data_ba19nas _audit_creation_method SHELXL-97 _audit_update_record ; ? ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H40 B N O6, 1.0(C2 H4 Cl2)' _chemical_formula_sum 'C38 H44 B Cl2 N O6' _chemical_formula_structural ? _chemical_formula_weight 692.45 _chemical_absolute_configuration rmad _chemical_formula_iupac ? _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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P2(1) ' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.4292(11) _cell_length_b 13.9385(13) _cell_length_c 11.4429(12) _cell_angle_alpha 90.00 _cell_angle_beta 91.216(6) _cell_angle_gamma 90.00 _cell_volume 1822.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1929 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 18.50 _exptl_crystal_description 'needle' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.254 _exptl_crystal_size_mid 0.127 _exptl_crystal_size_min 0.072 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_crystal_id ba19nas _exptl_crystal_preparation ; The data crystal was mounted using oil (Parantone-N, Exxon) to a 0.3 mm cryo-loop (Hampton Research) with the (2 -2 1) scattering planes roughly normal to the spindle axis. ; _exptl_absorpt_coefficient_mu 0.224 _exptl_absorpt_correction_type 'integration' _exptl_absorpt_correction_T_min 0.9487 _exptl_absorpt_correction_T_max 0.9890 _exptl_absorpt_process_details 'SHELXTL/XPREP V2005/2 (Bruker, 2005)' _exptl_special_details ; One distinct cell was identified using APEX2 (Bruker, 2004). Five frame series were integrated and filtered for statistical outliers using SAINT (Bruker, 2005) then corrected for absorption by integration using SHELXTL/XPREP V2005/2 (Bruker, 2005) before using SAINT/SADABS (Bruker, 2005) to sort, merge, and scale the combined data. No decay correction was applied. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id ba19nas _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_reflns_number 16736 _diffrn_reflns_av_R_equivalents 0.0658 _diffrn_reflns_av_sigmaI/netI 0.0980 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.36 _reflns_number_total 6569 _reflns_number_gt 4040 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 V2.0-1 (Bruker, 2004)' _computing_cell_refinement 'SAINT V7.23A (Bruker, 2005)' _computing_data_reduction ; SAINT V7.23A, XPREP V2005/2, SADABS V2007/4, TWINABS V2007/5 (Bruker, 2005 & 2007) ; _computing_structure_solution 'SHELXTL V6.12 (Bruker, 2005)' _computing_structure_refinement 'SHELXTL V6.12 (Bruker, 2005)' _computing_molecular_graphics ; SHELXTL V6.12 (Bruker, 2005), CrystalMaker v2.1.3 (CrystalMaker, 1994) ; _computing_publication_material 'XCIF V6.12 (Bruker, 2005)' _refine_special_details ; Structure was phased by direct methods (Sheldrick, 2008). 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 C37 and C38; the final map had no other significant features. A final analysis of variance between observed and calculated structure factors showed little dependence on amplitude or 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^)+(0.0512P)^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_abs_structure_details 'Flack (1983), 3078 Friedels' _refine_ls_abs_structure_Flack 0.11(10) _refine_ls_number_reflns 6569 _refine_ls_number_parameters 511 _refine_ls_number_restraints 249 _refine_ls_R_factor_all 0.1107 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1198 _refine_ls_wR_factor_gt 0.0994 _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_restrained_S_all 0.991 _refine_ls_shift/su_max 