data_sr03 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H26 D2 Cl7 N O4' _chemical_formula_weight 620.62 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' 'D' 'D' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.625(2) _cell_length_b 11.705(2) _cell_length_c 12.203(2) _cell_angle_alpha 80.13(3) _cell_angle_beta 68.04(3) _cell_angle_gamma 84.11(3) _cell_volume 1385.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 636 _exptl_absorpt_coefficient_mu 0.746 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8652 _exptl_absorpt_correction_T_max 0.9292 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Nonius KappaCCD' _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 11418 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0550 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 28.34 _reflns_number_total 6807 _reflns_number_gt 4992 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement Denzo _computing_data_reduction Denzo _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material XCIF _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^)+(0.0990P)^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_number_reflns 6807 _refine_ls_number_parameters 347 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1517 _refine_ls_wR_factor_gt 0.1356 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.367 _refine_ls_shift/su_mean 0.015 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 Cl1 Cl 0.66280(6) 0.75253(4) 0.54277(5) 0.03631(15) Uani 1 1 d . . . Cl2 Cl 0.7528(6) -0.0702(5) 1.0861(4) 0.0627(8) Uani 0.50 1 d P A 1 Cl3 Cl 0.8438(2) 0.1677(2) 1.02087(19) 0.0600(5) Uani 0.50 1 d P A 1 Cl4 Cl 0.6922(3) 0.0866(3) 1.2691(3) 0.0723(9) Uani 0.50 1 d P A 1 Cl2' Cl 0.7759(8) -0.0596(7) 1.0866(6) 0.109(2) Uani 0.50 1 d P A 2 Cl3' Cl 0.8652(3) 0.1544(3) 1.0733(4) 0.1328(15) Uani 0.50 1 d P A 2 Cl4' Cl 0.6586(5) 0.0493(4) 1.2851(5) 0.1161(18) Uani 0.50 1 d P A 2 Cl5 Cl 0.18698(7) 0.56811(7) 0.76122(7) 0.0635(2) Uani 1 1 d . . . Cl6 Cl 0.14516(7) 0.38013(6) 0.95552(6) 0.0536(2) Uani 1 1 d . . . Cl7 Cl 0.13893(6) 0.33907(7) 0.73127(6) 0.0530(2) Uani 1 1 d . . . O1 O 0.79083(14) 0.44534(12) 0.85905(12) 0.0247(3) Uani 1 1 d . . . H1 H 0.754(3) 0.491(3) 0.906(3) 0.055(9) Uiso 1 1 d . . . O2 O 0.65283(16) 0.64996(13) 0.91178(13) 0.0356(4) Uani 1 1 d . . . H2 H 0.599(4) 0.702(3) 0.955(3) 0.081(11) Uiso 1 1 d . . . O3 O 0.64010(12) 0.25046(10) 0.85266(11) 0.0225(3) Uani 1 1 d . . . O4 O 0.47787(13) 0.15081(11) 0.99662(12) 0.0292(3) Uani 1 1 d . . . N1 N 0.64035(16) 0.05404(14) 0.85924(15) 0.0264(4) Uani 1 1 d . . . H3 H 0.604(3) -0.009(2) 0.896(2) 0.041(7) Uiso 1 1 d . . . C1 C 0.72477(17) 0.46879(15) 