# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'John Ripmeester' 'Philip O. Brown' 'Gary D. Enright' 'Konstantin A. Udachin' _publ_contact_author_name 'Prof John Ripmeester' _publ_contact_author_address ; National Res Council Canada Steacie Inst Mol Sci, 100 Sussex Dr Ottawa ON K1A 0R6 CANADA ; _publ_contact_author_email JOHN.RIPMEESTER@NRC.CA data_ku78 _database_code_CSD 181105 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common p-tert-butylcalix[4]arene*3n-butylamine _chemical_melting_point ? _chemical_formula_moiety 4(C44 H56 O4), 12(C4H11N) _chemical_formula_sum 'C224 H356 N12 O16' _chemical_formula_weight 868.30 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.9405(10) _cell_length_b 20.0923(10) _cell_length_c 20.7519(10) _cell_angle_alpha 90.000(10) _cell_angle_beta 91.122(10) _cell_angle_gamma 90.000(10) _cell_volume 5394.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.069 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 0.066 _exptl_absorpt_correction_type empirical absorbtion correction sadabs _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63839 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_sigmaI/netI 0.0598 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 28.75 _reflns_number_total 13993 _reflns_number_gt 6997 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0896P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13993 _refine_ls_number_parameters 699 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.1280 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1788 _refine_ls_wR_factor_gt 0.1519 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.129 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.32978(3) 0.500617(18) 0.19726(2) 0.05297(13) Uani 1 1 d D . . H1 H 0.3404(6) 0.5287(3) 0.1585(3) 0.091(2) Uiso 1 1 d D . . O2 O 0.36944(3) 0.569504(17) 0.102560(18) 0.04763(12) Uani 1 1 d . . . O3 O 0.56400(3) 0.543332(18) 0.11176(2) 0.05401(13) Uani 1 1 d D . . H3 H 0.4913(4) 0.5586(4) 0.1064(4) 0.113(3) Uiso 1 1 d D . . O4 O 0.51467(3) 0.455235(18) 0.225048(19) 0.05090(12) Uani 1 1 d D . . H4 H 0.4436(4) 0.4696(4) 0.2147(4) 0.101(3) Uiso 1 1 d D . . C7 C 0.17128(4) 0.59332(3) 0.15583(3) 0.04663(17) Uani 1 1 d . . . H7A H 0.1842 0.5530 0.1298 0.056 Uiso 1 1 calc R F . H7B H 0.0985 0.6069 0.1482 0.056 Uiso 1 1 calc R . . C12 C 0.33903(4) 0.63388(3) 0.10835(2) 0.03943(15) Uani 1 1 d . . . C13 C 0.24208(4) 0.64866(3) 0.13436(3) 0.03837(15) Uani 1 1 d . . . C14 C 0.21284(4) 0.71475(3) 0.14094(3) 0.03841(15) Uani 1 1 d . . . H14 H 0.1479 0.7243 0.1594 0.046 Uiso 1 1 calc R F . C15 C 0.27452(4) 0.76772(3) 0.12169(3) 0.03712(15) Uani 1 1 d . . . C16 C 0.36814(4) 0.75146(3) 0.09425(3) 0.03818(15) Uani 1 1 d . . . H16 H 0.4113 0.7864 0.0796 0.046 Uiso 1 1 calc R F . C17 C 0.40144(4) 0.68589(3) 0.08725(2) 0.03734(15) Uani 1 1 d . . . C18 C 0.50570(4) 0.67147(3) 0.05764(3) 0.04562(17) Uani 1 1 d . . . H18A H 0.4993 0.6309 0.0308 0.055 Uiso 1 1 calc R F . H18B H 0.5236 0.7088 0.0288 0.055 Uiso 1 1 calc R . . C19 C 0.23952(5) 0.83986(3) 0.13275(3) 0.05095(19) Uani 1 1 d . . . C20 C 0.24925(7) 0.85580(4) 0.20494(4) 0.0803(3) Uani 1 1 d . . . H20A H 0.2078 0.8241 0.2293 0.120 Uiso 1 1 calc R . . H20B H 0.2243 0.9011 0.2127 0.120 Uiso 1 1 calc R . . H20C H 0.3218 0.8524 0.2189 0.120 Uiso 1 1 calc R . . C21 C 0.12698(5) 0.84871(3) 0.10949(5) 0.0791(3) Uani 1 1 d . . . H21A H 0.1201 0.8344 0.0645 0.119 Uiso 1 1 calc R . . H21B H 0.1074 0.8957 0.1129 0.119 Uiso 1 1 calc R . . H21C H 0.0816 0.8217 0.1362 0.119 Uiso 1 1 calc R . . C22 C 0.30593(6) 0.88958(3) 0.09644(4) 0.0680(2) Uani 1 1 d . . . H22A H 0.3777 0.8863 0.1120 0.102 Uiso 1 1 calc R . . H22B H 0.2802 0.9348 0.1038 0.102 Uiso 1 1 calc R . . H22C H 0.3025 0.8796 0.0502 0.102 Uiso 1 1 calc R . . C23 C 0.61551(4) 0.59872(3) 0.13276(3) 0.04199(16) Uani 1 1 d . . . C24 C 0.59382(4) 0.66155(3) 0.10625(3) 0.04027(16) Uani 1 1 d . . . C25 C 0.65414(4) 0.71530(3) 0.12575(3) 0.04190(16) Uani 1 1 d . . . H25 H 0.6396 0.7577 0.1076 0.050 Uiso 1 1 calc R F . C26 C 0.73497(4) 0.70993(3) 0.17069(3) 0.04097(16) Uani 1 1 d . . . C27 C 0.75140(4) 0.64728(3) 0.19736(3) 0.04008(16) Uani 1 1 d . . . H27 H 0.8055 0.6421 0.2286 0.048 Uiso 1 1 calc R F . C28 C 0.69259(4) 0.59192(3) 0.18056(3) 0.03966(15) Uani 1 1 d . . . C29 C 0.70625(4) 0.52770(3) 0.21831(3) 0.04140(16) Uani 1 1 d . . . H29A H 0.7795 0.5230 0.2322 0.050 Uiso 1 1 calc R F . H29B H 0.6882 0.4894 0.1902 0.050 Uiso 1 1 calc R . . C30 C 0.79715(4) 0.77064(3) 0.19342(3) 0.04627(17) Uani 1 1 d . . . C31 C 0.73904(6) 0.80320(3) 0.24907(4) 0.0691(2) Uani 1 1 d . . . H31A H 0.6674 0.8120 0.2354 0.104 Uiso 1 1 calc R . . H31B H 0.7729 0.8452 0.2610 0.104 Uiso 1 1 calc R . . H31C H 0.7397 0.7732 0.2863 0.104 Uiso 1 1 calc R . . C32 C 0.80840(6) 0.82253(3) 0.14005(3) 0.0640(2) Uani 1 1 d . . . H32A H 0.8446 0.8027 0.1037 0.096 Uiso 1 1 calc R . . H32B H 0.8481 0.8606 0.1567 0.096 Uiso 1 1 calc R . . H32C H 0.7397 0.8376 0.1256 0.096 Uiso 1 1 calc R . . C33 C 0.90607(5) 0.75149(4) 0.21627(5) 0.0816(3) Uani 1 1 d . . . H33A H 0.9020 0.7243 0.2553 0.122 Uiso 1 1 calc R . . H33B H 0.9460 0.7919 0.2257 0.122 Uiso 1 1 calc R . . H33C H 0.9401 0.7260 0.1824 0.122 Uiso 1 1 