) 0.067(4) 0.003(3) 0.017(2) -0.001(2) C2B 0.034(3) 0.039(3) 0.055(4) 0.000(3) 0.019(3) -0.005(2) C3B 0.048(4) 0.052(4) 0.054(4) 0.006(3) 0.017(3) -0.003(3) C4B 0.050(4) 0.044(4) 0.084(5) 0.014(4) 0.017(4) 0.003(3) C5B 0.049(4) 0.034(3) 0.067(4) 0.002(3) 0.020(3) -0.003(3) C6B 0.025(2) 0.034(3) 0.068(4) 0.001(3) 0.015(3) -0.003(2) C20B 0.046(4) 0.046(4) 0.058(4) -0.010(3) 0.018(3) -0.003(3) O1C 0.0242(17) 0.037(2) 0.066(3) -0.0090(19) 0.0065(18) 0.0052(16) C1C 0.028(2) 0.035(3) 0.051(3) -0.010(2) 0.003(2) 0.002(2) C2C 0.031(2) 0.025(2) 0.058(4) -0.004(2) 0.004(2) -0.0021(19) C3C 0.029(2) 0.036(3) 0.071(4) -0.002(3) -0.006(3) -0.006(2) C4C 0.039(3) 0.042(3) 0.066(4) 0.007(3) -0.015(3) -0.005(3) C5C 0.048(4) 0.053(4) 0.051(4) 0.006(3) -0.006(3) -0.006(3) C6C 0.037(3) 0.044(3) 0.046(3) -0.008(3) 0.007(3) -0.001(2) C20C 0.028(2) 0.028(3) 0.070(4) -0.002(3) -0.003(3) -0.002(2) O1D 0.0233(16) 0.038(2) 0.061(3) 0.0062(19) -0.0045(17) 0.0062(16) C1D 0.027(2) 0.036(3) 0.049(3) 0.010(2) -0.004(2) 0.005(2) C2D 0.037(3) 0.043(3) 0.049(4) 0.009(3) -0.002(3) 0.007(3) C3D 0.054(4) 0.039(3) 0.050(4) 0.012(3) 0.011(3) 0.004(3) C4D 0.040(3) 0.054(4) 0.084(5) 0.017(4) 0.023(4) 0.007(3) C5D 0.029(3) 0.047(4) 0.063(4) 0.018(3) 0.006(3) -0.003(3) C6D 0.030(2) 0.030(3) 0.055(3) 0.012(2) 0.000(2) 0.001(2) C20D 0.046(3) 0.047(4) 0.047(3) 0.000(3) -0.012(3) 0.006(3) O1 0.0183(17) 0.047(3) 0.099(4) 0.003(3) 0.001(2) 0.0196(17) O1G 0.0172(14) 0.0271(17) 0.057(2) -0.0058(16) -0.0032(15) 0.0070(13) C1G 0.021(2) 0.036(3) 0.048(3) -0.002(2) 0.005(2) 0.0028(19) N1G 0.0161(16) 0.035(2) 0.046(3) 0.004(2) 0.0008(17) 0.0041(16) C2G 0.035(3) 0.081(6) 0.070(5) 0.023(4) 0.018(3) 0.019(4) C3G 0.035(3) 0.075(5) 0.076(5) 0.022(4) 0.004(3) 0.024(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O1 1.706(4) . ? W1 O1D 1.892(4) . ? W1 O1C 1.922(4) . ? W1 O1A 1.927(4) . ? W1 O1B 1.928(5) . ? W1 O1G 2.310(3) . ? O1A C1A 1.368(7) . ? C1A C2A 1.391(9) . ? C1A C6A 1.403(9) . ? C2A C3A 1.401(8) . ? C2A C20A 1.545(9) . ? C3A C4A 1.374(10) . ? C4A C5A 1.396(9) . ? C5A C6A 1.406(9) . ? C6A C20D 1.505(9) . ? C20A C6B 1.520(9) . ? O1B C1B 1.366(7) . ? C1B C2B 1.391(10) . ? C1B C6B 1.429(9) . ? C2B C3B 1.380(9) . ? C2B C20B 1.522(9) . ? C3B C4B 1.388(10) . ? C4B C5B 1.387(11) . ? C5B C6B 1.361(9) . ? C20B C6C 1.548(9) . ? O1C C1C 1.378(7) . ? C1C C6C 1.364(9) . ? C1C C2C 1.429(8) . ? C2C C3C 1.405(8) . ? C2C C20C 1.507(9) . ? C3C C4C 1.381(10) . ? C4C C5C 1.377(11) . ? C5C C6C 1.402(11) . ? C20C C6D 1.507(9) . ? O1D C1D 1.379(7) . ? C1D C2D 1.379(9) . ? C1D C6D 1.422(8) . ? C2D C3D 1.417(10) . ? C2D C20D 1.527(9) . ? C3D C4D 1.381(11) . ? C4D C5D 1.370(11) . ? C5D C6D 1.395(8) . ? O1G C1G 1.247(7) . ? C1G N1G 1.307(7) . ? N1G C2G 1.463(9) . ? N1G C3G 1.482(8) . ? 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 W1 O1D 98.3(2) . . ? O1 W1 O1C 98.3(2) . . ? O1D W1 O1C 89.18(19) . . ? O1 W1 O1A 98.4(2) . . ? O1D W1 O1A 88.9(2) . . ? O1C W1 O1A 163.32(16) . . ? O1 W1 O1B 97.7(2) . . ? O1D W1 O1B 163.97(16) . . ? O1C W1 O1B 88.46(19) . . ? O1A W1 O1B 88.8(2) . . ? O1 W1 O1G 177.4(2) . . ? O1D W1 O1G 79.41(15) . . ? O1C W1 O1G 82.96(15) . . ? O1A W1 O1G 80.40(15) . . ? O1B W1 O1G 84.56(15) . . ? C1A O1A W1 128.0(3) . . ? O1A C1A C2A 118.9(6) . . ? O1A C1A C6A 118.8(5) . . ? C2A C1A C6A 122.3(6) . . ? C1A C2A C3A 118.1(6) . . ? C1A C2A C20A 121.1(5) . . ? C3A C2A C20A 120.7(6) . . ? C4A C3A C2A 121.1(6) . . ? C3A C4A C5A 120.2(6) . . ? C6A C5A C4A 120.6(7) . . ? C5A