Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_e:\xray\spheres\ibutyl\squeeze\final _database_code_CSD 167522 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Atwood, J. L.' 'Barbour, Leonard J.' 'Jerga, Agostona' _publ_contact_author_name 'Prof J L Atwood' _publ_contact_author_address ; 123 Chemistry Building University of Missouri Columbia Missouri 65211 USA ; _publ_contact_author_email 'ATWOODJ@MISSOURI.EDU' _publ_section_title ; Hydrogen-bonded molecular capsules are stable in polar media ; _chemical_name_common C-isobutylpyrogallol[4]arene . 4(MeOH) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H72 O16' _chemical_formula_weight 905.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 34.84(2) _cell_length_b 34.84(2) _cell_length_c 24.04(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 25268(36) _cell_formula_units_Z 18 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.071 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8784 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9765 _exptl_absorpt_correction_T_max 0.9804 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34690 _diffrn_reflns_av_R_equivalents 0.2997 _diffrn_reflns_av_sigmaI/netI 0.2089 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 22.00 _reflns_number_total 6889 _reflns_number_gt 2274 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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_extinction_coef ? _refine_ls_number_reflns 6889 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2604 _refine_ls_R_factor_gt 0.1482 _refine_ls_wR_factor_ref 0.4166 _refine_ls_wR_factor_gt 0.3622 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.967 _refine_ls_shift/su_max 0.187 _refine_ls_shift/su_mean 0.034 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 C2D C 0.0142(3) 0.2370(3) 0.3403(6) 0.076(3) Uani 1 1 d . . . O1C O -0.1566(2) 0.1139(2) 0.4870(3) 0.095(2) Uani 1 1 d . . . O3B O -0.2049(2) 0.0418(2) 0.4240(3) 0.103(2) Uani 1 1 d . . . C4D C 0.0763(3) 0.2237(3) 0.3407(5) 0.081(3) Uani 1 1 d . . . O1D O 0.0637(2) 0.25398(19) 0.4232(3) 0.091(2) Uani 1 1 d . . . O3D O 0.0925(2) 0.1933(2) 0.2635(3) 0.094(2) Uani 1 1 d . . . O1B O -0.1776(2) -0.0196(2) 0.2615(3) 0.106(2) Uani 1 1 d . . . C7D C 0.0190(3) 0.1905(3) 0.2007(4) 0.089(3) Uani 1 1 d . . . H7D H 0.0468 0.1943 0.1836 0.107 Uiso 1 1 calc R . . O3C O -0.0086(2) 0.2311(2) 0.4876(3) 0.100(2) Uani 1 1 d . . . C7C C -0.0116(3) 0.2543(3) 0.3728(4) 0.075(3) Uani 1 1 d . . . H7C H 0.0093 0.2747 0.4017 0.089 Uiso 1 1 calc R . . O2B O -0.2077(2) -0.0277(2) 0.3682(3) 0.124(3) Uani 1 1 d . . . C6C C -0.0504(3) 0.2184(3) 0.4044(4) 0.058(2) Uani 1 1 d . . . O2D O 0.1103(2) 0.2230(2) 0.3693(3) 0.121(3) Uani 1 1 d . . . C6D C 0.0309(3) 0.2081(3) 0.2598(4) 0.059(2) Uani 1 1 d . . . C7A C -0.1435(3) 0.0643(3) 0.2022(5) 0.085(3) Uani 1 1 d . . . H7A H -0.1594 0.0336 0.1866 0.102 Uiso 1 1 calc R . . O3A O -0.1076(3) 0.0042(2) 0.1983(3) 0.112(3) Uani 1 1 d . . . O1A O 0.0426(2) 0.1218(3) 0.1986(3) 0.107(2) Uani 1 1 d . . . O2A O -0.0189(3) 0.0329(3) 0.1949(4) 0.152(4) Uani 1 1 d . . . O2C O -0.0784(3) 0.1634(3) 0.5392(3) 0.118(3) Uani 1 1 d . . . C5D C 0.0648(3) 0.2072(3) 0.2878(4) 0.064(3) Uani 1 1 d . . . C7B C -0.1712(3) 0.1301(3) 0.3732(4) 0.075(3) Uani 1 1 d . . . H7B H -0.1935 0.1167 0.4037 0.090 Uiso 1 1 calc R . . C3D C 0.0514(4) 0.2376(3) 0.3677(5) 0.078(3) Uani 1 1 d . . . C2B C -0.1589(3) 0.0593(3) 0.2595(4) 0.056(2) Uani 1 1 d . . . C4B C -0.1919(3) 0.0150(4) 0.3432(6) 0.102(4) Uani 1 1 d . . . C6B C -0.1729(3) 0.0903(3) 0.3420(4) 0.060(2) Uani 1 1 d . . . C3B C -0.1734(3) 0.0200(4) 0.2858(5) 0.090(3) Uani 1 1 d . . . C1A C -0.0608(3) 0.1242(3) 0.1990(3) 0.055(2) Uani 1 1 d . . . H1A H -0.0708 0.1450 0.2011 0.066 Uiso 1 1 calc R . . C4C C -0.0859(5) 0.1709(4) 0.4840(5) 0.092(4) Uani 1 1 d . . . C1B C -0.1565(2) 0.0933(3) 0.2894(4) 0.060(2) Uani 1 1 d . . . H1B H -0.1421 0.1218 0.2725 0.071 Uiso 1 1 calc R . . C2C C -0.1277(3) 0.1575(3) 0.4017(4) 0.055(2) Uiso 1 1 d . . . C1C C -0.0905(3) 0.1930(3) 0.3775(4) 0.065(3) Uani 1 1 d . . . H1C H -0.0928 0.2003 0.3400 0.078 Uiso 1 1 calc R . . C5C C -0.0470(4) 0.2076(3) 0.4593(4) 0.071(3) Uani 1 1 d . . . C1D C 0.0060(3) 0.2219(3) 0.2889(5) 0.067(3) Uani 1 1 d . . . H1D H -0.0189 0.2205 0.2707 0.081 Uiso 1 1 calc R . . C6A C -0.0918(3) 0.0796(3) 0.1968(3) 0.070(3) Uani 1 1 d . . . C3C C -0.1241(4) 0.1471(4) 0.4556(5) 0.087(3) Uani 1 1 d . . . C5B C -0.1898(4) 0.0485(4) 0.3709(5) 0.086(3) Uani 1 1 d . . . C2A C -0.0155(3) 0.1398(4) 0.1983(3) 0.074(3) Uani 1 1 d . . . C5A C -0.0772(4) 0.0498(3) 0.1972(4) 0.081(3) Uani 1 1 d . . . C4A C -0.0322(4) 0.0629(4) 0.1976(4) 0.090(3) Uiso 1 1 d . . . C3A C -0.0021(4) 