data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H27 Br N2 O' _chemical_formula_sum 'C31 H27 Br N2 O' _chemical_formula_weight 523.46 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' 'Br' 'Br' -0.2901 2.4595 '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M I2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 25.396(6) _cell_length_b 7.751(2) _cell_length_c 27.382(7) _cell_angle_alpha 90.00 _cell_angle_beta 111.766(4) _cell_angle_gamma 90.00 _cell_volume 5006(2) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 5247 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.4 _exptl_crystal_description prisms _exptl_crystal_colour yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 1.669 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.800 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ; Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku SCX-Mini with Mercury CCD' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25025 _diffrn_reflns_av_R_equivalents 0.1349 _diffrn_reflns_av_sigmaI/netI 0.1878 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 11292 _reflns_number_gt 6270 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. An Integrated System of Windows Programs for the Solution, Refinement and Analysis of Single Crystal X-ray Diffraction Data. Flack H D (1983), Acta Cryst. A39, 876-881. Hooft, R. W. W., Straver, L. H. and Spek, A. L. (2008). J. Appl. Cryst., 41, 96-103. Determination of absolute structure using Bayesian statistics on Bijvoet differences. Sheldrick, G. M. (2008). SHELXL-97. Acta Cryst., A64, 112-122. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _publ_section_acknowledgements ; The data were collected using instrumentation purchased with funds provided by the National Science Foundation Grant No. 0741973. ; _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _chemical_absolute_configuration ad # syn absolute configuration from synthetic procedure # ad absolute configuration from anomalous dispersion effects # rm absolute configuration from reference to a chiral # reference molecule of known abs. conf. # Hooft, R. W. W., Straver, L. H. and Spek, A. L. (2008). J. Appl. Cryst., # 41, 96-103. Determination of absolute structure using Bayesian # statistics on Bijvoet differences. _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. The absolute configuration was determined by the method of Flack (1983). The Flack x-parameter refined to 0.016(12). The assignment was confirmed by use of the Hooft y-parameter (Hooft, Straver and Spek, 2008). The Hooft y-parameter refined to 0.026(13). ; _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^)+(0.0320P)^2^] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00172(19) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.016(12) _refine_ls_number_reflns 11292 _refine_ls_number_parameters 641 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1465 _refine_ls_R_factor_gt 0.0813 _refine_ls_wR_factor_ref 0.1966 _refine_ls_wR_factor_gt 0.1653 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.001 _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 C1 C 0.4251(3) 0.6264(8) 0.3497(2) 0.0310(15) Uani 1 1 d . . . C2 C 0.4820(3) 0.6755(9) 0.3775(2) 0.0321(16) Uani 1 1 d . . . C3 C 0.5117(3) 0.6473(9) 0.4322(2) 0.0336(16) Uani 1 1 d . . . H3 H 0.4925 0.5933 0.4520 0.040 Uiso 1 1 calc R . . C4 C 0.5673(3) 0.6955(9) 0.4574(3) 0.0375(17) Uani 1 1 d . . . H4 H 0.5864 0.6736 0.4939 0.045 Uiso 1 1 calc R . . C5 C 0.5958(3) 