0.77468(15) 0.0193(3) Uani 1 1 d . . . H1A H 0.62632(17) 0.45313(15) 0.81806(15) 0.023 Uiso 1 1 d R . . C2 C 0.73624(18) 0.59917(15) 0.71522(16) 0.0207(4) Uani 1 1 d . . . C3 C 0.7217(2) 0.60833(15) 0.59189(17) 0.0246(4) Uani 1 1 d . . . H3A H 0.8157(2) 0.59656(15) 0.53323(17) 0.030 Uiso 1 1 d R . . C4 C 0.6384(2) 0.51571(16) 0.58086(18) 0.0269(4) Uani 1 1 d . . . H4A H 0.6239(2) 0.53298(16) 0.50406(18) 0.032 Uiso 1 1 d R . . H4B H 0.5489(2) 0.51148(16) 0.64693(18) 0.032 Uiso 1 1 d R . . C5 C 0.72159(18) 0.40149(15) 0.58697(16) 0.0223(4) Uani 1 1 d . . . H5A H 0.79442(18) 0.39505(15) 0.50731(16) 0.027 Uiso 1 1 d R . . C6 C 0.78494(17) 0.38400(14) 0.68517(15) 0.0192(4) Uani 1 1 d . . . H6A H 0.88644(17) 0.38317(14) 0.65084(15) 0.023 Uiso 1 1 d R . . C7 C 0.62580(19) 0.67221(17) 0.80257(18) 0.0264(4) Uani 1 1 d . . . H7A H 0.63987(19) 0.75617(17) 0.76954(18) 0.032 Uiso 1 1 d R . . C8 C 0.4787(2) 0.6483(2) 0.8298(2) 0.0364(5) Uani 1 1 d . . . H8A H 0.4191(2) 0.7012(2) 0.8834(2) 0.055 Uiso 1 1 d R . . H8B H 0.4611(2) 0.5679(2) 0.8682(2) 0.055 Uiso 1 1 d R . . H8C H 0.4610(2) 0.6604(2) 0.7553(2) 0.055 Uiso 1 1 d R . . C9 C 0.87569(19) 0.64366(17) 0.69159(19) 0.0287(4) Uani 1 1 d . . . H9A H 0.88953(19) 0.63841(17) 0.76735(19) 0.043 Uiso 1 1 d R . . H9B H 0.88050(19) 0.72472(17) 0.65343(19) 0.043 Uiso 1 1 d R . . H9C H 0.94644(19) 0.59639(17) 0.63884(19) 0.043 Uiso 1 1 d R . . C10 C 0.72983(17) 0.26021(15) 0.72760(16) 0.0201(4) Uani 1 1 d . . . C11 C 0.64859(19) 0.28403(16) 0.63922(17) 0.0235(4) Uani 1 1 d . . . C12 C 0.6814(2) 0.20030(18) 0.5486(2) 0.0361(5) Uani 1 1 d . . . H12A H 0.6261(2) 0.22238(18) 0.4989(2) 0.054 Uiso 1 1 d R . . H12B H 0.6613(2) 0.12127(18) 0.5906(2) 0.054 Uiso 1 1 d R . . H12C H 0.7779(2) 0.20337(18) 0.4979(2) 0.054 Uiso 1 1 d R . . C13 C 0.4943(2) 0.29554(19) 0.7038(2) 0.0340(5) Uani 1 1 d . . . H13A H 0.4500(2) 0.30961(19) 0.6450(2) 0.051 Uiso 1 1 d R . . H13B H 0.4722(2) 0.36063(19) 0.7497(2) 0.051 Uiso 1 1 d R . . H13C H 0.4621(2) 0.22373(19) 0.7580(2) 0.051 Uiso 1 1 d R . . C14 C 0.82885(18) 0.15700(15) 0.71128(16) 0.0207(4) Uani 1 1 d . . . C15 C 0.77509(19) 0.05158(16) 0.77729(16) 0.0231(4) Uani 1 1 d . . . C16 C 0.8519(2) -0.05196(16) 0.76400(18) 0.0278(4) Uani 1 1 d . . . H16A H 0.8143(2) -0.12281(16) 0.80993(18) 0.033 Uiso 1 1 d R . . C17 C 0.9842(2) -0.05021(17) 0.68265(19) 0.0308(4) Uani 1 1 d . . . H17A H 1.0374(2) -0.12063(17) 0.67163(19) 0.037 Uiso 1 1 d R . . C18 C 1.0396(2) 0.05351(18) 0.61724(19) 0.0307(4) Uani 1 1 d . . . H18A H 1.1309(2) 0.05414(18) 0.56241(19) 0.037 Uiso 1 1 d R . . C19 C 0.96172(19) 0.15657(16) 0.63177(17) 0.0262(4) Uani 1 1 d . . . H19A H 1.00015(19) 