calc R . . C34 C 0.54298(4) 0.49437(2) 0.27728(3) 0.03880(15) Uani 1 1 d . . . C35 C 0.63820(4) 0.52714(2) 0.27712(3) 0.03663(15) Uani 1 1 d . . . C36 C 0.66718(4) 0.56283(2) 0.33231(3) 0.03480(14) Uani 1 1 d . . . H36 H 0.7328 0.5840 0.3334 0.042 Uiso 1 1 calc R F . C37 C 0.60448(4) 0.56886(2) 0.38581(3) 0.03370(14) Uani 1 1 d . . . C38 C 0.50900(4) 0.53730(2) 0.38230(3) 0.03686(15) Uani 1 1 d . . . H38 H 0.4635 0.5415 0.4175 0.044 Uiso 1 1 calc R F . C39 C 0.47759(4) 0.49969(2) 0.32903(3) 0.03890(15) Uani 1 1 d . . . C40 C 0.37263(4) 0.46603(3) 0.32863(3) 0.04894(17) Uani 1 1 d . . . H40A H 0.3599 0.4474 0.3719 0.059 Uiso 1 1 calc R F . H40B H 0.3727 0.4287 0.2975 0.059 Uiso 1 1 calc R . . C41 C 0.64211(4) 0.60643(3) 0.44608(3) 0.03780(15) Uani 1 1 d . . . C42 C 0.68452(5) 0.67480(3) 0.42781(3) 0.05323(19) Uani 1 1 d . . . H42A H 0.7431 0.6692 0.3991 0.080 Uiso 1 1 calc R . . H42B H 0.7074 0.6984 0.4669 0.080 Uiso 1 1 calc R . . H42C H 0.6302 0.7006 0.4057 0.080 Uiso 1 1 calc R . . C43 C 0.72740(5) 0.56527(3) 0.47988(3) 0.05292(19) Uani 1 1 d . . . H43A H 0.6996 0.5218 0.4921 0.079 Uiso 1 1 calc R . . H43B H 0.7521 0.5888 0.5186 0.079 Uiso 1 1 calc R . . H43C H 0.7849 0.5589 0.4505 0.079 Uiso 1 1 calc R . . C44 C 0.55600(5) 0.61726(3) 0.49446(3) 0.0541(2) Uani 1 1 d . . . H44A H 0.4996 0.6425 0.4739 0.081 Uiso 1 1 calc R . . H44B H 0.5833 0.6421 0.5317 0.081 Uiso 1 1 calc R . . H44C H 0.5299 0.5741 0.5088 0.081 Uiso 1 1 calc R . . N1A N 0.57533(5) 0.38973(3) 0.10975(3) 0.04657(17) Uani 0.68 1 d PD A -1 H1A1 H 0.5115 0.3914 0.0906 0.070 Uiso 0.34 1 calc PR A -1 H1A2 H 0.6218 0.4104 0.0842 0.070 Uiso 0.34 1 calc PR A -1 H1A3 H 0.5737 0.4106 0.1486 0.070 Uiso 0.68 1 calc PR A -1 C1A C 0.60598(7) 0.31969(4) 0.11920(5) 0.0521(3) Uani 0.68 1 d PD A -1 H1A4 H 0.6796 0.3180 0.1331 0.063 Uiso 0.68 1 calc PR A -1 H1A5 H 0.5993 0.2959 0.0775 0.063 Uiso 0.68 1 calc PR A -1 C2A C 0.54235(7) 0.28464(4) 0.16809(5) 0.0508(2) Uani 0.68 1 d PD A -1 H2A1 H 0.4707 0.2799 0.1511 0.061 Uiso 0.68 1 calc PR A -1 H2A2 H 0.5401 0.3119 0.2077 0.061 Uiso 0.68 1 calc PR A -1 C3A C 0.58599(9) 0.21484(4) 0.18511(4) 0.0593(3) Uani 0.68 1 d PD A -1 H3A1 H 0.5848 0.1868 0.1459 0.071 Uiso 0.68 1 calc PR A -1 H3A2 H 0.6588 0.2194 0.1999 0.071 Uiso 0.68 1 calc PR A -1 C4A C 0.52542(8) 0.18094(5) 0.23663(5) 0.0599(3) Uani 0.68 1 d PD A -1 H4A1 H 0.5293 0.2074 0.2763 0.090 Uiso 0.68 1 calc PR A -1 H4A2 H 0.5544 0.1366 0.2449 0.090 Uiso 0.68 1 calc PR A -1 H4A3 H 0.4531 0.1767 0.2224 0.090 Uiso 0.68 1 calc PR A -1 N1B N 0.54412(12) 0.38528(7) 0.10997(8) 0.04657(17) Uani 0.32 1 d PD B -2 H1B1 H 0.5444 0.4113 0.1459 0.070 Uiso 0.32 1 calc PR B -2 H1B2 H 0.4907 0.3974 0.0834 0.070 Uiso 0.16 1 calc PR B -2 H1B3 H 0.6048 0.3905 0.0891 0.070 Uiso 0.16 1 calc PR B -2 C1B C 0.53169(16) 0.31346(9) 0.12910(10) 0.0521(3) Uani 0.32 1 d PD B -2 H1B4 H 0.5135 0.2874 0.0900 0.063 Uiso 0.32 1 calc PR B -2 H1B5 H 0.4730 0.3101 0.1588 0.063 Uiso 0.32 1 calc PR B -2 C2B C 0.62611(14) 0.28192(9) 0.16146(10) 0.0508(2) Uani 0.32 1 d PD B -2 H2B1 H 0.6389 0.3029 0.2041 0.061 Uiso 0.32 1 calc PR B -2 H2B2 H 0.6876 0.2896 0.1348 0.061 Uiso 0.32 1 calc PR B -2 C3B C 0.60935(19) 0.20707(9) 0.17006(9) 0.0593(3) Uani 0.32 1 d PD B -2 H3B1 H 0.5735 0.1890 0.1313 0.071 Uiso 0.32 1 calc PR B -2 H3B2 H 0.6773 0.1846 0.1744 0.071 Uiso 0.32 1 calc PR B -2 C4B C 0.54685(17) 0.19228(10) 0.22814(10) 0.0599(3) Uani 0.32 1 d PD B -2 H4B1 H 0.5790 0.2135 0.2661 0.090 Uiso 0.32 1 calc PR B -2 H4B2 H 0.5440 0.1440 0.2348 0.090 Uiso 0.32 1 calc PR B -2 H4B3 H 0.4766 0.2096 0.2216 0.090 Uiso 0.32 1 calc PR B -2 N1C N 0.36880(4) 0.42071(3) 0.05451(3) 0.05795(18) Uani 0.86 1 d PD C -3 H1C1 H 0.3848 0.4305 0.0131 0.087 Uiso 0.86 1 calc PR C -3 H1C2 H 0.4266 0.4065 0.0761 0.087 Uiso 0.86 1 calc PR C -3 H1C3 H 0.3437 0.4577 0.0740 0.087 Uiso 0.86 1 calc PR C -3 C1C C 0.28926(6) 0.36736(4) 0.05499(4) 0.0598(2) Uani 0.86 1 d PD C -3 H1C4 H 0.2686 0.3600 0.1001 0.072 Uiso 0.86 1 calc PR C -3 H1C5 H 0.3214 0.3256 0.0398 0.072 Uiso 0.86 1 calc PR C -3 C2C C 0.19351(6) 0.37994(4) 0.01499(4) 0.0551(2) Uani 0.86 1 d PD C -3 H2C1 H 0.2140 0.3894 -0.0298 0.066 Uiso 0.86 1 calc PR C -3 H2C2 H 0.1589 0.4202 0.0316 0.066 Uiso 0.86 1 calc PR C -3 C3C C 0.11676(6) 0.32335(4) 0.01391(5) 0.0690(3) Uani 0.86 1 d PD C -3 H3C1 H 0.0902 0.3166 0.0579 0.083 Uiso 0.86 1 calc PR C -3 H3C2 H 0.1522 0.2819 0.0009 0.083 Uiso 0.86 1 calc PR C -3 C4C C 0.02562(7) 0.33678(6) -0.03276(5) 0.1006(4) Uani 0.86 1 d PD C -3 H4C1 H -0.0066 0.3793 -0.0219 0.151 Uiso 0.86 1 calc PR C -3 H4C2 H -0.0253 0.3009 -0.0292 0.151 Uiso 0.86 1 calc PR C -3 H4C3 H 0.0507 0.3386 -0.0770 0.151 Uiso 0.86 1 calc PR C -3 N1K N 0.3429(3) 0.42449(17) 0.04161(18) 0.05795(18) Uani 0.14 1 d PD D -4 H1K1 H 0.3160 0.4653 0.0501 0.087 Uiso 0.14 1 calc PR D -4 H1K2 H 0.3330 0.4148 -0.0009 0.087 Uiso 0.14 1 calc PR D -4 H1K3 H 0.4118 0.4245 0.0513 0.087 Uiso 0.14 1 calc PR D -4 C1K C 0.2906(3) 0.3737(2) 0.0813(2) 0.0598(2) Uani 0.14 1 d PD D -4 H1K4 H 0.2953 0.3855 0.1276 0.072 Uiso 0.14 1 calc PR D -4 H1K5 H 0.3224 0.3293 0.0752 0.072 Uiso 0.14 1 calc PR D -4 C2K C 0.1791(3) 0.3735(2) 0.05786(18) 0.0551(2) Uani 0.14 1 d PD D -4 H2K1 H 0.1387 0.3448 0.0869 