0.7781(9) 0.4282(3) 0.0383(17) Uani 1 1 d . . . C6 C 0.5707(3) 0.8103(9) 0.3764(2) 0.0342(17) Uani 1 1 d . . . H6 H 0.5910 0.8664 0.3579 0.041 Uiso 1 1 calc R . . C7 C 0.5130(3) 0.7590(9) 0.3495(2) 0.0345(16) Uani 1 1 d . . . C8 C 0.4843(3) 0.7905(9) 0.2950(2) 0.0362(17) Uani 1 1 d . . . H8 H 0.5043 0.8469 0.2764 0.043 Uiso 1 1 calc R . . C9 C 0.4288(3) 0.7431(8) 0.2678(2) 0.0312(16) Uani 1 1 d . . . C10 C 0.3963(3) 0.6610(8) 0.2954(2) 0.0319(16) Uani 1 1 d . . . C11 C 0.4014(3) 0.7887(9) 0.2110(2) 0.0335(16) Uani 1 1 d . . . C12 C 0.4352(3) 0.7916(10) 0.1791(3) 0.0460(19) Uani 1 1 d . . . H12 H 0.4739 0.7574 0.1934 0.055 Uiso 1 1 calc R . . C13 C 0.4106(4) 0.8457(11) 0.1261(3) 0.055(2) Uani 1 1 d . . . H13 H 0.4335 0.8532 0.1055 0.066 Uiso 1 1 calc R . . C14 C 0.3547(4) 0.8872(12) 0.1042(3) 0.053(2) Uani 1 1 d . . . H14 H 0.3382 0.9194 0.0682 0.063 Uiso 1 1 calc R . . C15 C 0.3217(3) 0.8819(10) 0.1353(3) 0.043(2) Uani 1 1 d . . . H15 H 0.2828 0.9137 0.1206 0.052 Uiso 1 1 calc R . . C16 C 0.3450(3) 0.8311(10) 0.1867(3) 0.0402(19) Uani 1 1 d . . . H16 H 0.3212 0.8249 0.2066 0.048 Uiso 1 1 calc R . . C17 C 0.3927(2) 0.5411(8) 0.3805(2) 0.0277(15) Uani 1 1 d . . . C18 C 0.3495(2) 0.6238(9) 0.3897(2) 0.0324(16) Uani 1 1 d . . . C19 C 0.3222(3) 0.5466(10) 0.4214(2) 0.0436(19) Uani 1 1 d . . . H19 H 0.2924 0.6058 0.4273 0.052 Uiso 1 1 calc R . . C20 C 0.3391(3) 0.3866(10) 0.4432(3) 0.042(2) Uani 1 1 d . . . H20 H 0.3213 0.3368 0.4648 0.050 Uiso 1 1 calc R . . C21 C 0.3822(3) 0.2964(10) 0.4339(2) 0.0385(18) Uani 1 1 d . . . C22 C 0.3985(3) 0.1271(10) 0.4565(3) 0.0464(19) Uani 1 1 d . . . H22 H 0.3814 0.0773 0.4787 0.056 Uiso 1 1 calc R . . C23 C 0.4388(3) 0.0417(10) 0.4450(3) 0.046(2) Uani 1 1 d . . . H23 H 0.4489 -0.0708 0.4592 0.056 Uiso 1 1 calc R . . C24 C 0.4672(3) 0.1093(10) 0.4130(3) 0.0452(19) Uani 1 1 d . . . H24 H 0.4956 0.0450 0.4061 0.054 Uiso 1 1 calc R . . C25 C 0.4515(3) 0.2754(10) 0.3920(3) 0.0395(18) Uani 1 1 d . . . H25 H 0.4696 0.3246 0.3706 0.047 Uiso 1 1 calc R . . C26 C 0.4091(3) 0.3704(10) 0.4021(3) 0.0384(19) Uani 1 1 d . . . C27 C 0.3257(3) 0.7966(9) 0.3644(3) 0.0398(18) Uani 1 1 d . . . H27A H 0.3119 0.8634 0.3881 0.048 Uiso 1 1 calc R . . H27B H 0.3558 0.8643 0.3584 0.048 Uiso 1 1 calc R . . C28 C 0.2237(3) 0.7783(9) 0.3054(3) 0.0378(17) Uani 1 1 d . . . C29 C 0.2029(3) 0.8531(12) 0.3453(3) 0.054(2) Uani 1 1 d . . . H29A H 0.2344 0.9106 0.3729 0.081 Uiso 1 1 calc R . . H29B H 0.1880 0.7607 0.3608 0.081 Uiso 1 1 calc R . . H29C H 0.1729 0.9371 0.3282 0.081 Uiso 1 1 calc R . . C30 C 0.2043(4) 0.6898(12) 0.2145(3) 0.067(3) Uani 1 1 d . . . H30A H 0.2146 0.7990 0.2023 0.101 Uiso 1 1 calc R . . H30B H 0.1737 0.6345 0.1855 0.101 Uiso 1 1 calc R . . H30C H 0.2374 0.6134 0.2266 0.101 Uiso 1 1 calc R . . C31 C 0.1240(3) 0.7293(11) 0.2486(3) 0.062(3) Uani 1 1 d . . . H31A H 0.1182 0.7077 0.2816 0.093 Uiso 1 1 calc R . . H31B H 0.1042 0.6407 0.2228 0.093 Uiso 1 1 calc R . . H31C H 0.1089 0.8433 0.2350 0.093 Uiso 1 1 calc R . . C32 C 0.5771(3) 0.1874(8) 0.1502(2) 0.0307(15) Uani 1 1 d . . . C33 C 0.6046(3) 0.2169(8) 0.2043(2) 0.0289(15) Uani 1 1 d . . . C34 C 0.5719(3) 0.2917(9) 0.2338(2) 0.0306(16) Uani 1 1 d . . . C35 C 0.5161(3) 0.3370(8) 0.2074(2) 0.0317(15) Uani 1 1 d . . . H35 H 0.4956 0.3865 0.2268 0.038 Uiso 1 1 calc R . . C36 C 0.4877(3) 0.3127(9) 0.1522(2) 0.0320(16) Uani 1 1 d . . . C37 C 0.4310(3) 0.3665(9) 0.1259(3) 0.0324(17) Uani 1 1 d . . . H37 H 0.4111 0.4214 0.1449 0.039 Uiso 1 1 calc R . . C38 C 0.4048(3) 