0.1087(4) 0.1998(4) 0.091(3) Uani 1 1 d . . . C8D C 0.0041(4) 0.2181(4) 0.1638(5) 0.112(4) Uiso 1 1 d . . . H8D1 H -0.0220 0.2176 0.1806 0.134 Uiso 1 1 calc R . . H8D2 H -0.0042 0.2048 0.1262 0.134 Uiso 1 1 calc R . . C8B C -0.1857(4) 0.1559(4) 0.3394(5) 0.124(4) Uiso 1 1 d . . . H8B1 H -0.1794 0.1828 0.3605 0.149 Uiso 1 1 calc R . . H8B2 H -0.1677 0.1656 0.3050 0.149 Uiso 1 1 calc R . . C9A C -0.2063(4) 0.0715(4) 0.1580(5) 0.125(4) Uiso 1 1 d . . . H9A H -0.2142 0.0751 0.1969 0.150 Uiso 1 1 calc R . . C8A C -0.1550(3) 0.0908(3) 0.1638(4) 0.097(3) Uiso 1 1 d . . . H8A1 H -0.1424 0.0917 0.1266 0.116 Uiso 1 1 calc R . . H8A2 H -0.1412 0.1217 0.1777 0.116 Uiso 1 1 calc R . . C8C C -0.0233(4) 0.2834(4) 0.3356(5) 0.115(4) Uiso 1 1 d . . . H8C1 H -0.0423 0.2918 0.3570 0.138 Uiso 1 1 calc R . . H8C2 H -0.0407 0.2657 0.3032 0.138 Uiso 1 1 calc R . . C11A C -0.2182(4) 0.1009(4) 0.1273(5) 0.145(5) Uiso 1 1 d . . . H11A H -0.1975 0.1319 0.1371 0.217 Uiso 1 1 calc R . . H11B H -0.2485 0.0936 0.1372 0.217 Uiso 1 1 calc R . . H11C H -0.2167 0.0968 0.0872 0.217 Uiso 1 1 calc R . . C10A C -0.2313(7) 0.0241(7) 0.1523(8) 0.233(8) Uiso 1 1 d . . . H10A H -0.2202 0.0105 0.1787 0.350 Uiso 1 1 calc R . . H10B H -0.2281 0.0159 0.1143 0.350 Uiso 1 1 calc R . . H10C H -0.2627 0.0136 0.1599 0.350 Uiso 1 1 calc R . . C9B C -0.2323(6) 0.1325(6) 0.3240(7) 0.186(7) Uiso 1 1 d . . . H9B H -0.2437 0.1004 0.3164 0.223 Uiso 1 1 calc R . . C9C C 0.0198(4) 0.3279(4) 0.3135(5) 0.104(3) Uiso 1 1 d . . . H9C H 0.0427 0.3199 0.3027 0.124 Uiso 1 1 calc R . . C11B C -0.2537(9) 0.1401(8) 0.3777(11) 0.313(13) Uiso 1 1 d . . . H11D H -0.2860 0.1253 0.3731 0.470 Uiso 1 1 calc R . . H11E H -0.2419 0.1720 0.3831 0.470 Uiso 1 1 calc R . . H11F H -0.2466 0.1279 0.4102 0.470 Uiso 1 1 calc R . . C10C C 0.0359(5) 0.3562(5) 0.3634(6) 0.180(6) Uiso 1 1 d . . . H10D H 0.0422 0.3406 0.3928 0.270 Uiso 1 1 calc R . . H10E H 0.0132 0.3629 0.3762 0.270 Uiso 1 1 calc R . . H10F H 0.0631 0.3838 0.3542 0.270 Uiso 1 1 calc R . . C10B C -0.2361(9) 0.1564(9) 0.2745(11) 0.320(13) Uiso 1 1 d . . . H10G H -0.2670 0.1414 0.2617 0.479 Uiso 1 1 calc R . . H10H H -0.2170 0.1565 0.2446 0.479 Uiso 1 1 calc R . . H10I H -0.2270 0.1870 0.2848 0.479 Uiso 1 1 calc R . . C11C C 0.0102(6) 0.3450(6) 0.2669(8) 0.223(8) Uiso 1 1 d . . . H11G H 0.0016 0.3238 0.2362 0.335 Uiso 1 1 calc R . . H11H