# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_130606r #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C38 H22 N2' _chemical_formula_moiety 'C38 H22 N2' _chemical_formula_weight 506.61 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,+Y,1/2-Z 3 -X,-Y,-Z 4 +X,-Y,1/2+Z 5 1/2+X,1/2+Y,+Z 6 1/2-X,1/2+Y,1/2-Z 7 1/2-X,1/2-Y,-Z 8 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 16.181(9) _cell_length_b 10.378(5) _cell_length_c 17.045(9) _cell_angle_alpha 90.0000 _cell_angle_beta 117.095(6) _cell_angle_gamma 90.0000 _cell_volume 2548(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3120 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 29.22 _cell_measurement_temperature 150 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056.00 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.761 _exptl_absorpt_correction_T_max 0.992 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 150 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Mercury70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_reflns_number 9875 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_theta_max 27.00 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measured_fraction_theta_full 0.989 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2769 _reflns_number_gt 1965 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1665 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 2769 _refine_ls_number_parameters 182 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 0.220 _refine_diff_density_min -0.250 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 0.30487(9) 0.07962(14) 0.05971(8) 0.0271(4) Uani 1.0 8 d . . . C1 C 0.46149(10) 0.40972(16) 0.20933(10) 0.0227(4) Uani 1.0 8 d . . . C2 C 0.43576(11) 0.54435(17) 0.18126(10) 0.0238(4) Uani 1.0 8 d . . . C3 C 0.36765(11) 0.60472(18) 0.10834(10) 0.0275(4) Uani 1.0 8 d . . . C4 C 0.36687(12) 0.74152(19) 0.10667(11) 0.0322(5) Uani 1.0 8 d . . . C5 C 0.42983(12) 0.81569(18) 0.17422(11) 0.0316(5) Uani 1.0 8 d . . . C6 C 0.5000 0.7557(2) 0.2500 0.0269(6) Uani 1.0 4 d . . . C7 C 0.5000 0.6223(2) 0.2500 0.0242(6) Uani 1.0 4 d . . . C8 C 0.40833(11) 0.29582(16) 0.15796(10) 0.0221(4) Uani 1.0 8 d . . . C9 C 0.35657(11) 0.22060(16) 0.18855(9) 0.0231(4) Uani 1.0 8 d . . . C10 C 0.35080(12) 0.24735(17) 0.26794(10) 0.0274(5) Uani 1.0 8 d . . . C11 C 0.29825(13) 0.17381(18) 0.29354(11) 0.0327(5) Uani 1.0 8 d . . . C12 C 0.24766(13) 0.06675(18) 0.24165(11) 0.0349(5) Uani 1.0 8 d . . . C13 C 0.25125(12) 0.03756(17) 0.16589(11) 0.0305(5) Uani 1.0 8 d . . . C14 C 0.30484(11) 0.11323(17) 0.13614(10) 0.0245(4) Uani 1.0 8 d . . . C15 C 0.35386(11) 0.15243(17) 0.03059(10) 0.0252(4) Uani 1.0 8 d . . . C16 C 0.35436(13) 0.11525(19) -0.04945(11) 0.0335(5) Uani 1.0 8 d . . . C17 C 0.40131(14) 0.18412(19) -0.08375(11) 0.0386(5) Uani 1.0 8 d . . . C18 C 0.45156(13) 0.2962(2) -0.03927(11) 0.0352(5) Uani 1.0 8 d . . . C19 C 0.45394(12) 0.33436(17) 0.03789(10) 0.0293(5) Uani 1.0 8 d . . . C20 C 0.40623(11) 0.26381(16) 0.07652(9) 0.0238(4) Uani 1.0 8 d . . . H3 H 0.3227 0.5563 0.0607 0.0330 Uiso 1.0 8 calc R . . H4 H 0.3206 0.7838 0.0564 0.0387 Uiso 1.0 8 calc R . . H5 H 0.4263 0.9070 0.1702 0.0380 Uiso 1.0 8 calc R . . H10 H 0.3844 0.3181 0.3035 0.0329 Uiso 1.0 8 calc R . . H11 H 0.2951 0.1938 0.3465 0.0392 Uiso 1.0 8 calc R . . H12 H 0.2112 0.0156 0.2603 0.0419 Uiso 1.0 8 calc R . . H13 H 0.2175 -0.0345 0.1321 0.0365 Uiso 1.0 8 calc R . . H16 H 0.3211 0.0405 -0.0795 0.0402 Uiso 1.0 8 calc R . . H17 H 0.4007 0.1577 -0.1374 0.0464 Uiso 1.0 8 calc R . . H18 H 0.4838 0.3449 -0.0639 0.0423 Uiso 1.0 8 calc R . . H19 H 0.4880 0.4093 0.0666 0.0351 Uiso 1.0 8 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 N1 0.0314(7) 0.0221(9) 0.0270(7) -0.0008(6) 0.0124(6) -0.0006(6) C1 0.0259(8) 0.0193(9) 0.0268(7) 0.0000(7) 0.0156(7) -0.0002(7) C2 0.0259(8) 0.0211(10) 0.0277(8) 0.0008(7) 0.0152(7) 0.0012(7) C3 0.0265(8) 0.0262(10) 0.0303(8) -0.0004(7) 0.0134(7) 0.0021(7) C4 0.0275(9) 0.0311(12) 0.0348(9) 0.0038(8) 0.0113(8) 0.0082(8) C5 0.0321(9) 0.0190(10) 0.0439(10) 0.0048(8) 0.0173(8) 0.0038(7) C6 0.0298(12) 0.0201(14) 0.0348(12) 0.0000 0.0181(10) 0.0000 C7 0.0240(11) 0.0223(14) 0.0292(11) 0.0000 0.0147(10) 0.0000 C8 0.0233(8) 0.0166(9) 0.0253(8) 0.0033(7) 0.0100(7) 0.0009(6) C9 0.0259(8) 0.0173(9) 0.0251(8) 0.0036(7) 0.0107(7) 0.0020(7) C10 0.0303(9) 0.0240(11) 0.0279(8) -0.0002(7) 0.0132(7) 0.0000(7) C11 0.0412(10) 0.0314(12) 0.0316(9) -0.0013(8) 0.0219(8) 0.0008(7) C12 0.0413(10) 0.0310(12) 0.0382(9) -0.0077(9) 0.0231(8) 0.0035(8) C13 0.0345(9) 0.0209(10) 0.0359(9) -0.0064(7) 0.0160(8) -0.0001(7) C14 0.0268(8) 0.0194(10) 0.0259(8) 0.0006(7) 0.0107(7) 0.0013(7) C15 0.0257(8) 0.0218(10) 0.0270(8) 0.0016(7) 0.0110(7) 0.0011(7) C16 0.0390(10) 0.0311(12) 0.0309(9) -0.0055(8) 0.0164(8) -0.0090(8) C17 0.0483(11) 0.0435(13) 0.0321(9) -0.0024(10) 0.0252(9) -0.0060(8) C18 0.0422(10) 0.0378(12) 0.0335(9) -0.0027(9) 0.0240(8) 0.0032(8) C19 0.0316(9) 0.0256(11) 0.0306(9) -0.0013(8) 0.0142(8) 0.0009(7) C20 0.0259(8) 0.0207(10) 0.0248(8) 0.0032(7) 0.0115(7) 0.0025(7) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SIR2004 (Burla, et al., 2005)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 N1 C14 1.349(3) yes . . N1 C15 1.343(3) yes . . C1 C1 1.3789(19) yes . 2_655 C1 C2 1.474(3) yes . . C1 C8 1.489(3) yes . . C2 C3 1.380(2) yes . . C2 C7 1.414(2) yes . . C3 C4 1.420(3) yes . . C4 C5 1.374(3) yes . . C5 C6 1.4175(19) yes . . C6 C7 1.384(3) yes . . C8 C9 1.407(3) yes . . C8 C20 1.413(3) yes . . C9 C10 1.426(3) yes . . C9 C14 1.435(3) yes . . C10 C11 1.354(3) yes . . C11 C12 1.424(3) yes . . C12 C13 1.353(3) yes . . C13 C14 1.423(3) yes . . C15 C16 1.421(3) yes . . C15 C20 1.436(3) yes . . C16 C17 1.354(4) yes . . C17 C18 1.424(3) yes . . C18 C19 1.357(3) yes . . C19 C20 1.424(3) yes . . C3 H3 0.950 no . . C4 H4 0.950 no . . C5 H5 0.950 no . . C10 H10 0.950 no . . C11 H11 0.950 no . . C12 H12 0.950 no . . C13 H13 0.950 no . . C16 H16 0.950 no . . C17 H17 0.950 no . . C18 H18 0.950 no . . C19 H19 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C14 N1 C15 118.12(15) yes . . . C1 C1 C2 108.58(14) yes 2_655 . . C1 C1 C8 127.35(15) yes 2_655 . . C2 C1 C8 124.01(12) yes . . . C1 C2 C3 135.59(15) yes . . . C1 C2 C7 106.32(13) yes . . . C3 C2 C7 118.09(17) yes . . . C2 C3 C4 117.91(14) yes . . . C3 C4 C5 123.16(15) yes . . . C4 C5 C6 119.87(18) yes . . . C5 C6 C5 127.89(19) yes . . 2_655 C5 C6 C7 116.05(11) yes . . . C5 C6 C7 116.05(11) yes 2_655 . . C2 C7 C2 110.19(17) yes . . 2_655 C2 C7 C6 124.91(10) yes . . . C2 C7 C6 124.91(10) yes 2_655 . . C1 C8 C9 120.28(17) yes . . . C1 C8 C20 120.89(17) yes . . . C9 C8 C20 118.79(15) yes . . . C8 C9 C10 123.44(15) yes . . . C8 C9 C14 118.48(17) yes . . . C10 C9 C14 118.06(18) yes . . . C9 C10 C11 121.22(16) yes . . . C10 C11 C12 120.5(2) yes . . . C11 C12 C13 120.3(2) yes . . . C12 C13 C14 120.96(16) yes . . . N1 C14 C9 123.05(18) yes . . . N1 C14 C13 118.01(15) yes . . . C9 C14 C13 118.94(17) yes . . . N1 C15 C16 117.67(16) yes . . . N1 C15 C20 123.52(17) yes . . . C16 C15 C20 118.80(18) yes . . . C15 C16 C17 121.37(17) yes . . . C16 C17 C18 119.9(2) yes . . . C17 C18 C19 120.8(2) yes . . . C18 C19 C20 121.07(17) yes . . . C8 C20 C15 117.97(17) yes . . . C8 C20 C19 123.91(15) yes . . . C15 C20 C19 118.11(16) yes . . . C2 C3 H3 121.041 no . . . C4 C3 H3 121.044 no . . . C3 C4 H4 118.420 no . . . C5 C4 H4 118.423 no . . . C4 C5 H5 120.063 no . . . C6 C5 H5 120.064 no . . . C9 C10 H10 119.392 no . . . C11 C10 H10 119.385 no . . . C10 C11 H11 119.756 no . . . C12 C11 H11 119.759 no . . . C11 C12 H12 119.832 no . . . C13 C12 H12 119.832 no . . . C12 C13 H13 119.521 no . . . C14 C13 H13 119.524 no . . . C15 C16 H16 119.311 no . . . C17 C16 H16 119.315 no . . . C16 C17 H17 120.073 no . . . C18 C17 H17 120.072 no . . . C17 C18 H18 119.616 no . . . C19 C18 H18 119.622 no . . . C18 C19 H19 119.463 no . . . C20 C19 H19 119.469 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C14 N1 C15 C16 179.24(12) no . . . . C14 N1 C15 C20 0.1(3) no . . . . C15 N1 C14 C9 -1.7(3) no . . . . C15 N1 C14 C13 178.67(12) no . . . . C1 C1 C2 C3 179.5(2) no 2_655 . . . C1 C1 C2 C7 -0.8(3) no 2_655 . . . C2 C1 C1 C2 1.0(3) no . . 2_655 2_655 C2 C1 C1 C8 -176.33(17) no . . 2_655 2_655 C1 C1 C8 C9 67.7(3) no 2_655 . . . C1 C1 C8 C20 -114.5(2) no 2_655 . . . C8 C1 C1 C2 -176.33(18) no . . 2_655 2_655 C8 C1 C1 C8 6.3(4) no . . 2_655 2_655 C2 C1 C8 C9 -109.3(2) no . . . . C2 C1 C8 C20 68.6(3) no . . . . C8 C1 C2 C3 -3.0(4) no . . . . C8 C1 C2 C7 176.62(17) no . . . . C1 C2 C3 C4 -179.9(2) no . . . . C1 C2 C7 C2 0.30(17) no . . . 2_655 C1 C2 C7 C6 -179.70(10) no . . . . C3 C2 C7 C2 -179.98(15) no . . . 2_655 C3 C2 C7 C6 0.0(3) no . . . . C7 C2 C3 C4 0.5(3) no . . . . C2 C3 C4 C5 -0.6(4) no . . . . C3 C4 C5 C6 0.2(4) no . . . . C4 C5 C6 C5 -179.71(15) no . . . 2_655 C4 C5 C6 C7 0.3(3) no . . . . C5 C6 C7 C2 -0.43(11) no . . . . C5 C6 C7 C2 179.57(11) no . . . 2_655 C5 C6 C7 C2 179.57(11) no 2_655 . . . C5 C6 C7 C2 -0.43(11) no 2_655 . . 2_655 C1 C8 C9 C10 0.4(3) no . . . . C1 C8 C9 C14 178.76(12) no . . . . C1 C8 C20 C15 179.79(12) no . . . . C1 C8 C20 C19 0.7(3) no . . . . C9 C8 C20 C15 -2.4(2) no . . . . C9 C8 C20 C19 178.52(13) no . . . . C20 C8 C9 C10 -177.43(13) no . . . . C20 C8 C9 C14 0.9(2) no . . . . C8 C9 C10 C11 178.41(14) no . . . . C8 C9 C14 N1 1.3(3) no . . . . C8 C9 C14 C13 -179.16(13) no . . . . C10 C9 C14 N1 179.66(13) no . . . . C10 C9 C14 C13 -0.8(2) no . . . . C14 C9 C10 C11 0.1(3) no . . . . C9 C10 C11 C12 0.4(3) no . . . . C10 C11 C12 C13 -0.3(3) no . . . . C11 C12 C13 C14 -0.4(3) no . . . . C12 C13 C14 N1 -179.46(14) no . . . . C12 C13 C14 C9 0.9(3) no . . . . N1 C15 C16 C17 179.38(14) no . . . . N1 C15 C20 C8 2.0(3) no . . . . N1 C15 C20 C19 -178.88(13) no . . . . C16 C15 C20 C8 -177.16(13) no . . . . C16 C15 C20 C19 2.0(2) no . . . . C20 C15 C16 C17 -1.5(3) no . . . . C15 C16 C17 C18 0.1(3) no . . . . C16 C17 C18 C19 0.8(3) no . . . . C17 C18 C19 C20 -0.1(3) no . . . . C18 C19 C20 C8 177.88(15) no . . . . C18 C19 C20 C15 -1.2(3) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 N1 C8 2.844(3) no . . C1 C9 3.299(3) no . 2_655 C1 C10 2.945(3) no . . C1 C10 3.338(3) no . 2_655 C1 C19 2.973(3) no . . C2 C5 2.818(3) no . . C2 C19 3.386(3) no . . C2 C20 3.334(3) no . . C3 C6 2.857(2) no . . C3 C8 3.304(3) no . . C3 C19 3.576(3) no . . C4 C7 2.710(2) no . . C8 C8 3.189(3) no . 2_655 C8 C9 3.586(3) no . 2_655 C8 C10 3.543(4) no . 2_655 C9 C12 2.815(3) no . . C9 C15 2.765(3) no . . C10 C13 2.794(3) no . . C10 C19 3.497(3) no . 2_655 C11 C14 2.805(4) no . . C14 C16 3.600(4) no . . C14 C20 2.772(3) no . . C15 C18 2.803(4) no . . C16 C19 2.792(3) no . . C17 C20 2.820(3) no . . N1 C3 3.518(3) no . 7_555 N1 C5 3.436(3) no . 1_545 N1 C20 3.532(3) no . 7_555 C3 N1 3.518(3) no . 7_555 C5 N1 3.436(3) no . 1_565 C5 C14 3.585(3) no . 1_565 C9 C16 3.578(3) no . 7_555 C13 C18 3.457(3) no . 7_555 C14 C5 3.585(3) no . 1_545 C16 C9 3.578(3) no . 7_555 C18 C13 3.457(3) no . 7_555 C20 N1 3.532(3) no . 7_555 N1 H13 2.5513 no . . N1 H16 2.5360 no . . C1 H3 2.9308 no . . C1 H10 2.6195 no . . C1 H10 2.7688 no . 2_655 C1 H19 2.6557 no . . C1 H19 3.5230 no . 2_655 C2 H4 3.2500 no . . C2 H10 3.4821 no . . C2 H19 2.8287 no . . C3 H5 3.3078 no . . C3 H19 3.1098 no . . C5 H3 3.3075 no . . C5 H5 2.7799 no . 2_655 C6 H4 3.2670 no . . C6 H4 3.2670 no . 2_655 C6 H5 2.0642 no . 2_655 C7 H3 3.2674 no . . C7 H3 3.2674 no . 2_655 C7 H5 3.2442 no . . C7 H5 3.2442 no . 2_655 C8 H3 3.1432 no . . C8 H10 2.6898 no . . C8 H10 3.1183 no . 2_655 C8 H19 2.7022 no . . C9 H11 3.2794 no . . C9 H13 3.3201 no . . C10 H12 3.2616 no . . C10 H19 3.2989 no . 2_655 C11 H13 3.2678 no . . C12 H10 3.2691 no . . C13 H11 3.2589 no . . C14 H10 3.3125 no . . C14 H12 3.2748 no . . C15 H17 3.2788 no . . C15 H19 3.3136 no . . C16 H18 3.2551 no . . C17 H19 3.2745 no . . C18 H16 3.2635 no . . C19 H3 3.2740 no . . C19 H10 2.7810 no . 2_655 C19 H17 3.2684 no . . C20 H3 3.2833 no . . C20 H10 3.1083 no . 2_655 C20 H16 3.3170 no . . C20 H18 3.2784 no . . H3 H4 2.3620 no . . H3 H19 3.0407 no . . H4 H5 2.3020 no . . H5 H5 2.6798 no . 2_655 H10 H11 2.2918 no . . H10 H19 2.4279 no . 2_655 H11 H12 2.3679 no . . H12 H13 2.2939 no . . H16 H17 2.2955 no . . H17 H18 2.3696 no . . H18 H19 2.2940 no . . N1 H3 2.5699 no . 7_555 N1 H4 3.0831 no . 1_545 N1 H5 2.6917 no . 1_545 C1 H12 3.2557 no . 6_555 C2 H12 2.9822 no . 6_555 C2 H18 3.0643 no . 3_665 C3 H4 3.2728 no . 7_565 C3 H11 3.1985 no . 6_555 C3 H12 3.1779 no . 6_555 C3 H16 3.2360 no . 7_555 C3 H18 2.8783 no . 3_665 C4 H4 3.0524 no . 7_565 C4 H11 3.1078 no . 6_555 C4 H13 3.5191 no . 1_565 C4 H18 2.9631 no . 3_665 C5 H13 3.5337 no . 1_565 C5 H17 3.0916 no . 3_665 C5 H17 3.4628 no . 4_565 C5 H18 3.2651 no . 3_665 C6 H17 3.1439 no . 3_665 C6 H17 3.1439 no . 4_565 C6 H18 3.4610 no . 3_665 C6 H18 3.4610 no . 4_565 C7 H12 3.5199 no . 5_555 C7 H12 3.5199 no . 6_555 C7 H18 3.3174 no . 3_665 C7 H18 3.3174 no . 4_565 C9 H5 3.5051 no . 1_545 C9 H12 3.4931 no . 6_555 C10 H12 2.9232 no . 6_555 C10 H13 3.3120 no . 6_555 C11 H13 3.3365 no . 6_555 C11 H16 3.0065 no . 4_555 C11 H17 3.5640 no . 7_555 C12 H10 3.2128 no . 6_545 C12 H16 2.9402 no . 4_555 C12 H17 3.3406 no . 4_555 C13 H5 3.1113 no . 1_545 C13 H10 3.3648 no . 6_545 C13 H18 3.5988 no . 7_555 C14 H3 3.5081 no . 7_555 C14 H5 2.7826 no . 1_545 C15 H3 3.3502 no . 7_555 C15 H5 3.3135 no . 1_545 C16 H3 3.3030 no . 7_555 C16 H11 3.5779 no . 4_554 C16 H12 3.2986 no . 4_554 C18 H13 3.4868 no . 7_555 C18 H19 3.3055 no . 3_665 C19 H18 3.4474 no . 3_665 C19 H19 3.5575 no . 3_665 H3 N1 2.5699 no . 7_555 H3 C14 3.5081 no . 7_555 H3 C15 3.3502 no . 7_555 H3 C16 3.3030 no . 7_555 H3 H4 2.8109 no . 7_565 H3 H11 3.3038 no . 6_555 H3 H12 3.3624 no . 6_555 H3 H13 3.0543 no . 7_555 H3 H16 2.6833 no . 7_555 H3 H18 3.2722 no . 3_665 H4 N1 3.0831 no . 1_565 H4 C3 3.2728 no . 7_565 H4 C4 3.0524 no . 7_565 H4 H3 2.8109 no . 7_565 H4 H4 2.3255 no . 7_565 H4 H11 3.4182 no . 4_564 H4 H11 3.1522 no . 6_555 H4 H13 3.1558 no . 1_565 H4 H16 3.5334 no . 1_565 H4 H18 3.3840 no . 3_665 H5 N1 2.6917 no . 1_565 H5 C9 3.5051 no . 1_565 H5 C13 3.1113 no . 1_565 H5 C14 2.7826 no . 1_565 H5 C15 3.3135 no . 1_565 H5 H13 3.1952 no . 1_565 H5 H17 3.1653 no . 3_665 H5 H17 3.5535 no . 4_565 H10 C12 3.2128 no . 6_555 H10 C13 3.3648 no . 6_555 H10 H12 2.4989 no . 6_555 H10 H13 2.8136 no . 6_555 H11 C3 3.1985 no . 6_545 H11 C4 3.1078 no . 6_545 H11 C16 3.5779 no . 4_555 H11 H3 3.3038 no . 6_545 H11 H4 3.4182 no . 4_565 H11 H4 3.1522 no . 6_545 H11 H13 2.8626 no . 6_555 H11 H16 2.6829 no . 4_555 H12 C1 3.2557 no . 6_545 H12 C2 2.9822 no . 6_545 H12 C3 3.1779 no . 6_545 H12 C7 3.5199 no . 5_445 H12 C9 3.4931 no . 6_545 H12 C10 2.9232 no . 6_545 H12 C16 3.2986 no . 4_555 H12 H3 3.3624 no . 6_545 H12 H10 2.4989 no . 6_545 H12 H16 2.5558 no . 4_555 H12 H17 3.2873 no . 4_555 H13 C4 3.5191 no . 1_545 H13 C5 3.5337 no . 1_545 H13 C10 3.3120 no . 6_545 H13 C11 3.3365 no . 6_545 H13 C18 3.4868 no . 7_555 H13 H3 3.0543 no . 7_555 H13 H4 3.1558 no . 1_545 H13 H5 3.1952 no . 1_545 H13 H10 2.8136 no . 6_545 H13 H11 2.8626 no . 6_545 H13 H18 3.5191 no . 7_555 H13 H19 3.4066 no . 5_445 H16 C3 3.2360 no . 7_555 H16 C11 3.0065 no . 4_554 H16 C12 2.9402 no . 4_554 H16 H3 2.6833 no . 7_555 H16 H4 3.5334 no . 1_545 H16 H11 2.6829 no . 4_554 H16 H12 2.5558 no . 4_554 H17 C5 3.0916 no . 3_665 H17 C5 3.4628 no . 4_564 H17 C6 3.1439 no . 3_665 H17 C11 3.5640 no . 7_555 H17 C12 3.3406 no . 4_554 H17 H5 3.1653 no . 3_665 H17 H5 3.5535 no . 4_564 H17 H12 3.2873 no . 4_554 H18 C2 3.0643 no . 3_665 H18 C3 2.8783 no . 3_665 H18 C4 2.9631 no . 3_665 H18 C5 3.2651 no . 3_665 H18 C6 3.4610 no . 3_665 H18 C7 3.3174 no . 3_665 H18 C13 3.5988 no . 7_555 H18 C19 3.4474 no . 3_665 H18 H3 3.2722 no . 3_665 H18 H4 3.3840 no . 3_665 H18 H13 3.5191 no . 7_555 H18 H19 2.5954 no . 3_665 H19 C18 3.3055 no . 3_665 H19 C19 3.5575 no . 3_665 H19 H13 3.4066 no . 5_555 H19 H18 2.5954 no . 3_665 H19 H19 3.1069 no . 3_665 #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 975883' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_130607r #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C39 H23 Cl3 N2' _chemical_formula_moiety 'C39 H23 Cl3 N2' _chemical_formula_weight 625.98 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 21.8437(16) _cell_length_b 13.9673(9) _cell_length_c 9.6149(11) _cell_angle_alpha 90.0000 _cell_angle_beta 94.127(4) _cell_angle_gamma 90.0000 _cell_volume 2925.9(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8784 _cell_measurement_theta_min 1.73 _cell_measurement_theta_max 29.23 _cell_measurement_temperature 150 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288.00 _exptl_absorpt_coefficient_mu 0.346 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.767 _exptl_absorpt_correction_T_max 0.933 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 150 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku Mercury70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_reflns_number 19951 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_theta_max 27.00 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measured_fraction_theta_full 0.981 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6267 _reflns_number_gt 4952 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1707 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 6265 _refine_ls_number_parameters 397 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_diff_density_max 0.510 _refine_diff_density_min -0.450 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.1484 0.1585 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 0.05234(3) 0.35004(5) 0.92861(6) 0.0468(2) Uani 1.0 4 d . . . Cl2 Cl -0.02724(3) 0.23647(5) 1.08676(7) 0.0535(3) Uani 1.0 4 d . . . Cl3 Cl 0.01627(4) 0.41855(6) 1.19430(7) 0.0601(3) Uani 1.0 4 d . . . N1 N 0.47575(8) 0.39886(13) 0.85354(16) 0.0272(4) Uani 1.0 4 d . . . N2 N 0.15870(8) 0.29052(13) 0.69059(16) 0.0281(4) Uani 1.0 4 d . . . C1 C 0.31072(9) 0.51023(13) 1.01796(18) 0.0210(4) Uani 1.0 4 d . . . C2 C 0.25003(9) 0.48998(13) 0.98092(19) 0.0223(4) Uani 1.0 4 d . . . C3 C 0.21175(9) 0.55032(14) 1.06693(19) 0.0231(4) Uani 1.0 4 d . . . C4 C 0.14940(10) 0.56091(15) 1.0790(2) 0.0274(5) Uani 1.0 4 d . . . C5 C 0.13017(10) 0.62670(16) 1.1795(2) 0.0305(5) Uani 1.0 4 d . . . C6 C 0.17072(10) 0.68026(15) 1.2634(2) 0.0292(5) Uani 1.0 4 d . . . C7 C 0.23467(9) 0.67159(14) 1.25176(19) 0.0240(5) Uani 1.0 4 d . . . C8 C 0.28348(10) 0.72143(14) 1.3260(2) 0.0276(5) Uani 1.0 4 d . . . C9 C 0.34314(10) 0.70374(15) 1.2986(2) 0.0284(5) Uani 1.0 4 d . . . C10 C 0.36003(10) 0.63430(14) 1.20003(18) 0.0251(5) Uani 1.0 4 d . . . C11 C 0.31369(9) 0.58479(14) 1.12753(18) 0.0226(4) Uani 1.0 4 d . . . C12 C 0.25250(9) 0.60532(13) 1.15409(18) 0.0216(4) Uani 1.0 4 d . . . C13 C 0.36611(9) 0.46991(14) 0.96027(18) 0.0215(4) Uani 1.0 4 d . . . C14 C 0.37809(9) 0.48496(14) 0.82022(19) 0.0222(4) Uani 1.0 4 d . . . C15 C 0.33885(10) 0.53922(14) 0.72569(19) 0.0262(5) Uani 1.0 4 d . . . C16 C 0.35235(10) 0.55161(15) 0.5906(2) 0.0308(5) Uani 1.0 4 d . . . C17 C 0.40556(10) 0.51037(17) 0.5413(2) 0.0339(5) Uani 1.0 4 d . . . C18 C 0.44515(10) 0.45942(16) 0.6283(2) 0.0324(5) Uani 1.0 4 d . . . C19 C 0.43346(9) 0.44681(14) 0.77130(19) 0.0252(5) Uani 1.0 4 d . . . C20 C 0.46377(9) 0.38494(15) 0.98735(19) 0.0247(5) Uani 1.0 4 d . . . C21 C 0.50799(10) 0.33282(16) 1.0736(2) 0.0313(5) Uani 1.0 4 d . . . C22 C 0.49818(11) 0.31225(17) 1.2089(3) 0.0347(5) Uani 1.0 4 d . . . C23 C 0.44336(11) 0.34252(16) 1.2661(2) 0.0315(5) Uani 1.0 4 d . . . C24 C 0.40065(10) 0.39431(15) 1.18895(19) 0.0264(5) Uani 1.0 4 d . . . C25 C 0.40957(9) 0.41850(14) 1.04636(18) 0.0225(4) Uani 1.0 4 d . . . C26 C 0.22279(9) 0.42087(14) 0.87626(19) 0.0232(4) Uani 1.0 4 d . . . C27 C 0.23341(9) 0.32217(14) 0.88830(18) 0.0230(4) Uani 1.0 4 d . . . C28 C 0.27430(10) 0.27865(15) 0.9929(2) 0.0277(5) Uani 1.0 4 d . . . C29 C 0.28291(10) 0.18265(16) 0.9976(2) 0.0325(5) Uani 1.0 4 d . . . C30 C 0.25024(12) 0.12160(17) 0.9023(3) 0.0366(6) Uani 1.0 4 d . . . C31 C 0.20931(11) 0.15847(16) 0.8021(3) 0.0330(5) Uani 1.0 4 d . . . C32 C 0.19970(10) 0.25891(15) 0.79172(19) 0.0263(5) Uani 1.0 4 d . . . C33 C 0.15158(10) 0.38551(15) 0.67542(19) 0.0267(5) Uani 1.0 4 d . . . C34 C 0.11039(11) 0.41880(17) 0.5634(2) 0.0339(5) Uani 1.0 4 d . . . C35 C 0.10103(11) 0.51351(17) 0.5410(3) 0.0367(6) Uani 1.0 4 d . . . C36 C 0.13264(12) 0.58250(17) 0.6284(3) 0.0361(6) Uani 1.0 4 d . . . C37 C 0.17161(10) 0.55355(15) 0.7367(2) 0.0299(5) Uani 1.0 4 d . . . C38 C 0.18243(9) 0.45457(14) 0.76564(19) 0.0251(5) Uani 1.0 4 d . . . C39 C 0.03424(10) 0.31752(17) 1.0973(2) 0.0326(5) Uani 1.0 4 d . . . H4 H 0.1204 0.5252 1.0217 0.0328 Uiso 1.0 4 calc R . . H5 H 0.0875 0.6341 1.1892 0.0366 Uiso 1.0 4 calc R . . H6 H 0.1557 0.7233 1.3295 0.0350 Uiso 1.0 4 calc R . . H8 H 0.2747 0.7672 1.3948 0.0331 Uiso 1.0 4 calc R . . H9 H 0.3747 0.7395 1.3478 0.0340 Uiso 1.0 4 calc R . . H10 H 0.4019 0.6226 1.1849 0.0301 Uiso 1.0 4 calc R . . H15 H 0.3027 0.5672 0.7571 0.0314 Uiso 1.0 4 calc R . . H16 H 0.3257 0.5884 0.5292 0.0369 Uiso 1.0 4 calc R . . H17 H 0.4138 0.5182 0.4463 0.0407 Uiso 1.0 4 calc R . . H18 H 0.4808 0.4320 0.5936 0.0389 Uiso 1.0 4 calc R . . H21 H 0.5448 0.3121 1.0362 0.0375 Uiso 1.0 4 calc R . . H22 H 0.5282 0.2776 1.2649 0.0416 Uiso 1.0 4 calc R . . H23 H 0.4364 0.3264 1.3596 0.0378 Uiso 1.0 4 calc R . . H24 H 0.3645 0.4148 1.2296 0.0317 Uiso 1.0 4 calc R . . H28 H 0.2959 0.3180 1.0605 0.0332 Uiso 1.0 4 calc R . . H29 H 0.3114 0.1561 1.0663 0.0390 Uiso 1.0 4 calc R . . H30 H 0.2567 0.0544 0.9076 0.0439 Uiso 1.0 4 calc R . . H31 H 0.1872 0.1167 0.7389 0.0396 Uiso 1.0 4 calc R . . H34 H 0.0892 0.3736 0.5038 0.0407 Uiso 1.0 4 calc R . . H35 H 0.0732 0.5341 0.4664 0.0440 Uiso 1.0 4 calc R . . H36 H 0.1265 0.6489 0.6109 0.0433 Uiso 1.0 4 calc R . . H37 H 0.1921 0.6004 0.7946 0.0358 Uiso 1.0 4 calc R . . H39 H 0.0708 0.2853 1.1454 0.0391 Uiso 1.0 4 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cl1 0.0479(5) 0.0534(5) 0.0401(4) -0.0110(3) 0.0092(3) 0.0040(3) Cl2 0.0395(4) 0.0586(5) 0.0616(5) -0.0202(4) -0.0011(3) 0.0135(3) Cl3 0.0672(6) 0.0550(5) 0.0596(5) 0.0061(4) 0.0147(4) -0.0162(3) N1 0.0232(10) 0.0309(10) 0.0279(9) 0.0034(8) 0.0039(7) -0.0012(7) N2 0.0296(10) 0.0273(10) 0.0274(9) -0.0016(8) 0.0019(7) -0.0037(7) C1 0.0219(10) 0.0203(10) 0.0205(9) 0.0013(8) 0.0004(7) 0.0008(7) C2 0.0228(11) 0.0195(10) 0.0245(10) 0.0016(8) 0.0018(7) 0.0017(7) C3 0.0225(11) 0.0213(11) 0.0255(10) 0.0008(8) 0.0019(7) 0.0009(7) C4 0.0224(11) 0.0266(11) 0.0328(11) -0.0005(9) 0.0004(8) -0.0016(8) C5 0.0213(11) 0.0320(12) 0.0388(12) 0.0036(9) 0.0059(9) -0.0001(9) C6 0.0286(12) 0.0259(11) 0.0336(11) 0.0044(9) 0.0060(8) -0.0024(8) C7 0.0259(11) 0.0209(10) 0.0256(10) 0.0015(8) 0.0032(8) 0.0000(7) C8 0.0348(13) 0.0221(11) 0.0258(10) 0.0008(9) 0.0013(8) -0.0028(8) C9 0.0303(12) 0.0256(11) 0.0287(10) -0.0041(9) -0.0013(8) -0.0035(8) C10 0.0226(11) 0.0285(11) 0.0241(10) -0.0013(9) 0.0017(8) 0.0010(8) C11 0.0251(11) 0.0205(10) 0.0221(9) 0.0003(8) 0.0006(8) 0.0018(7) C12 0.0244(11) 0.0185(10) 0.0219(9) 0.0003(8) 0.0024(7) 0.0015(7) C13 0.0209(10) 0.0191(10) 0.0246(10) -0.0015(8) 0.0028(7) -0.0011(7) C14 0.0205(10) 0.0226(10) 0.0237(9) -0.0020(8) 0.0014(7) 0.0007(7) C15 0.0251(11) 0.0253(11) 0.0280(10) 0.0005(9) 0.0013(8) 0.0005(8) C16 0.0332(13) 0.0304(12) 0.0280(11) -0.0001(10) -0.0028(8) 0.0038(8) C17 0.0358(13) 0.0440(14) 0.0223(10) -0.0048(11) 0.0047(9) 0.0014(9) C18 0.0296(12) 0.0393(14) 0.0291(11) 0.0012(10) 0.0072(9) -0.0029(9) C19 0.0252(11) 0.0252(11) 0.0255(10) -0.0017(9) 0.0040(8) -0.0027(8) C20 0.0225(11) 0.0253(11) 0.0264(10) 0.0009(9) 0.0018(8) -0.0018(8) C21 0.0253(12) 0.0343(13) 0.0345(11) 0.0086(10) 0.0045(9) 0.0030(9) C22 0.0321(13) 0.0354(13) 0.0357(12) 0.0099(10) -0.0032(9) 0.0056(9) C23 0.0329(13) 0.0352(13) 0.0266(10) 0.0047(10) 0.0024(8) 0.0041(8) C24 0.0251(12) 0.0304(12) 0.0240(10) 0.0022(9) 0.0031(8) -0.0005(8) C25 0.0210(11) 0.0218(10) 0.0250(10) -0.0002(8) 0.0028(7) -0.0010(7) C26 0.0184(10) 0.0269(11) 0.0247(10) -0.0019(8) 0.0037(7) -0.0022(7) C27 0.0225(11) 0.0228(11) 0.0244(10) -0.0001(8) 0.0055(7) -0.0017(7) C28 0.0262(12) 0.0279(12) 0.0289(11) 0.0009(9) 0.0023(8) 0.0008(8) C29 0.0300(13) 0.0295(13) 0.0381(12) 0.0032(10) 0.0040(9) 0.0036(9) C30 0.0420(15) 0.0231(12) 0.0454(13) 0.0027(10) 0.0082(10) -0.0007(9) C31 0.0387(14) 0.0244(12) 0.0367(12) -0.0042(10) 0.0086(9) -0.0071(8) C32 0.0289(12) 0.0249(11) 0.0257(10) -0.0018(9) 0.0049(8) -0.0032(8) C33 0.0261(12) 0.0291(12) 0.0250(10) -0.0006(9) 0.0024(8) -0.0021(8) C34 0.0335(13) 0.0375(14) 0.0295(11) -0.0029(10) -0.0064(9) -0.0031(9) C35 0.0391(14) 0.0358(13) 0.0331(12) 0.0011(11) -0.0112(9) 0.0021(9) C36 0.0425(15) 0.0279(12) 0.0366(12) 0.0033(10) -0.0062(10) 0.0026(9) C37 0.0296(12) 0.0270(12) 0.0324(11) -0.0012(9) -0.0017(8) -0.0014(8) C38 0.0223(11) 0.0261(11) 0.0270(10) -0.0011(9) 0.0031(7) -0.0021(8) C39 0.0240(12) 0.0356(13) 0.0374(12) 0.0005(10) -0.0026(9) 0.0032(9) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SIR2004 (Burla, et al., 2005)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cl1 C39 1.757(3) yes . . Cl2 C39 1.754(3) yes . . Cl3 C39 1.752(3) yes . . N1 C19 1.350(3) yes . . N1 C20 1.345(3) yes . . N2 C32 1.348(3) yes . . N2 C33 1.343(3) yes . . C1 C2 1.377(3) yes . . C1 C11 1.479(3) yes . . C1 C13 1.478(3) yes . . C2 C3 1.481(3) yes . . C2 C26 1.487(3) yes . . C3 C4 1.383(3) yes . . C3 C12 1.406(3) yes . . C4 C5 1.419(3) yes . . C5 C6 1.376(3) yes . . C6 C7 1.415(3) yes . . C7 C8 1.422(3) yes . . C7 C12 1.394(3) yes . . C8 C9 1.370(3) yes . . C9 C10 1.423(3) yes . . C10 C11 1.374(3) yes . . C11 C12 1.408(3) yes . . C13 C14 1.406(3) yes . . C13 C25 1.410(3) yes . . C14 C15 1.422(3) yes . . C14 C19 1.432(3) yes . . C15 C16 1.363(3) yes . . C16 C17 1.410(4) yes . . C17 C18 1.360(3) yes . . C18 C19 1.428(3) yes . . C20 C21 1.426(3) yes . . C20 C25 1.428(3) yes . . C21 C22 1.365(3) yes . . C22 C23 1.418(4) yes . . C23 C24 1.358(3) yes . . C24 C25 1.439(3) yes . . C26 C27 1.401(3) yes . . C26 C38 1.412(3) yes . . C27 C28 1.432(3) yes . . C27 C32 1.445(3) yes . . C28 C29 1.354(3) yes . . C29 C30 1.408(4) yes . . C30 C31 1.367(4) yes . . C31 C32 1.421(3) yes . . C33 C34 1.430(3) yes . . C33 C38 1.433(3) yes . . C34 C35 1.354(4) yes . . C35 C36 1.424(4) yes . . C36 C37 1.359(3) yes . . C37 C38 1.427(3) yes . . C4 H4 0.950 no . . C5 H5 0.950 no . . C6 H6 0.950 no . . C8 H8 0.950 no . . C9 H9 0.950 no . . C10 H10 0.950 no . . C15 H15 0.950 no . . C16 H16 0.950 no . . C17 H17 0.950 no . . C18 H18 0.950 no . . C21 H21 0.950 no . . C22 H22 0.950 no . . C23 H23 0.950 no . . C24 H24 0.950 no . . C28 H28 0.950 no . . C29 H29 0.950 no . . C30 H30 0.950 no . . C31 H31 0.950 no . . C34 H34 0.950 no . . C35 H35 0.950 no . . C36 H36 0.950 no . . C37 H37 0.950 no . . C39 H39 1.000 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C19 N1 C20 117.38(18) yes . . . C32 N2 C33 117.89(18) yes . . . C2 C1 C11 108.71(17) yes . . . C2 C1 C13 128.57(17) yes . . . C11 C1 C13 122.70(17) yes . . . C1 C2 C3 108.09(16) yes . . . C1 C2 C26 129.72(18) yes . . . C3 C2 C26 122.19(17) yes . . . C2 C3 C4 134.96(18) yes . . . C2 C3 C12 106.56(17) yes . . . C4 C3 C12 118.46(18) yes . . . C3 C4 C5 117.90(19) yes . . . C4 C5 C6 122.8(2) yes . . . C5 C6 C7 120.3(2) yes . . . C6 C7 C8 128.87(19) yes . . . C6 C7 C12 115.82(18) yes . . . C8 C7 C12 115.31(18) yes . . . C7 C8 C9 120.30(19) yes . . . C8 C9 C10 123.13(19) yes . . . C9 C10 C11 117.7(2) yes . . . C1 C11 C10 135.12(19) yes . . . C1 C11 C12 106.20(16) yes . . . C10 C11 C12 118.67(18) yes . . . C3 C12 C7 124.66(19) yes . . . C3 C12 C11 110.43(17) yes . . . C7 C12 C11 124.91(18) yes . . . C1 C13 C14 121.08(17) yes . . . C1 C13 C25 120.55(16) yes . . . C14 C13 C25 118.32(18) yes . . . C13 C14 C15 123.13(19) yes . . . C13 C14 C19 118.61(17) yes . . . C15 C14 C19 118.22(17) yes . . . C14 C15 C16 121.0(2) yes . . . C15 C16 C17 120.59(19) yes . . . C16 C17 C18 120.66(19) yes . . . C17 C18 C19 120.5(2) yes . . . N1 C19 C14 123.43(17) yes . . . N1 C19 C18 117.59(18) yes . . . C14 C19 C18 118.98(18) yes . . . N1 C20 C21 117.34(19) yes . . . N1 C20 C25 123.80(18) yes . . . C21 C20 C25 118.86(17) yes . . . C20 C21 C22 121.0(2) yes . . . C21 C22 C23 120.1(2) yes . . . C22 C23 C24 120.9(2) yes . . . C23 C24 C25 120.7(2) yes . . . C13 C25 C20 118.43(17) yes . . . C13 C25 C24 123.18(18) yes . . . C20 C25 C24 118.32(17) yes . . . C2 C26 C27 121.79(17) yes . . . C2 C26 C38 119.39(17) yes . . . C27 C26 C38 118.73(17) yes . . . C26 C27 C28 124.54(18) yes . . . C26 C27 C32 118.35(17) yes . . . C28 C27 C32 117.08(18) yes . . . C27 C28 C29 121.46(19) yes . . . C28 C29 C30 121.0(2) yes . . . C29 C30 C31 120.4(3) yes . . . C30 C31 C32 120.5(2) yes . . . N2 C32 C27 123.01(19) yes . . . N2 C32 C31 117.45(19) yes . . . C27 C32 C31 119.54(18) yes . . . N2 C33 C34 117.69(19) yes . . . N2 C33 C38 123.63(18) yes . . . C34 C33 C38 118.68(19) yes . . . C33 C34 C35 121.2(2) yes . . . C34 C35 C36 120.4(2) yes . . . C35 C36 C37 120.1(3) yes . . . C36 C37 C38 121.6(2) yes . . . C26 C38 C33 118.19(18) yes . . . C26 C38 C37 123.74(18) yes . . . C33 C38 C37 118.06(17) yes . . . Cl1 C39 Cl2 109.62(12) yes . . . Cl1 C39 Cl3 110.93(13) yes . . . Cl2 C39 Cl3 110.54(13) yes . . . C3 C4 H4 121.044 no . . . C5 C4 H4 121.060 no . . . C4 C5 H5 118.587 no . . . C6 C5 H5 118.592 no . . . C5 C6 H6 119.838 no . . . C7 C6 H6 119.841 no . . . C7 C8 H8 119.849 no . . . C9 C8 H8 119.852 no . . . C8 C9 H9 118.432 no . . . C10 C9 H9 118.441 no . . . C9 C10 H10 121.168 no . . . C11 C10 H10 121.180 no . . . C14 C15 H15 119.508 no . . . C16 C15 H15 119.518 no . . . C15 C16 H16 119.713 no . . . C17 C16 H16 119.698 no . . . C16 C17 H17 119.663 no . . . C18 C17 H17 119.674 no . . . C17 C18 H18 119.763 no . . . C19 C18 H18 119.767 no . . . C20 C21 H21 119.484 no . . . C22 C21 H21 119.494 no . . . C21 C22 H22 119.934 no . . . C23 C22 H22 119.933 no . . . C22 C23 H23 119.553 no . . . C24 C23 H23 119.551 no . . . C23 C24 H24 119.649 no . . . C25 C24 H24 119.648 no . . . C27 C28 H28 119.269 no . . . C29 C28 H28 119.272 no . . . C28 C29 H29 119.493 no . . . C30 C29 H29 119.487 no . . . C29 C30 H30 119.810 no . . . C31 C30 H30 119.805 no . . . C30 C31 H31 119.769 no . . . C32 C31 H31 119.765 no . . . C33 C34 H34 119.421 no . . . C35 C34 H34 119.415 no . . . C34 C35 H35 119.812 no . . . C36 C35 H35 119.805 no . . . C35 C36 H36 119.948 no . . . C37 C36 H36 119.945 no . . . C36 C37 H37 119.208 no . . . C38 C37 H37 119.209 no . . . Cl1 C39 H39 108.557 no . . . Cl2 C39 H39 108.570 no . . . Cl3 C39 H39 108.557 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C19 N1 C20 C21 178.94(16) no . . . . C19 N1 C20 C25 -0.5(3) no . . . . C20 N1 C19 C14 1.6(3) no . . . . C20 N1 C19 C18 -178.28(16) no . . . . C32 N2 C33 C34 176.83(17) no . . . . C32 N2 C33 C38 -3.8(3) no . . . . C33 N2 C32 C27 3.5(3) no . . . . C33 N2 C32 C31 -176.68(17) no . . . . C2 C1 C11 C10 -177.74(18) no . . . . C2 C1 C11 C12 1.13(19) no . . . . C11 C1 C2 C3 -0.63(19) no . . . . C11 C1 C2 C26 179.96(16) no . . . . C2 C1 C13 C14 63.7(3) no . . . . C2 C1 C13 C25 -118.9(2) no . . . . C13 C1 C2 C3 -178.83(16) no . . . . C13 C1 C2 C26 1.8(4) no . . . . C11 C1 C13 C14 -114.27(19) no . . . . C11 C1 C13 C25 63.2(3) no . . . . C13 C1 C11 C10 0.6(3) no . . . . C13 C1 C11 C12 179.45(15) no . . . . C1 C2 C3 C4 -178.77(18) no . . . . C1 C2 C3 C12 -0.1(2) no . . . . C1 C2 C26 C27 62.0(3) no . . . . C1 C2 C26 C38 -121.5(2) no . . . . C3 C2 C26 C27 -117.3(2) no . . . . C3 C2 C26 C38 59.2(3) no . . . . C26 C2 C3 C4 0.7(4) no . . . . C26 C2 C3 C12 179.37(15) no . . . . C2 C3 C4 C5 178.30(18) no . . . . C2 C3 C12 C7 -179.87(15) no . . . . C2 C3 C12 C11 0.8(2) no . . . . C4 C3 C12 C7 -0.9(3) no . . . . C4 C3 C12 C11 179.77(16) no . . . . C12 C3 C4 C5 -0.3(3) no . . . . C3 C4 C5 C6 0.6(3) no . . . . C4 C5 C6 C7 0.2(3) no . . . . C5 C6 C7 C8 178.57(18) no . . . . C5 C6 C7 C12 -1.3(3) no . . . . C6 C7 C8 C9 -179.22(18) no . . . . C6 C7 C12 C3 1.7(3) no . . . . C6 C7 C12 C11 -179.11(16) no . . . . C8 C7 C12 C3 -178.19(15) no . . . . C8 C7 C12 C11 1.0(3) no . . . . C12 C7 C8 C9 0.6(3) no . . . . C7 C8 C9 C10 -1.9(3) no . . . . C8 C9 C10 C11 1.5(3) no . . . . C9 C10 C11 C1 178.90(18) no . . . . C9 C10 C11 C12 0.1(3) no . . . . C1 C11 C12 C3 -1.20(19) no . . . . C1 C11 C12 C7 179.50(15) no . . . . C10 C11 C12 C3 177.88(15) no . . . . C10 C11 C12 C7 -1.4(3) no . . . . C1 C13 C14 C15 0.3(3) no . . . . C1 C13 C14 C19 178.00(15) no . . . . C1 C13 C25 C20 -177.02(15) no . . . . C1 C13 C25 C24 6.0(3) no . . . . C14 C13 C25 C20 0.5(3) no . . . . C14 C13 C25 C24 -176.51(16) no . . . . C25 C13 C14 C15 -177.22(16) no . . . . C25 C13 C14 C19 0.5(3) no . . . . C13 C14 C15 C16 -179.82(17) no . . . . C13 C14 C19 N1 -1.6(3) no . . . . C13 C14 C19 C18 178.24(16) no . . . . C15 C14 C19 N1 176.21(17) no . . . . C15 C14 C19 C18 -3.9(3) no . . . . C19 C14 C15 C16 2.4(3) no . . . . C14 C15 C16 C17 0.3(3) no . . . . C15 C16 C17 C18 -1.6(4) no . . . . C16 C17 C18 C19 0.0(4) no . . . . C17 C18 C19 N1 -177.36(19) no . . . . C17 C18 C19 C14 2.8(3) no . . . . N1 C20 C21 C22 -177.33(17) no . . . . N1 C20 C25 C13 -0.5(3) no . . . . N1 C20 C25 C24 176.62(17) no . . . . C21 C20 C25 C13 -179.96(17) no . . . . C21 C20 C25 C24 -2.8(3) no . . . . C25 C20 C21 C22 2.2(3) no . . . . C20 C21 C22 C23 0.1(4) no . . . . C21 C22 C23 C24 -1.7(4) no . . . . C22 C23 C24 C25 1.0(4) no . . . . C23 C24 C25 C13 178.30(18) no . . . . C23 C24 C25 C20 1.3(3) no . . . . C2 C26 C27 C28 -5.2(3) no . . . . C2 C26 C27 C32 172.89(16) no . . . . C2 C26 C38 C33 -173.18(16) no . . . . C2 C26 C38 C37 8.2(3) no . . . . C27 C26 C38 C33 3.4(3) no . . . . C27 C26 C38 C37 -175.17(17) no . . . . C38 C26 C27 C28 178.31(16) no . . . . C38 C26 C27 C32 -3.6(3) no . . . . C26 C27 C28 C29 -179.28(18) no . . . . C26 C27 C32 N2 0.2(3) no . . . . C26 C27 C32 C31 -179.64(17) no . . . . C28 C27 C32 N2 178.36(17) no . . . . C28 C27 C32 C31 -1.4(3) no . . . . C32 C27 C28 C29 2.6(3) no . . . . C27 C28 C29 C30 -2.2(4) no . . . . C28 C29 C30 C31 0.5(4) no . . . . C29 C30 C31 C32 0.7(4) no . . . . C30 C31 C32 N2 -180.0(2) no . . . . C30 C31 C32 C27 -0.2(4) no . . . . N2 C33 C34 C35 -179.65(18) no . . . . N2 C33 C38 C26 0.3(3) no . . . . N2 C33 C38 C37 178.99(17) no . . . . C34 C33 C38 C26 179.72(17) no . . . . C34 C33 C38 C37 -1.6(3) no . . . . C38 C33 C34 C35 0.9(3) no . . . . C33 C34 C35 C36 0.5(4) no . . . . C34 C35 C36 C37 -1.2(4) no . . . . C35 C36 C37 C38 0.5(4) no . . . . C36 C37 C38 C26 179.53(19) no . . . . C36 C37 C38 C33 0.9(3) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 N1 C13 2.851(3) no . . N2 C26 2.846(3) no . . C1 C15 2.947(3) no . . C1 C24 2.953(3) no . . C1 C27 3.317(3) no . . C1 C28 3.336(3) no . . C2 C14 3.292(3) no . . C2 C15 3.308(3) no . . C2 C28 3.000(3) no . . C2 C37 2.942(3) no . . C3 C6 2.812(3) no . . C3 C10 3.593(3) no . . C3 C37 3.233(3) no . . C3 C38 3.213(3) no . . C4 C7 2.859(3) no . . C4 C26 3.263(3) no . . C4 C37 3.362(3) no . . C4 C38 3.481(3) no . . C5 C12 2.717(3) no . . C7 C10 2.866(3) no . . C8 C11 2.811(3) no . . C9 C12 2.710(3) no . . C10 C13 3.263(3) no . . C10 C24 3.471(3) no . . C10 C25 3.559(3) no . . C11 C24 3.298(3) no . . C11 C25 3.260(3) no . . C13 C26 3.249(3) no . . C13 C27 3.585(3) no . . C13 C28 3.369(3) no . . C14 C17 2.813(3) no . . C14 C20 2.757(3) no . . C14 C26 3.586(3) no . . C15 C18 2.797(3) no . . C15 C26 3.433(3) no . . C16 C19 2.803(3) no . . C19 C21 3.599(3) no . . C19 C25 2.761(3) no . . C20 C23 2.811(3) no . . C21 C24 2.800(3) no . . C22 C25 2.821(3) no . . C25 C28 3.549(3) no . . C27 C30 2.827(3) no . . C27 C33 2.764(3) no . . C28 C31 2.797(3) no . . C29 C32 2.800(3) no . . C31 C33 3.593(3) no . . C32 C38 2.768(3) no . . C33 C36 2.814(4) no . . C34 C37 2.790(3) no . . C35 C38 2.820(3) no . . Cl1 N2 3.4773(19) no . . Cl1 C33 3.410(3) no . . N1 C20 3.594(3) no . 3_667 N1 C22 3.312(3) no . 4_554 N1 C23 3.534(3) no . 4_554 N2 Cl1 3.4773(19) no . . N2 C28 3.408(3) no . 4_554 N2 C29 3.416(3) no . 4_554 N2 C39 3.181(3) no . 4_554 C9 C16 3.515(3) no . 1_556 C16 C9 3.515(3) no . 1_554 C20 N1 3.594(3) no . 3_667 C20 C20 3.583(3) no . 3_667 C22 N1 3.312(3) no . 4_555 C23 N1 3.534(3) no . 4_555 C28 N2 3.408(3) no . 4_555 C28 C31 3.497(3) no . 4_555 C28 C32 3.444(3) no . 4_555 C29 N2 3.416(3) no . 4_555 C29 C32 3.565(3) no . 4_555 C29 C33 3.573(3) no . 4_555 C30 C33 3.516(4) no . 4_555 C30 C34 3.568(4) no . 4_555 C31 C28 3.497(3) no . 4_554 C31 C34 3.596(4) no . 4_555 C32 C28 3.444(3) no . 4_554 C32 C29 3.565(3) no . 4_554 C33 Cl1 3.410(3) no . . C33 C29 3.573(3) no . 4_554 C33 C30 3.516(4) no . 4_554 C34 C30 3.568(4) no . 4_554 C34 C31 3.596(4) no . 4_554 C39 N2 3.181(3) no . 4_555 N1 H18 2.5522 no . . N1 H21 2.5391 no . . N2 H31 2.5412 no . . N2 H34 2.5467 no . . C1 H10 2.9232 no . . C1 H15 2.6249 no . . C1 H24 2.6368 no . . C1 H28 2.7391 no . . C1 H37 3.4789 no . . C2 H4 2.9289 no . . C2 H15 2.7338 no . . C2 H24 3.4944 no . . C2 H28 2.6925 no . . C2 H37 2.6186 no . . C3 H5 3.2531 no . . C3 H37 2.7138 no . . C4 H6 3.3041 no . . C4 H37 3.0029 no . . C6 H4 3.3057 no . . C6 H8 2.7960 no . . C7 H5 3.2710 no . . C7 H9 3.2718 no . . C8 H6 2.7940 no . . C8 H10 3.3074 no . . C10 H8 3.3062 no . . C10 H24 3.0799 no . . C11 H9 3.2443 no . . C11 H15 3.5605 no . . C11 H24 2.7704 no . . C12 H4 3.2667 no . . C12 H6 3.2470 no . . C12 H8 3.2472 no . . C12 H10 3.2641 no . . C13 H10 3.0953 no . . C13 H15 2.6817 no . . C13 H24 2.7040 no . . C13 H28 2.8285 no . . C14 H16 3.2810 no . . C14 H18 3.3219 no . . C15 H17 3.2586 no . . C15 H37 3.4268 no . . C16 H18 3.2643 no . . C17 H15 3.2647 no . . C18 H16 3.2564 no . . C19 H15 3.3091 no . . C19 H17 3.2789 no . . C20 H22 3.2877 no . . C20 H24 3.3207 no . . C21 H23 3.2613 no . . C22 H24 3.2713 no . . C23 H21 3.2688 no . . C24 H10 3.1890 no . . C24 H22 3.2643 no . . C24 H28 2.7375 no . . C25 H10 3.1562 no . . C25 H21 3.3150 no . . C25 H23 3.2889 no . . C25 H28 2.8650 no . . C26 H4 3.0884 no . . C26 H15 2.9708 no . . C26 H28 2.7102 no . . C26 H37 2.6968 no . . C27 H29 3.2854 no . . C27 H31 3.3341 no . . C28 H24 3.4686 no . . C28 H30 3.2536 no . . C29 H31 3.2657 no . . C30 H28 3.2578 no . . C31 H29 3.2581 no . . C32 H28 3.3154 no . . C32 H30 3.2790 no . . C33 H35 3.2833 no . . C33 H37 3.3102 no . . C34 H36 3.2611 no . . C35 H37 3.2685 no . . C36 H34 3.2683 no . . C37 H4 3.0595 no . . C37 H15 2.8625 no . . C37 H35 3.2625 no . . C38 H4 3.0588 no . . C38 H15 3.0685 no . . C38 H34 3.3205 no . . C38 H36 3.2880 no . . H4 H5 2.3637 no . . H4 H37 2.9699 no . . H5 H6 2.3031 no . . H6 H8 2.7005 no . . H8 H9 2.2957 no . . H9 H10 2.3674 no . . H10 H24 3.0538 no . . H15 H16 2.3022 no . . H15 H37 2.5101 no . . H16 H17 2.3505 no . . H17 H18 2.3019 no . . H21 H22 2.3063 no . . H22 H23 2.3604 no . . H23 H24 2.2964 no . . H24 H28 2.5234 no . . H28 H29 2.2867 no . . H29 H30 2.3478 no . . H30 H31 2.3111 no . . H34 H35 2.2925 no . . H35 H36 2.3708 no . . H36 H37 2.2964 no . . Cl1 H4 2.9678 no . . Cl1 H5 3.1873 no . 3_567 Cl1 H34 3.2936 no . 4_555 Cl1 H39 3.3628 no . 4_554 Cl2 H5 2.9702 no . 2_547 Cl2 H5 3.3966 no . 3_567 Cl2 H6 2.9801 no . 2_547 Cl2 H34 3.1250 no . 4_555 Cl2 H35 3.0309 no . 2_546 Cl2 H36 3.0355 no . 2_546 Cl3 H4 3.2691 no . . Cl3 H4 3.5983 no . 3_567 Cl3 H5 3.3903 no . . Cl3 H34 3.3322 no . 1_556 Cl3 H35 3.2448 no . 1_556 N1 H10 2.7411 no . 3_667 N1 H22 2.8722 no . 4_554 N1 H23 3.2626 no . 4_554 N2 H39 2.2089 no . 4_554 C1 H8 3.3986 no . 4_564 C2 H8 3.5415 no . 4_564 C2 H31 3.2781 no . 4_555 C3 H8 3.3841 no . 4_564 C3 H31 2.9306 no . 4_555 C4 H31 3.0020 no . 4_555 C5 H35 3.3657 no . 1_556 C5 H36 3.2031 no . 4_565 C6 H36 3.5714 no . 1_556 C6 H36 2.9285 no . 4_565 C6 H37 3.1111 no . 4_565 C7 H16 3.4141 no . 1_556 C7 H30 3.5123 no . 4_555 C7 H37 3.3518 no . 4_565 C8 H15 3.0607 no . 4_565 C8 H16 2.8041 no . 1_556 C8 H37 3.1907 no . 4_565 C9 H15 3.3349 no . 4_565 C9 H16 2.7895 no . 1_556 C9 H17 3.2862 no . 1_556 C9 H21 3.2006 no . 2_657 C9 H22 3.0965 no . 2_657 C10 H16 3.3667 no . 1_556 C10 H17 3.0357 no . 1_556 C10 H21 3.2735 no . 3_667 C10 H22 3.1569 no . 2_657 C11 H8 3.1193 no . 4_564 C12 H8 3.1293 no . 4_564 C12 H30 3.3009 no . 4_555 C12 H31 3.5329 no . 4_555 C14 H21 3.5273 no . 3_667 C14 H29 3.3840 no . 4_554 C15 H8 3.4996 no . 4_564 C15 H9 3.3777 no . 4_564 C15 H29 3.1651 no . 4_554 C16 H9 3.5701 no . 1_554 C16 H29 3.0396 no . 4_554 C16 H30 3.0209 no . 4_554 C17 H18 2.9918 no . 3_666 C17 H23 3.2062 no . 1_554 C17 H24 3.3437 no . 1_554 C17 H29 3.1243 no . 4_554 C17 H30 3.5277 no . 4_554 C18 H17 3.2275 no . 