data_x _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Cyclopentene Absolute Structure' _chemical_melting_point ? _chemical_formula_moiety 'C26 H24 Br N O2' _chemical_formula_sum 'C26 H24 Br N O2' _chemical_formula_weight 462.36 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 P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.2308(5) _cell_length_b 23.0250(13) _cell_length_c 10.6007(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.9710(10) _cell_angle_gamma 90.00 _cell_volume 2250.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 7183 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 28.82 _exptl_crystal_description columnar _exptl_crystal_colour colorless _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 1.850 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.4767 _exptl_absorpt_correction_T_max 0.7219 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21120 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 28.85 _reflns_number_total 10633 _reflns_number_gt 9531 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0644P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.010(4) _refine_ls_number_reflns 10633 _refine_ls_number_parameters 549 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0356 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0798 _refine_ls_wR_factor_gt 0.0772 _refine_ls_goodness_of_fit_ref 0.836 _refine_ls_restrained_S_all 0.836 _refine_ls_shift/su_max 2.784 _refine_ls_shift/su_mean 0.018 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 0.92269(3) 0.363407(9) 0.49950(2) 0.04282(7) Uani 1 1 d . . . Br2 Br 0.28653(3) -0.007225(10) 0.51838(2) 0.04343(7) Uani 1 1 d . . . O3 O 0.58554(14) 0.24789(6) 1.00374(14) 0.0266(3) Uani 1 1 d . . . O2 O 0.84719(15) 0.13645(7) 0.92945(15) 0.0308(3) Uani 1 1 d . . . C24 C 0.9547(2) 0.31022(9) 0.63447(19) 0.0298(4) Uani 1 1 d . . . O1 O 1.03755(14) 0.12252(6) 1.06936(13) 0.0264(3) Uani 1 1 d . . . C40 C 0.4873(2) 0.21413(9) 0.94005(19) 0.0240(4) Uani 1 1 d . . . N1 N 1.05112(17) 0.19221(7) 0.92736(17) 0.0257(3) Uani 1 1 d . . . H1 H 1.1384 0.1962 0.9637 0.031 Uiso 1 1 calc R . . O4 O 0.35698(15) 0.22221(7) 0.93827(16) 0.0318(3) Uani 1 1 d . . . C41 C 0.4899(2) 0.13011(9) 0.79765(19) 0.0254(4) Uani 1 1 d . . . C44 C 0.3731(2) 0.04928(9) 0.62825(19) 0.0295(4) Uani 1 1 d . . . C22 C 