 
data_sk22-1 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C31 H31 Br Cl2 N4 O5' 
_chemical_formula_weight          690.41 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0181   0.0091 
 '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'   0.0311   0.0180 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0492   0.0322 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.3639   0.7018 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Br'  'Br'  -0.6763   1.2805 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            'triclinic' 
_symmetry_space_group_name_H-M    'P -1' 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
 
_cell_length_a                    8.498 
_cell_length_b                    11.409 
_cell_length_c                    17.093 
_cell_angle_alpha                 89.37 
_cell_angle_beta                  78.23 
_cell_angle_gamma                 78.19 
_cell_volume                      1587.2 
_cell_formula_units_Z             2 
_cell_measurement_temperature     213(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.5 
_exptl_crystal_size_mid           0.3 
_exptl_crystal_size_min           0.2 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.445 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              708 
_exptl_absorpt_coefficient_mu     3.692 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       213(2) 
_diffrn_radiation_wavelength      1.54178 
_diffrn_radiation_type            CuK\a 
_diffrn_radiation_source          'rotating anode' 
_diffrn_radiation_monochromator   ? 
_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             22184 
_diffrn_reflns_av_R_equivalents   0.0591 
_diffrn_reflns_av_sigmaI/netI     0.0404 
_diffrn_reflns_limit_h_min        -8 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -13 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        -20 
_diffrn_reflns_limit_l_max        20 
_diffrn_reflns_theta_min          2.64 
_diffrn_reflns_theta_max          72.39 
_reflns_number_total              5560 
_reflns_number_gt                 5331 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        ? 
_computing_cell_refinement        ? 
_computing_data_reduction         ? 
_computing_structure_solution     'SHELXD-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.1646P)²+0.4327P] where P=(Fo²+2Fc²)/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        0.0020(5) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          5560 
_refine_ls_number_parameters      389 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0641 
_refine_ls_R_factor_gt            0.0575 
_refine_ls_wR_factor_ref          0.2139 
_refine_ls_wR_factor_gt           0.1952 
_refine_ls_goodness_of_fit_ref    1.011 
_refine_ls_restrained_S_all       1.011 
_refine_ls_shift/su_max           0.000 
_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 
Br1 Br 0.87277(5) 0.03666(3) 0.22909(2) 0.0679(2) Uani 1 1 d . . . 
N5 N 0.7834(3) 0.44670(19) 0.47104(12) 0.0422(5) Uani 1 1 d . . . 
H5 H 0.8457 0.4979 0.4603 0.051 Uiso 1 1 calc R . . 
O7 O 1.1362(3) 0.64416(18) 0.30186(12) 0.0534(5) Uani 1 1 d . . . 
O4 O 0.4562(2) 0.68390(17) 0.79502(10) 0.0497(5) Uani 1 1 d . . . 
O9 O 0.5769(3) 0.39637(19) 0.56357(13) 0.0627(6) Uani 1 1 d . . . 
C1 C 0.7678(4) 0.1614(3) 0.37418(19) 0.0521(7) Uani 1 1 d . . . 
H1 H 0.7225 0.0943 0.3867 0.063 Uiso 1 1 calc R . . 
N4 N 0.9719(3) 0.46187(18) 0.32594(12) 0.0404(5) Uani 1 1 d . . . 
O8 O 1.0648(3) 0.19969(18) 0.14560(11) 0.0543(5) Uani 1 1 d . . . 
N6 N 0.7381(3) 0.65756(19) 0.56270(12) 0.0404(5) Uani 1 1 d . . . 
C2 C 0.5437(3) 0.6705(2) 0.71887(14) 0.0422(6) Uani 1 1 d . . . 
C3 C 0.9062(3) 0.3617(2) 0.33807(15) 0.0395(6) Uani 1 1 d . . . 
C4 C 0.7193(3) 0.7539(2) 0.61306(14) 0.0385(6) Uani 1 1 d . . . 
O6 O 1.2034(4) 0.6007(2) 0.17134(14) 0.0838(9) Uani 1 1 d . . . 
C6 C 0.6705(4) 0.4637(2) 0.54007(15) 0.0450(6) Uani 1 1 d . . . 
C7 C 0.7894(4) 0.9468(2) 0.63537(17) 0.0493(7) Uani 1 1 d . . . 
H7 H 0.8449 1.0072 0.6170 0.059 Uiso 1 1 calc R . . 
