data_ga74kas _audit_creation_method SHELXL-97 _audit_update_record ; 2006-06-01 text and data added, srw ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C13 H21 B2 N O6, 0.125(C4 H8 O2)' _chemical_formula_sum 'C13.50 H22 B2 N O6.25' _chemical_formula_structural ? _chemical_formula_weight 319.94 _chemical_absolute_configuration . _chemical_formula_analytical ? _chemical_compound_source ? 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' 'B' 'B' 0.0013 0.0007 '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 'Triclinic' _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.9032(14) _cell_length_b 16.060(3) _cell_length_c 16.510(3) _cell_angle_alpha 87.714(12) _cell_angle_beta 84.740(11) _cell_angle_gamma 80.831(12) _cell_volume 1798.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 688 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 13.95 _exptl_crystal_description 'acicular' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.78 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.181 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_crystal_id ga74kas _exptl_crystal_preparation ; The data crystal was mounted using epoxy to a 0.3 mm cryo-loop (Hampton Research) with the (0 1 0) scattering planes roughly normal to the spindle axis. ; _exptl_absorpt_coefficient_mu 0.090 _exptl_absorpt_correction_type 'integration' _exptl_absorpt_correction_T_min 0.9637 _exptl_absorpt_correction_T_max 0.9982 _exptl_absorpt_process_details 'SHELXTL/XPREP (Bruker, 2001)' _exptl_special_details ; All crystals examined had extremely weak diffraction patterns. Shaping the crystals was complicated by a tendency to fracture parallel to the a-axis. The data crystal was longer than ideal but selected to improve the number of observable reflections. One distinct cell was identified using APEX2 (Bruker, 2004). Four frame series were integrated and filtered for statistical outliers using SAINT (Bruker, 2001) then corrected for absorption by integration using SHELXTL/XPREP (Bruker, 2001) before using SAINT/SADABS (Bruker, 2001) to sort, merge, and scale the combined data. No decay correction was applied. Mean I/\s(I) was less than 1 for reflections beyond 1.4\%A resolution. Data between 1.4 and 1\%A resolution were included to improve the data-to-variable ratio at the expense of agreement factors. ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id ga74kas _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type ? _diffrn_measurement_device 'Bruker Kappa/ApexII CCD' _diffrn_measurement_method 'profile data from \f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15213 _diffrn_reflns_av_R_equivalents 0.1797 _diffrn_reflns_av_sigmaI/netI 0.2261 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 20.81 _reflns_number_total 3734 _reflns_number_gt 1285 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 V1.0-27 (Bruker, 2004)' _computing_cell_refinement 'SAINT V6.22 (Bruker, 2001)' _computing_data_reduction 'SAINT V6.22 (Bruker, 2001)' _computing_structure_solution 'SHELXTL V6.12 (Bruker, 2001)' _computing_structure_refinement 'SHELXTL V6.12 (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL V6.12 (Bruker, 2001)' _computing_publication_material 'XCIF (Bruker, 2001)' _refine_special_details ; Structure was phased by dual space methods (Schneider, 2002). Systematic conditions suggested the ambiguous space group. The space group choice was confirmed by successful convergence of the full-matrix least-squares refinement on F^2^. The highest peaks in the final difference Fourier map were in the vicinity of atoms O11, C40, and C36; the final map had no other significant features. A final analysis of variance between observed and calculated structure factors showed dependence on amplitude and resolution. ; _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^)+(0.0700P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3734 _refine_ls_number_parameters 407 _refine_ls_number_restraints 506 _refine_ls_R_factor_all 0.2781 _refine_ls_R_factor_gt 