data_10059 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H31 N10 O3, Br' _chemical_formula_sum 'C30 H31 Br N10 O3' _chemical_formula_weight 659.56 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 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.2935(19) _cell_length_b 11.3515(17) _cell_length_c 19.928(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.895(3) _cell_angle_gamma 90.00 _cell_volume 2978.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5831 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 27.00 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 1.431 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6052 _exptl_absorpt_correction_T_max 0.8033 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2007)' _exptl_special_details ; ; _diffrn_ambient_temperature 100(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 Bruker APEX' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28725 _diffrn_reflns_av_R_equivalents 0.1087 _diffrn_reflns_av_sigmaI/netI 0.0932 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 26.37 _reflns_number_total 6091 _reflns_number_gt 4188 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART, 1998' _computing_cell_refinement 'Bruker SAINT, 1998' _computing_data_reduction 'Bruker SAINT, 1998' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _refine_special_details ; ; _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^)+(0.0480P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6091 _refine_ls_number_parameters 418 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0909 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1150 _refine_ls_wR_factor_gt 0.1037 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 N1 N 0.6587(2) 0.2363(2) 0.62109(15) 0.0154(7) Uani 1 1 d . . . H1 H 0.592(3) 0.268(3) 0.6072(17) 0.018 Uiso 1 1 d . . . C2 C 0.7208(3) 0.3167(3) 0.67046(18) 0.0194(8) Uani 1 1 d . . . H2A H 0.7356 0.3897 0.6465 0.023 Uiso 1 1 calc R . . H2B H 0.7864 0.2778 0.6864 0.023 Uiso 1 1 calc R . . C3 C 0.6702(3) 0.3498(3) 0.73186(19) 0.0231(9) Uani 1 1 d . . . H3A H 0.6475 0.2768 0.7525 0.028 Uiso 1 1 calc R . . H3B H 0.7213 0.3880 0.7658 0.028 Uiso 1 1 calc R . . N4 N 0.5835(2) 0.4286(3) 0.71690(15) 0.0205(7) Uani 1 1 d . . . H4 H 0.598(3) 0.509(3) 0.7126(18) 0.025 Uiso 1 1 d . . . C5 C 0.4857(3) 0.3929(3) 0.71381(17) 0.0172(8) Uani 1 1 d . . . O6 O 0.46008(19) 0.2891(2) 0.71895(13) 0.0233(6) Uani 1 1 d . . . N7 N 0.4181(2) 0.4848(3) 0.70397(15) 0.0180(7) Uani 1 1 d . . . H7 H 0.443(3) 0.549(3) 0.6999(18) 0.022 Uiso 1 1 d . . . C8 C 0.3145(3) 0.4850(3) 0.70755(17) 0.0165(8) Uani 1 1 d . . . C9 C 0.2634(3) 0.3946(3) 0.73700(17) 0.0192(8) Uani 1 1 d . . . H9 H 0.2998 0.3275 0.7555 0.023 Uiso 1 1 calc R . . C10 C 0.1601(3) 0.4029(3) 0.73914(17) 0.0182(8) Uani 1 1 d . . . H10 H 