0.9051(2) 0.21944(9) 0.7340(2) 0.0284(4) Uani 1 1 d . . . H22 H 0.8518 0.1842 0.7359 0.034 Uiso 1 1 calc R . . C21 C 1.0118(2) 0.23140(9) 0.82838(19) 0.0241(4) Uani 1 1 d . . . C46 C 0.5599(2) 0.07698(9) 0.7814(2) 0.0285(4) Uani 1 1 d . . . H46 H 0.6477 0.0686 0.8286 0.034 Uiso 1 1 calc R . . C20 C 0.96800(19) 0.14938(8) 0.97130(19) 0.0232(4) Uani 1 1 d . . . C13 C 0.9687(2) 0.06988(9) 1.1163(2) 0.0258(4) Uani 1 1 d . . . H13 H 0.893(3) 0.0575(12) 1.051(3) 0.031 Uiso 1 1 calc . . . N2 N 0.55593(18) 0.17041(8) 0.88269(18) 0.0286(4) Uani 1 1 d . . . H2 H 0.6498 0.1668 0.8998 0.034 Uiso 1 1 calc R . . C14 C 0.8908(2) 0.08368(9) 1.2350(2) 0.0288(4) Uani 1 1 d . . . C39 C 0.6124(2) 0.34191(10) 0.8368(2) 0.0336(5) Uani 1 1 d . . . H39 H 0.6858 0.3130 0.8373 0.040 Uiso 1 1 calc R . . C23 C 0.8766(2) 0.25923(10) 0.6369(2) 0.0319(4) Uani 1 1 d . . . H23 H 0.8038 0.2513 0.5727 0.038 Uiso 1 1 calc R . . C27 C 0.6334(2) 0.32082(9) 1.1614(2) 0.0304(4) Uani 1 1 d . . . C29 C 0.6271(2) 0.27392(10) 1.2626(2) 0.0325(5) Uani 1 1 d . . . C15 C 0.9603(3) 0.09730(11) 1.3501(2) 0.0381(5) Uani 1 1 d . . . H15 H 1.0632 0.0998 1.3566 0.046 Uiso 1 1 calc R . . C25 C 1.0614(2) 0.32298(9) 0.7279(2) 0.0299(4) Uani 1 1 d . . . H25 H 1.1151 0.3581 0.7249 0.036 Uiso 1 1 calc R . . C6 C 1.1177(2) 0.00640(9) 0.9859(2) 0.0314(4) Uani 1 1 d . . . C2 C 1.0354(3) -0.02852(10) 1.2014(2) 0.0342(5) Uani 1 1 d . . . H2A H 0.9362 -0.0388 1.1725 0.051 Uiso 1 1 calc R . . H2B H 1.0371 -0.0173 1.2906 0.051 Uiso 1 1 calc R . . H2C H 1.0993 -0.0620 1.1913 0.051 Uiso 1 1 calc R . . C7 C 1.0105(2) -0.02148(10) 0.8948(2) 0.0350(5) Uani 1 1 d . . . C45 C 0.5010(2) 0.03646(9) 0.6962(2) 0.0294(4) Uani 1 1 d . . . H45 H 0.5481 0.0003 0.6848 0.035 Uiso 1 1 calc R . . C33 C 0.5318(2) 0.30334(9) 1.0470(2) 0.0262(4) Uani 1 1 d . . . H33 H 0.432(3) 0.2973(11) 1.077(2) 0.031 Uiso 1 1 calc . . . C1 C 1.0881(2) 0.02247(9) 1.1228(2) 0.0284(4) Uani 1 1 d . . . C43 C 0.3046(3) 0.10207(10) 0.6419(2) 0.0349(5) Uani 1 1 d . . . H43 H 0.2178 0.1104 0.5931 0.042 Uiso 1 1 calc R . . C28 C 0.5847(3) 0.38008(10) 1.2105(3) 0.0433(6) Uani 1 1 d . . . H28A H 0.4830 0.3778 1.2325 0.065 Uiso 1 1 calc R . . H28B H 0.5948 0.4095 1.1448 0.065 Uiso 1 1 calc R . . H28C H 0.6453 0.3907 1.2856 0.065 Uiso 1 1 calc R . . C47 C 0.4942(3) 0.26269(11) 1.3311(2) 0.0370(5) Uani 1 1 