# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2002 _chemical_name_systematic ; 5,17-Di-(N-p-tert-butyl-N-hydroxyamino)-11,23-di-bromo- 25,26,27,28-tetramethoxycalix(4)arene ; _chemical_name_common ? _chemical_melting_point 230 _chemical_formula_moiety ? _chemical_formula_sum 'C40 H48 Br2 N2 O6' _chemical_formula_weight 812.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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' _cell_length_a 32.255(7) _cell_length_b 14.394(3) _cell_length_c 21.753(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.210(9) _cell_angle_gamma 90.00 _cell_volume 9478(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 5 _cell_measurement_theta_max 12 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.139 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3360 _exptl_absorpt_coefficient_mu 1.749 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 Bruker P4 _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 5917 _diffrn_reflns_av_R_equivalents 0.0607 _diffrn_reflns_av_sigmaI/netI 0.0984 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 22.00 _reflns_number_total 5803 _reflns_number_gt 3081 _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^)+(0.0300P)^2^+75.0000P] 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 5803 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1467 _refine_ls_R_factor_gt 0.0738 _refine_ls_wR_factor_ref 0.1805 _refine_ls_wR_factor_gt 0.1603 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 0.21768(4) 0.56649(8) 0.10776(5) 0.0814(4) Uani 1 1 d . . . Br2 Br 0.34483(4) 0.44894(11) 0.63410(6) 0.1257(6) Uani 1 1 d . . . O1 O 0.0748(2) 0.5624(5) 0.2271(3) 0.0747(18) Uani 1 1 d . . . O2 O 0.1928(2) 0.3212(4) 0.2589(3) 0.0734(18) Uani 1 1 d . . . O3 O 0.0602(2) 0.4701(5) 0.3880(3) 0.092(2) Uani 1 1 d . . . H3B H 0.0667 0.5247 0.3972 0.111 Uiso 1 1 calc R . . O4 O 0.23186(17) 0.5139(4) 0.3535(3) 0.0568(15) Uani 1 1 d . . . O5 O 0.21432(19) 0.7477(4) 0.3046(3) 0.0637(16) Uani 1 1 d . . . O6 O 0.1348(2) 0.5695(5) 0.5001(3) 0.0833(19) Uani 1 1 d . . . H6A H 0.1293 0.5145 0.4911 0.100 Uiso 1 1 calc R . . N1 N 0.0976(2) 0.4110(5) 0.4239(3) 0.061(2) Uani 1 1 d . . . N2 N 0.1076(2) 0.6273(5) 0.4453(3) 0.0582(19) Uani 1 1 d . . . C1 C 0.1220(3) 0.7321(6) 0.2366(4) 0.069(3) Uani 