H 0.0364 0.3730 0.2563 0.335 Uiso 1 1 calc R . . H11I H -0.0143 0.3503 0.2754 0.335 Uiso 1 1 calc R . . C9D C 0.0441(7) 0.2679(7) 0.1593(9) 0.209(8) Uiso 1 1 d . . . H9D H 0.0561 0.2806 0.1968 0.251 Uiso 1 1 calc R . . C10D C 0.0742(10) 0.2637(10) 0.1286(13) 0.342(15) Uiso 1 1 d . . . H10J H 0.0849 0.2468 0.1496 0.513 Uiso 1 1 calc R . . H10K H 0.0991 0.2932 0.1200 0.513 Uiso 1 1 calc R . . H10L H 0.0603 0.2481 0.0939 0.513 Uiso 1 1 calc R . . C11D C 0.0149(9) 0.2878(9) 0.1336(10) 0.303(12) Uiso 1 1 d . . . H11J H -0.0045 0.2886 0.1625 0.455 Uiso 1 1 calc R . . H11K H -0.0031 0.2691 0.1028 0.455 Uiso 1 1 calc R . . H11L H 0.0347 0.3179 0.1199 0.455 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C2D 0.071(8) 0.034(5) 0.118(10) 0.015(6) -0.001(7) 0.023(5) O1C 0.082(5) 0.088(5) 0.113(5) 0.056(4) 0.032(4) 0.041(4) O3B 0.094(5) 0.098(6) 0.107(6) 0.032(4) 0.001(5) 0.039(4) C4D 0.071(7) 0.080(7) 0.112(9) -0.006(7) -0.022(7) 0.053(6) O1D 0.108(5) 0.059(4) 0.092(5) -0.006(4) -0.037(4) 0.032(4) O3D 0.065(4) 0.084(5) 0.136(6) -0.013(4) 0.000(4) 0.041(4) O1B 0.112(6) 0.066(5) 0.145(6) -0.019(4) -0.031(5) 0.048(4) C7D 0.075(7) 0.098(8) 0.105(9) 0.030(7) -0.010(6) 0.052(7) O3C 0.098(5) 0.087(5) 0.127(6) -0.043(4) -0.043(5) 0.055(4) C7C 0.079(7) 0.059(6) 0.103(7) 0.022(6) -0.020(6) 0.048(6) O2B 0.121(6) 0.066(5) 0.152(7) 0.046(5) -0.005(5) 0.022(4) C6C 0.041(6) 0.044(5) 0.097(8) 0.007(5) -0.029(6) 0.028(5) O2D 0.062(4) 0.141(7) 0.175(7) 0.035(5) -0.016(5) 0.061(5) C6D 0.063(6) 0.043(5) 0.054(6) 0.028(5) -0.007(6) 0.014(5) C7A 0.082(8) 0.072(7) 0.117(9) 0.002(6) -0.042(7) 0.051(6) O3A 0.154(7) 0.055(5) 0.135(6) -0.021(4) -0.033(5) 0.058(5) O1A 0.084(5) 0.160(7) 0.115(5) 0.012(5) 0.008(4) 0.090(5) O2A 0.147(7) 0.107(6) 0.257(10) -0.006(6) -0.004(6) 0.104(6) O2C 0.153(7) 0.132(6) 0.098(6) 0.024(5) 0.000(5) 0.094(6) C5D 0.076(7) 0.055(6) 0.069(7) 0.035(5) 0.011(6) 0.040(6) C7B 0.072(7) 0.086(7) 0.098(7) 0.020(6) -0.009(5) 0.063(6) C3D 0.074(7) 0.050(6) 0.102(9) -0.010(6) -0.002(7) 0.025(6) C2B 0.073(7) 0.016(5) 0.073(7) 0.018(5) -0.008(5) 0.017(5) C4B 0.058(7) 0.104(11) 0.130(12) 0.059(10) -0.021(7) 0.030(7) C6B 0.023(5) 0.063(7) 0.094(8) 0.014(6) -0.003(5) 0.020(5) C3B 0.064(7) 0.111(11) 0.104(9) -0.016(8) -0.036(7) 0.051(7) C1A 0.052(6) 0.067(7) 0.062(6) 0.009(5) -0.007(5) 0.041(5) C4C 0.151(12) 0.060(8) 0.085(9) 