0.1097 _refine_ls_wR_factor_ref 0.2804 _refine_ls_wR_factor_gt 0.2258 _refine_ls_goodness_of_fit_ref 1.345 _refine_ls_restrained_S_all 1.322 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.002 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 B1 B 0.599(2) 0.2969(9) 0.6512(10) 0.063(4) Uani 1 1 d . . . N1 N 0.4556(15) 0.3116(5) 0.5762(6) 0.053(3) Uani 1 1 d . . . O1 O 0.7284(11) 0.3611(5) 0.6292(6) 0.068(3) Uani 1 1 d . . . O2 O 0.7869(13) 0.4596(6) 0.5348(5) 0.081(3) Uani 1 1 d . . . O3 O 0.4624(17) 0.3247(5) 0.7204(5) 0.087(3) Uani 1 1 d . . . O4 O 0.1509(14) 0.3905(6) 0.7500(5) 0.107(4) Uani 1 1 d . . . C1 C 0.700(2) 0.4037(9) 0.5601(9) 0.066(4) Uani 1 1 d . . . C2 C 0.5526(18) 0.3680(8) 0.5177(7) 0.071(4) Uani 1 1 d . . . H2A H 0.6169 0.3364 0.4713 0.086 Uiso 1 1 calc R . . H2B H 0.4554 0.4130 0.4985 0.086 Uiso 1 1 calc R . . C3 C 0.284(3) 0.3589(9) 0.7024(9) 0.072(4) Uani 1 1 d . . . C4 C 0.2659(18) 0.3570(8) 0.6129(8) 0.082(4) Uani 1 1 d . . . H4A H 0.1584 0.3278 0.6024 0.099 Uiso 1 1 calc R . . H4B H 0.2408 0.4139 0.5901 0.099 Uiso 1 1 calc R . . C5 C 0.4304(17) 0.2322(7) 0.5366(6) 0.088(4) Uani 1 1 d . . . H5A H 0.3420 0.2456 0.4947 0.133 Uiso 1 1 calc R . . H5B H 0.3771 0.1950 0.5766 0.133 Uiso 1 1 calc R . . H5C H 0.5559 0.2050 0.5132 0.133 Uiso 1 1 calc R . . C6 C 0.7164(18) 0.2077(7) 0.6636(6) 0.063(4) Uani 1 1 d . A . H6A H 0.6437 0.1670 0.6857 0.076 Uiso 1 1 calc R . . C7 C 0.9009(18) 0.1828(6) 0.6472(8) 0.095(5) Uani 1 1 d D . . H7B H 0.9772 0.2242 0.6307 0.114 Uiso 0.316(9) 1 calc PR A 2 H7A H 0.9704 0.2225 0.6207 0.114 Uiso 0.684(9) 1 d PR A 1 B2 B 1.0266(18) 0.0936(9) 0.6674(14) 0.088(5) Uiso 0.684(9) 1 d PDU A 1 O5 O 1.2203(14) 0.0817(6) 0.6608(7) 0.098(4) Uiso 0.684(9) 1 d PDU A 1 O6 O 0.9401(13) 0.0274(5) 0.6869(6) 0.084(4) Uiso 0.684(9) 1 d PDU A 1 C8 C 1.2822(18) -0.0083(7) 0.6893(7) 0.096(4) Uiso 0.684(9) 1 d PDU A 1 C9 C 1.1009(17) -0.0490(7) 0.6821(7) 0.095(4) Uiso 0.684(9) 1 d PDU A 1 C10 C 1.447(2) -0.0482(11) 0.6285(11) 0.125(5) Uiso 0.684(9) 1 d PDU A 1 H10A H 1.4914 -0.1053 0.6457 0.188 Uiso 0.684(9) 1 calc PR A 1 H10B H 1.5541 -0.0166 0.6257 0.188 Uiso 0.684(9) 1 calc PR A 1 H10C H 1.3982 -0.0479 0.5758 0.188 Uiso 0.684(9) 1 calc PR A 1 C11 C 1.344(3) 0.0042(11) 0.7725(8) 0.119(6) Uiso 0.684(9) 1 d PDU A 1 H11A H 1.3818 -0.0497 0.7986 0.178 Uiso 0.684(9) 1 calc PR A 1 H11B H 1.2368 0.0359 0.8046 0.178 Uiso 0.684(9) 1 calc PR A 1 H11C H 1.4545 0.0344 0.7673 0.178 Uiso 0.684(9) 1 calc PR A 1 C12 C 1.080(2) -0.0895(10) 0.6029(8) 0.114(6) Uiso 0.684(9) 1 d PDU A 1 H12A H 1.1821 -0.1373 0.5947 0.171 Uiso 0.684(9) 1 calc PR A 1 H12B H 1.0921 -0.0493 0.5588 0.171 Uiso 0.684(9) 1 calc PR A 1 H12C H 0.9539 -0.1075 0.6049 0.171 Uiso 0.684(9) 1 calc PR A 1 C13 C 1.057(2) -0.1038(9) 0.7565(9) 0.106(5) Uiso 0.684(9) 1 d PDU A 1 H13A H 1.0618 -0.0731 0.8048 0.160 Uiso 0.684(9) 1 calc PR A 1 H13B H 1.1532 -0.1540 0.7563 0.160 Uiso 0.684(9) 1 calc PR A 1 H13C H 0.9281 -0.1188 0.7554 0.160 Uiso 0.684(9) 1 calc PR A 1 B3 B 0.320(2) 0.3174(9) 0.2784(9) 0.059(4) Uani 1 1 d . . . N2 N 0.1563(13) 0.4010(5) 0.2709(6) 0.049(3) Uani 1 1 d . . . O7 O 0.4702(10) 0.3532(5) 0.3193(4) 0.060(2) Uani 1 1 d . . . O8 O 0.5746(12) 0.4767(5) 0.3274(5) 0.082(3) Uani 1 1 d . . . O9 O 0.2176(13) 0.2654(5) 0.3386(5) 0.067(2) Uani 1 1 d . . . O10 O -0.0192(14) 0.2836(6) 0.4395(6) 0.096(3) Uani 1 1 d . . . C14 C 0.4563(19) 0.4363(9) 0.3055(7) 0.060(4) Uani 1 1 d . . . C15 C 0.2778(17) 0.4714(7) 0.2626(6) 0.060(3) Uani 1 1 d . . . H15A H 0.3134 0.4845 0.2059 0.072 Uiso 1 1 calc R . . H15B H 0.2073 0.5219 0.2884 0.072 Uiso 1 1 calc R . . C16 C 0.072(2) 0.3134(10) 0.3811(10) 0.074(4) Uani 1 1 d . . . C17 C 0.0405(15) 0.4004(7) 0.3495(7) 0.056(3) Uani 1 1 d . . . H17A H -0.0980 0.4191 0.3430 0.067 Uiso 1 1 calc R . . H17B H 0.0838 0.4377 0.3866 0.067 Uiso 1 1 calc R . . C18 C 0.0289(17) 0.4001(7) 0.2028(7) 0.088(4) Uani 1 1 d . . . H18A H -0.0635 0.4515 0.2020 0.132 Uiso 1 1 calc R . . H18B H -0.0412 0.3529 0.2103 0.132 Uiso 1 1 calc R . . H18C