d . . . C38 C 0.5969(3) 0.38044(11) 0.7361(2) 0.0412(5) Uani 1 1 d . . . H38 H 0.6601 0.3778 0.6685 0.049 Uiso 1 1 calc R . . C12 C 0.9489(3) -0.07553(11) 0.9163(3) 0.0409(5) Uani 1 1 d . . . H12 H 0.9682 -0.0945 0.9950 0.049 Uiso 1 1 calc R . . C34 C 0.5211(2) 0.34550(9) 0.9368(2) 0.0281(4) Uani 1 1 d . . . C42 C 0.3622(2) 0.14286(10) 0.7265(2) 0.0339(5) Uani 1 1 d . . . H42 H 0.3152 0.1792 0.7361 0.041 Uiso 1 1 calc R . . C3 C 1.2399(2) 0.04448(11) 1.1736(2) 0.0342(5) Uani 1 1 d . . . H3A H 1.2295 0.0804 1.2236 0.041 Uiso 1 1 calc R . . H3B H 1.2881 0.0147 1.2285 0.041 Uiso 1 1 calc R . . C32 C 0.7957(3) 0.32121(12) 1.1323(3) 0.0413(6) Uani 1 1 d . . . H32A H 0.8067 0.3219 1.0399 0.050 Uiso 1 1 calc R . . H32B H 0.8442 0.3560 1.1698 0.050 Uiso 1 1 calc R . . C26 C 1.0881(2) 0.28373(9) 0.8251(2) 0.0281(4) Uani 1 1 d . . . H26 H 1.1592 0.2925 0.8904 0.034 Uiso 1 1 calc R . . C8 C 0.9772(3) 0.00505(12) 0.7787(3) 0.0461(6) Uani 1 1 d . . . H8 H 1.0186 0.0419 0.7619 0.055 Uiso 1 1 calc R . . C17 C 0.7326(3) 0.10383(13) 1.4488(3) 0.0522(7) Uani 1 1 d . . . H17 H 0.6793 0.1103 1.5218 0.063 Uiso 1 1 calc R . . C4 C 1.3297(3) 0.05641(12) 1.0587(2) 0.0405(5) Uani 1 1 d . . . H4A H 1.3359 0.0986 1.0415 0.049 Uiso 1 1 calc R . . H4B H 1.4290 0.0404 1.0713 0.049 Uiso 1 1 calc R . . C16 C 0.8816(3) 0.10729(14) 1.4562(3) 0.0497(7) Uani 1 1 d . . . H16 H 0.9310 0.1166 1.5345 0.060 Uiso 1 1 calc R . . C35 C 0.4140(3) 0.38801(11) 0.9326(3) 0.0383(5) Uani 1 1 d . . . H35 H 0.3500 0.3907 0.9997 0.046 Uiso 1 1 calc R . . C19 C 0.7389(3) 0.08086(11) 1.2281(3) 0.0397(5) Uani 1 1 d . . . H19 H 0.6890 0.0720 1.1499 0.048 Uiso 1 1 calc R . . C30 C 0.7520(3) 0.24518(11) 1.2769(2) 0.0398(5) Uani 1 1 d . . . H30 H 0.7689 0.2147 1.3361 0.048 Uiso 1 1 calc R . . C36 C 0.3989(3) 0.42645(12) 0.8327(3) 0.0448(6) Uani 1 1 d . . . H36 H 0.3259 0.4555 0.8319 0.054 Uiso 1 1 calc R . . C31 C 0.8629(3) 0.26617(13) 1.1896(3) 0.0474(6) Uani 1 1 d . . . H31A H 0.8799 0.2370 1.1234 0.057 Uiso 1 1 calc R . . H31B H 0.9560 0.2748 1.2365 0.057 Uiso 1 1 calc R . . C5 C 1.2463(3) 0.02561(11) 0.9543(2) 0.0384(5) Uani 1 1 d . . . H5 H 1.2821 0.0203 0.8727 0.046 Uiso 1 1 calc R . . C11 C 0.8590(3) -0.10211(13) 0.8234(3) 0.0514(7) Uani 1 1 d . . . H11 H 0.8195 -0.1394 0.8387 0.062 Uiso 1 1 calc R . . C9 C 0.8856(3) -0.02055(15) 0.6870(3) 