# ja0204269.cif data_patbrs _publ_requested_journal ; Journal of the American Chemical Society Manuscript# JA0204269 ; _publ_contact_author ; Julius Rebek, Jr. Skaggs Institute for Chemical Biology (MB26) The Scripps Research Institute 10550 N. Torrey Pines Road La Jolla, CA 92037 ; _publ_contact_author_phone '858-784-2250' _publ_contact_author_fax '858-784-2876' _publ_contact_author_email 'jrebek@scripps.edu' loop_ _publ_author_name _publ_author_address 'Alexandr Shivanyuk' ; Skaggs Institute for Chemical Biology (MB26) The Scripps Research Institute 10550 N. Torrey Pines Road La Jolla, CA 92037 ; 'Patrick Amrhein' ; Skaggs Institute for Chemical Biology (MB26) The Scripps Research Institute 10550 N. Torrey Pines Road La Jolla, CA 92037 ; 'Darren W. Johnson' ; Skaggs Institute for Chemical Biology (MB26) The Scripps Research Institute 10550 N. Torrey Pines Road La Jolla, CA 92037 ; _publ_section_title ; Metal Switching and Self-Inclusion of Functional Cavitands ; _publ_section_references ; Altomare, A., Burla, M. C., Camalli, M., Cascarano, M., Giacovazzo, C., Guagliardi, A., Polidori, G. (1993). J. Appl. Cryst., 26, 343-350. Siemens Industrial Automation, Inc. (1995). SMART. Area Detector Software Package, Madison, WI, USA. Siemens Industrial Automation, Inc. (1995). SAINT. SAX Area Detector Integration Program (v. 4.024), Madison, WI, USA. Siemens Industrial Automation, Inc. (1993). SHELXL. SHELXTL Crystal Structure Determination Software Package, Madison, WI, USA. ; _audit_creation_method SHELXL-97 _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement ; SMART (Siemens, 1995), SAINT (Siemens, 1995) ; _computing_data_reduction ; SAINT (Siemens, 1995), XPREP (Siemens, 1995) ; _computing_structure_solution ; SHELXL-97 (Sheldrick, 1997) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #-------------------------------------------------------------- _cell_length_a 14.7937(6) _cell_length_b 17.8890(7) _cell_length_c 18.2308(8) _cell_angle_alpha 87.653(2) _cell_angle_beta 71.100(2) _cell_angle_gamma 83.745(2) _cell_volume 4537.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 117(2) _cell_measurement_reflns_used 17486 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 49.23 #-------------------------------------------------------------- _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' #-------------------------------------------------------------- _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.609 _exptl_crystal_F_000 2180 _chemical_formula_sum 'C94 H62 Br8 N8 O16' _chemical_formula_weight 2198.80 _chemical_compound_source 'synthetic' _exptl_absorpt_coefficient_mu 4.811 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.290 _exptl_absorpt_correction_T_max 0.633 _exptl_special_details ; ? ; #-------------------------------------------------------------- _diffrn_ambient_temperature 117(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_detector 'CCD area detector' _diffrn_measurement_device_type '3 circle diffractometer' _diffrn_measurement_method ; omega scans with profile analysis ; _diffrn_reflns_number 17483 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_sigmaI/netI 0.0523 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 49.35 _reflns_number_total 8122 _reflns_number_gt 6649 _reflns_threshold_expression >2sigma(I) _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. This octabromo-cavitand crystallizes in the vase conformation in space group P-1 with two molecules in the unit cell. Therefore one cavitand makes up the asymmetric unit of the cell and thus has no crystallographic symmetry. The cavitand does have approximate four-fold symmetry due to the seam of hydrogen bonds holding the molecule in the vase shape. A disordered molecule of solvent was found encapsulated within the pocket of the cavitand. This guest was disordered and modeled as cyclohexane based on the shape of the electron density, NMR spectroscopic measurements showing a bound cyclohexane, and the crystallization solvents used (ethyl acetate and cyclohexane). Constraints were used to maintain the cyclic structure of the cyclohexane, but, presumably due to disorder about the pseudo-four-fold axis of the cavitand, the cyclohexane molecule appears almost flat in the final structure and has very large thermal parameters. The cluster packs with no intermolecular hydrogen bonds, but there are Eight N-H---(O) intramolecular hydrogen bonds holding the cavitand in the vase shape. In addition, the molecule packs with the feet of one cavitand sitting above the upper rim of the cavitand below it. In addition, the two cavitands in the unit cell are related by an inversion axis and are making van der Waals contacts on their aromatic side walls. Only the Br atoms of the molecule were refined anisotropically. All other atoms were refined isotropically and hydrogen atoms were included on all appropriate atoms of the cavitand at fixed positions but not refined. Two reflections with large delF/sig were omitted on the last least squares cycles. A solvent water parameter (SWAT) was used to account for diffuse electron density in the final Fourier map which is attributed to highly disordered solvent molecules. Finally, the large residual electron density peaks correspond to noise near the heavy bromine atoms. ; _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^)+(0.1762P)^2^+69.1860P] 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_number_reflns 8122 _refine_ls_number_parameters 556 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1145 _refine_ls_R_factor_gt 0.1012 _refine_ls_wR_factor_ref 0.2815 _refine_ls_wR_factor_gt 0.2716 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.040 _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 Br1 Br 1.17491(10) 0.72071(9) 0.07031(9) 0.0384(5) Uani 1 1 d . . . Br2 Br 1.16926(10) 0.97943(9) 0.17108(9) 0.0405(5) Uani 1 1 d . . . Br3 Br 1.32558(13) 0.35338(9) 0.23904(9) 0.0455(5) Uani 1 1 d . . . Br4 Br 1.3890(2) 0.74002(15) 0.76489(12) 0.1020(10) Uani 1 1 d . . . Br5 Br 1.21492(11) 0.61138(10) 0.25136(10) 0.0483(6) Uani 1 1 d . . . Br6 Br 1.29779(16) 1.17238(10) 0.36147(10) 0.0610(6) Uani 1 1 d . . . Br7 Br 1.19832(15) 0.96045(17) 0.39736(15) 0.0944(9) Uani 1 1 d . . . Br8A Br 1.2252(3) 0.7346(2) 0.5129(3) 0.0585(14) Uani 0.40 1 d P . . Br8 Br 1.1719(2) 0.5950(2) 0.5064(2) 0.0732(11) Uani 0.60 1 d P . . O10 O 1.7514(5) 1.0046(4) 0.1302(4) 0.018(2) Uiso 1 1 d . . . O11 O 1.7689(5) 0.6837(4) -0.0921(4) 0.0149(19) Uiso 1 1 d . . . O12 O 1.7657(6) 0.7784(4) 0.4533(4) 0.019(2) Uiso 1 1 d . . . O13 O 1.7516(6) 0.9140(4) 0.3808(5) 0.020(2) Uiso 1 1 d . . . O14 O 1.7588(5) 0.5482(4) -0.0144(4) 0.0148(19) Uiso 1 1 d . . . O15 O 1.3801(6) 1.1320(5) 0.1434(5) 0.033(2) Uiso 1 1 d . . . O16 O 1.3779(7) 0.3913(5) 0.4200(5) 0.035(2) Uiso 1 1 d . . . O17 O 1.7468(5) 0.4607(4) 0.2411(4) 0.0132(19) Uiso 1 1 d . . . O18 O 1.3578(6) 0.6252(5) -0.0661(5) 0.031(2) Uiso 1 1 d . . . O19 O 1.7422(5) 0.9350(4) 0.0027(4) 0.0128(19) Uiso 1 1 d . . . O20 O 1.7423(5) 0.5307(4) 0.3749(4) 0.0122(18) Uiso 1 1 d . . . O21 O 1.4236(6) 0.6442(5) 0.5329(5) 0.032(2) Uiso 1 1 d . . . O22 O 1.4142(7) 0.8680(5) 0.0236(5) 0.035(2) Uiso 1 1 d . . . O23 O 1.4329(7) 0.5365(5) 0.1739(5) 0.035(2) Uiso 1 1 d . . . O28 O 1.4193(7) 0.9766(5) 0.3696(6) 0.042(3) Uiso 1 1 d . . . O38 O 1.3691(8) 0.8971(6) 0.6513(6) 0.051(3) Uiso 1 1 d . . . C149 C 1.6905(19) 0.7380(14) 0.2054(15) 0.105(8) Uiso 1 1 d D . . N24 N 1.4215(7) 0.7180(6) -0.0240(6) 0.018(2) Uiso 1 1 d . . . H24A H 1.4142 0.7648 -0.0122 0.022 Uiso 1 1 calc R . . N26 N 1.4010(7) 0.4785(5) 0.3268(6) 0.018(2) Uiso 1 1 d . . . H26A H 1.3769 0.5035 0.2950 0.021 Uiso 1 1 calc R . . N30 N 1.4010(7) 0.9247(6) 0.4882(6) 0.025(3) Uiso 1 1 d . . . H30A H 1.3595 0.9199 0.5334 0.030 Uiso 1 1 calc R . . N31 N 1.4092(7) 0.5851(5) 0.0639(6) 0.018(2) Uiso 1 1 d . . . H31A H 1.3675 0.5912 0.0399 0.021 Uiso 1 1 calc R . . N32 N 1.3913(8) 0.9579(6) 0.1124(6) 0.026(3) Uiso 1 1 d . . . H32A H 1.3459 0.9869 0.1432 0.031 Uiso 1 1 calc R . . N34 N 1.4040(7) 1.0450(5) 0.2295(6) 0.019(2) Uiso 1 1 d . . . H34A H 1.3816 1.0261 0.2751 0.022 Uiso 1 1 calc R . . N45 N 1.4232(7) 0.7940(6) 0.5754(6) 0.021(3) Uiso 1 1 d . . . H45A H 1.4079 0.7513 0.5656 0.026 Uiso 1 1 calc R . . N51 N 1.3916(7) 0.5660(5) 0.4503(6) 0.019(3) Uiso 1 1 d . . . H51A H 1.3446 0.5472 0.4423 0.023 Uiso 1 1 calc R . . C25 C 1.4874(8) 0.5000(6) 0.3362(7) 0.011(3) Uiso 1 1 d . . . C27 C 1.7961(8) 0.7207(6) 0.3974(7) 0.012(3) Uiso 1 1 d . . . C29 C 1.4838(8) 0.5407(6) 0.4005(7) 0.013(3) Uiso 1 1 d . . . C33 C 1.7987(8) 0.7355(7) -0.0498(7) 0.015(3) Uiso 1 1 d . . . C35 C 1.8666(8) 0.8426(6) 0.0196(7) 0.012(3) Uiso 1 1 d . . . C36 C 1.8769(8) 0.7307(6) 0.3317(7) 0.014(3) Uiso 1 1 d . . . C37 C 1.8723(8) 0.5881(6) 0.0429(7) 0.011(3) Uiso 1 1 d . . . C39 C 1.4902(8) 1.0100(6) 0.1745(7) 0.013(3) Uiso 1 1 d . . . C40 C 1.9067(8) 0.5345(6) 0.2391(7) 0.012(3) Uiso 1 1 d . . . H40A H 1.8796 0.4908 0.2691 0.015 Uiso 1 1 calc R . . C41 C 1.6557(8) 0.5273(6) 0.3582(7) 0.013(3) Uiso 1 1 d . . . C42 C 1.7857(8) 0.5073(6) 0.1758(6) 0.010(3) Uiso 1 1 d . . . C43 C 1.9108(8) 0.6690(6) 0.2817(7) 0.014(3) Uiso 1 1 d . . . H43A H 1.9641 0.6731 0.2378 0.017 Uiso 1 1 calc R . . C44 C 2.0206(9) 0.8937(7) 0.0179(7) 0.019(3) Uiso 1 1 d . . . H44A H 2.0444 0.9338 0.0384 0.023 Uiso 1 1 calc R . . H44B H 2.0450 0.8464 0.0358 0.023 Uiso 1 1 calc R . . C46 C 1.4934(9) 0.8896(7) 0.4787(7) 0.018(3) Uiso 1 1 d . . . C47 C 1.9071(8) 0.7688(6) 0.0111(6) 0.008(3) Uiso 1 1 d . . . H47A H 1.9584 0.7553 0.0295 0.010 Uiso 1 1 calc R . . C48 C 1.5024(8) 0.6091(6) 0.0235(7) 0.013(3) Uiso 1 1 d . . . C49 C 1.9193(8) 0.8063(7) 0.3170(7) 0.017(3) Uiso 1 1 d . . . H49A H 1.9006 0.8306 0.3677 0.020 Uiso 1 1 calc R . . C50 C 1.9203(8) 0.6321(6) -0.0317(7) 0.014(3) Uiso 1 1 d . . . H50A H 1.9052 0.6097 -0.0740 0.017 Uiso 1 1 calc R . . C52 C 1.7924(8) 0.5510(6) 0.0497(7) 0.013(3) Uiso 1 1 d . . . C53 C 1.6572(8) 0.9524(6) 0.0633(6) 0.009(3) Uiso 1 1 d . . . C54 C 1.5741(8) 0.4754(6) 0.2828(7) 0.015(3) Uiso 1 1 d . . . H54A H 1.5753 0.4488 0.2397 0.018 Uiso 1 1 calc R . . C55 C 1.9107(8) 0.9017(7) 0.0506(7) 0.012(3) Uiso 1 1 d . . . H55A H 1.8890 0.9503 0.0320 0.015 Uiso 1 1 calc R . . C56 C 1.7889(8) 0.9056(7) 0.2996(7) 0.014(3) Uiso 1 1 d . . . C57 C 2.0156(8) 0.5158(7) 0.2143(7) 0.017(3) Uiso 1 1 d . . . H57A H 2.0466 0.5618 0.1998 0.020 Uiso 1 1 calc R . . H57B H 2.0363 0.4833 0.1694 0.020 Uiso 1 1 calc R . . C58 C 1.2775(10) 0.3947(8) 0.3430(8) 0.034(4) Uiso 1 1 d . . . H58A H 1.2295 0.4367 0.3449 0.040 Uiso 1 1 calc R . . H58B H 1.2471 0.3567 0.3793 0.040 Uiso 1 1 calc R . . C59 C 1.7518(9) 0.6568(7) 0.4095(7) 0.018(3) Uiso 1 1 d . . . H59A H 1.6980 0.6528 0.4529 0.022 Uiso 1 1 calc R . . C60 C 1.6591(8) 0.4896(6) 0.2924(6) 0.008(3) Uiso 1 1 d . . . C61 C 2.0303(8) 0.6254(7) -0.0538(7) 0.018(3) Uiso 1 1 d . . . H61A H 2.0547 0.5727 -0.0554 0.022 Uiso 1 1 calc R . . H61B H 2.0480 0.6495 -0.0144 0.022 Uiso 1 1 calc R . . C62 C 1.9095(9) 0.8572(7) 0.1852(7) 0.018(3) Uiso 1 1 d . . . H62A H 1.9632 0.8239 0.1618 0.021 Uiso 1 1 calc R . . C63 C 1.9069(8) 0.5832(6) 0.1049(6) 0.013(3) Uiso 1 1 d . . . H63A H 1.9599 0.6085 0.1012 0.015 Uiso 1 1 calc R . . C64 C 2.0273(8) 0.8004(7) 0.2867(7) 0.020(3) Uiso 1 1 d . . . H64A H 2.0475 0.8497 0.2692 0.024 Uiso 1 1 calc R . . H64B H 2.0499 0.7672 0.2423 0.024 Uiso 1 1 calc R . . C65 C 1.6612(8) 0.9906(6) 0.1259(7) 0.012(3) Uiso 1 1 d . . . C66 C 1.4843(9) 0.9681(7) 0.1144(7) 0.018(3) Uiso 1 1 d . . . C67 C 1.7495(8) 0.5100(6) 0.1155(6) 0.012(3) Uiso 1 1 d . . . H67A H 1.6968 0.4846 0.1186 0.015 Uiso 1 1 calc R . . C68 C 1.8670(8) 0.5424(6) 0.1736(7) 0.014(3) Uiso 1 1 d . . . C69 C 1.8748(8) 0.7129(6) -0.0237(7) 0.012(3) Uiso 1 1 d . . . C70 C 1.5687(8) 0.5537(7) 0.4135(7) 0.017(3) Uiso 1 1 d . . . H70A H 1.5675 0.5791 0.4574 0.020 Uiso 1 1 calc R . . C71 C 1.5796(8) 1.0205(6) 0.1808(7) 0.014(3) Uiso 1 1 d . . . H71A H 1.5836 1.0475 0.2220 0.017 Uiso 1 1 calc R . . C72 C 1.7863(8) 0.8597(6) -0.0031(7) 0.012(3) Uiso 1 1 d . . . C73 C 1.5958(8) 0.6987(7) -0.0573(7) 0.017(3) Uiso 1 1 d . . . H73A H 1.5997 0.7431 -0.0861 0.020 Uiso 1 1 calc R . . C74 C 1.3810(9) 0.5545(7) 0.1347(8) 0.025(3) Uiso 1 1 d . . . C75 C 1.8686(8) 0.6022(6) 0.2947(7) 0.012(3) Uiso 1 1 d . . . C76 C 1.6740(8) 0.5924(6) -0.0114(6) 0.010(3) Uiso 1 1 d . . . C77 C 1.8704(8) 0.9041(6) 0.1383(6) 0.011(3) Uiso 1 1 d . . . C78 C 1.5053(8) 0.8245(7) 0.5210(7) 0.015(3) Uiso 1 1 d . . . C79 C 1.6658(9) 0.8812(7) 0.4216(7) 0.018(3) Uiso 1 1 d . . . C80 C 1.5780(9) 0.9193(7) 0.4291(7) 0.020(3) Uiso 1 1 d . . . H80A H 1.5735 0.9640 0.4021 0.024 Uiso 1 1 calc R . . C81 C 1.3569(9) 0.4205(7) 0.3662(7) 0.020(3) Uiso 1 1 d . . . C82 C 1.3673(9) 0.6154(7) 0.5086(7) 0.022(3) Uiso 1 1 d . . . C83 C 1.6741(8) 0.8154(7) 0.4614(7) 0.015(3) Uiso 1 1 d . . . C84 C 1.5857(8) 0.5672(7) 0.0274(7) 0.017(3) Uiso 1 1 d . . . H84A H 1.5820 0.5227 0.0560 0.021 Uiso 1 1 calc R . . C85 C 1.2716(11) 1.1447(9) 0.2709(9) 