H 0.1094 0.3952 0.1521 0.132 Uiso 1 1 calc R . . C19 C 0.4031(18) 0.2726(7) 0.1962(7) 0.079(4) Uani 1 1 d U B . H19A H 0.3326 0.2341 0.1767 0.094 Uiso 1 1 calc R . . C20 C 0.5641(17) 0.2863(7) 0.1540(6) 0.091(3) Uani 1 1 d DU . . H20B H 0.6455 0.3161 0.1794 0.110 Uiso 0.442(9) 1 calc PR B 2 H20A H 0.6346 0.3230 0.1766 0.110 Uiso 0.558(9) 1 d PR B 1 B4 B 0.664(3) 0.2399(17) 0.0729(13) 0.105(4) Uiso 0.558(9) 1 d PDU B 1 O11 O 0.823(2) 0.2621(9) 0.0338(6) 0.132(4) Uiso 0.558(9) 1 d PDU B 1 O12 O 0.5859(19) 0.1816(9) 0.0397(6) 0.114(4) Uiso 0.558(9) 1 d PDU B 1 C21 C 0.875(2) 0.2037(9) -0.0371(8) 0.139(4) Uiso 0.558(9) 1 d PDU B 1 C22 C 0.686(2) 0.1703(9) -0.0460(7) 0.139(4) Uiso 0.558(9) 1 d PDU B 1 C23 C 0.922(3) 0.2582(13) -0.1115(10) 0.152(6) Uiso 0.558(9) 1 d PDU B 1 H23A H 0.8056 0.2963 -0.1235 0.228 Uiso 0.558(9) 1 calc PR B 1 H23B H 0.9668 0.2228 -0.1571 0.228 Uiso 0.558(9) 1 calc PR B 1 H23C H 1.0231 0.2899 -0.1008 0.228 Uiso 0.558(9) 1 calc PR B 1 C24 C 1.049(3) 0.1442(13) -0.0075(13) 0.145(7) Uiso 0.558(9) 1 d PDU B 1 H24A H 1.0042 0.1088 0.0361 0.217 Uiso 0.558(9) 1 calc PR B 1 H24B H 1.1411 0.1764 0.0114 0.217 Uiso 0.558(9) 1 calc PR B 1 H24C H 1.1127 0.1097 -0.0515 0.217 Uiso 0.558(9) 1 calc PR B 1 C25 C 0.542(3) 0.2184(15) -0.1016(11) 0.157(6) Uiso 0.558(9) 1 d PDU B 1 H25A H 0.5959 0.2126 -0.1571 0.235 Uiso 0.558(9) 1 calc PR B 1 H25B H 0.5178 0.2770 -0.0882 0.235 Uiso 0.558(9) 1 calc PR B 1 H25C H 0.4199 0.1962 -0.0947 0.235 Uiso 0.558(9) 1 calc PR B 1 C26 C 0.718(3) 0.0759(10) -0.0587(13) 0.147(6) Uiso 0.558(9) 1 d PDU B 1 H26A H 0.8046 0.0481 -0.0201 0.220 Uiso 0.558(9) 1 calc PR B 1 H26B H 0.7768 0.0644 -0.1129 0.220 Uiso 0.558(9) 1 calc PR B 1 H26C H 0.5944 0.0555 -0.0511 0.220 Uiso 0.558(9) 1 calc PR B 1 B5 B 0.636(4) 0.257(2) 0.0642(14) 0.107(4) Uiso 0.442(9) 1 d PDU B 2 O13 O 0.793(2) 0.2834(12) 0.0262(7) 0.130(5) Uiso 0.442(9) 1 d PDU B 2 O14 O 0.555(2) 0.2030(11) 0.0269(8) 0.114(5) Uiso 0.442(9) 1 d PDU B 2 C27 C 0.815(2) 0.2443(11) -0.0564(7) 0.141(5) Uiso 0.442(9) 1 d PDU B 2 C28 C 0.703(2) 0.1704(10) -0.0430(7) 0.138(4) Uiso 0.442(9) 1 d PDU B 2 C29 C 0.708(4) 0.3089(13) -0.1131(12) 0.149(7) Uiso 0.442(9) 1 d PDU B 2 H29A H 0.5691 0.3173 -0.0963 0.223 Uiso 0.442(9) 1 calc PR B 2 H29B H 0.7288 0.2887 -0.1677 0.223 Uiso 0.442(9) 1 calc PR B 2 H29C H 0.7567 0.3613 -0.1112 0.223 Uiso 0.442(9) 1 calc PR B 2 C30 C 1.037(2) 0.2279(18) -0.0740(15) 0.151(6) Uiso 0.442(9) 1 d PDU B 2 H30A H 1.0701 0.2023 -0.1260 0.227 Uiso 0.442(9) 1 calc PR B 2 H30B H 1.0941 0.1907 -0.0325 0.227 Uiso 0.442(9) 1 calc PR B 2 H30C H 1.0876 0.2803 -0.0746 0.227 Uiso 0.442(9) 1 calc PR B 2 C31 C 0.582(3) 0.1509(18) -0.1098(11) 0.140(6) Uiso 0.442(9) 1 d PDU B 2 H31A H 0.6685 0.1295 -0.1558 0.210 Uiso 0.442(9) 1 calc PR B 2 H31B H 0.4990 0.2015 -0.1259 0.210 Uiso 0.442(9) 1 calc PR B 2 H31C H 0.5022 0.1094 -0.0901 0.210 Uiso 0.442(9) 1 calc PR B 2 C32 C 0.827(3) 0.0924(13) -0.0094(15) 0.155(7) Uiso 0.442(9) 1 d PDU B 2 H32A H 0.9015 0.1083 0.0322 0.233 Uiso 0.442(9) 1 calc PR B 2 H32B H 0.9151 0.0657 -0.0524 0.233 Uiso 0.442(9) 1 calc PR B 2 H32C H 0.7421 0.0539 0.0134 0.233 Uiso 0.442(9) 1 calc PR B 2 B6 B 1.014(4) 0.0883(13) 0.6522(19) 0.087(5) Uiso 0.316(9) 1 d PDU A 2 O15 O 1.191(2) 0.0679(9) 0.6145(12) 0.084(5) Uiso 0.316(9) 1 d PDU A 2 O16 O 0.963(2) 0.0373(9) 0.7122(12) 0.087(5) Uiso 0.316(9) 1 d PDU A 2 C33 C 1.248(3) -0.0247(9) 0.6354(11) 0.104(5) Uiso 0.316(9) 1 d PDU A 2 C34 C 1.124(3) -0.0376(9) 0.7141(11) 0.096(4) Uiso 0.316(9) 1 d PDU A 2 C35 C 1.181(5) -0.0730(16) 0.5688(13) 0.110(7) Uiso 0.316(9) 1 d PDU A 2 H35A H 1.2312 -0.1319 0.5750 0.165 Uiso 0.316(9) 1 calc PR A 2 H35B H 1.2292 -0.0525 0.5166 0.165 Uiso 0.316(9) 1 calc PR A 2 H35C H 1.0396 -0.0651 0.5726 0.165 Uiso 0.316(9) 1 calc PR A 2 C36 C 1.469(3) -0.0321(19) 0.638(2) 0.119(6) Uiso 0.316(9) 1 d PDU A 2 H36A H 1.5161 -0.0806 0.6706 0.179 Uiso 0.316(9) 1 calc PR A 2 H36B H 1.4998 0.0177 0.6609 0.179 Uiso 0.316(9) 1 calc PR A 2 H36C H 1.5321 -0.0381 0.5836 0.179 Uiso 0.316(9) 