0.002 _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 B1 B 0.5545(3) 0.5292(3) 0.5601(4) 0.0295(10) Uani 1 1 d . . . N1 N 0.4223(2) 0.5082(2) 0.6142(2) 0.0265(7) Uani 1 1 d . . . O1 O 0.63164(19) 0.51255(18) 0.6623(2) 0.0335(6) Uani 1 1 d . . . O2 O 0.6275(2) 0.4344(2) 0.8336(2) 0.0507(8) Uani 1 1 d . . . O3 O 0.4425(2) 0.35459(19) 0.3681(2) 0.0450(7) Uani 1 1 d . . . O4 O 0.5615(2) 0.44759(17) 0.4776(2) 0.0330(6) Uani 1 1 d . . . O5 O 0.74879(18) 0.58211(17) 0.3975(2) 0.0301(6) Uani 1 1 d . . . O6 O 0.71989(19) 0.74245(17) 0.4228(2) 0.0338(6) Uani 1 1 d . . . C1 C 0.5802(3) 0.4580(3) 0.7436(4) 0.0370(10) Uani 1 1 d . . . C2 C 0.4557(3) 0.4357(3) 0.7068(3) 0.0317(9) Uani 1 1 d . . . H2A H 0.4033 0.4410 0.7743 0.038 Uiso 1 1 calc R . . H2B H 0.4499 0.3698 0.6750 0.038 Uiso 1 1 calc R . . C3 C 0.3614(3) 0.4618(3) 0.5120(3) 0.0317(9) Uani 1 1 d . . . H3A H 0.3200 0.5102 0.4633 0.038 Uiso 1 1 calc R . . H3B H 0.3040 0.4137 0.5385 0.038 Uiso 1 1 calc R . . C4 C 0.4577(3) 0.4140(3) 0.4437(4) 0.0347(10) Uani 1 1 d . . . C5 C 0.3541(3) 0.5940(2) 0.6613(3) 0.0269(9) Uani 1 1 d . . . H5 H 0.3517 0.6422 0.5965 0.032 Uiso 1 1 calc R . . C6 C 0.2236(3) 0.5690(3) 0.6854(3) 0.0313(9) Uani 1 1 d . . . H6 H 0.2182 0.4976 0.6921 0.038 Uiso 1 1 calc R . . C7 C 0.1847(3) 0.6115(3) 0.8023(3) 0.0350(10) Uani 1 1 d . . . H7 H 0.1004 0.6001 0.8196 0.042 Uiso 1 1 calc R . . C8 C 0.2267(3) 0.7163(3) 0.8262(3) 0.0367(10) Uani 1 1 d . . . C9 C 0.3429(3) 0.6671(3) 0.8692(3) 0.0334(9) Uani 1 1 d . . . H9 H 0.3836 0.6991 0.9369 0.040 Uiso 1 1 calc R . . C10 C 0.4208(3) 0.6439(3) 0.7655(3) 0.0313(9) Uani 1 1 d . . . H10A H 0.4854 0.6016 0.7928 0.038 Uiso 1 1 calc R . . H10B H 0.4561 0.7042 0.7371 0.038 Uiso 1 1 calc R . . C11 C 0.1407(3) 0.5996(3) 0.5851(4) 0.0448(11) Uani 1 1 d . . . H11A H 0.0594 0.5916 0.6090 0.067 Uiso 1 1 calc R . . H11B H 0.1548 0.5598 0.5163 0.067 Uiso 1 1 calc R . . H11C H 0.1548 0.6671 0.5659 0.067 Uiso 1 1 calc R . . C12 C 0.2697(3) 0.5799(3) 0.9002(3) 0.0377(10) Uani 1 1 d . . . H12A H 0.2364 0.5822 0.9794 0.045 Uiso 1 1 calc R . . H12B H 0.3085 0.5176 0.8858 0.045 Uiso 1 1 calc R . . C13 C 0.1597(3) 0.7605(3) 0.9281(4) 0.0512(12) Uani 1 1 d . . . H13A H 0.2051 0.8138 0.9617 0.077 Uiso 1 1 calc R . . H13B H 0.1477 0.7116 0.9882 0.077 Uiso 1 1 calc R . . H13C H 0.0837 0.7842 0.8993 0.077 Uiso 1 1 calc R . . C14 C 0.2332(4) 0.7920(3) 0.7299(4) 0.0478(11) Uani 1 1 d . . . H14A H 0.2788 0.7668 0.6652 0.072 Uiso 1 1 calc R . . H14B H 0.2709 0.8499 0.7612 0.072 Uiso 1 1 calc R . . H14C H 0.1539 0.8076 0.7017 0.072 Uiso 1 1 calc R . . C15 C 0.5739(3) 0.6326(2) 0.5001(3) 0.0279(9) Uani 1 1 d . . . H15 H 0.5514 0.6812 0.5598 0.034 Uiso 1 1 calc R . . C16 C 0.4936(3) 0.6501(3) 0.3941(3) 0.0278(9) Uani 1 1 d . . . C17 C 0.4048(3) 0.7186(3) 0.4000(4) 0.0334(9) Uani 1 1 d . . . H17 H 0.3989 0.7571 0.4681 0.040 Uiso 1 1 calc R . . C18 C 0.3255(3) 0.7312(3) 0.3089(4) 0.0463(11) Uani 1 1 d . . . H18 H 0.2637 0.7764 0.3156 0.056 Uiso 1 1 calc R . . C19 C 0.3359(4) 0.6782(3) 0.2084(4) 0.0568(13) Uani 1 1 d . . . H19 H 0.2824 0.6880 0.1449 0.068 Uiso 1 1 calc R . . C20 C 0.4235(4) 0.6110(3) 0.1992(4) 0.0501(12) Uani 1 1 d . . . H20 H 0.4303 0.5743 0.1297 0.060 Uiso 1 1 calc R . . C21 C 0.5020(3) 0.5973(3) 0.2921(3) 0.0364(10) Uani 1 1 d . . . H21 H 0.5623 0.5508 0.2855 0.044 Uiso 1 1 calc R . . C22 C 0.7027(3) 0.6495(3) 0.4775(3) 0.0297(9) Uani 1 1 d . . . H22 H 0.7483 0.6466 0.5530 0.036 Uiso 1 1 calc R . . C23 C 0.8528(3) 0.6278(2) 0.3572(3) 0.0287(9) Uani 