1 1 d . . . H1A H 0.1350 0.7864 0.2241 0.083 Uiso 1 1 calc R . . H1B H 0.0905 0.7425 0.2249 0.083 Uiso 1 1 calc R . . C2 C 0.1305(3) 0.6455(7) 0.2015(4) 0.060(2) Uani 1 1 d . . . C3 C 0.1630(3) 0.6456(7) 0.1717(4) 0.063(3) Uani 1 1 d . . . H3A H 0.1774 0.7004 0.1686 0.075 Uiso 1 1 calc R . . C4 C 0.1731(3) 0.5649(8) 0.1476(4) 0.062(2) Uani 1 1 d . . . C5 C 0.1552(3) 0.4814(7) 0.1536(4) 0.068(3) Uani 1 1 d . . . H5A H 0.1645 0.4270 0.1392 0.082 Uiso 1 1 calc R . . C6 C 0.1217(3) 0.4795(7) 0.1829(4) 0.062(3) Uani 1 1 d . . . C7 C 0.1092(3) 0.5629(8) 0.2025(4) 0.061(2) Uani 1 1 d . . . C8 C 0.0322(3) 0.5719(10) 0.1803(5) 0.125(5) Uani 1 1 d . . . H8A H 0.0108 0.5730 0.2020 0.188 Uiso 1 1 calc R . . H8B H 0.0262 0.5205 0.1504 0.188 Uiso 1 1 calc R . . H8C H 0.0305 0.6288 0.1565 0.188 Uiso 1 1 calc R . . C9 C 0.1046(3) 0.3859(7) 0.1977(4) 0.077(3) Uani 1 1 d . . . H9A H 0.1129 0.3367 0.1738 0.092 Uiso 1 1 calc R . . H9B H 0.0726 0.3873 0.1844 0.092 Uiso 1 1 calc R . . C10 C 0.1251(3) 0.3683(6) 0.2719(4) 0.061(3) Uani 1 1 d . . . C11 C 0.1008(3) 0.3867(6) 0.3130(4) 0.062(2) Uani 1 1 d . . . H11A H 0.0708 0.4000 0.2946 0.074 Uiso 1 1 calc R . . C12 C 0.1206(3) 0.3854(6) 0.3799(4) 0.060(2) Uani 1 1 d . . . C13 C 0.1656(3) 0.3659(6) 0.4070(4) 0.057(2) Uani 1 1 d . . . H13A H 0.1793 0.3687 0.4522 0.068 Uiso 1 1 calc R . . C14 C 0.1907(3) 0.3426(6) 0.3687(4) 0.055(2) Uani 1 1 d . . . C15 C 0.1690(3) 0.3421(6) 0.3005(5) 0.063(3) Uani 1 1 d . . . C16 C 0.1935(4) 0.2237(7) 0.2460(5) 0.096(4) Uani 1 1 d . . . H16A H 0.2104 0.2130 0.2179 0.143 Uiso 1 1 calc R . . H16B H 0.1639 0.2018 0.2249 0.143 Uiso 1 1 calc R . . H16C H 0.2068 0.1909 0.2865 0.143 Uiso 1 1 calc R . . C17 C 0.0771(3) 0.3306(8) 0.4485(5) 0.077(3) Uani 1 1 d . . . C18 C 0.0417(4) 0.2833(8) 0.3947(5) 0.111(4) Uani 1 1 d . . . H18A H 0.0542 0.2546 0.3653 0.167 Uiso 1 1 calc R . . H18B H 0.0199 0.3281 0.3712 0.167 Uiso 1 1 calc R . . H18C H 0.0280 0.2367 0.4129 0.167 Uiso 1 1 calc R . . C19 C 0.1139(4) 0.2639(8) 0.4845(5) 0.101(4) Uani 1 1 d . . . H19A H 0.1251 0.2346 0.4538 0.151 Uiso 1 1 calc R . . H19B H 0.1026 0.2174 0.5062 0.151 Uiso 1 1 calc R . . H19C H 0.1373 0.2975 0.5164 0.151 Uiso 1 1 calc R . . C20 C 0.0581(3) 0.3734(8) 0.4986(5) 0.102(4) Uani 1 1 d . . . H20A H 0.0814 0.4032 0.5330 