C6A C1A 117.7(6) . . ? C5A C6A C20D 120.5(6) . . ? C1A C6A C20D 121.7(6) . . ? C6B C20A C2A 115.1(5) . . ? C1B O1B W1 134.1(3) . . ? O1B C1B C2B 119.5(6) . . ? O1B C1B C6B 119.1(6) . . ? C2B C1B C6B 121.4(6) . . ? C1B C2B C3B 118.8(6) . . ? C1B C2B C20B 121.4(6) . . ? C3B C2B C20B 119.5(6) . . ? C2B C3B C4B 120.8(7) . . ? C3B C4B C5B 119.2(7) . . ? C6B C5B C4B 122.8(7) . . ? C5B C6B C1B 116.9(6) . . ? C5B C6B C20A 122.5(6) . . ? C1B C6B C20A 120.4(6) . . ? C2B C20B C6C 111.0(5) . . ? C1C O1C W1 128.6(3) . . ? O1C C1C C6C 119.4(6) . . ? O1C C1C C2C 117.1(5) . . ? C6C C1C C2C 123.5(6) . . ? C3C C2C C1C 115.8(6) . . ? C3C C2C C20C 122.4(5) . . ? C1C C2C C20C 121.8(5) . . ? C4C C3C C2C 121.4(6) . . ? C3C C4C C5C 120.3(6) . . ? C6C C5C C4C 121.0(6) . . ? C1C C6C C5C 117.9(6) . . ? C1C C6C C20B 122.3(6) . . ? C5C C6C C20B 119.7(6) . . ? C6D C20C C2C 115.1(5) . . ? C1D O1D W1 136.7(4) . . ? O1D C1D C2D 118.8(5) . . ? O1D C1D C6D 118.1(6) . . ? C2D C1D C6D 123.2(6) . . ? C1D C2D C3D 117.7(6) . . ? C1D C2D C20D 121.4(6) . . ? C3D C2D C20D 120.8(7) . . ? C4D C3D C2D 120.0(7) . . ? C3D C4D C5D 121.0(7) . . ? C4D C5D C6D 121.8(7) . . ? C5D C6D C1D 116.3(6) . . ? C5D C6D C20C 122.4(6) . . ? C1D C6D C20C 121.2(5) . . ? C6A C20D C2D 112.6(5) . . ? C1G O1G W1 145.9(4) . . ? O1G C1G N1G 125.8(6) . . ? C1G N1G C2G 123.6(5) . . ? C1G N1G C3G 119.7(5) . . ? C2G N1G C3G 116.7(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 34.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 4.023 _refine_diff_density_min -8.021 _refine_diff_density_rms 0.272 # Attachment '4c_CH3CN.cif' data_calixw6 _database_code_depnum_ccdc_archive 'CCDC 299165' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13.50 H14 N0.25 O1.25 W0.25' _chemical_formula_weight 245.71 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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' _cell_length_a 13.292(5) _cell_length_b 13.292(5) _cell_length_c 13.743(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2428.1(16) _cell_formula_units_Z 8 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 34 _cell_measurement_theta_min 11 _cell_measurement_theta_max 16 _exptl_crystal_description 'Thin plate' _exptl_crystal_colour orange _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1002 _exptl_absorpt_coefficient_mu 2.425 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.78 _exptl_absorpt_correction_T_max 1.2 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Philips Pw1100' _diffrn_measurement_method 'scintil counter' _diffrn_detector_area_resol_mean 1K _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3115 _diffrn_reflns_av_R_equivalents 0.0587 _diffrn_reflns_av_sigmaI/netI 0.1000 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 22.00 _reflns_number_total 1490 _reflns_number_gt 1075 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DIPCHIGE sofware package, 2004' _computing_cell_refinement 'DIPCHIGE sofware package, 2004' _computing_data_reduction 'DIFAU92, 1992' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Accelrys DS-ViewerPro 2005' _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^)+(0.0628P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1490 _refine_ls_number_parameters 147 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0668 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.0995 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 0.780 _refine_ls_restrained_S_all 0.780 _refine_ls_shift/su_max 0.040 _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 W1 W 0.2500 0.2500 0.43247(5) 0.0513(3) Uani 1 4 d S . . O1 O 0.3072(3) 0.1185(3) 0.4542(4) 0.0537(14) Uani 1 1 d . . . O2 O 0.2500 0.2500 0.3115(8) 0.071(3) Uani 1 4 d S . . C1 C 0.3300(6) 0.0668(5) 0.5373(5) 0.051(2) Uani 1 1 d . . . C2 C 0.2565(6) 0.0037(5) 0.5764(6) 0.055(2) Uani 1 1 d . . . C4 C 0.3788(8) -0.0501(7) 0.6973(7) 0.075(3) Uani 1 1 d . . . C3 C 0.2843(7) -0.0534(6) 0.6557(7) 0.069(2) Uani 1 1 d . . . H3 H 0.2352 -0.0979 0.6836 0.061(16) Uiso 1 1 calc R . . C5 C 0.4472(7) 0.0180(7) 0.6564(7) 0.070(3) Uani 1 1 d . . . H5 H 0.5128 0.0239 0.6850 0.061(16) Uiso 1 1 calc R . . C6 C 0.4246(5) 0.0774(5) 0.5765(6) 0.0533(19) Uani 1 1 d . . . C7 C 0.4025(9) -0.1228(9) 0.7799(8) 0.112(4) Uani 1 1 d . . . C8 C 0.4653(13) -0.2073(9) 0.7472(10) 0.173(7) Uani 1 1 d . . . H8A H 0.5270 -0.1817 0.7207 0.25(3) Uiso 1 1 calc R . . H8B H 0.4309 -0.2431 0.6965 0.25(3) Uiso 1 1 calc R . . C9 C 0.4893(17) -0.2807(12) 0.8321(12) 0.197(8) Uani 1 1 d . . . H9A H 0.4290 -0.3167 0.8484 0.25(3) Uiso 1 1 calc R . . H9B H 0.5377 -0.3291 0.8097 0.25(3) Uiso 1 1 calc R . . C10 C 0.5263(17) -0.2359(15) 0.9158(15) 0.208(9) Uani 1 1 d . . . H10A H 0.5921 -0.2095 0.9026 0.25(3) Uiso 1 1 calc R . . H10B H 0.5331 -0.2863 0.9654 0.25(3) Uiso 1 1 calc R . . C11 C 0.4620(14) -0.1540(12) 0.9531(9) 0.166(6) Uani 1 1 d . . . H11A H 0.4963 -0.1195 1.0048 0.25(3) Uiso 1 1 calc R . . H11B H 0.4010 -0.1818 0.9791 0.25(3) Uiso 1 1 calc R . . C12 C 0.4350(12) -0.0748(10) 0.8672(9) 0.143(5) Uani 1 1 d . . . H12A H 0.3830 -0.0304 0.8895 0.25(3) Uiso 1 1 calc R . . H12B H 0.4934 -0.0348 0.8533 0.25(3) Uiso 1 1 calc R . . C20 C 0.1512(5) -0.0029(6) 0.5381(6) 0.063(2) Uani 1 1 d . . . H20A H 0.1253 -0.0685 0.5531 0.013(10) Uiso 1 1 calc R . . H20B H 0.1538 0.0028 0.4685 0.013(10) Uiso 1 1 calc R . . N1G N 0.2500 0.2500 0.6019(7) 0.026(3) Uani 1 4 d S . . C2G C 0.2500 0.2500 0.678(2) 0.146(11) Uani 1 4 d S . . C3G C 0.2500 0.2500 0.7681(12) 0.049(4) Uani 1 4 d S . . H1G H 0.1866 0.2253 0.7914 0.19(9) Uiso 0.25 1 calc PR . . H2G H 0.2603 0.3173 0.7914 0.19(9) Uiso 0.25 1 calc PR . . H3G H 0.3031 0.2074 0.7914 0.19(9) Uiso 0.25 1 calc PR . . 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 W1 0.0520(4) 0.0520(4) 0.0498(5) 0.000 0.000 0.000 O1 0.055(3) 0.041(3) 0.064(4) -0.009(3) -0.004(3) 0.012(2) O2 0.074(5) 0.074(5) 0.066(8) 0.000 0.000 0.000 C1 0.067(6) 0.039(5) 0.046(5) -0.003(4) -0.004(4) 0.017(4) C2 0.058(5) 0.041(4) 0.066(5) -0.002(5) -0.003(5) 0.001(4) C4 0.092(8) 0.060(6) 0.075(6) 0.006(5) -0.011(6) 0.010(6) C3 0.069(7) 0.053(5) 0.084(7) 0.013(5) -0.001(5) 0.000(5) C5 0.060(6) 0.062(6) 0.088(7) -0.012(5) -0.022(5) 0.012(5) C6 0.047(5) 0.050(5) 0.064(5) -0.002(5) -0.007(5) 0.008(4) C7 0.162(11) 0.097(8) 0.079(8) 0.004(7) -0.040(8) 0.051(8) C8 0.316(19) 0.102(9) 0.102(9) 0.024(8) -0.021(11) 0.100(12) C9 0.34(3) 0.107(12) 0.148(14) 0.033(11) -0.066(16) 0.079(14) C10 0.28(2) 0.175(17) 0.165(17) 0.026(15) -0.057(17) 0.103(17) C11 0.258(19) 0.171(14) 0.067(9) 0.026(9) -0.022(10) 0.054(14) C12 0.225(16) 0.101(9) 0.105(11) 0.007(8) -0.004(10) 0.024(10) C20 0.061(6) 0.062(5) 0.066(6) -0.016(4) -0.001(4) -0.013(5) N1G 0.034(4) 0.034(4) 0.010(6) 0.000 0.000 0.000 C2G 0.18(2) 0.18(2) 0.08(2) 0.000 0.000 0.000 C3G 0.053(7) 0.053(7) 0.039(11) 0.000 0.000 0.000 _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 W1 O2 1.663(11) . ? W1 O1 1.929(5) 3 ? W1 O1 1.929(5) 2 ? W1 O1 1.930(5) . ? W1 O1 