1 1 d . . . H23 H 0.9144 0.6260 0.4206 0.034 Uiso 1 1 calc R . . C24 C 0.8112(3) 0.7321(3) 0.3389(3) 0.0310(9) Uani 1 1 d . . . H24 H 0.7771 0.7393 0.2582 0.037 Uiso 1 1 calc R . . C25 C 0.8983(3) 0.5806(3) 0.2502(3) 0.0323(9) Uani 1 1 d . . . C26 C 0.8255(4) 0.5592(3) 0.1560(4) 0.0420(11) Uani 1 1 d . . . H26 H 0.7440 0.5718 0.1608 0.050 Uiso 1 1 calc R . . C27 C 0.8693(4) 0.5193(3) 0.0534(4) 0.0541(12) Uani 1 1 d . . . H27 H 0.8186 0.5054 -0.0113 0.065 Uiso 1 1 calc R . . C28 C 0.9889(4) 0.5003(3) 0.0482(4) 0.0564(13) Uani 1 1 d . . . H28 H 1.0202 0.4736 -0.0208 0.068 Uiso 1 1 calc R . . C29 C 1.0605(4) 0.5197(3) 0.1407(4) 0.0553(13) Uani 1 1 d . . . H29 H 1.1416 0.5053 0.1368 0.066 Uiso 1 1 calc R . . C30 C 1.0163(3) 0.5606(3) 0.2419(4) 0.0433(11) Uani 1 1 d . . . H30 H 1.0678 0.5748 0.3058 0.052 Uiso 1 1 calc R . . C31 C 0.9077(3) 0.8045(3) 0.3572(3) 0.0309(9) Uani 1 1 d . . . C32 C 0.9686(3) 0.8381(3) 0.2614(4) 0.0462(11) Uani 1 1 d . . . H32 H 0.9448 0.8199 0.1845 0.055 Uiso 1 1 calc R . . C33 C 1.0642(4) 0.8984(3) 0.2783(5) 0.0566(14) Uani 1 1 d . . . H33 H 1.1062 0.9203 0.2126 0.068 Uiso 1 1 calc R . . C34 C 1.0985(3) 0.9263(3) 0.3872(5) 0.0561(13) Uani 1 1 d . . . H34 H 1.1640 0.9675 0.3975 0.067 Uiso 1 1 calc R . . C35 C 1.0386(4) 0.8950(3) 0.4824(5) 0.0522(12) Uani 1 1 d . . . H35 H 1.0623 0.9149 0.5587 0.063 Uiso 1 1 calc R . . C36 C 0.9427(3) 0.8340(3) 0.4671(4) 0.0411(10) Uani 1 1 d . . . H36 H 0.9012 0.8126 0.5333 0.049 Uiso 1 1 calc R . . Cl1 Cl 0.6317(3) 0.7869(3) 1.0275(3) 0.0992(12) Uani 0.647(4) 1 d PDU A 1 Cl2 Cl 0.8723(3) 0.7077(4) 0.7642(3) 0.0890(15) Uani 0.647(4) 1 d PDU A 1 C37 C 0.7616(7) 0.7714(8) 0.9504(7) 0.093(2) Uani 0.647(4) 1 d PDU A 1 H37A H 0.7976 0.8349 0.9363 0.111 Uiso 0.647(4) 1 calc PR A 1 H37B H 0.8175 0.7330 0.9983 0.111 Uiso 0.647(4) 1 calc PR A 1 C38 C 0.7392(7) 0.7212(10) 0.8339(10) 0.087(2) Uani 0.647(4) 1 d PDU A 1 H38A H 0.6848 0.7597 0.7845 0.104 Uiso 0.647(4) 1 calc PR A 1 H38B H 0.7032 0.6576 0.8469 0.104 Uiso 0.647(4) 1 calc PR A 1 Cl1B Cl 0.7321(13) 0.8219(10) 1.0210(10) 0.109(4) Uani 0.150(4) 1 d PDU B 2 Cl2B Cl 0.8594(16) 0.7630(14) 0.7585(19) 0.130(6) Uani 0.150(4) 1 d PDU B 2 C37B C 0.675(2) 0.769(2) 0.8948(15) 0.095(3) Uani 0.150(4) 1 d PDU B 2 H37C H 0.6956 0.6996 0.8927 0.114 Uiso 0.150(4) 1 calc PR B 2 H37D H 0.5892 0.7753 0.8906 0.114 Uiso 0.150(4) 1 calc PR B 2 C38B C 0.7323(16) 0.8226(15) 0.7932(14) 0.105(5) Uani 0.150(4) 1 d PDU B 2 H38C H 0.7503 0.8894 0.8167 0.126 Uiso 0.150(4) 1 calc PR B 2 H38D H 0.6781 0.8242 0.7246 0.126 Uiso 0.150(4) 1 calc PR B 2 Cl1C Cl 0.5996(12) 0.8304(10) 0.9864(12) 0.124(4) Uani 0.203(5) 1 d PDU C 3 Cl2C Cl 0.8587(16) 0.6882(17) 0.7967(17) 0.138(6) Uani 0.203(5) 1 d PDU C 3 C37C C 0.710(2) 0.8151(17) 0.886(2) 0.094(3) Uani 0.203(5) 1 d PDU C 3 H37E H 0.6919 0.8559 0.8166 0.113 Uiso 0.203(5) 1 calc PR C 3 H37F H 0.7844 0.8378 0.9210 0.113 Uiso 0.203(5) 1 calc PR C 3 C38C C 0.724(2) 0.722(2) 0.849(4) 0.090(3) Uani 0.203(5) 1 d PDU C 3 H38E H 0.6645 0.7091 0.7862 0.108 Uiso 0.203(5) 1 calc PR C 3 H38F H 0.7055 0.6789 0.9150 0.108 Uiso 0.203(5) 1 calc PR C 3 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 0.026(2) 0.034(3) 0.029(3) 0.001(2) 0.0046(19) 0.003(2) N1 0.0293(15) 0.0220(16) 0.0283(17) 0.0014(16) 0.0022(14) -0.0016(14) O1 0.0297(13) 0.0342(15) 0.0367(15) 0.0053(14) 0.0038(12) 0.0069(12) O2 0.0557(17) 0.056(2) 0.0403(18) 0.0097(16) -0.0046(15) 0.0137(16) O3 0.0660(18) 0.0304(16) 0.0389(17) -0.0103(15) 0.0070(15) -0.0033(14) O4 0.0382(14) 