C8 C 1.0975(4) 0.3881(3) 0.19213(16) 0.0468(6) Uani 1 1 d . . . 
H8 H 1.1625 0.4011 0.1434 0.056 Uiso 1 1 calc R . . 
C9 C 0.6236(3) 0.7653(2) 0.69186(14) 0.0404(6) Uani 1 1 d . . . 
C10 C 0.3841(4) 0.5858(3) 0.82779(16) 0.0482(7) Uani 1 1 d . . . 
H10A H 0.4689 0.5145 0.8277 0.058 Uiso 1 1 calc R . . 
H10B H 0.3085 0.5685 0.7961 0.058 Uiso 1 1 calc R . . 
C11 C 1.0620(3) 0.4726(2) 0.25544(15) 0.0427(6) Uani 1 1 d . . . 
C12 C 1.0353(4) 0.2857(2) 0.20290(16) 0.0448(6) Uani 1 1 d . . . 
C13 C 0.8005(3) 0.8491(2) 0.58599(15) 0.0420(6) Uani 1 1 d . . . 
C14 C 1.1384(4) 0.5805(2) 0.23808(17) 0.0508(7) Uani 1 1 d . . . 
C15 C 0.8955(4) 0.8453(2) 0.50620(16) 0.0467(6) Uani 1 1 d . . . 
C16 C 0.7416(4) 0.2518(3) 0.43233(17) 0.0500(7) Uani 1 1 d . . . 
H16 H 0.6794 0.2443 0.4829 0.060 Uiso 1 1 calc R . . 
C17 C 1.1640(5) 0.2164(3) 0.06947(17) 0.0623(8) Uani 1 1 d . . . 
H17A H 1.2735 0.2215 0.0755 0.075 Uiso 1 1 calc R . . 
H17B H 1.1159 0.2901 0.0468 0.075 Uiso 1 1 calc R . . 
C18 C 0.6948(4) 0.9546(3) 0.71276(17) 0.0518(7) Uani 1 1 d . . . 
H18 H 0.6884 1.0203 0.7459 0.062 Uiso 1 1 calc R . . 
C20 C 0.6598(3) 0.5729(2) 0.59177(14) 0.0410(6) Uani 1 1 d . . . 
C21 C 0.5607(3) 0.5749(2) 0.66910(15) 0.0439(6) Uani 1 1 d . . . 
H21 H 0.5083 0.5122 0.6855 0.053 Uiso 1 1 calc R . . 
C22 C 0.6115(4) 0.8672(2) 0.74066(16) 0.0477(6) Uani 1 1 d . . . 
H22 H 0.5466 0.8747 0.7919 0.057 Uiso 1 1 calc R . . 
C23 C 0.8074(3) 0.3521(2) 0.41534(15) 0.0413(6) Uani 1 1 d . . . 
C24 C 1.2207(5) 0.7437(3) 0.2878(2) 0.0679(10) Uani 1 1 d . . . 
H24A H 1.2125 0.7847 0.3377 0.102 Uiso 1 1 calc R . . 
H24B H 1.1710 0.7983 0.2524 0.102 Uiso 1 1 calc R . . 
H24C H 1.3343 0.7138 0.2641 0.102 Uiso 1 1 calc R . . 
C25 C 0.8580(4) 0.1690(2) 0.29948(17) 0.0475(6) Uani 1 1 d . . . 
C26 C 0.2936(4) 0.6226(3) 0.91251(17) 0.0542(7) Uani 1 1 d . . . 
H26 H 0.2049 0.6918 0.9105 0.065 Uiso 1 1 calc R . . 
C27 C 0.9333(3) 0.2688(2) 0.27792(15) 0.0419(6) Uani 1 1 d . . . 
C28 C 0.4045(5) 0.6578(4) 0.9622(2) 0.0735(10) Uani 1 1 d . . . 
H28A H 0.3429 0.6810 1.0153 0.110 Uiso 1 1 calc R . . 
H28B H 0.4488 0.7238 0.9384 0.110 Uiso 1 1 calc R . . 
H28C H 0.4927 0.5910 0.9646 0.110 Uiso 1 1 calc R . . 
C29 C 0.2169(5) 0.5187(4) 0.9482(2) 0.0720(10) Uani 1 1 d . . . 