0.066 Uiso 0.14 1 calc PR D -4 H2K2 H 0.1515 0.4193 0.0613 0.066 Uiso 0.14 1 calc PR D -4 C3K C 0.1620(3) 0.3495(3) -0.0106(2) 0.0690(3) Uani 0.14 1 d PD D -4 H3K1 H 0.2019 0.3082 -0.0175 0.083 Uiso 0.14 1 calc PR D -4 H3K2 H 0.1869 0.3836 -0.0410 0.083 Uiso 0.14 1 calc PR D -4 C4K C 0.0463(3) 0.3361(4) -0.0237(3) 0.1006(4) Uani 0.14 1 d PD D -4 H4K1 H 0.0139 0.3214 0.0162 0.151 Uiso 0.14 1 calc PR D -4 H4K2 H 0.0386 0.3013 -0.0565 0.151 Uiso 0.14 1 calc PR D -4 H4K3 H 0.0127 0.3770 -0.0391 0.151 Uiso 0.14 1 calc PR D -4 N1D N 0.26753(6) 0.91890(5) 0.46865(3) 0.0796(3) Uani 0.80 1 d PD E -5 H1D1 H 0.2488 0.8766 0.4790 0.119 Uiso 0.80 1 calc PR E -5 H1D2 H 0.2914 0.9402 0.5047 0.119 Uiso 0.40 1 calc PR E -5 H1D3 H 0.3182 0.9176 0.4389 0.119 Uiso 0.40 1 calc PR E -5 C1D C 0.17990(8) 0.95382(5) 0.44261(5) 0.0827(3) Uani 0.80 1 d PD E -5 H1D4 H 0.2028 0.9981 0.4276 0.099 Uiso 0.80 1 calc PR E -5 H1D5 H 0.1299 0.9610 0.4775 0.099 Uiso 0.80 1 calc PR E -5 C2D C 0.12551(6) 0.91865(4) 0.38757(4) 0.0625(2) Uani 0.80 1 d PD E -5 H2D1 H 0.0943 0.8771 0.4040 0.075 Uiso 0.80 1 calc PR E -5 H2D2 H 0.1772 0.9061 0.3552 0.075 Uiso 0.80 1 calc PR E -5 C3D C 0.04174(7) 0.95997(5) 0.35488(5) 0.0765(3) Uani 0.80 1 d PD E -5 H3D1 H -0.0079 0.9742 0.3879 0.092 Uiso 0.80 1 calc PR E -5 H3D2 H 0.0738 1.0006 0.3372 0.092 Uiso 0.80 1 calc PR E -5 C4D C -0.01674(8) 0.92581(6) 0.30184(6) 0.1035(3) Uani 0.80 1 d PD E -5 H4D1 H 0.0308 0.9138 0.2675 0.155 Uiso 0.80 1 calc PR E -5 H4D2 H -0.0703 0.9557 0.2845 0.155 Uiso 0.80 1 calc PR E -5 H4D3 H -0.0492 0.8855 0.3186 0.155 Uiso 0.80 1 calc PR E -5 N1L N 0.2310(2) 0.91345(17) 0.47120(14) 0.0796(3) Uani 0.20 1 d PD F -6 H1L1 H 0.1877 0.8815 0.4862 0.119 Uiso 0.20 1 calc PR F -6 H1L2 H 0.2606 0.9356 0.5051 0.119 Uiso 0.10 1 calc PR F -6 H1L3 H 0.2811 0.8941 0.4474 0.119 Uiso 0.10 1 calc PR F -6 C1L C 0.1729(3) 0.95991(18) 0.43128(17) 0.0827(3) Uani 0.20 1 d PD F -6 H1L4 H 0.2198 0.9921 0.4106 0.099 Uiso 0.20 1 calc PR F -6 H1L5 H 0.1225 0.9848 0.4573 0.099 Uiso 0.20 1 calc PR F -6 C2L C 0.1180(2) 0.91766(17) 0.38112(16) 0.0625(2) Uani 0.20 1 d PD F -6 H2L1 H 0.1006 0.8733 0.3986 0.075 Uiso 0.20 1 calc PR F -6 H2L2 H 0.1608 0.9119 0.3425 0.075 Uiso 0.20 1 calc PR F -6 C3L C 0.0202(3) 0.95773(17) 0.36513(18) 0.0765(3) Uani 0.20 1 d PD F -6 H3L1 H -0.0311 0.9533 0.3997 0.092 Uiso 0.20 1 calc PR F -6 H3L2 H 0.0365 1.0054 0.3591 0.092 Uiso 0.20 1 calc PR F -6 C4L C -0.01998(2) 0.926745(14) 0.302689(16) 0.1035(3) Uani 0.20 1 d PD F -6 H4L1 H 0.0144 0.8839 0.2959 0.155 Uiso 0.20 1 calc PR F -6 H4L2 H -0.0055 0.9566 0.2666 0.155 Uiso 0.20 1 calc PR F -6 H4L3 H -0.0947 0.9197 0.3053 0.155 Uiso 0.20 1 calc PR F -6 C1 C 0.26587(3) 0.531954(15) 0.245399(18) 0.04016(17) Uani 0.74 1 d PR F -1 C2 C 0.18828(3) 0.576695(15) 0.228009(18) 0.0389(2) Uani 0.74 1 d PR F -1 C3 C 0.12746(3) 0.605185(15) 0.275099(18) 0.0447(2) Uani 0.74 1 d PR F -1 H3A H 0.0744 0.6358 0.2632 0.054 Uiso 0.74 1 calc PR F -1 C4 C 0.14423(3) 0.588935(15) 0.339569(17) 0.0519(2) Uani 0.74 1 d PRD F -1 C5 C 0.22182(3) 0.544205(15) 0.356949(18) 0.0500(2) Uani 0.74 1 d PR F -1 H5 H 0.2333 0.5331 0.4010 0.060 Uiso 0.74 1 calc PR F -1 C6 C 0.28264(3) 0.515714(15) 0.309869(18) 0.0410(2) Uani 0.74 1 d PR F -1 C8 C 0.07678(13) 0.62261(11) 0.39385(9) 0.0873(3) Uani 0.37 1 d PD G -7 C9 C 0.07225(16) 0.56782(11) 0.44645(9) 0.0742(3) Uani 0.37 1 d PD G -7 H9A H 0.1402 0.5635 0.4677 0.111 Uiso 0.37 1 calc PR G -7 H9B H 0.0530 0.5253 0.4264 0.111 Uiso 0.37 1 calc PR G -7 H9C H 0.0207 0.5800 0.4784 0.111 Uiso 0.37 1 calc PR G -7 C10 C -0.04022(14) 0.61204(12) 0.36226(10) 0.0833(6) Uani 0.37 1 d PD G -7 H10A H -0.0916 0.6300 0.3917 0.125 Uiso 0.37 1 calc PR G -7 H10B H -0.0530 0.5645 0.3555 0.125 Uiso 0.37 1 calc PR G -7 H10C H -0.0455 0.6354 0.3209 0.125 Uiso 0.37 1 calc PR G -7 C11 C 0.12911(19) 0.67763(9) 0.41127(9) 0.0786(5) Uani 0.37 1 d PD G -7 H11A H 0.0913 0.7012 0.4447 0.118 Uiso 0.37 1 calc PR G -7 H11B H 0.1365 0.7067 0.3737 0.118 Uiso 0.37 1 calc PR G -7 H11C H 0.1977 0.6651 0.4281 0.118 Uiso 0.37 1 calc PR G -7 C8E C 0.08220(15) 0.62040(13) 0.39346(10) 0.0873(3) Uani 0.37 1 d PD H -8 C9E C 0.04622(16) 0.58074(11) 0.45117(9) 0.0742(3) Uani 0.37 1 d PD H -8 H9E1 H 0.0053 0.6095 0.4790 0.111 Uiso 0.37 1 calc PR H -8 H9E2 H 0.1065 0.5639 0.4755 0.111 Uiso 0.37 1 calc PR H -8 H9E3 H 0.0037 0.5432 0.4363 0.111 Uiso 0.37 1 calc PR H -8 C10E C -0.01156(15) 0.66855(12) 0.37220(10) 0.0833(6) Uani 0.37 1 d PD H -8 H10D H -0.0458 0.6853 0.4107 0.125 Uiso 0.37 1 calc PR H -8 H10E H -0.0614 0.6437 0.3455 0.125 Uiso 0.37 1 calc PR H -8 H10F H 0.0153 0.7061 0.3475 0.125 Uiso 0.37 1 calc PR H -8 C11E C 0.15931(6) 0.68291(3) 0.43593(4) 0.0786(5) Uani 0.37 1 d PD H -8 H11D H 0.1581 0.7245 0.4113 0.118 Uiso 0.37 1 calc PR H -8 H11E H 0.2307 0.6672 0.4407 0.118 Uiso 0.37 1 calc PR H -8 H11F H 0.1306 0.6906 0.4786 0.118 Uiso 0.37 1 calc PR H -8 C1F C 0.27711(7) 0.52098(5) 0.23710(5) 0.04016(17) Uani 0.26 1 d PR F -2 C2F C 0.19523(7) 0.56234(5) 0.21945(4) 0.0363(6) Uani 0.26 1 d PR F -2 C3F C 0.12716(8) 0.58456(5) 0.26576(4) 0.0349(6) Uani 0.26 1 d PR F -2 H3F H 0.0712 0.6128 0.2537 0.042 Uiso 0.26 1 calc PR H -2 C4F C 0.14097(7) 0.56544(4) 0.32972(5) 0.0515(7) Uani 