0.0237(14) 0.0374(16) -0.0011(13) 0.0094(12) 0.0043(12) O5 0.0277(12) 0.0252(14) 0.0376(16) -0.0028(13) 0.0076(11) -0.0016(12) O6 0.0291(13) 0.0240(14) 0.0488(17) -0.0001(13) 0.0122(12) -0.0023(12) C1 0.042(2) 0.039(2) 0.030(2) 0.001(2) 0.004(2) 0.016(2) C2 0.040(2) 0.024(2) 0.032(2) 0.0025(19) 0.0084(18) 0.0036(18) C3 0.036(2) 0.026(2) 0.033(2) -0.0048(19) -0.0010(18) -0.0039(18) C4 0.046(3) 0.022(2) 0.036(2) 0.003(2) 0.011(2) 0.000(2) C5 0.0269(17) 0.021(2) 0.033(2) -0.0027(18) 0.0018(17) 0.0002(17) C6 0.0245(18) 0.029(2) 0.040(2) -0.003(2) 0.0017(17) -0.0031(17) C7 0.0300(19) 0.041(2) 0.034(2) -0.003(2) 0.0061(18) 0.0006(19) C8 0.036(2) 0.038(2) 0.036(2) -0.005(2) 0.0004(19) 0.0077(19) C9 0.034(2) 0.038(2) 0.028(2) -0.007(2) -0.0004(18) 0.0055(19) C10 0.0265(18) 0.029(2) 0.039(2) -0.0035(19) 0.0015(17) 0.0006(17) C11 0.031(2) 0.059(3) 0.044(3) -0.010(2) -0.0028(19) -0.001(2) C12 0.045(2) 0.037(2) 0.031(2) 0.001(2) 0.0093(19) 0.007(2) C13 0.046(2) 0.061(3) 0.048(3) -0.014(2) 0.003(2) 0.019(2) C14 0.055(3) 0.034(3) 0.054(3) -0.002(2) 0.004(2) 0.010(2) C15 0.0294(18) 0.024(2) 0.030(2) -0.0059(18) 0.0036(18) -0.0009(16) C16 0.0263(18) 0.024(2) 0.033(2) 0.0084(19) 0.0039(17) -0.0045(17) C17 0.0295(19) 0.027(2) 0.044(2) 0.007(2) 0.0045(19) -0.0021(18) C18 0.035(2) 0.043(3) 0.061(3) 0.015(3) -0.002(2) 0.005(2) C19 0.059(3) 0.060(3) 0.050(3) 0.008(3) -0.022(3) 0.004(3) C20 0.053(3) 0.053(3) 0.044(3) 0.002(2) -0.007(2) -0.003(2) C21 0.036(2) 0.037(2) 0.036(2) 0.003(2) 0.0025(19) -0.003(2) C22 0.0296(19) 0.027(2) 0.032(2) -0.0010(19) 0.0054(17) -0.0011(17) C23 0.0221(17) 0.028(2) 0.036(2) 0.0023(18) 0.0055(17) -0.0014(17) C24 0.0267(18) 0.032(2) 0.034(2) -0.0002(19) 0.0031(17) -0.0011(18) C25 0.036(2) 0.025(2) 0.036(2) 0.003(2) 0.0096(19) -0.0034(19) C26 0.045(2) 0.036(3) 0.046(3) -0.006(2) 0.014(2) -0.004(2) C27 0.070(3) 0.050(3) 0.043(3) -0.011(3) 0.009(2) -0.011(3) C28 0.072(3) 0.051(3) 0.048(3) -0.010(3) 0.029(3) -0.007(3) C29 0.047(3) 0.056(3) 0.063(3) 0.007(3) 0.022(3) 0.006(2) C30 0.041(2) 0.048(3) 0.042(3) -0.002(2) 0.017(2) 0.002(2) C31 0.0233(18) 0.031(2) 0.039(3) 0.005(2) 0.0014(18) 0.0052(17) C32 0.036(2) 0.047(3) 0.056(3) 0.010(2) 0.010(2) 0.001(2) C33 0.036(2) 0.046(3) 0.088(4) 0.014(3) 0.024(3) -0.006(2) C34 0.028(2) 0.041(3) 0.100(4) -0.001(3) 0.000(3) -0.008(2) C35 0.040(2) 0.041(3) 0.076(4) -0.008(3) -0.013(3) -0.005(2) C36 0.042(2) 0.031(2) 0.050(3) 0.003(2) 0.002(2) -0.002(2) Cl1 0.089(2) 0.130(3) 0.078(2) -0.0205(19) 0.0050(16) 0.005(2) Cl2 0.0500(14) 0.159(4) 0.0581(18) 0.004(2) -0.0057(13) -0.002(2) C37 0.087(4) 0.094(5) 0.096(5) -0.003(4) -0.010(4) -0.006(4) C38 0.073(4) 0.095(4) 0.092(5) 0.001(4) 0.002(4) -0.001(4) Cl1B 0.120(7) 0.107(6) 0.099(6) -0.026(5) -0.002(6) -0.007(6) Cl2B 0.126(8) 0.130(9) 0.133(9) 0.009(7) 0.008(7) -0.014(7) C37B 0.090(5) 0.100(5) 0.096(5) -0.005(5) -0.003(5) -0.006(5) C38B 0.104(7) 0.106(7) 0.106(7) 0.000(7) 0.001(7) -0.006(7) Cl1C 0.128(7) 0.112(7) 0.131(7) -0.034(6) -0.011(6) -0.013(6) Cl2C 0.115(8) 0.158(8) 0.141(9) 0.028(7) -0.008(6) 0.016(6) C37C 0.091(5) 0.097(5) 0.093(5) 0.001(5) -0.001(5) -0.007(5) C38C 0.083(5) 0.094(5) 0.093(6) -0.001(5) -0.004(5) -0.005(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 O1 1.468(5) . ? B1 O4 1.481(5) . ? B1 C15 1.613(6) . ? B1 N1 1.671(5) . ? N1 C3 1.496(4) . ? N1 C2 1.508(4) . ? N1 C5 1.532(4) . ? O1 C1 1.347(4) . ? O2 C1 1.199(4) . ? O3 C4 1.208(4) . ? O4 C4 1.326(4) . ? O5 C22 1.421(4) . ? O5 C23 1.433(4) . ? O6 C24 1.440(4) . ? O6 C22 1.453(4) . ? C1 