0.1262 0.3414 0.7594 0.022 Uiso 1 1 calc R . . C11 C 0.1046(3) 0.5008(3) 0.71180(17) 0.0172(8) Uani 1 1 d . . . C12 C 0.1567(3) 0.5925(3) 0.68402(18) 0.0195(8) Uani 1 1 d . . . H12 H 0.1207 0.6605 0.6663 0.023 Uiso 1 1 calc R . . C13 C 0.2595(3) 0.5844(3) 0.68229(18) 0.0190(8) Uani 1 1 d . . . H13 H 0.2938 0.6473 0.6636 0.023 Uiso 1 1 calc R . . C14 C -0.0029(3) 0.5076(3) 0.71113(17) 0.0185(8) Uani 1 1 d . . . N15 N -0.0902(2) 0.5138(3) 0.70863(15) 0.0242(8) Uani 1 1 d . . . C16 C 0.7076(3) 0.2236(3) 0.55696(17) 0.0179(8) Uani 1 1 d . . . H16A H 0.7824 0.2245 0.5690 0.021 Uiso 1 1 calc R . . H16B H 0.6883 0.1465 0.5358 0.021 Uiso 1 1 calc R . . C17 C 0.6767(3) 0.3207(3) 0.50599(18) 0.0196(8) Uani 1 1 d . . . H17A H 0.6826 0.3974 0.5298 0.023 Uiso 1 1 calc R . . H17B H 0.7246 0.3214 0.4721 0.023 Uiso 1 1 calc R . . N18 N 0.5738(2) 0.3083(3) 0.47086(16) 0.0195(7) Uani 1 1 d . . . H18 H 0.560(3) 0.276(3) 0.4346(19) 0.023 Uiso 1 1 d . . . C19 C 0.4923(3) 0.3420(3) 0.50046(19) 0.0182(8) Uani 1 1 d . . . O20 O 0.50149(17) 0.3746(2) 0.56059(12) 0.0194(6) Uani 1 1 d . . . N21 N 0.4019(2) 0.3376(3) 0.45916(15) 0.0193(7) Uani 1 1 d . . . H21 H 0.405(3) 0.320(3) 0.4199(19) 0.023 Uiso 1 1 d . . . C22 C 0.3044(3) 0.3486(3) 0.47694(18) 0.0168(8) Uani 1 1 d . . . C23 C 0.2842(3) 0.3653(3) 0.54309(19) 0.0217(9) Uani 1 1 d . . . H23 H 0.3385 0.3741 0.5791 0.026 Uiso 1 1 calc R . . C24 C 0.1851(3) 0.3690(3) 0.55588(18) 0.0222(9) Uani 1 1 d . . . H24 H 0.1714 0.3798 0.6010 0.027 Uiso 1 1 calc R . . C25 C 0.1051(3) 0.3572(3) 0.50399(19) 0.0193(8) Uani 1 1 d . . . C26 C 0.1252(3) 0.3450(3) 0.43827(19) 0.0261(9) Uani 1 1 d . . . H26 H 0.0707 0.3390 0.4022 0.031 Uiso 1 1 calc R . . C27 C 0.2236(3) 0.3413(3) 0.42467(19) 0.0228(9) Uani 1 1 d . . . H27 H 0.2367 0.3338 0.3792 0.027 Uiso 1 1 calc R . . C28 C 0.0021(3) 0.3566(3) 0.5193(2) 0.0236(9) Uani 1 1 d . . . N29 N -0.0801(3) 0.3533(3) 0.53124(18) 0.0333(9) Uani 1 1 d . . . C30 C 0.6453(3) 0.1170(3) 0.65175(19) 0.0217(9) Uani 1 1 d . . . H30A H 0.7097 0.0726 0.6532 0.026 Uiso 1 1 calc R . . H30B H 0.6320 0.1278 0.6990 0.026 Uiso 1 1 calc R . . C31 C 0.5607(3) 0.0446(3) 0.61436(19) 0.0236(9) Uani 1 1 d . . . H31A H 0.5680 0.0418 0.5656 0.028 Uiso 1 1 calc R . . H31B H 0.5647 -0.0371 0.6320 0.028 Uiso 1 1 calc R . . N32 N 0.4631(2) 0.0955(3) 0.62286(17) 0.0235(8) Uani 1 1 d . . . H32 H 0.463(3) 0.150(3) 0.6496(19) 0.028 Uiso 1 1 d . . . C33 C 0.3764(3) 0.0352(3) 0.60412(18) 0.0219(9) Uani 1 1 d . . . O34 O 0.37300(19) -0.0594(2) 0.57406(13) 0.0259(6) Uani 1 1 d . . . N35 N 0.2913(2) 0.0902(3) 0.62261(16) 0.0231(8) Uani 1 1 d . . . H35 H 0.304(3) 0.159(3) 0.6416(19) 0.028 Uiso 1 1 d . . . C36 C 0.1911(3) 0.0521(3) 0.61324(18) 0.0216(9) Uani 1 1 d . . . C37 C 0.1565(3) -0.0493(3) 0.57776(19) 0.0263(10) Uani 1 1 d . . . H37 H 0.2027 -0.0978 0.5580 0.032 Uiso 1 1 calc R . . C38 C 0.0557(3) -0.0786(3) 0.5715(2) 0.0287(10) Uani 1 1 d . . . H38 H 0.0331 -0.1477 0.5470 0.034 Uiso 1 1 calc R . . C39 C -0.0149(3) -0.0104(3) 0.59980(19) 0.0250(9) Uani 1 1 d . . . C40 C 0.0195(3) 0.0908(3) 0.63572(18) 0.0239(9) Uani 1 1 d . . . H40 H -0.0268 0.1390 0.6556 0.029 Uiso 1 1 calc R . . C41 C 0.1205(3) 0.1205(3) 0.64216(19) 0.0251(9) Uani 1 1 d . . . H41 H 0.1432 0.1893 0.6669 0.030 Uiso 1 1 calc R . . C42 C -0.1208(3) -0.0409(3) 0.5924(2) 0.0293(10) Uani 1 1 d . . . N43 N -0.2055(3) -0.0632(3) 0.5869(2) 0.0422(10) Uani 1 1 d . . . Br1 Br 0.56028(3) 0.72617(3) 0.700263(18) 0.01964(12) Uani 1 1 d . . . 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 N1 0.0151(16) 0.0144(16) 0.0170(16) -0.0001(13) 0.0039(13) 0.0026(13) C2 0.014(2) 0.021(2) 0.022(2) -0.0015(16) -0.0018(16) -0.0002(16) C3 0.022(2) 0.025(2) 0.021(2) -0.0051(17) -0.0002(17) 0.0037(17) N4 0.0177(18) 0.0198(17) 0.0234(18) -0.0004(14) 0.0007(14) 0.0031(14) C5 0.021(2) 0.020(2) 0.0109(19) -0.0020(16) 0.0049(16) 0.0012(17) O6 0.0265(15) 0.0186(15) 0.0256(15) -0.0030(12) 0.0064(12) 0.0032(12) N7 0.0182(18) 0.0143(16) 0.0213(18) -0.0018(14) 0.0026(14) -0.0029(14) C8 0.017(2) 0.021(2) 0.0117(19) -0.0032(15) 0.0014(16) -0.0019(16) C9 0.024(2) 0.018(2) 0.016(2) 0.0011(16) 0.0028(16) 0.0028(16) C10 0.024(2) 0.0170(19) 0.0144(19) -0.0032(16) 0.0038(16) -0.0046(16) C11 0.019(2) 0.021(2) 0.0112(18) -0.0043(15) 0.0010(15) -0.0002(16) C12 0.023(2) 0.0152(19) 0.019(2) -0.0002(16) 0.0010(17) 0.0028(16) C13 0.022(2) 0.0133(19) 0.022(2) 0.0004(16) 0.0050(17) -0.0023(16) C14 0.027(2) 0.018(2) 0.0112(19) -0.0033(15) 0.0034(17) -0.0017(17) N15 0.025(2) 0.0285(19) 0.0187(18) -0.0012(15) 0.0026(15) -0.0005(15) C16 0.015(2) 0.0203(19) 0.019(2) -0.0001(17) 0.0072(16) 0.0022(17) C17 0.019(2) 0.023(2) 0.017(2) -0.0015(16) 0.0030(16) -0.0001(17) N18 0.0176(18) 0.0245(19) 0.0164(17) -0.0027(14) 0.0019(15) 0.0006(14) C19 0.024(2) 0.0115(18) 0.019(2) 0.0055(16) 0.0031(18) -0.0020(16) O20 0.0190(15) 0.0233(14) 0.0151(14) -0.0047(11) -0.0006(11) 0.0030(11) N21 0.0198(19) 0.0287(19) 0.0090(16) -0.0027(14) 0.0008(15) -0.0011(14) C22 0.020(2) 0.0138(19) 0.017(2) 0.0034(15) 0.0031(16) -0.0014(15) C23 0.023(2) 0.022(2) 0.019(2) -0.0027(17) -0.0003(17) -0.0034(17) C24 0.027(2) 0.022(2) 0.018(2) -0.0038(17) 0.0054(18) -0.0006(17) C25 0.020(2) 0.0147(19) 0.023(2) 0.0017(16) 0.0022(17) 0.0004(16) C26 0.023(2) 0.030(2) 0.023(2) 0.0078(18) -0.0043(18) -0.0037(18) C27 0.025(2) 0.027(2) 0.016(2) 0.0010(17) 0.0009(17) -0.0033(18) C28 0.022(2) 0.016(2) 0.033(2) -0.0004(17) 0.0031(19) -0.0008(17) N29 0.024(2) 0.028(2) 0.048(2) 0.0020(17) 0.0065(18) -0.0032(16) C30 0.025(2) 0.018(2) 0.023(2) 0.0044(16) 0.0061(18) 0.0039(17) C31 0.030(2) 0.014(2) 0.028(2) 0.0003(17) 0.0072(18) -0.0024(17) N32 