0.039(4) Uiso 1 1 d . . . H85A H 1.2221 1.1105 0.2858 0.047 Uiso 1 1 calc R . . H85B H 1.2468 1.1894 0.2489 0.047 Uiso 1 1 calc R . . C86 C 1.7889(8) 0.9532(6) 0.1750(7) 0.013(3) Uiso 1 1 d . . . C87 C 2.0597(9) 0.8962(7) -0.0699(7) 0.018(3) Uiso 1 1 d . . . H87A H 2.1286 0.8911 -0.0863 0.028 Uiso 1 1 calc R . . H87B H 2.0372 0.9434 -0.0882 0.028 Uiso 1 1 calc R . . H87C H 2.0380 0.8558 -0.0907 0.028 Uiso 1 1 calc R . . C88 C 1.5064(9) 0.6738(7) -0.0198(7) 0.017(3) Uiso 1 1 d . . . C89 C 1.7852(8) 0.5976(6) 0.3583(6) 0.011(3) Uiso 1 1 d . . . C90 C 1.7492(9) 0.9550(7) 0.2551(7) 0.019(3) Uiso 1 1 d . . . H90A H 1.6964 0.9890 0.2787 0.023 Uiso 1 1 calc R . . C91 C 2.0772(9) 0.6623(7) -0.1334(7) 0.026(3) Uiso 1 1 d . . . H91A H 2.1457 0.6573 -0.1452 0.039 Uiso 1 1 calc R . . H91B H 2.0538 0.7146 -0.1318 0.039 Uiso 1 1 calc R . . H91C H 2.0611 0.6378 -0.1728 0.039 Uiso 1 1 calc R . . C92 C 1.8712(8) 0.8580(7) 0.2669(7) 0.015(3) Uiso 1 1 d . . . C93 C 1.6786(8) 0.6586(7) -0.0525(7) 0.016(3) Uiso 1 1 d . . . C94 C 1.3592(9) 1.1074(7) 0.2090(8) 0.025(3) Uiso 1 1 d . . . C95 C 1.5931(9) 0.7873(7) 0.5108(7) 0.020(3) Uiso 1 1 d . . . H95A H 1.5987 0.7424 0.5374 0.024 Uiso 1 1 calc R . . C96 C 1.3622(9) 0.9132(7) 0.0730(8) 0.025(3) Uiso 1 1 d . . . C97 C 1.7524(8) 0.8070(6) -0.0397(7) 0.014(3) Uiso 1 1 d . . . H97A H 1.6999 0.8200 -0.0567 0.017 Uiso 1 1 calc R . . C98 C 1.3688(10) 0.9641(8) 0.4375(8) 0.028(3) Uiso 1 1 d . . . C99 C 1.2594(10) 0.6349(8) 0.5507(8) 0.035(4) Uiso 1 1 d . . . C100 C 1.2540(9) 0.9117(8) 0.0881(8) 0.026(3) Uiso 1 1 d . . . H10A H 1.2380 0.8606 0.1015 0.032 Uiso 1 1 calc R . . H10B H 1.2404 0.9250 0.0404 0.032 Uiso 1 1 calc R . . C101 C 1.2745(9) 0.5433(8) 0.1647(8) 0.027(3) Uiso 1 1 d . . . H10C H 1.2658 0.4917 0.1815 0.033 Uiso 1 1 calc R . . H10D H 1.2457 0.5546 0.1242 0.033 Uiso 1 1 calc R . . C102 C 1.5699(9) 0.9399(7) 0.0560(7) 0.020(3) Uiso 1 1 d . . . H10E H 1.5673 0.9137 0.0138 0.024 Uiso 1 1 calc R . . C103 C 1.2614(10) 0.9915(8) 0.4668(8) 0.035(4) Uiso 1 1 d . . . H10F H 1.2532 1.0459 0.4705 0.042 Uiso 1 1 calc R . . H10G H 1.2324 0.9711 0.5182 0.042 Uiso 1 1 calc R . . C104 C 1.3523(9) 0.6910(7) -0.0454(8) 0.026(3) Uiso 1 1 d . . . C105 C 2.0456(11) 0.4768(8) 0.2801(8) 0.038(4) Uiso 1 1 d . . . H10H H 2.1141 0.4653 0.2634 0.057 Uiso 1 1 calc R . . H10I H 2.0155 0.4311 0.2941 0.057 Uiso 1 1 calc R . . H10J H 2.0262 0.5094 0.3242 0.057 Uiso 1 1 calc R . . C106 C 1.2637(10) 0.7434(8) -0.0340(8) 0.032(4) Uiso 1 1 d . . . H10K H 1.2349 0.7358 -0.0736 0.039 Uiso 1 1 calc R . . H10L H 1.2784 0.7952 -0.0368 0.039 Uiso 1 1 calc R . . C107 C 1.3065(12) 0.7826(10) 0.7033(10) 0.055(5) Uiso 1 1 d . . . H10M H 1.2859 0.7428 0.6798 0.066 Uiso 1 1 calc R . . H10N H 1.2501 0.8124 0.7359 0.066 Uiso 1 1 calc R . . C110 C 1.3684(10) 0.8307(8) 0.6424(8) 0.030(4) Uiso 1 1 d . . . C111 C 2.0729(11) 0.7712(9) 0.3464(9) 0.044(4) Uiso 1 1 d . . . H11A H 2.1415 0.7685 0.3240 0.066 Uiso 1 1 calc R . . H11B H 2.0542 0.7220 0.3632 0.066 Uiso 1 1 calc R . . H11C H 2.0521 0.8045 0.3900 0.066 Uiso 1 1 calc R . . C150 C 1.591(2) 0.748(4) 0.268(2) 0.38(4) Uiso 1 1 d D . . C151 C 1.482(2) 0.759(5) 0.290(3) 0.44(5) Uiso 1 1 d D . . C152 C 1.492(3) 0.750(3) 0.199(3) 0.30(3) Uiso 1 1 d D . . C153 C 1.601(3) 0.738(4) 0.180(3) 0.39(5) Uiso 1 1 d D . . C154 C 1.394(3) 0.774(4) 0.261(3) 0.33(4) Uiso 1 1 d D . . C198 C 0.981(4) 0.748(3) 0.697(4) 0.26(3) Uiso 1 1 d . . . C199 C 1.012(4) 0.860(3) 0.648(4) 0.24(2) Uiso 1 1 d . . . C200 C 1.041(2) 0.9963(18) 0.6311(18) 0.131(10) Uiso 1 1 d . . . C201 C 1.074(3) 0.938(2) 0.678(2) 0.155(13) Uiso 1 1 d . . . C202 C 1.134(3) 0.891(2) 0.649(2) 0.156(13) Uiso 1 1 d . . . C203 C 1.165(3) 0.827(3) 0.612(3) 0.196(17) Uiso 1 1 d . . . C204 C 0.986(2) 0.8967(19) 0.714(2) 0.128(10) Uiso 1 1 d . . . C205 C 1.007(5) 0.827(4) 0.740(4) 0.28(3) Uiso 1 1 d . . . C206 C 0.983(6) 0.766(5) 0.604(5) 0.38(4) Uiso 1 1 d . . . C207 C 1.054(2) 0.4038(17) 0.5166(17) 0.121(9) Uiso 1 1 d . . . C208 C 1.041(2) 0.484(2) 0.491(2) 0.150(12) Uiso 1 1 d . . . C209 C 1.032(4) 0.342(3) 0.463(4) 0.26(2) Uiso 1 1 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 Br1 0.0157(9) 0.0433(10) 0.0494(11) -0.0059(8) 0.0000(7) -0.0045(7) Br2 0.0123(9) 0.0581(12) 0.0398(10) -0.0126(8) 0.0107(7) -0.0107(8) Br3 0.0626(12) 0.0410(11) 0.0370(10) -0.0153(8) -0.0177(9) -0.0123(9) Br4 0.129(2) 0.0996(19) 0.0436(13) 0.0139(12) 0.0012(13) 0.0379(16) Br5 0.0217(10) 0.0653(12) 0.0492(11) -0.0269(9) 0.0045(8) -0.0066(8) Br6 0.1101(17) 0.0400(11) 0.0322(11) -0.0212(8) -0.0233(11) 0.0047(10) Br7 0.0452(13) 0.153(2) 0.0927(18) -0.0381(16) -0.0222(12) -0.0289(14) Br8A 0.014(2) 0.030(2) 0.123(4) -0.012(2) -0.013(2) 0.0074(18) Br8 0.0216(17) 0.118(3) 0.071(2) -0.036(2) -0.0010(16) 0.0036(17) _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 Br1 C106 1.985(14) . ? Br2 C100 1.979(13) . ? Br3 C58 1.942(14) . ? Br4 C107 1.986(17) . ? Br5 C101 1.943(13) . ? Br6 C85 1.908(15) . ? Br7 C103 1.929(14) . ? Br8A C99 1.960(15) . ? Br8A C203 2.39(5) . ? Br8A Br8 2.719(6) . ? Br8 C99 1.941(15) . ? O10 C86 1.395(14) . ? O10 C65 1.411(14) . ? O11 C93 1.410(14) . ? O11 C33 1.419(14) . ? O12 C83 1.406(14) . ? O12 C27 1.413(14) . ? O13 C56 1.411(14) . ? O13 C79 1.423(14) . ? O14 C76 1.395(13) . ? O14 C52 1.415(14) . ? O15 C94 1.210(15) . ? O16 C81 1.204(14) . ? O17 C60 1.390(13) . ? O17 C42 1.423(14) . ? O18 C104 1.236(15) . ? O19 C53 1.394(13) . ? O19 C72 1.423(14) . ? O20 C89 1.393(14) . ? O20 C41 1.418(14) . ? O21 C82 1.228(15) . ? O22 C96 1.238(15) . ? O23 C74 1.218(14) . ? O28 C98 1.246(16) . ? O38 C110 1.207(16) . ? C149 C153 1.538(19) . ? C149 C150 1.542(19) . ? N24 C104 1.348(16) . ? N24 C88 1.432(16) . ? N26 C81 1.342(16) . ? N26 C25 1.438(15) . ? N30 C98 1.318(16) . ? N30 C46 1.401(16) . ? N31 C74 1.337(16) . ? N31 C48 1.439(15) . ? N32 C96 1.289(16) . ? N32 C66 1.419(16) . ? N34 C94 1.338(15) . ? N34 C39 1.440(16) . ? N45 C110 1.375(17) . ? N45 C78 1.441(16) . ? N51 C82 1.341(16) . ? N51 C29 1.409(15) . ? C25 C54 1.375(16) . ? C25 C29 1.388(17) . ? C27 C59 1.353(17) . ? C27 C36 1.413(17) . ? C29 C70 1.396(17) . ? C33 C97 1.374(16) . ? C33 C69 1.374(16) . ? C35 C72 1.381(16) . ? C35 C47 1.383(16) . ? C35 C55 1.516(17) . ? C36 C43 1.403(17) . ? C36 C49 1.531(18) . ? C37 C63 1.379(16) . ? C37 C52 1.387(17) . ? C37 C50 1.544(16) . ? C39 C66 1.384(17) . ? C39 C71 1.398(17) . ? C40 C68 1.488(17) . ? C40 C57 1.528(17) . ? C40 C75 1.546(17) . ? C41 C60 1.384(16) . ? C41 C70 1.401(17) . ? C42 C67 1.368(16) . ? C42 