C2 1.507(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.517(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C5 C6 1.561(4) . ? C5 C10 1.566(5) . ? C5 H5 1.0000 . ? C6 C11 1.533(5) . ? C6 C7 1.538(5) . ? C6 H6 1.0000 . ? C7 C12 1.532(5) . ? C7 C8 1.561(6) . ? C7 H7 1.0000 . ? C8 C14 1.528(6) . ? C8 C13 1.537(5) . ? C8 C9 1.565(5) . ? C9 C12 1.522(5) . ? C9 C10 1.533(5) . ? C9 H9 1.0000 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C22 1.519(5) . ? C15 C16 1.525(5) . ? C15 H15 1.0000 . ? C16 C21 1.385(5) . ? C16 C17 1.396(5) . ? C17 C18 1.378(5) . ? C17 H17 0.9500 . ? C18 C19 1.374(6) . ? C18 H18 0.9500 . ? C19 C20 1.376(6) . ? C19 H19 0.9500 . ? C20 C21 1.389(5) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 H22 1.0000 . ? C23 C25 1.493(5) . ? C23 C24 1.543(5) . ? C23 H23 1.0000 . ? C24 C31 1.506(5) . ? C24 H24 1.0000 . ? C25 C30 1.383(5) . ? C25 C26 1.381(5) . ? C26 C27 1.402(5) . ? C26 H26 0.9500 . ? C27 C28 1.395(6) . ? C27 H27 0.9500 . ? C28 C29 1.351(6) . ? C28 H28 0.9500 . ? C29 C30 1.396(5) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.374(5) . ? C31 C32 1.393(5) . ? C32 C33 1.388(6) . ? C32 H32 0.9500 . ? C33 C34 1.355(7) . ? C33 H33 0.9500 . ? C34 C35 1.370(6) . ? C34 H34 0.9500 . ? C35 C36 1.396(5) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? Cl1 C37 1.756(7) . ? Cl2 C38 1.743(6) . ? C37 C38 1.524(7) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? Cl1B C37B 1.736(10) . ? Cl2B C38B 1.727(9) . ? C37B C38B 1.539(10) . ? C37B H37C 0.9900 . ? C37B H37D 0.9900 . ? C38B H38C 0.9900 . ? C38B H38D 0.9900 . ? Cl1C C37C 1.737(9) . ? Cl2C C38C 1.728(9) . ? C37C C38C 1.380(18) . ? C37C H37E 0.9900 . ? C37C H37F 0.9900 . ? C38C H38E 0.9900 . ? C38C H38F 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 B1 O4 110.3(3) . . ? O1 B1 C15 113.2(3) . . ? O4 B1 C15 113.9(3) . . ? O1 B1 N1 102.1(3) . . ? O4 B1 N1 99.4(3) . . ? C15 B1 N1 116.6(3) . . ? C3 N1 C2 111.5(3) . . ? C3 N1 C5 112.4(3) . . ? C2 N1 C5 113.5(3) . . ? C3 N1 B1 101.3(2) . . ? C2 N1 B1 99.2(3) . . ? C5 N1 B1 117.7(3) . . ? C1 O1 B1 112.1(3) . . ? C4 O4 B1 113.4(3) . . ? C22 O5 C23 103.6(2) . . ? C24 O6 C22 107.7(2) . . ? O2 C1 O1 123.6(4) . . ? O2 C1 C2 126.1(4) . . ? O1 C1 C2 110.3(3) . . ? C1 C2 N1 106.4(3) . . ? C1 C2 H2A 110.5 . . ? N1 C2 H2A 110.5 . . ? C1 C2 H2B 110.5 . . ? N1 C2 H2B 110.5 . . ? H2A C2 H2B 108.6 . . ? N1 C3 C4 105.2(3) . . ? N1 C3 H3A 110.7 . . ? C4 C3 H3A 110.7 . . ? N1 C3 H3B 110.7 . . ? C4 C3 H3B 110.7 . . ? H3A C3 H3B 108.8 . . ? O3 C4 O4 124.5(4) . . ? O3 C4 C3 125.1(4) . . ? O4 C4 C3 110.4(3) . . ? N1 C5 C6 112.5(3) . . ? N1 C5 C10 111.8(3) . . ? C6 C5 C10 114.6(3) . . ? N1 C5 H5 105.7 . . ? C6 C5 H5 105.7 . . ? C10 C5 H5 105.7 . . ? C11 C6 C7 111.0(3) . . ? C11 C6 C5 112.5(3) . . ? C7 C6 C5 111.3(3) . . ? C11 C6 H6 107.3 . . ? C7 C6 H6 107.3 . . ? C5 C6 H6 107.3 . . ? C12 C7 C6 109.5(3) . . ? C12 C7 C8 87.3(3) . . ? C6 C7 C8 114.8(3) . . ? C12 C7 H7 114.1 . . ? C6 C7 H7 114.1 . . ? C8 C7 H7 114.1 . . ? C14 C8 C13 107.6(3) . . ? C14 C8 C7 122.6(3) . . ? C13 C8 C7 110.6(3) . . ? C14 C8 C9 118.4(3) . . ? C13 C8 C9 111.8(3) . . ? C7 C8 C9 84.3(3) . . ? C12 C9 C10 110.1(3) . . ? C12 C9 C8 87.5(3) . . ? C10 C9 C8 110.6(3) . . ? C12 C9 H9 115.2 . . ? C10 C9 H9 115.2 . . ? C8 C9 H9 115.2 . . ? C9 C10 C5 113.7(3) . . ? C9 C10 H10A 108.8 . . ? C5 C10 H10A 108.8 . . ? C9 C10 H10B 108.8 . . ? C5 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 C7 86.8(3) . . ? C9 C12 H12A 114.2 . . ? C7 C12 H12A 114.2 . . ? C9 C12 H12B 