0.3392(10) 0.0729(3) 0.0389(17) Uani 1 1 d . . . C39 C 0.4332(3) 0.2639(9) 0.0436(2) 0.0353(16) Uani 1 1 d . . . H39 H 0.4146 0.2474 0.0068 0.042 Uiso 1 1 calc R . . C40 C 0.4886(3) 0.2136(8) 0.0688(2) 0.0333(16) Uani 1 1 d . . . H40 H 0.5075 0.1598 0.0488 0.040 Uiso 1 1 calc R . . C41 C 0.5185(3) 0.2383(8) 0.1230(2) 0.0318(16) Uani 1 1 d . . . C42 C 0.5987(3) 0.3146(8) 0.2914(2) 0.0321(16) Uani 1 1 d . . . C43 C 0.6530(3) 0.3834(9) 0.3150(3) 0.0392(19) Uani 1 1 d . . . H43 H 0.6740 0.4127 0.2939 0.047 Uiso 1 1 calc R . . C44 C 0.6769(4) 0.4099(10) 0.3695(3) 0.046(2) Uani 1 1 d . . . H44 H 0.7135 0.4603 0.3848 0.056 Uiso 1 1 calc R . . C45 C 0.6472(4) 0.3627(11) 0.4010(3) 0.050(2) Uani 1 1 d . . . H45 H 0.6641 0.3772 0.4380 0.060 Uiso 1 1 calc R . . C46 C 0.5930(3) 0.2944(10) 0.3785(3) 0.049(2) Uani 1 1 d . . . H46 H 0.5723 0.2655 0.4000 0.059 Uiso 1 1 calc R . . C47 C 0.5690(3) 0.2685(10) 0.3248(3) 0.0439(19) Uani 1 1 d . . . H47 H 0.5322 0.2192 0.3099 0.053 Uiso 1 1 calc R . . C48 C 0.6085(3) 0.1075(9) 0.1188(2) 0.0314(16) Uani 1 1 d . . . C49 C 0.6527(3) 0.1919(9) 0.1102(2) 0.0340(16) Uani 1 1 d . . . C50 C 0.6799(3) 0.1168(10) 0.0786(2) 0.0389(18) Uani 1 1 d . . . H50 H 0.7097 0.1768 0.0728 0.047 Uiso 1 1 calc R . . C51 C 0.6633(3) -0.0419(11) 0.0565(3) 0.044(2) Uani 1 1 d . . . H51 H 0.6820 -0.0901 0.0354 0.053 Uiso 1 1 calc R . . C52 C 0.6207(3) -0.1340(9) 0.0638(2) 0.0371(19) Uani 1 1 d . . . C53 C 0.6025(3) -0.3046(10) 0.0428(3) 0.049(2) Uani 1 1 d . . . H53 H 0.6200 -0.3565 0.0212 0.059 Uiso 1 1 calc R . . C54 C 0.5615(3) -0.3932(10) 0.0526(3) 0.051(2) Uani 1 1 d . . . H54 H 0.5503 -0.5039 0.0374 0.061 Uiso 1 1 calc R . . C55 C 0.5356(3) -0.3220(10) 0.0851(3) 0.047(2) Uani 1 1 d . . . H55 H 0.5075 -0.3866 0.0924 0.057 Uiso 1 1 calc R . . C56 C 0.5499(3) -0.1613(9) 0.1066(2) 0.0394(17) Uani 1 1 d . . . H56 H 0.5315 -0.1152 0.1283 0.047 Uiso 1 1 calc R . . C57 C 0.5930(3) -0.0612(9) 0.0966(2) 0.0346(18) Uani 1 1 d . . . C58 C 0.6757(3) 0.3642(9) 0.1365(2) 0.0362(18) Uani 1 1 d . . . H58A H 0.6906 0.4324 0.1139 0.043 Uiso 1 1 calc R . . H58B H 0.6448 0.4311 0.1415 0.043 Uiso 1 1 calc R . . C59 C 0.7767(3) 0.3311(9) 0.1972(3) 0.0385(17) Uani 1 1 d . . . C60 C 0.8003(3) 0.3970(11) 0.1584(3) 0.049(2) Uani 1 1 d . . . H60A H 0.7711 0.4631 0.1311 0.074 Uiso 1 1 calc R . . H60B H 0.8124 0.2996 0.1422 0.074 Uiso 1 1 calc R . . H60C H 0.8329 0.4717 0.1763 0.074 Uiso 1 1 calc R . . C61 C 0.7933(3) 0.2640(10) 0.2888(3) 0.051(2) Uani 1 1 d . . . H61A H 0.7792 0.3756 0.2956 0.076 Uiso 1 1 calc R . . H61B H 0.8249 0.2263 0.3203 0.076 Uiso 1 1 calc R . . H61C H 0.7627 0.1785 0.2798 0.076 Uiso 1 1 calc R . . C62 C 0.8741(3) 0.2787(10) 0.2559(3) 0.053(2) Uani 1 1 d . . . H62A H 0.8811 0.2284 0.2260 0.080 Uiso 1 1 calc R . . H62B H 0.8932 0.2093 0.2874 0.080 Uiso 1 1 calc R . . H62C H 0.8889 0.3968 0.2618 0.080 Uiso 1 1 calc R . . Br1 Br 0.67401(3) 0.84152(9) 0.46491(3) 0.0489(4) Uani 1 1 d . . . Br2 Br 0.32758(3) 0.40886(10) 0.03764(3) 0.0517(4) Uani 1 1 d . . . N1 N 0.2784(2) 0.7652(7) 0.3137(2) 0.0394(15) Uani 1 1 d . . . N2 N 0.1849(3) 0.7236(8) 0.2584(2) 0.0471(16) Uani 1 1 d . . . N3 N 0.7214(2) 0.3313(7) 0.1880(2) 0.0367(14) Uani 1 1 d . . . N4 N 0.8130(2) 0.2812(8) 0.2445(2) 0.0450(16) Uani 1 1 d . . . O1 O 0.34407(17) 0.6142(6) 0.27037(16) 0.0359(12) Uani 1 1 d . . . H1 H 0.3230 0.6651 0.2832 0.054 Uiso 1 1 calc R . . O2 O 0.65729(18) 0.1733(6) 0.22982(15) 0.0342(11) Uani 1 1 d . . . H2 H 0.6717 0.1394 0.2084 0.051 