Supplementary Material (ESI) for Perkin Transactions This journal is © The Royal Society of Chemistry data_fro1044 _database_code_CSD 160321 _journal_coden_Cambridge 188 _publ_requested_journal 'Perkin Transactions 2' loop_ _publ_author_name 'Frohlich, Roland' 'Singh, N. B.' 'Srivastava, Archana' _publ_contact_author_name 'Prof N B Singh' _publ_contact_author_address ; Prof N B Singh Department of Chemistry D D Gorakhpur University Gorakhpur 273009 INDIA ; _publ_contact_author_email 'DR_N_B_SINGH@REDIFFMAIL.COM' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H20 Cl6 N2 O4' _chemical_formula_weight 685.18 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' 'Cl' 'Cl' 0.1484 0.1585 '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/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 11.023(1) _cell_length_b 16.872(1) _cell_length_c 16.682(1) _cell_angle_alpha 90.00 _cell_angle_beta 107.57(1) _cell_angle_gamma 90.00 _cell_volume 2957.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.621 _exptl_absorpt_correction_type 'SORTAV (Blessing, 1995 & 1997)' _exptl_absorpt_correction_T_min 0.8355 _exptl_absorpt_correction_T_max 0.9405 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9690 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 24.71 _reflns_number_total 5016 _reflns_number_gt 3570 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo_SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+1.3563P] 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 'refined as riding atoms' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5016 _refine_ls_number_parameters 391 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0688 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1039 _refine_ls_wR_factor_gt 0.0910 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O11 O 0.8585(2) 0.02983(13) 0.52090(13) 0.0593(6) Uani 1 d . . . H11 H 0.825(4) 0.047(2) 0.478(2) 0.089 Uiso 1 d . . . C11 C 0.7798(3) -0.02444(16) 0.54075(18) 0.0478(7) Uani 1 d . . . C12 C 0.8150(3) -0.06032(18) 0.6163(2) 0.0605(8) Uani 1 d . . . H12 H 0.8926 -0.0480 0.6555 0.073 Uiso 1 calc R . . C13 C 0.7335(4) -0.1168(2) 0.6358(2) 0.0716(10) Uani 1 d . . . H13 H 0.7582 -0.1419 0.6879 0.086 Uiso 1 calc R . . C14 C 0.6196(3) -0.13490(19) 0.5794(2) 0.0696(9) Uani 1 d . . . H14 H 0.5667 -0.1719 0.5932 0.084 Uiso 1 calc R . . C15 C 0.5811(3) -0.09810(16) 0.5004(2) 0.0520(7) Uani 1 d . . . C16 C 0.4645(3) -0.11219(18) 0.4377(2) 0.0653(9) Uani 1 d . . . H16 H 0.4063 -0.1479 0.4476 0.078 Uiso 1 calc R . . C17 C 0.4377(3) -0.0740(2) 0.3637(2) 0.0706(10) Uani 1 d . . . H17 H 0.3609 -0.0831 0.3222 0.085 Uiso 1 calc R . . C18 C 0.5253(3) -0.02087(19) 0.3496(2) 0.0645(9) Uani 1 d . . . H18 H 0.5053 0.0042 0.2976 0.077 Uiso 1 calc R . . N11 N 0.6349(2) -0.00395(14) 