114.2 . . ? C7 C12 H12B 114.2 . . ? H12A C12 H12B 111.4 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C8 C14 H14A 109.5 . . ? C8 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C8 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C22 C15 C16 114.1(3) . . ? C22 C15 B1 110.7(3) . . ? C16 C15 B1 113.4(3) . . ? C22 C15 H15 106.0 . . ? C16 C15 H15 106.0 . . ? B1 C15 H15 106.0 . . ? C21 C16 C17 117.9(3) . . ? C21 C16 C15 122.3(3) . . ? C17 C16 C15 119.8(3) . . ? C18 C17 C16 121.2(4) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 119.8(4) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C18 C19 C20 120.4(4) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C19 C20 C21 119.6(4) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C16 C21 C20 121.1(4) . . ? C16 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? O5 C22 O6 104.9(3) . . ? O5 C22 C15 112.4(3) . . ? O6 C22 C15 110.6(3) . . ? O5 C22 H22 109.6 . . ? O6 C22 H22 109.6 . . ? C15 C22 H22 109.6 . . ? O5 C23 C25 111.9(3) . . ? O5 C23 C24 101.9(2) . . ? C25 C23 C24 114.5(3) . . ? O5 C23 H23 109.4 . . ? C25 C23 H23 109.4 . . ? C24 C23 H23 109.4 . . ? O6 C24 C31 112.3(3) . . ? O6 C24 C23 103.3(3) . . ? C31 C24 C23 112.9(3) . . ? O6 C24 H24 109.4 . . ? C31 C24 H24 109.4 . . ? C23 C24 H24 109.4 . . ? C30 C25 C26 118.4(4) . . ? C30 C25 C23 120.2(4) . . ? C26 C25 C23 121.4(3) . . ? C25 C26 C27 121.3(4) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C26 C27 C28 118.6(4) . . ? C26 C27 H27 120.7 . . ? C28 C27 H27 120.7 . . ? C29 C28 C27 120.4(4) . . ? C29 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? C28 C29 C30 120.5(4) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C25 C30 C29 120.7(4) . . ? C25 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C36 C31 C32 118.6(4) . . ? C36 C31 C24 121.7(3) . . ? C32 C31 C24 119.6(4) . . ? C31 C32 C33 120.0(4) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C34 C33 C32 120.8(4) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C33 C34 C35 120.1(4) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C34 C35 C36 119.9(5) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C31 C36 C35 120.6(4) . . ? C31 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C38 C37 Cl1 111.6(6) . . ? C38 C37 H37A 109.3 . . ? Cl1 C37 H37A 109.3 . . ? C38 C37 H37B 109.3 . . ? Cl1 C37 H37B 109.3 . . ? H37A C37 H37B 108.0 . . ? C37 C38 Cl2 108.5(6) . . ? C37 C38 H38A 110.0 . . ? Cl2 C38 H38A 110.0 . . ? C37 C38 H38B 110.0 . . ? Cl2 C38 H38B 110.0 . . ? H38A C38 H38B 108.4 . . ? C38B C37B Cl1B 105.2(11) . . ? C38B C37B H37C 110.7 . . ? Cl1B C37B H37C 110.7 . . ? C38B C37B H37D 110.7 . . ? Cl1B C37B H37D 110.7 . . ? H37C C37B H37D 108.8 . . ? C37B C38B Cl2B 108.1(11) . . ? C37B C38B H38C 110.1 . . ? Cl2B C38B H38C 110.1 . . ? C37B C38B H38D 110.1 . . ? Cl2B C38B H38D 110.1 . . ? H38C C38B H38D 108.4 . . ? C38C C37C Cl1C 114.2(13) . . ? C38C C37C H37E 108.7 . . ? Cl1C C37C H37E 108.7 . . ? C38C C37C H37F 108.7 . . ? Cl1C C37C H37F 108.7 . . ? H37E C37C H37F 107.6 . . ? C37C C38C Cl2C 118.2(15) . . ? C37C C38C H38E 107.8 . . ? Cl2C C38C H38E 107.8 . . ? C37C C38C H38F 107.8 . . ? Cl2C C38C H38F 107.8 . . ? H38E C38C H38F 107.1 . . ? 