0.22742(16) 0.58666(17) 0.031 Uiso 1 1 d R . . C20 C 0.58158(18) 0.15014(15) 0.90636(16) 0.0232(4) Uani 1 1 d . . . C21 C 0.8078(3) 0.0379(3) 1.1470(3) 0.0660(9) Uani 1 1 d . . . D21A H 0.8929(3) 0.0093(3) 1.1616(3) 0.079 Uiso 1 1 d R A . C22 C 0.1003(2) 0.4397(2) 0.8318(2) 0.0390(5) Uani 1 1 d . . . D22A H 0.0004(2) 0.4588(2) 0.8605(2) 0.047 Uiso 1 1 d 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 Cl1 0.0521(3) 0.0232(2) 0.0363(3) 0.0029(2) -0.0224(2) -0.0005(2) Cl2 0.0853(14) 0.0634(16) 0.0487(13) 0.0042(12) -0.0312(11) -0.0385(13) Cl3 0.0544(10) 0.0581(11) 0.0664(11) -0.0041(8) -0.0211(8) -0.0096(8) Cl4 0.0732(18) 0.090(2) 0.0551(12) -0.0280(12) -0.0284(12) 0.0390(16) Cl2' 0.157(5) 0.090(2) 0.099(3) -0.032(2) -0.050(3) -0.038(3) Cl3' 0.0864(17) 0.0673(14) 0.234(5) 0.039(2) -0.066(2) -0.0303(12) Cl4' 0.090(2) 0.121(3) 0.127(3) -0.055(2) -0.0127(18) 0.0010(18) Cl5 0.0515(4) 0.0748(5) 0.0682(5) 0.0045(4) -0.0291(4) -0.0172(3) Cl6 0.0690(4) 0.0647(4) 0.0371(3) -0.0166(3) -0.0300(3) 0.0097(3) Cl7 0.0439(3) 0.0832(5) 0.0425(4) -0.0316(3) -0.0218(3) 0.0119(3) O1 0.0301(7) 0.0244(7) 0.0228(7) -0.0047(6) -0.0136(6) 0.0021(5) O2 0.0445(9) 0.0371(8) 0.0303(8) -0.0164(7) -0.0188(7) 0.0150(7) O3 0.0243(7) 0.0187(6) 0.0191(6) -0.0031(5) -0.0010(5) -0.0031(5) O4 0.0278(7) 0.0220(7) 0.0266(7) -0.0050(5) 0.0041(6) -0.0035(5) N1 0.0260(8) 0.0181(8) 0.0279(9) -0.0040(6) -0.0005(7) -0.0036(6) C1 0.0185(8) 0.0213(8) 0.0190(9) -0.0026(7) -0.0079(7) -0.0010(6) C2 0.0221(9) 0.0195(8) 0.0217(9) -0.0032(7) -0.0094(7) -0.0003(7) C3 0.0301(10) 0.0187(9) 0.0240(9) -0.0012(7) -0.0098(8) 0.0005(7) C4 0.0343(10) 0.0233(9) 0.0265(10) -0.0013(7) -0.0160(8) -0.0015(8) C5 0.0247(9) 0.0236(9) 0.0180(9) -0.0041(7) -0.0066(7) -0.0016(7) C6 0.0199(8) 0.0190(8) 0.0179(8) -0.0035(6) -0.0057(7) -0.0005(6) C7 0.0285(10) 0.0239(9) 0.0285(10) -0.0063(8) -0.0127(8) 0.0052(7) C8 0.0281(11) 0.0374(12) 0.0417(13) -0.0144(10) -0.0091(9) 0.0077(9) C9 0.0279(10) 0.0248(10) 0.0325(11) -0.0026(8) -0.0097(8) -0.0054(8) C10 0.0197(8) 0.0205(8) 0.0176(8) -0.0046(6) -0.0025(7) -0.0025(6) C11 0.0237(9) 0.0221(9) 0.0269(10) -0.0048(7) -0.0107(8) -0.0025(7) C12 0.0494(13) 0.0291(11) 0.0392(12) -0.0100(9) -0.0247(11) -0.0016(9) C13 0.0261(10) 0.0334(11) 0.0420(12) 0.0047(9) -0.0152(9) -0.0056(8) C14 0.0212(9) 0.0216(9) 0.0192(9) -0.0063(7) -0.0058(7) 0.0000(7) C15 0.0238(9) 0.0238(9) 0.0201(9) -0.0065(7) -0.0044(7) -0.0022(7) C16 0.0309(10) 0.0208(9) 0.0291(10) -0.0056(8) -0.0073(8) 0.0001(7) C17 0.0293(10) 0.0254(10) 0.0355(11) -0.0117(8) -0.0078(9) 0.0052(8) C18 0.0221(9) 0.0323(10) 0.0329(11) -0.0110(8) -0.0027(8) 0.0020(8) C19 0.0259(9) 0.0225(9) 