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 C1 0.024(3) 0.030(4) 0.035(4) 0.001(3) 0.006(3) 0.000(3) C2 0.022(3) 0.034(4) 0.032(3) 0.001(3) 0.001(3) -0.002(3) C3 0.024(3) 0.042(4) 0.029(3) -0.003(3) 0.003(3) -0.005(3) C4 0.027(4) 0.050(5) 0.032(4) 0.002(3) 0.008(3) 0.007(3) C5 0.023(4) 0.044(5) 0.044(4) 0.000(3) 0.009(3) 0.004(3) C6 0.025(4) 0.040(5) 0.034(4) 0.000(3) 0.007(3) -0.003(3) C7 0.026(4) 0.039(4) 0.035(4) 0.005(3) 0.008(3) 0.007(3) C8 0.030(4) 0.047(5) 0.031(4) 0.002(3) 0.010(3) 0.005(3) C9 0.034(4) 0.032(4) 0.028(3) -0.004(3) 0.011(3) -0.006(3) C10 0.024(4) 0.033(4) 0.035(4) 0.001(3) 0.007(3) 0.003(3) C11 0.040(4) 0.030(4) 0.027(3) -0.002(3) 0.007(3) -0.001(3) C12 0.043(4) 0.053(5) 0.037(4) 0.004(3) 0.010(3) 0.001(4) C13 0.060(6) 0.072(6) 0.035(4) -0.001(4) 0.021(4) -0.007(5) C14 0.052(6) 0.061(6) 0.039(4) 0.016(4) 0.010(4) -0.002(5) C15 0.033(4) 0.046(5) 0.042(4) 0.005(4) 0.003(3) 0.008(4) C16 0.032(4) 0.053(5) 0.035(4) 0.000(4) 0.012(3) 0.008(4) C17 0.018(3) 0.031(4) 0.026(3) 0.001(3) -0.001(2) -0.003(3) C18 0.021(3) 0.044(4) 0.026(3) -0.009(3) 0.001(3) -0.007(3) C19 0.024(4) 0.068(6) 0.034(4) -0.009(4) 0.006(3) -0.005(4) C20 0.037(5) 0.056(6) 0.029(4) -0.003(3) 0.008(3) -0.007(4) C21 0.027(4) 0.052(5) 0.026(3) -0.002(3) -0.002(3) -0.002(4) C22 0.038(4) 0.063(6) 0.032(4) -0.002(4) 0.006(3) -0.012(4) C23 0.047(5) 0.044(5) 0.038(4) 0.013(3) 0.005(4) -0.009(4) C24 0.032(4) 0.039(5) 0.053(5) 0.001(4) 0.003(3) 0.003(4) C25 0.032(4) 0.049(5) 0.035(4) 0.003(3) 0.010(3) -0.007(4) C26 0.028(4) 0.052(5) 0.033(4) -0.007(3) 0.008(3) -0.014(4) C27 0.028(4) 0.040(5) 0.042(4) -0.009(3) 0.003(3) 0.007(3) C28 0.025(4) 0.038(4) 0.043(4) 0.000(3) 0.005(3) -0.009(3) C29 0.033(5) 0.059(6) 0.072(6) 0.006(5) 0.023(4) 0.014(4) C30 0.054(6) 0.079(7) 0.050(5) -0.016(5) -0.003(4) 0.020(5) C31 0.025(4) 0.061(6) 0.076(6) 0.012(4) -0.008(4) -0.006(4) C32 0.025(3) 0.034(4) 0.034(4) -0.005(3) 0.011(3) -0.003(3) C33 0.030(4) 0.033(4) 0.027(3) 0.004(3) 0.013(3) -0.003(3) C34 0.026(4) 0.040(4) 0.027(3) -0.001(3) 0.012(3) -0.004(3) C35 0.028(4) 0.035(4) 0.031(3) 0.000(3) 0.010(3) 0.005(3) C36 0.024(3) 0.037(4) 0.036(4) -0.002(3) 0.012(3) -0.001(3) C37 0.024(4) 0.037(4) 0.038(4) -0.001(3) 0.013(3) 0.004(3) C38 0.023(4) 0.050(5) 0.041(4) 0.010(4) 0.009(3) -0.002(3) C39 0.029(4) 0.047(4) 0.028(3) 0.006(3) 0.008(3) 0.002(3) C40 0.030(4) 0.036(4) 0.032(4) -0.007(3) 0.008(3) -0.003(3) C41 0.034(4) 0.038(4) 0.024(3) -0.006(3) 0.011(3) -0.006(3) C42 0.038(4) 0.027(4) 0.032(3) -0.001(3) 0.014(3) -0.002(3) C43 0.033(4) 0.034(5) 0.042(4) -0.003(3) 0.004(3) 0.003(3) C44 0.049(5) 0.037(5) 0.044(4) -0.005(4) 0.006(4) -0.003(4) C45 0.061(6) 0.057(6) 0.026(4) -0.008(4) 0.010(4) 0.015(5) C46 0.053(5) 0.061(6) 0.033(4) -0.003(4) 0.017(3) 0.002(4) C47 0.035(4) 0.059(5) 0.034(4) -0.003(3) 0.009(3) -0.006(4) C48 0.031(4) 0.038(4) 0.023(3) 0.003(3) 0.007(3) 0.009(3) C49 0.031(4) 0.039(4) 0.028(4) 0.010(3) 0.006(3) 0.006(3) C50 0.030(4) 0.063(5) 0.023(3) 0.004(3) 0.009(3) 0.001(4) C51 0.033(4) 0.063(6) 0.036(4) -0.003(4) 0.013(3) 0.011(4) C52 0.037(4) 0.044(5) 0.021(3) 0.000(3) 0.001(3) 0.020(4) C53 0.044(5) 0.055(5) 0.039(4) -0.006(4) 0.005(3) 0.015(4) C54 0.055(5) 0.042(5) 0.044(5) -0.005(4) 0.004(4) 0.005(4) C55 0.043(5) 0.040(5) 0.045(4) 0.005(4) 0.000(4) 0.000(4) C56 0.034(4) 0.042(5) 0.034(4) 0.001(3) 0.003(3) -0.004(4) C57 0.032(4) 0.041(5) 0.019(3) 0.003(3) -0.005(3) 0.008(3) C58 0.022(4) 0.042(5) 0.038(4) 0.013(3) 0.003(3) 0.002(3) C59 0.039(4) 0.035(4) 0.041(4) -0.012(3) 