3_666 C18 H18 3.1559 no . 3_666 C18 H23 3.1767 no . 1_554 C18 H29 3.3524 no . 4_554 C19 H29 3.5071 no . 4_554 C20 H10 3.4737 no . 3_667 C20 H22 3.4838 no . 4_554 C20 H23 3.2358 no . 4_554 C21 H9 2.9250 no . 2_647 C21 H10 3.3383 no . 3_667 C21 H22 3.4008 no . 4_554 C21 H23 3.3402 no . 4_554 C22 H9 3.0420 no . 2_647 C22 H10 3.5361 no . 2_647 C22 H18 3.5990 no . 4_555 C23 H17 3.0989 no . 1_556 C23 H18 3.4319 no . 1_556 C24 H17 3.0165 no . 1_556 C28 H31 3.4646 no . 4_555 C29 H24 3.5115 no . 4_554 C30 H16 3.5376 no . 4_555 C30 H24 3.1372 no . 4_554 C31 H28 3.1156 no . 4_554 C31 H34 3.4023 no . 4_555 C31 H39 3.3746 no . 4_554 C32 H28 3.3434 no . 4_554 C32 H29 3.5816 no . 4_554 C32 H39 3.1180 no . 4_554 C33 H39 2.9695 no . 4_554 C34 H39 3.0976 no . 4_554 C36 H6 3.5478 no . 1_554 C36 H6 3.3484 no . 4_564 C37 H6 3.2676 no . 4_564 C39 H4 3.5612 no . . C39 H34 3.0880 no . 4_555 H4 Cl1 2.9678 no . . H4 Cl3 3.2691 no . . H4 Cl3 3.5983 no . 3_567 H4 C39 3.5612 no . . H4 H31 3.1584 no . 4_555 H5 Cl1 3.1873 no . 3_567 H5 Cl2 2.9702 no . 2_557 H5 Cl2 3.3966 no . 3_567 H5 Cl3 3.3903 no . . H5 H35 3.0449 no . 1_556 H5 H36 3.2520 no . 4_565 H6 Cl2 2.9801 no . 2_557 H6 C36 3.5478 no . 1_556 H6 C36 3.3484 no . 4_565 H6 C37 3.2676 no . 4_565 H6 H35 3.5077 no . 1_556 H6 H36 3.0095 no . 1_556 H6 H36 2.7966 no . 4_565 H6 H37 2.6179 no . 4_565 H8 C1 3.3986 no . 4_565 H8 C2 3.5415 no . 4_565 H8 C3 3.3841 no . 4_565 H8 C11 3.1193 no . 4_565 H8 C12 3.1293 no . 4_565 H8 C15 3.4996 no . 4_565 H8 H15 2.7553 no . 4_565 H8 H16 2.9902 no . 1_556 H8 H37 2.7115 no . 4_565 H9 C15 3.3777 no . 4_565 H9 C16 3.5701 no . 1_556 H9 C21 2.9250 no . 2_657 H9 C22 3.0420 no . 2_657 H9 H15 3.2127 no . 4_565 H9 H16 2.9865 no . 1_556 H9 H17 3.3264 no . 1_556 H9 H21 2.2537 no . 2_657 H9 H22 2.5077 no . 2_657 H10 N1 2.7411 no . 3_667 H10 C20 3.4737 no . 3_667 H10 C21 3.3383 no . 3_667 H10 C22 3.5361 no . 2_657 H10 H17 2.9008 no . 1_556 H10 H18 3.3010 no . 3_667 H10 H21 2.6573 no . 3_667 H10 H22 2.6736 no . 2_657 H15 C8 3.0607 no . 4_564 H15 C9 3.3349 no . 4_564 H15 H8 2.7553 no . 4_564 H15 H9 3.2127 no . 4_564 H16 C7 3.4141 no . 1_554 H16 C8 2.8041 no . 1_554 H16 C9 2.7895 no . 1_554 H16 C10 3.3667 no . 1_554 H16 C30 3.5376 no . 4_554 H16 H8 2.9902 no . 1_554 H16 H9 2.9865 no . 1_554 H16 H29 3.4492 no . 4_554 H16 H30 2.7129 no . 4_554 H17 C9 3.2862 no . 1_554 H17 C10 3.0357 no . 1_554 H17 C18 3.2275 no . 3_666 H17 C23 3.0989 no . 1_554 H17 C24 3.0165 no . 1_554 H17 H9 3.3264 no . 1_554 H17 H10 2.9008 no . 1_554 H17 H18 2.4598 no . 3_666 H17 H23 2.8600 no . 1_554 H17 H24 2.6959 no . 1_554 H17 H29 3.5544 no . 4_554 H17 H30 3.5735 no . 4_554 H18 C17 2.9918 no . 3_666 H18 C18 3.1559 no . 3_666 H18 C22 3.5990 no . 4_554 H18 C23 3.4319 no . 1_554 H18 H10 3.3010 no . 3_667 H18 H17 2.4598 no . 3_666 H18 H18 2.7863 no . 3_666 H18 H22 3.4796 no . 4_554 H18 H23 2.8047 no . 1_554 H21 C9 3.2006 no . 2_647 H21 C10 3.2735 no . 3_667 H21 C14 3.5273 no . 3_667 H21 H9 2.2537 no . 2_647 H21 H10 2.6573 no . 3_667 H21 H22 2.8924 no . 4_554 H21 H23 3.4135 no . 4_554 H22 N1 2.8722 no . 4_555 H22 C9 3.0965 no . 2_647 H22 C10 3.1569 no . 2_647 H22 C20 3.4838 no . 4_555 H22 C21 3.4008 no . 4_555 H22 H9 2.5077 no . 2_647 H22 H10 2.6736 no . 2_647 H22 H18 3.4796 no . 4_555 H22 H21 2.8924 no . 4_555 H23 N1 3.2626 no . 4_555 H23 C17 3.2062 no . 1_556 H23 C18 3.1767 no . 1_556 H23 C20 3.2358 no . 4_555 H23 C21 3.3402 no . 4_555 H23 H17 2.8600 no . 1_556 H23 H18 2.8047 no . 1_556 H23 H21 3.4135 no . 4_555 H23 H29 3.4986 no . 4_555 H24 C17 3.3437 no . 1_556 H24 C29 3.5115 no . 4_555 H24 C30 3.1372 no . 4_555 H24 H17 2.6959 no . 1_556 H24 H30 3.0406 no . 4_555 H28 C31 3.1156 no . 4_555 H28 C32 3.3434 no . 4_555 H28 H31 3.1620 no . 4_555 H29 C14 3.3840 no . 4_555 H29 C15 3.1651 no . 4_555 H29 C16 3.0396 no . 4_555 H29 C17 3.1243 no . 4_555 H29 C18 3.3524 no . 4_555 H29 C19 3.5071 no . 4_555 H29 C32 3.5816 no . 4_555 H29 H16 3.4492 no . 4_555 H29 H17 3.5544 no . 4_555 H29 H23 3.4986 no . 4_554 H30 C7 3.5123 no . 4_554 H30 C12 3.3009 no . 4_554 H30 C16 3.0209 no . 4_555 H30 C17 3.5277 no . 4_555 H30 H16 2.7129 no . 4_555 H30 H17 3.5735 no . 4_555 H30 H24 3.0406 no . 4_554 H31 C2 3.2781 no . 4_554 H31 C3 2.9306 no . 4_554 H31 C4 3.0020 no . 4_554 H31 C12 3.5329 no . 4_554 H31 C28 3.4646 no . 4_554 H31 H4 3.1584 no . 4_554 H31 H28 3.1620 no . 4_554 H31 H34 3.4446 no . 4_555 H31 H39 2.9693 no . 4_554 H34 Cl1 3.2936 no . 4_554 H34 Cl2 3.1250 no . 4_554 H34 Cl3 3.3322 no . 1_554 H34 C31 3.4023 no . 4_554 H34 C39 3.0880 no . 4_554 H34 H31 3.4446 no . 4_554 H34 H39 2.6503 no . 4_554 H35 Cl2 3.0309 no . 2_556 H35 Cl3 3.2448 no . 1_554 H35 C5 3.3657 no . 1_554 H35 H5 3.0449 no . 1_554 H35 H6 3.5077 no . 1_554 H35 H35 3.4424 no . 3_566 H36 Cl2 3.0355 no . 2_556 H36 C5 3.2031 no . 4_564 H36 C6 3.5714 no . 1_554 H36 C6 2.9285 no . 4_564 H36 H5 3.2520 no . 4_564 H36 H6 3.0095 no . 1_554 H36 H6 2.7966 no . 4_564 H37 C6 3.1111 no . 4_564 H37 C7 3.3518 no . 4_564 H37 C8 3.1907 no . 4_564 H37 H6 2.6179 no . 4_564 H37 H8 2.7115 no . 4_564 H39 Cl1 3.3628 no . 4_555 H39 N2 2.2089 no . 4_555 H39 C31 3.3746 no . 4_555 H39 C32 3.1180 no . 4_555 H39 C33 2.9695 no . 4_555 H39 C34 3.0976 no . 4_555 H39 H31 2.9693 no . 4_555 H39 H34 2.6503 no . 4_555 #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 975884' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data__051107tt #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C43 H29 Cl3 F6 N2 O6 S2' _chemical_formula_moiety 'C43 H29 Cl3 F6 N2 O6 S2' _chemical_formula_weight 954.18 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 13.040(3) _cell_length_b 13.546(3) _cell_length_c 13.7353(13) _cell_angle_alpha 67.069(17) _cell_angle_beta 66.224(16) _cell_angle_gamma 81.35(2) _cell_volume 2044.7(7) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4047 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 27.10 _cell_measurement_temperature 153 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972.00 _exptl_absorpt_coefficient_mu 0.406 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.744 _exptl_absorpt_correction_T_max 0.980 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 153 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_reflns_number 16279 _diffrn_reflns_av_R_equivalents 0.1197 _diffrn_reflns_theta_max 25.13 _diffrn_reflns_theta_full 25.13 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measured_fraction_theta_full 0.985 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7202 _reflns_number_gt 2481 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0758 _refine_ls_wR_factor_ref 0.1024 _refine_ls_number_restraints ? _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 7199 _refine_ls_number_parameters 588 _refine_ls_goodness_of_fit_ref 0.911 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[1.0000\s(Fo^2^)]/(4Fo^2^)' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 1.610 _refine_diff_density_min -1.620 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; F F 0.0171 0.0103 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.1246 0.1234 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.1484 0.1585 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Cl(1) Cl 1.1349(2) 0.0600(2) 0.8806(2) 0.0815(10) Uani 1.0 2 d . . . Cl(2) Cl 1.00507(19) 0.20693(19) 0.98911(19) 0.0745(9) Uani 1.0 2 d . . . Cl(3) Cl 1.08749(18) 0.2708(2) 0.74583(18) 0.0763(9) Uani 1.0 2 d . . . S(1) S 0.65411(16) 0.71185(17) 0.02325(18) 0.0452(7) Uani 1.0 2 d . . . S(2) S 0.88176(15) 0.21613(16) 0.53570(16) 0.0378(6) Uani 1.0 2 d . . . F(1) F 0.4508(4) 0.6901(4) 0.1760(4) 0.0713(17) Uani 1.0 2 d . . . F(2) F 0.4880(4) 0.5915(4) 0.0750(5) 0.082(2) Uani 1.0 2 d . . . F(3) F 0.5518(4) 0.5499(4) 0.2073(5) 0.0839(19) Uani 1.0 2 d . . . F(4) F 0.7675(4) 0.3725(4) 0.5945(4) 0.0681(17) Uani 1.0 2 d . . . F(5) F 0.9426(4) 0.3766(4) 0.5606(4) 0.078(2) Uani 1.0 2 d . . . F(6) F 0.8887(5) 0.4229(4) 0.4227(4) 0.084(2) Uani 1.0 2 d . . . O(1) O 0.6937(4) 0.7357(5) 0.0956(5) 0.066(3) Uani 1.0 2 d . . . O(2) O 0.6122(5) 0.8033(4) -0.0476(5) 0.065(2) Uani 1.0 2 d . . . O(3) O 0.7239(4) 0.6397(4) -0.0307(4) 0.0551(19) Uani 1.0 2 d . . . O(4) O 0.9943(4) 0.2120(4) 0.4578(4) 0.0538(18) Uani 1.0 2 d . . . O(5) O 0.7965(4) 0.2078(4) 0.4977(4) 0.0494(18) Uani 1.0 2 d . . . O(6) O 0.8605(4) 0.1554(4) 0.6541(4) 0.0506(17) Uani 1.0 2 d . . . N(1) N 0.6683(5) 0.1033(5) 0.0063(5) 0.0329(19) Uani 1.0 2 d . . . N(2) N 0.9543(5) 0.1780(5) 0.2614(5) 0.0352(19) Uani 1.0 2 d . . . C(1) C 0.6117(5) 0.2574(5) 0.3121(6) 0.028(2) Uani 1.0 2 d . . . C(2) C 0.5484(5) 0.2498(6) 0.2543(6) 0.030(2) Uani 1.0 2 d . . . C(3) C 0.4345(5) 0.2908(6) 0.3018(6) 0.032(3) Uani 1.0 2 d . . . C(4) C 0.3405(6) 0.3018(6) 0.2778(6) 0.037(3) Uani 1.0 2 d . . . C(5) C 0.2463(6) 0.3449(6) 0.3423(6) 0.037(3) Uani 1.0 2 d . . . C(6) C 0.2447(6) 0.3771(6) 0.4269(6) 0.039(3) Uani 1.0 2 d . . . C(7) C 0.3406(6) 0.3665(5) 0.4523(6) 0.034(3) Uani 1.0 2 d . . . C(8) C 0.3567(6) 0.3901(6) 0.5386(7) 0.044(3) Uani 1.0 2 d . . . C(9) C 0.4564(6) 0.3711(6) 0.5509(6) 0.044(3) Uani 1.0 2 d . . . C(10) C 0.5505(6) 0.3275(6) 0.4816(6) 0.039(3) Uani 1.0 2 d . . . C(11) C 0.5382(6) 0.3050(5) 0.3988(6) 0.030(3) Uani 1.0 2 d . . . C(12) C 0.4355(5) 0.3237(5) 0.3874(6) 0.027(2) Uani 1.0 2 d . . . C(13) C 0.7296(6) 0.2311(6) 0.2927(6) 0.030(2) Uani 1.0 2 d . . . C(14) C 0.7613(6) 0.1234(6) 0.3298(5) 0.029(3) Uani 1.0 2 d . . . C(15) C 0.6814(6) 0.0377(6) 0.3846(6) 0.039(3) Uani 1.0 2 d . . . C(16) C 0.7148(7) -0.0683(6) 0.4244(6) 0.050(3) Uani 1.0 2 d . . . C(17) C 0.8304(8) -0.0885(7) 0.4100(7) 0.059(3) Uani 1.0 2 d . . . C(18) C 0.9069(7) -0.0094(7) 0.3588(7) 0.050(3) Uani 1.0 2 d . . . C(19) C 0.8766(6) 0.0972(6) 0.3152(6) 0.032(3) Uani 1.0 2 d . . . C(20) C 0.9249(6) 0.2827(6) 0.2265(6) 0.035(3) Uani 1.0 2 d . . . C(21) C 1.0058(6) 0.3657(6) 0.1731(6) 0.038(3) Uani 1.0 2 d . . . C(22) C 0.9733(6) 0.4704(6) 0.1397(6) 0.043(3) Uani 1.0 2 d . . . C(23) C 0.8590(6) 0.4997(6) 0.1591(6) 0.039(3) Uani 1.0 2 d . . . C(24) C 0.7822(6) 0.4212(6) 0.2082(6) 0.032(3) Uani 1.0 2 d . . . C(25) C 0.8115(5) 0.3108(6) 0.2449(5) 0.026(2) Uani 1.0 2 d . . . C(26) C 1.0743(6) 0.1499(6) 0.2413(7) 0.057(3) Uani 1.0 2 d . . . C(27) C 0.5871(5) 0.2013(6) 0.1656(6) 0.030(3) Uani 1.0 2 d . . . C(28) C 0.5452(6) 0.1010(6) 0.1916(6) 0.032(3) Uani 1.0 2 d . . . C(29) C 0.4598(6) 0.0468(6) 0.2986(6) 0.039(3) Uani 1.0 2 d . . . C(30) C 0.4214(6) -0.0496(7) 0.3221(6) 0.046(3) Uani 1.0 2 d . . . C(31) C 0.4656(6) -0.0993(6) 0.2422(7) 0.051(3) Uani 1.0 2 d . . . C(32) C 0.5472(6) -0.0524(6) 0.1379(7) 0.044(3) Uani 1.0 2 d . . . C(33) C 0.5887(5) 0.0512(6) 0.1082(6) 0.033(3) Uani 1.0 2 d . . . C(34) C 0.7037(5) 0.2051(6) -0.0251(6) 0.031(3) Uani 1.0 2 d . . . C(35) C 0.7786(6) 0.2603(6) -0.1359(6) 0.037(3) Uani 1.0 2 d . . . C(36) C 0.8055(6) 0.3634(6) -0.1645(6) 0.043(3) Uani 1.0 2 d . . . C(37) C 0.7640(5) 0.4181(6) -0.0874(6) 0.032(3) Uani 1.0 2 d . . . C(38) C 0.6961(5) 0.3646(6) 0.0202(6) 0.037(3) Uani 1.0 2 d . . . C(39) C 0.6630(5) 0.2570(6) 0.0558(6) 0.028(2) Uani 1.0 2 d . . . C(40) C 0.7215(6) 0.0477(6) -0.0786(6) 0.056(3) Uani 1.0 2 d . . . C(41) C 0.5288(7) 0.6307(7) 0.1267(8) 0.051(3) Uani 1.0 2 d . . . C(42) C 0.8692(7) 0.3551(7) 0.5247(7) 0.050(3) Uani 1.0 2 d . . . C(43) C 1.1153(6) 0.1940(7) 0.8695(7) 0.059(3) Uani 1.0 2 d . . . H(1) H 0.3393 0.2811 0.2196 0.045(3) Uiso 1.0 2 calc R . . H(2) H 0.1799 0.3533 0.3273 0.044(3) Uiso 1.0 2 calc R . . H(3) H 0.1786 0.4063 0.4685 0.042(3) Uiso 1.0 2 calc R . . H(4) H 0.2964 0.4193 0.5866 0.053(4) Uiso 1.0 2 calc R . . H(5) H 0.4640 0.3886 0.6083 0.054(3) Uiso 1.0 2 calc R . . H(6) H 0.6191 0.3133 0.4934 0.049(3) Uiso 1.0 2 calc R . . H(7) H 0.6056 0.0542 0.3926 0.046(3) Uiso 1.0 2 calc R . . H(8) H 0.6621 -0.1253 0.4597 0.057(3) Uiso 1.0 2 calc R . . H(9) H 0.8525 -0.1608 0.4387 0.071(4) Uiso 1.0 2 calc R . . H(10) H 0.9819 -0.0269 0.3530 0.058(4) Uiso 1.0 2 calc R . . H(11) H 1.0822 0.3485 0.1613 0.047(3) Uiso 1.0 2 calc R . . H(12) H 1.0286 0.5254 0.1019 0.047(3) Uiso 1.0 2 calc R . . H(13) H 0.8377 0.5728 0.1388 0.048(3) Uiso 1.0 2 calc R . . H(14) H 0.7062 0.4391 0.2187 0.039(3) Uiso 1.0 2 calc R . . H(15) H 0.4284 0.0804 0.3533 0.0428 Uiso 1.0 2 calc R . . H(16) H 0.3647 -0.0854 0.3940 0.0501 Uiso 1.0 2 calc R . . H(17) H 0.4386 -0.1681 0.2601 0.0615 Uiso 1.0 2 calc R . . H(18) H 0.5754 -0.0872 0.0842 0.0586 Uiso 1.0 2 calc R . . H(19) H 0.8070 0.2269 -0.1909 0.0480 Uiso 1.0 2 calc R . . H(20) H 0.8559 0.4012 -0.2397 0.0476 Uiso 1.0 2 calc R . . H(21) H 0.7837 0.4907 -0.1102 0.0391 Uiso 1.0 2 calc R . . H(22) H 0.6690 0.3995 0.0739 0.0465 Uiso 1.0 2 calc R . . H(23) H 1.0897 0.0828 0.2317 0.0673 Uiso 1.0 2 calc R . . H(24) H 1.1203 0.2039 0.1744 0.0673 Uiso 1.0 2 calc R . . H(25) H 1.0896 0.1458 0.3048 0.0673 Uiso 1.0 2 calc R . . H(26) H 0.7854 0.0097 -0.0664 0.0689 Uiso 1.0 2 calc R . . H(27) H 0.7439 0.0999 -0.1539 0.0689 Uiso 1.0 2 calc R . . H(28) H 0.6698 -0.0010 -0.0691 0.0688 Uiso 1.0 2 calc R . . H(29) H 1.1823 0.2205 0.8629 0.0752 Uiso 1.0 2 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cl(1) 0.102(2) 0.076(2) 0.0867(19) 0.0189(15) -0.0557(16) -0.0352(16) Cl(2) 0.0873(18) 0.087(2) 0.0549(15) -0.0060(15) -0.0253(13) -0.0308(15) Cl(3) 0.0632(16) 0.092(2) 0.0500(15) 0.0020(14) -0.0122(12) -0.0116(14) S(1) 0.0393(12) 0.0496(15) 0.0533(14) 0.0012(11) -0.0176(11) -0.0257(13) S(2) 0.0398(12) 0.0435(14) 0.0297(12) 0.0045(10) -0.0138(10) -0.0138(11) F(1) 0.038(3) 0.083(4) 0.084(4) 0.018(3) -0.015(3) -0.036(4) F(2) 0.060(4) 0.081(5) 0.138(5) -0.005(3) -0.057(4) -0.050(4) F(3) 0.060(4) 0.070(4) 0.079(4) 0.013(3) -0.024(3) 0.010(4) F(4) 0.070(4) 0.068(4) 0.074(4) 0.029(3) -0.029(3) -0.042(3) F(5) 0.077(4) 0.094(5) 0.086(4) -0.021(3) -0.027(3) -0.051(4) F(6) 0.139(5) 0.047(4) 0.049(4) -0.003(4) -0.036(4) 0.001(3) O(1) 0.057(4) 0.068(5) 0.111(5) 0.009(3) -0.045(4) -0.059(4) O(2) 0.085(5) 0.039(4) 0.061(4) 0.007(4) -0.035(4) -0.004(3) O(3) 0.056(4) 0.056(4) 0.058(4) 0.007(3) -0.017(3) -0.033(4) O(4) 0.033(3) 0.083(5) 0.045(4) 0.016(3) -0.011(3) -0.033(4) O(5) 0.047(4) 0.064(4) 0.054(4) -0.002(3) -0.031(3) -0.025(3) O(6) 0.059(4) 0.050(4) 0.032(4) 0.015(3) -0.018(3) -0.009(3) N(1) 0.035(4) 0.037(4) 0.027(4) 0.004(3) -0.010(3) -0.016(4) N(2) 0.037(4) 0.032(4) 0.038(4) 0.013(4) -0.018(3) -0.015(4) C(1) 0.021(4) 0.024(5) 0.027(4) -0.006(4) -0.002(4) -0.001(4) C(2) 0.023(4) 0.034(5) 0.025(4) 0.004(4) -0.005(4) -0.009(4) C(3) 0.026(4) 0.026(5) 0.034(5) -0.008(4) -0.006(4) -0.002(4) C(4) 0.032(5) 0.041(5) 0.040(5) 0.004(4) -0.012(4) -0.021(4) C(5) 0.031(5) 0.042(5) 0.036(5) 0.001(4) -0.015(4) -0.010(4) C(6) 0.024(4) 0.032(5) 0.049(6) 0.007(4) -0.005(4) -0.014(4) C(7) 0.037(5) 0.018(5) 0.038(5) -0.002(4) -0.006(4) -0.006(4) C(8) 0.037(5) 0.043(6) 0.053(6) 0.008(4) -0.016(4) -0.024(5) C(9) 0.048(5) 0.053(6) 0.035(5) 0.008(5) -0.016(4) -0.022(5) C(10) 0.034(5) 0.044(5) 0.044(5) 0.010(4) -0.017(4) -0.024(5) C(11) 0.032(5) 0.024(5) 0.035(5) 0.003(4) -0.014(4) -0.012(4) C(12) 0.025(4) 0.025(5) 0.031(5) -0.004(4) -0.009(4) -0.009(4) C(13) 0.034(5) 0.030(5) 0.024(4) 0.009(4) -0.014(4) -0.006(4) C(14) 0.033(5) 0.037(5) 0.017(4) 0.004(4) -0.009(4) -0.012(4) C(15) 0.044(5) 0.034(5) 0.038(5) 0.001(4) -0.019(4) -0.010(4) C(16) 0.065(6) 0.036(6) 0.041(5) -0.015(5) -0.012(5) -0.009(5) C(17) 0.078(7) 0.049(7) 0.051(6) 0.030(6) -0.039(5) -0.013(5) C(18) 0.044(5) 0.058(7) 0.043(6) 0.009(5) -0.016(5) -0.018(5) C(19) 0.038(5) 0.032(5) 0.030(5) 0.007(4) -0.018(4) -0.012(4) C(20) 0.038(5) 0.037(5) 0.036(5) 0.006(4) -0.017(4) -0.016(4) C(21) 0.033(5) 0.048(6) 0.037(5) -0.002(4) -0.010(4) -0.020(5) C(22) 0.033(5) 0.046(6) 0.038(5) -0.019(4) -0.006(4) -0.003(5) C(23) 0.032(5) 0.040(6) 0.047(5) -0.002(4) -0.021(4) -0.010(5) C(24) 0.026(4) 0.041(5) 0.031(5) -0.004(4) -0.013(4) -0.010(4) C(25) 0.027(4) 0.025(5) 0.021(4) -0.000(4) -0.008(3) -0.005(4) C(26) 0.047(5) 0.063(7) 0.058(6) 0.021(5) -0.024(5) -0.022(5) C(27) 0.027(4) 0.029(5) 0.037(5) 0.005(4) -0.018(4) -0.010(4) C(28) 0.038(5) 0.035(5) 0.030(5) -0.000(4) -0.022(4) -0.010(4) C(29) 0.047(5) 0.029(5) 0.031(5) -0.001(4) -0.010(4) -0.005(4) C(30) 0.041(5) 0.054(6) 0.031(5) -0.001(5) -0.003(4) -0.013(5) C(31) 0.059(6) 0.036(6) 0.059(6) -0.006(5) -0.026(5) -0.013(5) C(32) 0.058(6) 0.041(6) 0.048(6) 0.006(5) -0.026(5) -0.026(5) C(33) 0.025(4) 0.046(6) 0.033(5) 0.000(4) -0.014(4) -0.015(4) C(34) 0.029(4) 0.034(5) 0.027(5) 0.007(4) -0.014(4) -0.007(4) C(35) 0.037(5) 0.039(5) 0.044(5) 0.006(4) -0.025(4) -0.018(4) C(36) 0.025(4) 0.061(6) 0.032(5) -0.001(4) -0.004(4) -0.014(5) C(37) 0.030(4) 0.037(5) 0.031(5) -0.000(4) -0.016(4) -0.011(4) C(38) 0.034(5) 0.042(5) 0.041(5) -0.001(4) -0.019(4) -0.016(4) C(39) 0.018(4) 0.041(5) 0.022(4) -0.003(4) -0.004(3) -0.012(4) C(40) 0.056(6) 0.054(6) 0.062(6) 0.001(5) -0.024(5) -0.023(6) C(41) 0.035(5) 0.049(7) 0.064(7) 0.002(5) -0.019(5) -0.016(6) C(42) 0.064(6) 0.040(6) 0.043(6) -0.003(5) -0.024(5) -0.007(5) C(43) 0.049(5) 0.072(7) 0.068(7) 0.010(5) -0.032(5) -0.030(6) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution SIR97 _computing_structure_refinement 'CRYSTALS (Carruthers, et al., 1999)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cl(1) C(43) 1.749(10) yes . . Cl(2) C(43) 1.744(8) yes . . Cl(3) C(43) 1.763(9) yes . . S(1) O(1) 1.439(9) yes . . S(1) O(2) 1.437(6) yes . . S(1) O(3) 1.444(6) yes . . S(1) C(41) 1.830(8) yes . . S(2) O(4) 1.434(5) yes . . S(2) O(5) 1.440(7) yes . . S(2) O(6) 1.435(5) yes . . S(2) C(42) 1.817(10) yes . . F(1) C(41) 1.328(10) yes . . F(2) C(41) 1.323(14) yes . . F(3) C(41) 1.319(10) yes . . F(4) C(42) 1.338(9) yes . . F(5) C(42) 1.350(13) yes . . F(6) C(42) 1.284(9) yes . . N(1) C(33) 1.347(7) yes . . N(1) C(34) 1.367(10) yes . . N(1) C(40) 1.510(11) yes . . N(2) C(19) 1.368(10) yes . . N(2) C(20) 1.357(9) yes . . N(2) C(26) 1.492(9) yes . . C(1) C(2) 1.391(12) yes . . C(1) C(11) 1.499(10) yes . . C(1) C(13) 1.464(10) yes . . C(2) C(3) 1.482(9) yes . . C(2) C(27) 1.484(12) yes . . C(3) C(4) 1.367(12) yes . . C(3) C(12) 1.414(13) yes . . C(4) C(5) 1.394(9) yes . . C(5) C(6) 1.383(13) yes . . C(6) C(7) 1.402(12) yes . . C(7) C(8) 1.438(14) yes . . C(7) C(12) 1.399(9) yes . . C(8) C(9) 1.352(12) yes . . C(9) C(10) 1.428(10) yes . . C(10) C(11) 1.358(13) yes . . C(11) C(12) 1.386(11) yes . . C(13) C(14) 1.403(10) yes . . C(13) C(25) 1.402(10) yes . . C(14) C(15) 1.431(10) yes . . C(14) C(19) 1.442(10) yes . . C(15) C(16) 1.394(11) yes . . C(16) C(17) 1.437(13) yes . . C(17) C(18) 1.344(13) yes . . C(18) C(19) 1.395(11) yes . . C(20) C(21) 1.416(11) yes . . C(20) C(25) 1.414(10) yes . . C(21) C(22) 1.369(11) yes . . C(22) C(23) 1.425(10) yes . . C(23) C(24) 1.343(10) yes . . C(24) C(25) 1.427(10) yes . . C(27) C(28) 1.399(11) yes . . C(27) C(39) 1.399(8) yes . . C(28) C(29) 1.422(8) yes . . C(28) C(33) 1.432(12) yes . . C(29) C(30) 1.341(12) yes . . C(30) C(31) 1.393(13) yes . . C(31) C(32) 1.362(9) yes . . C(32) C(33) 1.426(12) yes . . C(34) C(35) 1.401(8) yes . . C(34) C(39) 1.426(12) yes . . C(35) C(36) 1.355(12) yes . . C(36) C(37) 1.412(13) yes . . C(37) C(38) 1.340(8) yes . . C(38) C(39) 1.419(11) yes . . C(4) H(1) 0.950 no . . C(5) H(2) 0.950 no . . C(6) H(3) 0.950 no . . C(8) H(4) 0.950 no . . C(9) H(5) 0.950 no . . C(10) H(6) 0.950 no . . C(15) H(7) 0.950 no . . C(16) H(8) 0.950 no . . C(17) H(9) 0.950 no . . C(18) H(10) 0.950 no . . C(21) H(11) 0.950 no . . C(22) H(12) 0.950 no . . C(23) H(13) 0.950 no . . C(24) H(14) 0.950 no . . C(26) H(23) 0.950 no . . C(26) H(24) 0.950 no . . C(26) H(25) 0.950 no . . C(29) H(15) 0.950 no . . C(30) H(16) 0.950 no . . C(31) H(17) 0.950 no . . C(32) H(18) 0.950 no . . C(35) H(19) 0.950 no . . C(36) H(20) 0.950 no . . C(37) H(21) 0.950 no . . C(38) H(22) 0.950 no . . C(40) H(26) 0.950 no . . C(40) H(27) 0.950 no . . C(40) H(28) 0.950 no . . C(43) H(29) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(1) S(1) O(2) 114.1(4) yes . . . O(1) S(1) O(3) 114.9(4) yes . . . O(1) S(1) C(41) 102.2(5) yes . . . O(2) S(1) O(3) 116.3(4) yes . . . O(2) S(1) C(41) 104.0(4) yes . . . O(3) S(1) C(41) 102.9(4) yes . . . O(4) S(2) O(5) 114.4(4) yes . . . O(4) S(2) O(6) 115.7(3) yes . . . O(4) S(2) C(42) 102.6(4) yes . . . O(5) S(2) O(6) 115.2(3) yes . . . O(5) S(2) C(42) 101.9(4) yes . . . O(6) S(2) C(42) 104.6(4) yes . . . C(33) N(1) C(34) 