1.930(5) 4 ? W1 N1G 2.329(10) . ? O1 C1 1.368(8) . ? C1 C6 1.375(10) . ? C1 C2 1.394(10) . ? C2 C3 1.379(11) . ? C2 C20 1.498(10) . ? C4 C3 1.381(12) . ? C4 C5 1.401(12) . ? C4 C7 1.524(12) . ? C3 H3 0.9600 . ? C5 C6 1.384(10) . ? C5 H5 0.9600 . ? C6 C20 1.526(10) 3 ? C7 C12 1.425(15) . ? C7 C8 1.470(15) . ? C8 C9 1.555(16) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C9 C10 1.385(19) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C10 C11 1.48(2) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C11 C12 1.622(17) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C20 C6 1.526(10) 4 ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? N1G C2G 1.05(3) . ? C2G C3G 1.23(3) . ? C3G H1G 0.9643 . ? C3G H2G 0.9643 . ? C3G H3G 0.9643 . ? 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 O2 W1 O1 98.88(14) . 3 ? O2 W1 O1 98.88(14) . 2 ? O1 W1 O1 88.64(4) 3 2 ? O2 W1 O1 98.88(14) . . ? O1 W1 O1 88.63(4) 3 . ? O1 W1 O1 162.2(3) 2 . ? O2 W1 O1 98.88(14) . 4 ? O1 W1 O1 162.2(3) 3 4 ? O1 W1 O1 88.63(4) 2 4 ? O1 W1 O1 88.63(4) . 4 ? O2 W1 N1G 180.000(2) . . ? O1 W1 N1G 81.12(14) 3 . ? O1 W1 N1G 81.12(14) 2 . ? O1 W1 N1G 81.12(14) . . ? O1 W1 N1G 81.12(14) 4 . ? C1 O1 W1 132.2(4) . . ? O1 C1 C6 118.6(7) . . ? O1 C1 C2 117.9(7) . . ? C6 C1 C2 123.4(7) . . ? C1 C2 C3 116.6(7) . . ? C1 C2 C20 123.6(8) . . ? C3 C2 C20 119.7(8) . . ? C3 C4 C5 116.4(8) . . ? C3 C4 C7 118.4(10) . . ? C5 C4 C7 125.1(10) . . ? C4 C3 C2 123.5(8) . . ? C4 C3 H3 118.2 . . ? C2 C3 H3 118.2 . . ? C4 C5 C6 123.0(8) . . ? C4 C5 H5 118.5 . . ? C6 C5 H5 118.5 . . ? C1 C6 C5 116.8(8) . . ? C1 C6 C20 123.7(8) . 3 ? C5 C6 C20 119.5(7) . 3 ? C12 C7 C8 115.3(11) . . ? C12 C7 C4 114.0(10) . . ? C8 C7 C4 111.9(10) . . ? C7 C8 C9 111.5(12) . . ? C7 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? C7 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? C10 C9 C8 115.2(15) . . ? C10 C9 H9A 108.5 . . ? C8 C9 H9A 108.5 . . ? C10 C9 H9B 108.5 . . ? C8 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? C9 C10 C11 113.6(16) . . ? C9 C10 H10A 108.9 . . ? C11 C10 H10A 108.8 . . ? C9 C10 H10B 108.8 . . ? C11 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C10 C11 C12 110.7(12) . . ? C10 C11 H11A 109.5 . . ? C12 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? C7 C12 C11 112.9(11) . . ? C7 C12 H12A 109.0 . . ? C11 C12 H12A 109.0 . . ? C7 C12 H12B 109.0 . . ? C11 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? C2 C20 C6 116.0(6) . 4 ? C2 C20 H20A 108.3 . . ? C6 C20 H20A 108.3 4 . ? C2 C20 H20B 108.3 . . ? C6 C20 H20B 108.3 4 . ? H20A C20 H20B 107.4 . . ? C2G N1G W1 180.000(7) . . ? N1G C2G C3G 180.000(7) . . ? C2G C3G H1G 110.0 . . ? C2G C3G H2G 110.0 . . ? H1G C3G H2G 108.9 . . ? C2G C3G H3G 110.0 . . ? H1G C3G H3G 108.9 . . ? H2G C3G H3G 108.9 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 22.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.594 _refine_diff_density_min -0.506 _refine_diff_density_rms 0.085 # Attachment '4a_H2O-AcOEt.cif' data_calixw7 _database_code_depnum_ccdc_archive 'CCDC 299166' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H30 O8 W' _chemical_formula_weight 726.41 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' W W -0.8490 6.8722 '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/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.302(5) _cell_length_b 14.802(5) _cell_length_c 17.226(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.050(5) _cell_angle_gamma 90.00 _cell_volume 2881.3(18) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 34 _cell_measurement_theta_min 14 _cell_measurement_theta_max 18 _exptl_crystal_description 'thin plate' _exptl_crystal_colour orange _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.675 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 4.060 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 1.12 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens AED' _diffrn_measurement_method 'scintil counter' _diffrn_detector_area_resol_mean 1K _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4670 _diffrn_reflns_av_R_equivalents 0.0302 _diffrn_reflns_av_sigmaI/netI 0.0641 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 24.04 _reflns_number_total 4510 _reflns_number_gt 2845 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DIPCHIGE software package, 2004' _computing_cell_refinement 'DIPCHIGE software package, 2004' _computing_data_reduction 'DIFAU92, 1992' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Accelrys DS-ViewerPro, 2005' _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^)+(0.0356P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4510 _refine_ls_number_parameters 382 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0664 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0689 _refine_ls_wR_factor_gt 0.0643 _refine_ls_goodness_of_fit_ref 0.843 _refine_ls_restrained_S_all 0.842 _refine_ls_shift/su_max 0.003 _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 W1 W 0.47141(2) 0.155242(16) 0.197660(16) 0.04648(10) Uani 1 1 d . . . O1A O 0.5570(4) 0.0948(3) 0.2784(2) 0.0564(11) Uani 1 1 d . . . C1A C 0.6182(7) 0.1238(4) 0.3429(4) 0.0593(18) Uani 1 1 d . . . C2A C 0.5623(7) 0.1353(4) 0.4114(4) 0.065(2) Uani 1 1 d . . . C3A C 0.6234(10) 0.1613(6) 0.4769(4) 0.098(3) Uani 1 1 d . . . H3A H 0.5843 0.1637 0.5259 0.099(8) Uiso 1 1 calc R . . C4A C 0.7387(10) 0.1836(7) 0.4724(6) 0.110(4) Uani 1 1 d . . . H4A H 0.7806 0.2046 0.5179 0.099(8) Uiso 1 1 calc R . . C5A C 0.7976(8) 0.1766(5) 0.4025(5) 0.086(3) Uani 1 1 d . . . H5A H 0.8799 0.1924 0.4007 0.099(8) Uiso 1 1 calc R . . C6A C 0.7396(6) 0.1469(4) 0.3351(4) 0.067(2) Uani 1 1 d . . . C20A C 0.4270(8) 0.1143(5) 0.4151(4) 0.084(2) Uani 1 1 d . . . H20A H 0.4072 0.0688 0.3773 0.054(6) Uiso 1 1 calc R . . H20B H 0.4094 0.0906 0.4654 0.054(6) Uiso 1 1 calc R . . O1B O 0.3399(3) 0.1630(3) 0.2645(2) 0.0574(11) Uani 1 1 d . . . C1B C 0.3128(6) 0.2200(5) 0.3254(4) 0.0622(19) Uani 1 1 d . . . C2B C 0.2480(6) 0.2977(5) 0.3084(5) 0.070(2) Uani 1 1 d . . . C3B C 0.2196(7) 0.3531(6) 0.3717(6) 0.092(3) Uani 1 1 d . . . H3B H 0.1742 0.4071 0.3629 0.099(8) Uiso 1 1 calc R . . C4B C 0.2553(9) 0.3316(7) 0.4451(6) 0.109(3) Uani 1 1 d . . . H4B H 0.2344 0.3707 0.4871 0.099(8) Uiso 1 1 calc R . . C5B C 0.3206(8) 0.2553(6) 0.4609(5) 0.093(3) Uani 1 1 d . . . H5B H 0.3449 0.2415 0.5132 0.099(8) Uiso 1 1 calc R . . C6B C 0.3513(7) 0.1979(5) 0.3996(5) 0.070(2) Uani 1 1 d . . . C20B C 0.2157(5) 0.3243(5) 0.2256(5) 0.076(2) Uani 1 1 d . . . H20C H 0.2020 0.2704 0.1958 0.054(6) Uiso 1 1 calc R . . H20D H 0.1430 0.3578 0.2259 0.054(6) Uiso 1 1 calc R . . O1C O 0.4017(3) 0.2498(3) 0.1364(2) 0.0520(11) Uani 1 1 d . . . C1C C 0.3985(5) 0.3414(4) 0.1443(3) 0.0468(14) Uani 1 1 d . . . C2C C 0.4878(6) 0.3918(4) 0.1095(3) 0.0529(16) Uani 1 1 d . . . C3C C 0.4794(6) 0.4862(4) 0.1156(4) 0.0604(18) Uani 1 1 d . . . H3C H 0.5381 0.5231 0.0914 0.099(8) Uiso 1 1 calc R . . C4C C 0.3897(6) 