0.26 1 d PRD F -2 C5F C 0.22285(6) 0.52408(4) 0.34737(5) 0.0431(6) Uani 0.26 1 d PR F -2 H5F H 0.2323 0.5110 0.3911 0.052 Uiso 0.26 1 calc PR H -2 C6F C 0.29092(6) 0.50186(4) 0.30106(5) 0.0351(6) Uani 0.26 1 d PR F -2 C8F C 0.06043(19) 0.59503(15) 0.37690(13) 0.0873(3) Uani 0.26 1 d PD F -2 C9F C 0.0670(2) 0.55943(16) 0.44229(13) 0.0742(3) Uani 0.26 1 d PD F -2 H9F1 H 0.0534 0.5119 0.4362 0.111 Uiso 0.26 1 calc PR F -2 H9F2 H 0.0156 0.5783 0.4712 0.111 Uiso 0.26 1 calc PR F -2 H9F3 H 0.1363 0.5654 0.4613 0.111 Uiso 0.26 1 calc PR F -2 C10F C -0.04849(18) 0.57637(15) 0.34990(14) 0.0698(9) Uani 0.26 1 d PD F -2 H10D' H -0.1012 0.5930 0.3791 0.105 Uiso 0.26 1 calc PR F -2 H10E' H -0.0541 0.5279 0.3463 0.105 Uiso 0.26 1 calc PR F -2 H10F' H -0.0588 0.5965 0.3072 0.105 Uiso 0.26 1 calc PR F -2 C11F C 0.0697(3) 0.66944(13) 0.38447(12) 0.0786(5) Uani 0.26 1 d PD F -2 H11D' H 0.0326 0.6836 0.4228 0.118 Uiso 0.26 1 calc PR F -2 H11E' H 0.0398 0.6914 0.3463 0.118 Uiso 0.26 1 calc PR F -2 H11F' H 0.1428 0.6817 0.3892 0.118 Uiso 0.26 1 calc PR F -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 O1 0.0649(2) 0.03706(19) 0.0559(2) 0.00065(18) -0.0251(2) 0.00001(18) O2 0.0603(2) 0.03564(18) 0.0462(2) -0.00565(17) -0.01815(19) 0.00738(18) O3 0.0656(3) 0.0430(2) 0.0527(2) -0.01355(18) -0.0199(2) 0.01391(19) O4 0.0608(2) 0.03637(18) 0.0546(2) -0.01071(18) -0.0215(2) 0.00444(18) C7 0.0438(3) 0.0382(3) 0.0570(3) 0.0117(3) -0.0215(3) -0.0092(2) C12 0.0479(3) 0.0364(3) 0.0332(3) -0.0028(2) -0.0181(2) 0.0033(2) C13 0.0392(3) 0.0364(2) 0.0389(3) 0.0036(2) -0.0161(2) -0.0045(2) C14 0.0338(3) 0.0394(3) 0.0417(3) 0.0044(2) -0.0064(2) -0.0021(2) C15 0.0366(3) 0.0355(2) 0.0391(3) 0.0014(2) -0.0043(2) -0.0022(2) C16 0.0376(3) 0.0377(3) 0.0390(3) 0.0034(2) -0.0054(2) -0.0027(2) C17 0.0384(3) 0.0429(3) 0.0304(3) 0.0006(2) -0.0068(2) 0.0048(2) C18 0.0509(3) 0.0532(3) 0.0326(3) 0.0026(3) -0.0041(3) 0.0121(3) C19 0.0474(3) 0.0335(3) 0.0723(4) 0.0010(3) 0.0118(3) 0.0006(3) C20 0.1055(6) 0.0559(4) 0.0804(5) -0.0227(4) 0.0240(4) -0.0047(4) C21 0.0554(4) 0.0479(3) 0.1342(7) 0.0175(4) 0.0084(5) 0.0114(3) C22 0.0708(4) 0.0346(3) 0.0994(5) 0.0003(3) 0.0233(4) -0.0049(3) C23 0.0456(3) 0.0460(3) 0.0341(3) -0.0057(2) -0.0037(3) 0.0142(2) C24 0.0398(3) 0.0504(3) 0.0307(3) 0.0009(2) 0.0023(2) 0.0119(2) C25 0.0408(3) 0.0446(3) 0.0404(3) 0.0088(2) 0.0038(3) 0.0096(2) C26 0.0341(3) 0.0499(3) 0.0390(3) 0.0053(3) 0.0028(2) 0.0083(2) C27 0.0354(3) 0.0495(3) 0.0352(3) 0.0027(2) -0.0009(2) 0.0102(2) C28 0.0421(3) 0.0423(3) 0.0346(3) -0.0038(2) 0.0009(2) 0.0137(2) C29 0.0441(3) 0.0392(3) 0.0405(3) -0.0061(2) -0.0083(3) 0.0132(2) C30 0.0403(3) 0.0480(3) 0.0504(3) 0.0104(3) -0.0009(3) 0.0021(3) C31 0.0792(5) 0.0662(4) 0.0621(4) -0.0087(4) 0.0073(4) -0.0152(4) C32 0.0696(4) 0.0549(4) 0.0674(4) 0.0126(3) 0.0049(4) -0.0043(3) C33 0.0532(4) 0.0636(4) 0.1270(7) 0.0165(4) -0.0297(4) -0.0047(3) C34 0.0478(3) 0.0252(2) 0.0427(3) -0.0012(2) -0.0167(3) 0.0053(2) C35 0.0433(3) 0.0272(2) 0.0389(3) 0.0012(2) -0.0099(2) 0.0108(2) C36 0.0333(3) 0.0301(2) 0.0407(3) 0.0012(2) -0.0077(2) 0.0031(2) C37 0.0371(3) 0.0257(2) 0.0381(3) 0.0011(2) -0.0065(2) 0.0044(2) C38 0.0376(3) 0.0309(2) 0.0418(3) 0.0058(2) -0.0053(2) 0.0041(2) C39 0.0408(3) 0.0268(2) 0.0484(3) 0.0076(2) -0.0162(2) 0.0007(2) C40 0.0484(3) 0.0395(3) 0.0581(3) 0.0171(3) -0.0199(3) -0.0107(2) C41 0.0420(3) 0.0336(2) 0.0375(3) -0.0028(2) -0.0059(2) 0.0034(2) C42 0.0657(4) 0.0383(3) 0.0553(4) -0.0064(3) -0.0081(3) -0.0074(3) C43 0.0610(4) 0.0524(3) 0.0445(3) -0.0069(3) -0.0192(3) 0.0117(3) C44 0.0558(4) 0.0602(4) 0.0463(3) -0.0132(3) -0.0009(3) 0.0024(3) N1A 0.0517(4) 0.0382(2) 0.0489(3) -0.0093(2) -0.0197(3) -0.0033(3) C1A 0.0572(5) 0.0494(4) 0.0494(4) -0.0010(4) -0.0040(5) -0.0009(5) C2A 0.0462(4) 0.0506(4) 0.0553(5) -0.0029(4) -0.0036(4) -0.0081(4) C3A 0.0889(6) 0.0486(4) 0.0409(4) -0.0040(3) 0.0110(4) -0.0064(4) C4A 0.0642(5) 0.0590(4) 0.0566(4) 0.0022(4) 0.0040(4) -0.0130(4) N1B 0.0517(4) 0.0382(2) 0.0489(3) -0.0093(2) -0.0197(3) -0.0033(3) C1B 0.0572(5) 0.0494(4) 0.0494(4) -0.0010(4) -0.0040(5) -0.0009(5) C2B 0.0462(4) 0.0506(4) 0.0553(5) -0.0029(4) -0.0036(4) -0.0081(4) C3B 0.0889(6) 0.0486(4) 0.0409(4) -0.0040(3) 0.0110(4) -0.0064(4) C4B 0.0642(5) 0.0590(4) 0.0566(4) 0.0022(4) 0.0040(4) -0.0130(4) N1C 0.0468(3) 0.0588(3) 0.0675(3) -0.0253(3) -0.0159(3) 0.0053(3) C1C 0.0553(4) 0.0651(4) 0.0588(5) -0.0083(4) -0.0032(4) 0.0011(3) C2C 0.0538(4) 0.0542(4) 0.0574(5) -0.0017(4) 0.0005(4) 0.0081(3) C3C 0.0532(5) 0.0665(5) 0.0869(6) 0.0069(5) -0.0111(4) -0.0013(4) C4C 0.0719(6) 0.1233(7) 0.1051(7) -0.0085(6) -0.0358(5) 0.0109(5) N1K 0.0468(3) 0.0588(3) 0.0675(3) -0.0253(3) -0.0159(3) 0.0053(3) C1K 0.0553(4) 0.0651(4) 0.0588(5) -0.0083(4) -0.0032(4) 0.0011(3) C2K 0.0538(4) 0.0542(4) 0.0574(5) -0.0017(4) 0.0005(4) 0.0081(3) C3K 0.0532(5) 0.0665(5) 0.0869(6) 0.0069(5) -0.0111(4) -0.0013(4) C4K 0.0719(6) 0.1233(7) 0.1051(7) -0.0085(6) -0.0358(5) 0.0109(5) N1D 0.0636(5) 0.1250(6) 0.0493(3) 0.0043(4) -0.0170(4) -0.0128(4) C1D 0.1070(6) 0.0834(5) 0.0572(5) -0.0035(4) -0.0077(5) -0.0242(5) C2D 0.0517(4) 0.0757(4) 0.0598(4) -0.0141(4) -0.0056(3) -0.0111(3) C3D 0.0621(5) 0.0593(4) 0.1094(6) -0.0050(4) 0.0324(5) 0.0057(4) C4D 