0.0561(8) Uani 1 1 d . . . H9 H 0.8630 -0.0012 0.6092 0.067 Uiso 1 1 calc R . . C18 C 0.6608(3) 0.09088(13) 1.3344(3) 0.0518(7) Uani 1 1 d . . . H18 H 0.5579 0.0889 1.3286 0.062 Uiso 1 1 calc R . . C10 C 0.8272(3) -0.07503(15) 0.7106(3) 0.0542(7) Uani 1 1 d . . . H10 H 0.7652 -0.0934 0.6483 0.065 Uiso 1 1 calc R . . C37 C 0.4906(3) 0.42241(12) 0.7336(3) 0.0446(6) Uani 1 1 d . . . H37 H 0.4801 0.4485 0.6643 0.054 Uiso 1 1 calc R . . C52 C 0.3843(3) 0.22614(12) 1.2808(3) 0.0474(6) Uani 1 1 d . . . H52 H 0.3961 0.2068 1.2028 0.057 Uiso 1 1 calc R . . C51 C 0.2581(3) 0.21801(15) 1.3446(4) 0.0600(8) Uani 1 1 d . . . H51 H 0.1831 0.1938 1.3094 0.072 Uiso 1 1 calc R . . C48 C 0.4742(4) 0.28968(14) 1.4466(3) 0.0550(7) Uani 1 1 d . . . H48 H 0.5474 0.3145 1.4825 0.066 Uiso 1 1 calc R . . C50 C 0.2417(4) 0.24508(15) 1.4589(4) 0.0637(9) Uani 1 1 d . . . H50 H 0.1557 0.2391 1.5027 0.076 Uiso 1 1 calc R . . C49 C 0.3476(4) 0.28041(17) 1.5097(3) 0.0671(9) Uani 1 1 d . . . H49 H 0.3352 0.2988 1.5886 0.081 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 0.05753(15) 0.03735(12) 0.03342(12) 0.01322(10) 0.00085(10) 0.00663(11) Br2 0.06034(15) 0.03758(12) 0.03116(11) -0.01132(10) -0.00928(10) -0.00483(11) O3 0.0179(6) 0.0250(7) 0.0365(8) -0.0076(6) -0.0031(6) -0.0008(5) O2 0.0176(6) 0.0321(8) 0.0421(9) 0.0088(7) -0.0051(6) -0.0016(5) C24 0.0352(11) 0.0298(10) 0.0249(10) 0.0070(8) 0.0049(8) 0.0102(8) O1 0.0212(6) 0.0269(7) 0.0305(7) 0.0081(6) -0.0031(5) -0.0031(5) C40 0.0198(9) 0.0224(9) 0.0294(10) -0.0012(7) -0.0027(7) -0.0029(7) N1 0.0164(7) 0.0282(8) 0.0319(9) 0.0063(7) -0.0030(6) -0.0010(6) O4 0.0165(7) 0.0318(8) 0.0469(9) -0.0075(7) 0.0008(6) -0.0013(5) C41 0.0214(9) 0.0262(10) 0.0287(10) -0.0017(8) 0.0014(7) -0.0018(7) C44 0.0369(11) 0.0296(10) 0.0220(9) -0.0026(8) 0.0012(8) -0.0061(8) C22 0.0288(10) 0.0295(10) 0.0268(10) 0.0012(8) -0.0003(8) -0.0023(8) C21 0.0212(9) 0.0242(9) 0.0271(9) 0.0025(7) 0.0025(7) 0.0041(7) C46 0.0203(9) 0.0307(10) 0.0345(11) -0.0027(8) 0.0008(8) 0.0010(7) C20 0.0184(9) 0.0231(9) 0.0282(10) 0.0027(7) 0.0029(7) 0.0039(7) C13 0.0234(9) 0.0232(9) 0.0307(10) 0.0060(8) 0.0002(8) -0.0012(7) N2 0.0179(7) 0.0281(9) 0.0392(10) -0.0065(7) -0.0047(7) 0.0004(6) C14 0.0283(10) 0.0241(9) 0.0344(11) 0.0067(8) 0.0060(8) 0.0004(8) C39 0.0319(11) 0.0347(11) 0.0344(12) -0.0057(9) 0.0032(9) -0.0028(9) C23 