0.024(2) 0.0198(19) 0.028(2) -0.0046(15) 0.0069(16) -0.0009(15) C33 0.029(2) 0.021(2) 0.016(2) 0.0040(17) 0.0034(18) 0.0032(18) O34 0.0309(16) 0.0211(15) 0.0259(16) -0.0085(12) 0.0045(13) 0.0020(12) N35 0.026(2) 0.0162(18) 0.0263(19) -0.0059(15) 0.0024(15) 0.0030(15) C36 0.028(2) 0.024(2) 0.012(2) 0.0026(16) 0.0030(17) 0.0034(18) C37 0.027(2) 0.023(2) 0.030(2) -0.0083(18) 0.0077(19) 0.0018(18) C38 0.030(3) 0.021(2) 0.037(3) -0.0132(19) 0.008(2) -0.0016(18) C39 0.028(2) 0.024(2) 0.024(2) 0.0016(18) 0.0082(19) 0.0047(18) C40 0.033(3) 0.021(2) 0.019(2) 0.0015(17) 0.0090(18) 0.0096(18) C41 0.032(3) 0.021(2) 0.022(2) -0.0047(17) 0.0037(18) 0.0050(18) C42 0.032(3) 0.024(2) 0.035(3) -0.0007(19) 0.015(2) 0.007(2) N43 0.034(2) 0.031(2) 0.066(3) -0.006(2) 0.020(2) 0.0044(18) Br1 0.0224(2) 0.01961(19) 0.0175(2) -0.00066(17) 0.00481(15) -0.00211(17) _geom_special_details ; ; 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 N1 C2 1.503(5) . ? N1 C30 1.507(4) . ? N1 C16 1.519(4) . ? N1 H1 0.96(3) . ? C2 C3 1.522(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N4 1.457(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N4 C5 1.355(4) . ? N4 H4 0.94(4) . ? C5 O6 1.235(4) . ? C5 N7 1.374(4) . ? N7 C8 1.389(4) . ? N7 H7 0.81(4) . ? C8 C13 1.400(5) . ? C8 C9 1.403(5) . ? C9 C10 1.383(5) . ? C9 H9 0.9500 . ? C10 C11 1.402(5) . ? C10 H10 0.9500 . ? C11 C12 1.405(5) . ? C11 C14 1.429(5) . ? C12 C13 1.375(5) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 N15 1.158(4) . ? C16 C17 1.516(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 N18 1.455(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? N18 C19 1.358(4) . ? N18 H18 0.81(4) . ? C19 O20 1.244(4) . ? C19 N21 1.361(5) . ? N21 C22 1.395(4) . ? N21 H21 0.81(4) . ? C22 C27 1.392(5) . ? C22 C23 1.394(5) . ? C23 C24 1.377(5) . ? C23 H23 0.9500 . ? C24 C25 1.384(5) . ? C24 H24 0.9500 . ? C25 C26 1.380(5) . ? C25 C28 1.443(5) . ? C26 C27 1.372(5) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 N29 1.150(4) . ? C30 C31 1.505(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 N32 1.452(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? N32 C33 1.348(5) . ? N32 H32 0.81(4) . ? C33 O34 1.228(4) . ? C33 N35 1.385(5) . ? N35 C36 1.388(5) . ? N35 H35 0.87(4) . ? C36 C37 1.395(5) . ? C36 C41 1.402(5) . ? C37 C38 1.369(5) . ? C37 H37 0.9500 . ? C38 C39 1.395(5) . ? C38 H38 0.9500 . ? C39 C40 1.397(5) . ? C39 C42 1.438(5) . ? C40 C41 1.373(5) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 N43 1.144(5) . ? 