0.037(7) 0.031(9) 0.067(9) C1B 0.034(5) 0.045(6) 0.096(8) 0.023(6) 0.002(5) 0.018(4) C1C 0.099(8) 0.069(6) 0.058(5) 0.009(5) 0.000(6) 0.065(6) C5C 0.090(8) 0.065(7) 0.081(8) -0.027(6) -0.029(7) 0.056(7) C1D 0.055(6) 0.076(7) 0.072(7) 0.013(6) -0.001(6) 0.034(6) C6A 0.103(8) 0.057(7) 0.068(6) -0.018(5) -0.045(6) 0.053(7) C3C 0.076(8) 0.062(7) 0.096(9) -0.006(7) 0.010(7) 0.014(6) C5B 0.101(9) 0.047(7) 0.096(9) -0.001(7) 0.019(7) 0.026(6) C2A 0.068(7) 0.094(8) 0.062(6) 0.024(5) 0.023(5) 0.041(7) C5A 0.102(8) 0.054(7) 0.094(7) 0.002(5) 0.030(6) 0.043(6) C3A 0.092(9) 0.136(11) 0.083(7) -0.007(7) -0.002(6) 0.086(9) _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 C2D C1D 1.315(12) . ? C2D C3D 1.447(13) . ? C2D C7C 1.526(13) . ? O1C C3C 1.371(11) . ? O3B C5B 1.357(11) . ? C4D C3D 1.353(12) . ? C4D O2D 1.379(10) . ? C4D C5D 1.370(12) . ? O1D C3D 1.430(11) . ? O3D C5D 1.403(10) . ? O1B C3B 1.437(12) . ? C7D C6D 1.521(12) . ? C7D C8D 1.573(13) . ? C7D C2A 1.564(13) . ? O3C C5C 1.351(10) . ? C7C C6C 1.509(11) . ? C7C C8C 1.551(12) . ? O2B C4B 1.436(12) . ? C6C C1C 1.384(11) . ? C6C C5C 1.392(12) . ? C6D C1D 1.378(12) . ? C6D C5D 1.374(11) . ? C7A C2B 1.457(12) . ? C7A C8A 1.494(12) . ? C7A C6A 1.608(13) . ? O3A C5A 1.399(10) . ? O1A C3A 1.386(11) . ? O2A C4A 1.340(12) . ? O2C C4C 1.400(12) . ? C7B C8B 1.475(13) . ? C7B C2C 1.495(11) . ? C7B C6B 1.549(12) . ? C2B C3B 1.357(13) . ? C2B C1B 1.352(11) . ? C4B C5B 1.314(15) . ? C4B C3B 1.494(15) . ? C6B C1B 1.369(11) . ? C6B C5B 1.447(13) . ? C1A C6A 1.380(11) . ? C1A C2A 1.390(11) . ? C4C C3C 1.351(14) . ? C4C C5C 1.448(14) . ? C2C C3C 1.367(13) . ? C2C C1C 1.395(11) . ? C6A C5A 1.367(11) . ? C2A C3A 1.378(13) . ? C5A C4A 1.398(13) . ? C4A C3A 1.404(14) . ? C8D C9D 1.59(2) . ? C8B C9B 1.454(18) . ? C9A C10A 1.437(19) . ? C9A C11A 1.484(15) . ? C9A C8A 1.570(14) . ? C8C C9C 1.617(14) . ? C9B C10B 1.50(3) . ? C9B C11B 1.58(3) . ? C9C C11C 1.386(17) . ? C9C C10C 1.472(15) . ? C9D C10D 1.35(3) . ? C9D C11D 1.61(3) . ? 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 C1D C2D C3D 116.6(10) . . ? C1D C2D C7C 125.9(10) . . ? C3D C2D C7C 117.5(11) . . ? C3D C4D O2D 118.4(11) . . ? C3D C4D C5D 119.5(10) . . ? O2D C4D C5D 121.9(10) . . ? C6D C7D C8D 112.9(9) . . ? C6D C7D C2A 113.0(7) . . ? C8D C7D C2A 111.6(8) . . ? C6C C7C C2D 112.9(7) . . ? C6C C7C C8C 114.5(8) . . ? C2D