0.0868(5) 0.1035(6) 0.1185(7) -0.0078(6) -0.0426(5) 0.0284(5) N1L 0.0636(5) 0.1250(6) 0.0493(3) 0.0043(4) -0.0170(4) -0.0128(4) C1L 0.1070(6) 0.0834(5) 0.0572(5) -0.0035(4) -0.0077(5) -0.0242(5) C2L 0.0517(4) 0.0757(4) 0.0598(4) -0.0141(4) -0.0056(3) -0.0111(3) C3L 0.0621(5) 0.0593(4) 0.1094(6) -0.0050(4) 0.0324(5) 0.0057(4) C4L 0.0868(5) 0.1035(6) 0.1185(7) -0.0078(6) -0.0426(5) 0.0284(5) C1 0.0387(3) 0.0277(3) 0.0533(3) 0.0056(3) -0.0169(3) -0.0088(2) C2 0.0323(3) 0.0260(3) 0.0575(4) 0.0123(3) -0.0180(3) -0.0105(3) C3 0.0286(4) 0.0411(4) 0.0641(5) 0.0178(4) -0.0080(4) -0.0083(3) C4 0.0282(4) 0.0716(5) 0.0558(5) 0.0276(4) -0.0014(4) 0.0043(4) C5 0.0299(4) 0.0641(4) 0.0558(4) 0.0296(4) -0.0053(4) -0.0045(3) C6 0.0340(4) 0.0356(3) 0.0526(4) 0.0174(3) -0.0142(3) -0.0112(3) C8 0.0431(4) 0.1578(8) 0.0614(5) 0.0458(5) 0.0099(4) 0.0333(5) C9 0.0655(6) 0.1055(7) 0.0523(4) 0.0041(5) 0.0178(4) -0.0080(5) C10 0.0498(7) 0.1377(15) 0.0622(8) -0.0018(10) 0.0012(6) 0.0321(9) C11 0.1321(10) 0.0687(6) 0.0358(8) -0.0148(6) 0.0239(6) 0.0020(7) C8E 0.0431(4) 0.1578(8) 0.0614(5) 0.0458(5) 0.0099(4) 0.0333(5) C9E 0.0655(6) 0.1055(7) 0.0523(4) 0.0041(5) 0.0178(4) -0.0080(5) C10E 0.0498(7) 0.1377(15) 0.0622(8) -0.0018(10) 0.0012(6) 0.0321(9) C11E 0.1321(10) 0.0687(6) 0.0358(8) -0.0148(6) 0.0239(6) 0.0020(7) C1F 0.0387(3) 0.0277(3) 0.0533(3) 0.0056(3) -0.0169(3) -0.0088(2) C2F 0.0428(11) 0.0255(8) 0.0403(11) -0.0066(8) -0.0054(10) -0.0106(8) C3F 0.0327(10) 0.0152(7) 0.0564(12) 0.0150(8) -0.0063(9) 0.0049(7) C4F 0.0492(12) 0.0376(10) 0.0680(15) 0.0105(10) 0.0058(12) -0.0261(9) C5F 0.0459(12) 0.0362(10) 0.0467(12) 0.0028(10) -0.0150(10) -0.0115(9) C6F 0.0327(10) 0.0145(7) 0.0581(13) -0.0044(8) -0.0014(10) -0.0011(7) C8F 0.0431(4) 0.1578(8) 0.0614(5) 0.0458(5) 0.0099(4) 0.0333(5) C9F 0.0655(6) 0.1055(7) 0.0523(4) 0.0041(5) 0.0178(4) -0.0080(5) C10F 0.0520(15) 0.0902(18) 0.0677(16) -0.0202(15) 0.0186(13) 0.0052(14) C11F 0.1321(10) 0.0687(6) 0.0358(8) -0.0148(6) 0.0239(6) 0.0020(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1F 1.1566 . ? O1 C1 1.4528 . ? O2 C12 1.3581(6) . ? O3 C23 1.3644(7) . ? O4 C34 1.3826(7) . ? C7 C2F 1.4869(12) . ? C7 C13 1.5133(8) . ? C7 C2 1.5462 . ? C12 C17 1.3963(8) . ? C12 C13 1.4071(8) . ? C13 C14 1.3884(7) . ? C14 C15 1.3934(7) . ? C15 C16 1.3877(8) . ? C15 C19 1.5372(8) . ? C16 C17 1.3947(7) . ? C17 C18 1.5213(8) . ? C18 C24 1.5207(8) . ? C19 C22 1.5263(9) . ? C19 C20 1.5347(10) . ? C19 C21 1.5356(9) . ? C23 C28 1.3996(8) . ? C23 C24 1.4031(8) . ? C24 C25 1.3883(8) . ? C25 C26 1.3919(8) . ? C26 C27 1.3895(8) . ? C26 C30 1.5307(8) . ? C27 C28 1.3884(8) . ? C28 C29 1.5180(8) . ? C29 C35 1.5190(8) . ? C30 C33 1.5276(9) . ? C30 C32 1.5300(9) . ? C30 C31 1.5365(10) . ? C34 C39 1.3844(8) . ? C34 C35 1.3972(8) . ? C35 C36 1.3963(7) . ? C36 C37 1.3931(8) . ? C37 C38 1.3894(7) . ? C37 C41 1.5321(7) . ? C38 C39 1.3931(8) . ? C39 C40 1.5171(8) . ? C40 C6F 1.3928(11) . ? C40 C6 1.5768 . ? C41 C42 1.5297(8) . ? C41 C44 1.5300(9) . ? C41 C43 1.5375(8) . ? N1A C1A 1.4742(11) . ? C1A C2A 1.4952(13) . ? C2A C3A 1.5501(13) . ? C3A C4A 1.5014(14) . ? N1B C1B 1.506(2) . ? C1B C2B 1.521(3) . ? C2B C3B 1.531(3) . ? C3B C4B 1.494(3) . ? N1C C1C 1.4862(10) . ? C1C C2C 1.4993(11) . ? C2C C3C 1.5095(11) . ? C3C C4C 1.5352(13) . ? N1K C1K 1.484(5) . ? C1K C2K 1.514(5) . ? C2K C3K 1.512(6) . ? C3K C4K 1.540(6) . ? N1D C1D 1.4304(13) . ? C1D C2D 1.5060(13) . ? C2D C3D 1.5153(13) . ? C3D C4D 1.4909(15) . ? N1L C1L 1.448(5) . ? C1L C2L 1.510(5) . ? C2L C3L 1.531(5) . ? C3L C4L 1.520(4) . ? C1 C6 1.3900 . ? C1 C2 1.3901 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3899 . ? C5 C6 1.3899 . ? C8 C11 1.342(3) . ? C8 C9 1.552(3) . ? C8 C10 1.652(3) . ? C8E C9E 1.519(3) . ? C8E C10E 1.607(3) . ? C8E C11E 1.821(2) . ? C1F C6F 1.3899 . ? C1F C2F 1.3901 . ? C2F C3F 1.3899 . ? C3F C4F 1.3899 . ? C4F C5F 1.3900 . ? C4F C8F 1.561(3) . ? C5F C6F 1.3899 . ? C8F C11F 1.508(4) . ? C8F C9F 1.535(4) . ? C8F C10F 1.552(4) . ? 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 C1F O1 C1 4.97(5) . . ? C2F C7 C13 116.88(5) . . ? C2F C7 C2 13.1 . . ? C13 C7 C2 111.62(4) . . ? O2 C12 C17 120.97(5) . . ? O2 C12 C13 119.80(5) . . ? C17 C12 C13 119.20(5) . . ? C14 C13 C12 119.10(5) . . ? C14 C13 C7 120.40(5) . . ? C12 C13 C7 120.49(5) . . ? C13 C14 C15 122.93(5) . . ? C16 C15 C14 116.58(5) . . ? C16 C15 C19 123.05(5) . . ? C14 C15 C19 120.35(5) . . ? C15 C16 C17 122.62(5) . . ? C16 C17 C12 119.51(5) . . ? C16 C17 C18 120.01(5) . . ? C12 C17 C18 120.48(5) . . ? C24 C18 C17 114.61(5) . . ? C22 C19 C20 108.01(6) . . ? C22 C19 C21 107.97(6) . . ? C20 C19 C21 109.99(6) . . ? C22 C19 C15 111.90(5) . . ? C20 C19 C15 108.89(5) . . ? C21 C19 C15 110.04(5) . . ? O3 C23 C28 118.93(5) . . ? O3 C23 C24 121.06(5) . . ? C28 C23 C24 120.00(5) . . ? C25 C24 C23 118.59(5) . . ? C25 C24 C18 120.09(5) . . ? C23 C24 C18 121.31(5) . . ? C24 C25 C26 123.08(5) . . ? C27 C26 C25 116.37(5) . . ? C27 C26 C30 121.59(5) . . ? C25 C26 C30 121.88(5) . . ? C28 C27 C26 123.15(5) . . ? C27 C28 C23 118.64(5) . . ? C27 C28 C29 119.59(5) . . ? C23 C28 C29 121.53(5) . . ? C28 C29 C35 110.94(4) . . ? C33 C30 C32 107.22(6) . . ? C33 C30 C26 111.79(5) . . ? C32 C30 C26 112.14(5) . . ? C33 