C68 1.404(17) . ? C43 C75 1.385(17) . ? C44 C87 1.516(17) . ? C44 C55 1.532(17) . ? C46 C78 1.397(17) . ? C46 C80 1.427(17) . ? C47 C69 1.408(16) . ? C48 C88 1.369(16) . ? C48 C84 1.391(17) . ? C49 C64 1.504(17) . ? C49 C92 1.551(17) . ? C50 C69 1.519(16) . ? C50 C61 1.537(17) . ? C52 C67 1.383(16) . ? C53 C65 1.374(16) . ? C53 C102 1.382(17) . ? C54 C60 1.376(16) . ? C55 C77 1.515(16) . ? C56 C92 1.382(17) . ? C56 C90 1.386(17) . ? C57 C105 1.528(18) . ? C58 C81 1.492(19) . ? C59 C89 1.380(17) . ? C61 C91 1.547(17) . ? C62 C77 1.387(16) . ? C62 C92 1.412(17) . ? C63 C68 1.410(16) . ? C64 C111 1.505(19) . ? C65 C71 1.366(16) . ? C66 C102 1.423(18) . ? C72 C97 1.398(16) . ? C73 C93 1.377(17) . ? C73 C88 1.390(17) . ? C74 C101 1.525(18) . ? C75 C89 1.401(16) . ? C76 C93 1.371(16) . ? C76 C84 1.383(16) . ? C77 C86 1.402(16) . ? C78 C95 1.353(17) . ? C79 C83 1.372(17) . ? C79 C80 1.368(17) . ? C82 C99 1.54(2) . ? C83 C95 1.377(17) . ? C85 C94 1.53(2) . ? C86 C90 1.386(17) . ? C96 C100 1.536(18) . ? C98 C103 1.53(2) . ? C104 C106 1.488(19) . ? C107 C110 1.50(2) . ? C150 C151 1.532(17) . ? C150 C153 1.59(8) . ? C151 C154 1.551(19) . ? C151 C152 1.64(7) . ? C152 C153 1.532(17) . ? C152 C154 1.548(19) . ? C198 C206 1.70(9) . ? C198 C205 1.78(8) . ? C199 C204 1.32(6) . ? C199 C205 1.75(8) . ? C199 C201 1.93(7) . ? C199 C202 1.95(6) . ? C200 C201 1.46(4) . ? C201 C202 1.15(5) . ? C201 C204 1.51(4) . ? C202 C203 1.31(5) . ? C204 C205 1.36(7) . ? C207 C208 1.50(4) . ? C207 C209 1.63(6) . ? C208 C208 1.23(6) 2_766 ? 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 C99 Br8A C203 113.8(12) . . ? C99 Br8A Br8 45.5(4) . . ? C203 Br8A Br8 130.1(11) . . ? C99 Br8 Br8A 46.1(4) . . ? C86 O10 C65 114.9(8) . . ? C93 O11 C33 114.3(8) . . ? C83 O12 C27 114.5(9) . . ? C56 O13 C79 118.4(9) . . ? C76 O14 C52 117.5(8) . . ? C60 O17 C42 114.8(8) . . ? C53 O19 C72 118.2(8) . . ? C89 O20 C41 117.7(8) . . ? C153 C149 C150 62(3) . . ? C104 N24 C88 124.1(11) . . ? C81 N26 C25 121.8(10) . . ? C98 N30 C46 128.9(11) . . ? C74 N31 C48 126.6(10) . . ? C96 N32 C66 132.1(11) . . ? C94 N34 C39 119.3(10) . . ? C110 N45 C78 122.2(11) . . ? C82 N51 C29 128.9(11) . . ? C54 C25 C29 120.6(11) . . ? C54 C25 N26 118.6(11) . . ? C29 C25 N26 120.7(10) . . ? C59 C27 O12 120.3(10) . . ? C59 C27 C36 122.1(11) . . ? O12 C27 C36 117.5(10) . . ? C25 C29 C70 120.0(11) . . ? C25 C29 N51 116.5(10) . . ? C70 C29 N51 123.5(11) . . ? C97 C33 C69 123.0(11) . . ? C97 C33 O11 118.2(10) . . ? C69 C33 O11 118.8(10) . . ? C72 C35 C47 116.8(11) . . ? C72 C35 C55 122.3(10) . . ? C47 C35 C55 120.9(10) . . ? C43 C36 C27 115.7(11) . . ? C43 C36 C49 124.1(11) . . ? C27 C36 C49 120.1(11) . . ? C63 C37 C52 117.2(10) . . ? C63 C37 C50 122.1(10) . . ? C52 C37 C50 120.7(10) . . ? C66 C39 C71 120.4(11) . . ? C66 C39 N34 119.9(10) . . ? C71 C39 N34 119.7(11) . . ? C68 C40 C57 114.1(9) . . ? C68 C40 C75 111.0(9) . . ? C57 C40 C75 114.0(10) . . ? C60 C41 C70 122.2(11) . . ? C60 C41 O20 118.6(10) . . ? C70 C41 O20 118.7(10) . . ? C67 C42 C68 123.1(10) . . ? C67 C42 O17 119.5(10) . . ? C68 C42 O17 117.1(10) . . ? C75 C43 C36 122.9(11) . . ? C87 C44 C55 113.9(10) . . ? C78 C46 N30 119.8(11) . . ? C78 C46 C80 117.6(11) . . ? N30 C46 C80 122.6(10) . . ? C35 C47 C69 123.6(10) . . ? C88 C48 C84 121.2(11) . . ? C88 C48 N31 117.8(10) . . ? C84 C48 N31 121.0(10) . . ? C64 C49 C36 114.5(10) . . ? C64 C49 C92 113.3(10) . . ? C36 C49 C92 110.3(10) . . ? C69 C50 C61 113.2(10) . . ? C69 C50 C37 109.1(9) . . ? C61 C50 C37 112.9(9) . . ? C67 C52 C37 121.6(11) . . ? C67 C52 O14 118.2(10) . . ? C37 C52 O14 119.9(10) . . ? C65 C53 C102 120.9(11) . . ? C65 C53 O19 118.3(10) . . ? C102 C53 O19 120.4(11) . . ? C60 C54 C25 120.8(12) . . ? C35 C55 C77 110.2(9) . . ? C35 C55 C44 112.6(10) . . ? C77 C55 C44 114.6(9) . . ? C92 C56 C90 122.0(11) . . ? C92 C56 O13 120.0(10) . . ? C90 C56 O13 117.2(10) . . ? C40 C57 C105 110.7(10) . . ? C81 C58 Br3 111.0(9) . . ? C27 C59 C89 121.0(12) . . ? C54 C60 C41 118.6(11) . . ? C54 C60 O17 120.9(10) . . ? C41 C60 O17 120.2(10) . . ? C50 C61 C91 111.8(10) . . ? C77 C62 C92 122.7(11) . . ? C37 C63 C68 124.3(11) . . ? C49 C64 C111 112.9(11) . . ? C71 C65 C53 121.3(11) . . ? C71 C65 O10 119.1(10) . . ? C53 C65 O10 119.3(10) . . ? C39 C66 N32 117.6(11) . . ? C39 C66 C102 119.5(11) . . ? N32 C66 C102 122.8(11) . . ? C42 C67 C52 119.2(11) . . ? C42 C68 C63 114.7(11) . . ? C42 C68 C40 121.0(10) . . ? C63 C68 C40 124.3(11) . . ? C33 C69 C47 116.1(10) . . ? C33 C69 C50 121.5(11) . . ? C47 C69 C50 122.4(10) . . ? C29 C70 C41 117.7(12) . . ? C65 C71 C39 119.3(12) . . ? C35 C72 C97 121.9(10) . . ? C35 C72 O19 119.6(10) . . ? C97 C72 O19 118.1(9) . . ? C93 C73 C88 120.9(11) . . ? O23 C74 N31 125.2(12) . . ? O23 C74 C101 121.1(11) . . ? N31 C74 C101 113.8(11) . . ? C43 C75 C89 118.4(11) . . ? C43 C75 C40 122.5(10) . . ? C89 C75 C40 119.1(10) . . ? C93 C76 C84 119.9(10) . . ? C93 C76 O14 119.3(10) . . ? C84 C76 O14 120.6(10) . . ? C62 C77 C86 117.4(10) . . ? C62 C77 C55 122.3(10) . . ? C86 C77 C55 120.3(10) . . ? C95 C78 C46 121.4(11) . . ? C95 C78 N45 118.1(10) . . ? C46 C78 N45 120.4(10) . . ? C83 C79 C80 121.2(11) . . ? C83 C79 O13 117.7(10) . . ? C80 C79 O13 120.5(10) . . ? C79 C80 C46 119.3(11) . . ? O16 C81 N26 121.9(12) . . ? O16 C81 C58 120.5(12) . . ? N26 C81 C58 117.5(11) . . ? O21 C82 N51 125.6(12) . . ? O21 C82 C99 117.3(12) . . ? N51 C82 C99 117.0(12) . . ? C79 C83 C95 119.9(11) . . ? C79 C83 O12 119.6(10) . . ? C95 C83 O12 120.5(10) . . ? C76 C84 C48 119.4(11) . . ? C94 C85 Br6 113.7(10) . . ? C90 C86 O10 119.4(10) . . ? C90 C86 C77 121.4(10) . . ? O10 C86 C77 119.0(10) . . ? C48 C88 C73 118.4(11) . . ? C48 C88 N24 122.0(10) . . ? C73 C88 N24 119.5(10) . . ? C59 C89 O20 119.8(10) . . ? C59 C89 C75 119.6(11) . . ? O20 C89 C75 120.2(10) . . ? C86 C90 C56 119.2(11) . . ? C56 C92 C62 117.1(10) . . ? C56 C92 C49 122.0(10) . . ? C62 C92 C49 120.9(10) . . ? C76 C93 C73 120.1(11) . . ? C76 C93 O11 119.5(10) . . ? C73 C93 O11 120.4(10) . . ? O15 C94 N34 123.6(12) . . ? O15 C94 C85 119.0(12) . . ? N34 C94 C85 117.2(11) . . ? C78 C95 C83 120.4(11) . . ? O22 C96 N32 125.7(12) . . ? O22 C96 C100 114.6(12) . . ? N32 C96 C100 119.6(11) . . ? C33 C97 C72 118.3(11) . . ? O28 C98 N30 123.9(13) . . ? O28 C98 C103 121.2(12) . . ? N30 C98 C103 114.9(11) . . ? C82 C99 Br8 116.6(10) . . ? C82 C99 Br8A 106.3(9) . . ? Br8 C99 Br8A 88.4(6) . . ? C96 C100 Br2 115.3(9) . . ? C74 C101 Br5 107.1(9) . . ? C53 C102 C66 118.5(12) . . ? C98 C103 Br7 110.4(10) . . ? O18 C104 N24 