1 calc PR A 2 C37 C 1.023(4) -0.1153(12) 0.7205(18) 0.098(6) Uiso 0.316(9) 1 d PDU A 2 H37A H 1.1181 -0.1645 0.7081 0.147 Uiso 0.316(9) 1 calc PR A 2 H37B H 0.9235 -0.1094 0.6827 0.147 Uiso 0.316(9) 1 calc PR A 2 H37C H 0.9627 -0.1210 0.7748 0.147 Uiso 0.316(9) 1 calc PR A 2 C38 C 1.231(4) -0.027(2) 0.7883(12) 0.111(6) Uiso 0.316(9) 1 d PDU A 2 H38A H 1.2632 0.0291 0.7877 0.167 Uiso 0.316(9) 1 calc PR A 2 H38B H 1.3501 -0.0672 0.7876 0.167 Uiso 0.316(9) 1 calc PR A 2 H38C H 1.1480 -0.0359 0.8367 0.167 Uiso 0.316(9) 1 calc PR A 2 O17 O -0.390(5) 0.5195(19) -0.0593(13) 0.090(9) Uiso 0.25 1 d PDU . . C39 C -0.470(3) 0.4990(16) 0.0067(14) 0.101(9) Uiso 0.25 1 d PDU . . C40 C -0.670(4) 0.479(3) 0.011(3) 0.105(12) Uiso 0.25 1 d PDU . . H40A H -0.7173 0.4849 -0.0420 0.158 Uiso 0.25 1 calc PR . . H40B H -0.7551 0.5164 0.0476 0.158 Uiso 0.25 1 calc PR . . H40C H -0.6694 0.4217 0.0309 0.158 Uiso 0.25 1 calc PR . . O18 O -0.365(5) 0.497(2) 0.0710(14) 0.120(9) Uiso 0.25 1 d PDU . . C41 C -0.266(5) 0.569(2) 0.061(2) 0.122(11) Uiso 0.25 1 d PDU . . H41A H -0.2423 0.5878 0.1136 0.146 Uiso 0.25 1 calc PR . . H41B H -0.3471 0.6145 0.0338 0.146 Uiso 0.25 1 calc PR . . C42 C -0.071(6) 0.544(3) 0.010(3) 0.135(13) Uiso 0.25 1 d PDU . . H42A H -0.0697 0.4902 -0.0141 0.203 Uiso 0.25 1 calc PR . . H42B H 0.0359 0.5396 0.0440 0.203 Uiso 0.25 1 calc PR . . H42C H -0.0556 0.5857 -0.0323 0.203 Uiso 0.25 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.067(13) 0.049(12) 0.067(12) -0.014(8) 0.005(11) 0.004(9) N1 0.058(8) 0.041(7) 0.064(7) -0.017(5) -0.007(6) -0.012(5) O1 0.075(7) 0.041(6) 0.093(7) -0.016(5) -0.032(5) -0.006(5) O2 0.081(8) 0.069(8) 0.097(7) -0.018(5) 0.007(5) -0.023(5) O3 0.086(8) 0.090(7) 0.075(7) -0.005(5) -0.024(7) 0.030(6) O4 0.105(8) 0.109(8) 0.093(7) -0.031(6) 0.044(6) 0.006(6) C1 0.070(13) 0.047(11) 0.076(12) -0.022(9) 0.005(10) 0.005(8) C2 0.067(10) 0.082(11) 0.070(9) 0.001(8) -0.010(8) -0.027(8) C3 0.096(15) 0.073(11) 0.048(12) -0.013(8) 0.032(11) -0.034(10) C4 0.062(11) 0.091(11) 0.092(12) -0.021(8) -0.002(9) -0.001(8) C5 0.122(12) 0.050(9) 0.099(10) -0.031(7) -0.032(8) -0.011(7) C6 0.062(10) 0.050(9) 0.077(9) -0.005(6) 0.004(8) -0.011(7) C7 0.085(12) 0.039(9) 0.159(13) 0.002(8) 0.004(11) -0.014(8) B3 0.060(12) 0.049(11) 0.063(11) -0.023(9) -0.014(10) 0.020(9) N2 0.041(7) 0.057(7) 0.047(7) -0.020(5) -0.006(6) -0.001(5) O7 0.059(6) 0.049(6) 0.070(6) -0.023(4) -0.017(4) 0.008(4) O8 0.063(7) 0.071(7) 0.116(7) -0.027(5) -0.017(5) -0.011(5) O9 0.083(7) 0.049(6) 0.069(6) -0.019(5) -0.001(5) -0.011(5) O10 0.115(9) 0.066(7) 0.107(8) -0.014(6) 0.018(6) -0.024(6) C14 0.043(11) 0.057(11) 0.078(10) -0.026(8) -0.008(8) 0.008(8) C15 0.058(10) 0.052(9) 0.066(9) -0.007(6) 0.000(7) -0.001(7) C16 0.076(13) 0.060(13) 0.091(13) -0.015(10) -0.015(11) -0.020(9) C17 0.034(8) 0.050(9) 0.081(10) -0.017(7) -0.008(7) 0.005(6) C18 0.096(11) 0.083(11) 0.088(10) -0.024(7) -0.041(9) 0.002(8) C19 0.093(9) 0.068(7) 0.080(8) -0.019(6) -0.027(7) -0.016(7) C20 0.098(6) 0.091(6) 0.089(6) -0.020(5) -0.016(5) -0.019(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 O3 1.451(14) . ? B1 O1 1.481(16) . ? B1 C6 1.544(16) . ? B1 N1 1.643(15) . ? N1 C4 1.482(12) . ? N1 C2 1.486(12) . ? N1 C5 1.498(11) . ? O1 C1 1.320(13) . ? O2 C1 1.199(14) . ? O3 C3 1.321(15) . ? O4 C3 1.213(13) . ? C1 C2 1.483(15) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.496(14) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.280(12) . ? C6 H6A 0.9300 . ? C7 B2 1.593(14) . ? C7 B6 1.594(15) . ? C7 H7B 0.9300 . ? C7 H7A 0.9300 . ? B2 O5 1.315(9) . ? B2 O6 1.316(9) . ? O5 C8 1.508(9) . ? O6 C9 1.517(9) . ? C8 C11 1.507(7) . ? C8 C9 1.517(7) . ? C8 C10 1.522(8) . ? C9 C12 1.512(7) . ? C9 C13 1.517(7) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? B3 O9 1.475(16) . ? B3 O7 1.488(15) . ? B3 C19 1.579(15) . ? B3 N2 1.619(14) . ? N2 C17 1.461(11) . ? N2 C18 1.492(11) . ? N2 C15 1.507(12) . ? O7 C14 1.334(13) . ? O8 C14 1.208(12) . ? O9 C16 1.329(14) . ? O10 C16 1.225(14) . ? C14 C15 