C30 C31 109.64(6) . . ? C32 C30 C31 107.99(5) . . ? C26 C30 C31 107.99(5) . . ? O4 C34 C39 119.70(5) . . ? O4 C34 C35 119.11(5) . . ? C39 C34 C35 121.19(5) . . ? C36 C35 C34 117.57(5) . . ? C36 C35 C29 120.31(5) . . ? C34 C35 C29 122.04(5) . . ? C37 C36 C35 123.16(5) . . ? C38 C37 C36 116.73(5) . . ? C38 C37 C41 122.39(5) . . ? C36 C37 C41 120.83(5) . . ? C37 C38 C39 122.31(5) . . ? C34 C39 C38 118.96(5) . . ? C34 C39 C40 121.47(5) . . ? C38 C39 C40 119.57(5) . . ? C6F C40 C39 116.38(6) . . ? C6F C40 C6 11.6 . . ? C39 C40 C6 112.08(4) . . ? C42 C41 C44 107.72(5) . . ? C42 C41 C37 110.49(5) . . ? C44 C41 C37 112.44(5) . . ? C42 C41 C43 109.77(5) . . ? C44 C41 C43 107.62(5) . . ? C37 C41 C43 108.74(4) . . ? N1A C1A C2A 112.93(8) . . ? C1A C2A C3A 112.20(8) . . ? C4A C3A C2A 112.32(8) . . ? N1B C1B C2B 115.25(15) . . ? C1B C2B C3B 110.27(16) . . ? C4B C3B C2B 111.69(17) . . ? N1C C1C C2C 116.08(6) . . ? C1C C2C C3C 114.68(7) . . ? C2C C3C C4C 111.97(8) . . ? N1K C1K C2K 105.4(3) . . ? C3K C2K C1K 115.1(3) . . ? C2K C3K C4K 110.2(4) . . ? N1D C1D C2D 114.30(8) . . ? C1D C2D C3D 113.71(8) . . ? C4D C3D C2D 115.25(8) . . ? N1L C1L C2L 105.3(3) . . ? C1L C2L C3L 103.3(3) . . ? C4L C3L C2L 103.7(2) . . ? C6 C1 C2 120.0 . . ? C6 C1 O1 118.7 . . ? C2 C1 O1 121.3 . . ? C3 C2 C1 120.0 . . ? C3 C2 C7 121.4 . . ? C1 C2 C7 118.7 . . ? C2 C3 C4 120.0 . . ? C5 C4 C3 120.0 . . ? C4 C5 C6 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 C40 120.9 . . ? C1 C6 C40 119.1 . . ? C11 C8 C9 114.87(16) . . ? C11 C8 C10 131.79(19) . . ? C9 C8 C10 98.10(15) . . ? C9E C8E C10E 106.91(16) . . ? C9E C8E C11E 98.84(14) . . ? C10E C8E C11E 96.97(16) . . ? O1 C1F C6F 121.22(7) . . ? O1 C1F C2F 118.68(7) . . ? C6F C1F C2F 120.0 . . ? C3F C2F C1F 120.0 . . ? C3F C2F C7 110.8 . . ? C1F C2F C7 129.0 . . ? C4F C3F C2F 120.0 . . ? C3F C4F C5F 120.0 . . ? C3F C4F C8F 114.74(10) . . ? C5F C4F C8F 125.25(10) . . ? C6F C5F C4F 120.0 . . ? C1F C6F C5F 120.0 . . ? C1F C6F C40 128.13(6) . . ? C5F C6F C40 111.6 . . ? C11F C8F C9F 111.5(2) . . ? C11F C8F C10F 110.3(2) . . ? C9F C8F C10F 104.0(2) . . ? C11F C8F C4F 113.0(2) . . ? C9F C8F C4F 110.5(2) . . ? C10F C8F C4F 107.1(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.75 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.420 _refine_diff_density_min -0.379 _refine_diff_density_rms 0.040 data_ku81 _database_code_CSD 181106 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 2p-tert-butylcalix[4]arene*n-butylamine _chemical_melting_point ? _chemical_formula_moiety 2(C44H56O4),C4H11N _chemical_formula_sum 'C184 H246 N2 O16' _chemical_formula_weight 1370.985 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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4/nnc 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+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' 'y, x, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' 'x-1/2, -y, z-1/2' '-x, y-1/2, z-1/2' '-y, -x, z-1/2' 'y-1/2, x-1/2, z-1/2' _cell_length_a 12.8837(10) _cell_length_b 12.8837(10) _cell_length_c 25.102(2) _cell_angle_alpha 90.000(10) _cell_angle_beta 90.000(10) _cell_angle_gamma 90.000(10) _cell_volume 4166.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.093 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1492 _exptl_absorpt_coefficient_mu 0.068 _exptl_absorpt_correction_type empirical sadabs _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45537 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0165 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 28.73 _reflns_number_total 2721 _reflns_number_gt 2130 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0886P)^2^+1.3051P] 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 ? _refine_ls_number_reflns 2721 _refine_ls_number_parameters 154 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.0660 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1584 _refine_ls_wR_factor_gt 0.1488 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.034 _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 O1 O 0.18613(3) 0.11897(3) 0.473289(14) 0.02821(10) Uani 1 1 d . . . H1 H 0.1546 0.1759 0.4715 0.034 Uiso 1 1 calc R . . C1 C 0.15818(4) 0.06784(4) 0.51994(2) 0.02256(12) Uani 1 1 d . . . C2 C 0.06055(4) 0.08375(4) 0.54234(2) 0.02252(12) Uani 1 1 d . . . C3 C 0.03328(4) 0.02575(4) 0.58692(2) 0.02437(12) Uani 1 1 d . . . H3 H -0.0333 0.0359 0.6024 0.029 Uiso 1 1 calc R . . C4 C 0.10020(4) -0.04675(4) 0.60978(2) 0.02521(12) Uani 1 1 d . . . C5 C 0.19857(4) -0.05709(4) 0.58679(2) 0.02503(12) Uani 1 1 d . . . H5 H 0.2465 -0.1042 0.6024 0.030 Uiso 1 1 calc R . . C6 C 0.22911(4) -0.00161(4) 0.54217(2) 0.02283(12) Uani 1 1 d . . . C7 C -0.01566(4) 0.16224(4) 0.51950(2) 0.02437(12) Uani 1 1 d . . . H7A H -0.0873 0.1385 0.5270 0.029 Uiso 1 1 calc R . . H7B H -0.0069 0.1650 0.4803 0.029 Uiso 1 1 calc R . . C8 C 0.07004(5) -0.11499(5) 0.65740(2) 0.03376(15) Uani 1 1 d . . . C9 C 0.14255(7) -0.09304(8) 0.70397(3) 0.0605(2) Uani 1 1 d . . . H9A H 0.1355 -0.0203 0.7148 0.073 Uiso 1 1 calc R . . H9B H 0.2144 -0.1065 0.6931 0.073 Uiso 1 1 calc R . . H9C H 0.1244 -0.1382 0.7340 0.073 Uiso 1 1 calc R . . C10 C -0.04182(6) -0.09752(7) 0.67507(3) 0.0530(2) Uani 