122.7(12) . . ? O18 C104 C106 121.9(12) . . ? N24 C104 C106 115.0(12) . . ? C104 C106 Br1 106.4(9) . . ? C110 C107 Br4 105.1(11) . . ? O38 C110 N45 122.5(12) . . ? O38 C110 C107 122.3(14) . . ? N45 C110 C107 115.1(13) . . ? C151 C150 C149 150(2) . . ? C151 C150 C153 90.8(14) . . ? C149 C150 C153 58.8(17) . . ? C150 C151 C154 146(2) . . ? C150 C151 C152 89.2(14) . . ? C154 C151 C152 58.1(17) . . ? C153 C152 C154 147(2) . . ? C153 C152 C151 89.1(14) . . ? C154 C152 C151 58.3(17) . . ? C152 C153 C149 150(2) . . ? C152 C153 C150 90.9(14) . . ? C149 C153 C150 59.1(18) . . ? C152 C154 C151 64(3) . . ? C206 C198 C205 112(5) . . ? C204 C199 C205 50(3) . . ? C204 C199 C201 51(3) . . ? C205 C199 C201 81(4) . . ? C204 C199 C202 78(3) . . ? C205 C199 C202 82(3) . . ? C201 C199 C202 34.4(17) . . ? C202 C201 C200 121(4) . . ? C202 C201 C204 105(4) . . ? C200 C201 C204 103(3) . . ? C202 C201 C199 74(3) . . ? C200 C201 C199 94(3) . . ? C204 C201 C199 43(2) . . ? C201 C202 C203 153(5) . . ? C201 C202 C199 72(3) . . ? C203 C202 C199 81(3) . . ? C202 C203 Br8A 163(4) . . ? C199 C204 C205 82(4) . . ? C199 C204 C201 86(4) . . ? C205 C204 C201 112(4) . . ? C204 C205 C199 48(3) . . ? C204 C205 C198 118(5) . . ? C199 C205 C198 77(4) . . ? C208 C207 C209 115(3) . . ? C208 C208 C207 118(5) 2_766 . ? _diffrn_measured_fraction_theta_max 0.896 _diffrn_reflns_theta_full 49.35 _diffrn_measured_fraction_theta_full 0.896 _refine_diff_density_max 2.622 _refine_diff_density_min -1.329 _refine_diff_density_rms 0.189 #===END data_pphos _publ_requested_journal ; Journal of the American Chemical Society ; _publ_contact_author ; Julius Rebek, Jr. Skaggs Institute for Chemical Biology (MB26) The Scripps Research Institute 10550 N. Torrey Pines Road La Jolla, CA 92037 ; _publ_contact_author_phone '858-784-2250' _publ_contact_author_fax '858-784-2876' _publ_contact_author_email 'jrebek@scripps.edu' loop_ _publ_author_name _publ_author_address 'Alexandr Shivanyuk' ; Skaggs Institute for Chemical Biology (MB26) The Scripps Research Institute 10550 N. Torrey Pines Road La Jolla, CA 92037 ; 'Patrick Amrhein' ; Skaggs Institute for Chemical Biology (MB26) The Scripps Research Institute 10550 N. Torrey Pines Road La Jolla, CA 92037 ; 'Darren W. Johnson' ; Skaggs Institute for Chemical Biology (MB26) The Scripps Research Institute 10550 N. Torrey Pines Road La Jolla, CA 92037 ; _publ_section_title ; Metal Switching and Self-Inclusion of Functional Cavitands ; _publ_section_references ; Altomare, A., Burla, M. C., Camalli, M., Cascarano, M., Giacovazzo, C., Guagliardi, A., Polidori, G. (1993). J. Appl. Cryst., 26, 343-350. Siemens Industrial Automation, Inc. (1995). SMART. Area Detector Software Package, Madison, WI, USA. Siemens Industrial Automation, Inc. (1995). SAINT. SAX Area Detector Integration Program (v. 4.024), Madison, WI, USA. Siemens Industrial Automation, Inc. (1993). SHELXL. SHELXTL Crystal Structure Determination Software Package, Madison, WI, USA. ; _audit_creation_method SHELXL-97 _computing_cell_refinement ; SMART (Siemens, 1995), SAINT (Siemens, 1995) ; _computing_data_reduction ; SAINT (Siemens, 1995), XPREP (Siemens, 1995) ; _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #-------------------------------------------------------------- _cell_length_a 19.817(4) _cell_length_b 29.334(6) _cell_length_c 17.757(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.94(3) _cell_angle_gamma 90.00 _cell_volume 10060(4) _cell_formula_units_Z 4 _cell_measurement_temperature 119(2) _cell_measurement_reflns_used 11540 _cell_measurement_theta_min 3.38 _cell_measurement_theta_max 44.49 #-------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' #-------------------------------------------------------------- _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.165 _exptl_crystal_F_000 3617 _exptl_absorpt_coefficient_mu 1.011 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.725 _exptl_absorpt_correction_T_max 0.963 _chemical_formula_sum 'C94.25 H48 N8 O25.60 P2' _chemical_formula_weight 1763.95 _exptl_special_details ; ? ; #-------------------------------------------------------------- _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_detector 'CCD area detector' _diffrn_measurement_device_type '3 circle diffractometer' _diffrn_measurement_method ; omega scans with profile analysis ; _diffrn_reflns_number 11540 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 44.49 _reflns_number_total 3523 _reflns_number_gt 2976 _reflns_threshold_expression >2sigma(I) _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^)+(0.2000P)^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_number_reflns 3523 _refine_ls_number_parameters 589 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1515 _refine_ls_R_factor_gt 0.1418 _refine_ls_wR_factor_ref 0.4256 _refine_ls_wR_factor_gt 0.4085 _refine_ls_goodness_of_fit_ref 2.035 _refine_ls_restrained_S_all 2.035 _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 O1 O -0.8087(3) 0.8744(2) -0.0377(4) 0.0955(18) Uani 1 1 d . . . O2 O -1.1632(3) 0.8860(2) -0.0656(3) 0.0889(17) Uani 1 1 d . . . O3 O -0.9177(3) 0.8783(2) 0.0340(3) 0.1048(19) Uani 1 1 d . . . O4 O -0.7567(3) 0.88675(19) -0.2862(3) 0.0923(18) Uani 1 1 d . . . C5 C -0.9265(4) 0.7983(4) 0.0291(5) 0.087(3) Uani 1 1 d . . . H5A H -0.9604 0.8001 0.0577 0.104 Uiso 1 1 calc R . . O6 O -1.0823(4) 0.7290(2) 0.0125(4) 0.129(2) Uani 1 1 d . . . N7 N -0.8375(4) 0.7093(3) -0.0595(6) 0.102(2) Uani 1 1 d . . . H7A H -0.8483 0.6870 -0.0330 0.122 Uiso 1 1 calc R . . C8 C -1.1859(4) 0.8455(3) -0.1014(6) 0.083(2) Uani 1 1 d . . . C9 C -1.1741(4) 0.8049(3) -0.0591(5) 0.086(2) Uani 1 1 d . . . H9A H -1.1481 0.8051 -0.0086 0.104 Uiso 1 1 calc R . . C10 C -0.7872(4) 0.8787(3) -0.1638(7) 0.087(3) Uani 1 1 d . . . H10A H -0.7586 0.8533 -0.1529 0.104 Uiso 1 1 calc R . . C11 C -1.0973(5) 0.9011(3) -0.0689(5) 0.082(2) Uani 1 1 d . . . C12 C -1.0915(5) 0.9378(3) -0.1150(5) 0.090(2) Uani 1 1 d . . . C13 C -1.2011(4) 0.7648(4) -0.0924(7) 0.102(3) Uani 1 1 d . . . N14 N -0.9394(4) 0.7164(3) 0.0285(5) 0.113(3) Uani 1 1 d . . . H14A H -0.9828 0.7127 0.0088 0.135 Uiso 1 1 calc R . . N15 N -1.2652(5) 0.7241(3) -0.2082(5) 0.123(3) Uani 1 1 d . . . H15A H -1.2512 0.7162 -0.2488 0.148 Uiso 1 1 calc R . . C16 C -0.8538(5) 0.7525(4) -0.0370(5) 0.091(3) Uani 1 1 d . . . C17 C -0.8230(4) 0.7917(4) -0.0522(5) 0.091(3) Uani 1 1 d . . . H17A H -0.7874 0.7903 -0.0784 0.109 Uiso 1 1 calc R . . C18 C -0.8380(5) 0.9389(3) -0.2526(6) 0.092(3) Uani 1 1 