1.499(13) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.463(16) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.301(13) . ? C19 H19A 0.9300 . ? C20 B5 1.584(15) . ? C20 B4 1.604(15) . ? C20 H20B 0.9300 . ? C20 H20A 0.9300 . ? B4 O12 1.312(9) . ? B4 O11 1.317(9) . ? O11 C21 1.511(9) . ? O12 C22 1.520(9) . ? C21 C22 1.511(7) . ? C21 C24 1.517(8) . ? C21 C23 1.521(8) . ? C22 C25 1.514(8) . ? C22 C26 1.518(8) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? B5 O14 1.312(9) . ? B5 O13 1.317(9) . ? O13 C27 1.509(10) . ? O14 C28 1.521(9) . ? C27 C30 1.514(8) . ? C27 C28 1.515(7) . ? C27 C29 1.520(8) . ? C28 C32 1.515(8) . ? C28 C31 1.515(8) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? B6 O16 1.318(9) . ? B6 O15 1.322(9) . ? O15 C33 1.510(10) . ? O16 C34 1.507(9) . ? C33 C36 1.515(8) . ? C33 C34 1.516(8) . ? C33 C35 1.518(8) . ? C34 C38 1.517(8) . ? C34 C37 1.520(8) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? O17 C39 1.231(10) . ? C39 O18 1.334(9) . ? C39 C40 1.465(9) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? O18 C41 1.429(10) . ? C41 C42 1.530(10) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? 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 O3 B1 O1 109.7(11) . . ? O3 B1 C6 113.5(12) . . ? O1 B1 C6 112.7(12) . . ? O3 B1 N1 101.7(10) . . ? O1 B1 N1 100.5(10) . . ? C6 B1 N1 117.6(11) . . ? C4 N1 C2 110.3(10) . . ? C4 N1 C5 112.0(9) . . ? C2 N1 C5 111.1(9) . . ? C4 N1 B1 104.8(9) . . ? C2 N1 B1 103.9(9) . . ? C5 N1 B1 114.3(9) . . ? C1 O1 B1 116.3(11) . . ? C3 O3 B1 115.2(10) . . ? O2 C1 O1 124.8(15) . . ? O2 C1 C2 126.1(14) . . ? O1 C1 C2 109.0(13) . . ? C1 C2 N1 108.2(10) . . ? C1 C2 H2A 110.1 . . ? N1 C2 H2A 110.1 . . ? C1 C2 H2B 110.1 . . ? N1 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? O4 C3 O3 126.1(14) . . ? O4 C3 C4 122.8(16) . . ? O3 C3 C4 111.1(12) . . ? N1 C4 C3 106.6(11) . . ? N1 C4 H4A 110.4 . . ? C3 C4 H4A 110.4 . . ? N1 C4 H4B 110.4 . . ? C3 C4 H4B 110.4 . . ? H4A C4 H4B 108.6 . . ? N1 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 B1 128.1(12) . . ? C7 C6 H6A 115.9 . . ? B1 C6 H6A 115.9 . . ? C6 C7 B2 128.5(10) . . ? C6 C7 B6 126.8(12) . . ? C6 C7 H7B 116.6 . . ? B6 C7 H7B 116.6 . . ? C6 C7 H7A 115.4 . . ? B2 C7 H7A 116.1 . . ? O5 B2 O6 117.2(12) . . ? O5 B2 C7 121.7(9) . . ? O6 B2 C7 121.0(9) . . ? B2 O5 C8 105.5(9) . . ? B2 O6 C9 106.6(9) . . ? C11 C8 O5 101.4(9) . . ? C11 C8 C9 119.2(11) . . ? O5 C8 C9 103.5(8) . . ? C11 C8 C10 114.9(12) . . ? O5 C8 C10 107.5(10) . . ? C9 C8 C10 108.7(10) . . ? C12 C9 O6 104.9(9) . . ? C12 C9 C13 113.3(11) . . ? O6 C9 C13 105.6(9) . . ? C12 C9 C8 118.3(10) . . ? O6 C9 C8 101.1(8) . . ? C13 C9 C8 111.7(10) . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 H13A 109.5 . . ? C9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O9 B3 O7 108.4(10) . . ? O9 B3 C19 115.3(12) . . ? O7 B3 C19 113.7(11) . . ? O9 B3 N2 101.8(10) . . ? O7 B3 N2 99.8(9) . . ? C19 B3 N2 116.2(10) . . ? C17 N2 C18 110.9(9) . . ? C17 N2 C15 112.3(8) . . ? C18 N2 C15 113.2(9) . . ? C17 N2 B3 102.3(9) . . ? C18 N2 B3 114.3(8) . . ? C15 N2 B3 103.2(9) . . ? C14 O7 B3 111.6(10) . . ? C16 O9 B3 110.3(11) . . ? O8 C14 O7 122.3(12) . . ? O8 C14 C15 125.6(13) . . ? O7 C14 C15 112.0(11) . . ? C14 C15 N2 103.3(9) . . ? C14 C15 H15A 111.1 . . ? N2 C15 H15A 111.1 . . ? C14 C15 H15B 111.1 . . ? N2 C15 H15B 111.1 . . ? H15A C15 H15B 109.1 . . ? O10 C16 O9 120.5(15) . . ? O10 C16 C17 127.3(15) . . ? O9 C16 C17 112.2(13) . . ? N2 C17 C16 106.6(10) . . ? N2 C17 H17A 110.4 . . ? C16 C17 H17A 110.4 . . ? N2 C17 H17B 110.4 . . ? C16 C17 H17B 110.4 . . ? H17A C17 H17B 108.6 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 B3 124.1(12) . . ? C20 C19 H19A 117.9 . . ? B3 C19 H19A 117.9 . . ? C19 C20 B5 126.9(11) . . ? C19 C20 B4 127.0(10) . . ? C19 C20 H20B 116.5 . . ? B5 C20 H20B 116.5 . . ? C19 C20 H20A 115.8 . . ? B4 C20 H20A 116.9 . . ? O12 B4 O11 116.7(12) . . ? O12 B4 C20 122.1(10) . . ? O11 B4 C20 121.0(10) . . ? B4 O11 C21 105.6(9) . . ? B4 O12 C22 106.9(9) . . ? C22 C21 O11 103.7(8) . . ? C22 C21 C24 119.2(11) . . ? O11 C21 C24 100.9(9) . . ? C22 C21 C23 109.3(10) . . ? O11 C21 C23 106.8(10) . . ? C24 C21 C23 115.2(12) . . ? C21 C22 C25 118.3(11) . . ? C21 C22 C26 112.6(10) . . ? C25 C22 C26 112.7(11) . . ? C21 C22 O12 100.6(8) . . ? C25 C22 O12 105.7(9) . . ? C26 C22 O12 105.1(9) . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O14 B5 O13 117.3(12) . . ? O14 B5 C20 122.6(10) . . ? O13 B5 C20 119.9(10) . . ? B5 O13 C27 104.9(9) . . ? B5 O14 C28 106.1(10) . . ? O13 C27 C30 101.7(9) . . ? O13 C27 C28 103.5(9) . . ? C30 C27 C28 119.5(11) . . ? O13 C27 C29 106.7(10) . . ? C30 C27 C29 114.9(12) . . ? C28 C27 C29 108.9(11) . . ? C32 C28 C27 112.7(11) . . ? C32 C28 C31 112.8(11) . . ? C27 C28 C31 118.1(11) . . ? C32 C28 O14 105.6(9) . . ? C27 C28 O14 100.0(8) . . ? C31 C28 O14 105.7(9) . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C28 C32 H32A 109.5 . . ? C28 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C28 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O16 B6 O15 116.7(13) . . ? O16 B6 C7 119.6(12) . . ? O15 B6 C7 120.4(12) . . ? B6 O15 C33 104.3(10) . . ? B6 O16 C34 107.5(9) . . ? O15 C33 C36 101.8(10) . . ? O15 C33 C34 103.9(8) . . ? C36 C33 C34 118.4(12) . . ? O15 C33 C35 106.5(10) . . ? C36 C33 C35 115.6(13) . . ? C34 C33 C35 108.9(11) . . ? O16 C34 C33 101.9(8) . . ? O16 C34 C38 105.6(9) . . ? C33 C34 C38 112.2(11) . . ? O16 C34 C37 106.1(10) . . ? C33 C34 C37 116.7(11) . . ? C38 C34 C37 112.9(11) . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C34 C38 H38A 109.5 . . ? C34 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C34 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O17 C39 O18 116.7(14) . . ? O17 C39 C40 119.6(15) . . ? O18 C39 C40 123.7(15) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 O18 C41 105.5(14) . . ? O18 C41 C42 108.4(15) . . ? O18 C41 H41A 110.0 . . ? C42 C41 H41A 110.0 . . ? O18 C41 H41B 110.0 . . ? C42 C41 H41B 110.0 . . ? H41A C41 H41B 108.4 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 B1 N1 C4 7.9(12) . . . . ? O1 B1 N1 C4 -105.0(10) . . . . ? C6 B1 N1 C4 132.5(13) . . . . ? O3 B1 N1 C2 123.7(11) . . . . ? O1 B1 N1 C2 10.8(11) . . . . ? C6 B1 N1 C2 -111.7(13) . . . . ? O3 B1 N1 C5 -115.1(10) . . . . ? O1 B1 N1 C5 132.1(9) . . . . ? C6 B1 N1 C5 9.5(17) . . . . ? O3 B1 O1 C1 -109.9(12) . . . . ? C6 B1 O1 C1 122.6(12) . . . . ? N1 B1 O1 C1 -3.3(13) . . . . ? O1 B1 O3 C3 99.3(14) . . . . ? C6 B1 O3 C3 -133.7(12) . . . . ? N1 B1 O3 C3 -6.4(14) . . . . ? B1 O1 C1 O2 177.4(12) . . . . ? B1 O1 C1 C2 -5.8(14) . . . . ? O2 C1 C2 N1 -169.9(12) . . . . ? O1 C1 C2 N1 13.4(13) . . . . ? C4 N1 C2 C1 97.2(11) . . . . ? C5 N1 C2 C1 -137.9(10) . . . . ? B1 N1 C2 C1 -14.6(12) . . . . ? B1 O3 C3 O4 -175.7(12) . . . . ? B1 O3 C3 C4 2.4(15) . . . . ? C2 N1 C4 C3 -118.1(10) . . . . ? C5 N1 C4 C3 117.6(10) . . . . ? B1 N1 C4 C3 -6.9(12) . . . . ? O4 C3 C4 N1 -178.5(11) . . . . ? O3 C3 C4 N1 3.4(13) . . . . ? O3 B1 C6 C7 -135.1(15) . . . . ? O1 B1 C6 C7 -10(2) . . . . ? N1 B1 C6 C7 106.4(17) . . . . ? B1 C6 C7 B2 173.6(15) . . . . ? B1 C6 C7 B6 -173.2(19) . . . . ? C6 C7 B2 O5 -167.0(17) . . . . ? B6 C7 B2 O5 108(5) . . . . ? C6 C7 B2 O6 17(3) . . . . ? B6 C7 B2 O6 -68(4) . . . . ? O6 B2 O5 C8 -7(2) . . . . ? C7 B2 O5 C8 177.0(15) . . . . ? O5 B2 O6 C9 -9(2) . . . . ? C7 B2 O6 C9 166.8(15) . . . . ? B2 O5 C8 C11 -104.3(16) . . . . ? B2 O5 C8 C9 19.7(16) . . . . ? B2 O5 C8 C10 134.7(16) . . . . ? B2 O6 C9 C12 -102.8(16) . . . . ? B2 O6 C9 C13 137.3(15) . . . . ? B2 O6 C9 C8 20.8(15) . . . . ? C11 C8 C9 C12 -158.3(12) . . . . ? O5 C8 C9 C12 90.1(11) . . . . ? C10 C8 C9 C12 -24.0(14) . . . . ? C11 C8 C9 O6 87.9(11) . . . . ? O5 C8 C9 O6 -23.7(10) . . . . ? C10 C8 C9 O6 -137.8(10) . . . . ? C11 C8 C9 C13 -24.0(14) . . . . ? O5 C8 C9 C13 -135.6(10) . . . . ? C10 C8 C9 C13 110.3(12) . . . . ? O9 B3 N2 C17 25.4(11) . . . . ? O7 B3 N2 C17 -85.9(11) . . . . ? C19 B3 N2 C17 151.4(12) . . . . ? O9 B3 N2 C18 -94.5(11) . . . . ? O7 B3 N2 C18 154.2(9) . . . . ? C19 B3 