0.013(3) -0.008(4) C60 0.038(5) 0.059(6) 0.052(5) -0.009(4) 0.018(4) -0.008(4) C61 0.055(5) 0.049(5) 0.035(4) 0.011(3) 0.001(4) -0.012(4) C62 0.038(5) 0.045(5) 0.059(5) -0.011(4) -0.003(4) 0.005(4) Br1 0.0267(6) 0.0762(10) 0.0374(5) -0.0050(4) 0.0043(4) -0.0093(4) Br2 0.0272(6) 0.0823(11) 0.0397(6) 0.0051(4) 0.0055(4) 0.0057(4) N1 0.024(3) 0.046(4) 0.038(3) -0.007(3) -0.001(2) -0.002(3) N2 0.037(4) 0.042(4) 0.050(4) 0.007(3) 0.001(3) 0.000(3) N3 0.024(3) 0.042(4) 0.035(3) 0.001(3) 0.000(2) -0.002(3) N4 0.026(3) 0.042(4) 0.048(4) -0.007(3) -0.008(3) 0.003(3) O1 0.021(2) 0.046(3) 0.036(3) -0.006(2) 0.004(2) -0.001(2) O2 0.037(3) 0.038(3) 0.024(2) 0.000(2) 0.007(2) 0.003(2) _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 C1 C2 1.411(8) . ? C1 C10 1.417(8) . ? C1 C17 1.529(8) . ? C2 C3 1.423(8) . ? C2 C7 1.442(9) . ? C3 C4 1.373(8) . ? C3 H3 0.9500 . ? C4 C5 1.415(9) . ? C4 H4 0.9500 . ? C5 C6 1.347(9) . ? C5 Br1 1.927(7) . ? C6 C7 1.430(9) . ? C6 H6 0.9500 . ? C7 C8 1.417(8) . ? C8 C9 1.379(8) . ? C8 H8 0.9500 . ? C9 C10 1.456(9) . ? C9 C11 1.491(8) . ? C10 O1 1.300(7) . ? C11 C16 1.378(9) . ? C11 C12 1.435(10) . ? C12 C13 1.412(9) . ? C12 H12 0.9500 . ? C13 C14 1.360(11) . ? C13 H13 0.9500 . ? C14 C15 1.399(10) . ? C14 H14 0.9500 . ? C15 C16 1.367(9) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.372(8) . ? C17 C26 1.446(9) . ? C18 C19 1.429(9) . ? C18 C27 1.526(9) . ? C19 C20 1.374(10) . ? C19 H19 0.9500 . ? C20 C21 1.399(10) . ? C20 H20 0.9500 . ? C21 C26 1.414(10) . ? C21 C22 1.444(10) . ? C22 C23 1.350(10) . ? C22 H22 0.9500 . ? C23 C24 1.427(9) . ? C23 H23 0.9500 . ? C24 C25 1.406(10) . ? C24 H24 0.9500 . ? C25 C26 1.414(10) . ? C25 H25 0.9500 . ? C27 N1 1.482(8) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 N1 1.324(8) . ? C28 N2 1.365(8) . ? C28 C29 1.496(10) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 N2 1.484(10) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 N2 1.468(9) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.402(8) . ? C32 C41 1.451(8) . ? C32 C48 1.506(8) . ? C33 O2 1.304(7) . ? C33 C34 1.475(8) . ? C34 C35 1.375(8) . ? C34 C42 1.479(8) . ? C35 C36 1.427(8) . ? C35 H35 0.9500 . ? C36 C37 1.413(9) . ? C36 C41 1.430(9) . ? C37 C38 1.370(9) . ? C37 H37 0.9500 . ? C38 C39 1.390(9) . ? C38 Br2 1.915(7) . ? C39 C40 1.374(8) . ? C39 H39 0.9500 . ? C40 C41 1.406(8) . ? C40 H40 0.9500 . ? C42 C43 1.392(9) . ? C42 C47 1.431(9) . ? C43 C44 1.400(9) . ? C43 H43 0.9500 . ? C44 C45 1.389(10) . ? C44 H44 0.9500 . ? C45 C46 1.389(11) . ? C45 H45 0.9500 . ? C46 C47 1.380(9) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? C48 C49 1.393(9) . ? C48 C57 1.434(10) . ? C49 C50 1.417(9) . ? C49 C58 1.527(9) . ? C50 C51 1.366(10) . ? C50 H50 0.9500 . ? C51 C52 1.373(10) . ? C51 H51 0.9500 . ? C52 C57 1.446(9) . ? C52 C53 1.448(10) . ? C53 C54 1.353(11) . ? C53 H53 0.9500 . ? C54 C55 1.403(10) . ? C54 H54 0.9500 . ? C55 C56 1.368(10) . ? C55 H55 0.9500 . ? C56 C57 1.448(9) . ? C56 H56 0.9500 . ? C58 N3 1.480(8) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 N3 1.331(9) . ? C59 N4 1.339(8) . ? C59 C60 1.491(9) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 N4 1.478(9) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 N4 1.466(9) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? O1 H1 0.8400 . ? O2 H2 0.8400 . ? 