d . . . C19 C -0.8613(5) 0.9343(4) -0.1233(7) 0.100(3) Uani 1 1 d . . . C20 C -0.7952(4) 0.8998(3) -0.2323(6) 0.081(2) Uani 1 1 d . . . O21 O -1.3306(4) 0.7005(3) -0.1229(6) 0.138(3) Uani 1 1 d . . . C22 C -0.9651(5) 0.9348(3) -0.0636(6) 0.095(3) Uani 1 1 d . . . C23 C -0.8969(5) 0.8365(4) 0.0088(5) 0.083(2) Uani 1 1 d . . . C24 C -1.0399(5) 0.8811(3) -0.0190(4) 0.080(2) Uani 1 1 d . . . H24A H -1.0458 0.8569 0.0127 0.095 Uiso 1 1 calc R . . C25 C -0.8918(5) 0.9533(3) -0.0587(5) 0.103(3) Uani 1 1 d . . . H25A H -0.8627 0.9424 -0.0099 0.124 Uiso 1 1 calc R . . C26 C -0.9758(6) 0.8978(3) -0.0176(5) 0.093(3) Uani 1 1 d . . . O27 O -0.7858(4) 0.7258(3) -0.1550(5) 0.143(3) Uani 1 1 d . . . C28 C -0.9058(5) 0.7565(4) 0.0068(6) 0.102(3) Uani 1 1 d . . . C29 C -1.2517(4) 0.8054(4) -0.2091(5) 0.092(3) Uani 1 1 d . . . H29A H -1.2792 0.8057 -0.2590 0.110 Uiso 1 1 calc R . . N30 N -1.1946(4) 0.7230(3) -0.0499(5) 0.101(2) Uani 1 1 d . . . H30A H -1.2303 0.7055 -0.0577 0.121 Uiso 1 1 calc R . . C31 C -0.8697(4) 0.9542(3) -0.1949(7) 0.087(2) Uani 1 1 d . . . H31A H -0.8984 0.9796 -0.2054 0.105 Uiso 1 1 calc R . . C32 C -1.2396(5) 0.7648(4) -0.1707(6) 0.097(3) Uani 1 1 d . . . C33 C -1.1508(5) 0.9605(2) -0.1689(5) 0.097(3) Uani 1 1 d . . . H33B H -1.1920 0.9531 -0.1493 0.117 Uiso 1 1 calc R . . C34 C -1.2250(4) 0.8450(3) -0.1769(5) 0.079(2) Uani 1 1 d . . . C35 C -1.0235(7) 0.9531(3) -0.1102(5) 0.107(3) Uani 1 1 d . . . H35A H -1.0175 0.9777 -0.1411 0.128 Uiso 1 1 calc R . . C36 C -0.8213(5) 0.8948(4) -0.1098(6) 0.090(3) Uani 1 1 d . . . C37 C -0.8442(5) 0.8348(4) -0.0289(5) 0.092(3) Uani 1 1 d . . . O38 O -0.8430(4) 0.6805(3) 0.0920(5) 0.194(4) Uani 1 1 d . . . C39 C -0.8073(6) 0.6976(3) -0.1168(8) 0.100(3) Uani 1 1 d . . . C40 C -0.9509(6) 0.6474(4) 0.0982(8) 0.151(4) Uiso 1 1 d . . . C41 C -1.2152(8) 1.0339(4) -0.2077(9) 0.186(6) Uani 1 1 d . . . H41A H -1.2098 1.0665 -0.2045 0.279 Uiso 1 1 calc R . . H41B H -1.2505 1.0248 -0.1817 0.279 Uiso 1 1 calc R . . H41C H -1.2282 1.0250 -0.2610 0.279 Uiso 1 1 calc R . . C42 C -0.8905(6) 1.0061(3) -0.0562(6) 0.126(4) Uani 1 1 d . . . H42A H -0.9167 1.0180 -0.1050 0.151 Uiso 1 1 calc R . . H42B H -0.9123 1.0166 -0.0157 0.151 Uiso 1 1 calc R . . C43 C -1.1470(6) 1.0112(3) -0.1697(7) 0.143(4) Uani 1 1 d . . . H43A H -1.1118 1.0203 -0.1969 0.171 Uiso 1 1 calc R . . H43B H -1.1326 1.0221 -0.1169 0.171 Uiso 1 1 calc R . . C44 C -0.7977(4) 0.6496(3) -0.1306(6) 0.114(3) Uiso 1 1 d . . . C45 C -0.9066(6) 0.6849(4) 0.0777(7) 0.134(4) Uani 1 1 d . . . C47 C -1.1397(7) 0.7090(3) -0.0005(8) 0.121(4) Uani 1 1 d . . . C48 C -1.1465(6) 0.6680(4) 0.0451(7) 0.142(4) Uiso 1 1 d . . . C49 C -1.3113(7) 0.6964(4) -0.1832(10) 0.146(4) Uani 1 1 d . . . C51 C -0.8167(6) 1.0241(4) -0.0413(7) 0.162(5) Uani 1 1 d . . . H51A H -0.8174 1.0568 -0.0430 0.243 Uiso 1 1 calc R . . H51B H -0.7943 1.0126 -0.0802 0.243 Uiso 1 1 calc R . . H51C H -0.7916 1.0142 0.0087 0.243 Uiso 1 1 calc R . . C59 C -1.3433(7) 0.6572(5) -0.2464(9) 0.180(5) Uiso 1 1 d . . . C80 C -1.5144(11) 0.7499(7) -0.2830(13) 0.112(7) Uiso 0.38 1 d PD . . C100 C -0.9723(8) 0.8392(5) -0.2793(9) 0.168(5) Uiso 1 1 d . . . C101 C -0.9641(9) 0.7999(6) -0.3179(12) 0.206(6) Uiso 1 1 d . . . C102 C -0.975(2) 0.7695(15) -0.280(3) 0.240(16) Uiso 0.50 1 d P . . C103 C -1.0000 0.855(2) -0.2500 0.21(2) Uiso 0.50 2 d SP . . C310 C -1.3956(9) 0.6261(6) -0.2197(11) 0.157(5) Uiso 0.75 1 d P . . P310 P -1.4279(5) 0.6592(4) -0.2215(7) 0.118(3) Uiso 0.25 1 d P . . O310 O -1.463(2) 0.7146(14) -0.275(3) 0.236(18) Uiso 0.25 1 d PD . . C311 C -1.543(2) 0.7941(14) -0.253(3) 0.150(15) Uiso 0.25 1 d PD . . O311 O -1.4568(13) 0.6552(9) -0.1502(17) 0.137(8) Uiso 0.25 1 d P . . O312 O -1.4375(15) 0.6202(9) -0.2751(19) 0.140(8) Uiso 0.25 1 d P . . C312 C -1.4683(18) 0.5716(13) -0.251(3) 0.135(13) Uiso 0.25 1 d P . . C320 C -1.1791(14) 0.6324(7) 0.0145(16) 0.189(8) Uiso 0.75 1 d P . . P320 P -1.1465(8) 0.6288(4) -0.0085(9) 0.133(4) Uiso 0.25 1 d P . . O320 O -1.2069(12) 0.6259(7) -0.0454(16) 0.110(6) Uiso 0.25 1 d P . . O321 O -1.1209(14) 0.5887(9) 0.0437(18) 0.143(8) Uiso 0.25 1 d PD . . O322 O -1.082(3) 0.6310(15) -0.037(3) 0.234(17) Uiso 0.25 1 d P . . C322 C -1.009(2) 0.6217(13) -0.029(3) 0.136(12) Uiso 0.25 1 d P . . C323 C -1.162(3) 0.582(3) 0.107(3) 0.26(3) Uiso 0.25 1 d PD . . C324 C -1.126(2) 0.5519(15) 0.177(3) 0.141(13) Uiso 0.25 1 d PD . . C330 C -0.8287(12) 0.6195(7) -0.0991(14) 0.194(7) Uiso 0.75 1 d P . . P330 P -0.8502(7) 0.6359(4) -0.2195(9) 0.144(4) Uiso 0.25 1 d P . . O330 O -0.913(2) 0.6663(12) -0.237(3) 0.196(13) Uiso 0.25 1 d P . . O331 O -0.809(2) 0.6356(14) -0.286(3) 0.210(15) Uiso 0.25 1 d P . . C331 C -0.919(2) 0.7151(15) -0.285(3) 0.144(14) Uiso 0.25 1 d P . . C332 C -0.960(2) 0.7347(14) -0.321(3) 0.129(12) Uiso 0.25 1 d P . . O332 O -0.8746(17) 0.5940(12) -0.208(2) 0.179(12) Uiso 0.25 1 d P . . C333 C -0.910(2) 0.5646(15) -0.275(3) 0.140(13) Uiso 0.25 1 d PD . . C335 C -0.8861(14) 0.6083(8) -0.1256(16) 0.162(8) Uiso 0.50 1 d PD . . C336 C -0.892(13) 0.516(4) -0.245(15) 0.56(13) Uiso 0.25 1 d PD . . C340 C -0.9109(19) 0.6349(13) 0.195(2) 0.169(12) Uiso 0.38 1 d P . . P340 P -0.9439(12) 0.6059(8) 0.0316(15) 0.233(8) Uiso 0.25 1 d PD . . O341 O -0.901(3) 0.615(2) -0.043(2) 0.29(2) Uiso 0.25 1 d PD . . C341 C -0.9759(14) 0.6467(9) 0.1880(17) 0.131(8) Uiso 0.38 1 d P . . C342 C -0.9125(17) 0.6094(13) 0.149(2) 0.107(10) Uiso 0.25 1 d PD . . O342 O -0.908(7) 0.568(2) 0.098(3) 0.50(7) Uiso 0.25 1 d PD . . O400 O -0.851(2) 0.5209(14) 0.083(3) 0.371(19) Uiso 0.50 1 d P . . O401 O -1.5582(8) 0.7642(6) -0.2175(9) 0.212(5) Uiso 0.75 1 d P . . O402 O -1.1141(16) 0.5218(11) 0.127(2) 0.297(13) Uiso 0.50 1 d P . . O403 O -0.929(3) 0.6443(16) -0.345(3) 0.275(19) Uiso 0.30 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.104(4) 0.123(5) 0.064(5) -0.026(3) 0.029(3) -0.024(4) O2 0.112(5) 0.090(4) 0.074(4) -0.015(3) 0.040(3) 0.012(3) O3 0.119(4) 0.132(5) 0.068(4) -0.029(4) 0.030(4) -0.018(4) O4 0.105(4) 0.103(4) 0.076(4) -0.013(3) 0.036(3) -0.025(3) C5 0.081(5) 0.103(8) 0.074(6) -0.002(5) 0.014(4) 0.007(6) O6 0.093(4) 0.142(5) 0.170(7) 0.054(4) 0.071(4) 0.030(4) N7 0.104(5) 0.108(7) 0.094(7) -0.002(5) 0.025(5) 0.010(4) C8 0.094(5) 0.087(7) 0.084(8) 0.021(6) 0.053(5) 0.017(5) C9 0.087(5) 0.095(7) 0.088(7) -0.017(6) 0.042(4) 0.006(5) C10 0.102(6) 0.094(6) 0.064(7) -0.011(6) 0.017(6) -0.015(4) C11 0.103(7) 0.083(6) 0.072(6) -0.025(5) 0.043(6) 0.003(5) C12 0.116(8) 0.085(7) 0.078(7) -0.019(5) 0.040(6) 0.002(6) C13 0.091(6) 0.117(9) 0.109(9) 