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 O1 B1 N1 C3 -143.9(3) . . . . ? O4 B1 N1 C3 -30.7(3) . . . . ? C15 B1 N1 C3 92.1(4) . . . . ? O1 B1 N1 C2 -29.7(3) . . . . ? O4 B1 N1 C2 83.6(3) . . . . ? C15 B1 N1 C2 -153.7(3) . . . . ? O1 B1 N1 C5 93.1(3) . . . . ? O4 B1 N1 C5 -153.6(3) . . . . ? C15 B1 N1 C5 -30.8(4) . . . . ? O4 B1 O1 C1 -83.8(3) . . . . ? C15 B1 O1 C1 147.3(3) . . . . ? N1 B1 O1 C1 21.1(4) . . . . ? O1 B1 O4 C4 130.4(3) . . . . ? C15 B1 O4 C4 -101.0(4) . . . . ? N1 B1 O4 C4 23.7(4) . . . . ? B1 O1 C1 O2 179.1(4) . . . . ? B1 O1 C1 C2 -3.3(4) . . . . ? O2 C1 C2 N1 159.1(4) . . . . ? O1 C1 C2 N1 -18.3(4) . . . . ? C3 N1 C2 C1 134.5(3) . . . . ? C5 N1 C2 C1 -97.4(3) . . . . ? B1 N1 C2 C1 28.4(3) . . . . ? C2 N1 C3 C4 -76.8(3) . . . . ? C5 N1 C3 C4 154.4(3) . . . . ? B1 N1 C3 C4 27.9(3) . . . . ? B1 O4 C4 O3 172.0(3) . . . . ? B1 O4 C4 C3 -7.0(4) . . . . ? N1 C3 C4 O3 165.4(3) . . . . ? N1 C3 C4 O4 -15.5(4) . . . . ? C3 N1 C5 C6 51.2(4) . . . . ? C2 N1 C5 C6 -76.5(3) . . . . ? B1 N1 C5 C6 168.3(3) . . . . ? C3 N1 C5 C10 -178.1(3) . . . . ? C2 N1 C5 C10 54.2(3) . . . . ? B1 N1 C5 C10 -61.0(4) . . . . ? N1 C5 C6 C11 -98.0(4) . . . . ? C10 C5 C6 C11 132.8(3) . . . . ? N1 C5 C6 C7 136.7(3) . . . . ? C10 C5 C6 C7 7.5(4) . . . . ? C11 C6 C7 C12 -179.7(3) . . . . ? C5 C6 C7 C12 -53.6(4) . . . . ? C11 C6 C7 C8 -83.5(4) . . . . ? C5 C6 C7 C8 42.7(4) . . . . ? C12 C7 C8 C14 147.8(3) . . . . ? C6 C7 C8 C14 37.5(5) . . . . ? C12 C7 C8 C13 -83.6(3) . . . . ? C6 C7 C8 C13 166.1(3) . . . . ? C12 C7 C8 C9 27.5(3) . . . . ? C6 C7 C8 C9 -82.8(3) . . . . ? C14 C8 C9 C12 -151.9(3) . . . . ? C13 C8 C9 C12 82.2(4) . . . . ? C7 C8 C9 C12 -27.7(3) . . . . ? C14 C8 C9 C10 -41.3(5) . . . . ? C13 C8 C9 C10 -167.2(3) . . . . ? C7 C8 C9 C10 82.9(3) . . . . ? C12 C9 C10 C5 47.8(4) . . . . ? C8 C9 C10 C5 -47.2(4) . . . . ? N1 C5 C10 C9 -134.5(3) . . . . ? C6 C5 C10 C9 -4.9(4) . . . . ? C10 C9 C12 C7 -82.9(3) . . . . ? C8 C9 C12 C7 28.2(3) . . . . ? C6 C7 C12 C9 87.2(3) . . . . ? C8 C7 C12 C9 -28.3(3) . . . . ? O1 B1 C15 C22 50.4(4) . . . . ? O4 B1 C15 C22 -76.6(4) . . . . ? N1 B1 C15 C22 168.5(3) . . . . ? O1 B1 C15 C16 -179.8(3) . . . . ? O4 B1 C15 C16 53.1(4) . . . . ? N1 B1 C15 C16 -61.8(4) . . . . ? C22 C15 C16 C21 62.0(4) . . . . ? B1 C15 C16 C21 -66.0(4) . . . . ? C22 C15 C16 C17 -121.0(3) . . . . ? B1 C15 C16 C17 111.0(4) . . . . ? C21 C16 C17 C18 2.0(5) . . . . ? C15 C16 C17 C18 -175.2(3) . . . . ? C16 C17 C18 C19 -2.4(6) . . . . ? C17 C18 C19 C20 1.5(7) . . . . ? C18 C19 C20 C21 -0.3(7) . . . . ? C17 C16 C21 C20 -0.8(5) . . . . ? C15 C16 C21 C20 176.3(3) . . . . ? C19 C20 C21 C16 0.0(6) . . . . ? C23 O5 C22 O6 40.5(3) . . . . ? C23 O5 C22 C15 160.7(3) . . . . ? C24 O6 C22 O5 -21.4(3) . . . . ? C24 O6 C22 C15 -142.7(3) . . . . ? C16 C15 C22 O5 -66.5(4) . . . . ? B1 C15 C22 O5 62.8(4) . . . . ? C16 C15 C22 O6 50.3(4) . . . . ? B1 C15 C22 O6 179.7(3) . . . . ? C22 O5 C23 C25 -165.3(3) . . . . ? C22 O5 C23 C24 -42.4(3) . . . . ? C22 O6 C24 C31 -126.7(3) . . . . ? C22 O6 C24 C23 -4.7(3) . . . . ? O5 C23 C24 O6 28.7(3) . . . . ? C25 C23 C24 O6 149.8(3) . . . . ? O5 C23 C24 C31 150.2(3) . . . . ? C25 C23 C24 C31 -88.7(4) . . . . ? O5 C23 C25 C30 -134.5(4) . . . . ? C24 C23 C25 C30 110.1(4) . . . . ? O5 C23 C25 C26 48.0(5) . . . . ? C24 C23 C25 C26 -67.4(4) . . . . ? C30 C25 C26 C27 -0.8(6) . . . . ? C23 C25 C26 C27 176.8(4) . . . . ? C25 C26 C27 C28 0.7(6) . . . . ? C26 C27 C28 C29 0.4(7) . . . . ? C27 C28 C29 C30 -1.2(7) . . . . ? C26 C25 C30 C29 -0.1(6) . . . . ? C23 C25 C30 C29 -177.7(4) . . . . ? C28 C29 C30 C25 1.1(7) . . . . ? O6 C24 C31 C36 35.8(5) . . . . ? C23 C24 C31 C36 -80.5(4) . . . . ? O6 C24 C31 C32 -148.4(3) . . . . ? C23 C24 C31 C32 95.4(4) . . . . ? C36 C31 C32 C33 1.5(6) . . . . ? C24 C31 C32 C33 -174.5(4) . . . . ? C31 C32 C33 C34 -1.0(6) . . . . ? C32 