0.153 Uiso 1 1 calc R . . H20B H 0.0453 0.3252 0.5168 0.153 Uiso 1 1 calc R . . H20C H 0.0359 0.4183 0.4769 0.153 Uiso 1 1 calc R . . C21 C 0.2402(3) 0.3290(6) 0.3982(4) 0.064(3) Uani 1 1 d . . . H21A H 0.2464 0.2722 0.4237 0.077 Uiso 1 1 calc R . . H21B H 0.2522 0.3224 0.3633 0.077 Uiso 1 1 calc R . . C22 C 0.2624(3) 0.4084(6) 0.4411(4) 0.054(2) Uani 1 1 d . . . C23 C 0.2885(3) 0.3949(8) 0.5072(5) 0.071(3) Uani 1 1 d . . . H23A H 0.2938 0.3352 0.5246 0.086 Uiso 1 1 calc R . . C24 C 0.3060(3) 0.4704(9) 0.5458(4) 0.069(3) Uani 1 1 d . . . C25 C 0.2974(3) 0.5608(7) 0.5241(4) 0.061(2) Uani 1 1 d . . . H25A H 0.3086 0.6106 0.5521 0.073 Uiso 1 1 calc R . . C26 C 0.2715(3) 0.5751(7) 0.4588(4) 0.054(2) Uani 1 1 d . . . C27 C 0.2563(3) 0.4991(6) 0.4184(4) 0.052(2) Uani 1 1 d . . . C28 C 0.2581(3) 0.5174(7) 0.3123(4) 0.084(3) Uani 1 1 d . . . H28A H 0.2393 0.5290 0.2679 0.126 Uiso 1 1 calc R . . H28B H 0.2730 0.4592 0.3145 0.126 Uiso 1 1 calc R . . H28C H 0.2794 0.5665 0.3267 0.126 Uiso 1 1 calc R . . C29 C 0.2582(3) 0.6717(6) 0.4327(4) 0.053(2) Uani 1 1 d . . . H29A H 0.2702 0.7161 0.4679 0.063 Uiso 1 1 calc R . . H29B H 0.2711 0.6850 0.3993 0.063 Uiso 1 1 calc R . . C30 C 0.2090(3) 0.6845(6) 0.4038(4) 0.048(2) Uani 1 1 d . . . C31 C 0.1826(3) 0.6559(5) 0.4396(4) 0.050(2) Uani 1 1 d . . . H31A H 0.1957 0.6347 0.4823 0.060 Uiso 1 1 calc R . . C32 C 0.1371(3) 0.6590(6) 0.4119(4) 0.055(2) Uani 1 1 d . . . C33 C 0.1172(3) 0.6854(6) 0.3471(4) 0.061(2) Uani 1 1 d . . . H33A H 0.0866 0.6838 0.3279 0.073 Uiso 1 1 calc R . . C34 C 0.1431(3) 0.7147(6) 0.3100(4) 0.060(2) Uani 1 1 d . . . C35 C 0.1886(3) 0.7169(6) 0.3408(4) 0.052(2) Uani 1 1 d . . . C36 C 0.2276(3) 0.8426(7) 0.3176(5) 0.087(3) Uani 1 1 d . . . H36A H 0.2448 0.8605 0.2912 0.130 Uiso 1 1 calc R . . H36B H 0.2451 0.8496 0.3631 0.130 Uiso 1 1 calc R . . H36C H 0.2019 0.8814 0.3072 0.130 Uiso 1 1 calc R . . C37 C 0.0902(3) 0.7013(7) 0.4781(4) 0.070(3) Uani 1 1 d . . . C38 C 0.0624(3) 0.7703(7) 0.4264(5) 0.096(3) Uani 1 1 d . . . H38A H 0.0810 0.8015 0.4067 0.143 Uiso 1 1 calc R . . H38B H 0.0493 0.8151 0.4468 0.143 Uiso 1 1 calc R . . H38C H 0.0395 0.7373 0.3933 0.143 Uiso 1 1 calc R . . C39 C 0.1272(3) 0.7523(7) 0.5310(5) 0.087(3) Uani 1 1 d . . . H39A H 0.1443 0.7084 0.5629 0.131 Uiso 1 1 calc R . . H39B