0.40544(16) 0.0527(6) Uani 1 d . . . C19 C 0.6625(3) -0.04229(15) 0.48045(18) 0.0445(7) Uani 1 d . . . O21 O 0.89229(18) -0.01116(10) 0.28006(12) 0.0507(5) Uani 1 d . . . C21 C 0.8072(3) -0.06862(15) 0.26395(17) 0.0452(7) Uani 1 d . . . C22 C 0.7113(3) -0.08011(17) 0.18941(19) 0.0595(8) Uani 1 d . . . H22 H 0.7064 -0.0467 0.1442 0.071 Uiso 1 calc R . . C23 C 0.6216(3) -0.1405(2) 0.1800(2) 0.0693(9) Uani 1 d . . . H23 H 0.5575 -0.1451 0.1291 0.083 Uiso 1 calc R . . C24 C 0.6244(3) -0.19249(19) 0.2421(2) 0.0635(9) Uani 1 d . . . H24 H 0.5633 -0.2321 0.2338 0.076 Uiso 1 calc R . . C25 C 0.7208(3) -0.18607(15) 0.31951(19) 0.0488(7) Uani 1 d . . . C26 C 0.7349(3) -0.23652(17) 0.3885(2) 0.0586(8) Uani 1 d . . . H26 H 0.6784 -0.2784 0.3841 0.070 Uiso 1 calc R . . C27 C 0.8297(3) -0.22543(17) 0.4616(2) 0.0584(8) Uani 1 d . . . H27 H 0.8364 -0.2587 0.5072 0.070 Uiso 1 calc R . . C28 C 0.9159(3) -0.16478(16) 0.46814(18) 0.0511(7) Uani 1 d . . . H28 H 0.9811 -0.1570 0.5180 0.061 Uiso 1 calc R . . N21 N 0.9051(2) -0.11778(13) 0.40294(15) 0.0432(6) Uani 1 d . . . H21 H 0.960(3) -0.0831(16) 0.4081(17) 0.052 Uiso 1 d . . . C29 C 0.8107(2) -0.12443(15) 0.32856(17) 0.0415(6) Uani 1 d . . . O31 O 0.84022(18) 0.11083(11) 0.35959(12) 0.0494(5) Uani 1 d . . . H31 H 0.851(3) 0.0708(19) 0.336(2) 0.074 Uiso 1 d . . . C31 C 0.7303(2) 0.14610(15) 0.31474(16) 0.0402(6) Uani 1 d . . . C32 C 0.6823(3) 0.20793(15) 0.35094(16) 0.0414(6) Uani 1 d . . . Cl32 Cl 0.76171(8) 0.23678(5) 0.45243(4) 0.0621(2) Uani 1 d . . . C33 C 0.5720(3) 0.24632(16) 0.30722(17) 0.0489(7) Uani 1 d . . . H33 H 0.5420 0.2882 0.3321 0.059 Uiso 1 calc R . . C34 C 0.5061(3) 0.22302(17) 0.22690(17) 0.0468(7) Uani 1 d . . . Cl34 Cl 0.36821(9) 0.27243(6) 0.17330(5) 0.0840(3) Uani 1 d . . . C35 C 0.5516(3) 0.16066(15) 0.19079(16) 0.0434(6) Uani 1 d . . . Cl35 Cl 0.47195(8) 0.12829(5) 0.09022(5) 0.0672(2) Uani 1 d . . . C36 C 0.6633(3) 0.12343(15) 0.23373(16) 0.0441(7) Uani 1 d . . . H36 H 0.6942 0.0825 0.2080 0.053 Uiso 1 calc R . . O41 O 0.9612(2) 0.07442(12) 0.17409(13) 0.0583(6) Uani 1 d . . . H41 H 0.941(3) 0.041(2) 0.208(2) 0.087 Uiso 1 d . . . C41 C 1.0444(3) 0.04140(16) 0.13948(17) 0.0444(7) Uani 1 d . . . C42 C 1.0821(3) 0.08414(15) 0.07964(18) 0.0462(7) Uani 1 d . . . Cl42 Cl 1.02269(8) 0.17839(4) 0.05322(6) 0.0732(3) Uani 1 d . . . C43 C 1.1642(3) 0.05281(15) 0.04064(17) 0.0475(7) Uani 1 d . . . H43 H 1.1871 0.0822 0.0004 0.057 Uiso 1 calc R . . C44 C 1.2127(3) -0.02235(16) 0.06107(17) 0.0470(7) Uani 1 d . . . Cl44 Cl 1.31569(8) -0.05992(5) 0.00998(5) 0.0639(2) Uani 1 d . . . C45 C 1.1785(3) -0.06517(15) 0.12082(17) 0.0467(7) Uani 1 d . . . Cl45 Cl 1.23883(9) -0.15944(4) 0.14834(5) 0.0704(3) Uani 1 d . . . C46 C 1.0950(3) -0.03393(16) 0.15973(17) 0.0489(7) Uani 1 d . . . H46 H 