1 1 d . . . H10A H -0.0579 -0.1437 0.7050 0.064 Uiso 1 1 calc R . . H10B H -0.0888 -0.1124 0.6453 0.064 Uiso 1 1 calc R . . H10C H -0.0506 -0.0252 0.6863 0.064 Uiso 1 1 calc R . . C11 C 0.07993(6) -0.23012(5) 0.64117(3) 0.0510(2) Uani 1 1 d . . . H11A H 0.1509 -0.2439 0.6290 0.061 Uiso 1 1 calc R . . H11B H 0.0310 -0.2452 0.6123 0.061 Uiso 1 1 calc R . . H11C H 0.0641 -0.2743 0.6719 0.061 Uiso 1 1 calc R . . N1G N 0.2069(5) 0.2317(6) 0.66536(14) 0.114(4) Uani 0.13 1 d PDU A -1 H1G1 H 0.1868 0.1648 0.6709 0.171 Uiso 0.13 1 calc PR A -1 H1G2 H 0.2462 0.2354 0.6353 0.171 Uiso 0.06 1 calc PR A -1 H1G3 H 0.1497 0.2725 0.6615 0.171 Uiso 0.06 1 calc PR A -1 C1G C 0.2687(3) 0.2682(5) 0.71165(13) 0.090(2) Uani 0.13 1 d PDU A -1 H1G4 H 0.3050 0.3334 0.7022 0.108 Uiso 0.13 1 calc PR A -1 H1G5 H 0.3217 0.2155 0.7208 0.108 Uiso 0.13 1 calc PR A -1 C2G C 0.1981(4) 0.2872(7) 0.76002(13) 0.159(4) Uani 0.13 1 d PDU A -1 H2G1 H 0.1429 0.3372 0.7504 0.191 Uiso 0.13 1 calc PR A -1 H2G2 H 0.1645 0.2213 0.7707 0.191 Uiso 0.13 1 calc PR A -1 C3G C 0.2611(6) 0.3299(5) 0.80646(13) 0.159(4) Uani 0.13 1 d PDU A -1 H3G1 H 0.2491 0.4055 0.8093 0.191 Uiso 0.13 1 calc PR A -1 H3G2 H 0.3359 0.3188 0.7993 0.191 Uiso 0.13 1 calc PR A -1 C4G C 0.2327(8) 0.2781(7) 0.85948(16) 0.223(8) Uani 0.13 1 d PDU A -1 H4G1 H 0.2960 0.2643 0.8799 0.268 Uiso 0.13 1 calc PR A -1 H4G2 H 0.1966 0.2125 0.8525 0.268 Uiso 0.13 1 calc PR A -1 H4G3 H 0.1872 0.3242 0.8799 0.268 Uiso 0.13 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.03026(18) 0.02711(18) 0.02727(17) 0.00159(15) -0.00055(15) 0.00120(16) C1 0.0236(2) 0.0200(2) 0.0241(2) -0.00304(18) -0.00276(18) -0.00191(19) C2 0.0208(2) 0.0191(2) 0.0276(2) -0.00416(18) -0.00526(19) -0.00019(18) C3 0.0209(2) 0.0225(2) 0.0297(2) -0.00329(19) -0.00027(19) 0.00053(18) C4 0.0251(2) 0.0235(2) 0.0270(2) -0.0004(2) -0.0014(2) -0.0005(2) C5 0.0226(2) 0.0217(2) 0.0308(2) 0.0004(2) -0.0036(2) 0.00131(19) C6 0.0209(2) 0.0196(2) 0.0280(2) -0.00490(19) -0.00187(19) -0.00061(18) C7 0.0201(2) 0.0213(2) 0.0317(2) 0.00007(19) -0.00509(19) -0.00049(18) C8 0.0302(3) 0.0380(3) 0.0331(3) 0.0101(2) 0.0010(2) 0.0018(2) C9 0.0621(5) 0.0800(5) 0.0394(3) 0.0158(4) -0.0102(3) -0.0115(4) C10 0.0413(3) 0.0660(4) 0.0517(4) 0.0224(3) 0.0145(3) 0.0092(3) C11 0.0530(4) 0.0365(3) 0.0635(4) 0.0179(3) 0.0084(3) -0.0002(3) N1G 0.175(11) 0.084(5) 0.083(3) -0.016(5) -0.039(4) 0.025(5) C1G 0.034(4) 0.061(4) 0.174(5) -0.047(5) -0.010(4) 0.020(2) C2G 0.215(9) 0.175(7) 0.088(4) -0.066(4) -0.049(6) 0.073(6) C3G 0.215(9) 0.175(7) 0.088(4) -0.066(4) -0.049(6) 0.073(6) C4G 0.054(5) 0.157(14) 0.46(2) 0.039(15) -0.064(12) -0.041(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.3910(6) . ? C1 C2 1.3929(7) . ? C1 C6 1.3954(7) . ? C2 C3 1.3908(7) . ? C2 C7 1.5217(7) . ? C3 C4 1.3947(8) . ? C4 C5 1.3989(8) . ? C4 C8 1.5341(8) . ? C5 C6 1.3858(7) . ? C6 C7 1.5219(7) 3 ? C7 C6 1.5219(7) 4 ? C8 C9 1.5227(10) . ? C8 C10 1.5247(10) . ? C8 C11 1.5434(10) . ? N1G C1G 1.485(5) . ? C1G C2G 1.537(5) . ? C2G C3G 1.523(6) . ? C3G C4G 1.533(6) . ? 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 C1 C2 120.26(5) . . ? O1 C1 C6 118.08(5) . . ? C2 C1 C6 121.62(5) . . ? C3 C2 C1 118.29(5) . . ? C3 C2 C7 119.81(5) . . ? C1 C2 C7 121.90(5) . . ? C2 C3 C4 122.32(5) . . ? C3 C4 C5 117.01(5) . . ? C3 C4 C8 123.22(5) . . ? C5 C4 C8 119.76(5) . . ? C6 C5 C4 122.79(5) . . ? C5 C6 C1 117.91(5) . . ? C5 C6 C7 120.13(5) . 3 ? C1 C6 C7 121.95(5) . 3 ? C2 C7 C6 113.18(4) . 4 ? C9 C8 C10 109.22(6) . . ? C9 C8 C4 109.66(5) . . ? C10 C8 C4 112.42(5) . . ? C9 C8 C11 109.30(6) . . ? C10 C8 C11 107.26(6) . . ? C4 C8 C11 108.92(5) . . ? N1G C1G C2G 110.6(4) . . ? C3G C2G C1G 110.3(4) . . ? C2G C3G C4G 112.3(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.73 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.367 _refine_diff_density_min -0.239 _refine_diff_density_rms 0.045 data_ku88 _database_code_CSD 181107 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common p-tert-butylcalix[4]arene*n-butylamine _chemical_melting_point ? _chemical_formula_moiety C44H56O4, C4H11N _chemical_formula_sum 'C48 H67 N O4' _chemical_formula_weight 722.03 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' _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 12.9816(10) _cell_length_b 12.9816(10) _cell_length_c 12.6459(10) _cell_angle_alpha 90.000(10) _cell_angle_beta 90.000(10) _cell_angle_gamma 90.000(10) _cell_volume 2131.