H 0.1147 0.7974 0.5519 0.131 Uiso 1 1 calc R . . H39C H 0.1459 0.7830 0.5113 0.131 Uiso 1 1 calc R . . C40 C 0.0596(3) 0.6538(8) 0.5086(5) 0.091(3) Uani 1 1 d . . . H40A H 0.0762 0.6100 0.5410 0.136 Uiso 1 1 calc R . . H40B H 0.0365 0.6219 0.4751 0.136 Uiso 1 1 calc R . . H40C H 0.0469 0.6997 0.5287 0.136 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 Br1 0.0918(8) 0.0886(8) 0.0765(7) -0.0034(6) 0.0453(6) -0.0057(7) Br2 0.1136(11) 0.1745(15) 0.0713(8) 0.0262(9) 0.0096(7) 0.0229(10) O1 0.065(4) 0.102(5) 0.058(4) -0.003(4) 0.023(4) 0.003(4) O2 0.094(5) 0.066(5) 0.080(4) -0.012(4) 0.055(4) -0.005(4) O3 0.070(5) 0.120(6) 0.087(5) -0.001(4) 0.027(4) -0.001(4) O4 0.061(4) 0.061(4) 0.046(4) 0.000(3) 0.016(3) -0.003(3) O5 0.078(4) 0.060(4) 0.063(4) -0.005(3) 0.036(3) -0.009(3) O6 0.088(5) 0.097(5) 0.073(4) 0.012(4) 0.039(4) -0.006(4) N1 0.054(5) 0.076(6) 0.057(4) 0.003(4) 0.026(4) 0.009(4) N2 0.069(5) 0.065(5) 0.045(4) 0.011(4) 0.024(4) 0.014(4) C1 0.074(7) 0.075(7) 0.059(6) 0.016(5) 0.024(5) 0.020(6) C2 0.070(7) 0.071(7) 0.033(5) 0.005(5) 0.010(5) 0.012(6) C3 0.072(7) 0.076(7) 0.038(5) 0.001(5) 0.016(5) -0.007(6) C4 0.062(6) 0.080(7) 0.048(5) -0.013(6) 0.023(5) -0.015(6) C5 0.081(7) 0.074(7) 0.049(6) -0.014(5) 0.022(5) -0.009(6) C6 0.061(6) 0.080(8) 0.033(5) -0.002(5) 0.002(5) -0.015(6) C7 0.068(7) 0.067(7) 0.042(5) -0.002(5) 0.012(5) -0.002(6) C8 0.066(8) 0.213(15) 0.086(8) 0.002(9) 0.012(7) 0.022(9) C9 0.091(8) 0.086(8) 0.060(6) -0.026(6) 0.035(6) -0.028(6) C10 0.075(7) 0.064(7) 0.051(6) -0.011(5) 0.030(6) -0.023(5) C11 0.052(6) 0.070(7) 0.067(7) -0.006(5) 0.024(5) -0.014(5) C12 0.053(6) 0.068(7) 0.062(6) -0.003(5) 0.023(5) -0.009(5) C13 0.060(7) 0.058(6) 0.056(6) 0.001(5) 0.026(5) -0.002(5) C14 0.066(7) 0.044(6) 0.061(6) 0.001(5) 0.028(5) -0.004(5) C15 0.072(7) 0.052(6) 0.084(8) -0.005(5) 0.051(6) -0.012(5) C16 0.134(10) 0.067(8) 0.111(9) -0.021(7) 0.075(8) 0.008(7) C17 0.079(8) 0.083(8) 0.078(7) -0.007(6) 0.040(6) -0.014(7) C18 0.120(10) 0.124(11) 0.100(9) -0.014(8) 0.052(8) -0.048(8) C19 0.110(9) 0.094(9) 0.118(9) 0.040(8) 0.065(8) 0.004(8) C20 0.087(8) 0.138(10) 0.104(8) 0.005(8) 0.064(7) -0.013(7) C21 0.064(7) 0.061(7) 0.075(6) 0.010(6) 0.034(5) 0.003(5) C22 0.046(5) 0.061(7) 0.059(6) 0.008(5) 0.024(5) 0.008(5) C23 0.059(7) 0.077(8) 0.089(8) 