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 C2 C1 C10 122.7(6) . . ? C2 C1 C17 118.1(5) . . ? C10 C1 C17 119.1(5) . . ? C1 C2 C3 124.4(6) . . ? C1 C2 C7 119.1(5) . . ? C3 C2 C7 116.5(6) . . ? C4 C3 C2 122.3(6) . . ? C4 C3 H3 118.9 . . ? C2 C3 H3 118.9 . . ? C3 C4 C5 119.0(6) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C6 C5 C4 122.6(6) . . ? C6 C5 Br1 119.7(5) . . ? C4 C5 Br1 117.7(5) . . ? C5 C6 C7 119.1(6) . . ? C5 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? C8 C7 C6 121.6(6) . . ? C8 C7 C2 117.9(6) . . ? C6 C7 C2 120.6(6) . . ? C9 C8 C7 123.2(6) . . ? C9 C8 H8 118.4 . . ? C7 C8 H8 118.4 . . ? C8 C9 C10 119.8(6) . . ? C8 C9 C11 119.2(6) . . ? C10 C9 C11 120.8(6) . . ? O1 C10 C1 122.0(6) . . ? O1 C10 C9 120.7(5) . . ? C1 C10 C9 117.2(6) . . ? C16 C11 C12 117.0(6) . . ? C16 C11 C9 123.9(6) . . ? C12 C11 C9 119.1(6) . . ? C13 C12 C11 119.5(7) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C14 C13 C12 121.0(7) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C15 119.2(7) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C16 C15 C14 120.5(7) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 C11 122.7(7) . . ? C15 C16 H16 118.7 . . ? C11 C16 H16 118.7 . . ? C18 C17 C26 118.7(6) . . ? C18 C17 C1 122.0(6) . . ? C26 C17 C1 119.3(6) . . ? C17 C18 C19 121.2(6) . . ? C17 C18 C27 122.5(6) . . ? C19 C18 C27 116.2(6) . . ? C20 C19 C18 119.9(7) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 120.7(7) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C20 C21 C26 119.9(7) . . ? C20 C21 C22 119.8(7) . . ? C26 C21 C22 120.3(7) . . ? C23 C22 C21 118.0(7) . . ? C23 C22 H22 121.0 . . ? C21 C22 H22 121.0 . . ? C22 C23 C24 124.3(7) . . ? C22 C23 H23 117.9 . . ? C24 C23 H23 117.9 . . ? C25 C24 C23 117.1(7) . . ? C25 C24 H24 121.5 . . ? C23 C24 H24 121.5 . . ? C24 C25 C26 121.3(7) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C25 C26 C21 119.1(7) . . ? C25 C26 C17 121.4(6) . . ? C21 C26 C17 119.5(7) . . ? N1 C27 C18 109.2(5) . . ? N1 C27 H27A 109.8 . . ? C18 C27 H27A 109.8 . . ? N1 C27 H27B 109.8 . . ? C18 C27 H27B 109.8 . . ? H27A C27 H27B 108.3 . . ? N1 C28 N2 118.9(6) . . ? N1 C28 C29 122.4(6) . . ? N2 C28 C29 118.7(6) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N2 C30 H30A 109.5 . . ? N2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N2 C31 H31A 109.5 . . ? N2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C41 120.9(5) . . ? C33 C32 C48 120.6(6) . . ? C41 C32 C48 118.5(5) . . ? O2 C33 C32 122.3(6) . . ? O2 C33 C34 118.9(5) . . ? C32 C33 C34 118.7(6) . . ? C35 C34 C33 119.5(5) . . ? C35 C34 C42 120.5(6) . . ? C33 C34 C42 120.0(6) . . ? C34 C35 C36 122.7(6) . . ? C34 C35 H35 118.7 . . ? C36 C35 H35 118.7 . . ? C37 C36 C35 121.3(6) . . ? C37 C36 C41 120.0(6) . . ? C35 C36 C41 118.7(6) . . ? C38 C37 C36 119.7(6) . . ? C38 C37 H37 120.1 . . ? C36 C37 H37 120.1 . . ? C37 C38 C39 121.7(6) . . ? C37 C38 Br2 119.6(5) . . ? C39 C38 Br2 118.7(5) . . ? C40 C39 C38 118.8(6) . . ? C40 C39 H39 120.6 . . ? C38 C39 H39 120.6 . . ? C39 C40 C41 122.9(6) . . ? C39 C40 H40 118.5 . . ? C41 C40 H40 118.5 . . ? C40 C41 C36 116.8(6) . . ? C40 C41 C32 123.7(6) . . ? C36 C41 C32 119.4(5) . . ? C43 C42 C47 117.6(6) . . ? C43 C42 C34 121.8(6) . . ? C47 C42 C34 120.6(6) . . ? C42 C43 C44 121.0(7) . . ? C42 C43 H43 119.5 . . ? C44 C43 H43 119.5 . . ? C45 C44 C43 120.1(8) . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C46 C45 C44 120.1(7) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C47 C46 C45 120.1(7) . . ? C47 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? C46 C47 C42 121.0(7) . . ? C46 C47 H47 119.5 . . ? C42 C47 H47 119.5 . . ? C49 C48 C57 118.0(6) . . ? C49 C48 C32 122.3(6) . . ? C57 C48 C32 119.7(6) . . ? C48 C49 C50 121.1(6) . . ? C48 C49 C58 121.5(6) . . ? C50 C49 C58 117.4(6) . . ? C51 C50 C49 120.0(7) . . ? C51 C50 H50 120.0 . . ? C49 C50 H50 120.0 . . ? C50 C51 C52 122.3(7) . . ? C50 C51 H51 118.8 . . ? C52 C51 H51 118.8 . . ? C51 C52 C57 118.6(7) . . ? C51 C52 C53 124.8(7) . . ? C57 C52 C53 116.5(7) . . ? C54 C53 C52 122.7(7) . . ? C54 C53 H53 118.7 . . ? C52 C53 H53 118.7 . . ? C53 C54 C55 120.2(7) . . ? C53 C54 H54 119.9 . . ? C55 C54 H54 119.9 . . ? C56 C55 C54 121.3(7) . . ? C56 C55 H55 119.4 . . ? C54 C55 H55 119.4 . . ? C55 C56 C57 120.4(7) . . ? C55 C56 H56 119.8 . . ? C57 C56 H56 119.8 . . ? C48 C57 C56 121.1(6) . . ? C48 C57 C52 119.9(7) . . ? C56 C57 C52 119.0(7) . . ? N3 C58 C49 109.0(5) . . ? N3 C58 H58A 109.9 . . ? C49 C58 H58A 109.9 . . ? N3 C58 H58B 109.9 . . ? C49 C58 H58B 109.9 . . ? H58A C58 H58B 108.3 . . ? N3 C59 N4 118.9(6) . . ? N3 C59 C60 122.6(6) . . ? N4 C59 C60 118.3(7) . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N4 C61 H61A 109.5 . . ? N4 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? N4 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? N4 C62 H62A 109.5 . . ? N4 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? N4 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C28 N1 C27 125.6(6) . . ? C28 N2 C31 120.5(7) . . ? C28 N2 C30 118.5(6) . . ? C31 N2 C30 120.1(6) . . ? C59 N3 C58 125.5(6) . . ? C59 N4 C62 120.3(7) . . ? C59 N4 C61 119.9(6) . . ? C62 N4 C61 118.6(6) . . ? C10 O1 H1 109.5 . . ? C33 O2 H2 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 C10 C1 C2 C3 178.2(6) . . . . ? C17 C1 C2 C3 1.5(10) . . . . ? C10 C1 C2 C7 -2.2(10) . . . . ? C17 C1 C2 C7 -178.9(6) . . . . ? C1 C2 C3 C4 179.2(6) . . . . ? C7 C2 C3 C4 -0.4(10) . . . . ? C2 C3 C4 C5 0.9(10) . . . . ? C3 C4 C5 C6 -0.6(11) . . . . ? C3 C4 C5 Br1 -179.4(5) . . . . ? C4 C5 C6 C7 -0.2(11) . . . . ? Br1 C5 C6 C7 178.6(5) . . . . ? C5 C6 C7 C8 179.6(6) . . . . ? C5 C6 C7 C2 0.6(10) . . . . ? C1 C2 C7 C8 1.0(10) . . . . ? C3 C2 C7 C8 -179.4(6) . . . . ? C1 C2 C7 C6 -180.0(6) . . . . ? C3 C2 C7 C6 -0.3(9) . . . . ? C6 C7 C8 C9 -179.9(6) . . . . ? C2 C7 C8 C9 -0.9(10) . . . . ? C7 C8 C9 C10 1.8(10) . . . . ? C7 C8 C9 C11 177.3(6) . . . . ? C2 C1 C10 O1 179.7(6) . . . . ? C17 C1 C10 O1 -3.7(9) . . . . ? C2 C1 C10 C9 3.1(10) . . . . ? C17 C1 C10 C9 179.7(6) . . . . ? C8 C9 C10 O1 -179.4(6) . . . . ? C11 C9 C10 O1 5.1(9) . . . . ? C8 C9 C10 C1 -2.8(9) . . . . ? C11 C9 C10 C1 -178.3(6) . . . . ? C8 C9 C11 C16 -145.7(7) . . . . ? C10 C9 C11 C16 29.8(10) . . . . ? C8 C9 C11 C12 33.5(9) . . . . ? C10 C9 C11 C12 -151.0(6) . . . . ? C16 C11 C12 C13 3.4(10) . . . . ? C9 C11 C12 C13 -175.8(6) . . . . ? C11 C12 C13 C14 -3.2(12) . . . . ? C12 C13 C14 C15 2.3(13) . . . . ? C13 C14 C15 C16 -1.7(13) . . . . ? C14 C15 C16 C11 2.2(13) . . . . ? C12 C11 C16 C15 -3.0(11) . . . . ? C9 C11 C16 C15 176.2(7) . . . . ? C2 C1 C17 C18 109.8(7) . . . . ? C10 C1 C17 C18 -66.9(8) . . . . ? C2 C1 C17 C26 -68.2(8) . . . . ? C10 C1 C17 C26 115.0(7) . . . . ? C26 C17 C18 C19 2.1(8) . . . . ? C1 C17 C18 C19 -175.9(6) . . . . ? C26 C17 C18 C27 -174.3(6) . . . . ? C1 C17 C18 C27 7.7(9) . . . . ? C17 C18 C19 C20 -0.1(9) . . . . ? C27 C18 C19 C20 176.5(6) . . . . ? C18 C19 C20 C21 -1.2(10) . . . . ? C19 C20 C21 C26 0.5(10) . . . . ? C19 C20 C21 C22 -178.8(6) . . . . ? C20 C21 C22 C23 177.6(6) . . . . ? C26 C21 C22 C23 -1.7(10) . . . . ? C21 C22 C23 C24 1.5(10) . . . . ? C22 C23 C24 C25 -0.5(10) . . . . ? C23 