0.032(8) 0.043(6) 0.016(5) N14 0.090(4) 0.126(6) 0.119(7) 0.041(5) 0.018(5) 0.032(5) N15 0.160(7) 0.115(6) 0.114(7) 0.003(5) 0.072(5) -0.033(5) C16 0.076(6) 0.127(10) 0.075(7) 0.014(6) 0.024(5) 0.000(6) C17 0.081(5) 0.140(9) 0.054(6) -0.008(6) 0.021(4) -0.003(6) C18 0.130(7) 0.071(6) 0.081(8) -0.005(6) 0.034(6) -0.036(5) C19 0.106(6) 0.087(7) 0.112(10) -0.033(7) 0.034(6) -0.025(5) C20 0.100(5) 0.098(7) 0.060(7) -0.025(6) 0.049(5) -0.018(5) O21 0.137(5) 0.184(7) 0.101(6) 0.019(5) 0.042(5) -0.012(4) C22 0.143(9) 0.078(6) 0.073(6) -0.022(5) 0.041(6) 0.000(6) C23 0.101(7) 0.099(8) 0.046(5) -0.012(5) 0.013(5) -0.002(6) C24 0.101(7) 0.086(5) 0.062(6) -0.021(4) 0.039(5) -0.003(5) C25 0.128(7) 0.108(7) 0.088(7) -0.043(5) 0.054(6) -0.027(5) C26 0.118(8) 0.110(7) 0.049(6) -0.026(5) 0.016(6) 0.019(6) O27 0.192(7) 0.126(6) 0.124(6) 0.015(5) 0.061(5) 0.032(5) C28 0.092(7) 0.127(10) 0.078(7) 0.038(6) 0.002(6) -0.007(6) C29 0.119(6) 0.098(8) 0.069(6) 0.016(6) 0.045(5) -0.001(6) N30 0.101(5) 0.103(6) 0.111(6) 0.026(5) 0.049(5) 0.022(4) C31 0.133(7) 0.071(5) 0.068(7) -0.014(5) 0.046(6) -0.017(4) C32 0.123(7) 0.090(8) 0.089(8) -0.010(7) 0.048(6) -0.012(5) C33 0.143(7) 0.058(6) 0.102(8) 0.009(5) 0.053(6) 0.028(4) C34 0.096(5) 0.092(7) 0.062(7) 0.011(6) 0.048(5) 0.004(5) C35 0.184(11) 0.063(5) 0.083(7) -0.021(4) 0.050(8) 0.025(7) C36 0.112(6) 0.115(8) 0.050(8) -0.028(6) 0.030(6) -0.034(6) C37 0.083(6) 0.137(10) 0.055(6) -0.023(5) 0.016(5) -0.011(6) O38 0.112(6) 0.271(9) 0.209(9) 0.152(8) 0.059(5) 0.049(5) C39 0.120(7) 0.093(7) 0.080(8) 0.004(6) 0.009(6) 0.019(6) C41 0.221(13) 0.124(8) 0.233(15) 0.047(9) 0.092(11) 0.079(9) C42 0.187(9) 0.088(7) 0.128(9) -0.053(5) 0.087(7) -0.042(6) C43 0.204(11) 0.111(9) 0.133(10) 0.002(6) 0.080(8) 0.038(7) C45 0.086(7) 0.183(9) 0.146(10) 0.057(8) 0.054(6) 0.006(7) C47 0.119(9) 0.108(7) 0.170(11) 0.050(7) 0.104(8) 0.032(7) C49 0.162(11) 0.151(10) 0.123(12) -0.021(9) 0.027(9) -0.009(8) C51 0.203(11) 0.134(8) 0.168(11) -0.080(8) 0.080(9) -0.072(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C37 1.383(10) . ? O1 C36 1.386(10) . ? O2 C8 1.375(10) . ? O2 C11 1.394(10) . ? O3 C23 1.398(9) . ? O3 C26 1.421(10) . ? O4 C34 1.399(9) 2_354 ? O4 C20 1.404(9) . ? C5 C23 1.352(11) . ? C5 C28 1.377(12) . ? O6 C47 1.254(12) . ? N7 C39 1.335(13) . ? N7 C16 1.390(11) . ? C8 C34 1.389(12) . ? C8 C9 1.398(11) . ? C9 C13 1.371(12) . ? C10 C20 1.341(11) . ? C10 C36 1.374(12) . ? C11 C12 1.373(11) . ? C11 C24 1.404(11) . ? C12 C35 1.406(13) . ? C12 C33 1.494(12) . ? C13 C32 1.428(13) . ? C13 N30 1.429(11) . ? N14 C45 1.336(12) . ? N14 C28 1.447(11) . ? N15 C49 1.369(18) . ? N15 C32 1.406(12) . ? C16 C17 1.356(12) . ? C16 C28 1.428(13) . ? C17 C37 1.423(12) . ? C18 C31 1.391(11) . ? C18 C20 1.425(12) . ? C18 C33 1.502(12) 2_354 ? C19 C31 1.376(12) . ? C19 C36 1.393(12) . ? C19 C25 1.516(12) . ? O21 C49 1.222(16) . ? C22 C35 1.371(12) . ? C22 C26 1.403(13) . ? C22 C25 1.536(12) . ? C23 C37 1.362(11) . ? C24 C26 1.356(11) . ? C25 C42 1.550(12) . ? O27 C39 1.206(11) . ? C29 C34 1.350(11) . ? C29 C32 1.366(12) . ? N30 C47 1.301(13) . ? C33 C43 1.489(12) . ? C33 C18 1.502(12) 2_354 ? C34 O4 1.399(9) 2_354 ? O38 C45 1.234(11) . ? C39 C44 1.450(13) . ? C40 C45 1.503(15) . ? C40 C342 1.53(4) . ? C40 P340 1.72(3) . ? C40 C340 1.77(4) . ? C40 C341 1.77(3) . ? C41 C43 1.523(17) . ? C42 C51 1.521(14) . ? C44 C330 1.27(2) . ? C44 P330 1.733(17) . ? C47 C48 1.474(14) . ? C47 P320 2.359(15) . ? C48 C320 1.28(2) . ? C48 P320 1.491(19) . ? C49 C59 1.633(19) . ? C59 C310 1.53(2) . ? C59 P310 1.829(19) . ? C80 C80 1.18(4) 2_254 ? C80 O310 1.43(2) . ? C80 O401 1.50(3) 2_254 ? C80 C311 1.56(2) . ? C80 O310 1.59(5) 2_254 ? C80 O401 1.65(3) . ? C80 C311 1.75(4) 2_254 ? C100 C103 0.96(3) . ? C100 C101 1.369(19) . ? C100 C100 1.67(4) 2_354 ? C101 C102 1.16(4) . ? C101 C332 1.92(5) . ? C102 C332 1.32(5) . ? C102 C102 1.62(8) 2_354 ? C102 C331 1.96(6) . ? C103 C100 0.96(3) 2_354 ? C310 O312 1.15(3) . ? C310 P310 1.160(16) . ? P310 O312 1.47(3) . ? P310 O311 1.51(3) . ? P310 O310 1.93(4) . ? O310 O401 1.53(4) 2_254 ? O310 C80 1.59(5) 2_254 ? C311 O401 1.15(5) . ? C311 C311 1.70(9) 2_254 ? C311 C80 1.75(4) 2_254 ? O312 C312 1.64(5) . ? C312 C312 1.27(7) 2_254 ? C320 P320 0.85(3) . ? C320 O320 1.10(3) . ? C320 O321 1.72(4) . ? P320 O320 1.23(3) . ? P320 O322 1.48(5) . ? P320 O321 1.51(3) . ? O321 C323 1.55(2) . ? O322 C322 1.45(6) . ? C322 P340 1.55(5) . ? C323 C324 1.55(2) . ? C324 O402 1.31(5) . ? C330 C335 1.18(3) . ? C330 O341 1.92(5) . ? C330 P330 2.14(3) . ? P330 O332 1.36(4) . ? P330 O330 1.51(4) . ? P330 O331 1.58(5) . ? P330 C335 2.12(3) . ? O330 C331 1.66(6) . ? C331 C332 1.08(5) . ? O332 C333 1.52(5) . ? O332 C335 1.58(4) . ? C333 C336 1.55(2) . ? C335 O341 1.58(2) . ? C340 C342 1.11(4) . ? C340 C341 1.31(4) . ? P340 O342 1.68(3) . ? P340 O341 1.75(3) . ? P340 C342 2.04(5) . ? C341 C342 1.91(5) . ? C342 O342 1.54(5) . ? O401 C80 1.50(3) 2_254 ? O401 O310 1.53(4) 2_254 ? 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 C37 O1 C36 118.5(5) . . ? C8 O2 C11 118.0(5) . . ? C23 O3 C26 113.6(5) . . ? C34 O4 C20 115.8(5) 2_354 . ? C23 C5 C28 119.0(9) . . ? C39 N7 C16 128.8(9) . . ? O2 C8 C34 120.6(8) . . ? O2 C8 C9 119.3(9) . . ? C34 C8 C9 119.9(9) . . ? C13 C9 C8 119.8(10) . . ? C20 C10 C36 119.8(9) . . ? C12 C11 O2 118.6(9) . . ? C12 C11 C24 122.7(8) . . ? O2 C11 C24 118.3(9) . . ? C11 C12 C35 114.9(8) . . ? C11 C12 C33 124.9(9) . . ? C35 C12 C33 120.2(10) . . ? C9 C13 C32 119.4(8) . . ? C9 C13 N30 121.8(11) . . ? C32 C13 N30 118.7(10) . . ? C45 N14 C28 123.5(7) . . ? C49 N15 C32 123.2(9) . . ? C17 C16 N7 124.9(11) . . ? C17 C16 C28 116.7(10) . . ? N7 C16 C28 118.4(11) . . ? C16 C17 C37 121.4(10) . . ? C31 C18 C20 114.5(8) . . ? C31 C18 C33 123.4(10) . 2_354 ? C20 C18 C33 122.1(10) . 2_354 ? C31 C19 C36 117.3(9) . . ? C31 C19 C25 123.8(10) . . ? C36 C19 C25 118.9(11) . . ? C10 C20 O4 121.4(9) . . ? C10 C20 C18 122.9(8) . . ? O4 C20 C18 115.5(9) . . ? C35 C22 C26 116.0(9) . . ? C35 C22 C25 123.7(11) . . ? C26 C22 C25 120.3(10) . . ? C5 C23 C37 121.8(9) . . ? C5 C23 O3 117.7(10) . . ? C37 C23 O3 120.2(10) . . ? C26 C24 C11 119.0(8) . . ? C19 C25 C22 111.1(6) . . ? C19 C25 C42 112.5(8) . . ? C22 C25 C42 111.3(8) . . ? C24 C26 C22 122.0(8) . . ? C24 C26 O3 119.1(10) . . ? C22 C26 O3 118.8(10) . . ? C5 C28 C16 121.9(9) . . ? C5 C28 N14 117.5(11) . . ? C16 C28 N14 120.6(11) . . ? C34 C29 C32 121.9(9) . . ? C47 N30 C13 126.1(8) . . ? C19 C31 C18 124.2(9) . . ? C29 C32 N15 119.9(10) . . ? C29 C32 C13 118.9(8) . . ? N15 C32 C13 121.2(10) . . ? C43 C33 C12 114.6(8) . . ? C43 C33 C18 114.2(7) . 