C33 C34 C35 0.0(7) . . . . ? C33 C34 C35 C36 0.4(6) . . . . ? C32 C31 C36 C35 -1.2(5) . . . . ? C24 C31 C36 C35 174.7(3) . . . . ? C34 C35 C36 C31 0.2(6) . . . . ? Cl1 C37 C38 Cl2 -179.4(7) . . . . ? Cl1B C37B C38B Cl2B 90.9(19) . . . . ? Cl1C C37C C38C Cl2C -155(3) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 0.999 _diffrn_standards_number ? _diffrn_standards_decay_% ? _diffrn_standards_interval_time ? _refine_diff_density_max 0.187 _refine_diff_density_min -0.224 _refine_diff_density_rms 0.042 _publ_requested_category o _publ_section_references ; Allen, F.H., Kennard, O., Watson, D.G., Brammer, L., Orpen, A.G., and Taylor, R. (1987). J. Chem. Soc. Perkin Trans. II. S1-S19. Bruker (2004). APEX2. Bruker AXS, Inc., Madison, Wisconsin, USA. Bruker (2005). SAINT, SHELXTL, XCIF, XPREP. Bruker AXS, Inc., Madison, Wisconsin, USA. Bruker (2007). SADABS, TWINABS. Bruker AXS, Inc., Madison, Wisconsin, USA. CrystalMaker (1994). CrystalMaker, a crystal and molecular structures program for Mac and Windows. CrystalMaker Software Ltd., Oxford, England (www.crystalmaker.com). Flack, H. D. (1983), Acta Cryst. A39, 876-881. Flack, H. D. (2000), J. Appl. Cryst., 33, 1143-1148. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122 ; _publ_section_figure_captions ; Figure 1. SHELXTL (Bruker, 2005) plot showing 35% probability ellipsoids for non-H atoms and circles of arbitrary size for H atoms. ; _publ_section_exptl_prep ; Crystals were grown from a solution of dichloroethane and hexane. ; _publ_section_exptl_refinement ; A structural model consisting of the host plus one disordered dichloroethane solvate molecule was developed. The dichloroethane solvate molecule was disordered over three sites. The sum of the occupancy of the three sites was restrained to one. Like C-CL bond distances and C-C-CL bond angles were restrained to be similiar (esd 0.01 and 0.02 respectively). The C-C bond was restrained to be 1.54 /%A (esd 0.01). Disorded sites were restrained so that the displacement parameters refined as approximately isotropic. Similar displacement amplitudes (esd 0.01) were imposed on disordered sites overlapping by less than the sum of van der Waals radii. H atom treatment - Methyl H atom positions, R-CH~3~, were optimized by rotation about R-C bonds with idealized C-H, R--H and H--H distances. Remaining 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~. On the basis of 3078 unmerged Friedel opposites, the absolute structure determination Flack parameter was not reliable (Flack, 1983 & 2000). The absolute structure of the molecule was set by the known stereochemistry of the bicycle. The stereochemistry of the bicycle is R, R, R, S for centers C5, C6, C7 and C9 restectively. These centers were set to the correct stereochemistry, and the remaining stereocenters at C15, C23, and C24 were found to be R, S, S respectively. ; _publ_contact_author ; Danielle L. Gray 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 dgray@illinois.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 'Gray, Danielle L.' ; University of Illinois School of Chemical Sciences, Box 59-1 505 South Mathews Avenue Urbana, Illinois 61801 USA ; 'Fuller, Amy L.' ; University of Illinois School of Chemical Sciences, Box 59-1 505 South Mathews Avenue Urbana, Illinois 61801 USA ; 'Gao, Yi-Gui' ; 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 1.00 0.00 0.00 0.0630 -1.00 0.00 0.00 0.0350 0.00 -1.00 0.00 0.1270 0.00 1.00 0.00 0.1220 0.00 0.00 1.00 0.0360 0.00 0.00 -1.00 0.0130