123.2(7) yes . . . C(33) N(1) C(40) 119.1(7) yes . . . C(34) N(1) C(40) 117.7(5) yes . . . C(19) N(2) C(20) 121.8(6) yes . . . C(19) N(2) C(26) 118.9(6) yes . . . C(20) N(2) C(26) 119.3(6) yes . . . C(2) C(1) C(11) 107.4(6) yes . . . C(2) C(1) C(13) 129.0(7) yes . . . C(11) C(1) C(13) 123.5(8) yes . . . C(1) C(2) C(3) 108.8(7) yes . . . C(1) C(2) C(27) 125.2(6) yes . . . C(3) C(2) C(27) 125.9(8) yes . . . C(2) C(3) C(4) 133.5(8) yes . . . C(2) C(3) C(12) 105.6(7) yes . . . C(4) C(3) C(12) 120.9(6) yes . . . C(3) C(4) C(5) 117.0(9) yes . . . C(4) C(5) C(6) 123.4(8) yes . . . C(5) C(6) C(7) 120.2(7) yes . . . C(6) C(7) C(8) 129.8(7) yes . . . C(6) C(7) C(12) 116.6(8) yes . . . C(8) C(7) C(12) 113.6(7) yes . . . C(7) C(8) C(9) 120.4(7) yes . . . C(8) C(9) C(10) 123.4(9) yes . . . C(9) C(10) C(11) 117.6(8) yes . . . C(1) C(11) C(10) 134.8(7) yes . . . C(1) C(11) C(12) 106.4(8) yes . . . C(10) C(11) C(12) 118.7(7) yes . . . C(3) C(12) C(7) 122.0(7) yes . . . C(3) C(12) C(11) 111.7(6) yes . . . C(7) C(12) C(11) 126.3(9) yes . . . C(1) C(13) C(14) 119.5(6) yes . . . C(1) C(13) C(25) 121.9(6) yes . . . C(14) C(13) C(25) 118.5(7) yes . . . C(13) C(14) C(15) 121.7(7) yes . . . C(13) C(14) C(19) 119.7(7) yes . . . C(15) C(14) C(19) 118.5(6) yes . . . C(14) C(15) C(16) 120.3(7) yes . . . C(15) C(16) C(17) 118.2(8) yes . . . C(16) C(17) C(18) 122.5(8) yes . . . C(17) C(18) C(19) 120.6(8) yes . . . N(2) C(19) C(14) 119.3(6) yes . . . N(2) C(19) C(18) 120.9(7) yes . . . C(14) C(19) C(18) 119.8(7) yes . . . N(2) C(20) C(21) 121.2(7) yes . . . N(2) C(20) C(25) 120.1(7) yes . . . C(21) C(20) C(25) 118.6(7) yes . . . C(20) C(21) C(22) 119.8(7) yes . . . C(21) C(22) C(23) 122.1(7) yes . . . C(22) C(23) C(24) 118.4(7) yes . . . C(23) C(24) C(25) 121.8(7) yes . . . C(13) C(25) C(20) 120.4(6) yes . . . C(13) C(25) C(24) 120.2(6) yes . . . C(20) C(25) C(24) 119.3(6) yes . . . C(2) C(27) C(28) 119.6(5) yes . . . C(2) C(27) C(39) 119.9(7) yes . . . C(28) C(27) C(39) 120.5(8) yes . . . C(27) C(28) C(29) 122.0(8) yes . . . C(27) C(28) C(33) 119.3(6) yes . . . C(29) C(28) C(33) 118.7(7) yes . . . C(28) C(29) C(30) 121.0(8) yes . . . C(29) C(30) C(31) 120.4(6) yes . . . C(30) C(31) C(32) 122.0(8) yes . . . C(31) C(32) C(33) 119.5(9) yes . . . N(1) C(33) C(28) 118.7(7) yes . . . N(1) C(33) C(32) 122.9(8) yes . . . C(28) C(33) C(32) 118.3(6) yes . . . N(1) C(34) C(35) 121.4(8) yes . . . N(1) C(34) C(39) 119.6(5) yes . . . C(35) C(34) C(39) 119.1(7) yes . . . C(34) C(35) C(36) 118.9(8) yes . . . C(35) C(36) C(37) 123.4(6) yes . . . C(36) C(37) C(38) 118.2(7) yes . . . C(37) C(38) C(39) 121.5(8) yes . . . C(27) C(39) C(34) 118.3(7) yes . . . C(27) C(39) C(38) 122.7(8) yes . . . C(34) C(39) C(38) 118.9(6) yes . . . S(1) C(41) F(1) 110.1(6) yes . . . S(1) C(41) F(2) 110.2(6) yes . . . S(1) C(41) F(3) 111.1(6) yes . . . F(1) C(41) F(2) 108.8(7) yes . . . F(1) C(41) F(3) 108.2(8) yes . . . F(2) C(41) F(3) 108.4(8) yes . . . S(2) C(42) F(4) 110.2(6) yes . . . S(2) C(42) F(5) 109.9(6) yes . . . S(2) C(42) F(6) 113.8(8) yes . . . F(4) C(42) F(5) 105.8(8) yes . . . F(4) C(42) F(6) 109.6(7) yes . . . F(5) C(42) F(6) 107.1(7) yes . . . Cl(1) C(43) Cl(2) 111.3(4) yes . . . Cl(1) C(43) Cl(3) 109.6(6) yes . . . Cl(2) C(43) Cl(3) 109.5(5) yes . . . C(3) C(4) H(1) 121.558 no . . . C(5) C(4) H(1) 121.448 no . . . C(4) C(5) H(2) 118.607 no . . . C(6) C(5) H(2) 118.036 no . . . C(5) C(6) H(3) 120.377 no . . . C(7) C(6) H(3) 119.396 no . . . C(7) C(8) H(4) 118.996 no . . . C(9) C(8) H(4) 120.564 no . . . C(8) C(9) H(5) 117.914 no . . . C(10) C(9) H(5) 118.685 no . . . C(9) C(10) H(6) 121.675 no . . . C(11) C(10) H(6) 120.729 no . . . C(14) C(15) H(7) 119.038 no . . . C(16) C(15) H(7) 120.637 no . . . C(15) C(16) H(8) 120.430 no . . . C(17) C(16) H(8) 121.335 no . . . C(16) C(17) H(9) 117.966 no . . . C(18) C(17) H(9) 119.547 no . . . C(17) C(18) H(10) 119.141 no . . . C(19) C(18) H(10) 120.289 no . . . C(20) C(21) H(11) 119.935 no . . . C(22) C(21) H(11) 120.308 no . . . C(21) C(22) H(12) 119.008 no . . . C(23) C(22) H(12) 118.936 no . . . C(22) C(23) H(13) 120.736 no . . . C(24) C(23) H(13) 120.865 no . . . C(23) C(24) H(14) 119.646 no . . . C(25) C(24) H(14) 118.519 no . . . N(2) C(26) H(23) 109.887 no . . . N(2) C(26) H(24) 109.022 no . . . N(2) C(26) H(25) 109.501 no . . . H(23) C(26) H(24) 109.477 no . . . H(23) C(26) H(25) 109.472 no . . . H(24) C(26) H(25) 109.467 no . . . C(28) C(29) H(15) 119.261 no . . . C(30) C(29) H(15) 119.711 no . . . C(29) C(30) H(16) 120.484 no . . . C(31) C(30) H(16) 119.109 no . . . C(30) C(31) H(17) 119.772 no . . . C(32) C(31) H(17) 118.263 no . . . C(31) C(32) H(18) 120.618 no . . . C(33) C(32) H(18) 119.825 no . . . C(34) C(35) H(19) 120.299 no . . . C(36) C(35) H(19) 120.737 no . . . C(35) C(36) H(20) 119.119 no . . . C(37) C(36) H(20) 117.490 no . . . C(36) C(37) H(21) 121.498 no . . . C(38) C(37) H(21) 120.261 no . . . C(37) C(38) H(22) 119.461 no . . . C(39) C(38) H(22) 119.080 no . . . N(1) C(40) H(26) 108.811 no . . . N(1) C(40) H(27) 109.260 no . . . N(1) C(40) H(28) 110.337 no . . . H(26) C(40) H(27) 109.476 no . . . H(26) C(40) H(28) 109.468 no . . . H(27) C(40) H(28) 109.472 no . . . Cl(1) C(43) H(29) 108.834 no . . . Cl(2) C(43) H(29) 109.109 no . . . Cl(3) C(43) H(29) 108.445 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O(1) S(1) C(41) F(1) 66.8(7) no . . . . O(1) S(1) C(41) F(2) -173.1(5) no . . . . O(1) S(1) C(41) F(3) -53.0(8) no . . . . O(2) S(1) C(41) F(1) -52.1(8) no . . . . O(2) S(1) C(41) F(2) 67.9(6) no . . . . O(2) S(1) C(41) F(3) -171.9(7) no . . . . O(3) S(1) C(41) F(1) -173.8(6) no . . . . O(3) S(1) C(41) F(2) -53.7(6) no . . . . O(3) S(1) C(41) F(3) 66.4(8) no . . . . O(4) S(2) C(42) F(4) -179.3(6) no . . . . O(4) S(2) C(42) F(5) -63.0(6) no . . . . O(4) S(2) C(42) F(6) 57.1(7) no . . . . O(5) S(2) C(42) F(4) 62.1(7) no . . . . O(5) S(2) C(42) F(5) 178.4(4) no . . . . O(5) S(2) C(42) F(6) -61.5(7) no . . . . O(6) S(2) C(42) F(4) -58.1(7) no . . . . O(6) S(2) C(42) F(5) 58.1(5) no . . . . O(6) S(2) C(42) F(6) 178.2(6) no . . . . C(33) N(1) C(34) C(35) -173.6(6) no . . . . C(33) N(1) C(34) C(39) 5.8(11) no . . . . C(34) N(1) C(33) C(28) -5.3(11) no . . . . C(34) N(1) C(33) C(32) 176.0(6) no . . . . C(40) N(1) C(33) C(28) 175.0(6) no . . . . C(40) N(1) C(33) C(32) -3.7(10) no . . . . C(40) N(1) C(34) C(35) 6.0(10) no . . . . C(40) N(1) C(34) C(39) -174.5(6) no . . . . C(19) N(2) C(20) C(21) 178.6(7) no . . . . C(19) N(2) C(20) C(25) -0.3(12) no . . . . C(20) N(2) C(19) C(14) 3.5(12) no . . . . C(20) N(2) C(19) C(18) -174.7(7) no . . . . C(26) N(2) C(19) C(14) -176.9(7) no . . . . C(26) N(2) C(19) C(18) 5.0(12) no . . . . C(26) N(2) C(20) C(21) -1.0(12) no . . . . C(26) N(2) C(20) C(25) -180.0(7) no . . . . C(2) C(1) C(11) C(10) 176.9(6) no . . . . C(2) C(1) C(11) C(12) -0.3(6) no . . . . C(11) C(1) C(2) C(3) -0.4(6) no . . . . C(11) C(1) C(2) C(27) -176.4(5) no . . . . C(2) C(1) C(13) C(14) -76.2(8) no . . . . C(2) C(1) C(13) C(25) 108.3(9) no . . . . C(13) C(1) C(2) C(3) -177.2(5) no . . . . C(13) C(1) C(2) C(27) 6.8(10) no . . . . C(11) C(1) C(13) C(14) 107.4(8) no . . . . C(11) C(1) C(13) C(25) -68.1(8) no . . . . C(13) C(1) C(11) C(10) -6.1(10) no . . . . C(13) C(1) C(11) C(12) 176.7(5) no . . . . C(1) C(2) C(3) C(4) -179.9(6) no . . . . C(1) C(2) C(3) C(12) 0.9(6) no . . . . C(1) C(2) C(27) C(28) 106.3(7) no . . . . C(1) C(2) C(27) C(39) -75.1(8) no . . . . C(3) C(2) C(27) C(28) -69.0(8) no . . . . C(3) C(2) C(27) C(39) 109.5(7) no . . . . C(27) C(2) C(3) C(4) -4.0(10) no . . . . C(27) C(2) C(3) C(12) 176.9(5) no . . . . C(2) C(3) C(4) C(5) -180.0(6) no . . . . C(2) C(3) C(12) C(7) -179.4(5) no . . . . C(2) C(3) C(12) C(11) -1.2(6) no . . . . C(4) C(3) C(12) C(7) 1.3(9) no . . . . C(4) C(3) C(12) C(11) 179.6(5) no . . . . C(12) C(3) C(4) C(5) -0.9(8) no . . . . C(3) C(4) C(5) C(6) 0.5(9) no . . . . C(4) C(5) C(6) C(7) -0.4(9) no . . . . C(5) C(6) C(7) C(8) -177.2(5) no . . . . C(5) C(6) C(7) C(12) 0.7(8) no . . . . C(6) C(7) C(8) C(9) 178.2(6) no . . . . C(6) C(7) C(12) C(3) -1.1(8) no . . . . C(6) C(7) C(12) C(11) -179.1(5) no . . . . C(8) C(7) C(12) C(3) 177.1(5) no . . . . C(8) C(7) C(12) C(11) -0.9(8) no . . . . C(12) C(7) C(8) C(9) 0.3(8) no . . . . C(7) C(8) C(9) C(10) -0.1(10) no . . . . C(8) C(9) C(10) C(11) 0.5(9) no . . . . C(9) C(10) C(11) C(1) -178.0(6) no . . . . C(9) C(10) C(11) C(12) -1.0(8) no . . . . C(1) C(11) C(12) C(3) 1.0(6) no . . . . C(1) C(11) C(12) C(7) 179.1(5) no . . . . C(10) C(11) C(12) C(3) -176.8(5) no . . . . C(10) C(11) C(12) C(7) 1.4(9) no . . . . C(1) C(13) C(14) C(15) 1.1(12) no . . . . C(1) C(13) C(14) C(19) -177.4(7) no . . . . C(1) C(13) C(25) C(20) -179.5(7) no . . . . C(1) C(13) C(25) C(24) -3.2(11) no . . . . C(14) C(13) C(25) C(20) 4.9(11) no . . . . C(14) C(13) C(25) C(24) -178.8(6) no . . . . C(25) C(13) C(14) C(15) 176.8(7) no . . . . C(25) C(13) C(14) C(19) -1.7(11) no . . . . C(13) C(14) C(15) C(16) -177.5(7) no . . . . C(13) C(14) C(19) N(2) -2.5(12) no . . . . C(13) C(14) C(19) C(18) 175.7(7) no . . . . C(15) C(14) C(19) N(2) 179.0(7) no . . . . C(15) C(14) C(19) C(18) -2.8(12) no . . . . C(19) C(14) C(15) C(16) 1.0(12) no . . . . C(14) C(15) C(16) C(17) 0.8(12) no . . . . C(15) C(16) C(17) C(18) -0.8(14) no . . . . C(16) C(17) C(18) C(19) -1.0(15) no . . . . C(17) C(18) C(19) N(2) -179.0(8) no . . . . C(17) C(18) C(19) C(14) 2.9(14) no . . . . N(2) C(20) C(21) C(22) -179.5(7) no . . . . N(2) C(20) C(25) C(13) -4.0(12) no . . . . N(2) C(20) C(25) C(24) 179.6(7) no . . . . C(21) C(20) C(25) C(13) 177.0(7) no . . . . C(21) C(20) C(25) C(24) 0.7(12) no . . . . C(25) C(20) C(21) C(22) -0.6(12) no . . . . C(20) C(21) C(22) C(23) 1.4(13) no . . . . C(21) C(22) C(23) C(24) -2.3(13) no . . . . C(22) C(23) C(24) C(25) 2.5(12) no . . . . C(23) C(24) C(25) C(13) -178.1(7) no . . . . C(23) C(24) C(25) C(20) -1.7(12) no . . . . C(2) C(27) C(28) C(29) 4.8(11) no . . . . C(2) C(27) C(28) C(33) -175.6(6) no . . . . C(2) C(27) C(39) C(34) 176.1(6) no . . . . C(2) C(27) C(39) C(38) -7.5(10) no . . . . C(28) C(27) C(39) C(34) -5.4(10) no . . . . C(28) C(27) C(39) C(38) 171.0(6) no . . . . C(39) C(27) C(28) C(29) -173.7(6) no . . . . C(39) C(27) C(28) C(33) 5.9(10) no . . . . C(27) C(28) C(29) C(30) -179.5(7) no . . . . C(27) C(28) C(33) N(1) -0.6(11) no . . . . C(27) C(28) C(33) C(32) 178.2(6) no . . . . C(29) C(28) C(33) N(1) 178.9(6) no . . . . C(29) C(28) C(33) C(32) -2.3(10) no . . . . C(33) C(28) C(29) C(30) 1.0(11) no . . . . C(28) C(29) C(30) C(31) 0.6(12) no . . . . C(29) C(30) C(31) C(32) -0.9(13) no . . . . C(30) C(31) C(32) C(33) -0.5(13) no . . . . C(31) C(32) C(33) N(1) -179.2(7) no . . . . C(31) C(32) C(33) C(28) 2.1(12) no . . . . N(1) C(34) C(35) C(36) 175.9(6) no . . . . N(1) C(34) C(39) C(27) -0.3(10) no . . . . N(1) C(34) C(39) C(38) -176.8(6) no . . . . C(35) C(34) C(39) C(27) 179.2(6) no . . . . C(35) C(34) C(39) C(38) 2.6(10) no . . . . C(39) C(34) C(35) C(36) -3.5(11) no . . . . C(34) C(35) C(36) C(37) 1.6(12) no . . . . C(35) C(36) C(37) C(38) 1.2(11) no . . . . C(36) C(37) C(38) C(39) -2.2(11) no . . . . C(37) C(38) C(39) C(27) -176.1(7) no . . . . C(37) C(38) C(39) C(34) 0.3(11) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Cl(1) N(1) 3.566(7) no . 2_756 Cl(2) N(2) 3.394(8) no . 1_556 Cl(2) C(20) 3.509(10) no . 1_556 Cl(3) F(5) 3.509(7) no . . Cl(3) C(36) 3.574(7) no . 1_556 F(1) F(4) 3.189(6) no . 2_666 F(1) N(1) 3.589(8) no . 2_665 F(1) C(31) 3.365(12) no . 1_565 F(1) C(34) 3.253(10) no . 2_665 F(1) C(35) 3.185(10) no . 2_665 F(2) C(34) 3.485(8) no . 2_665 F(2) C(36) 3.552(8) no . 2_665 F(2) C(37) 3.240(9) no . 2_665 F(2) C(38) 3.053(11) no . 2_665 F(2) C(39) 3.175(9) no . 2_665 F(3) C(3) 3.578(9) no . . F(3) C(11) 3.310(8) no . . F(3) C(12) 3.205(7) no . . F(3) C(24) 3.241(9) no . . F(4) F(1) 3.189(6) no . 2_666 F(4) C(6) 3.274(9) no . 2_666 F(4) C(7) 3.516(8) no . 2_666 F(4) C(8) 3.542(9) no . 2_666 F(4) C(35) 3.468(10) no . 1_556 F(4) C(36) 3.493(11) no . 1_556 F(5) Cl(3) 3.509(7) no . . F(5) F(5) 3.369(8) no . 2_766 F(5) C(36) 3.407(10) no . 1_556 F(6) C(21) 3.490(10) no . . F(6) C(22) 3.398(9) no . . F(6) C(23) 3.523(11) no . . O(1) C(23) 3.592(9) no . . O(1) C(32) 3.314(10) no . 1_565 O(1) C(43) 3.061(13) no . 2_766 O(2) N(1) 3.577(8) no . 2_665 O(2) C(27) 3.592(12) no . 2_665 O(2) C(28) 3.207(11) no . 2_665 O(2) C(32) 3.560(12) no . 1_565 O(2) C(33) 3.220(9) no . 2_665 O(3) C(4) 3.585(11) no . 2_665 O(3) C(21) 3.275(8) no . 2_765 O(3) C(23) 3.514(10) no . . O(3) C(37) 3.304(11) no . . O(3) C(38) 3.561(10) no . . O(4) N(2) 3.152(10) no . . O(4) C(5) 3.451(9) no . 1_655 O(4) C(17) 3.340(11) no . 2_756 O(4) C(18) 3.422(10) no . 2_756 O(4) C(20) 3.392(11) no . . O(4) C(21) 3.594(9) no . . O(4) C(26) 3.133(11) no . . O(5) N(2) 3.212(8) no . . O(5) C(10) 3.420(9) no . . O(5) C(13) 3.161(11) no . . O(5) C(14) 3.148(12) no . . O(5) C(19) 3.156(11) no . . O(5) C(20) 3.201(8) no . . O(5) C(25) 3.130(9) no . . O(5) C(30) 3.289(8) no . 2_656 O(6) C(18) 3.344(10) no . 2_756 O(6) C(35) 3.426(11) no . 1_556 O(6) C(40) 3.186(8) no . 1_556 N(1) Cl(1) 3.566(7) no . 2_756 N(1) F(1) 3.589(8) no . 2_665 N(1) O(2) 3.577(8) no . 2_665 N(2) Cl(2) 3.394(8) no . 1_554 N(2) O(4) 3.152(10) no . . N(2) O(5) 3.212(8) no . . C(3) F(3) 3.578(9) no . . C(4) O(3) 3.585(11) no . 2_665 C(5) O(4) 3.451(9) no . 1_455 C(6) F(4) 3.274(9) no . 2_666 C(7) F(4) 3.516(8) no . 2_666 C(8) F(4) 3.542(9) no . 2_666 C(9) C(9) 3.397(11) no . 2_666 C(10) O(5) 3.420(9) no . . C(11) F(3) 3.310(8) no . . C(12) F(3) 3.205(7) no . . C(13) O(5) 3.161(11) no . . C(14) O(5) 3.148(12) no . . C(17) O(4) 3.340(11) no . 2_756 C(18) O(4) 3.422(10) no . 2_756 C(18) O(6) 3.344(10) no . 2_756 C(19) O(5) 3.156(11) no . . C(20) Cl(2) 3.509(10) no . 1_554 C(20) O(4) 3.392(11) no . . C(20) O(5) 3.201(8) no . . C(21) F(6) 3.490(10) no . . C(21) O(3) 3.275(8) no . 2_765 C(21) O(4) 3.594(9) no . . C(22) F(6) 3.398(9) no . . C(22) C(22) 3.388(11) no . 2_765 C(23) F(6) 3.523(11) no . . C(23) O(1) 3.592(9) no . . C(23) O(3) 3.514(10) no . . C(24) F(3) 3.241(9) no . . C(25) O(5) 3.130(9) no . . C(26) O(4) 3.133(11) no . . C(27) O(2) 3.592(12) no . 2_665 C(28) O(2) 3.207(11) no . 2_665 C(30) O(5) 3.289(8) no . 2_656 C(31) F(1) 3.365(12) no . 1_545 C(32) O(1) 3.314(10) no . 1_545 C(32) O(2) 3.560(12) no . 1_545 C(33) O(2) 3.220(9) no . 2_665 C(34) F(1) 3.253(10) no . 2_665 C(34) F(2) 3.485(8) no . 2_665 C(35) F(1) 3.185(10) no . 2_665 C(35) F(4) 3.468(10) no . 1_554 C(35) O(6) 3.426(11) no . 1_554 C(36) Cl(3) 3.574(7) no . 1_554 C(36) F(2) 3.552(8) no . 2_665 C(36) F(4) 3.493(11) no . 1_554 C(36) F(5) 3.407(10) no . 1_554 C(37) F(2) 3.240(9) no . 2_665 C(37) O(3) 3.304(11) no . . C(38) F(2) 3.053(11) no . 2_665 C(38) O(3) 3.561(10) no . . C(39) F(2) 3.175(9) no . 2_665 C(40) O(6) 3.186(8) no . 1_554 C(43) O(1) 3.061(13) no . 2_766 Cl(1) H(26) 2.9079 no . 2_756 Cl(2) H(12) 3.3668 no . 2_766 Cl(2) H(13) 3.3229 no . 2_766 Cl(2) H(24) 3.4235 no . 1_556 Cl(3) H(3) 3.2932 no . 1_655 Cl(3) H(4) 3.1085 no . 1_655 Cl(3) H(9) 3.2029 no . 2_756 Cl(3) H(13) 3.5252 no . 2_766 Cl(3) H(19) 3.4894 no . 1_556 Cl(3) H(20) 3.2349 no . 1_556 S(1) H(1) 3.2662 no . 2_665 S(1) H(11) 3.5572 no . 2_765 S(1) H(13) 3.3427 no . . S(1) H(18) 3.0664 no . 1_565 S(1) H(24) 3.0794 no . 2_765 S(1) H(29) 3.4982 no . 2_766 S(2) H(9) 3.5624 no . 2_756 S(2) H(10) 3.1355 no . 2_756 S(2) H(16) 3.5034 no . 2_656 S(2) H(19) 3.5364 no . 1_556 S(2) H(25) 3.5995 no . . F(1) H(5) 3.3135 no . 2_666 F(1) H(17) 2.5562 no . 1_565 F(1) H(18) 3.1910 no . 1_565 F(1) H(19) 3.3311 no . 2_665 F(1) H(27) 3.5230 no . 2_665 F(2) H(1) 3.5782 no . 2_665 F(2) H(22) 3.2399 no . . F(2) H(22) 3.3906 no . 2_665 F(3) H(5) 2.8843 no . 2_666 F(3) H(13) 3.4886 no . . F(3) H(14) 2.3435 no . . F(3) H(22) 3.0922 no . . F(4) H(3) 2.8893 no . 2_666 F(4) H(4) 3.2144 no . 2_666 F(4) H(6) 3.1336 no . . F(4) H(17) 3.5322 no . 2_656 F(4) H(19) 3.0383 no . 1_556 F(4) H(20) 3.0993 no . 1_556 F(5) H(2) 3.5275 no . 1_655 F(5) H(3) 2.8402 no . 1_655 F(5) H(3) 3.0836 no . 2_666 F(5) H(19) 3.1155 no . 1_556 F(5) H(20) 2.6477 no . 1_556 F(6) H(2) 3.5918 no . 1_655 F(6) H(3) 3.0636 no . 2_666 F(6) H(4) 2.9822 no . 2_666 O(1) H(5) 3.5446 no . 2_666 O(1) H(13) 2.7160 no . . O(1) H(17) 3.5772 no . 1_565 O(1) H(18) 2.6351 no . 1_565 O(1) H(24) 3.3594 no . 2_765 O(1) H(26) 3.5935 no . 1_565 O(1) H(28) 3.4472 no . 1_565 O(1) H(29) 2.1433 no . 2_766 O(2) H(1) 2.8237 no . 2_665 O(2) H(18) 2.6236 no . 1_565 O(2) H(24) 3.2160 no . 2_765 O(2) H(28) 2.7374 no . 1_565 O(3) H(1) 2.8026 no . 2_665 O(3) H(11) 2.4240 no . 2_765 O(3) H(13) 3.0297 no . . O(3) H(14) 3.3864 no . . O(3) H(21) 2.5362 no . . O(3) H(22) 3.0655 no . . O(3) H(24) 2.7045 no . 2_765 O(4) H(2) 2.8207 no . 1_655 O(4) H(9) 2.7571 no . 2_756 O(4) H(10) 2.9112 no . 2_756 O(4) H(11) 3.5101 no . . O(4) H(25) 2.4063 no . . O(5) H(6) 2.5396 no . . O(5) H(16) 2.4462 no . 2_656 O(5) H(17) 3.4107 no . 2_656 O(6) H(9) 3.4356 no . 2_756 O(6) H(10) 2.4808 no . 2_756 O(6) H(16) 3.5836 no . 2_656 O(6) H(17) 3.5885 no . 2_656 O(6) H(19) 2.4836 no . 1_556 O(6) H(23) 3.0886 no . 2_756 O(6) H(26) 3.3523 no . 1_556 O(6) H(27) 2.3240 no . 1_556 O(6) H(28) 3.5798 no . 1_556 C(3) H(8) 3.0233 no . 2_656 C(4) H(8) 3.4530 no . 2_656 C(4) H(9) 3.5903 no . 2_656 C(4) H(21) 3.5236 no . 2_665 C(5) H(8) 3.5938 no . 2_656 C(5) H(9) 2.9875 no . 2_656 C(5) H(20) 3.4564 no . 2_665 C(5) H(21) 3.2385 no . 2_665 C(6) H(8) 3.4167 no . 2_656 C(6) H(9) 2.9355 no . 2_656 C(6) H(20) 3.5871 no . 2_665 C(7) H(8) 3.0101 no . 2_656 C(7) H(9) 3.4885 no . 2_656 C(8) H(5) 3.4802 no . 2_666 C(9) H(5) 3.1766 no . 2_666 C(9) H(17) 3.5139 no . 2_656 C(10) H(5) 3.5522 no . 2_666 C(10) H(16) 3.3106 no . 2_656 C(10) H(17) 3.4085 no . 2_656 C(11) H(8) 3.2647 no . 2_656 C(12) H(8) 2.7799 no . 2_656 C(14) H(16) 3.3272 no . 2_656 C(15) H(15) 3.1010 no . 2_656 C(15) H(16) 3.1580 no . 2_656 C(16) H(15) 2.8182 no . 2_656 C(16) H(16) 3.5992 no . 2_656 C(21) H(21) 3.2326 no . 2_765 C(22) H(12) 3.3073 no . 2_765 C(22) H(21) 3.1281 no . 2_765 C(23) H(12) 3.4179 no . 2_765 C(29) H(8) 3.5586 no . 2_656 C(30) H(6) 3.4494 no . 2_656 C(31) H(6) 3.5127 no . 2_656 C(31) H(27) 3.4091 no . 2_655 C(31) H(28) 3.2808 no . 2_655 C(32) H(28) 3.2299 no . 2_655 C(36) H(2) 3.5992 no . 2_665 C(36) H(12) 3.3437 no . 2_765 C(37) H(2) 3.4302 no . 2_665 C(37) H(11) 3.5801 no . 2_765 C(37) H(12) 2.8306 no . 2_765 C(38) H(12) 3.5678 no . 2_765 C(40) H(23) 3.3197 no . 2_755 C(41) H(5) 3.5847 no . 2_666 C(41) H(14) 3.4174 no . . C(41) H(22) 3.5579 no . . C(42) H(3) 3.2290 no . 2_666 C(42) H(19) 3.3937 no . 1_556 C(42) H(20) 3.4611 no . 1_556 C(43) H(13) 3.2570 no . 2_766 C(43) H(26) 3.5409 no . 2_756 H(1) S(1) 3.2662 no . 2_665 H(1) F(2) 3.5782 no . 2_665 H(1) O(2) 2.8237 no . 2_665 H(1) O(3) 2.8026 no . 2_665 H(1) H(21) 3.3492 no . 2_665 H(1) H(24) 3.5311 no . 1_455 H(1) H(25) 3.5181 no . 1_455 H(2) F(5) 3.5275 no . 1_455 H(2) F(6) 3.5918 no . 1_455 H(2) O(4) 2.8207 no . 1_455 H(2) C(36) 3.5992 no . 2_665 H(2) C(37) 3.4302 no . 2_665 H(2) H(9) 3.1648 no . 2_656 H(2) H(11) 3.0505 no . 1_455 H(2) H(20) 3.0971 no . 2_665 H(2) H(21) 2.7986 no . 2_665 H(2) H(25) 3.3676 no . 1_455 H(3) Cl(3) 3.2932 no . 1_455 H(3) F(4) 2.8893 no . 2_666 H(3) F(5) 2.8402 no . 1_455 H(3) F(5) 3.0836 no . 2_666 H(3) F(6) 3.0636 no . 2_666 H(3) C(42) 3.2290 no . 2_666 H(3) H(9) 3.0878 no . 2_656 H(3) H(20) 3.3588 no . 2_665 H(4) Cl(3) 3.1085 no . 1_455 H(4) F(4) 3.2144 no . 2_666 H(4) F(6) 2.9822 no . 2_666 H(4) H(6) 3.5589 no . 2_666 H(4) H(13) 3.4972 no . 2_666 H(4) H(29) 3.5437 no . 1_455 H(5) F(1) 3.3135 no . 2_666 H(5) F(3) 2.8843 no . 2_666 H(5) O(1) 3.5446 no . 2_666 H(5) C(8) 3.4802 no . 2_666 H(5) C(9) 3.1766 no . 2_666 H(5) C(10) 3.5522 no . 2_666 H(5) C(41) 3.5847 no . 2_666 H(5) H(5) 3.2323 no . 2_666 H(5) H(17) 3.2100 no . 2_656 H(6) F(4) 3.1336 no . . H(6) O(5) 2.5396 no . . H(6) C(30) 3.4494 no . 2_656 H(6) C(31) 3.5127 no . 2_656 H(6) H(4) 3.5589 no . 2_666 H(6) H(16) 2.8832 no . 2_656 H(6) H(17) 3.0177 no . 2_656 H(7) H(7) 3.1205 no . 2_656 H(7) H(8) 3.4685 no . 2_656 H(7) H(15) 3.1206 no . 2_656 H(7) H(16) 3.2945 no . 2_656 H(8) C(3) 3.0233 no . 2_656 H(8) C(4) 3.4530 no . 2_656 H(8) C(5) 3.5938 no . 2_656 H(8) C(6) 3.4167 no . 2_656 H(8) C(7) 3.0101 no . 2_656 H(8) C(11) 3.2647 no . 