0.0319(11) 0.0369(11) 0.0266(10) 0.0019(9) -0.0008(8) 0.0025(9) C27 0.0304(11) 0.0270(10) 0.0334(11) -0.0031(8) -0.0020(9) -0.0071(8) C29 0.0369(11) 0.0297(11) 0.0305(11) -0.0049(9) -0.0009(9) -0.0037(9) C15 0.0355(12) 0.0418(13) 0.0371(12) 0.0055(10) 0.0038(10) 0.0032(10) C25 0.0302(10) 0.0240(9) 0.0360(11) 0.0028(8) 0.0044(8) 0.0021(8) C6 0.0290(10) 0.0306(11) 0.0351(11) 0.0059(8) 0.0055(8) 0.0052(8) C2 0.0343(11) 0.0281(10) 0.0406(12) 0.0106(9) 0.0043(9) 0.0031(9) C7 0.0306(11) 0.0368(12) 0.0382(12) -0.0036(9) 0.0083(9) 0.0074(8) C45 0.0310(10) 0.0271(10) 0.0306(10) -0.0035(8) 0.0056(8) -0.0009(8) C33 0.0211(9) 0.0240(9) 0.0336(11) -0.0045(8) 0.0024(8) -0.0018(7) C1 0.0232(9) 0.0289(10) 0.0332(11) 0.0087(8) 0.0025(8) 0.0033(8) C43 0.0348(12) 0.0364(12) 0.0321(11) -0.0018(9) -0.0114(9) 0.0018(9) C28 0.0560(15) 0.0302(12) 0.0430(13) -0.0099(10) -0.0042(11) -0.0032(10) C47 0.0383(12) 0.0342(12) 0.0388(12) 0.0042(9) 0.0044(10) 0.0038(9) C38 0.0415(12) 0.0464(14) 0.0362(12) 0.0003(10) 0.0056(10) -0.0078(10) C12 0.0374(12) 0.0371(12) 0.0493(14) -0.0046(11) 0.0125(11) 0.0022(10) C34 0.0241(9) 0.0267(10) 0.0330(11) -0.0036(8) -0.0015(8) -0.0050(7) C42 0.0352(11) 0.0261(10) 0.0392(12) -0.0020(9) -0.0090(9) 0.0036(9) C3 0.0224(10) 0.0436(13) 0.0363(12) 0.0108(10) -0.0015(9) 0.0047(9) C32 0.0304(11) 0.0502(14) 0.0428(13) -0.0058(11) -0.0031(10) -0.0140(10) C26 0.0246(10) 0.0245(9) 0.0347(11) 0.0023(8) -0.0017(8) 0.0038(7) C8 0.0490(14) 0.0471(16) 0.0423(13) 0.0011(11) 0.0022(11) 0.0051(11) C17 0.0601(18) 0.0492(15) 0.0497(16) 0.0069(13) 0.0277(14) 0.0032(13) C4 0.0254(10) 0.0502(14) 0.0462(14) 0.0096(11) 0.0063(10) -0.0038(10) C16 0.0600(17) 0.0560(17) 0.0335(13) 0.0069(12) 0.0061(12) 0.0089(13) C35 0.0327(11) 0.0360(12) 0.0467(14) 0.0047(10) 0.0072(10) 0.0006(9) C19 0.0294(11) 0.0396(13) 0.0506(15) -0.0043(11) 0.0081(10) -0.0024(9) C30 0.0402(12) 0.0388(12) 0.0400(13) -0.0049(10) -0.0006(10) 0.0056(10) C36 0.0333(12) 0.0386(13) 0.0620(17) 0.0121(12) -0.0016(11) 0.0002(10) C31 0.0337(12) 0.0537(16) 0.0549(16) -0.0098(13) 0.0039(11) 0.0053(11) C5 0.0347(12) 0.0411(13) 0.0402(13) 0.0044(10) 0.0100(10) 0.0026(10) C11 0.0363(13) 0.0505(16) 0.0690(19) -0.0218(14) 0.0175(13) -0.0041(11) C9 0.0549(17) 0.068(2) 0.0450(15) -0.0086(13) -0.0042(12) 0.0101(14) C18 0.0352(13) 0.0543(16) 