0.024(7) 0.040(6) 0.017(6) C24 0.046(6) 0.104(9) 0.057(6) 0.004(7) 0.016(5) -0.003(6) C25 0.056(6) 0.073(7) 0.053(6) -0.008(6) 0.020(5) -0.009(6) C26 0.048(5) 0.061(7) 0.057(6) -0.005(5) 0.022(5) -0.008(5) C27 0.051(6) 0.049(6) 0.053(6) 0.011(5) 0.017(5) 0.006(5) C28 0.119(9) 0.082(8) 0.059(6) 0.003(6) 0.041(6) -0.011(7) C29 0.057(6) 0.050(6) 0.053(5) -0.015(5) 0.021(5) -0.014(5) C30 0.053(6) 0.046(6) 0.045(5) -0.008(4) 0.017(5) -0.003(4) C31 0.052(6) 0.050(6) 0.048(5) 0.000(4) 0.015(5) 0.003(5) C32 0.062(7) 0.055(6) 0.051(6) -0.001(5) 0.025(5) 0.005(5) C33 0.056(6) 0.076(7) 0.053(6) 0.002(5) 0.023(5) 0.023(5) C34 0.070(7) 0.059(6) 0.048(6) 0.002(5) 0.016(5) 0.010(5) C35 0.061(7) 0.050(6) 0.049(6) -0.006(5) 0.024(5) -0.003(5) C36 0.115(9) 0.066(8) 0.098(8) 0.004(6) 0.062(7) -0.009(7) C37 0.065(7) 0.093(8) 0.057(6) -0.017(6) 0.025(5) -0.007(6) C38 0.083(8) 0.105(9) 0.102(8) 0.013(7) 0.035(7) 0.030(7) C39 0.092(8) 0.098(8) 0.085(7) -0.024(7) 0.047(7) -0.002(7) C40 0.067(7) 0.140(10) 0.079(7) -0.005(7) 0.042(6) -0.002(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 C4 1.918(8) . ? Br2 C24 1.921(9) . ? O1 C7 1.388(10) . ? O1 C8 1.406(10) . ? O2 C15 1.406(9) . ? O2 C16 1.434(10) . ? O3 N1 1.463(8) . ? O4 C27 1.374(9) . ? O4 C28 1.431(9) . ? O5 C35 1.398(9) . ? O5 C36 1.431(10) . ? O6 N2 1.469(8) . ? N1 C12 1.445(10) . ? N1 C17 1.519(11) . ? N2 C32 1.455(10) . ? N2 C37 1.497(10) . ? C1 C34 1.525(11) . ? C1 C2 1.534(12) . ? C2 C7 1.379(12) . ? C2 C3 1.409(11) . ? C3 C4 1.359(12) . ? C4 C5 1.359(12) . ? C5 C6 1.432(12) . ? C6 C7 1.380(12) . ? C6 C9 1.532(12) . ? C9 C10 1.538(11) . ? C10 C15 1.387(12) . ? C10 C11 1.403(11) . ? C11 C12 1.373(11) . ? C12 C13 1.395(11) . ? C13 C14 1.387(10) . ? C14 C15 1.406(11) . ? C14 C21 1.513(11) . ? C17 C18 1.489(13) . ? C17 C19 1.517(13) . ? C17 C20 1.550(12) . ? C21 C22 1.493(11) . ? C22 C27 1.385(11) . ? C22 C23 1.407(12) . ? C23 C24 1.371(13) . ? C24 C25 1.379(12) . ? C25 C26 1.391(11) . ? C26 C27 1.383(11) . ? C26 C29 1.508(11) . ? C29 C30 1.505(10) . ? C30 C35 1.380(10) . ? C30 C31 1.400(10) . ? C31 C32 1.380(10) . ? C32 C33 1.385(10) . ? C33 C34 1.410(11) . ? C34 C35 1.389(11) . ? C37 C40 1.527(11) . ? C37 C39 1.528(12) . ? C37 C38 1.536(12) . ? 