2_656 H(8) C(12) 2.7799 no . 2_656 H(8) C(29) 3.5586 no . 2_656 H(8) H(7) 3.4685 no . 2_656 H(8) H(15) 2.6292 no . 2_656 H(9) Cl(3) 3.2029 no . 2_756 H(9) S(2) 3.5624 no . 2_756 H(9) O(4) 2.7571 no . 2_756 H(9) O(6) 3.4356 no . 2_756 H(9) C(4) 3.5903 no . 2_656 H(9) C(5) 2.9875 no . 2_656 H(9) C(6) 2.9355 no . 2_656 H(9) C(7) 3.4885 no . 2_656 H(9) H(2) 3.1648 no . 2_656 H(9) H(3) 3.0878 no . 2_656 H(10) S(2) 3.1355 no . 2_756 H(10) O(4) 2.9112 no . 2_756 H(10) O(6) 2.4808 no . 2_756 H(11) S(1) 3.5572 no . 2_765 H(11) O(3) 2.4240 no . 2_765 H(11) O(4) 3.5101 no . . H(11) C(37) 3.5801 no . 2_765 H(11) H(2) 3.0505 no . 1_655 H(11) H(13) 3.5580 no . 2_765 H(11) H(21) 2.6947 no . 2_765 H(12) Cl(2) 3.3668 no . 2_766 H(12) C(22) 3.3073 no . 2_765 H(12) C(23) 3.4179 no . 2_765 H(12) C(36) 3.3437 no . 2_765 H(12) C(37) 2.8306 no . 2_765 H(12) C(38) 3.5678 no . 2_765 H(12) H(12) 3.4938 no . 2_765 H(12) H(20) 3.3251 no . 2_765 H(12) H(21) 2.4694 no . 2_765 H(13) Cl(2) 3.3229 no . 2_766 H(13) Cl(3) 3.5252 no . 2_766 H(13) S(1) 3.3427 no . . H(13) F(3) 3.4886 no . . H(13) O(1) 2.7160 no . . H(13) O(3) 3.0297 no . . H(13) C(43) 3.2570 no . 2_766 H(13) H(4) 3.4972 no . 2_666 H(13) H(11) 3.5580 no . 2_765 H(13) H(29) 2.7646 no . 2_766 H(14) F(3) 2.3435 no . . H(14) O(3) 3.3864 no . . H(14) C(41) 3.4174 no . . H(15) C(15) 3.1010 no . 2_656 H(15) C(16) 2.8182 no . 2_656 H(15) H(7) 3.1206 no . 2_656 H(15) H(8) 2.6292 no . 2_656 H(16) S(2) 3.5034 no . 2_656 H(16) O(5) 2.4462 no . 2_656 H(16) O(6) 3.5836 no . 2_656 H(16) C(10) 3.3106 no . 2_656 H(16) C(14) 3.3272 no . 2_656 H(16) C(15) 3.1580 no . 2_656 H(16) C(16) 3.5992 no . 2_656 H(16) H(6) 2.8832 no . 2_656 H(16) H(7) 3.2945 no . 2_656 H(17) F(1) 2.5562 no . 1_545 H(17) F(4) 3.5322 no . 2_656 H(17) O(1) 3.5772 no . 1_545 H(17) O(5) 3.4107 no . 2_656 H(17) O(6) 3.5885 no . 2_656 H(17) C(9) 3.5139 no . 2_656 H(17) C(10) 3.4085 no . 2_656 H(17) H(5) 3.2100 no . 2_656 H(17) H(6) 3.0177 no . 2_656 H(17) H(27) 3.1199 no . 2_655 H(17) H(28) 3.3851 no . 2_655 H(18) S(1) 3.0664 no . 1_545 H(18) F(1) 3.1910 no . 1_545 H(18) O(1) 2.6351 no . 1_545 H(18) O(2) 2.6236 no . 1_545 H(18) H(18) 3.5804 no . 2_655 H(18) H(28) 3.3001 no . 2_655 H(18) H(29) 3.5891 no . 2_756 H(19) Cl(3) 3.4894 no . 1_554 H(19) S(2) 3.5364 no . 1_554 H(19) F(1) 3.3311 no . 2_665 H(19) F(4) 3.0383 no . 1_554 H(19) F(5) 3.1155 no . 1_554 H(19) O(6) 2.4836 no . 1_554 H(19) C(42) 3.3937 no . 1_554 H(20) Cl(3) 3.2349 no . 1_554 H(20) F(4) 3.0993 no . 1_554 H(20) F(5) 2.6477 no . 1_554 H(20) C(5) 3.4564 no . 2_665 H(20) C(6) 3.5871 no . 2_665 H(20) C(42) 3.4611 no . 1_554 H(20) H(2) 3.0971 no . 2_665 H(20) H(3) 3.3588 no . 2_665 H(20) H(12) 3.3251 no . 2_765 H(21) O(3) 2.5362 no . . H(21) C(4) 3.5236 no . 2_665 H(21) C(5) 3.2385 no . 2_665 H(21) C(21) 3.2326 no . 2_765 H(21) C(22) 3.1281 no . 2_765 H(21) H(1) 3.3492 no . 2_665 H(21) H(2) 2.7986 no . 2_665 H(21) H(11) 2.6947 no . 2_765 H(21) H(12) 2.4694 no . 2_765 H(22) F(2) 3.2399 no . . H(22) F(2) 3.3906 no . 2_665 H(22) F(3) 3.0922 no . . H(22) O(3) 3.0655 no . . H(22) C(41) 3.5579 no . . H(23) O(6) 3.0886 no . 2_756 H(23) C(40) 3.3197 no . 2_755 H(23) H(26) 2.8275 no . 2_755 H(23) H(27) 3.2475 no . 2_755 H(23) H(28) 3.3594 no . 2_755 H(24) Cl(2) 3.4235 no . 1_554 H(24) S(1) 3.0794 no . 2_765 H(24) O(1) 3.3594 no . 2_765 H(24) O(2) 3.2160 no . 2_765 H(24) O(3) 2.7045 no . 2_765 H(24) H(1) 3.5311 no . 1_655 H(24) H(26) 3.5898 no . 2_755 H(25) S(2) 3.5995 no . . H(25) O(4) 2.4063 no . . H(25) H(1) 3.5181 no . 1_655 H(25) H(2) 3.3676 no . 1_655 H(26) Cl(1) 2.9079 no . 2_756 H(26) O(1) 3.5935 no . 1_545 H(26) O(6) 3.3523 no . 1_554 H(26) C(43) 3.5409 no . 2_756 H(26) H(23) 2.8275 no . 2_755 H(26) H(24) 3.5898 no . 2_755 H(26) H(29) 3.3881 no . 2_756 H(27) F(1) 3.5230 no . 2_665 H(27) O(6) 2.3240 no . 1_554 H(27) C(31) 3.4091 no . 2_655 H(27) H(17) 3.1199 no . 2_655 H(27) H(23) 3.2475 no . 2_755 H(28) O(1) 3.4472 no . 1_545 H(28) O(2) 2.7374 no . 1_545 H(28) O(6) 3.5798 no . 1_554 H(28) C(31) 3.2808 no . 2_655 H(28) C(32) 3.2299 no . 2_655 H(28) H(17) 3.3851 no . 2_655 H(28) H(18) 3.3001 no . 2_655 H(28) H(23) 3.3594 no . 2_755 H(29) S(1) 3.4982 no . 2_766 H(29) O(1) 2.1433 no . 2_766 H(29) H(4) 3.5437 no . 1_655 H(29) H(13) 2.7646 no . 2_766 H(29) H(18) 3.5891 no . 2_756 H(29) H(26) 3.3881 no . 2_756 #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 975885' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data__050830tt #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C42 H30 F6 N2 O6 S2' _chemical_formula_moiety 'C42 H30 F6 N2 O6 S2' _chemical_formula_weight 836.82 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 12.972(3) _cell_length_b 13.438(3) _cell_length_c 13.490(3) _cell_angle_alpha 67.715(13) _cell_angle_beta 67.100(12) _cell_angle_gamma 82.254(15) _cell_volume 2004.1(8) _cell_formula_units_Z 2 _cell_measurement_reflns_used 6596 _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 27.10 _cell_measurement_temperature 153 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.550 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 860.00 _exptl_absorpt_coefficient_mu 0.210 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.911 _exptl_absorpt_correction_T_max 0.979 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 153 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_reflns_number 15831 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measured_fraction_theta_full 0.986 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6960 _reflns_number_gt 5178 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1529 _refine_ls_number_restraints ? _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 6960 _refine_ls_number_parameters 581 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0021Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 0.676 _refine_diff_density_min -0.407 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; F F 0.0171 0.0103 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.1246 0.1234 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 S(1) S 0.11289(6) 0.28689(5) 0.46058(6) 0.03246(19) Uani 1.0 2 d . . . S(2) S 0.33919(6) -0.21277(6) 0.97635(6) 0.0360(2) Uani 1.0 2 d . . . F(1) F 0.1078(3) 0.07950(15) 0.57327(17) 0.0847(8) Uani 1.0 2 d . . . F(2) F 0.05327(17) 0.12421(18) 0.43170(18) 0.0733(8) Uani 1.0 2 d . . . F(3) F 0.22669(16) 0.13030(14) 0.39903(16) 0.0604(6) Uani 1.0 2 d . . . F(4) F 0.54883(15) -0.19291(16) 0.83729(18) 0.0665(7) Uani 1.0 2 d . . . F(5) F 0.50319(16) -0.09701(16) 0.94310(19) 0.0662(7) Uani 1.0 2 d . . . F(6) F 0.45373(15) -0.04960(15) 0.79877(16) 0.0618(6) Uani 1.0 2 d . . . O(1) O 0.20061(16) 0.29529(17) 0.49685(17) 0.0459(7) Uani 1.0 2 d . . . O(2) O 0.00219(16) 0.29051(17) 0.54012(17) 0.0467(7) Uani 1.0 2 d . . . O(3) O 0.13144(18) 0.34778(16) 0.34118(16) 0.0481(7) Uani 1.0 2 d . . . O(4) O 0.30437(18) -0.23268(17) 0.8968(2) 0.0536(8) Uani 1.0 2 d . . . O(5) O 0.37516(19) -0.30625(16) 1.05157(18) 0.0522(7) Uani 1.0 2 d . . . O(6) O 0.26839(17) -0.14166(16) 1.03042(18) 0.0474(7) Uani 1.0 2 d . . . N(1) N 0.32626(18) 0.39869(17) 0.99070(18) 0.0314(7) Uani 1.0 2 d . . . N(2) N 0.05290(18) 0.32085(18) 0.74021(18) 0.0329(7) Uani 1.0 2 d . . . N(3) N 0.0430(6) 0.3709(7) 0.9593(5) 0.180(3) Uani 1.0 2 d . . . C(1) C 0.4583(2) 0.24663(19) 0.7416(2) 0.0267(7) Uani 1.0 2 d . . . C(2) C 0.3968(2) 0.23781(19) 0.6825(2) 0.0261(7) Uani 1.0 2 d . . . C(3) C 0.4687(2) 0.19341(19) 0.5935(2) 0.0280(7) Uani 1.0 2 d . . . C(4) C 0.4569(3) 0.1722(2) 0.5068(3) 0.0356(8) Uani 1.0 2 d . . . C(5) C 0.5507(3) 0.1318(3) 0.4353(3) 0.0442(9) Uani 1.0 2 d . . . C(6) C 0.6515(3) 0.1123(3) 0.4502(3) 0.0419(9) Uani 1.0 2 d . . . C(7) C 0.6663(3) 0.1338(2) 0.5392(3) 0.0335(8) Uani 1.0 2 d . . . C(8) C 0.7633(3) 0.1218(2) 0.5661(3) 0.0390(8) Uani 1.0 2 d . . . C(9) C 0.7621(3) 0.1507(3) 0.6546(3) 0.0396(8) Uani 1.0 2 d . . . C(10) C 0.6668(2) 0.1927(2) 0.7217(3) 0.0348(8) Uani 1.0 2 d . . . C(11) C 0.5716(2) 0.20540(19) 0.6965(2) 0.0282(7) Uani 1.0 2 d . . . C(12) C 0.5732(2) 0.17420(19) 0.6071(2) 0.0275(7) Uani 1.0 2 d . . . C(13) C 0.4184(2) 0.2953(2) 0.8316(2) 0.0280(7) Uani 1.0 2 d . . . C(14) C 0.3371(2) 0.2426(2) 0.9403(2) 0.0269(7) Uani 1.0 2 d . . . C(15) C 0.3033(2) 0.1347(2) 0.9748(3) 0.0290(7) Uani 1.0 2 d . . . C(16) C 0.2303(2) 0.0824(3) 1.0820(3) 0.0330(8) Uani 1.0 2 d . . . C(17) C 0.1830(3) 0.1373(3) 1.1602(3) 0.0363(8) Uani 1.0 2 d . . . C(18) C 0.2117(3) 0.2412(3) 1.1309(3) 0.0348(8) Uani 1.0 2 d . . . C(19) C 0.2912(2) 0.29657(19) 1.0209(2) 0.0270(7) Uani 1.0 2 d . . . C(20) C 0.4134(3) 0.4479(2) 0.8896(3) 0.0310(8) Uani 1.0 2 d . . . C(21) C 0.4557(3) 0.5495(3) 0.8650(3) 0.0433(9) Uani 1.0 2 d . . . C(22) C 0.5409(3) 0.5959(3) 0.7631(3) 0.0498(10) Uani 1.0 2 d . . . C(23) C 0.5892(3) 0.5461(3) 0.6818(3) 0.0450(9) Uani 1.0 2 d . . . C(24) C 0.5503(3) 0.4478(3) 0.7041(3) 0.0377(8) Uani 1.0 2 d . . . C(25) C 0.4613(2) 0.3954(2) 0.8085(3) 0.0298(7) Uani 1.0 2 d . . . C(26) C 0.2661(3) 0.4595(3) 1.0692(3) 0.0552(11) Uani 1.0 2 d . . . C(27) C 0.2785(2) 0.2673(2) 0.7012(2) 0.0275(7) Uani 1.0 2 d . . . C(28) C 0.1965(2) 0.1868(2) 0.7504(2) 0.0277(7) Uani 1.0 2 d . . . C(29) C 0.2243(3) 0.0756(2) 0.7819(3) 0.0309(8) Uani 1.0 2 d . . . C(30) C 0.1444(3) -0.0022(3) 0.8343(3) 0.0370(8) Uani 1.0 2 d . . . C(31) C 0.0319(3) 0.0265(3) 0.8584(3) 0.0411(9) Uani 1.0 2 d . . . C(32) C 0.0002(3) 0.1316(3) 0.8285(3) 0.0386(8) Uani 1.0 2 d . . . C(33) C 0.0819(3) 0.2143(2) 0.7722(2) 0.0308(8) Uani 1.0 2 d . . . C(34) C 0.1318(3) 0.4013(2) 0.6869(3) 0.0330(8) Uani 1.0 2 d . . . C(35) C 0.1019(3) 0.5106(3) 0.6475(3) 0.0477(10) Uani 1.0 2 d . . . C(36) C 0.1812(3) 0.5893(3) 0.5967(3) 0.0548(11) Uani 1.0 2 d . . . C(37) C 0.2932(3) 0.5656(3) 0.5829(3) 0.0478(9) Uani 1.0 2 d . . . C(38) C 0.3256(3) 0.4618(2) 0.6161(3) 0.0367(8) Uani 1.0 2 d . . . C(39) C 0.2462(3) 0.37571(19) 0.6693(2) 0.0289(7) Uani 1.0 2 d . . . C(40) C -0.0666(3) 0.3487(3) 0.7647(3) 0.0525(11) Uani 1.0 2 d . . . C(41) C 0.1259(3) 0.1494(3) 0.4665(3) 0.0434(9) Uani 1.0 2 d . . . C(42) C 0.4670(3) -0.1347(3) 0.8845(3) 0.0426(9) Uani 1.0 2 d . . . C(43) C -0.1158(5) 0.3310(6) 1.1564(5) 0.140(3) Uani 1.0 2 d . . . C(44) C -0.0274(6) 0.3515(6) 1.0458(6) 0.118(3) Uani 1.0 2 d . . . H(1) H 0.3878 0.1846 0.4954 0.0432 Uiso 1.0 2 calc R . . H(2) H 0.5438 0.1174 0.3744 0.0541 Uiso 1.0 2 calc R . . H(3) H 0.7120 0.0843 0.4010 0.0472 Uiso 1.0 2 calc R . . H(4) H 0.8293 0.0938 0.5232 0.0406 Uiso 1.0 2 calc R . . H(5) H 0.8284 0.1420 0.6710 0.0445 Uiso 1.0 2 calc R . . H(6) H 0.6675 0.2116 0.7825 0.0396 Uiso 1.0 2 calc R . . H(7) H 0.3329 0.0985 0.9213 0.0345 Uiso 1.0 2 calc R . . H(8) H 0.2102 0.0094 1.1048 0.0398 Uiso 1.0 2 calc R . . H(9) H 0.1305 0.1007 1.2350 0.0408 Uiso 1.0 2 calc R . . H(10) H 0.1783 0.2770 1.1844 0.0407 Uiso 1.0 2 calc R . . H(11) H 0.4246 0.5846 0.9194 0.0520 Uiso 1.0 2 calc R . . H(12) H 0.5686 0.6646 0.7469 0.0574 Uiso 1.0 2 calc R . . H(13) H 0.6487 0.5805 0.6116 0.0489 Uiso 1.0 2 calc R . . H(14) H 0.5826 0.4136 0.6491 0.0423 Uiso 1.0 2 calc R . . H(15) H 0.1914 0.4329 1.1123 0.0643 Uiso 1.0 2 calc R . . H(16) H 0.3034 0.4503 1.1203 0.0642 Uiso 1.0 2 calc R . . H(17) H 0.2654 0.5338 1.0249 0.0644 Uiso 1.0 2 calc R . . H(18) H 0.3007 0.0563 0.7654 0.0367 Uiso 1.0 2 calc R . . H(19) H 0.1643 -0.0759 0.8549 0.0437 Uiso 1.0 2 calc R . . H(20) H -0.0241 -0.0284 0.8967 0.0474 Uiso 1.0 2 calc R . . H(21) H -0.0766 0.1491 0.8453 0.0449 Uiso 1.0 2 calc R . . H(22) H 0.0263 0.5286 0.6562 0.0566 Uiso 1.0 2 calc R . . H(23) H 0.1599 0.6622 0.5705 0.0619 Uiso 1.0 2 calc R . . H(24) H 0.3467 0.6221 0.5505 0.0526 Uiso 1.0 2 calc R . . H(25) H 0.4021 0.4455 0.6039 0.0413 Uiso 1.0 2 calc R . . H(26) H -0.1091 0.3134 0.8441 0.0634 Uiso 1.0 2 calc R . . H(27) H -0.0743 0.4243 0.7456 0.0635 Uiso 1.0 2 calc R . . H(28) H -0.0931 0.3266 0.7197 0.0635 Uiso 1.0 2 calc R . . H(29) H -0.1764 0.2948 1.1609 0.1787 Uiso 1.0 2 calc R . . H(30) H -0.0877 0.2872 1.2142 0.1787 Uiso 1.0 2 calc R . . H(31) H -0.1410 0.3970 1.1679 0.1788 Uiso 1.0 2 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S(1) 0.0319(4) 0.0332(4) 0.0296(4) 0.0016(3) -0.0095(3) -0.0107(3) S(2) 0.0369(4) 0.0326(4) 0.0432(5) 0.0027(3) -0.0156(4) -0.0183(4) F(1) 0.147(3) 0.0393(12) 0.0456(13) -0.0088(13) -0.0214(14) -0.0031(10) F(2) 0.0671(14) 0.0876(16) 0.0752(15) -0.0277(12) -0.0088(12) -0.0478(13) F(3) 0.0652(13) 0.0509(12) 0.0613(13) 0.0182(10) -0.0160(11) -0.0293(10) F(4) 0.0388(11) 0.0663(13) 0.0806(15) 0.0171(10) -0.0109(10) -0.0289(12) F(5) 0.0592(13) 0.0614(13) 0.0985(16) -0.0054(10) -0.0463(12) -0.0303(12) F(6) 0.0468(11) 0.0534(12) 0.0580(12) 0.0021(9) -0.0165(10) 0.0053(10) O(1) 0.0399(12) 0.0575(14) 0.0427(12) -0.0114(10) -0.0162(10) -0.0152(11) O(2) 0.0325(11) 0.0650(15) 0.0412(12) 0.0075(10) -0.0069(10) -0.0267(11) O(3) 0.0632(15) 0.0447(13) 0.0302(11) 0.0157(11) -0.0173(10) -0.0119(10) O(4) 0.0565(14) 0.0570(14) 0.0756(16) 0.0094(11) -0.0388(13) -0.0414(13) O(5) 0.0691(16) 0.0349(12) 0.0519(14) 0.0037(11) -0.0276(12) -0.0101(11) O(6) 0.0408(12) 0.0477(13) 0.0533(13) 0.0044(10) -0.0071(10) -0.0294(11) N(1) 0.0370(13) 0.0275(12) 0.0299(13) -0.0010(10) -0.0106(11) -0.0118(10) N(2) 0.0299(12) 0.0375(14) 0.0295(12) 0.0098(10) -0.0099(10) -0.0143(11) N(3) 0.172(6) 0.301(9) 0.097(4) 0.079(6) -0.075(5) -0.101(6) C(1) 0.0279(14) 0.0197(13) 0.0268(13) -0.0040(10) -0.0055(11) -0.0057(11) C(2) 0.0269(14) 0.0194(13) 0.0270(14) -0.0004(10) -0.0063(11) -0.0066(11) C(3) 0.0296(14) 0.0202(13) 0.0286(14) -0.0028(11) -0.0065(12) -0.0061(11) C(4) 0.0372(16) 0.0339(15) 0.0371(16) 0.0017(12) -0.0133(13) -0.0150(13) C(5) 0.054(2) 0.0425(18) 0.0385(17) 0.0046(15) -0.0138(15) -0.0221(15) C(6) 0.0419(18) 0.0365(16) 0.0398(17) 0.0036(13) -0.0022(14) -0.0201(14) C(7) 0.0302(15) 0.0223(14) 0.0371(16) -0.0025(11) -0.0021(12) -0.0088(12) C(8) 0.0263(15) 0.0265(15) 0.0484(18) -0.0010(12) -0.0011(13) -0.0095(14) C(9) 0.0266(15) 0.0331(16) 0.0514(18) -0.0011(12) -0.0107(13) -0.0104(14) C(10) 0.0288(15) 0.0316(15) 0.0382(16) -0.0048(12) -0.0088(13) -0.0084(13) C(11) 0.0273(14) 0.0239(13) 0.0280(14) -0.0039(11) -0.0062(11) -0.0063(11) C(12) 0.0278(14) 0.0188(13) 0.0292(14) -0.0025(10) -0.0048(11) -0.0067(11) C(13) 0.0249(13) 0.0290(14) 0.0306(14) 0.0017(11) -0.0108(12) -0.0110(12) C(14) 0.0253(13) 0.0282(14) 0.0277(14) 0.0015(11) -0.0114(11) -0.0093(12) C(15) 0.0271(14) 0.0300(14) 0.0302(14) -0.0012(11) -0.0106(12) -0.0104(12) C(16) 0.0324(15) 0.0329(15) 0.0345(15) -0.0056(12) -0.0108(13) -0.0123(13) C(17) 0.0365(16) 0.0388(16) 0.0263(15) -0.0097(13) -0.0042(12) -0.0083(13) C(18) 0.0361(16) 0.0371(16) 0.0287(15) -0.0001(12) -0.0072(12) -0.0138(13) C(19) 0.0269(14) 0.0263(14) 0.0298(14) -0.0001(11) -0.0121(12) -0.0103(12) C(20) 0.0376(16) 0.0260(14) 0.0305(15) 0.0002(12) -0.0139(13) -0.0098(12) C(21) 0.057(2) 0.0294(16) 0.0438(18) -0.0050(14) -0.0139(16) -0.0164(14) C(22) 0.061(2) 0.0296(16) 0.052(2) -0.0140(15) -0.0130(17) -0.0114(15) C(23) 0.0458(18) 0.0356(17) 0.0409(18) -0.0151(14) -0.0052(15) -0.0064(14) C(24) 0.0390(16) 0.0320(15) 0.0351(16) -0.0046(13) -0.0063(13) -0.0106(13) C(25) 0.0298(14) 0.0254(14) 0.0336(15) 0.0005(11) -0.0122(12) -0.0093(12) C(26) 0.069(3) 0.0397(18) 0.052(2) -0.0025(16) -0.0049(18) -0.0271(17) C(27) 0.0297(14) 0.0283(14) 0.0207(13) 0.0013(11) -0.0075(11) -0.0071(11) C(28) 0.0280(14) 0.0289(14) 0.0244(13) 0.0005(11) -0.0092(11) -0.0082(12) C(29) 0.0326(15) 0.0271(14) 0.0320(15) 0.0025(11) -0.0150(12) -0.0072(12) C(30) 0.0399(17) 0.0275(15) 0.0415(16) -0.0040(12) -0.0185(14) -0.0049(13) C(31) 0.0349(16) 0.0409(17) 0.0424(17) -0.0102(13) -0.0141(14) -0.0059(14) C(32) 0.0270(15) 0.0469(18) 0.0382(16) 0.0005(13) -0.0114(13) -0.0121(14) C(33) 0.0321(15) 0.0338(15) 0.0251(14) 0.0036(12) -0.0119(12) -0.0088(12) C(34) 0.0401(16) 0.0314(15) 0.0245(14) 0.0072(13) -0.0109(12) -0.0101(12) C(35) 0.056(2) 0.0366(18) 0.0483(19) 0.0174(15) -0.0252(17) -0.0128(15) C(36) 0.076(3) 0.0290(17) 0.050(2) 0.0174(17) -0.0254(19) -0.0073(15) C(37) 0.065(3) 0.0278(16) 0.0382(17) -0.0029(15) -0.0132(16) -0.0041(14) C(38) 0.0444(18) 0.0282(15) 0.0308(15) -0.0009(13) -0.0107(13) -0.0064(12) C(39) 0.0373(15) 0.0235(14) 0.0227(13) 0.0020(11) -0.0106(12) -0.0058(11) C(40) 0.0403(18) 0.058(3) 0.059(3) 0.0176(16) -0.0176(16) -0.0269(18) C(41) 0.0473(19) 0.0409(18) 0.0389(17) -0.0052(14) -0.0107(15) -0.0144(15) C(42) 0.0369(17) 0.0391(17) 0.0530(19) 0.0084(14) -0.0229(15) -0.0138(16) C(43) 0.124(5) 0.214(8) 0.108(5) -0.053(5) -0.026(4) -0.083(5) C(44) 0.127(6) 0.179(7) 0.090(4) 0.023(5) -0.064(4) -0.076(5) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution SIR97 _computing_structure_refinement 'CRYSTALS (Carruthers, et al., 1999)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 S(1) O(1) 1.434(3) yes . . S(1) O(2) 1.4273(19) yes . . S(1) O(3) 1.440(2) yes . . S(1) C(41) 1.806(4) yes . . S(2) O(4) 1.434(4) yes . . S(2) O(5) 1.438(3) yes . . S(2) O(6) 1.435(3) yes . . S(2) C(42) 1.808(3) yes . . F(1) C(41) 1.335(4) yes . . F(2) C(41) 1.332(5) yes . . F(3) C(41) 1.328(4) yes . . F(4) C(42) 1.332(4) yes . . F(5) C(42) 1.326(6) yes . . F(6) C(42) 1.331(4) yes . . N(1) C(19) 1.362(4) yes . . N(1) C(20) 1.375(3) yes . . N(1) C(26) 1.496(5) yes . . N(2) C(33) 1.375(4) yes . . N(2) C(34) 1.368(4) yes . . N(2) C(40) 1.481(4) yes . . N(3) C(44) 1.127(8) yes . . C(1) C(2) 1.371(5) yes . . C(1) C(11) 1.475(4) yes . . C(1) C(13) 1.480(5) yes . . C(2) C(3) 1.480(4) yes . . C(2) C(27) 1.479(4) yes . . C(3) C(4) 1.370(5) yes . . C(3) C(12) 1.415(5) yes . . C(4) C(5) 1.418(4) yes . . C(5) C(6) 1.375(5) yes . . C(6) C(7) 1.421(6) yes . . C(7) C(8) 1.414(5) yes . . C(7) C(12) 1.389(4) yes . . C(8) C(9) 1.383(6) yes . . C(9) C(10) 1.413(4) yes . . C(10) C(11) 1.376(5) yes . . C(11) C(12) 1.412(5) yes . . C(13) C(14) 1.404(3) yes . . C(13) C(25) 1.402(4) yes . . C(14) C(15) 1.419(4) yes . . C(14) C(19) 1.429(5) yes . . C(15) C(16) 1.351(3) yes . . C(16) C(17) 1.414(5) yes . . C(17) C(18) 1.361(5) yes . . C(18) C(19) 1.413(3) yes . . C(20) C(21) 1.412(5) yes . . C(20) C(25) 1.421(5) yes . . C(21) C(22) 1.361(4) yes . . C(22) C(23) 1.397(6) yes . . C(23) C(24) 1.361(5) yes . . C(24) C(25) 1.419(3) yes . . C(27) C(28) 1.399(4) yes . . C(27) C(39) 1.409(4) yes . . C(28) C(29) 1.427(4) yes . . C(28) C(33) 1.424(4) yes . . C(29) C(30) 1.352(4) yes . . C(30) C(31) 1.400(4) yes . . C(31) C(32) 1.366(5) yes . . C(32) C(33) 1.409(4) yes . . C(34) C(35) 1.416(4) yes . . C(34) C(39) 1.423(4) yes . . C(35) C(36) 1.358(5) yes . . C(36) C(37) 1.398(6) yes . . C(37) C(38) 1.356(4) yes . . C(38) C(39) 1.425(4) yes . . C(43) C(44) 1.434(8) yes . . C(4) H(1) 0.950 no . . C(5) H(2) 0.950 no . . C(6) H(3) 0.950 no . . C(8) H(4) 0.950 no . . C(9) H(5) 0.950 no . . C(10) H(6) 0.950 no . . C(15) H(7) 0.950 no . . C(16) H(8) 0.950 no . . C(17) H(9) 0.950 no . . C(18) H(10) 0.950 no . . C(21) H(11) 0.950 no . . C(22) H(12) 0.950 no . . C(23) H(13) 0.950 no . . C(24) H(14) 0.950 no . . C(26) H(15) 0.950 no . . C(26) H(16) 0.950 no . . C(26) H(17) 0.950 no . . C(29) H(18) 0.950 no . . C(30) H(19) 0.950 no . . C(31) H(20) 0.950 no . . C(32) H(21) 0.950 no . . C(35) H(22) 0.950 no . . C(36) H(23) 0.950 no . . C(37) H(24) 0.950 no . . C(38) H(25) 0.950 no . . C(40) H(26) 0.950 no . . C(40) H(27) 0.950 no . . C(40) H(28) 0.950 no . . C(43) H(29) 0.950 no . . C(43) H(30) 0.950 no . . C(43) H(31) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(1) S(1) O(2) 114.88(15) yes . . . O(1) S(1) O(3) 115.14(13) yes . . . O(1) S(1) C(41) 101.80(16) yes . . . O(2) S(1) O(3) 115.57(14) yes . . . O(2) S(1) C(41) 103.74(14) yes . . . O(3) S(1) C(41) 103.02(16) yes . . . O(4) S(2) O(5) 114.92(16) yes . . . O(4) S(2) O(6) 114.60(15) yes . . . O(4) S(2) C(42) 103.36(16) yes . . . O(5) S(2) O(6) 115.33(14) yes . . . O(5) S(2) C(42) 103.19(15) yes . . . O(6) S(2) C(42) 103.03(15) yes . . . C(19) N(1) C(20) 122.0(3) yes . . . C(19) N(1) C(26) 118.6(2) yes . . . C(20) N(1) C(26) 119.3(3) yes . . . C(33) N(2) C(34) 121.5(3) yes . . . C(33) N(2) C(40) 119.1(3) yes . . . C(34) N(2) C(40) 119.4(3) yes . . . C(2) C(1) C(11) 109.0(3) yes . . . C(2) C(1) C(13) 124.9(3) yes . . . C(11) C(1) C(13) 126.0(3) yes . . . C(1) C(2) C(3) 108.7(3) yes . . . C(1) C(2) C(27) 127.2(3) yes . . . C(3) C(2) C(27) 124.0(3) yes . . . C(2) C(3) C(4) 135.7(3) yes . . . C(2) C(3) C(12) 105.6(3) yes . . . C(4) C(3) C(12) 118.6(3) yes . . . C(3) C(4) C(5) 117.9(3) yes . . . C(4) C(5) C(6) 122.9(4) yes . . . C(5) C(6) C(7) 120.4(3) yes . . . C(6) C(7) C(8) 128.7(3) yes . . . C(6) C(7) C(12) 115.3(3) yes . . . C(8) C(7) C(12) 116.0(4) yes . . . C(7) C(8) C(9) 120.1(3) yes . . . C(8) C(9) C(10) 122.9(4) yes . . . C(9) C(10) C(11) 117.9(4) yes . . . C(1) C(11) C(10) 135.4(3) yes . . . C(1) C(11) C(12) 105.8(3) yes . . . C(10) C(11) C(12) 118.8(3) yes . . . C(3) C(12) C(7) 124.8(3) yes . . . C(3) C(12) C(11) 110.8(3) yes . . . C(7) C(12) C(11) 124.4(3) yes . . . C(1) C(13) C(14) 120.8(3) yes . . . C(1) C(13) C(25) 119.9(2) yes . . . C(14) C(13) C(25) 119.3(3) yes . . . C(13) C(14) C(15) 121.7(3) yes . . . C(13) C(14) C(19) 119.5(3) yes . . . C(15) C(14) C(19) 118.7(2) yes . . . C(14) C(15) C(16) 121.3(3) yes . . . C(15) C(16) C(17) 119.6(3) yes . . . C(16) C(17) C(18) 121.4(3) yes . . . C(17) C(18) C(19) 120.3(3) yes . . . N(1) C(19) C(14) 119.41(19) yes . . . N(1) C(19) C(18) 121.9(3) yes . . . C(14) C(19) C(18) 118.7(3) yes . . . N(1) C(20) C(21) 121.2(3) yes . . . N(1) C(20) C(25) 119.3(3) yes . . . C(21) C(20) C(25) 119.5(3) yes . . . C(20) C(21) C(22) 119.2(4) yes . . . C(21) C(22) C(23) 122.3(4) yes . . . C(22) C(23) C(24) 119.4(3) yes . . . C(23) C(24) C(25) 120.9(3) yes . . . C(13) C(25) C(20) 119.8(2) yes . . . C(13) C(25) C(24) 121.6(3) yes . . . C(20) C(25) C(24) 118.6(3) yes . . . C(2) C(27) C(28) 120.0(3) yes . . . C(2) C(27) C(39) 121.2(3) yes . . . C(28) C(27) C(39) 118.8(3) yes . . . C(27) C(28) C(29) 121.5(3) yes . . . C(27) C(28) C(33) 120.3(3) yes . . . C(29) C(28) C(33) 118.2(3) yes . . . C(28) C(29) C(30) 121.4(3) yes . . . C(29) C(30) C(31) 119.5(3) yes . . . C(30) C(31) C(32) 121.7(3) yes . . . C(31) C(32) C(33) 119.9(3) yes . . . N(2) C(33) C(28) 119.5(3) yes . . . N(2) C(33) C(32) 121.3(3) yes . . . C(28) C(33) C(32) 119.2(3) yes . . . N(2) C(34) C(35) 121.0(3) yes . . . N(2) C(34) C(39) 120.0(3) yes . . . C(35) C(34) C(39) 119.0(3) yes . . . C(34) C(35) C(36) 120.0(4) yes . . . C(35) C(36) C(37) 121.6(3) yes . . . C(36) C(37) C(38) 119.9(3) yes . . . C(37) C(38) C(39) 120.9(3) yes . . . C(27) C(39) C(34) 119.8(3) yes . . . C(27) C(39) C(38) 121.8(3) yes . . . C(34) C(39) C(38) 118.4(3) yes . . . S(1) C(41) F(1) 111.9(3) yes . . . S(1) C(41) F(2) 112.3(3) yes . . . S(1) C(41) F(3) 112.1(2) yes . . . F(1) C(41) F(2) 106.7(3) yes . . . F(1) C(41) F(3) 107.5(3) yes . . . F(2) C(41) F(3) 106.0(3) yes . . . S(2) C(42) F(4) 111.8(3) yes . . . S(2) C(42) F(5) 111.3(2) yes . . . S(2) C(42) F(6) 112.4(3) yes . . . F(4) C(42) F(5) 107.3(3) yes . . . F(4) C(42) F(6) 107.3(3) yes . . . F(5) C(42) F(6) 106.4(3) yes . . . N(3) C(44) C(43) 177.4(10) yes . . . C(3) C(4) H(1) 120.486 no . . . C(5) C(4) H(1) 121.565 no . . . C(4) C(5) H(2) 118.742 no . . . C(6) C(5) H(2) 118.345 no . . . C(5) C(6) H(3) 120.267 no . . . C(7) C(6) H(3) 119.316 no . . . C(7) C(8) H(4) 119.800 no . . . C(9) C(8) H(4) 120.098 no . . . C(8) C(9) H(5) 118.555 no . . . C(10) C(9) H(5) 118.567 no . . . C(9) C(10) H(6) 121.613 no . . . C(11) C(10) H(6) 120.496 no . . . C(14) C(15) H(7) 119.191 no . . . C(16) C(15) H(7) 119.491 no . . . C(15) C(16) H(8) 120.480 no . . . C(17) C(16) H(8) 119.958 no . . . C(16) C(17) H(9) 119.317 no . . . C(18) C(17) H(9) 119.308 no . . . C(17) C(18) H(10) 120.072 no . . . C(19) C(18) H(10) 119.639 no . . . C(20) C(21) H(11) 119.905 no . . . C(22) C(21) H(11) 120.870 no . . . C(21) C(22) H(12) 118.781 no . . . C(23) C(22) H(12) 118.879 no . . . C(22) C(23) H(13) 120.378 no . . . C(24) C(23) H(13) 120.188 no . . . C(23) C(24) H(14) 119.838 no . . . C(25) C(24) H(14) 119.250 no . . . N(1) C(26) H(15) 109.410 no . . . N(1) C(26) H(16) 109.356 no . . . N(1) C(26) H(17) 109.645 no . . . H(15) C(26) H(16) 109.469 no . . . H(15) C(26) H(17) 109.478 no . . . H(16) C(26) H(17) 109.469 no . . . C(28) C(29) H(18) 118.938 no . . . C(30) C(29) H(18) 119.659 no . . . C(29) C(30) H(19) 120.318 no . . . C(31) C(30) H(19) 120.156 no . . . C(30) C(31) H(20) 119.208 no . . . C(32) C(31) H(20) 119.049 no . . . C(31) C(32) H(21) 120.166 no . . . C(33) C(32) H(21) 119.937 no . . . C(34) C(35) H(22) 119.884 no . . . C(36) C(35) H(22) 120.113 no . . . C(35) C(36) H(23) 119.053 no . . . C(37) C(36) H(23) 119.303 no . . . C(36) C(37) H(24) 120.207 no . . . C(38) C(37) H(24) 119.845 no . . . C(37) C(38) H(25) 120.150 no . . . C(39) C(38) H(25) 118.934 no . . . N(2) C(40) H(26) 109.782 no . . . N(2) C(40) H(27) 109.330 no . . . N(2) C(40) H(28) 109.301 no . . . H(26) C(40) H(27) 109.476 no . . . H(26) C(40) H(28) 109.468 no . . . H(27) C(40) H(28) 109.469 no . . . C(44) C(43) H(29) 109.943 no . . . C(44) C(43) H(30) 108.548 no . . . C(44) C(43) H(31) 109.921 no . . . H(29) C(43) H(30) 109.473 no . . . H(29) C(43) H(31) 109.469 no . . . H(30) C(43) H(31) 109.470 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O(1) S(1) C(41) F(1) 62.2(3) no . . . . O(1) S(1) C(41) F(2) -177.84(16) no . . . . O(1) S(1) C(41) F(3) -58.6(3) no . . . . O(2) S(1) C(41) F(1) -57.3(3) no . . . . O(2) S(1) C(41) F(2) 62.6(2) no . . . . O(2) S(1) C(41) F(3) -178.2(3) no . . . . O(3) S(1) C(41) F(1) -178.2(2) no . . . . O(3) S(1) C(41) F(2) -58.2(2) no . . . . O(3) S(1) C(41) F(3) 61.0(3) no . . . . O(4) S(2) C(42) F(4) -68.3(3) no . . . . O(4) S(2) C(42) F(5) 171.78(18) no . . . . O(4) S(2) C(42) F(6) 52.5(3) no . . . . O(5) S(2) C(42) F(4) 51.8(3) no . . . . O(5) S(2) C(42) F(5) -68.2(3) no . . . . O(5) S(2) C(42) F(6) 172.5(3) no . . . . O(6) S(2) C(42) F(4) 172.1(3) no . . . . O(6) S(2) C(42) F(5) 52.2(3) no . . . . O(6) S(2) C(42) F(6) -67.1(3) no . . . . C(19) N(1) C(20) C(21) -173.7(3) no . . . . C(19) N(1) C(20) C(25) 6.4(5) no . . . . C(20) N(1) C(19) C(14) -7.2(4) no . . . . C(20) N(1) C(19) C(18) 171.7(3) no . . . . C(26) N(1) C(19) C(14) 171.5(3) no . . . . C(26) N(1) C(19) C(18) -9.6(4) no . . . . C(26) N(1) C(20) C(21) 7.7(5) no . . . . C(26) N(1) C(20) C(25) -172.2(3) no . . . . C(33) N(2) C(34) C(35) 175.7(3) no . . . . C(33) N(2) C(34) C(39) -3.6(5) no . . . . C(34) N(2) C(33) C(28) 0.6(5) no . . . . C(34) N(2) C(33) C(32) 179.1(3) no . . . . C(40) N(2) C(33) C(28) -179.1(3) no . . . . C(40) N(2) C(33) C(32) -0.6(5) no . . . . C(40) N(2) C(34) C(35) -4.5(5) no . . . . C(40) N(2) C(34) C(39) 176.1(3) no . . . . C(2) C(1) C(11) C(10) -179.0(2) no . . . . C(2) C(1) C(11) C(12) 1.1(3) no . . . . C(11) C(1) C(2) C(3) -1.8(3) no . . . . C(11) C(1) C(2) C(27) 178.57(17) no . . . . C(2) C(1) C(13) C(14) 71.3(3) no . . . . C(2) C(1) C(13) C(25) -108.3(3) no . . . . C(13) C(1) C(2) C(3) 175.23(18) no . . . . C(13) C(1) C(2) C(27) -4.4(4) no . . . . C(11) C(1) C(13) C(14) -112.2(3) no . . . . C(11) C(1) C(13) C(25) 68.2(3) no . . . . C(13) C(1) C(11) C(10) 4.0(4) no . . . . C(13) C(1) C(11) C(12) -175.88(18) no . . . . C(1) C(2) C(3) C(4) -176.0(2) no . . . . C(1) C(2) C(3) C(12) 1.8(3) no . . . . C(1) C(2) C(27) C(28) -108.6(3) no . . . . C(1) C(2) C(27) C(39) 72.0(3) no . . . . C(3) C(2) C(27) C(28) 71.7(3) no . . . . C(3) C(2) C(27) C(39) -107.6(3) no . . . . C(27) C(2) C(3) C(4) 3.7(4) no . . . . C(27) C(2) C(3) C(12) -178.54(18) no . . . . C(2) C(3) C(4) C(5) 177.7(2) no . . . . C(2) C(3) C(12) C(7) -178.92(18) no . . . . C(2) C(3) C(12) C(11) -1.1(3) no . . . . C(4) C(3) C(12) C(7) -0.7(4) no . . . . C(4) C(3) C(12) C(11) 177.11(18) no . . . . C(12) C(3) C(4) C(5) 0.1(3) no . . . . C(3) C(4) C(5) C(6) 0.6(4) no . . . . C(4) C(5) C(6) C(7) -0.8(4) no . . . . C(5) C(6) C(7) C(8) -178.3(3) no . . . . C(5) C(6) C(7) C(12) 0.2(4) no . . . . C(6) C(7) C(8) C(9) 177.8(3) no . . . . C(6) C(7) C(12) C(3) 0.5(4) no . . . . C(6) C(7) C(12) C(11) -177.02(19) no . . . . C(8) C(7) C(12) C(3) 179.22(19) no . . . . C(8) C(7) C(12) C(11) 1.7(4) no . . . . C(12) C(7) C(8) C(9) -0.7(3) no . . . . C(7) C(8) C(9) C(10) 0.0(4) no . . . . C(8) C(9) C(10) C(11) -0.3(4) no . . . . C(9) C(10) C(11) C(1) -178.7(2) no . . . . C(9) C(10) C(11) C(12) 1.2(3) no . . . . C(1) C(11) C(12) C(3) 0.1(3) no . . . . C(1) C(11) C(12) C(7) 177.91(17) no . . . . C(10) C(11) C(12) C(3) -179.83(18) no . . . . C(10) C(11) C(12) C(7) -2.0(4) no . . . . C(1) C(13) C(14) C(15) 10.3(4) no . . . . C(1) C(13) C(14) C(19) -173.1(3) no . . . . C(1) C(13) C(25) C(20) 172.4(3) no . . . . C(1) C(13) C(25) C(24) -5.9(4) no . . . . C(14) C(13) C(25) C(20) -7.2(4) no . . . . C(14) C(13) C(25) C(24) 174.5(3) no . . . . C(25) C(13) C(14) C(15) -170.2(3) no . . . . C(25) C(13) C(14) C(19) 6.4(4) no . . . . C(13) C(14) C(15) C(16) 175.8(3) no . . . . C(13) C(14) C(19) N(1) 0.6(4) no . . . . C(13) C(14) C(19) C(18) -178.3(3) no . . . . C(15) C(14) C(19) N(1) 177.3(3) no . . . . C(15) C(14) C(19) C(18) -1.6(4) no . . . . C(19) C(14) C(15) C(16) -0.9(4) no . . . . C(14) C(15) C(16) C(17) 2.6(5) no . . . . C(15) C(16) C(17) C(18) -1.8(5) no . . . . C(16) C(17) C(18) C(19) -0.8(5) no . . . . C(17) C(18) C(19) N(1) -176.5(3) no . . . . C(17) C(18) C(19) C(14) 2.4(5) no . . . . N(1) C(20) C(21) C(22) -179.0(3) no . . . . N(1) C(20) C(25) C(13) 0.9(5) no . . . . N(1) C(20) C(25) C(24) 179.3(3) no . . . . C(21) C(20) C(25) C(13) -179.0(3) no . . . . C(21) C(20) C(25) C(24) -0.6(5) no . . . . C(25) C(20) C(21) C(22) 0.9(5) no . . . . C(20) C(21) C(22) C(23) -0.7(6) no . . . . C(21) C(22) C(23) C(24) 0.2(6) no . . . . C(22) C(23) C(24) C(25) 0.1(5) no . . . . C(23) C(24) C(25) C(13) 178.4(3) no . . . . C(23) C(24) C(25) C(20) 0.1(5) no . . . . C(2) C(27) C(28) C(29) -1.0(5) no . . . . C(2) C(27) C(28) C(33) 177.9(3) no . . . . C(2) C(27) C(39) C(34) 179.1(3) no . . . . C(2) C(27) C(39) C(38) 0.9(5) no . . . . C(28) C(27) C(39) C(34) -0.3(5) no . . . . C(28) C(27) C(39) C(38) -178.4(3) no . . . . C(39) C(27) C(28) C(29) 178.4(3) no . . . . C(39) C(27) C(28) C(33) -2.7(5) no . . . . C(27) C(28) C(29) C(30) 176.9(3) no . . . . C(27) C(28) C(33) N(2) 2.6(5) no . . . . C(27) C(28) C(33) C(32) -176.0(3) no . . . . C(29) C(28) C(33) N(2) -178.4(3) no . . . . C(29) C(28) C(33) C(32) 3.0(5) no . . . . C(33) C(28) C(29) C(30) -2.1(5) no . . . . C(28) C(29) C(30) C(31) 0.0(5) no . . . . C(29) C(30) C(31) C(32) 1.2(6) no . . . . C(30) C(31) C(32) C(33) -0.2(6) no . . . . C(31) C(32) C(33) N(2) 179.5(3) no . . . . C(31) C(32) C(33) C(28) -1.9(5) no . . . . N(2) C(34) C(35) C(36) 178.8(3) no . . . . N(2) C(34) C(39) C(27) 3.4(5) no . . . . N(2) C(34) C(39) C(38) -178.4(3) no . . . . C(35) C(34) C(39) C(27) -175.9(3) no . . . . C(35) C(34) C(39) C(38) 2.3(5) no . . . . C(39) C(34) C(35) C(36) -1.9(5) no . . . . C(34) C(35) C(36) C(37) -0.6(6) no . . . . C(35) C(36) C(37) C(38) 2.9(6) no . . . . C(36) C(37) C(38) C(39) -2.4(5) no . . . . C(37) C(38) C(39) C(27) 178.0(3) no . . . . C(37) C(38) C(39) C(34) -0.1(5) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 F(1) C(30) 3.472(5) no . . F(1) C(31) 3.381(4) no . . F(1) C(32) 3.481(5) no . . F(2) F(2) 3.324(4) no . 2_556 F(2) C(8) 3.481(4) no . 1_455 F(2) C(17) 3.327(4) no . 1_554 F(2) C(18) 3.564(4) no . 1_554 F(3) F(4) 3.279(3) no . 2_656 F(3) C(7) 3.543(4) no . 2_656 F(3) C(8) 3.231(4) no . 2_656 F(3) C(17) 3.447(5) no . 1_554 F(3) C(18) 3.424(4) no . 1_554 F(4) F(3) 3.279(3) no . 2_656 F(4) N(1) 3.537(3) no . 2_657 F(4) C(18) 3.246(4) no . 2_657 F(4) C(19) 3.193(4) no . 2_657 F(4) C(22) 3.373(5) no . 1_545 F(5) F(5) 3.470(4) no . 2_657 F(5) C(13) 3.592(4) no . 2_657 F(5) C(14) 3.115(4) no . 2_657 F(5) C(15) 3.030(4) no . 2_657 F(5) C(16) 3.365(4) no . 2_657 F(5) C(19) 3.554(4) no . 2_657 F(6) C(3) 3.356(3) no . . F(6) C(11) 3.489(4) no . . F(6) C(12) 3.221(3) no . . F(6) C(29) 3.260(4) no . . O(1) N(2) 3.217(4) no . . O(1) C(4) 3.536(4) no . . O(1) C(23) 3.216(4) no . 2_666 O(1) C(27) 3.169(5) no . . O(1) C(28) 3.150(4) no . . O(1) C(33) 3.207(4) no . . O(1) C(34) 3.170(5) no . . O(1) C(39) 3.174(5) no . . O(2) N(2) 3.190(4) no . . O(2) C(9) 3.353(4) no . 1_455 O(2) C(33) 3.423(4) no . . O(2) C(35) 3.454(4) no . 2_566 O(2) C(36) 3.435(5) no . 2_566 O(2) C(40) 3.177(5) no . . O(3) C(18) 3.400(5) no . 1_554 O(3) C(26) 3.211(4) no . 1_554 O(3) C(35) 3.334(4) no . 2_566 O(4) C(21) 3.370(4) no . 1_545 O(4) C(30) 3.501(4) no . . O(4) C(43) 3.347(9) no . 2_557 O(5) C(20) 3.304(4) no . 2_657 O(5) C(21) 3.506(5) no . 1_545 O(5) C(24) 3.556(4) no . 2_657 O(5) C(25) 3.195(5) no . 2_657 O(5) C(26) 3.513(5) no . 1_545 O(6) C(10) 3.557(5) no . 2_657 O(6) C(15) 3.554(4) no . . O(6) C(16) 3.273(5) no . . O(6) C(30) 3.441(4) no . . O(6) C(32) 3.269(4) no . 2_557 O(6) C(40) 3.568(4) no . 2_557 N(1) F(4) 3.537(3) no . 2_657 N(2) O(1) 3.217(4) no . . N(2) O(2) 3.190(4) no . . N(2) N(3) 3.224(9) no . . N(3) N(2) 3.224(9) no . . N(3) C(19) 3.555(9) no . . N(3) C(34) 3.269(8) no . . N(3) C(40) 3.552(10) no . . C(3) F(6) 3.356(3) no . . C(4) O(1) 3.536(4) no . . C(5) C(5) 3.479(5) no . 2_656 C(7) F(3) 3.543(4) no . 2_656 C(8) F(2) 3.481(4) no . 1_655 C(8) F(3) 3.231(4) no . 2_656 C(9) O(2) 3.353(4) no . 1_655 C(10) O(6) 3.557(5) no . 2_657 C(11) F(6) 3.489(4) no . . C(12) F(6) 3.221(3) no . . C(13) F(5) 3.592(4) no . 2_657 C(14) F(5) 3.115(4) no . 2_657 C(15) F(5) 3.030(4) no . 2_657 C(15) O(6) 3.554(4) no . . C(16) F(5) 3.365(4) no . 2_657 C(16) O(6) 3.273(5) no . . C(16) C(31) 3.561(5) no . 2_557 C(17) F(2) 3.327(4) no . 1_556 C(17) F(3) 3.447(5) no . 1_556 C(18) F(2) 3.564(4) no . 1_556 C(18) F(3) 3.424(4) no . 1_556 C(18) F(4) 3.246(4) no . 2_657 C(18) O(3) 3.400(5) no . 1_556 C(19) F(4) 3.193(4) no . 2_657 C(19) F(5) 3.554(4) no . 2_657 C(19) N(3) 3.555(9) no . . C(20) O(5) 3.304(4) no . 2_657 C(21) O(4) 3.370(4) no . 1_565 C(21) O(5) 3.506(5) no . 1_565 C(22) F(4) 3.373(5) no . 1_565 C(23) O(1) 3.216(4) no . 2_666 C(24) O(5) 3.556(4) no . 2_657 C(25) O(5) 3.195(5) no . 2_657 C(26) O(3) 3.211(4) no . 1_556 C(26) O(5) 3.513(5) no . 1_565 C(27) O(1) 3.169(5) no . . C(28) O(1) 3.150(4) no . . C(29) F(6) 3.260(4) no . . C(30) F(1) 3.472(5) no . . C(30) O(4) 3.501(4) no . . C(30) O(6) 3.441(4) no . . C(31) F(1) 3.381(4) no . . C(31) C(16) 3.561(5) no . 2_557 C(31) C(31) 3.380(5) no . 2_557 C(32) F(1) 3.481(5) no . . C(32) O(6) 3.269(4) no . 2_557 C(33) O(1) 3.207(4) no . . C(33) O(2) 3.423(4) no . . C(34) O(1) 3.170(5) no . . C(34) N(3) 3.269(8) no . . C(35) O(2) 3.454(4) no . 2_566 C(35) O(3) 3.334(4) no . 2_566 C(36) O(2) 3.435(5) no . 2_566 C(39) O(1) 3.174(5) no . . C(40) O(2) 3.177(5) no . . C(40) O(6) 3.568(4) no . 2_557 C(40) N(3) 3.552(10) no . . C(43) O(4) 3.347(9) no . 2_557 S(1) H(10) 3.5363 no . 1_554 S(1) H(13) 3.3928 no . 2_666 S(1) H(22) 3.1510 no . 2_566 S(2) H(6) 3.2262 no . 2_657 S(2) H(11) 3.0576 no . 1_545 S(2) H(17) 3.4126 no . 1_545 S(2) H(19) 3.2702 no . . S(2) H(21) 3.5377 no . 2_557 S(2) H(26) 3.0954 no . 2_557 F(1) H(3) 3.0159 no . 2_656 F(1) H(4) 2.9570 no . 2_656 F(1) H(5) 3.4467 no . 1_455 F(2) H(4) 2.6975 no . 1_455 F(2) H(4) 3.0723 no . 2_656 F(2) H(5) 3.4720 no . 1_455 F(2) H(9) 2.5741 no . 1_554 F(2) H(10) 3.0768 no . 1_554 F(3) H(1) 3.1357 no . . F(3) H(3) 3.3731 no . 2_656 F(3) H(4) 2.8807 no . 2_656 F(3) H(9) 3.0922 no . 1_554 F(3) H(10) 3.0684 no . 1_554 F(3) H(12) 3.5092 no . 2_666 F(4) H(2) 3.2824 no . 2_656 F(4) H(10) 3.5011 no . 2_657 F(4) H(11) 3.1881 no . 1_545 F(4) H(12) 2.5722 no . 1_545 F(5) H(6) 3.3453 no . 2_657 F(5) H(7) 3.1981 no . . F(5) H(7) 3.2943 no . 2_657 F(6) H(2) 2.7998 no . 2_656 F(6) H(7) 2.9652 no . . F(6) H(18) 2.3692 no . . F(6) H(19) 3.5683 no . . O(1) H(1) 2.6687 no . . O(1) H(12) 3.3903 no . 2_666 O(1) H(13) 2.3552 no . 2_666 O(2) H(5) 2.7615 no . 1_455 O(2) H(21) 3.5947 no . . O(2) H(22) 2.9481 no . 2_566 O(2) H(23) 2.9011 no . 2_566 O(2) H(28) 2.4556 no . . O(3) H(10) 2.4736 no . 1_554 O(3) H(12) 3.5994 no . 2_666 O(3) H(13) 3.4766 no . 2_666 O(3) H(15) 2.6715 no . 1_554 O(3) H(16) 2.8800 no . 1_554 O(3) H(22) 2.4529 no . 2_566 O(3) H(23) 3.4977 no . 2_566 O(3) H(27) 2.9398 no . 2_566 O(4) H(2) 3.2524 no . 2_656 O(4) H(11) 2.7071 no . 1_545 O(4) H(17) 2.9541 no . 1_545 O(4) H(19) 2.6311 no . . O(4) H(26) 3.2842 no . 2_557 O(4) H(29) 2.4349 no . 2_557 O(5) H(6) 2.8178 no . 2_657 O(5) H(11) 2.5664 no . 1_545 O(5) H(16) 3.2065 no . 1_545 O(5) H(17) 2.9308 no . 1_545 O(5) H(26) 3.1797 no . 2_557 O(6) H(6) 2.7509 no . 2_657 O(6) H(7) 3.0745 no . . O(6) H(8) 2.4980 no . . O(6) H(18) 3.4570 no . . O(6) H(19) 2.9644 no . . O(6) H(21) 2.3876 no . 2_557 O(6) H(26) 2.8392 no . 2_557 O(6) H(28) 3.4519 no . 2_557 N(3) H(26) 3.2575 no . . N(3) H(27) 3.5629 no . . N(3) H(31) 3.0988 no . 2_567 C(3) H(24) 3.1601 no . 2_666 C(4) H(12) 3.4095 no . 2_666 C(4) H(13) 3.4527 no . 2_666 C(5) H(2) 3.3829 no . 2_656 C(5) H(12) 3.5558 no . 2_666 C(6) H(24) 3.5683 no . 2_666 C(7) H(23) 3.2829 no . 2_666 C(7) H(24) 3.0412 no . 2_666 C(8) H(23) 2.8469 no . 2_666 C(8) H(24) 3.5595 no . 2_666 C(9) H(8) 3.2691 no . 2_657 C(9) H(9) 3.4787 no . 2_657 C(9) H(23) 3.0118 no . 2_666 C(10) H(8) 3.5090 no . 2_657 C(10) H(23) 3.5846 no . 2_666 C(11) H(24) 3.1078 no . 2_666 C(12) H(24) 2.7799 no . 2_666 C(15) H(20) 3.5767 no . 2_557 C(16) H(5) 3.4344 no . 2_657 C(16) H(20) 2.7444 no . 2_557 C(16) H(21) 3.5288 no . 2_557 C(17) H(5) 3.5629 no . 2_657 C(17) H(20) 3.1426 no . 2_557 C(21) H(11) 3.5912 no . 2_667 C(21) H(16) 3.2077 no . 2_667 C(22) H(1) 3.4840 no . 2_666 C(22) H(16) 2.8872 no . 2_667 C(23) H(1) 3.4747 no . 2_666 C(23) H(16) 3.4761 no . 2_667 C(26) H(27) 3.4566 no . 2_567 C(30) H(3) 3.5023 no . 2_656 C(30) H(20) 3.5111 no . 2_557 C(31) H(8) 3.0586 no . 2_557 C(31) H(20) 3.2760 no . 2_557 C(32) H(5) 3.5884 no . 1_455 C(32) H(8) 3.1695 no . 2_557 C(32) H(20) 3.5559 no . 2_557 C(35) H(31) 3.3914 no . 2_567 C(36) H(14) 3.5409 no . 2_666 C(36) H(30) 3.3160 no . 2_567 C(36) H(31) 3.0845 no . 2_567 C(37) H(14) 2.8289 no . 2_666 C(37) H(31) 3.3609 no . 2_567 C(38) H(13) 3.2165 no . 2_666 C(38) H(14) 3.1144 no . 2_666 C(39) H(13) 3.3258 no . 2_666 C(41) H(4) 3.2010 no . 2_656 C(41) H(9) 3.4030 no . 1_554 C(41) H(10) 3.3521 no . 1_554 C(42) H(2) 3.4684 no . 2_656 C(42) H(7) 3.4832 no . . C(42) H(18) 3.4483 no . . C(43) H(17) 3.5243 no . 2_567 C(43) H(23) 3.5361 no . 2_567 C(44) H(17) 3.5649 no . 2_567 C(44) H(26) 3.4974 no . . H(1) F(3) 3.1357 no . . H(1) O(1) 2.6687 no . . H(1) C(22) 3.4840 no . 2_666 H(1) C(23) 3.4747 no . 2_666 H(1) H(3) 3.5650 no . 2_656 H(1) H(12) 2.9928 no . 2_666 H(1) H(13) 2.9910 no . 2_666 H(2) F(4) 3.2824 no . 2_656 H(2) F(6) 2.7998 no . 2_656 H(2) O(4) 3.2524 no . 2_656 H(2) C(5) 3.3829 no . 2_656 H(2) C(42) 3.4684 no . 2_656 H(2) H(2) 3.5485 no . 2_656 H(2) H(12) 3.2338 no . 2_666 H(2) H(18) 3.4904 no . 2_656 H(3) F(1) 3.0159 no . 2_656 H(3) F(3) 3.3731 no . 2_656 H(3) C(30) 3.5023 no . 2_656 H(3) H(1) 3.5650 no . 2_656 H(3) H(18) 3.4967 no . 2_656 H(3) H(19) 3.2316 no . 2_656 H(3) H(29) 3.3308 no . 1_654 H(3) H(30) 3.4838 no . 1_654 H(4) F(1) 2.9570 no . 2_656 H(4) F(2) 2.6975 no . 1_655 H(4) F(2) 3.0723 no . 2_656 H(4) F(3) 2.8807 no . 2_656 H(4) C(41) 3.2010 no . 2_656 H(4) H(9) 3.4975 no . 2_657 H(4) H(23) 3.0348 no . 2_666 H(5) F(1) 3.4467 no . 1_655 H(5) F(2) 3.4720 no . 1_655 H(5) O(2) 2.7615 no . 1_655 H(5) C(16) 3.4344 no . 2_657 H(5) C(17) 3.5629 no . 2_657 H(5) C(32) 3.5884 no . 1_655 H(5) H(8) 2.8217 no . 2_657 H(5) H(9) 3.0739 no . 2_657 H(5) H(21) 3.0844 no . 1_655 H(5) H(23) 3.2838 no . 2_666 H(5) H(28) 3.1718 no . 1_655 H(6) S(2) 3.2262 no . 2_657 H(6) F(5) 3.3453 no . 2_657 H(6) O(5) 2.8178 no . 2_657 H(6) O(6) 2.7509 no . 2_657 H(6) H(8) 3.2903 no . 2_657 H(6) H(28) 3.3170 no . 1_655 H(7) F(5) 3.1981 no . . H(7) F(5) 3.2943 no . 2_657 H(7) F(6) 2.9652 no . . H(7) O(6) 3.0745 no . . H(7) C(42) 3.4832 no . . H(8) O(6) 2.4980 no . . H(8) C(9) 3.2691 no . 2_657 H(8) C(10) 3.5090 no . 2_657 H(8) C(31) 3.0586 no . 2_557 H(8) C(32) 3.1695 no . 2_557 H(8) H(5) 2.8217 no . 2_657 H(8) H(6) 3.2903 no . 2_657 H(8) H(20) 2.4008 no . 2_557 H(8) H(21) 2.6447 no . 2_557 H(9) F(2) 2.5741 no . 1_556 H(9) F(3) 3.0922 no . 1_556 H(9) C(9) 3.4787 no . 2_657 H(9) C(41) 3.4030 no . 1_556 H(9) H(4) 3.4975 no . 2_657 H(9) H(5) 3.0739 no . 2_657 H(9) H(20) 3.0953 no . 2_557 H(9) H(30) 3.5413 no . . H(10) S(1) 3.5363 no . 1_556 H(10) F(2) 3.0768 no . 1_556 H(10) F(3) 3.0684 no . 1_556 H(10) F(4) 3.5011 no . 2_657 H(10) O(3) 2.4736 no . 1_556 H(10) C(41) 3.3521 no . 1_556 H(10) H(30) 3.3046 no . . H(11) S(2) 3.0576 no . 1_565 H(11) F(4) 3.1881 no . 1_565 H(11) O(4) 2.7071 no . 