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 N1 C30 111.4(3) . . ? C2 N1 C16 110.4(3) . . ? C30 N1 C16 110.1(3) . . ? C2 N1 H1 111(2) . . ? C30 N1 H1 107(2) . . ? C16 N1 H1 106(2) . . ? N1 C2 C3 114.3(3) . . ? N1 C2 H2A 108.7 . . ? C3 C2 H2A 108.7 . . ? N1 C2 H2B 108.7 . . ? C3 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? N4 C3 C2 114.3(3) . . ? N4 C3 H3A 108.7 . . ? C2 C3 H3A 108.7 . . ? N4 C3 H3B 108.7 . . ? C2 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C5 N4 C3 123.6(3) . . ? C5 N4 H4 120(2) . . ? C3 N4 H4 117(2) . . ? O6 C5 N4 123.7(3) . . ? O6 C5 N7 123.7(3) . . ? N4 C5 N7 112.6(3) . . ? C5 N7 C8 128.9(3) . . ? C5 N7 H7 115(3) . . ? C8 N7 H7 115(3) . . ? N7 C8 C13 117.1(3) . . ? N7 C8 C9 124.2(3) . . ? C13 C8 C9 118.7(3) . . ? C10 C9 C8 120.2(3) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 120.9(3) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C10 C11 C12 118.6(3) . . ? C10 C11 C14 121.2(3) . . ? C12 C11 C14 120.2(3) . . ? C13 C12 C11 120.4(3) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C8 121.1(3) . . ? C12 C13 H13 119.4 . . ? C8 C13 H13 119.4 . . ? N15 C14 C11 178.0(4) . . ? C17 C16 N1 112.7(3) . . ? C17 C16 H16A 109.0 . . ? N1 C16 H16A 109.0 . . ? C17 C16 H16B 109.0 . . ? N1 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? N18 C17 C16 113.8(3) . . ? N18 C17 H17A 108.8 . . ? C16 C17 H17A 108.8 . . ? N18 C17 H17B 108.8 . . ? C16 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? C19 N18 C17 121.2(3) . . ? C19 N18 H18 114(3) . . ? C17 N18 H18 124(3) . . ? O20 C19 N18 121.5(3) . . ? O20 C19 N21 123.8(3) . . ? N18 C19 N21 114.7(3) . . ? C19 N21 C22 128.1(3) . . ? C19 N21 H21 116(3) . . ? C22 N21 H21 116(3) . . ? C27 C22 C23 119.1(3) . . ? C27 C22 N21 116.9(3) . . ? C23 C22 N21 124.0(3) . . ? C24 C23 C22 119.5(4) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C25 121.0(3) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C26 C25 C24 119.3(3) . . ? C26 C25 C28 120.9(4) . . ? C24 C25 C28 119.8(3) . . ? C27 C26 C25 120.3(4) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C26 C27 C22 120.6(4) . . ? C26 C27 H27 119.7 . . ? C22 C27 H27 119.7 . . ? N29 C28 C25 178.5(4) . . ? C31 C30 N1 114.3(3) . . ? C31 C30 H30A 108.7 . . ? N1 C30 H30A 108.7 . . ? C31 C30 H30B 108.7 . . ? N1 C30 H30B 108.7 . . ? H30A C30 H30B 107.6 . . ? N32 C31 C30 110.1(3) . . ? N32 C31 H31A 109.6 . . ? C30 C31 H31A 109.6 . . ? N32 C31 H31B 109.6 . . ? C30 C31 H31B 109.6 . . ? H31A C31 H31B 108.2 . . ? C33 N32 C31 120.6(3) . . ? C33 N32 H32 120(3) . . ? C31 N32 H32 117(3) . . ? O34 C33 N32 123.5(4) . . ? O34 C33 N35 123.2(4) . . ? N32 C33 N35 113.3(3) . . ? C33 N35 C36 128.8(3) . . ? C33 N35 H35 114(2) . . ? C36 N35 H35 117(2) . . ? N35 C36 C37 124.7(3) . . ? N35 C36 C41 117.1(3) . . ? C37 C36 C41 118.2(4) . . ? C38 C37 C36 119.9(3) . . ? C38 C37 H37 120.1 . . ? C36 C37 H37 120.1 . . ? C37 C38 C39 122.1(4) . . ? C37 C38 H38 118.9 . . ? C39 C38 H38 118.9 . . ? C38 C39 C40 118.3(4) . . ? C38 C39 C42 121.9(4) . . ? C40 C39 C42 119.9(3) . . ? C41 C40 C39 119.8(3) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C40 C41 C36 121.8(4) . . ? C40 C41 H41 119.1 . . ? C36 C41 H41 119.1 . . ? N43 C42 C39 178.7(4) . . ? 