N2 C18 31.5(17) . . . . ? O9 B3 N2 C15 142.2(9) . . . . ? O7 B3 N2 C15 30.8(11) . . . . ? C19 B3 N2 C15 -91.8(13) . . . . ? O9 B3 O7 C14 -130.0(10) . . . . ? C19 B3 O7 C14 100.5(11) . . . . ? N2 B3 O7 C14 -23.9(13) . . . . ? O7 B3 O9 C16 84.6(11) . . . . ? C19 B3 O9 C16 -146.7(10) . . . . ? N2 B3 O9 C16 -20.1(12) . . . . ? B3 O7 C14 O8 -173.7(11) . . . . ? B3 O7 C14 C15 7.7(12) . . . . ? O8 C14 C15 N2 -164.7(11) . . . . ? O7 C14 C15 N2 13.9(11) . . . . ? C17 N2 C15 C14 82.2(9) . . . . ? C18 N2 C15 C14 -151.2(8) . . . . ? B3 N2 C15 C14 -27.2(10) . . . . ? B3 O9 C16 O10 -173.0(12) . . . . ? B3 O9 C16 C17 7.0(14) . . . . ? C18 N2 C17 C16 100.0(9) . . . . ? C15 N2 C17 C16 -132.2(9) . . . . ? B3 N2 C17 C16 -22.2(11) . . . . ? O10 C16 C17 N2 -168.9(13) . . . . ? O9 C16 C17 N2 11.2(13) . . . . ? O9 B3 C19 C20 -146.2(13) . . . . ? O7 B3 C19 C20 -20.2(18) . . . . ? N2 B3 C19 C20 94.9(16) . . . . ? B3 C19 C20 B5 -168(2) . . . . ? B3 C19 C20 B4 176.4(19) . . . . ? C19 C20 B4 O12 1(4) . . . . ? B5 C20 B4 O12 -94(5) . . . . ? C19 C20 B4 O11 177(2) . . . . ? B5 C20 B4 O11 83(4) . . . . ? O12 B4 O11 C21 -5(3) . . . . ? C20 B4 O11 C21 179(2) . . . . ? O11 B4 O12 C22 -12(3) . . . . ? C20 B4 O12 C22 165(2) . . . . ? B4 O11 C21 C22 19(2) . . . . ? B4 O11 C21 C24 -105(2) . . . . ? B4 O11 C21 C23 135(2) . . . . ? O11 C21 C22 C25 90.2(13) . . . . ? C24 C21 C22 C25 -158.8(15) . . . . ? C23 C21 C22 C25 -23.4(15) . . . . ? O11 C21 C22 C26 -135.6(12) . . . . ? C24 C21 C22 C26 -24.6(16) . . . . ? C23 C21 C22 C26 110.8(14) . . . . ? O11 C21 C22 O12 -24.2(11) . . . . ? C24 C21 C22 O12 86.8(13) . . . . ? C23 C21 C22 O12 -137.8(12) . . . . ? B4 O12 C22 C21 22(2) . . . . ? B4 O12 C22 C25 -101(2) . . . . ? B4 O12 C22 C26 139(2) . . . . ? C19 C20 B5 O14 -12(5) . . . . ? B4 C20 B5 O14 83(4) . . . . ? C19 C20 B5 O13 173(2) . . . . ? B4 C20 B5 O13 -92(5) . . . . ? O14 B5 O13 C27 5(4) . . . . ? C20 B5 O13 C27 -180(2) . . . . ? O13 B5 O14 C28 13(4) . . . . ? C20 B5 O14 C28 -161(3) . . . . ? B5 O13 C27 C30 -146(2) . . . . ? B5 O13 C27 C28 -22(2) . . . . ? B5 O13 C27 C29 93(3) . . . . ? O13 C27 C28 C32 -84.2(14) . . . . ? C30 C27 C28 C32 27.8(16) . . . . ? C29 C27 C28 C32 162.5(16) . . . . ? O13 C27 C28 C31 141.4(14) . . . . ? C30 C27 C28 C31 -106.6(17) . . . . ? C29 C27 C28 C31 28.1(17) . . . . ? O13 C27 C28 O14 27.4(12) . . . . ? C30 C27 C28 O14 139.4(13) . . . . ? C29 C27 C28 O14 -85.8(14) . . . . ? B5 O14 C28 C32 92(2) . . . . ? B5 O14 C28 C27 -25(2) . . . . ? B5 O14 C28 C31 -148(2) . . . . ? C6 C7 B6 O16 -39(4) . . . . ? B2 C7 B6 O16 64(4) . . . . ? C6 C7 B6 O15 163(2) . . . . ? B2 C7 B6 O15 -94(6) . . . . ? O16 B6 O15 C33 19(4) . . . . ? C7 B6 O15 C33 179(3) . . . . ? O15 B6 O16 C34 -6(4) . . . . ? C7 B6 O16 C34 -165(2) . . . . ? B6 O15 C33 C36 -147(2) . . . . ? B6 O15 C33 C34 -24(2) . . . . ? B6 O15 C33 C35 91(2) . . . . ? B6 O16 C34 C33 -10(3) . . . . ? B6 O16 C34 C38 107(3) . . . . ? B6 O16 C34 C37 -133(3) . . . . ? O15 C33 C34 O16 20.2(14) . . . . ? C36 C33 C34 O16 132.1(16) . . . . ? C35 C33 C34 O16 -93.1(16) . . . . ? O15 C33 C34 C38 -92.3(16) . . . . ? C36 C33 C34 C38 19.6(19) . . . . ? C35 C33 C34 C38 154.5(18) . . . . ? O15 C33 C34 C37 135.2(16) . . . . ? C36 C33 C34 C37 -112.9(19) . . . . ? C35 C33 C34 C37 22.0(19) . . . . ? O17 C39 O18 C41 40(2) . . . . ? C40 C39 O18 C41 -140(2) . . . . ? C39 O18 C41 C42 -88(4) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 20.81 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.347 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.066 _publ_requested_category FO _publ_section_references ; Bruker (2001). SAINT, SHELXTL, XCIF. Bruker AXS, Inc., Madison, Wisconsin, USA. Bruker (2004). APEX2. Bruker AXS, Inc., Madison, Wisconsin, USA. Schneider, T.R. and Sheldrick, G.M. (2002). Acta Cryst. D58, 1772-1779. ; _publ_section_figure_captions ; Figure 1. SHELXTL (Bruker, 2001) plot of host molecule 1 showing 35% probability ellipsoids for non-H atoms and circles of arbitrary size for H atoms. The disordered solvate and minor