1.0725 -0.0637 0.2000 0.059 Uiso 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 O11 0.0484(13) 0.0636(13) 0.0616(14) 0.0105(11) 0.0102(11) -0.0118(10) C11 0.0431(17) 0.0444(16) 0.0582(19) 0.0044(14) 0.0187(15) 0.0024(13) C12 0.0489(18) 0.068(2) 0.063(2) 0.0068(17) 0.0143(16) 0.0043(16) C13 0.078(3) 0.071(2) 0.074(2) 0.0222(18) 0.034(2) 0.0105(19) C14 0.066(2) 0.057(2) 0.097(3) 0.0147(19) 0.041(2) -0.0024(17) C15 0.0472(18) 0.0385(15) 0.077(2) -0.0021(15) 0.0289(16) 0.0014(13) C16 0.050(2) 0.0492(19) 0.102(3) -0.0202(19) 0.031(2) -0.0137(15) C17 0.051(2) 0.072(2) 0.083(3) -0.023(2) 0.0122(19) -0.0051(18) C18 0.058(2) 0.071(2) 0.064(2) -0.0056(17) 0.0155(18) 0.0043(17) N11 0.0453(15) 0.0535(14) 0.0586(16) -0.0027(12) 0.0146(13) 0.0012(11) C19 0.0392(16) 0.0391(15) 0.0581(18) -0.0043(13) 0.0191(14) 0.0059(12) O21 0.0554(12) 0.0444(11) 0.0578(12) 0.0067(9) 0.0251(10) 0.0014(9) C21 0.0481(17) 0.0401(15) 0.0509(18) 0.0026(13) 0.0203(14) 0.0108(13) C22 0.072(2) 0.0517(18) 0.0501(18) 0.0002(15) 0.0118(17) 0.0181(17) C23 0.062(2) 0.063(2) 0.070(2) -0.0184(18) 0.0002(18) 0.0108(18) C24 0.0478(19) 0.0549(19) 0.084(3) -0.0178(18) 0.0145(18) -0.0024(15) C25 0.0412(16) 0.0406(16) 0.069(2) -0.0077(14) 0.0237(16) 0.0026(13) C26 0.059(2) 0.0412(16) 0.089(3) 0.0007(16) 0.041(2) -0.0028(14) C27 0.068(2) 0.0455(17) 0.069(2) 0.0116(15) 0.0330(19) 0.0052(16) C28 0.0527(18) 0.0487(17) 0.0530(18) 0.0096(14) 0.0178(15) 0.0099(14) N21 0.0383(14) 0.0383(13) 0.0554(15) 0.0046(11) 0.0179(12) 0.0010(10) C29 0.0372(15) 0.0399(15) 0.0505(17) -0.0028(12) 0.0180(14) 0.0054(12) O31 0.0466(12) 0.0489(12) 0.0483(12) -0.0014(9) 0.0078(9) 0.0063(10) C31 0.0361(15) 0.0408(15) 0.0425(16) 0.0054(12) 0.0098(13) -0.0006(12) C32 0.0437(16) 0.0449(15) 0.0357(15) -0.0001(12) 0.0119(13) -0.0018(12) Cl32 0.0642(5) 0.0746(5) 0.0429(4) -0.0112(4) 0.0095(4) 0.0078(4) C33 0.0496(18) 0.0535(17) 0.0468(18) -0.0002(13) 0.0193(15) 0.0088(14) C34 0.0398(16) 0.0562(17) 0.0434(17) 0.0077(13) 0.0109(13) 0.0081(13) Cl34 0.0652(6) 0.1203(8) 0.0594(5) 0.0039(5) 0.0078(4) 0.0435(5) C35 0.0424(16) 0.0466(16) 0.0400(15) 0.0012(12) 0.0109(13) -0.0060(13) Cl35 0.0578(5) 0.0808(6) 0.0528(5) -0.0127(4) 0.0012(4) -0.0027(4) C36 0.0462(17) 0.0384(14) 0.0466(17) -0.0015(12) 0.0122(14) 0.0008(12) O41 0.0633(14) 0.0536(12) 0.0686(14) 0.0117(10) 0.0360(12) 0.0087(10) C41 0.0417(16) 0.0460(16) 0.0484(16) -0.0004(13) 0.0177(13) -0.0012(13) C42 0.0430(16) 0.0379(15) 0.0583(18) 0.0065(13) 0.0161(14) 0.0003(12) Cl42 0.0787(6) 0.0479(4) 0.1098(7) 0.0233(4) 0.0539(5) 0.0155(4) C43 0.0474(17) 0.0451(16) 0.0549(18) 0.0066(13) 0.0228(14) -0.0017(13) C44 0.0480(17) 0.0460(16) 0.0491(17) -0.0022(13) 0.0178(14) 0.0014(13) Cl44 0.0719(5) 0.0607(5) 0.0694(5) 0.0019(4) 0.0369(4) 0.0118(4) C45 0.0540(18) 0.0372(15) 