H29A H 0.1585 0.5400 1.0020 0.108 Uiso 1 1 calc R . . 
H29B H 0.3019 0.4488 0.9482 0.108 Uiso 1 1 calc R . . 
H29C H 0.1421 0.5020 0.9166 0.108 Uiso 1 1 calc R . . 
C31 C 1.1728(6) 0.1112(4) 0.0153(2) 0.0870(13) Uani 1 1 d . . . 
H31 H 1.0604 0.1060 0.0124 0.104 Uiso 1 1 calc R . . 
C32 C 1.2523(8) -0.0035(5) 0.0466(4) 0.125(2) Uani 1 1 d . . . 
H32A H 1.2541 -0.0687 0.0113 0.188 Uiso 1 1 calc R . . 
H32B H 1.1913 -0.0154 0.0988 0.188 Uiso 1 1 calc R . . 
H32C H 1.3627 -0.0001 0.0499 0.188 Uiso 1 1 calc R . . 
C33 C 1.2614(10) 0.1372(6) -0.0673(3) 0.146(3) Uani 1 1 d . . . 
H33A H 1.2688 0.0716 -0.1035 0.219 Uiso 1 1 calc R . . 
H33B H 1.3699 0.1471 -0.0650 0.219 Uiso 1 1 calc R . . 
H33C H 1.2016 0.2093 -0.0856 0.219 Uiso 1 1 calc R . . 
N3 N 0.9701(4) 0.8501(3) 0.44319(16) 0.0673(8) Uani 1 1 d . . . 
Cl2 Cl 0.56404(12) 0.87009(9) 0.40581(7) 0.0795(3) Uani 1 1 d . . . 
Cl1 Cl 0.69748(17) 0.72112(13) 0.26000(7) 0.0972(4) Uani 1 1 d . . . 
C30 C 0.7004(4) 0.7395(3) 0.3613(2) 0.0632(8) Uani 1 1 d . . . 
H30A H 0.8109 0.7430 0.3664 0.076 Uiso 1 1 calc R . . 
H30B H 0.6712 0.6704 0.3897 0.076 Uiso 1 1 calc R . . 
 
 
_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 C25 1.909(3) . ? 
N5 C6 1.348(3) . ? 
N5 C23 1.402(3) . ? 
O7 C14 1.311(4) . ? 
O7 C24 1.457(3) . ? 
O4 C2 1.354(3) . ? 
O4 C10 1.439(3) . ? 
O9 C6 1.224(3) . ? 
C1 C25 1.361(4) . ? 
C1 C16 1.392(4) . ? 
N4 C11 1.309(3) . ? 
N4 C3 1.368(3) . ? 
O8 C12 1.344(3) . ? 
O8 C17 1.433(3) . ? 
N6 C20 1.320(3) . ? 
N6 C4 1.367(3) . ? 
C2 C21 1.356(4) . ? 
C2 C9 1.416(3) . ? 
C3 C23 1.429(3) . ? 
C3 C27 1.435(4) . ? 
C4 C9 1.416(3) . ? 
C4 C13 1.427(3) . ? 
O6 C14 1.204(3) . ? 
C6 C20 1.512(4) . ? 
C7 C13 1.381(4) . ? 
C7 C18 1.394(4) . ? 
C8 C12 1.373(4) . ? 
C8 C11 1.401(4) . ? 
C9 C22 1.412(4) . ? 
C10 C26 1.514(4) . ? 
C11 C14 1.506(4) . ? 
C12 C27 1.429(4) . ? 
C13 C15 1.432(3) . ? 
C15 N3 1.140(4) . ? 
C16 C23 1.377(4) . ? 
C17 C31 1.504(5) . ? 
C18 C22 1.366(4) . ? 
C20 C21 1.413(3) . ? 
C25 C27 1.426(4) . ? 
C26 C28 1.503(5) . ? 
C26 C29 1.530(4) . ? 
C31 C32 1.491(7) . ? 
C31 C33 1.516(6) . ? 
Cl2 C30 1.761(4) . ? 
Cl1 C30 1.752(4) . ? 
 
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 
C6 N5 C23 125.2(2) . . ? 
C14 O7 C24 115.5(2) . . ? 
C2 O4 C10 117.6(2) . . ? 
C25 C1 C16 121.6(3) . . ? 
C11 N4 C3 117.5(2) . . ? 
C12 O8 C17 118.4(2) . . ? 