0.0679(19) -0.0044(14) 0.0219(13) -0.0055(12) C10 0.0364(13) 0.071(2) 0.0563(18) -0.0252(15) 0.0080(12) 0.0015(13) C37 0.0423(13) 0.0437(14) 0.0473(15) 0.0139(12) -0.0037(11) -0.0086(11) C52 0.0500(15) 0.0431(14) 0.0495(15) 0.0023(12) 0.0072(12) -0.0073(11) C51 0.0462(15) 0.0523(17) 0.082(2) 0.0183(16) 0.0123(15) -0.0090(13) C48 0.0604(18) 0.0594(18) 0.0462(16) -0.0079(13) 0.0112(13) -0.0014(14) C50 0.0607(19) 0.0541(18) 0.079(2) 0.0179(17) 0.0341(18) 0.0126(15) C49 0.076(2) 0.071(2) 0.0570(19) -0.0056(16) 0.0337(17) 0.0053(18) _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 C24 1.895(2) . ? Br2 C44 1.895(2) . ? O3 C40 1.349(2) . ? O3 C33 1.453(2) . ? O2 C20 1.216(2) . ? C24 C23 1.379(3) . ? C24 C25 1.391(3) . ? O1 C20 1.344(2) . ? O1 C13 1.467(2) . ? C40 O4 1.217(2) . ? C40 N2 1.351(3) . ? N1 C20 1.347(3) . ? N1 C21 1.417(3) . ? C41 C46 1.398(3) . ? C41 C42 1.398(3) . ? C41 N2 1.410(3) . ? C44 C43 1.381(3) . ? C44 C45 1.382(3) . ? C22 C23 1.392(3) . ? C22 C21 1.395(3) . ? C21 C26 1.397(3) . ? C46 C45 1.390(3) . ? C13 C14 1.515(3) . ? C13 C1 1.550(3) . ? C14 C15 1.385(3) . ? C14 C19 1.401(3) . ? C39 C34 1.391(3) . ? C39 C38 1.389(4) . ? C27 C29 1.525(3) . ? C27 C28 1.536(3) . ? C27 C33 1.548(3) . ? C27 C32 1.546(3) . ? C29 C30 1.331(3) . ? C29 C47 1.480(3) . ? C15 C16 1.390(4) . ? C25 C26 1.383(3) . ? C6 C5 1.326(3) . ? C6 C7 1.491(3) . ? C6 C1 1.536(3) . ? C2 C1 1.533(3) . ? C7 C8 1.394(4) . ? C7 C12 1.392(3) . ? C33 C34 1.518(3) . ? C1 C3 1.560(3) . ? C43 C42 1.386(3) . ? C47 C48 1.394(4) . ? C47 C52 1.402(4) . ? C38 C37 1.376(4) . ? C12 C11 1.396(4) . ? C34 C35 1.390(3) . ? C3 C4 1.533(3) . ? C32 C31 1.523(4) . ? C8 C9 1.387(4) . ? C17 C16 1.375(4) . ? C17 C18 1.385(5) . ? C4 C5 1.495(4) . ? C35 C36 1.382(4) . ? C19 C18 1.388(4) . ? C30 C31 1.495(4) . ? C36 C37 1.386(4) . ? C11 C10 1.367(5) . ? C9 C10 1.393(5) . ? C52 C51 1.390(4) . ? C51 C50 1.378(5) . ? C48 C49 1.392(5) . ? C50 C49 1.362(6) . ? 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 C40 O3 C33 115.64(14) . . ? C23 C24 C25 121.19(19) . . ? C23 C24 Br1 120.23(17) . . ? C25 C24 Br1 118.54(17) . . ? C20 O1 C13 116.41(15) . . ? O4 C40 O3 123.94(18) . . ? O4 C40 N2 126.41(18) . . ? O3 C40 N2 109.64(16) . . ? C20 N1 C21 126.42(17) . . ? C46 C41 C42 119.96(19) . . ? C46 C41 N2 117.88(18) . . ? C42 C41 N2 122.10(19) . . ? C43 C44 C45 