0.5271(5) 0.1552(4) 0.072(2) Uani 1 1 d . . . H4C H 0.3847 0.5917 0.1575 0.099(8) Uiso 1 1 calc R . . C5C C 0.3071(6) 0.4746(5) 0.1914(4) 0.070(2) Uani 1 1 d . . . H5C H 0.2470 0.5034 0.2213 0.099(8) Uiso 1 1 calc R . . C6C C 0.3084(5) 0.3803(4) 0.1857(4) 0.0552(17) Uani 1 1 d . . . C20C C 0.5879(6) 0.3479(5) 0.0685(3) 0.0597(17) Uani 1 1 d . . . H20E H 0.5606 0.2925 0.0453 0.054(6) Uiso 1 1 calc R . . H20F H 0.6136 0.3869 0.0276 0.054(6) Uiso 1 1 calc R . . O1D O 0.6176(3) 0.1800(2) 0.1491(2) 0.0484(10) Uani 1 1 d . . . C1D C 0.7032(5) 0.2457(4) 0.1610(4) 0.0490(16) Uani 1 1 d . . . C2D C 0.7961(5) 0.2277(4) 0.2139(4) 0.0547(17) Uani 1 1 d . . . C3D C 0.8821(5) 0.2939(5) 0.2234(5) 0.074(2) Uani 1 1 d . . . H3D H 0.9498 0.2821 0.2563 0.099(8) Uiso 1 1 calc R . . C4D C 0.8723(6) 0.3760(5) 0.1867(5) 0.077(2) Uani 1 1 d . . . H4D H 0.9302 0.4223 0.1968 0.099(8) Uiso 1 1 calc R . . C5D C 0.7801(6) 0.3922(4) 0.1355(4) 0.0600(18) Uani 1 1 d . . . H5D H 0.7765 0.4488 0.1083 0.099(8) Uiso 1 1 calc R . . C6D C 0.6913(5) 0.3279(4) 0.1222(3) 0.0510(16) Uani 1 1 d . . . C20D C 0.8013(5) 0.1400(4) 0.2590(4) 0.070(2) Uani 1 1 d . . . H20G H 0.7651 0.0929 0.2284 0.054(6) Uiso 1 1 calc R . . H20H H 0.8825 0.1237 0.2684 0.054(6) Uiso 1 1 calc R . . O1E O 0.4286(4) 0.0640(3) 0.1451(3) 0.0704(13) Uani 1 1 d . . . O1W O 0.5302(3) 0.2801(3) 0.2713(2) 0.0413(9) Uani 1 1 d D . . O1G O 0.6627(14) 0.3822(10) 0.3599(9) 0.322(8) Uani 1 1 d . . . O2G O 0.6304(8) 0.5059(5) 0.4109(4) 0.125(2) Uani 1 1 d . . . C1G C 0.7112(14) 0.4355(9) 0.3978(7) 0.134(4) Uani 1 1 d . . . C2G C 0.8249(11) 0.4447(7) 0.4339(7) 0.157(5) Uani 1 1 d . . . H2G1 H 0.8166 0.4696 0.4850 0.22(2) Uiso 1 1 calc R . . H2G2 H 0.8729 0.4841 0.4034 0.22(2) Uiso 1 1 calc R . . H2G3 H 0.8620 0.3864 0.4376 0.22(2) Uiso 1 1 calc R . . C3G C 0.5169(11) 0.4872(12) 0.3673(10) 0.218(9) Uani 1 1 d . . . H3G1 H 0.4756 0.4354 0.3865 0.22(2) Uiso 1 1 calc R . . H3G2 H 0.5269 0.4825 0.3123 0.22(2) Uiso 1 1 calc R . . C4G C 0.4575(11) 0.5826(10) 0.3934(7) 0.170(6) Uani 1 1 d . . . H4G1 H 0.5097 0.6315 0.3811 0.22(2) Uiso 1 1 calc R . . H4G2 H 0.4443 0.5819 0.4483 0.22(2) Uiso 1 1 calc R . . H4G3 H 0.3834 0.5907 0.3661 0.22(2) Uiso 1 1 calc R . . H1W H 0.470(6) 0.310(5) 0.300(5) 0.20(4) Uiso 1 1 d D . . H2W H 0.592(6) 0.322(4) 0.261(6) 0.20(4) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.04901(15) 0.03597(13) 0.05407(16) -0.00727(16) -0.00975(10) -0.00625(15) O1A 0.070(3) 0.038(2) 0.061(3) 0.009(2) -0.010(2) 0.003(2) C1A 0.090(6) 0.040(4) 0.048(4) 0.005(3) -0.019(4) 0.004(3) C2A 0.083(5) 0.060(5) 0.052(4) 0.018(4) -0.008(4) 0.033(4) C3A 0.146(9) 0.114(7) 0.034(4) 0.017(5) -0.032(5) -0.001(7) C4A 0.128(9) 0.113(8) 0.085(7) 0.010(6) -0.067(7) 0.011(7) C5A 0.085(6) 0.088(6) 0.084(6) 0.007(5) -0.046(5) 0.012(5) C6A 0.067(4) 0.043(4) 0.089(5) 0.010(4) -0.034(4) 0.017(4) C20A 0.141(8) 0.066(5) 0.046(5) 0.015(4) 0.015(5) -0.003(5) O1B 0.049(2) 0.052(3) 0.072(3) -0.001(3) 0.001(2) -0.007(2) C1B 0.062(4) 0.053(4) 0.073(5) -0.010(4) 0.021(4) -0.016(4) C2B 0.041(4) 0.055(4) 0.113(7) -0.002(5) 0.016(4) -0.005(3) C3B 0.082(6) 0.068(6) 0.127(8) -0.004(6) 0.052(6) 0.012(5) C4B 0.137(9) 0.085(7) 0.106(8) -0.017(6) 0.071(7) -0.005(6) C5B 0.129(8) 0.076(6) 0.075(6) 0.003(5) 0.041(5) -0.014(6) C6B 0.081(5) 0.062(5) 0.068(5) 0.006(4) 0.029(4) -0.019(4) C20B 0.036(4) 0.066(5) 0.127(7) -0.006(5) -0.014(4) 0.008(3) O1C 0.056(3) 0.046(2) 0.054(3) -0.005(2) -0.022(2) -0.007(2) C1C 0.046(3) 0.049(3) 