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 C7 O1 C8 115.5(7) . . ? C15 O2 C16 112.7(7) . . ? C27 O4 C28 113.4(6) . . ? C35 O5 C36 112.7(6) . . ? C12 N1 O3 108.2(6) . . ? C12 N1 C17 115.2(7) . . ? O3 N1 C17 104.6(7) . . ? C32 N2 O6 105.9(6) . . ? C32 N2 C37 115.6(7) . . ? O6 N2 C37 103.5(6) . . ? C34 C1 C2 107.3(7) . . ? C7 C2 C3 117.6(9) . . ? C7 C2 C1 121.1(8) . . ? C3 C2 C1 121.1(9) . . ? C4 C3 C2 119.5(9) . . ? C3 C4 C5 123.5(8) . . ? C3 C4 Br1 118.8(8) . . ? C5 C4 Br1 117.6(8) . . ? C4 C5 C6 118.0(9) . . ? C7 C6 C5 117.9(9) . . ? C7 C6 C9 122.2(9) . . ? C5 C6 C9 119.5(9) . . ? C2 C7 C6 122.9(9) . . ? C2 C7 O1 118.7(9) . . ? C6 C7 O1 118.3(9) . . ? C6 C9 C10 108.1(7) . . ? C15 C10 C11 118.3(8) . . ? C15 C10 C9 121.2(8) . . ? C11 C10 C9 120.3(9) . . ? C12 C11 C10 121.0(8) . . ? C11 C12 C13 119.1(8) . . ? C11 C12 N1 122.8(8) . . ? C13 C12 N1 117.9(8) . . ? C14 C13 C12 122.2(8) . . ? C13 C14 C15 116.9(8) . . ? C13 C14 C21 121.7(8) . . ? C15 C14 C21 121.0(8) . . ? C10 C15 C14 122.2(8) . . ? C10 C15 O2 117.9(9) . . ? C14 C15 O2 119.7(9) . . ? C18 C17 C19 111.6(10) . . ? C18 C17 N1 112.4(8) . . ? C19 C17 N1 107.8(8) . . ? C18 C17 C20 110.5(9) . . ? C19 C17 C20 108.5(9) . . ? N1 C17 C20 105.7(8) . . ? C22 C21 C14 111.9(7) . . ? C27 C22 C23 117.2(9) . . ? C27 C22 C21 121.3(8) . . ? C23 C22 C21 121.4(9) . . ? C24 C23 C22 119.4(9) . . ? C23 C24 C25 123.1(9) . . ? C23 C24 Br2 118.2(9) . . ? C25 C24 Br2 118.6(8) . . ? C24 C25 C26 117.9(9) . . ? C27 C26 C25 119.2(9) . . ? C27 C26 C29 119.8(8) . . ? C25 C26 C29 120.9(8) . . ? O4 C27 C26 118.8(8) . . ? O4 C27 C22 118.3(8) . . ? C26 C27 C22 122.9(8) . . ? C30 C29 C26 113.0(7) . . ? C35 C30 C31 118.7(8) . . ? C35 C30 C29 121.8(7) . . ? C31 C30 C29 119.3(7) . . ? C32 C31 C30 120.5(8) . . ? C31 C32 C33 120.0(8) . . ? C31 C32 N2 123.4(8) . . ? C33 C32 N2 116.3(8) . . ? C32 C33 C34 120.5(8) . . ? C35 C34 C33 117.8(8) . . ? C35 C34 C1 121.0(8) . . ? C33 C34 C1 120.7(8) . . ? C30 C35 C34 122.1(8) . . ? C30 C35 O5 119.7(8) . . ? C34 C35 O5 118.0(8) . . ? N2 C37 C40 107.1(8) . . ? N2 C37 C39 112.1(7) . . ? C40 C37 C39 110.1(7) . . ? N2 C37 C38 109.3(7) . . ? C40 C37 C38 107.8(8) . . ? C39 C37 C38 110.4(9) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 22.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.699 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.083