site disordered host atoms for molecule 1 were omitted for clarity. Figure 2. SHELXTL (Bruker, 2001) plot of host molecule 2 showing 35% probability ellipsoids for non-H atoms and circles of arbitrary size for H atoms. The disordered solvate and minor site disordered host atoms for molecule 2 were omitted for clarity. ; _publ_section_exptl_prep ; Crystals were grown by evaporation from an ethylacetate solution. ; _publ_section_exptl_refinement ; The proposed model for both host molecules includes rotational disorder about the elongated bond between the vinyl C atom and the planar B atom (C7-B2 and C20-B4). The ethylacetate solvate was disordered about 2 symmetry centers and refined as an idealized group. Chemically similar disordered groups of the host molecules were restrained to similar geometry using effective standard deviations of 0.01\%A and 0.02\%A for bond lengths and angles, respectively. Owing to the paucity of data and complexity of the model, disordered sites were refined with isotropic displacement parameters. Similar displacement parameters (esd 0.01) were imposed on overlapping disordered sites. H atoms were included as riding idealized contributors. Methyl H atom U's were assigned as 1.5 times U~eq~ of the carrier atom; remaining H atom U's were assigned as 1.2 times carrier U~eq~. ; _publ_contact_author ; Scott R. Wilson University of Illinois School of Chemical Sciences, Box 59-1 505 South Mathews Avenue Urbana, Illinois 61801 USA ; _publ_contact_author_phone '1 217 244 1708' _publ_contact_author_fax '1 217 244 8068' _publ_contact_author_email srwilson@uiuc.edu _publ_contact_letter ; Please consider this CIF submission for publication as a structural paper in Acta Crystallographica E. ; _publ_requested_journal 'Acta Crystallographica E' _publ_requested_coeditor_name ? _publ_section_title ; ? ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_acknowledgements ; The Materials Chemistry Laboratory at the University of Illinois was supported in part by grants NSF CHE 95-03145 and NSF CHE 03-43032 from the National Science Foundation. ; loop_ _publ_author_name _publ_author_address 'Wilson, Scott R.' ; University of Illinois School of Chemical Sciences, Box 59-1 505 South Mathews Avenue Urbana, Illinois 61801 USA ; 'Prussak-Wieckowska, Teresa' ; University of Illinois School of Chemical Sciences, Box 59-1 505 South Mathews Avenue Urbana, Illinois 61801 USA ; loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 1.00 0.00 0.0200 0.00 -1.00 0.00 0.0200 0.00 0.00 1.00 0.0100 0.00 0.00 -1.00 0.0100 -1.00 0.00 0.00 0.3800 1.00 0.00 0.00 0.3800 _vrf_THETM01_ga74kas ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: All crystals examined had extremely weak diffraction patterns. For the largest available crystal, mean I/\s(I) was less than 1 for reflections beyond 1.4\%A resolution. Data between 1.4 and 1\%A resolution were included to improve the data-to-variable ratio at the expense of agreement factors. ; _vrf_PLAT023_ga74kas ; PROBLEM: Resolution (too) Low [sin(th)/Lambda < 0.6]..... 20.81 Deg. RESPONSE: All crystals examined had extremely weak diffraction patterns. For the largest available crystal, mean I/\s(I) was less than 1 for reflections beyond 1.4\%A resolution. Data between 1.4 and 1\%A resolution were included to improve the data-to-variable ratio at the expense of agreement factors. ; _vrf_PLAT027_ga74kas ; PROBLEM: _diffrn_reflns_theta_full (too) Low ............ 20.81 Deg. RESPONSE: All crystals examined had extremely weak diffraction patterns. For the largest available crystal, mean I/\s(I) was less than 1 for reflections beyond 1.4\%A resolution. Data between 1.4 and 1\%A resolution were included to improve the data-to-variable ratio at the expense of agreement factors. ; _vrf_PLAT201_ga74kas ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 18 RESPONSE: Owing to the paucity of data and complexity of the model, disordered sites were refined with isotropic displacement parameters. ; # end Validation Reply Form