C24 C25 C26 -0.2(10) . . . . ? C24 C25 C26 C21 -0.1(10) . . . . ? C24 C25 C26 C17 -179.9(6) . . . . ? C20 C21 C26 C25 -178.2(6) . . . . ? C22 C21 C26 C25 1.1(10) . . . . ? C20 C21 C26 C17 1.6(9) . . . . ? C22 C21 C26 C17 -179.1(6) . . . . ? C18 C17 C26 C25 177.0(6) . . . . ? C1 C17 C26 C25 -4.9(9) . . . . ? C18 C17 C26 C21 -2.8(9) . . . . ? C1 C17 C26 C21 175.3(6) . . . . ? C17 C18 C27 N1 90.1(7) . . . . ? C19 C18 C27 N1 -86.5(7) . . . . ? C41 C32 C33 O2 -179.7(6) . . . . ? C48 C32 C33 O2 -1.9(10) . . . . ? C41 C32 C33 C34 3.5(9) . . . . ? C48 C32 C33 C34 -178.6(6) . . . . ? O2 C33 C34 C35 -179.4(6) . . . . ? C32 C33 C34 C35 -2.6(10) . . . . ? O2 C33 C34 C42 -0.6(9) . . . . ? C32 C33 C34 C42 176.3(6) . . . . ? C33 C34 C35 C36 0.8(10) . . . . ? C42 C34 C35 C36 -178.1(6) . . . . ? C34 C35 C36 C37 -177.6(6) . . . . ? C34 C35 C36 C41 0.0(10) . . . . ? C35 C36 C37 C38 -179.2(6) . . . . ? C41 C36 C37 C38 3.2(10) . . . . ? C36 C37 C38 C39 -1.9(11) . . . . ? C36 C37 C38 Br2 178.9(5) . . . . ? C37 C38 C39 C40 0.9(11) . . . . ? Br2 C38 C39 C40 -179.9(5) . . . . ? C38 C39 C40 C41 -1.4(10) . . . . ? C39 C40 C41 C36 2.7(10) . . . . ? C39 C40 C41 C32 -179.5(6) . . . . ? C37 C36 C41 C40 -3.6(10) . . . . ? C35 C36 C41 C40 178.8(6) . . . . ? C37 C36 C41 C32 178.5(6) . . . . ? C35 C36 C41 C32 1.0(10) . . . . ? C33 C32 C41 C40 179.5(6) . . . . ? C48 C32 C41 C40 1.6(10) . . . . ? C33 C32 C41 C36 -2.8(10) . . . . ? C48 C32 C41 C36 179.3(6) . . . . ? C35 C34 C42 C43 -136.1(7) . . . . ? C33 C34 C42 C43 45.0(9) . . . . ? C35 C34 C42 C47 43.0(9) . . . . ? C33 C34 C42 C47 -135.9(7) . . . . ? C47 C42 C43 C44 -1.5(10) . . . . ? C34 C42 C43 C44 177.7(6) . . . . ? C42 C43 C44 C45 2.0(11) . . . . ? C43 C44 C45 C46 -2.2(12) . . . . ? C44 C45 C46 C47 1.9(12) . . . . ? C45 C46 C47 C42 -1.5(12) . . . . ? C43 C42 C47 C46 1.2(10) . . . . ? C34 C42 C47 C46 -177.9(7) . . . . ? C33 C32 C48 C49 -66.7(8) . . . . ? C41 C32 C48 C49 111.2(7) . . . . ? C33 C32 C48 C57 113.2(7) . . . . ? C41 C32 C48 C57 -68.9(8) . . . . ? C57 C48 C49 C50 2.8(9) . . . . ? C32 C48 C49 C50 -177.3(6) . . . . ? C57 C48 C49 C58 -174.2(5) . . . . ? C32 C48 C49 C58 5.7(9) . . . . ? C48 C49 C50 C51 -0.8(9) . . . . ? C58 C49 C50 C51 176.3(6) . . . . ? C49 C50 C51 C52 -0.1(10) . . . . ? C50 C51 C52 C57 -1.0(10) . . . . ? C50 C51 C52 C53 -178.0(7) . . . . ? C51 C52 C53 C54 177.5(7) . . . . ? C57 C52 C53 C54 0.4(10) . . . . ? C52 C53 C54 C55 -1.3(11) . . . . ? C53 C54 C55 C56 1.5(11) . . . . ? C54 C55 C56 C57 -0.7(10) . . . . ? C49 C48 C57 C56 176.1(6) . . . . ? C32 C48 C57 C56 -3.9(8) . . . . ? C49 C48 C57 C52 -3.8(9) . . . . ? C32 C48 C57 C52 176.3(5) . . . . ? C55 C56 C57 C48 179.9(6) . . . . ? C55 C56 C57 C52 -0.2(9) . . . . ? C51 C52 C57 C48 2.9(9) . . . . ? C53 C52 C57 C48 -179.8(6) . . . . ? C51 C52 C57 C56 -176.9(6) . . . . ? C53 C52 C57 C56 0.4(9) . . . . ? C48 C49 C58 N3 88.9(7) . . . . ? C50 C49 C58 N3 -88.2(7) . . . . ? N2 C28 N1 C27 -171.4(6) . . . . ? C29 C28 N1 C27 9.4(11) . . . . ? C18 C27 N1 C28 102.6(8) . . . . ? N1 C28 N2 C31 177.4(7) . . . . ? C29 C28 N2 C31 -3.4(10) . . . . ? N1 C28 N2 C30 -13.8(10) . . . . ? C29 C28 N2 C30 165.3(7) . . . . ? N4 C59 N3 C58 -173.0(6) . . . . ? C60 C59 N3 C58 11.9(11) . . . . ? C49 C58 N3 C59 96.7(8) . . . . ? N3 C59 N4 C62 179.7(6) . . . . ? C60 C59 N4 C62 -4.9(10) . . . . ? N3 C59 N4 C61 -13.2(10) . . . . ? C60 C59 N4 C61 162.2(7) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.208 _refine_diff_density_min -0.718 _refine_diff_density_rms 0.112