0.0490(17) -0.0011(13) 0.0155(14) 0.0010(13) Cl45 0.0930(7) 0.0487(4) 0.0764(6) 0.0137(4) 0.0361(5) 0.0191(4) C46 0.0564(18) 0.0453(16) 0.0476(16) 0.0076(13) 0.0196(14) -0.0024(14) _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 O11 C11 1.369(3) . ? C11 C12 1.345(4) . ? C11 C19 1.411(4) . ? C12 C13 1.413(4) . ? C13 C14 1.357(5) . ? C14 C15 1.401(4) . ? C15 C19 1.408(4) . ? C15 C16 1.410(4) . ? C16 C17 1.343(5) . ? C17 C18 1.389(5) . ? C18 N11 1.315(4) . ? N11 C19 1.359(4) . ? O21 C21 1.319(3) . ? C21 C22 1.381(4) . ? C21 C29 1.423(4) . ? C22 C23 1.395(4) . ? C23 C24 1.351(5) . ? C24 C25 1.407(4) . ? C25 C26 1.402(4) . ? C25 C29 1.413(4) . ? C26 C27 1.358(4) . ? C27 C28 1.378(4) . ? C28 N21 1.322(3) . ? N21 C29 1.362(3) . ? O31 C31 1.355(3) . ? C31 C36 1.384(4) . ? C31 C32 1.388(4) . ? C32 C33 1.376(4) . ? C32 Cl32 1.725(3) . ? C33 C34 1.375(4) . ? C34 C35 1.380(4) . ? C34 Cl34 1.728(3) . ? C35 C36 1.375(4) . ? C35 Cl35 1.730(3) . ? O41 C41 1.343(3) . ? C41 C46 1.388(4) . ? C41 C42 1.393(4) . ? C42 C43 1.370(4) . ? C42 Cl42 1.725(3) . ? C43 C44 1.379(4) . ? C44 C45 1.373(4) . ? C44 Cl44 1.732(3) . ? C45 C46 1.380(4) . ? C45 Cl45 1.732(3) . ? 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 C12 C11 O11 120.2(3) . . ? C12 C11 C19 121.0(3) . . ? O11 C11 C19 118.8(2) . . ? C11 C12 C13 119.7(3) . . ? C14 C13 C12 120.7(3) . . ? C13 C14 C15 120.4(3) . . ? C14 C15 C19 119.0(3) . . ? C14 C15 C16 124.8(3) . . ? C19 C15 C16 116.2(3) . . ? C17 C16 C15 119.9(3) . . ? C16 C17 C18 119.6(3) . . ? N11 C18 C17 123.9(3) . . ? C18 N11 C19 116.8(3) . . ? N11 C19 C15 123.7(3) . . ? N11 C19 C11 117.2(2) . . ? C15 C19 C11 119.1(3) . . ? O21 C21 C22 126.2(3) . . ? O21 C21 C29 118.5(2) . . ? C22 C21 C29 115.3(3) . . ? C21 C22 C23 121.8(3) . . ? C24 C23 C22 122.5(3) . . ? C23 C24 C25 119.3(3) . . ? C26 C25 C24 124.9(3) . . ? C26 C25 C29 117.3(3) . . ? C24 C25 C29 117.8(3) . . ? C27 C26 C25 121.2(3) . . ? C26 C27 C28 119.9(3) . . ? N21 C28 C27 119.5(3) . . ? C28 N21 C29 123.6(2) . . ? N21 C29 C25 118.4(2) . . ? N21 C29 C21 118.3(2) . . ? C25 C29 C21 123.3(3) . . ? O31 C31 C36 122.8(2) . . ? O31 C31 C32 119.0(2) . . ? C36 C31 C32 118.1(2) . . ? C33 C32 C31 121.0(2) . . ? C33 C32 Cl32 119.5(2) . . ? C31 C32 Cl32 119.5(2) . . ? C34 C33 C32 120.3(3) . . ? C33 C34 C35 119.2(2) . . ? C33 C34 Cl34 119.3(2) . . ? C35 C34 Cl34 121.4(2) . . ? C36 C35 C34 120.5(2) . . ? C36 C35 Cl35 118.3(2) . . ? C34 C35 Cl35 121.3(2) . . ? C35 C36 C31 120.8(2) . . ? O41 C41 C46 123.5(2) . . ? O41 C41 C42 118.9(2) . . ? C46 C41 C42 117.6(2) . . ? C43 C42 C41 121.6(2) . . ? C43 C42 Cl42 119.2(2) . . ? C41 C42 Cl42 119.2(2) . . ? C42 C43 C44 120.0(3) . . ? C45 C44 C43 119.5(2) . . ? C45 C44 Cl44 122.0(2) . . ? C43 C44 Cl44 118.6(2) . . ? C44 C45 C46 120.6(2) . . ? C44 C45 Cl45 120.5(2) . . ? C46 C45 Cl45 118.9(2) . . ? C45 C46 C41 120.7(3) . . ? 