0.0257(10) -0.0048(7) -0.0031(8) -0.0039(7) C20 0.0235(9) 0.0208(9) 0.0224(9) -0.0034(7) -0.0044(7) -0.0026(7) C21 0.0577(18) 0.072(2) 0.088(2) -0.0360(18) -0.0431(17) 0.0179(15) C22 0.0298(11) 0.0572(15) 0.0352(12) -0.0154(10) -0.0148(9) 0.0014(10) _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 Cl1 C3 1.8212(19) . ? Cl2 C21 1.815(6) . ? Cl3 C21 1.923(4) . ? Cl4 C21 1.683(5) . ? Cl2' C21 1.586(8) . ? Cl3' C21 1.543(5) . ? Cl4' C21 1.846(6) . ? Cl5 C22 1.759(3) . ? Cl6 C22 1.761(2) . ? Cl7 C22 1.755(2) . ? O1 H1 0.81(3) . ? O1 C1 1.425(2) . ? O2 H2 0.89(4) . ? O2 C7 1.442(2) . ? O3 C20 1.333(2) . ? O3 C10 1.458(2) . ? O4 C20 1.233(2) . ? N1 H3 0.84(3) . ? N1 C20 1.340(2) . ? N1 C15 1.408(2) . ? C1 H1A 1.0000 . ? C1 C6 1.519(2) . ? C1 C2 1.569(2) . ? C2 C9 1.529(3) . ? C2 C7 1.554(3) . ? C2 C3 1.554(3) . ? C3 H3A 1.0000 . ? C3 C4 1.520(3) . ? C4 H4B 0.9900 . ? C4 H4A 0.9900 . ? C4 C5 1.532(3) . ? C5 H5A 1.0000 . ? C5 C6 1.556(2) . ? C5 C11 1.564(3) . ? C6 H6A 1.0000 . ? C6 C10 1.549(2) . ? C7 H7A 1.0000 . ? C7 C8 1.516(3) . ? C8 H8C 0.9800 . ? C8 H8B 0.9800 . ? C8 H8A 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C14 1.507(2) . ? C10 C11 1.591(3) . ? C11 C12 1.523(3) . ? C11 C13 1.533(3) . ? C12 H12B 0.9800 . ? C12 H12A 0.9800 . ? C12 H12C 0.9800 . ? C13 H13C 0.9800 . ? C13 H13B 0.9800 . ? C13 H13A 0.9800 . ? C14 C19 1.382(3) . ? C14 C15 1.399(3) . ? C15 C16 1.388(3) . ? C16 H16A 0.9500 . ? C16 C17 1.385(3) . ? C17 H17A 0.9500 . ? C17 C18 1.386(3) . ? C18 H18A 0.9500 . ? C18 C19 1.389(3) . ? C19 H19A 0.9500 . ? C21 D21A 1.0000 . ? C22 D22A 1.0000 . ? 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 H1 O1 C1 105(2) . . ? H2 O2 C7 103(2) . . ? C20 O3 C10 118.96(14) . . ? H3 N1 C20 116.7(17) . . ? H3 N1 C15 118.9(17) . . ? C20 N1 C15 121.62(16) . . ? H1A C1 O1 108.13(9) . . ? H1A C1 C6 108.13(9) . . ? O1 C1 C6 107.68(14) . . ? H1A C1 C2 108.13(10) . . ? O1 C1 C2 111.35(14) . . ? C6 C1 C2 113.28(14) . . ? C9 C2 C7 108.74(15) . . ? C9 C2 C3 106.82(15) . . ? C7 C2 C3 113.42(15) . . ? C9 C2 C1 111.20(15) . . ? C7 C2 C1 108.02(14) . . ? C3 C2 C1 108.66(14) . . ? H3A C3 C4 105.80(11) . . ? H3A C3 C2 105.80(10) . . ? C4 C3 C2 115.38(15) . . ? H3A C3 Cl1 105.80(7) . . ? C4 C3 Cl1 110.66(13) . . ? C2 C3 Cl1 112.58(13) . . ? H4B C4 H4A 108.7 . . ? H4B C4 C3 110.60(11) . . ? H4A C4 C3 110.61(11) . . ? H4B C4 C5 110.61(11) . . ? H4A C4 C5 110.60(10) . . ? C3 C4 C5 105.67(15) . . ? H5A C5 C4 109.89(11) . . ? H5A C5 C6 109.89(9) . . ? C4 C5 C6 114.38(15) . . ? H5A C5 C11 109.90(10) . . ? C4 C5 C11 120.27(15) . . ? C6 C5 C11 91.10(13) . . ? H6A C6 C1 112.40(10) . . ? H6A C6 C10 112.39(10) . . ? C1 C6 C10 115.39(14) . . ? H6A C6 C5 112.40(9) . . ? C1 C6 C5 112.69(14) . . ? C10 C6 C5 89.71(13) . . ? H7A C7 O2 108.26(10) . . ? H7A C7 C8 108.26(12) . . ? O2 C7 C8 109.27(17) . . ? H7A C7 C2 108.25(10) . . ? O2 C7 C2 105.40(14) . . ? C8 C7 C2 117.10(16) . . ? H8C C8 H8B 109.5 . . ? H8C C8 H8A 109.5 . . ? H8B C8 H8A 109.5 . . ? H8C C8 C7 109.46(12) . . ? H8B C8 C7 109.48(12) . . ? H8A C8 C7 109.47(11) . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? H9A C9 C2 109.48(11) . . ? H9B C9 C2 109.46(10) . . ? H9C C9 C2 109.47(10) . . ? O3 C10 C14 108.69(15) . . ? O3 C10 C6 109.52(14) . . ? C14 C10 C6 119.14(15) . . ? O3 C10 C11 112.47(14) . . ? C14 C10 C11 115.69(15) . . ? C6 C10 C11 90.37(13) . . ? C12 C11 C13 109.59(17) . . ? C12 C11 C5 113.71(16) . . ? C13 C11 C5 115.14(16) . . ? C12 C11 C10 115.96(16) . . ? C13 C11 C10 113.26(16) . . ? C5 C11 C10 87.94(13) . . ? H12B C12 H12A 109.5 . . ? H12B C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 C11 109.47(11) . . ? H12A C12 C11 109.47(11) . . ? H12C C12 C11 109.48(11) . . ? H13C C13 H13B 109.5 . . ? H13C C13 H13A 109.5 . . ? H13B C13 H13A 109.5 . . ? H13C C13 C11 109.47(11) . . ? H13B C13 C11 109.47(12) . . ? H13A C13 C11 109.47(12) . . ? C19 C14 C15 118.52(17) . . ? C19 C14 C10 125.97(16) . . ? C15 C14 C10 115.31(15) . . ? C16 C15 C14 121.46(17) . . ? C16 C15 N1 120.84(17) . . ? C14 C15 N1 117.69(16) . . ? H16A C16 C17 120.57(12) . . ? H16A C16 C15 120.56(11) . . ? C17 C16 C15 118.86(18) . . ? H17A C17 C16 119.75(12) . . ? H17A C17 C18 119.76(12) . . ? C16 C17 C18 120.49(18) . . ? H18A C18 C17 119.98(12) . . ? H18A C18 C19 119.99(12) . . ? C17 C18 C19 120.03(18) . . ? H19A C19 C14 119.69(11) . . ? H19A C19 C18 119.69(12) . . ? C14 C19 C18 120.63(17) . . ? O4 C20 O3 118.46(16) . . ? O4 C20 N1 123.90(17) . . ? O3 C20 N1 117.64(16) . . ? D21A C21 Cl3' 94.82(16) . . ? D21A C21 Cl2' 105.2(3) . . ? Cl3' C21 Cl2' 121.2(4) . . ? D21A C21 Cl4 110.37(14) . . ? Cl3' C21 Cl4 99.7(3) . . ? Cl2' C21 Cl4 122.2(4) . . ? D21A C21 Cl2 110.0(2) . . ? Cl3' C21 Cl2 123.0(3) . . ? Cl2' C21 Cl2 5.9(5) . . ? Cl4 C21 Cl2 116.6(3) . . ? D21A C21 Cl4' 113.6(2) . . ? Cl3' C21 Cl4' 115.5(3) . . ? Cl2' C21 Cl4' 105.8(4) . . ? Cl4 C21 Cl4' 17.3(2) . . ? Cl2 C21 Cl4' 100.4(3) . . ? D21A C21 Cl3 110.37(11) . . ? Cl3' C21 Cl3 21.36(17) . . ? Cl2' C21 Cl3 101.9(3) . . ? Cl4 C21 Cl3 106.3(2) . . ? Cl2 C21 Cl3 102.8(2) . . ? Cl4' C21 Cl3 118.3(2) . . ? D22A C22 Cl7 108.82(8) . . ? D22A C22 Cl5 108.81(8) . . ? Cl7 C22 Cl5 110.48(13) . . ? D22A C22 Cl6 108.82(8) . . ? Cl7 C22 Cl6 110.19(13) . . ? Cl5 C22 Cl6 109.69(12) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.381 _refine_diff_density_min -0.419 _refine_diff_density_rms 0.056