0.044(3) 0.000(3) -0.022(3) 0.001(3) C2C 0.061(4) 0.054(4) 0.043(4) 0.005(3) -0.019(3) 0.005(3) C3C 0.060(4) 0.051(4) 0.069(5) 0.012(4) -0.016(4) -0.008(3) C4C 0.055(5) 0.059(5) 0.101(6) 0.007(4) -0.019(4) 0.013(4) C5C 0.050(4) 0.071(5) 0.090(6) 0.005(4) -0.022(4) 0.020(4) C6C 0.034(3) 0.054(4) 0.077(5) 0.006(4) -0.016(3) 0.001(3) C20C 0.076(4) 0.061(4) 0.042(4) 0.007(4) -0.002(3) -0.014(4) O1D 0.051(2) 0.045(2) 0.049(2) -0.0129(19) 0.0004(19) -0.0074(19) C1D 0.042(4) 0.044(4) 0.062(4) -0.014(3) 0.009(3) 0.000(3) C2D 0.038(3) 0.048(4) 0.078(5) -0.003(3) 0.003(3) 0.009(3) C3D 0.033(4) 0.070(5) 0.118(7) -0.007(5) -0.009(4) -0.002(4) C4D 0.046(4) 0.059(5) 0.126(7) -0.006(5) 0.004(5) -0.006(3) C5D 0.051(4) 0.052(4) 0.078(5) -0.001(4) 0.023(4) 0.001(3) C6D 0.053(4) 0.051(4) 0.049(4) -0.004(3) 0.012(3) 0.002(3) C20D 0.042(4) 0.056(5) 0.111(6) -0.004(4) -0.012(4) 0.011(3) O1E 0.085(3) 0.040(3) 0.086(3) -0.027(2) -0.007(3) -0.014(2) O1W 0.038(2) 0.040(2) 0.046(2) -0.0051(18) 0.000(2) -0.0043(18) O1G 0.347(18) 0.271(15) 0.344(18) -0.154(13) -0.115(14) -0.044(13) O2G 0.158(7) 0.096(5) 0.121(5) -0.007(4) 0.019(5) -0.016(5) C1G 0.176(13) 0.106(9) 0.117(9) -0.033(7) -0.028(9) -0.035(9) C2G 0.139(10) 0.136(10) 0.196(12) -0.058(9) -0.017(9) -0.022(8) C3G 0.081(8) 0.30(2) 0.275(19) 0.190(18) -0.032(10) 0.004(11) C4G 0.123(10) 0.250(18) 0.138(10) 0.045(11) -0.017(8) -0.030(11) _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 W1 O1E 1.691(4) . ? W1 O1A 1.903(4) . ? W1 O1D 1.901(4) . ? W1 O1B 1.901(4) . ? W1 O1C 1.914(4) . ? W1 O1W 2.331(4) . ? O1A C1A 1.367(7) . ? C1A C2A 1.359(9) . ? C1A C6A 1.424(9) . ? C2A C3A 1.367(10) . ? C2A C20A 1.563(10) . ? C3A C4A 1.348(12) . ? C3A H3A 0.9600 . ? C4A C5A 1.390(12) . ? C4A H4A 0.9600 . ? C5A C6A 1.395(10) . ? C5A H5A 0.9600 . ? C6A C20D 1.499(9) . ? C20A C6B 1.525(10) . ? C20A H20A 0.9600 . ? C20A H20B 0.9600 . ? O1B C1B 1.384(7) . ? C1B C2B 1.392(9) . ? C1B C6B 1.383(9) . ? C2B C3B 1.407(10) . ? C2B C20B 1.518(10) . ? C3B C4B 1.358(12) . ? C3B H3B 0.9600 . ? C4B C5B 1.373(12) . ? C4B H4B 0.9600 . ? C5B C6B 1.404(10) . ? C5B H5B 0.9600 . ? C20B C6C 1.511(9) . ? C20B H20C 0.9600 . ? C20B H20D 0.9600 . ? O1C C1C 1.364(7) . ? C1C C6C 1.380(8) . ? C1C C2C 1.398(8) . ? C2C C3C 1.405(8) . ? C2C C20C 1.493(8) . ? C3C C4C 1.373(9) . ? C3C H3C 0.9600 . ? C4C C5C 1.372(9) . ? C4C H4C 0.9600 . ? C5C C6C 1.400(9) . ? C5C H5C 0.9600 . ? C20C C6D 1.506(8) . ? C20C H20E 0.9600 . ? C20C H20F 0.9600 . ? O1D C1D 1.383(6) . ? C1D C6D 1.394(8) . ? C1D C2D 1.404(8) . ? C2D C3D 1.388(8) . ? C2D C20D 1.514(8) . ? C3D C4D 1.374(10) . ? C3D H3D 0.9600 . ? C4D C5D 1.374(9) . ? C4D H4D 0.9600 . ? C5D C6D 1.399(8) . ? C5D H5D 0.9600 . ? C20D H20G 0.9600 . ? C20D H20H 0.9600 . ? O1W H1W 0.955(10) . ? O1W H2W 0.956(10) . ? O1G C1G 1.156(12) . ? O2G C1G 1.406(13) . ? O2G C3G 1.500(14) . ? C1G C2G 1.424(14) . ? C2G H2G1 0.9599 . ? C2G H2G2 0.9599 . ? C2G H2G3 0.9599 . ? C3G C4G 1.630(19) . ? C3G H3G1 0.9600 . ? C3G H3G2 0.9600 . ? C4G H4G1 0.9599 . ? C4G H4G2 0.9599 . ? C4G H4G3 0.9599 . ? 