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 O11 C11 C12 C13 -179.4(3) . . . . ? C19 C11 C12 C13 0.0(4) . . . . ? C11 C12 C13 C14 -0.5(5) . . . . ? C12 C13 C14 C15 0.4(5) . . . . ? C13 C14 C15 C19 0.1(5) . . . . ? C13 C14 C15 C16 -179.5(3) . . . . ? C14 C15 C16 C17 -179.4(3) . . . . ? C19 C15 C16 C17 1.0(4) . . . . ? C15 C16 C17 C18 0.0(5) . . . . ? C16 C17 C18 N11 -1.0(5) . . . . ? C17 C18 N11 C19 0.9(4) . . . . ? C18 N11 C19 C15 0.2(4) . . . . ? C18 N11 C19 C11 -179.9(2) . . . . ? C14 C15 C19 N11 179.3(3) . . . . ? C16 C15 C19 N11 -1.1(4) . . . . ? C14 C15 C19 C11 -0.6(4) . . . . ? C16 C15 C19 C11 179.0(2) . . . . ? C12 C11 C19 N11 -179.4(3) . . . . ? O11 C11 C19 N11 0.1(4) . . . . ? C12 C11 C19 C15 0.5(4) . . . . ? O11 C11 C19 C15 180.0(2) . . . . ? O21 C21 C22 C23 -176.6(3) . . . . ? C29 C21 C22 C23 2.5(4) . . . . ? C21 C22 C23 C24 -1.6(5) . . . . ? C22 C23 C24 C25 0.1(5) . . . . ? C23 C24 C25 C26 -179.4(3) . . . . ? C23 C24 C25 C29 0.3(4) . . . . ? C24 C25 C26 C27 -178.9(3) . . . . ? C29 C25 C26 C27 1.4(4) . . . . ? C25 C26 C27 C28 -1.6(4) . . . . ? C26 C27 C28 N21 0.2(4) . . . . ? C27 C28 N21 C29 1.5(4) . . . . ? C28 N21 C29 C25 -1.6(4) . . . . ? C28 N21 C29 C21 178.1(2) . . . . ? C26 C25 C29 N21 0.2(4) . . . . ? C24 C25 C29 N21 -179.5(2) . . . . ? C26 C25 C29 C21 -179.5(2) . . . . ? C24 C25 C29 C21 0.8(4) . . . . ? O21 C21 C29 N21 -2.7(4) . . . . ? C22 C21 C29 N21 178.2(2) . . . . ? O21 C21 C29 C25 177.0(2) . . . . ? C22 C21 C29 C25 -2.1(4) . . . . ? O31 C31 C32 C33 178.9(2) . . . . ? C36 C31 C32 C33 -0.8(4) . . . . ? O31 C31 C32 Cl32 -1.3(3) . . . . ? C36 C31 C32 Cl32 178.9(2) . . . . ? C31 C32 C33 C34 1.1(4) . . . . ? Cl32 C32 C33 C34 -178.7(2) . . . . ? C32 C33 C34 C35 0.1(4) . . . . ? C32 C33 C34 Cl34 -179.8(2) . . . . ? C33 C34 C35 C36 -1.6(4) . . . . ? Cl34 C34 C35 C36 178.3(2) . . . . ? C33 C34 C35 Cl35 179.5(2) . . . . ? Cl34 C34 C35 Cl35 -0.6(3) . . . . ? C34 C35 C36 C31 1.9(4) . . . . ? Cl35 C35 C36 C31 -179.2(2) . . . . ? O31 C31 C36 C35 179.6(2) . . . . ? C32 C31 C36 C35 -0.7(4) . . . . ? O41 C41 C42 C43 -178.4(3) . . . . ? C46 C41 C42 C43 1.3(4) . . . . ? O41 C41 C42 Cl42 1.0(4) . . . . ? C46 C41 C42 Cl42 -179.4(2) . . . . ? C41 C42 C43 C44 -0.8(4) . . . . ? Cl42 C42 C43 C44 179.9(2) . . . . ? C42 C43 C44 C45 -0.2(4) . . . . ? C42 C43 C44 Cl44 179.7(2) . . . . ? C43 C44 C45 C46 0.7(4) . . . . ? Cl44 C44 C45 C46 -179.2(2) . . . . ? C43 C44 C45 Cl45 -179.5(2) . . . . ? Cl44 C44 C45 Cl45 0.5(4) . . . . ? C44 C45 C46 C41 -0.2(4) . . . . ? Cl45 C45 C46 C41 -180.0(2) . . . . ? O41 C41 C46 C45 178.8(3) . . . . ? C42 C41 C46 C45 -0.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.318 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.046