C20 N6 C4 115.7(2) . . ? 
O4 C2 C21 125.3(2) . . ? 
O4 C2 C9 115.3(2) . . ? 
C21 C2 C9 119.5(2) . . ? 
N4 C3 C23 116.5(2) . . ? 
N4 C3 C27 123.2(2) . . ? 
C23 C3 C27 120.3(2) . . ? 
N6 C4 C9 123.8(2) . . ? 
N6 C4 C13 119.0(2) . . ? 
C9 C4 C13 117.2(2) . . ? 
O9 C6 N5 124.3(3) . . ? 
O9 C6 C20 118.1(2) . . ? 
N5 C6 C20 117.7(2) . . ? 
C13 C7 C18 119.9(2) . . ? 
C12 C8 C11 119.2(2) . . ? 
C22 C9 C4 120.5(2) . . ? 
C22 C9 C2 122.3(2) . . ? 
C4 C9 C2 117.2(2) . . ? 
O4 C10 C26 107.4(2) . . ? 
N4 C11 C8 124.6(2) . . ? 
N4 C11 C14 120.2(2) . . ? 
C8 C11 C14 115.1(2) . . ? 
O8 C12 C8 123.0(2) . . ? 
O8 C12 C27 117.7(2) . . ? 
C8 C12 C27 119.3(2) . . ? 
C7 C13 C4 121.3(2) . . ? 
C7 C13 C15 118.5(2) . . ? 
C4 C13 C15 120.3(2) . . ? 
O6 C14 O7 124.1(3) . . ? 
O6 C14 C11 121.6(3) . . ? 
O7 C14 C11 114.2(2) . . ? 
N3 C15 C13 175.5(3) . . ? 
C23 C16 C1 120.4(3) . . ? 
O8 C17 C31 108.1(3) . . ? 
C22 C18 C7 120.9(3) . . ? 
N6 C20 C21 125.4(2) . . ? 
N6 C20 C6 119.7(2) . . ? 
C21 C20 C6 115.0(2) . . ? 
C2 C21 C20 118.5(2) . . ? 
C18 C22 C9 120.2(2) . . ? 
C16 C23 N5 122.9(2) . . ? 
C16 C23 C3 119.5(2) . . ? 
N5 C23 C3 117.6(2) . . ? 
C1 C25 C27 121.3(3) . . ? 
C1 C25 Br1 114.2(2) . . ? 
C27 C25 Br1 124.4(2) . . ? 
C28 C26 C10 111.9(3) . . ? 
C28 C26 C29 112.0(3) . . ? 
C10 C26 C29 107.9(3) . . ? 
C25 C27 C12 126.9(2) . . ? 
C25 C27 C3 116.9(2) . . ? 
C12 C27 C3 116.2(2) . . ? 
C32 C31 C33 113.0(5) . . ? 
C32 C31 C17 111.6(4) . . ? 
C33 C31 C17 107.3(4) . . ? 
Cl1 C30 Cl2 112.57(19) . . ? 
 
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 O4 C2 C21 4.3(4) . . . . ? 
C10 O4 C2 C9 -174.9(2) . . . . ? 
C11 N4 C3 C23 -179.7(2) . . . . ? 
C11 N4 C3 C27 0.8(4) . . . . ? 
C20 N6 C4 C9 0.2(4) . . . . ? 
C20 N6 C4 C13 179.9(2) . . . . ? 
C23 N5 C6 O9 1.8(5) . . . . ? 
C23 N5 C6 C20 -178.5(2) . . . . ? 
N6 C4 C9 C22 179.3(2) . . . . ? 
C13 C4 C9 C22 -0.3(4) . . . . ? 
N6 C4 C9 C2 0.0(4) . . . . ? 
C13 C4 C9 C2 -179.7(2) . . . . ? 
O4 C2 C9 C22 -0.6(4) . . . . ? 
C21 C2 C9 C22 -179.8(3) . . . . ? 
O4 C2 C9 C4 178.7(2) . . . . ? 
C21 C2 C9 C4 -0.5(4) . . . . ? 
C2 O4 C10 C26 -179.9(2) . . . . ? 
C3 N4 C11 C8 -0.9(4) . . . . ? 
C3 N4 C11 C14 -179.9(2) . . . . ? 
C12 C8 C11 N4 0.0(4) . . . . ? 