C7C C8C 111.2(8) . . ? C1C C6C C5C 117.8(9) . . ? C1C C6C C7C 119.5(8) . . ? C5C C6C C7C 122.6(8) . . ? C1D C6D C5D 117.4(9) . . ? C1D C6D C7D 121.5(9) . . ? C5D C6D C7D 120.9(10) . . ? C2B C7A C8A 117.6(9) . . ? C2B C7A C6A 113.6(7) . . ? C8A C7A C6A 110.3(8) . . ? C6D C5D C4D 121.2(10) . . ? C6D C5D O3D 123.4(10) . . ? C4D C5D O3D 115.2(9) . . ? C8B C7B C2C 114.1(9) . . ? C8B C7B C6B 114.0(9) . . ? C2C C7B C6B 111.6(6) . . ? C4D C3D O1D 118.3(11) . . ? C4D C3D C2D 120.4(10) . . ? O1D C3D C2D 121.3(10) . . ? C3B C2B C1B 117.7(10) . . ? C3B C2B C7A 119.4(10) . . ? C1B C2B C7A 122.7(8) . . ? C5B C4B O2B 122.0(13) . . ? C5B C4B C3B 122.4(11) . . ? O2B C4B C3B 115.2(14) . . ? C1B C6B C5B 117.6(9) . . ? C1B C6B C7B 123.4(9) . . ? C5B C6B C7B 118.8(10) . . ? C2B C3B O1B 126.0(11) . . ? C2B C3B C4B 117.9(11) . . ? O1B C3B C4B 115.7(12) . . ? C6A C1A C2A 122.4(8) . . ? C3C C4C O2C 125.7(11) . . ? C3C C4C C5C 122.3(10) . . ? O2C C4C C5C 112.0(13) . . ? C2B C1B C6B 125.8(8) . . ? C3C C2C C1C 117.6(9) . . ? C3C C2C C7B 117.5(9) . . ? C1C C2C C7B 124.8(9) . . ? C6C C1C C2C 124.3(8) . . ? O3C C5C C6C 120.4(10) . . ? O3C C5C C4C 122.3(11) . . ? C6C C5C C4C 117.3(10) . . ? C2D C1D C6D 124.6(9) . . ? C5A C6A C1A 118.4(9) . . ? C5A C6A C7A 122.0(9) . . ? C1A C6A C7A 119.1(8) . . ? C4C C3C O1C 112.5(10) . . ? C4C C3C C2C 120.6(10) . . ? O1C C3C C2C 126.9(11) . . ? C4B C5B O3B 118.7(11) . . ? C4B C5B C6B 117.7(11) . . ? O3B C5B C6B 123.6(10) . . ? C3A C2A C1A 117.3(10) . . ? C3A C2A C7D 121.1(9) . . ? C1A C2A C7D 121.4(9) . . ? C6A C5A O3A 120.3(9) . . ? C6A C5A C4A 122.3(10) . . ? O3A C5A C4A 117.4(9) . . ? O2A C4A C3A 122.3(11) . . ? O2A C4A C5A 120.8(11) . . ? C3A C4A C5A 116.9(11) . . ? C2A C3A O1A 120.4(11) . . ? C2A C3A C4A 122.5(10) . . ? O1A C3A C4A 116.9(10) . . ? C7D C8D C9D 109.1(11) . . ? C9B C8B C7B 115.2(12) . . ? C10A C9A C11A 121.9(13) . . ? C10A C9A C8A 114.1(13) . . ? C11A C9A C8A 113.6(11) . . ? C7A C8A C9A 112.8(9) . . ? C7C C8C C9C 113.2(9) . . ? C8B C9B C10B 106.1(17) . . ? C8B C9B C11B 100.8(15) . . ? C10B C9B C11B 112.0(18) . . ? C11C C9C C10C 117.6(13) . . ? C11C C9C C8C 111.6(12) . . ? C10C C9C C8C 103.6(10) . . ? C10D C9D C8D 103(2) . . ? C10D C9D C11D 122(2) . . ? C8D C9D C11D 95.7(15) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.498 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.088