121.1(2) . . ? C43 C44 Br2 119.17(17) . . ? C45 C44 Br2 119.69(16) . . ? C23 C22 C21 119.9(2) . . ? C26 C21 C22 119.40(19) . . ? C26 C21 N1 117.23(18) . . ? C22 C21 N1 123.35(18) . . ? C45 C46 C41 120.0(2) . . ? O2 C20 O1 124.19(18) . . ? O2 C20 N1 125.54(18) . . ? O1 C20 N1 110.27(16) . . ? O1 C13 C14 109.94(16) . . ? O1 C13 C1 106.11(15) . . ? C14 C13 C1 118.58(17) . . ? C40 N2 C41 125.53(17) . . ? C15 C14 C19 118.2(2) . . ? C15 C14 C13 124.11(19) . . ? C19 C14 C13 117.6(2) . . ? C34 C39 C38 120.3(2) . . ? C24 C23 C22 119.7(2) . . ? C29 C27 C28 111.60(19) . . ? C29 C27 C33 108.89(16) . . ? C28 C27 C33 108.70(18) . . ? C29 C27 C32 102.53(19) . . ? C28 C27 C32 111.48(19) . . ? C33 C27 C32 113.56(18) . . ? C30 C29 C47 126.3(2) . . ? C30 C29 C27 111.6(2) . . ? C47 C29 C27 122.1(2) . . ? C14 C15 C16 120.8(2) . . ? C26 C25 C24 119.0(2) . . ? C5 C6 C7 123.6(2) . . ? C5 C6 C1 111.3(2) . . ? C7 C6 C1 124.78(18) . . ? C8 C7 C12 117.6(2) . . ? C8 C7 C6 119.4(2) . . ? C12 C7 C6 122.8(2) . . ? C46 C45 C44 119.4(2) . . ? O3 C33 C34 109.22(16) . . ? O3 C33 C27 105.83(16) . . ? C34 C33 C27 116.70(17) . . ? C2 C1 C6 113.97(19) . . ? C2 C1 C13 108.58(16) . . ? C6 C1 C13 106.82(17) . . ? C2 C1 C3 111.41(18) . . ? C6 C1 C3 101.77(17) . . ? C13 C1 C3 114.22(18) . . ? C44 C43 C42 120.1(2) . . ? C48 C47 C52 118.4(2) . . ? C48 C47 C29 120.2(2) . . ? C52 C47 C29 121.4(2) . . ? C37 C38 C39 120.6(2) . . ? C7 C12 C11 120.6(3) . . ? C35 C34 C39 118.4(2) . . ? C35 C34 C33 119.54(19) . . ? C39 C34 C33 122.05(19) . . ? C43 C42 C41 119.4(2) . . ? C4 C3 C1 107.27(19) . . ? C31 C32 C27 107.1(2) . . ? C25 C26 C21 120.7(2) . . ? C9 C8 C7 122.1(3) . . ? C16 C17 C18 119.6(2) . . ? C5 C4 C3 102.96(19) . . ? C17 C16 C15 120.5(3) . . ? C36 C35 C34 121.3(2) . . ? C18 C19 C14 120.7(3) . . ? C29 C30 C31 112.7(2) . . ? C35 C36 C37 119.8(2) . . ? C30 C31 C32 103.8(2) . . ? C6 C5 C4 113.9(2) . . ? C10 C11 C12 120.7(3) . . ? C8 C9 C10 119.0(3) . . ? C17 C18 C19 120.1(3) . . ? C11 C10 C9 120.0(3) . . ? C38 C37 C36 119.7(2) . . ? C51 C52 C47 120.3(3) . . ? C50 C51 C52 120.0(3) . . ? C49 C48 C47 120.4(3) . . ? C49 C50 C51 120.6(3) . . ? C50 C49 C48 120.3(3) . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 28.85 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 0.796 _refine_diff_density_min -0.232 _refine_diff_density_rms 0.058