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.125 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_absorpt_coefficient_mu 0.070 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24975 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0144 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 28.69 _reflns_number_total 2772 _reflns_number_gt 2162 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0938P)^2^+0.3134P] 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 ? _refine_ls_number_reflns 2772 _refine_ls_number_parameters 200 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.0618 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1505 _refine_ls_wR_factor_gt 0.1413 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.099 _refine_ls_shift/su_mean 0.009 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.11756(3) 0.18851(3) 0.56124(3) 0.02941(8) Uani 1 1 d . . . H12 H 0.1763(7) 0.1565(7) 0.5587(7) 0.076(3) Uiso 1 1 d . . . C1 C 0.06782(3) 0.16151(3) 0.46828(3) 0.02329(10) Uani 1 1 d . . . C2 C 0.08343(3) 0.06501(3) 0.42258(3) 0.02345(10) Uani 1 1 d . . . C3 C 0.02920(3) 0.04071(3) 0.33058(4) 0.02580(10) Uani 1 1 d . . . H3A H 0.0389(4) -0.0257(4) 0.3003(5) 0.0308(14) Uiso 1 1 d . . . C4 C -0.03995(3) 0.10892(3) 0.28386(4) 0.02612(10) Uani 1 1 d . . . C5 C -0.05279(3) 0.20499(3) 0.33228(4) 0.02595(10) Uani 1 1 d . . . H5A H -0.0996(5) 0.2571(5) 0.3026(5) 0.0333(15) Uiso 1 1 d . . . C6 C 0.00021(3) 0.23307(3) 0.42326(3) 0.02373(10) Uani 1 1 d . . . C7 C -0.01256(3) 0.34088(3) 0.46861(4) 0.02587(10) Uani 1 1 d . . . H7B H -0.0055(4) 0.3404(4) 0.5487(4) 0.0270(14) Uiso 1 1 d . . . H7A H -0.0844(5) 0.3643(5) 0.4496(5) 0.0333(15) Uiso 1 1 d . . . C8 C -0.10227(4) 0.08207(4) 0.18446(4) 0.03306(12) Uani 1 1 d . . . C9 C -0.06790(6) -0.02055(5) 0.13644(5) 0.05565(18) Uani 1 1 d . . . H9C H 0.0083(8) -0.0191(8) 0.1125(7) 0.084(3) Uiso 1 1 d . . . H9B H -0.1067(7) -0.0336(6) 0.0702(6) 0.068(2) Uiso 1 1 d . . . H9A H -0.0800(7) -0.0823(7) 0.1892(7) 0.081(3) Uiso 1 1 d . . . C10 C -0.21687(5) 0.07410(5) 0.21397(5) 0.04834(17) Uani 1 1 d . . . H10C H -0.2609(6) 0.0612(6) 0.1508(6) 0.058(2) Uiso 1 1 d . . . H10B H -0.2241(7) 0.0104(6) 0.2653(7) 0.070(2) Uiso 1 1 d . . . H10A H -0.2434(6) 0.1367(6) 0.2473(7) 0.069(2) Uiso 1 1 d . . . C11 C -0.08952(6) 0.16639(5) 0.10089(5) 0.05045(17) Uani 1 1 d . . . H11A H -0.0165 0.1736 0.0829 0.076 Uiso 1 1 calc R . . H11B H -0.1154 0.2319 0.1289 0.076 Uiso 1 1 calc R . . H11C H -0.1286 0.1478 0.0374 0.076 Uiso 1 1 calc R . . N1G N 0.23154(11) 0.25113(18) -0.1165(2) 0.2057(16) Uani 0.25 1 d PDU A -1 H1G1 H 0.1762 0.2415 -0.1490 0.050 Uiso 0.25 1 d P B -1 H1G3 H 0.2427 0.3263 -0.1093 0.050 Uiso 0.25 1 d P C -1 C1G C 0.26410(17) 0.2096(2) -0.0118(2) 0.179(4) Uani 0.25 1 d PDU A -1 H1G4 H 0.3403 0.2084 -0.0108 0.215 Uiso 0.25 1 calc PR A -1 H1G5 H 0.2405 0.1372 -0.0078 0.215 Uiso 0.25 1 calc PR A -1 C2G C 0.22906(11) 0.26271(15) 0.0868(2) 0.254(4) Uani 0.25 1 d PDU A -1 H2G1 H 0.1528 0.2635 0.0884 0.304 Uiso 0.25 1 calc PR A -1 H2G2 H 0.2531 0.3351 0.0854 0.304 Uiso 0.25 1 calc PR A -1 C3G C 0.2694(2) 0.2103(2) 0.1881(2) 0.168(2) Uani 0.25 1 d PDU A -1 H3G1 H 0.2447 0.1382 0.1923 0.201 Uiso 0.25 1 calc PR A -1 H3G2 H 0.3456 0.2102 0.1893 0.201 Uiso 0.25 1 calc PR A -1 C4G C 0.2276(2) 0.2723(3) 0.2773(3) 0.279(2) Uani 0.25 1 d PDU A -1 H4G1 H 0.2842 0.2937 0.3237 0.419 Uiso 0.25 1 calc PR A -1 H4G2 H 0.1784 0.2307 0.3177 0.419 Uiso 0.25 1 calc PR A -1 H4G3 H 0.1927 0.3335 0.2494 0.419 Uiso 0.25 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.02934(15) 0.03049(15) 0.02841(15) -0.00039(13) -0.00114(13) 0.00099(13) C1 0.01987(17) 0.02375(18) 0.02626(18) 0.00211(15) 0.00341(15) -0.00200(15) C2 0.01910(17) 0.02050(17) 0.03076(19) 0.00396(15) 0.00388(16) -0.00082(15) C3 0.02355(18) 0.02199(18) 0.0319(2) -0.00095(16) 0.00411(16) -0.00091(16) C4 0.02426(19) 0.02564(19) 0.02847(19) 0.00101(17) 0.00109(16) -0.00165(16) C5 0.02155(18) 0.02349(19) 0.0328(2) 0.00340(17) 0.00125(16) 0.00020(16) C6 0.01956(17) 0.02081(17) 0.0308(2) 0.00141(16) 0.00597(15) -0.00069(15) C7 0.02108(18) 0.02149(18) 0.0350(2) -0.00194(16) 0.00531(16) 0.00050(15) C8 0.0350(2) 0.0323(2) 0.0319(2) -0.00156(19) -0.00494(19) -0.0004(2) C9 0.0703(4) 0.0482(3) 0.0484(3) -0.0195(2) -0.0197(3) 0.0119(3) C10 0.0341(3) 0.0643(4) 0.0466(3) -0.0004(3) -0.0106(2) -0.0085(3) C11 0.0636(4) 0.0531(3) 0.0346(3) 0.0073(2) -0.0073(3) -0.0072(3) N1G 0.0363(15) 0.0793(12) 0.501(4) 0.160(2) -0.0808(18) -0.0266(13) C1G 0.118(4) 0.196(9) 0.223(5) 0.051(4) 0.082(4) 0.042(4) C2G 0.211(6) 0.112(4) 0.438(9) -0.014(6) 0.136(6) 0.078(5) C3G 0.281(6) 0.098(2) 0.123(3) 0.0633(19) 0.100(4) 0.099(3) C4G 0.266(3) 0.110(4) 0.460(5) -0.037(4) 0.303(3) -0.065(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 O1 C1 1.3863(5) . ? C1 C2 1.3944(6) . ? C1 C6 1.3990(6) . ? C2 C3 1.3959(6) . ? C2 C7 1.5226(6) 3 ? C3 C4 1.3925(6) . ? C4 C5 1.3994(6) . ? C4 C8 1.5349(7) . ? C5 C6 1.3891(6) . ? C6 C7 1.5215(6) . ? C7 C2 1.5226(6) 4 ? C8 C11 1.5305(8) . ? C8 C9 1.5306(8) . ? C8 C10 1.5372(8) . ? N1G C1G 1.491(4) . ? C1G C2G 1.495(4) . ? C2G C3G 1.542(4) . ? C3G C4G 1.489(4) . ? 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 C1 C2 120.72(4) . . ? O1 C1 C6 118.00(4) . . ? C2 C1 C6 121.27(4) . . ? C1 C2 C3 118.36(4) . . ? C1 C2 C7 121.98(4) . 3 ? C3 C2 C7 119.64(4) . 3 ? C4 C3 C2 122.35(4) . . ? C3 C4 C5 117.24(4) . . ? C3 C4 C8 122.89(4) . . ? C5 C4 C8 119.87(4) . . ? C6 C5 C4 122.50(4) . . ? C5 C6 C1 118.26(4) . . ? C5 C6 C7 119.97(4) . . ? C1 C6 C7 121.71(4) . . ? C6 C7 C2 112.17(4) . 4 ? C11 C8 C9 108.48(5) . . ? C11 C8 C4 110.25(4) . . ? C9 C8 C4 111.65(4) . . ? C11 C8 C10 108.69(5) . . ? C9 C8 C10 108.65(5) . . ? C4 C8 C10 109.06(4) . . ? N1G C1G C2G 119.2(2) . . ? C1G C2G C3G 112.70(19) . . ? C4G C3G C2G 105.5(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.69 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.313 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.044