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 O1E W1 O1A 98.8(2) . . ? O1E W1 O1D 99.27(19) . . ? O1A W1 O1D 88.73(17) . . ? O1E W1 O1B 98.8(2) . . ? O1A W1 O1B 88.77(18) . . ? O1D W1 O1B 161.90(16) . . ? O1E W1 O1C 100.22(19) . . ? O1A W1 O1C 160.99(16) . . ? O1D W1 O1C 88.21(17) . . ? O1B W1 O1C 88.34(18) . . ? O1E W1 O1W 179.40(18) . . ? O1A W1 O1W 80.73(15) . . ? O1D W1 O1W 81.09(14) . . ? O1B W1 O1W 80.82(15) . . ? O1C W1 O1W 80.26(14) . . ? C1A O1A W1 133.6(4) . . ? C2A C1A O1A 120.6(7) . . ? C2A C1A C6A 121.1(7) . . ? O1A C1A C6A 118.2(6) . . ? C3A C2A C1A 121.0(8) . . ? C3A C2A C20A 120.2(8) . . ? C1A C2A C20A 118.7(7) . . ? C2A C3A C4A 119.7(9) . . ? C2A C3A H3A 120.2 . . ? C4A C3A H3A 120.2 . . ? C3A C4A C5A 120.7(8) . . ? C3A C4A H4A 119.6 . . ? C5A C4A H4A 119.6 . . ? C6A C5A C4A 121.3(8) . . ? C6A C5A H5A 119.4 . . ? C4A C5A H5A 119.4 . . ? C5A C6A C1A 115.8(8) . . ? C5A C6A C20D 122.1(7) . . ? C1A C6A C20D 122.1(6) . . ? C6B C20A C2A 112.2(6) . . ? C6B C20A H20A 109.2 . . ? C2A C20A H20A 109.2 . . ? C6B C20A H20B 109.2 . . ? C2A C20A H20B 109.2 . . ? H20A C20A H20B 107.9 . . ? C1B O1B W1 133.0(4) . . ? C2B C1B C6B 123.1(7) . . ? C2B C1B O1B 117.8(7) . . ? C6B C1B O1B 119.1(7) . . ? C1B C2B C3B 116.5(8) . . ? C1B C2B C20B 121.9(7) . . ? C3B C2B C20B 121.5(7) . . ? C4B C3B C2B 121.1(8) . . ? C4B C3B H3B 119.5 . . ? C2B C3B H3B 119.5 . . ? C3B C4B C5B 121.9(9) . . ? C3B C4B H4B 119.1 . . ? C5B C4B H4B 119.1 . . ? C4B C5B C6B 119.2(9) . . ? C4B C5B H5B 120.4 . . ? C6B C5B H5B 120.4 . . ? C1B C6B C5B 118.3(8) . . ? C1B C6B C20A 121.3(7) . . ? C5B C6B C20A 120.4(8) . . ? C6C C20B C2B 114.4(5) . . ? C6C C20B H20C 108.7 . . ? C2B C20B H20C 108.7 . . ? C6C C20B H20D 108.7 . . ? C2B C20B H20D 108.7 . . ? H20C C20B H20D 107.6 . . ? C1C O1C W1 133.1(3) . . ? O1C C1C C6C 119.1(6) . . ? O1C C1C C2C 117.8(6) . . ? C6C C1C C2C 123.0(6) . . ? C1C C2C C3C 116.6(6) . . ? C1C C2C C20C 122.0(6) . . ? C3C C2C C20C 121.4(6) . . ? C4C C3C C2C 121.8(7) . . ? C4C C3C H3C 119.1 . . ? C2C C3C H3C 119.1 . . ? C5C C4C C3C 119.4(7) . . ? C5C C4C H4C 120.3 . . ? C3C C4C H4C 120.3 . . ? C4C C5C C6C 121.6(7) . . ? C4C C5C H5C 119.2 . . ? C6C C5C H5C 119.2 . . ? C1C C6C C5C 117.4(6) . . ? C1C C6C C20B 122.1(6) . . ? C5C C6C C20B 120.5(7) . . ? C6D C20C C2C 112.5(5) . . ? C6D C20C H20E 109.1 . . ? C2C C20C H20E 109.1 . . ? C6D C20C H20F 109.1 . . ? C2C C20C H20F 109.1 . . ? H20E C20C H20F 107.8 . . ? C1D O1D W1 133.0(3) . . ? O1D C1D C6D 118.8(5) . . ? O1D C1D C2D 118.4(6) . . ? C6D C1D C2D 122.7(6) . . ? C3D C2D C1D 117.2(6) . . ? C3D C2D C20D 121.7(6) . . ? C1D C2D C20D 121.1(6) . . ? C4D C3D C2D 121.4(7) . . ? C4D C3D H3D 119.3 . . ? C2D C3D H3D 119.3 . . ? C3D C4D C5D 120.2(7) . . ? C3D C4D H4D 119.9 . . ? C5D C4D H4D 119.9 . . ? C6D C5D C4D 121.3(7) . . ? C6D C5D H5D 119.3 . . ? C4D C5D H5D 119.3 . . ? C1D C6D C5D 117.0(6) . . ? C1D C6D C20C 122.2(6) . . ? C5D C6D C20C 120.9(6) . . ? C6A C20D C2D 112.0(5) . . ? C6A C20D H20G 109.2 . . ? C2D C20D H20G 109.2 . . ? C6A C20D H20H 109.2 . . ? C2D C20D H20H 109.2 . . ? H20G C20D H20H 107.9 . . ? W1 O1W H1W 117(5) . . ? W1 O1W H2W 128(5) . . ? H1W O1W H2W 109.5(16) . . ? C1G O2G C3G 109.6(10) . . ? O1G C1G C2G 136.6(16) . . ? O1G C1G O2G 107.0(14) . . ? C2G C1G O2G 116.3(10) . . ? C1G C2G H2G1 109.5 . . ? C1G C2G H2G2 109.5 . . ? H2G1 C2G H2G2 109.5 . . ? C1G C2G H2G3 109.5 . . ? H2G1 C2G H2G3 109.5 . . ? H2G2 C2G H2G3 109.5 . . ? O2G C3G C4G 93.2(13) . . ? O2G C3G H3G1 113.1 . . ? C4G C3G H3G1 113.1 . . ? O2G C3G H3G2 113.1 . . ? C4G C3G H3G2 113.1 . . ? H3G1 C3G H3G2 110.5 . . ? C3G C4G H4G1 109.5 . . ? C3G C4G H4G2 109.5 . . ? H4G1 C4G H4G2 109.5 . . ? C3G C4G H4G3 109.5 . . ? H4G1 C4G H4G3 109.5 . . ? H4G2 C4G H4G3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.04 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.000 _refine_diff_density_min -1.210 _refine_diff_density_rms 0.093