C12 C8 C11 C14 179.0(3) . . . . ? 
C17 O8 C12 C8 -0.8(4) . . . . ? 
C17 O8 C12 C27 178.8(3) . . . . ? 
C11 C8 C12 O8 -179.3(3) . . . . ? 
C11 C8 C12 C27 1.1(4) . . . . ? 
C18 C7 C13 C4 -1.2(4) . . . . ? 
C18 C7 C13 C15 178.5(3) . . . . ? 
N6 C4 C13 C7 -178.1(3) . . . . ? 
C9 C4 C13 C7 1.6(4) . . . . ? 
N6 C4 C13 C15 2.2(4) . . . . ? 
C9 C4 C13 C15 -178.2(3) . . . . ? 
C24 O7 C14 O6 -0.6(5) . . . . ? 
C24 O7 C14 C11 175.3(3) . . . . ? 
N4 C11 C14 O6 -170.1(3) . . . . ? 
C8 C11 C14 O6 10.9(5) . . . . ? 
N4 C11 C14 O7 13.9(4) . . . . ? 
C8 C11 C14 O7 -165.1(3) . . . . ? 
C7 C13 C15 N3 -20(4) . . . . ? 
C4 C13 C15 N3 160(4) . . . . ? 
C25 C1 C16 C23 -0.1(5) . . . . ? 
C12 O8 C17 C31 -177.7(3) . . . . ? 
C13 C7 C18 C22 -0.5(5) . . . . ? 
C4 N6 C20 C21 0.0(4) . . . . ? 
C4 N6 C20 C6 178.9(2) . . . . ? 
O9 C6 C20 N6 -168.6(3) . . . . ? 
N5 C6 C20 N6 11.7(4) . . . . ? 
O9 C6 C20 C21 10.4(4) . . . . ? 
N5 C6 C20 C21 -169.4(2) . . . . ? 
O4 C2 C21 C20 -178.4(2) . . . . ? 
C9 C2 C21 C20 0.7(4) . . . . ? 
N6 C20 C21 C2 -0.5(4) . . . . ? 
C6 C20 C21 C2 -179.4(2) . . . . ? 
C7 C18 C22 C9 1.7(5) . . . . ? 
C4 C9 C22 C18 -1.3(4) . . . . ? 
C2 C9 C22 C18 178.0(3) . . . . ? 
C1 C16 C23 N5 179.1(3) . . . . ? 
C1 C16 C23 C3 -1.5(4) . . . . ? 
C6 N5 C23 C16 -14.0(4) . . . . ? 
C6 N5 C23 C3 166.5(2) . . . . ? 
N4 C3 C23 C16 -178.0(3) . . . . ? 
C27 C3 C23 C16 1.5(4) . . . . ? 
N4 C3 C23 N5 1.4(4) . . . . ? 
C27 C3 C23 N5 -179.0(2) . . . . ? 
C16 C1 C25 C27 1.5(5) . . . . ? 
C16 C1 C25 Br1 -178.5(3) . . . . ? 
O4 C10 C26 C28 -56.2(3) . . . . ? 
O4 C10 C26 C29 -179.8(3) . . . . ? 
C1 C25 C27 C12 177.7(3) . . . . ? 
Br1 C25 C27 C12 -2.3(4) . . . . ? 
C1 C25 C27 C3 -1.4(4) . . . . ? 
Br1 C25 C27 C3 178.63(19) . . . . ? 
O8 C12 C27 C25 0.1(4) . . . . ? 
C8 C12 C27 C25 179.7(3) . . . . ? 
O8 C12 C27 C3 179.2(2) . . . . ? 
C8 C12 C27 C3 -1.2(4) . . . . ? 
N4 C3 C27 C25 179.4(2) . . . . ? 
C23 C3 C27 C25 -0.1(4) . . . . ? 
N4 C3 C27 C12 0.2(4) . . . . ? 
C23 C3 C27 C12 -179.3(2) . . . . ? 
O8 C17 C31 C32 -62.0(5) . . . . ? 
O8 C17 C31 C33 173.6(5) . . . . ? 
 
_diffrn_measured_fraction_theta_max    0.885 
_diffrn_reflns_theta_full              72.39 
_diffrn_measured_fraction_theta_full   0.885 
_refine_diff_density_max    0.552 
_refine_diff_density_min   -0.572 
_refine_diff_density_rms    0.137 