2_354 ? C12 C33 C18 109.7(6) . 2_354 ? C29 C34 C8 120.0(8) . . ? C29 C34 O4 121.2(9) . 2_354 ? C8 C34 O4 118.2(8) . 2_354 ? C22 C35 C12 125.4(9) . . ? C10 C36 O1 118.8(10) . . ? C10 C36 C19 121.0(9) . . ? O1 C36 C19 119.7(10) . . ? C23 C37 O1 119.3(10) . . ? C23 C37 C17 118.9(9) . . ? O1 C37 C17 121.5(10) . . ? O27 C39 N7 121.9(9) . . ? O27 C39 C44 119.7(13) . . ? N7 C39 C44 118.4(11) . . ? C45 C40 C342 116.0(15) . . ? C45 C40 P340 102.2(12) . . ? C342 C40 P340 78(2) . . ? C45 C40 C340 103.3(14) . . ? C342 C40 C340 38.4(16) . . ? P340 C40 C340 115.9(17) . . ? C45 C40 C341 121.5(12) . . ? C342 C40 C341 70.2(19) . . ? P340 C40 C341 133.7(14) . . ? C340 C40 C341 43.5(14) . . ? C51 C42 C25 111.2(9) . . ? C33 C43 C41 113.6(10) . . ? C330 C44 C39 120.4(14) . . ? C330 C44 P330 89.3(13) . . ? C39 C44 P330 107.7(7) . . ? O38 C45 N14 122.1(8) . . ? O38 C45 C40 119.8(11) . . ? N14 C45 C40 116.1(10) . . ? O6 C47 N30 124.3(8) . . ? O6 C47 C48 118.1(12) . . ? N30 C47 C48 117.6(11) . . ? O6 C47 P320 120.9(8) . . ? N30 C47 P320 104.3(9) . . ? C48 C47 P320 37.6(7) . . ? C320 C48 C47 122.1(16) . . ? C320 C48 P320 34.5(12) . . ? C47 C48 P320 105.4(11) . . ? O21 C49 N15 126.1(11) . . ? O21 C49 C59 121.5(15) . . ? N15 C49 C59 112.3(15) . . ? C310 C59 C49 113.1(14) . . ? C310 C59 P310 39.1(7) . . ? C49 C59 P310 92.6(11) . . ? C80 C80 O310 74(3) 2_254 . ? C80 C80 O401 75(2) 2_254 2_254 ? O310 C80 O401 63(2) . 2_254 ? C80 C80 C311 78(2) 2_254 . ? O310 C80 C311 151(3) . . ? O401 C80 C311 101(2) 2_254 . ? C80 C80 O310 60.1(19) 2_254 2_254 ? O310 C80 O310 76(4) . 2_254 ? O401 C80 O310 126(2) 2_254 2_254 ? C311 C80 O310 98(3) . 2_254 ? C80 C80 O401 61(2) 2_254 . ? O310 C80 O401 126(3) . . ? O401 C80 O401 125.5(16) 2_254 . ? C311 C80 O401 42(2) . . ? O310 C80 O401 56.2(19) 2_254 . ? C80 C80 C311 60.7(18) 2_254 2_254 ? O310 C80 C311 96(3) . 2_254 ? O401 C80 C311 40.7(17) 2_254 2_254 ? C311 C80 C311 61(4) . 2_254 ? O310 C80 C311 120(3) 2_254 2_254 ? O401 C80 C311 88(2) . 2_254 ? C103 C100 C101 146(4) . . ? C103 C100 C100 29(4) . 2_354 ? C101 C100 C100 118.7(12) . 2_354 ? C102 C101 C100 107(3) . . ? C102 C101 C332 43(2) . . ? C100 C101 C332 150(2) . . ? C101 C102 C332 101(4) . . ? C101 C102 C102 127(3) . 2_354 ? C332 C102 C102 127(3) . 2_354 ? C101 C102 C331 115(3) . . ? C332 C102 C331 32(2) . . ? C102 C102 C331 118(3) 2_354 . ? C100 C103 C100 122(7) 2_354 . ? O312 C310 P310 79.2(19) . . ? O312 C310 C59 104(2) . . ? P310 C310 C59 84.3(13) . . ? C310 P310 O312 50.1(12) . . ? C310 P310 O311 102.9(16) . . ? O312 P310 O311 117.6(16) . . ? C310 P310 C59 56.5(11) . . ? O312 P310 C59 79.1(13) . . ? O311 P310 C59 138.0(13) . . ? C310 P310 O310 149(2) . . ? O312 P310 O310 111(2) . . ? O311 P310 O310 108.3(18) . . ? C59 P310 O310 99.2(15) . . ? C80 O310 O401 60.6(18) . 2_254 ? C80 O310 C80 45.7(18) . 2_254 ? O401 O310 C80 64.0(17) 2_254 2_254 ? C80 O310 P310 146(4) . . ? O401 O310 P310 140(3) 2_254 . ? C80 O310 P310 111(3) 2_254 . ? O401 C311 C80 73(2) . . ? O401 C311 C311 110(4) . 2_254 ? C80 C311 C311 65(2) . 2_254 ? O401 C311 C80 57.8(19) . 2_254 ? C80 C311 C80 41.4(16) . 2_254 ? C311 C311 C80 53.8(18) 2_254 2_254 ? C310 O312 P310 50.7(15) . . ? C310 O312 C312 99(3) . . ? P310 O312 C312 121(3) . . ? C312 C312 O312 115.9(19) 2_254 . ? P320 C320 O320 77(3) . . ? P320 C320 C48 86(2) . . ? O320 C320 C48 130(3) . . ? P320 C320 O321 61(2) . . ? O320 C320 O321 109(3) . . ? C48 C320 O321 103.8(19) . . ? C320 P320 O320 61(2) . . ? C320 P320 O322 167(3) . . ? O320 P320 O322 129(3) . . ? C320 P320 C48 59(2) . . ? O320 P320 C48 104.7(15) . . ? O322 P320 C48 108(2) . . ? C320 P320 O321 89(2) . . ? O320 P320 O321 115.1(16) . . ? O322 P320 O321 93(2) . . ? C48 P320 O321 104.9(16) . . ? C320 P320 C47 83.5(19) . . ? O320 P320 C47 97.8(12) . . ? O322 P320 C47 86.3(18) . . ? C48 P320 C47 37.0(6) . . ? O321 P320 C47 137.1(14) . . ? C320 O320 P320 42.0(17) . . ? P320 O321 C323 113(3) . . ? P320 O321 C320 29.4(11) . . ? C323 O321 C320 84(2) . . ? C322 O322 P320 152(4) . . ? O322 C322 P340 141(4) . . ? O321 C323 C324 115(4) . . ? O402 C324 C323 88(4) . . ? C335 C330 C44 122(2) . . ? C335 C330 O341 55.0(19) . . ? C44 C330 O341 139(2) . . ? C335 C330 P330 72.8(18) . . ? C44 C330 P330 54.1(11) . . ? O341 C330 P330 122(2) . . ? O332 P330 O330 105(2) . . ? O332 P330 O331 112(2) . . ? O330 P330 O331 113(2) . . ? O332 P330 C44 103.3(18) . . ? O330 P330 C44 110.6(18) . . ? O331 P330 C44 112.2(17) . . ? O332 P330 C335 48.3(18) . . ? O330 P330 C335 89(2) . . ? O331 P330 C335 155.3(18) . . ? C44 P330 C335 67.0(10) . . ? O332 P330 C330 68.8(19) . . ? O330 P330 C330 108(2) . . ? O331 P330 C330 136.5(18) . . ? C44 P330 C330 36.5(7) . . ? C335 P330 C330 32.1(8) . . ? P330 O330 C331 125(3) . . ? C332 C331 O330 135(5) . . ? C332 C331 C102 40(3) . . ? O330 C331 C102 130(4) . . ? C331 C332 C102 109(5) . . ? C331 C332 C101 123(4) . . ? C102 C332 C101 37(2) . . ? P330 O332 C333 121(3) . . ? P330 O332 C335 92(2) . . ? C333 O332 C335 138(3) . . ? O332 C333 C336 103(10) . . ? C330 C335 O341 87(3) . . ? C330 C335 O332 97(3) . . ? O341 C335 O332 172(3) . . ? C330 C335 P330 75.1(19) . . ? O341 C335 P330 148(3) . . ? O332 C335 P330 39.8(15) . . ? C342 C340 C341 104(4) . . ? C342 C340 C40 59(3) . . ? C341 C340 C40 68(2) . . ? C322 P340 O342 148(5) . . ? C322 P340 C40 95(2) . . ? O342 P340 C40 94(3) . . ? C322 P340 O341 84(3) . . ? O342 P340 O341 116(5) . . ? C40 P340 O341 122(2) . . ? C322 P340 C342 135(2) . . ? O342 P340 C342 48(2) . . ? C40 P340 C342 46.9(13) . . ? O341 P340 C342 132(3) . . ? C335 O341 P340 155(4) . . ? C335 O341 C330 37.6(13) . . ? P340 O341 C330 162(4) . . ? C340 C341 C40 68(2) . . ? C340 C341 C342 34.3(19) . . ? C40 C341 C342 48.8(14) . . ? C340 C342 C40 83(3) . . ? C340 C342 O342 168(4) . . ? C40 C342 O342 109(3) . . ? C340 C342 C341 42(3) . . ? C40 C342 C341 61.0(16) . . ? O342 C342 C341 143(6) . . ? C340 C342 P340 138(3) . . ? C40 C342 P340 55.5(15) . . ? O342 C342 P340 53.6(18) . . ? C341 C342 P340 108.9(19) . . ? C342 O342 P340 79(3) . . ? C311 O401 C80 82(2) . 2_254 ? C311 O401 O310 124(2) . 2_254 ? C80 O401 O310 56.5(12) 2_254 2_254 ? C311 O401 C80 64.7(16) . . ? C80 O401 C80 43.8(15) 2_254 . ? O310 O401 C80 59.8(18) 2_254 . ? _diffrn_measured_fraction_theta_max 0.890 _diffrn_reflns_theta_full 44.49 _diffrn_measured_fraction_theta_full 0.890 _refine_diff_density_max 0.456 _refine_diff_density_min -0.319 _refine_diff_density_rms 0.098 #===END