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 C30 N1 C2 C3 -66.1(4) . . . . ? C16 N1 C2 C3 171.3(3) . . . . ? N1 C2 C3 N4 -70.3(4) . . . . ? C2 C3 N4 C5 104.4(4) . . . . ? C3 N4 C5 O6 -5.0(5) . . . . ? C3 N4 C5 N7 175.4(3) . . . . ? O6 C5 N7 C8 10.2(6) . . . . ? N4 C5 N7 C8 -170.2(3) . . . . ? C5 N7 C8 C13 -167.6(3) . . . . ? C5 N7 C8 C9 15.0(6) . . . . ? N7 C8 C9 C10 179.1(3) . . . . ? C13 C8 C9 C10 1.7(5) . . . . ? C8 C9 C10 C11 0.3(5) . . . . ? C9 C10 C11 C12 -2.0(5) . . . . ? C9 C10 C11 C14 177.2(3) . . . . ? C10 C11 C12 C13 1.7(5) . . . . ? C14 C11 C12 C13 -177.6(3) . . . . ? C11 C12 C13 C8 0.4(5) . . . . ? N7 C8 C13 C12 -179.7(3) . . . . ? C9 C8 C13 C12 -2.1(5) . . . . ? #C10 C11 C14 N15 -129(11) . . . . ? #C12 C11 C14 N15 51(11) . . . . ? C2 N1 C16 C17 -85.9(4) . . . . ? C30 N1 C16 C17 150.8(3) . . . . ? N1 C16 C17 N18 -74.6(4) . . . . ? C16 C17 N18 C19 80.0(4) . . . . ? C17 N18 C19 O20 -6.6(5) . . . . ? C17 N18 C19 N21 173.1(3) . . . . ? O20 C19 N21 C22 -11.2(6) . . . . ? N18 C19 N21 C22 169.1(3) . . . . ? C19 N21 C22 C27 179.7(3) . . . . ? C19 N21 C22 C23 -0.8(6) . . . . ? C27 C22 C23 C24 2.9(5) . . . . ? N21 C22 C23 C24 -176.6(3) . . . . ? C22 C23 C24 C25 -0.5(5) . . . . ? C23 C24 C25 C26 -1.9(6) . . . . ? C23 C24 C25 C28 177.4(3) . . . . ? C24 C25 C26 C27 1.7(6) . . . . ? C28 C25 C26 C27 -177.5(3) . . . . ? C25 C26 C27 C22 0.7(6) . . . . ? C23 C22 C27 C26 -3.1(5) . . . . ? N21 C22 C27 C26 176.5(3) . . . . ? #C26 C25 C28 N29 74(16) . . . . ? #C24 C25 C28 N29 -105(16) . . . . ? C2 N1 C30 C31 163.0(3) . . . . ? C16 N1 C30 C31 -74.2(4) . . . . ? N1 C30 C31 N32 -69.8(4) . . . . ? C30 C31 N32 C33 -168.3(3) . . . . ? C31 N32 C33 O34 -6.4(6) . . . . ? C31 N32 C33 N35 173.1(3) . . . . ? O34 C33 N35 C36 1.4(6) . . . . ? N32 C33 N35 C36 -178.1(3) . . . . ? C33 N35 C36 C37 -4.8(6) . . . . ? C33 N35 C36 C41 174.7(3) . . . . ? N35 C36 C37 C38 -179.9(4) . . . . ? C41 C36 C37 C38 0.6(5) . . . . ? C36 C37 C38 C39 -0.3(6) . . . . ? C37 C38 C39 C40 -0.1(6) . . . . ? C37 C38 C39 C42 179.3(4) . . . . ? C38 C39 C40 C41 0.1(5) . . . . ? C42 C39 C40 C41 -179.4(4) . . . . ? C39 C40 C41 C36 0.3(6) . . . . ? N35 C36 C41 C40 179.8(3) . . . . ? C37 C36 C41 C40 -0.7(6) . . . . ? #C38 C39 C42 N43 -165(100) . . . . ? #C40 C39 C42 N43 15(22) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O20 0.96(3) 1.86(4) 2.755(4) 153(3) . N1 H1 N32 0.96(3) 2.65(3) 3.056(4) 106(2) . N4 H4 Br1 0.94(4) 2.52(4) 3.405(3) 157(3) . N7 H7 Br1 0.81(4) 2.54(4) 3.335(3) 166(3) . N18 H18 Br1 0.81(4) 2.93(4) 3.645(3) 149(3) 3_666 N32 H32 O6 0.81(4) 2.11(4) 2.919(4) 178(4) . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.349 _refine_diff_density_min -0.412 _refine_diff_density_rms 0.101 #===END