1_565 H(11) O(5) 2.5664 no . 1_565 H(11) C(21) 3.5912 no . 2_667 H(11) H(11) 3.4762 no . 2_667 H(11) H(16) 3.3512 no . 2_667 H(12) F(3) 3.5092 no . 2_666 H(12) F(4) 2.5722 no . 1_565 H(12) O(1) 3.3903 no . 2_666 H(12) O(3) 3.5994 no . 2_666 H(12) C(4) 3.4095 no . 2_666 H(12) C(5) 3.5558 no . 2_666 H(12) H(1) 2.9928 no . 2_666 H(12) H(2) 3.2338 no . 2_666 H(12) H(16) 2.8067 no . 2_667 H(13) S(1) 3.3928 no . 2_666 H(13) O(1) 2.3552 no . 2_666 H(13) O(3) 3.4766 no . 2_666 H(13) C(4) 3.4527 no . 2_666 H(13) C(38) 3.2165 no . 2_666 H(13) C(39) 3.3258 no . 2_666 H(13) H(1) 2.9910 no . 2_666 H(13) H(25) 3.3650 no . 2_666 H(14) C(36) 3.5409 no . 2_666 H(14) C(37) 2.8289 no . 2_666 H(14) C(38) 3.1144 no . 2_666 H(14) H(24) 2.6945 no . 2_666 H(14) H(25) 3.1532 no . 2_666 H(15) O(3) 2.6715 no . 1_556 H(15) H(22) 3.4585 no . 2_567 H(15) H(27) 3.0660 no . 2_567 H(16) O(3) 2.8800 no . 1_556 H(16) O(5) 3.2065 no . 1_565 H(16) C(21) 3.2077 no . 2_667 H(16) C(22) 2.8872 no . 2_667 H(16) C(23) 3.4761 no . 2_667 H(16) H(11) 3.3512 no . 2_667 H(16) H(12) 2.8067 no . 2_667 H(16) H(27) 3.4240 no . 2_567 H(17) S(2) 3.4126 no . 1_565 H(17) O(4) 2.9541 no . 1_565 H(17) O(5) 2.9308 no . 1_565 H(17) C(43) 3.5243 no . 2_567 H(17) C(44) 3.5649 no . 2_567 H(17) H(26) 3.2089 no . 2_567 H(17) H(27) 3.3203 no . 2_567 H(17) H(29) 3.1743 no . 2_567 H(17) H(31) 3.3559 no . 2_567 H(18) F(6) 2.3692 no . . H(18) O(6) 3.4570 no . . H(18) C(42) 3.4483 no . . H(18) H(2) 3.4904 no . 2_656 H(18) H(3) 3.4967 no . 2_656 H(19) S(2) 3.2702 no . . H(19) F(6) 3.5683 no . . H(19) O(4) 2.6311 no . . H(19) O(6) 2.9644 no . . H(19) H(3) 3.2316 no . 2_656 H(19) H(21) 3.5097 no . 2_557 H(19) H(29) 3.0088 no . 2_557 H(20) C(15) 3.5767 no . 2_557 H(20) C(16) 2.7444 no . 2_557 H(20) C(17) 3.1426 no . 2_557 H(20) C(30) 3.5111 no . 2_557 H(20) C(31) 3.2760 no . 2_557 H(20) C(32) 3.5559 no . 2_557 H(20) H(8) 2.4008 no . 2_557 H(20) H(9) 3.0953 no . 2_557 H(20) H(20) 3.4418 no . 2_557 H(21) S(2) 3.5377 no . 2_557 H(21) O(2) 3.5947 no . . H(21) O(6) 2.3876 no . 2_557 H(21) C(16) 3.5288 no . 2_557 H(21) H(5) 3.0844 no . 1_455 H(21) H(8) 2.6447 no . 2_557 H(21) H(19) 3.5097 no . 2_557 H(22) S(1) 3.1510 no . 2_566 H(22) O(2) 2.9481 no . 2_566 H(22) O(3) 2.4529 no . 2_566 H(22) H(15) 3.4585 no . 2_567 H(23) O(2) 2.9011 no . 2_566 H(23) O(3) 3.4977 no . 2_566 H(23) C(7) 3.2829 no . 2_666 H(23) C(8) 2.8469 no . 2_666 H(23) C(9) 3.0118 no . 2_666 H(23) C(10) 3.5846 no . 2_666 H(23) C(43) 3.5361 no . 2_567 H(23) H(4) 3.0348 no . 2_666 H(23) H(5) 3.2838 no . 2_666 H(23) H(30) 2.9976 no . 2_567 H(23) H(31) 3.2236 no . 2_567 H(24) C(3) 3.1601 no . 2_666 H(24) C(6) 3.5683 no . 2_666 H(24) C(7) 3.0412 no . 2_666 H(24) C(8) 3.5595 no . 2_666 H(24) C(11) 3.1078 no . 2_666 H(24) C(12) 2.7799 no . 2_666 H(24) H(14) 2.6945 no . 2_666 H(24) H(25) 3.3370 no . 2_666 H(25) H(13) 3.3650 no . 2_666 H(25) H(14) 3.1532 no . 2_666 H(25) H(24) 3.3370 no . 2_666 H(25) H(25) 2.9664 no . 2_666 H(26) S(2) 3.0954 no . 2_557 H(26) O(4) 3.2842 no . 2_557 H(26) O(5) 3.1797 no . 2_557 H(26) O(6) 2.8392 no . 2_557 H(26) N(3) 3.2575 no . . H(26) C(44) 3.4974 no . . H(26) H(17) 3.2089 no . 2_567 H(27) O(3) 2.9398 no . 2_566 H(27) N(3) 3.5629 no . . H(27) C(26) 3.4566 no . 2_567 H(27) H(15) 3.0660 no . 2_567 H(27) H(16) 3.4240 no . 2_567 H(27) H(17) 3.3203 no . 2_567 H(28) O(2) 2.4556 no . . H(28) O(6) 3.4519 no . 2_557 H(28) H(5) 3.1718 no . 1_455 H(28) H(6) 3.3170 no . 1_455 H(29) O(4) 2.4349 no . 2_557 H(29) H(3) 3.3308 no . 1_456 H(29) H(17) 3.1743 no . 2_567 H(29) H(19) 3.0088 no . 2_557 H(30) C(36) 3.3160 no . 2_567 H(30) H(3) 3.4838 no . 1_456 H(30) H(9) 3.5413 no . . H(30) H(10) 3.3046 no . . H(30) H(23) 2.9976 no . 2_567 H(31) N(3) 3.0988 no . 2_567 H(31) C(35) 3.3914 no . 2_567 H(31) C(36) 3.0845 no . 2_567 H(31) C(37) 3.3609 no . 2_567 H(31) H(17) 3.3559 no . 2_567 H(31) H(23) 3.2236 no . 2_567 #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 975886' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data__051104tt #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C39 H26 N2' _chemical_formula_moiety 'C39 H26 N2' _chemical_formula_weight 522.65 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 9.848(6) _cell_length_b 11.966(6) _cell_length_c 12.247(7) _cell_angle_alpha 97.950(6) _cell_angle_beta 111.742(10) _cell_angle_gamma 95.696(8) _cell_volume 1309.7(12) _cell_formula_units_Z 2 _cell_measurement_reflns_used 3451 _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 27.10 _cell_measurement_temperature 153 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.030 _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 548.00 _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.778 _exptl_absorpt_correction_T_max 0.998 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 153 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_reflns_number 10700 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_theta_max 25.50 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measured_fraction_theta_full 0.981 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4785 _reflns_number_gt 2476 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.0894 _refine_ls_number_restraints ? _refine_ls_hydrogen_treatment refxyz _refine_ls_number_reflns 4782 _refine_ls_number_parameters 474 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[1.0000\s(Fo^2^)]/(4Fo^2^)' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_diff_density_max 0.503 _refine_diff_density_min -0.442 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 N(1) N 1.0981(3) 0.75209(19) 0.3802(2) 0.0350(8) Uani 1.0 2 d . . . N(2) N 0.6851(3) 0.8724(2) 0.3031(2) 0.0416(8) Uani 1.0 2 d . . . C(1) C 0.8147(3) 0.6863(3) -0.0844(3) 0.0290(9) Uani 1.0 2 d . . . C(2) C 0.9224(4) 0.6295(3) -0.0989(3) 0.0384(10) Uani 1.0 2 d . . . C(3) C 0.9074(4) 0.5821(3) -0.2169(4) 0.0475(12) Uani 1.0 2 d . . . C(4) C 0.7873(4) 0.5914(3) -0.3169(3) 0.0453(12) Uani 1.0 2 d . . . C(5) C 0.6721(4) 0.6489(3) -0.3043(3) 0.0378(10) Uani 1.0 2 d . . . C(6) C 0.5384(4) 0.6665(3) -0.3951(3) 0.0447(11) Uani 1.0 2 d . . . C(7) C 0.4423(4) 0.7274(3) -0.3653(3) 0.0415(10) Uani 1.0 2 d . . . C(8) C 0.4689(4) 0.7752(3) -0.2442(3) 0.0356(10) Uani 1.0 2 d . . . C(9) C 0.5947(3) 0.7584(3) -0.1553(3) 0.0291(9) Uani 1.0 2 d . . . C(10) C 0.6924(3) 0.6956(3) -0.1873(3) 0.0296(9) Uani 1.0 2 d . . . C(11) C 0.7912(3) 0.7472(3) 0.0185(3) 0.0264(8) Uani 1.0 2 d . . . C(12) C 0.6617(3) 0.7902(3) -0.0231(3) 0.0276(9) Uani 1.0 2 d . . . C(13) C 0.8941(3) 0.7518(2) 0.1436(3) 0.0253(8) Uani 1.0 2 d . . . C(14) C 1.0278(3) 0.8282(3) 0.1947(3) 0.0278(9) Uani 1.0 2 d . . . C(15) C 1.0695(4) 0.9110(3) 0.1349(3) 0.0356(10) Uani 1.0 2 d . . . C(16) C 1.1992(4) 0.9846(3) 0.1888(3) 0.0428(11) Uani 1.0 2 d . . . C(17) C 1.2992(4) 0.9787(3) 0.3050(3) 0.0433(11) Uani 1.0 2 d . . . C(18) C 1.2641(4) 0.9015(3) 0.3656(3) 0.0386(10) Uani 1.0 2 d . . . C(19) C 1.1273(3) 0.8243(3) 0.3134(3) 0.0303(9) Uani 1.0 2 d . . . C(20) C 0.9682(3) 0.6792(3) 0.3301(3) 0.0313(9) Uani 1.0 2 d . . . C(21) C 0.9341(4) 0.6026(3) 0.3997(3) 0.0391(10) Uani 1.0 2 d . . . C(22) C 0.8068(4) 0.5257(3) 0.3546(3) 0.0413(11) Uani 1.0 2 d . . . C(23) C 0.7030(4) 0.5197(3) 0.2363(3) 0.0389(10) Uani 1.0 2 d . . . C(24) C 0.7308(3) 0.5912(3) 0.1659(3) 0.0325(9) Uani 1.0 2 d . . . C(25) C 0.8624(3) 0.6742(3) 0.2109(3) 0.0266(8) Uani 1.0 2 d . . . C(26) C 0.5909(3) 0.8613(3) 0.0477(3) 0.0283(9) Uani 1.0 2 d . . . C(27) C 0.6993(3) 0.9591(3) 0.1395(3) 0.0307(9) Uani 1.0 2 d . . . C(28) C 0.7599(4) 1.0487(3) 0.1025(3) 0.0380(10) Uani 1.0 2 d . . . C(29) C 0.8640(4) 1.1387(3) 0.1822(4) 0.0479(12) Uani 1.0 2 d . . . C(30) C 0.9042(4) 1.1408(3) 0.3035(4) 0.0515(12) Uani 1.0 2 d . . . C(31) C 0.8447(4) 1.0542(3) 0.3440(3) 0.0469(11) Uani 1.0 2 d . . . C(32) C 0.7434(3) 0.9616(3) 0.2625(3) 0.0345(9) Uani 1.0 2 d . . . C(33) C 0.5590(4) 0.7956(3) 0.2263(3) 0.0351(10) Uani 1.0 2 d . . . C(34) C 0.4800(4) 0.7232(3) 0.2725(4) 0.0486(12) Uani 1.0 2 d . . . C(35) C 0.3612(4) 0.6425(3) 0.1966(4) 0.0554(14) Uani 1.0 2 d . . . C(36) C 0.3154(4) 0.6307(3) 0.0746(4) 0.0522(13) Uani 1.0 2 d . . . C(37) C 0.3891(4) 0.7047(3) 0.0285(3) 0.0394(10) Uani 1.0 2 d . . . C(38) C 0.5095(3) 0.7868(3) 0.1028(3) 0.0304(9) Uani 1.0 2 d . . . C(39) C 0.7565(6) 0.8589(4) 0.4274(4) 0.0614(14) Uani 1.0 2 d . . . H(1) H 1.021(3) 0.621(3) -0.027(3) 0.059(10) Uiso 1.0 2 d . . . H(2) H 0.985(3) 0.537(3) -0.229(3) 0.051(9) Uiso 1.0 2 d . . . H(3) H 0.772(3) 0.552(3) -0.402(3) 0.059(10) Uiso 1.0 2 d . . . H(4) H 0.517(4) 0.627(3) -0.486(3) 0.071(11) Uiso 1.0 2 d . . . H(5) H 0.342(3) 0.737(2) -0.433(3) 0.042(9) Uiso 1.0 2 d . . . H(6) H 0.392(3) 0.825(3) -0.226(3) 0.045(9) Uiso 1.0 2 d . . . H(7) H 0.993(3) 0.915(2) 0.050(3) 0.039(8) Uiso 1.0 2 d . . . H(8) H 1.223(3) 1.049(2) 0.145(2) 0.028(7) Uiso 1.0 2 d . . . H(9) H 1.404(3) 1.035(2) 0.348(3) 0.042(8) Uiso 1.0 2 d . . . H(10) H 1.334(3) 0.902(3) 0.445(3) 0.038(9) Uiso 1.0 2 d . . . H(11) H 1.009(3) 0.610(3) 0.480(3) 0.041(9) Uiso 1.0 2 d . . . H(12) H 0.773(3) 0.463(2) 0.401(2) 0.037(8) Uiso 1.0 2 d . . . H(13) H 0.603(3) 0.457(3) 0.199(3) 0.045(9) Uiso 1.0 2 d . . . H(14) H 0.661(3) 0.5884(19) 0.080(2) 0.025(7) Uiso 1.0 2 d . . . H(15) H 0.724(3) 1.046(2) 0.014(2) 0.027(8) Uiso 1.0 2 d . . . H(16) H 0.903(3) 1.202(3) 0.150(3) 0.045(9) Uiso 1.0 2 d . . . H(17) H 0.983(4) 1.209(3) 0.366(3) 0.080(12) Uiso 1.0 2 d . . . H(18) H 0.875(4) 1.058(3) 0.438(3) 0.073(11) Uiso 1.0 2 d . . . H(19) H 0.520(3) 0.735(3) 0.361(3) 0.045(9) Uiso 1.0 2 d . . . H(20) H 0.309(3) 0.587(3) 0.237(3) 0.046(9) Uiso 1.0 2 d . . . H(21) H 0.222(3) 0.562(3) 0.019(3) 0.049(9) Uiso 1.0 2 d . . . H(22) H 0.354(4) 0.700(3) -0.064(3) 0.076(12) Uiso 1.0 2 d . . . H(23) H 0.753(3) 0.774(3) 0.430(3) 0.050(9) Uiso 1.0 2 d . . . H(24) H 0.867(4) 0.896(3) 0.458(3) 0.059(11) Uiso 1.0 2 d . . . H(25) H 0.703(4) 0.902(4) 0.477(4) 0.110(16) Uiso 1.0 2 d . . . H(26) H 0.511(3) 0.8996(19) -0.014(2) 0.024(7) Uiso 1.0 2 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 N(1) 0.0375(16) 0.0352(15) 0.0298(15) 0.0063(13) 0.0101(13) 0.0066(12) N(2) 0.0566(18) 0.0431(17) 0.0234(15) 0.0117(14) 0.0119(14) 0.0087(13) C(1) 0.0314(17) 0.0310(17) 0.0290(17) 0.0010(14) 0.0173(15) 0.0075(14) C(2) 0.039(2) 0.038(2) 0.045(2) -0.0002(16) 0.0261(18) 0.0026(16) C(3) 0.053(3) 0.046(3) 0.057(3) 0.0068(18) 0.039(2) 0.0041(19) C(4) 0.066(3) 0.038(2) 0.044(3) -0.0009(18) 0.039(2) 0.0001(17) C(5) 0.049(2) 0.0356(19) 0.0291(18) -0.0070(16) 0.0197(17) 0.0041(15) C(6) 0.062(3) 0.040(2) 0.0266(19) -0.0101(18) 0.0147(19) 0.0073(16) C(7) 0.045(2) 0.040(2) 0.031(2) -0.0056(17) 0.0068(17) 0.0110(16) C(8) 0.0378(19) 0.0356(19) 0.0296(18) -0.0057(15) 0.0108(16) 0.0090(15) C(9) 0.0322(17) 0.0302(17) 0.0271(17) 0.0015(14) 0.0134(14) 0.0097(14) C(10) 0.0384(18) 0.0249(16) 0.0269(17) -0.0028(14) 0.0168(15) 0.0036(13) C(11) 0.0294(16) 0.0259(16) 0.0244(16) 0.0018(13) 0.0114(14) 0.0056(13) C(12) 0.0324(17) 0.0269(16) 0.0262(16) 0.0013(13) 0.0152(14) 0.0054(13) C(13) 0.0258(16) 0.0248(16) 0.0264(16) 0.0068(13) 0.0114(14) 0.0027(13) C(14) 0.0288(17) 0.0285(17) 0.0265(16) 0.0062(14) 0.0115(14) 0.0034(13) C(15) 0.0385(19) 0.0388(19) 0.0322(19) 0.0057(16) 0.0164(16) 0.0080(16) C(16) 0.043(2) 0.041(2) 0.048(3) -0.0044(17) 0.0253(18) 0.0073(17) C(17) 0.036(2) 0.039(2) 0.049(3) -0.0047(16) 0.0170(18) -0.0025(17) C(18) 0.0316(19) 0.043(2) 0.032(2) 0.0022(16) 0.0065(16) -0.0020(16) C(19) 0.0293(17) 0.0319(17) 0.0282(17) 0.0059(14) 0.0103(14) 0.0030(14) C(20) 0.0372(18) 0.0315(17) 0.0273(17) 0.0101(15) 0.0127(15) 0.0089(14) C(21) 0.053(3) 0.0356(19) 0.032(2) 0.0130(17) 0.0167(18) 0.0114(16) C(22) 0.055(3) 0.0356(19) 0.042(2) 0.0094(17) 0.0265(18) 0.0144(17) C(23) 0.043(2) 0.0347(19) 0.047(2) 0.0076(16) 0.0247(18) 0.0105(16) C(24) 0.0301(18) 0.0340(18) 0.0351(19) 0.0086(14) 0.0131(15) 0.0084(15) C(25) 0.0263(16) 0.0269(16) 0.0276(17) 0.0069(13) 0.0108(14) 0.0060(13) C(26) 0.0293(17) 0.0280(17) 0.0269(17) 0.0046(14) 0.0098(14) 0.0063(14) C(27) 0.0304(17) 0.0298(17) 0.0318(18) 0.0057(14) 0.0124(14) 0.0046(14) C(28) 0.042(2) 0.0361(19) 0.040(2) 0.0112(16) 0.0199(17) 0.0079(17) C(29) 0.044(3) 0.036(2) 0.064(3) 0.0004(17) 0.024(2) 0.0068(19) C(30) 0.043(3) 0.045(3) 0.049(3) 0.0066(18) 0.0041(19) -0.0055(19) C(31) 0.051(3) 0.042(2) 0.034(2) 0.0097(17) 0.0050(18) -0.0012(17) C(32) 0.0382(19) 0.0330(18) 0.0304(18) 0.0111(15) 0.0101(15) 0.0056(15) C(33) 0.0414(19) 0.0337(18) 0.0388(19) 0.0138(15) 0.0225(16) 0.0091(15) C(34) 0.069(3) 0.048(3) 0.050(3) 0.024(2) 0.040(3) 0.020(2) C(35) 0.059(3) 0.048(3) 0.085(3) 0.016(2) 0.050(3) 0.028(3) C(36) 0.037(2) 0.046(3) 0.083(3) 0.0052(17) 0.034(2) 0.018(3) C(37) 0.0304(18) 0.039(2) 0.049(3) 0.0056(15) 0.0152(17) 0.0088(17) C(38) 0.0299(17) 0.0305(17) 0.0348(18) 0.0072(14) 0.0161(15) 0.0075(14) C(39) 0.096(4) 0.050(3) 0.032(3) 0.020(3) 0.015(3) 0.013(2) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'CRYSTALS (Carruthers, et al., 1999)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 N(1) C(19) 1.348(5) yes . . N(1) C(20) 1.350(4) yes . . N(2) C(32) 1.398(5) yes . . N(2) C(33) 1.393(4) yes . . N(2) C(39) 1.460(5) yes . . C(1) C(2) 1.366(5) yes . . C(1) C(10) 1.412(4) yes . . C(1) C(11) 1.474(5) yes . . C(2) C(3) 1.425(6) yes . . C(3) C(4) 1.379(5) yes . . C(4) C(5) 1.428(6) yes . . C(5) C(6) 1.432(5) yes . . C(5) C(10) 1.396(5) yes . . C(6) C(7) 1.371(6) yes . . C(7) C(8) 1.429(5) yes . . C(8) C(9) 1.368(4) yes . . C(9) C(10) 1.410(5) yes . . C(9) C(12) 1.479(4) yes . . C(11) C(12) 1.369(4) yes . . C(11) C(13) 1.480(4) yes . . C(12) C(26) 1.525(5) yes . . C(13) C(14) 1.398(4) yes . . C(13) C(25) 1.408(5) yes . . C(14) C(15) 1.425(5) yes . . C(14) C(19) 1.431(4) yes . . C(15) C(16) 1.354(4) yes . . C(16) C(17) 1.416(5) yes . . C(17) C(18) 1.357(6) yes . . C(18) C(19) 1.424(4) yes . . C(20) C(21) 1.430(5) yes . . C(20) C(25) 1.435(4) yes . . C(21) C(22) 1.357(5) yes . . C(22) C(23) 1.417(4) yes . . C(23) C(24) 1.372(5) yes . . C(24) C(25) 1.426(4) yes . . C(26) C(27) 1.507(4) yes . . C(26) C(38) 1.523(5) yes . . C(27) C(28) 1.385(5) yes . . C(27) C(32) 1.400(5) yes . . C(28) C(29) 1.383(4) yes . . C(29) C(30) 1.384(6) yes . . C(30) C(31) 1.378(6) yes . . C(31) C(32) 1.398(4) yes . . C(33) C(34) 1.416(6) yes . . C(33) C(38) 1.391(5) yes . . C(34) C(35) 1.373(5) yes . . C(35) C(36) 1.374(6) yes . . C(36) C(37) 1.394(6) yes . . C(37) C(38) 1.386(4) yes . . C(2) H(1) 1.07(3) no . . C(3) H(2) 1.02(4) no . . C(4) H(3) 1.04(3) no . . C(6) H(4) 1.08(4) no . . C(7) H(5) 1.06(3) no . . C(8) H(6) 1.08(3) no . . C(15) H(7) 1.05(3) no . . C(16) H(8) 1.06(3) no . . C(17) H(9) 1.08(3) no . . C(18) H(10) 0.96(3) no . . C(21) H(11) 0.97(3) no . . C(22) H(12) 1.10(3) no . . C(23) H(13) 1.08(3) no . . C(24) H(14) 1.02(2) no . . C(26) H(26) 1.06(3) no . . C(28) H(15) 1.00(3) no . . C(29) H(16) 1.01(3) no . . C(30) H(17) 1.05(3) no . . C(31) H(18) 1.07(4) no . . C(34) H(19) 0.99(3) no . . C(35) H(20) 1.07(3) no . . C(36) H(21) 1.10(3) no . . C(37) H(22) 1.04(4) no . . C(39) H(23) 1.02(3) no . . C(39) H(24) 1.04(3) no . . C(39) H(25) 1.06(5) no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C(19) N(1) C(20) 117.2(3) yes . . . C(32) N(2) C(33) 120.7(3) yes . . . C(32) N(2) C(39) 120.0(3) yes . . . C(33) N(2) C(39) 119.3(3) yes . . . C(2) C(1) C(10) 118.6(3) yes . . . C(2) C(1) C(11) 135.3(3) yes . . . C(10) C(1) C(11) 106.1(3) yes . . . C(1) C(2) C(3) 119.0(3) yes . . . C(2) C(3) C(4) 122.0(4) yes . . . C(3) C(4) C(5) 120.2(4) yes . . . C(4) C(5) C(6) 129.2(3) yes . . . C(4) C(5) C(10) 115.9(3) yes . . . C(6) C(5) C(10) 115.0(4) yes . . . C(5) C(6) C(7) 120.6(3) yes . . . C(6) C(7) C(8) 122.5(3) yes . . . C(7) C(8) C(9) 118.3(4) yes . . . C(8) C(9) C(10) 118.5(3) yes . . . C(8) C(9) C(12) 135.7(3) yes . . . C(10) C(9) C(12) 105.7(3) yes . . . C(1) C(10) C(5) 124.3(3) yes . . . C(1) C(10) C(9) 110.6(3) yes . . . C(5) C(10) C(9) 125.1(3) yes . . . C(1) C(11) C(12) 108.7(3) yes . . . C(1) C(11) C(13) 122.1(3) yes . . . C(12) C(11) C(13) 129.2(3) yes . . . C(9) C(12) C(11) 108.9(3) yes . . . C(9) C(12) C(26) 122.4(3) yes . . . C(11) C(12) C(26) 128.7(3) yes . . . C(11) C(13) C(14) 120.9(3) yes . . . C(11) C(13) C(25) 120.2(2) yes . . . C(14) C(13) C(25) 118.8(3) yes . . . C(13) C(14) C(15) 123.2(3) yes . . . C(13) C(14) C(19) 118.6(3) yes . . . C(15) C(14) C(19) 118.2(3) yes . . . C(14) C(15) C(16) 121.1(3) yes . . . C(15) C(16) C(17) 120.6(4) yes . . . C(16) C(17) C(18) 120.4(3) yes . . . C(17) C(18) C(19) 120.8(3) yes . . . N(1) C(19) C(14) 123.6(3) yes . . . N(1) C(19) C(18) 117.6(3) yes . . . C(14) C(19) C(18) 118.8(3) yes . . . N(1) C(20) C(21) 118.3(3) yes . . . N(1) C(20) C(25) 123.6(3) yes . . . C(21) C(20) C(25) 118.1(3) yes . . . C(20) C(21) C(22) 121.6(3) yes . . . C(21) C(22) C(23) 120.4(4) yes . . . C(22) C(23) C(24) 120.3(3) yes . . . C(23) C(24) C(25) 120.8(3) yes . . . C(13) C(25) C(20) 118.1(3) yes . . . C(13) C(25) C(24) 123.1(3) yes . . . C(20) C(25) C(24) 118.8(3) yes . . . C(12) C(26) C(27) 112.8(3) yes . . . C(12) C(26) C(38) 111.5(3) yes . . . C(27) C(26) C(38) 111.9(3) yes . . . C(26) C(27) C(28) 119.8(3) yes . . . C(26) C(27) C(32) 121.9(3) yes . . . C(28) C(27) C(32) 118.4(3) yes . . . C(27) C(28) C(29) 122.5(4) yes . . . C(28) C(29) C(30) 118.3(4) yes . . . C(29) C(30) C(31) 121.0(3) yes . . . C(30) C(31) C(32) 120.2(4) yes . . . N(2) C(32) C(27) 119.9(3) yes . . . N(2) C(32) C(31) 120.4(3) yes . . . C(27) C(32) C(31) 119.6(3) yes . . . N(2) C(33) C(34) 120.5(3) yes . . . N(2) C(33) C(38) 120.9(3) yes . . . C(34) C(33) C(38) 118.6(3) yes . . . C(33) C(34) C(35) 120.5(4) yes . . . C(34) C(35) C(36) 121.0(4) yes . . . C(35) C(36) C(37) 118.8(3) yes . . . C(36) C(37) C(38) 121.5(4) yes . . . C(26) C(38) C(33) 121.0(3) yes . . . C(26) C(38) C(37) 119.3(3) yes . . . C(33) C(38) C(37) 119.6(3) yes . . . C(1) C(2) H(1) 123.9(18) no . . . C(3) C(2) H(1) 117.0(18) no . . . C(2) C(3) H(2) 120.2(15) no . . . C(4) C(3) H(2) 117.8(15) no . . . C(3) C(4) H(3) 122.3(16) no . . . C(5) C(4) H(3) 117.4(16) no . . . C(5) C(6) H(4) 116.4(17) no . . . C(7) C(6) H(4) 123.0(17) no . . . C(6) C(7) H(5) 120.0(16) no . . . C(8) C(7) H(5) 117.4(17) no . . . C(7) C(8) H(6) 119.3(13) no . . . C(9) C(8) H(6) 122.4(13) no . . . C(14) C(15) H(7) 117.0(15) no . . . C(16) C(15) H(7) 121.8(15) no . . . C(15) C(16) H(8) 119.4(11) no . . . C(17) C(16) H(8) 120.0(10) no . . . C(16) C(17) H(9) 121.4(15) no . . . C(18) C(17) H(9) 118.2(15) no . . . C(17) C(18) H(10) 117.6(17) no . . . C(19) C(18) H(10) 121.6(17) no . . . C(20) C(21) H(11) 114.8(17) no . . . C(22) C(21) H(11) 123.6(18) no . . . C(21) C(22) H(12) 126.1(11) no . . . C(23) C(22) H(12) 113.5(11) no . . . C(22) C(23) H(13) 120.9(15) no . . . C(24) C(23) H(13) 118.7(15) no . . . C(23) C(24) H(14) 123.1(14) no . . . C(25) C(24) H(14) 116.1(14) no . . . C(12) C(26) H(26) 107.1(15) no . . . C(27) C(26) H(26) 105.8(11) no . . . C(38) C(26) H(26) 107.3(15) no . . . C(27) C(28) H(15) 116.7(14) no . . . C(29) C(28) H(15) 120.8(14) no . . . C(28) C(29) H(16) 119.1(13) no . . . C(30) C(29) H(16) 122.6(13) no . . . C(29) C(30) H(17) 120(2) no . . . C(31) C(30) H(17) 119(2) no . . . C(30) C(31) H(18) 120.3(16) no . . . C(32) C(31) H(18) 119.5(16) no . . . C(33) C(34) H(19) 114.6(17) no . . . C(35) C(34) H(19) 124.9(17) no . . . C(34) C(35) H(20) 117.2(12) no . . . C(36) C(35) H(20) 121.8(12) no . . . C(35) C(36) H(21) 117.4(17) no . . . C(37) C(36) H(21) 123.8(17) no . . . C(36) C(37) H(22) 120.5(17) no . . . C(38) C(37) H(22) 118.0(17) no . . . N(2) C(39) H(23) 108.8(15) no . . . N(2) C(39) H(24) 107.5(19) no . . . N(2) C(39) H(25) 108(2) no . . . H(23) C(39) H(24) 108(3) no . . . H(23) C(39) H(25) 114(3) no . . . H(24) C(39) H(25) 110(3) no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C(19) N(1) C(20) C(21) -179.3(3) no . . . . C(19) N(1) C(20) C(25) 0.6(5) no . . . . C(20) N(1) C(19) C(14) 0.9(5) no . . . . C(20) N(1) C(19) C(18) 180.0(3) no . . . . C(32) N(2) C(33) C(34) -164.9(3) no . . . . C(32) N(2) C(33) C(38) 16.3(5) no . . . . C(33) N(2) C(32) C(27) -15.6(5) no . . . . C(33) N(2) C(32) C(31) 163.8(3) no . . . . C(39) N(2) C(32) C(27) 164.4(4) no . . . . C(39) N(2) C(32) C(31) -16.2(5) no . . . . C(39) N(2) C(33) C(34) 15.1(5) no . . . . C(39) N(2) C(33) C(38) -163.7(4) no . . . . C(2) C(1) C(10) C(5) 1.0(5) no . . . . C(2) C(1) C(10) C(9) -178.9(3) no . . . . C(10) C(1) C(2) C(3) 0.2(5) no . . . . C(2) C(1) C(11) C(12) 178.5(4) no . . . . C(2) C(1) C(11) C(13) -3.9(5) no . . . . C(11) C(1) C(2) C(3) -178.6(3) no . . . . C(10) C(1) C(11) C(12) -0.3(3) no . . . . C(10) C(1) C(11) C(13) 177.2(3) no . . . . C(11) C(1) C(10) C(5) -180.0(3) no . . . . C(11) C(1) C(10) C(9) 0.2(3) no . . . . C(1) C(2) C(3) C(4) -0.4(5) no . . . . C(2) C(3) C(4) C(5) -0.5(6) no . . . . C(3) C(4) C(5) C(6) -179.0(3) no . . . . C(3) C(4) C(5) C(10) 1.5(5) no . . . . C(4) C(5) C(6) C(7) -178.2(3) no . . . . C(4) C(5) C(10) C(1) -1.7(5) no . . . . C(4) C(5) C(10) C(9) 178.1(3) no . . . . C(6) C(5) C(10) C(1) 178.7(3) no . . . . C(6) C(5) C(10) C(9) -1.5(5) no . . . . C(10) C(5) C(6) C(7) 1.3(5) no . . . . C(5) C(6) C(7) C(8) -0.4(6) no . . . . C(6) C(7) C(8) C(9) -0.5(5) no . . . . C(7) C(8) C(9) C(10) 0.4(5) no . . . . C(7) C(8) C(9) C(12) -179.0(3) no . . . . C(8) C(9) C(10) C(1) -179.5(3) no . . . . C(8) C(9) C(10) C(5) 0.6(5) no . . . . C(8) C(9) C(12) C(11) 179.2(4) no . . . . C(8) C(9) C(12) C(26) -1.6(6) no . . . . C(10) C(9) C(12) C(11) -0.2(3) no . . . . C(10) C(9) C(12) C(26) 178.9(3) no . . . . C(12) C(9) C(10) C(1) 0.0(3) no . . . . C(12) C(9) C(10) C(5) -179.8(3) no . . . . C(1) C(11) C(12) C(9) 0.3(3) no . . . . C(1) C(11) C(12) C(26) -178.8(3) no . . . . C(1) C(11) C(13) C(14) 79.7(4) no . . . . C(1) C(11) C(13) C(25) -96.7(4) no . . . . C(12) C(11) C(13) C(14) -103.3(4) no . . . . C(12) C(11) C(13) C(25) 80.3(4) no . . . . C(13) C(11) C(12) C(9) -177.0(3) no . . . . C(13) C(11) C(12) C(26) 3.9(5) no . . . . C(9) C(12) C(26) C(27) -131.6(3) no . . . . C(9) C(12) C(26) C(38) 101.4(3) no . . . . C(11) C(12) C(26) C(27) 47.4(4) no . . . . C(11) C(12) C(26) C(38) -79.6(4) no . . . . C(11) C(13) C(14) C(15) 4.5(5) no . . . . C(11) C(13) C(14) C(19) -176.2(3) no . . . . C(11) C(13) C(25) C(20) 177.7(3) no . . . . C(11) C(13) C(25) C(24) -2.1(5) no . . . . C(14) C(13) C(25) C(20) 1.2(4) no . . . . C(14) C(13) C(25) C(24) -178.6(3) no . . . . C(25) C(13) C(14) C(15) -179.1(3) no . . . . C(25) C(13) C(14) C(19) 0.2(4) no . . . . C(13) C(14) C(15) C(16) 178.9(3) no . . . . C(13) C(14) C(19) N(1) -1.3(5) no . . . . C(13) C(14) C(19) C(18) 179.7(3) no . . . . C(15) C(14) C(19) N(1) 178.0(3) no . . . . C(15) C(14) C(19) C(18) -1.0(5) no . . . . C(19) C(14) C(15) C(16) -0.4(5) no . . . . C(14) C(15) C(16) C(17) 2.0(6) no . . . . C(15) C(16) C(17) C(18) -2.3(6) no . . . . C(16) C(17) C(18) C(19) 0.8(6) no . . . . C(17) C(18) C(19) N(1) -178.2(3) no . . . . C(17) C(18) C(19) C(14) 0.8(5) no . . . . N(1) C(20) C(21) C(22) -178.9(3) no . . . . N(1) C(20) C(25) C(13) -1.7(5) no . . . . N(1) C(20) C(25) C(24) 178.1(3) no . . . . C(21) C(20) C(25) C(13) 178.3(3) no . . . . C(21) C(20) C(25) C(24) -2.0(5) no . . . . C(25) C(20) C(21) C(22) 1.1(5) no . . . . C(20) C(21) C(22) C(23) -0.3(6) no . . . . C(21) C(22) C(23) C(24) 0.4(6) no . . . . C(22) C(23) C(24) C(25) -1.3(5) no . . . . C(23) C(24) C(25) C(13) -178.1(3) no . . . . C(23) C(24) C(25) C(20) 2.1(5) no . . . . C(12) C(26) C(27) C(28) 66.9(4) no . . . . C(12) C(26) C(27) C(32) -112.0(3) no . . . . C(12) C(26) C(38) C(33) 113.4(3) no . . . . C(12) C(26) C(38) C(37) -63.1(3) no . . . . C(27) C(26) C(38) C(33) -14.1(4) no . . . . C(27) C(26) C(38) C(37) 169.4(3) no . . . . C(38) C(26) C(27) C(28) -166.4(3) no . . . . C(38) C(26) C(27) C(32) 14.7(4) no . . . . C(26) C(27) C(28) C(29) -177.6(3) no . . . . C(26) C(27) C(32) N(2) -0.8(5) no . . . . C(26) C(27) C(32) C(31) 179.8(3) no . . . . C(28) C(27) C(32) N(2) -179.7(3) no . . . . C(28) C(27) C(32) C(31) 0.9(5) no . . . . C(32) C(27) C(28) C(29) 1.4(5) no . . . . C(27) C(28) C(29) C(30) -2.5(5) no . . . . C(28) C(29) C(30) C(31) 1.4(6) no . . . . C(29) C(30) C(31) C(32) 0.8(6) no . . . . C(30) C(31) C(32) N(2) 178.7(3) no . . . . C(30) C(31) C(32) C(27) -1.9(5) no . . . . N(2) C(33) C(34) C(35) -175.9(3) no . . . . N(2) C(33) C(38) C(26) -0.4(5) no . . . . N(2) C(33) C(38) C(37) 176.1(3) no . . . . C(34) C(33) C(38) C(26) -179.3(3) no . . . . C(34) C(33) C(38) C(37) -2.8(5) no . . . . C(38) C(33) C(34) C(35) 2.9(5) no . . . . C(33) C(34) C(35) C(36) -0.5(6) no . . . . C(34) C(35) C(36) C(37) -2.0(6) no . . . . C(35) C(36) C(37) C(38) 2.1(6) no . . . . C(36) C(37) C(38) C(26) 176.9(3) no . . . . C(36) C(37) C(38) C(33) 0.4(5) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 C(18) C(34) 3.522(6) no . 1_655 C(24) C(36) 3.541(5) no . 2_665 C(34) C(18) 3.522(6) no . 1_455 C(36) C(24) 3.541(5) no . 2_665 N(1) H(2) 3.55(3) no . 2_765 N(1) H(5) 2.68(3) no . 1_656 N(1) H(17) 3.46(4) no . 2_776 N(1) H(18) 2.87(3) no . 2_776 C(1) H(8) 3.38(3) no . 2_775 C(1) H(16) 3.37(3) no . 2_775 C(1) H(20) 3.39(3) no . 2_665 C(1) H(21) 3.21(3) no . 2_665 C(2) H(1) 3.55(3) no . 2_765 C(2) H(16) 2.81(3) no . 2_775 C(2) H(20) 3.09(3) no . 2_665 C(2) H(21) 3.01(3) no . 1_655 C(2) H(21) 3.04(3) no . 2_665 C(3) H(16) 2.85(3) no . 2_775 C(3) H(20) 2.71(3) no . 2_665 C(3) H(21) 3.42(3) no . 1_655 C(4) H(12) 3.53(3) no . 1_554 C(4) H(16) 3.47(3) no . 2_775 C(4) H(17) 3.40(4) no . 2_775 C(4) H(20) 2.70(3) no . 2_665 C(5) H(20) 3.06(3) no . 2_665 C(6) H(4) 3.52(3) no . 2_664 C(6) H(9) 3.49(3) no . 2_775 C(6) H(12) 3.27(3) no . 2_665 C(6) H(19) 3.15(4) no . 1_554 C(7) H(9) 3.02(3) no . 2_775 C(7) H(10) 3.29(3) no . 1_454 C(7) H(12) 2.82(3) no . 2_665 C(7) H(13) 3.31(3) no . 2_665 C(8) H(8) 3.22(3) no . 2_775 C(8) H(9) 3.12(3) no . 2_775 C(8) H(12) 3.35(2) no . 2_665 C(8) H(13) 2.98(3) no . 2_665 C(9) H(8) 2.73(3) no . 2_775 C(9) H(13) 2.93(3) no . 2_665 C(10) H(8) 3.01(3) no . 2_775 C(10) H(13) 3.22(3) no . 2_665 C(10) H(20) 3.35(3) no . 2_665 C(11) H(8) 3.34(3) no . 2_775 C(12) H(8) 2.97(3) no . 2_775 C(12) H(13) 3.57(3) no . 2_665 C(15) H(7) 3.22(3) no . 2_775 C(15) H(15) 3.25(3) no . 2_775 C(16) H(7) 3.30(3) no . 2_775 C(16) H(15) 2.84(3) no . 2_775 C(17) H(25) 2.85(5) no . 2_776 C(18) H(5) 3.29(3) no . 1_656 C(18) H(18) 3.19(4) no . 2_776 C(18) H(19) 3.38(3) no . 1_655 C(18) H(25) 2.73(4) no . 2_776 C(19) H(5) 3.42(3) no . 1_656 C(19) H(18) 3.18(4) no . 2_776 C(20) H(2) 2.87(3) no . 2_765 C(21) H(2) 2.88(4) no . 2_765 C(21) H(3) 3.44(4) no . 1_556 C(21) H(3) 3.58(4) no . 2_765 C(21) H(11) 3.11(3) no . 2_766 C(21) H(12) 3.26(3) no . 2_766 C(21) H(17) 3.18(3) no . 2_776 C(22) H(2) 3.07(4) no . 2_765 C(22) H(3) 3.10(4) no . 1_556 C(22) H(11) 2.97(3) no . 2_766 C(23) H(2) 3.24(4) no . 2_765 C(23) H(21) 3.50(4) no . 2_665 C(23) H(22) 3.00(3) no . 2_665 C(24) H(2) 3.22(3) no . 2_765 C(24) H(21) 2.91(3) no . 2_665 C(24) H(22) 3.44(3) no . 2_665 C(25) H(2) 3.06(3) no . 2_765 C(25) H(21) 3.49(3) no . 2_665 C(26) H(15) 3.25(3) no . 2_675 C(26) H(26) 3.15(3) no . 2_675 C(27) H(6) 3.00(3) no . 2_675 C(27) H(26) 2.92(3) no . 2_675 C(28) H(6) 2.88(3) no . 2_675 C(28) H(8) 3.16(3) no . 2_775 C(28) H(22) 3.34(4) no . 2_675 C(28) H(26) 2.65(3) no . 2_675 C(29) H(6) 2.82(3) no . 2_675 C(29) H(22) 3.12(3) no . 2_675 C(29) H(26) 3.44(2) no . 2_675 C(30) H(6) 2.80(3) no . 2_675 C(30) H(11) 3.51(3) no . 2_776 C(30) H(24) 3.08(3) no . 2_776 C(31) H(5) 3.52(3) no . 2_675 C(31) H(6) 2.89(3) no . 2_675 C(31) H(18) 3.58(3) no . 2_776 C(31) H(24) 2.91(3) no . 2_776 C(32) H(6) 3.01(3) no . 2_675 C(34) H(4) 3.23(4) no . 1_556 C(34) H(10) 3.57(3) no . 1_455 C(35) H(1) 3.41(3) no . 1_455 C(36) H(1) 2.68(3) no . 1_455 C(36) H(14) 3.09(3) no . 2_665 C(37) H(1) 3.44(3) no . 1_455 C(37) H(13) 3.19(3) no . 2_665 C(37) H(14) 3.49(3) no . 2_665 C(37) H(15) 3.33(3) no . 2_675 C(37) H(16) 3.31(3) no . 2_675 C(38) H(15) 3.26(3) no . 2_675 C(39) H(10) 3.42(3) no . 2_776 C(39) H(17) 3.13(3) no . 2_776 C(39) H(18) 3.36(3) no . 2_776 H(1) C(2) 3.55(3) no . 2_765 H(1) C(35) 3.41(3) no . 1_655 H(1) C(36) 2.68(3) no . 1_655 H(1) C(37) 3.44(3) no . 1_655 H(1) H(1) 3.08(5) no . 2_765 H(1) H(16) 2.95(5) no . 2_775 H(1) H(20) 3.52(4) no . 1_655 H(1) H(21) 2.07(4) no . 1_655 H(1) H(21) 3.12(5) no . 2_665 H(1) H(22) 3.53(5) no . 1_655 H(2) N(1) 3.55(3) no . 2_765 H(2) C(20) 2.87(3) no . 2_765 H(2) C(21) 2.88(4) no . 2_765 H(2) C(22) 3.07(4) no . 2_765 H(2) C(23) 3.24(4) no . 2_765 H(2) C(24) 3.22(3) no . 2_765 H(2) C(25) 3.06(3) no . 2_765 H(2) H(11) 3.34(5) no . 2_765 H(2) H(16) 3.09(4) no . 2_775 H(2) H(20) 3.09(4) no . 2_665 H(2) H(21) 3.02(4) no . 1_655 H(3) C(21) 3.44(4) no . 1_554 H(3) C(21) 3.58(4) no . 2_765 H(3) C(22) 3.10(4) no . 1_554 H(3) H(4) 3.11(4) no . 2_664 H(3) H(5) 3.59(4) no . 2_664 H(3) H(11) 3.23(5) no . 1_554 H(3) H(11) 3.34(5) no . 2_765 H(3) H(12) 2.50(5) no . 1_554 H(3) H(17) 3.42(5) no . 2_775 H(3) H(20) 3.07(5) no . 2_665 H(3) H(23) 3.55(5) no . 1_554 H(4) C(6) 3.52(3) no . 2_664 H(4) C(34) 3.23(4) no . 1_554 H(4) H(3) 3.11(4) no . 2_664 H(4) H(4) 2.98(5) no . 2_664 H(4) H(12) 3.51(5) no . 2_665 H(4) H(19) 2.42(5) no . 1_554 H(4) H(20) 3.19(4) no . 1_554 H(4) H(23) 3.32(5) no . 1_554 H(5) N(1) 2.68(3) no . 1_454 H(5) C(18) 3.29(3) no . 1_454 H(5) C(19) 3.42(3) no . 1_454 H(5) C(31) 3.52(3) no . 2_675 H(5) H(3) 3.59(4) no . 2_664 H(5) H(9) 3.27(4) no . 2_775 H(5) H(10) 2.63(4) no . 1_454 H(5) H(11) 3.19(4) no . 1_454 H(5) H(12) 2.68(4) no . 2_665 H(5) H(18) 3.40(5) no . 2_675 H(5) H(19) 3.57(5) no . 1_554 H(6) C(27) 3.00(3) no . 2_675 H(6) C(28) 2.88(3) no . 2_675 H(6) C(29) 2.82(3) no . 2_675 H(6) C(30) 2.80(3) no . 2_675 H(6) C(31) 2.89(3) no . 2_675 H(6) C(32) 3.01(3) no . 2_675 H(6) H(9) 3.36(5) no . 2_775 H(6) H(13) 3.44(4) no . 2_665 H(6) H(15) 3.44(4) no . 2_675 H(6) H(16) 3.36(5) no . 2_675 H(6) H(17) 3.40(4) no . 2_675 H(6) H(18) 3.51(4) no . 2_675 H(7) C(15) 3.22(3) no . 2_775 H(7) C(16) 3.30(3) no . 2_775 H(7) H(7) 2.53(4) no . 2_775 H(7) H(8) 2.66(3) no . 2_775 H(7) H(15) 3.18(4) no . 2_775 H(7) H(16) 3.20(5) no . 2_775 H(8) C(1) 3.38(3) no . 2_775 H(8) C(8) 3.22(3) no . 2_775 H(8) C(9) 2.73(3) no . 2_775 H(8) C(10) 3.01(3) no . 2_775 H(8) C(11) 3.34(3) no . 2_775 H(8) C(12) 2.97(3) no . 2_775 H(8) C(28) 3.16(3) no . 2_775 H(8) H(7) 2.66(3) no . 2_775 H(8) H(15) 2.37(4) no . 2_775 H(8) H(26) 3.59(4) no . 2_775 H(9) C(6) 3.49(3) no . 2_775 H(9) C(7) 3.02(3) no . 2_775 H(9) C(8) 3.12(3) no . 2_775 H(9) H(5) 3.27(4) no . 2_775 H(9) H(6) 3.36(5) no . 2_775 H(9) H(10) 2.81(3) no . 2_876 H(9) H(25) 3.44(5) no . 1_655 H(9) H(25) 2.76(6) no . 2_776 H(10) C(7) 3.29(3) no . 1_656 H(10) C(34) 3.57(3) no . 1_655 H(10) C(39) 3.42(3) no . 2_776 H(10) H(5) 2.63(4) no . 1_656 H(10) H(9) 2.81(3) no . 2_876 H(10) H(10) 3.52(4) no . 2_876 H(10) H(18) 2.95(5) no . 2_776 H(10) H(19) 3.16(5) no . 1_655 H(10) H(25) 3.50(5) no . 1_655 H(10) H(25) 2.51(5) no . 2_776 H(11) C(21) 3.11(3) no . 2_766 H(11) C(22) 2.97(3) no . 2_766 H(11) C(30) 3.51(3) no . 2_776 H(11) H(2) 3.34(5) no . 2_765 H(11) H(3) 3.23(5) no . 1_556 H(11) H(3) 3.34(5) no . 2_765 H(11) H(5) 3.19(4) no . 1_656 H(11) H(11) 2.74(4) no . 2_766 H(11) H(12) 2.43(4) no . 2_766 H(11) H(17) 2.64(5) no . 2_776 H(12) C(4) 3.53(3) no . 1_556 H(12) C(6) 3.27(3) no . 2_665 H(12) C(7) 2.82(3) no . 2_665 H(12) C(8) 3.35(2) no . 2_665 H(12) C(21) 3.26(3) no . 2_766 H(12) H(3) 2.50(5) no . 1_556 H(12) H(4) 3.51(5) no . 2_665 H(12) H(5) 2.68(4) no . 2_665 H(12) H(11) 2.43(4) no . 2_766 H(13) C(7) 3.31(3) no . 2_665 H(13) C(8) 2.98(3) no . 2_665 H(13) C(9) 2.93(3) no . 2_665 H(13) C(10) 3.22(3) no . 2_665 H(13) C(12) 3.57(3) no . 2_665 H(13) C(37) 3.19(3) no . 2_665 H(13) H(6) 3.44(4) no . 2_665 H(13) H(14) 3.36(3) no . 2_665 H(13) H(22) 2.51(5) no . 2_665 H(14) C(36) 3.09(3) no . 2_665 H(14) C(37) 3.49(3) no . 2_665 H(14) H(13) 3.36(3) no . 2_665 H(14) H(14) 3.36(3) no . 2_665 H(14) H(21) 2.62(4) no . 2_665 H(14) H(22) 3.42(4) no . 2_665 H(15) C(15) 3.25(3) no . 2_775 H(15) C(16) 2.84(3) no . 2_775 H(15) C(26) 3.25(3) no . 2_675 H(15) C(37) 3.33(3) no . 2_675 H(15) C(38) 3.26(3) no . 2_675 H(15) H(6) 3.44(4) no . 2_675 H(15) H(7) 3.18(4) no . 2_775 H(15) H(8) 2.37(4) no . 2_775 H(15) H(22) 3.24(4) no . 2_675 H(15) H(26) 2.46(4) no . 2_675 H(16) C(1) 3.37(3) no . 2_775 H(16) C(2) 2.81(3) no . 2_775 H(16) C(3) 2.85(3) no . 2_775 H(16) C(4) 3.47(3) no . 2_775 H(16) C(37) 3.31(3) no . 2_675 H(16) H(1) 2.95(5) no . 2_775 H(16) H(2) 3.09(4) no . 2_775 H(16) H(6) 3.36(5) no . 2_675 H(16) H(7) 3.20(5) no . 2_775 H(16) H(22) 2.80(4) no . 2_675 H(17) N(1) 3.46(4) no . 2_776 H(17) C(4) 3.40(4) no . 2_775 H(17) C(21) 3.18(3) no . 2_776 H(17) C(39) 3.13(3) no . 2_776 H(17) H(3) 3.42(5) no . 2_775 H(17) H(6) 3.40(4) no . 2_675 H(17) H(11) 2.64(5) no . 2_776 H(17) H(23) 2.83(4) no . 2_776 H(17) H(24) 2.67(5) no . 2_776 H(17) H(25) 3.49(5) no . 2_776 H(18) N(1) 2.87(3) no . 2_776 H(18) C(18) 3.19(4) no . 2_776 H(18) C(19) 3.18(4) no . 2_776 H(18) C(31) 3.58(3) no . 2_776 H(18) C(39) 3.36(3) no . 2_776 H(18) H(5) 3.40(5) no . 2_675 H(18) H(6) 3.51(4) no . 2_675 H(18) H(10) 2.95(5) no . 2_776 H(18) H(18) 2.96(5) no . 2_776 H(18) H(24) 2.35(4) no . 2_776 H(19) C(6) 3.15(4) no . 1_556 H(19) C(18) 3.38(3) no . 1_455 H(19) H(4) 2.42(5) no . 1_556 H(19) H(5) 3.57(5) no . 1_556 H(19) H(10) 3.16(5) no . 1_455 H(20) C(1) 3.39(3) no . 2_665 H(20) C(2) 3.09(3) no . 2_665 H(20) C(3) 2.71(3) no . 2_665 H(20) C(4) 2.70(3) no . 2_665 H(20) C(5) 3.06(3) no . 2_665 H(20) C(10) 3.35(3) no . 2_665 H(20) H(1) 3.52(4) no . 1_455 H(20) H(2) 3.09(4) no . 2_665 H(20) H(3) 3.07(5) no . 2_665 H(20) H(4) 3.19(4) no . 1_556 H(21) C(1) 3.21(3) no . 2_665 H(21) C(2) 3.01(3) no . 1_455 H(21) C(2) 3.04(3) no . 2_665 H(21) C(3) 3.42(3) no . 1_455 H(21) C(23) 3.50(4) no . 2_665 H(21) C(24) 2.91(3) no . 2_665 H(21) C(25) 3.49(3) no . 2_665 H(21) H(1) 2.07(4) no . 1_455 H(21) H(1) 3.12(5) no . 2_665 H(21) H(2) 3.02(4) no . 1_455 H(21) H(14) 2.62(4) no . 2_665 H(22) C(23) 3.00(3) no . 2_665 H(22) C(24) 3.44(3) no . 2_665 H(22) C(28) 3.34(4) no . 2_675 H(22) C(29) 3.12(3) no . 2_675 H(22) H(1) 3.53(5) no . 1_455 H(22) H(13) 2.51(5) no . 2_665 H(22) H(14) 3.42(4) no . 2_665 H(22) H(15) 3.24(4) no . 2_675 H(22) H(16) 2.80(4) no . 2_675 H(23) H(3) 3.55(5) no . 1_556 H(23) H(4) 3.32(5) no . 1_556 H(23) H(17) 2.83(4) no . 2_776 H(24) C(30) 3.08(3) no . 2_776 H(24) C(31) 2.91(3) no . 2_776 H(24) H(17) 2.67(5) no . 2_776 H(24) H(18) 2.35(4) no . 2_776 H(24) H(24) 3.17(4) no . 2_776 H(25) C(17) 2.85(5) no . 2_776 H(25) C(18) 2.73(4) no . 2_776 H(25) H(9) 3.44(5) no . 1_455 H(25) H(9) 2.76(6) no . 2_776 H(25) H(10) 3.50(5) no . 1_455 H(25) H(10) 2.51(5) no . 2_776 H(25) H(17) 3.49(5) no . 2_776 H(26) C(26) 3.15(3) no . 2_675 H(26) C(27) 2.92(3) no . 2_675 H(26) C(28) 2.65(3) no . 2_675 H(26) C(29) 3.44(2) no . 2_675 H(26) H(8) 3.59(4) no . 2_775 H(26) H(15) 2.46(4) no . 2_675 H(26) H(26) 2.42(4) no . 2_675 #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 975887' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data__051111tt #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C42 H30 Cl3 F3 N2 O3 S' _chemical_formula_moiety 'C42 H30 Cl3 F3 N2 O3 S' _chemical_formula_weight 806.12 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 14.643(4) _cell_length_b 31.409(8) _cell_length_c 16.869(5) _cell_angle_alpha 90.0000 _cell_angle_beta 105.429(6) _cell_angle_gamma 90.0000 _cell_volume 7479(4) _cell_formula_units_Z 8 _cell_measurement_reflns_used 13963 _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 27.48 _cell_measurement_temperature 295 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour red _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3312.00 _exptl_absorpt_coefficient_mu 0.359 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.774 _exptl_absorpt_correction_T_max 0.982 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 295 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_reflns_number 47016 _diffrn_reflns_av_R_equivalents 0.0846 _diffrn_reflns_theta_max 24.00 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 14 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 11687 _reflns_number_gt 3738 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0905 _refine_ls_wR_factor_ref 0.2065 _refine_ls_number_restraints ? _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 11681 _refine_ls_number_parameters 1054 _refine_ls_goodness_of_fit_ref 0.608 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0010Fo^2^ + 3.0000\s(Fo^2^) + 0.5000]/(4Fo^2^)' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.003 _refine_diff_density_max 1.080 _refine_diff_density_min -0.811 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; F F 0.0171 0.0103 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.1246 0.1234 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; C C 0.0033 0.0016 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.1484 0.1585 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Cl(1) Cl 0.3212(3) -0.12081(11) 0.3229(2) 0.1598(16) Uani 1.0 4 d . . . Cl(2) Cl 0.1714(4) -0.07760(13) 0.3571(3) 0.193(2) Uani 1.0 4 d . . . Cl(3) Cl 0.3265(3) -0.03105(12) 0.3448(3) 0.201(2) Uani 1.0 4 d . . . Cl(4) Cl 0.7681(3) 0.38062(11) 1.1287(2) 0.1558(15) Uani 1.0 4 d . . . Cl(5) Cl 0.6003(3) 0.42704(11) 1.10950(19) 0.1536(14) Uani 1.0 4 d . . . Cl(6) Cl 0.7713(3) 0.47112(11) 1.1271(2) 0.1587(16) Uani 1.0 4 d . . . S(1) S 0.29679(17) 0.07655(8) -0.08438(15) 0.0843(9) Uani 1.0 4 d . . . S(2) S 0.14911(16) -0.07836(7) 0.05154(13) 0.0704(8) Uani 1.0 4 d . . . F(1) F 0.4012(5) 0.0408(3) -0.1652(5) 0.183(4) Uani 1.0 4 d . . . F(2) F 0.4765(5) 0.0727(4) -0.0563(5) 0.219(4) Uani 1.0 4 d . . . F(3) F 0.3984(7) 0.1085(4) -0.1643(6) 0.218(5) Uani 1.0 4 d . . . F(4) F 0.3007(5) -0.0782(3) -0.0000(4) 0.154(3) Uani 1.0 4 d . . . F(5) F 0.3145(5) -0.0474(3) 0.1151(5) 0.152(3) Uani 1.0 4 d . . . F(6) F 0.3123(5) -0.1144(3) 0.1062(4) 0.161(3) Uani 1.0 4 d . . . O(1) O 0.3058(5) 0.11405(19) -0.0371(4) 0.118(3) Uani 1.0 4 d . . . O(2) O 0.3050(6) 0.0370(2) -0.0354(4) 0.146(4) Uani 1.0 4 d . . . O(3) O 0.2227(4) 0.07547(19) -0.1581(3) 0.091(2) Uani 1.0 4 d . . . O(4) O 0.1227(5) -0.03884(17) 0.0127(4) 0.092(3) Uani 1.0 4 d . . . O(5) O 0.1382(4) -0.08125(17) 0.1338(3) 0.078(2) Uani 1.0 4 d . . . O(6) O 0.1174(5) -0.11488(17) 0.0017(4) 0.102(3) Uani 1.0 4 d . . . N(1) N 0.5430(5) 0.30738(17) 0.3517(4) 0.057(2) Uani 1.0 4 d . . . N(2) N 0.4759(5) 0.2755(2) 0.1198(4) 0.066(3) Uani 1.0 4 d . . . N(3) N -0.0349(5) 0.03870(17) 0.1659(4) 0.055(2) Uani 1.0 4 d . . . N(4) N 0.0505(5) 0.0722(2) 0.3845(4) 0.061(3) Uani 1.0 4 d . . . C(1) C 0.4790(5) 0.1168(2) 0.1944(5) 0.047(3) Uani 1.0 4 d . . . C(2) C 0.4577(5) 0.0833(3) 0.1409(5) 0.063(3) Uani 1.0 4 d . . . C(3) C 0.4675(6) 0.0416(3) 0.1714(7) 0.080(4) Uani 1.0 4 d . . . C(4) C 0.4971(6) 0.0340(3) 0.2544(7) 0.085(4) Uani 1.0 4 d . . . C(5) C 0.5198(5) 0.0667(3) 0.3118(6) 0.061(3) Uani 1.0 4 d . . . C(6) C 0.5520(6) 0.0650(4) 0.3971(6) 0.083(4) Uani 1.0 4 d . . . C(7) C 0.5691(6) 0.0993(4) 0.4432(6) 0.085(4) Uani 1.0 4 d . . . C(8) C 0.5574(5) 0.1423(3) 0.4077(5) 0.066(3) Uani 1.0 4 d . . . C(9) C 0.5281(5) 0.1445(3) 0.3244(5) 0.051(3) Uani 1.0 4 d . . . C(10) C 0.5085(5) 0.1072(3) 0.2772(5) 0.052(3) Uani 1.0 4 d . . . C(11) C 0.4791(5) 0.1637(2) 0.1870(5) 0.049(3) Uani 1.0 4 d . . . C(12) C 0.5070(5) 0.1805(2) 0.2649(4) 0.046(3) Uani 1.0 4 d . . . C(13) C 0.5190(5) 0.2249(3) 0.2920(4) 0.049(3) Uani 1.0 4 d . . . C(14) C 0.6071(5) 0.2446(3) 0.3077(4) 0.048(3) Uani 1.0 4 d . . . C(15) C 0.6870(5) 0.2238(3) 0.2903(5) 0.063(3) Uani 1.0 4 d . . . C(16) C 0.7699(6) 0.2440(3) 0.3027(5) 0.072(3) Uani 1.0 4 d . . . C(17) C 0.7802(6) 0.2855(3) 0.3325(6) 0.087(4) Uani 1.0 4 d . . . C(18) C 0.7066(6) 0.3069(3) 0.3501(5) 0.075(3) Uani 1.0 4 d . . . C(19) C 0.6199(5) 0.2865(3) 0.3371(4) 0.053(3) Uani 1.0 4 d . . . C(20) C 0.4534(6) 0.2888(3) 0.3352(4) 0.054(3) Uani 1.0 4 d . . . C(21) C 0.3760(6) 0.3113(3) 0.3478(5) 0.070(3) Uani 1.0 4 d . . . C(22) C 0.2895(6) 0.2924(3) 0.3295(5) 0.077(4) Uani 1.0 4 d . . . C(23) C 0.2765(6) 0.2506(3) 0.3008(5) 0.069(3) Uani 1.0 4 d . . . C(24) C 0.3513(6) 0.2286(3) 0.2900(5) 0.056(3) Uani 1.0 4 d . . . C(25) C 0.4413(5) 0.2469(3) 0.3069(4) 0.048(3) Uani 1.0 4 d . . . C(26) C 0.4540(5) 0.1865(3) 0.1040(5) 0.050(3) Uani 1.0 4 d . . . C(27) C 0.5361(6) 0.2090(3) 0.0885(5) 0.061(3) Uani 1.0 4 d . . . C(28) C 0.6088(6) 0.1852(3) 0.0701(5) 0.071(3) Uani 1.0 4 d . . . C(29) C 0.6890(7) 0.2039(4) 0.0612(6) 0.094(4) Uani 1.0 4 d . . . C(30) C 0.6994(7) 0.2469(5) 0.0721(6) 0.106(5) Uani 1.0 4 d . . . C(31) C 0.6332(7) 0.2716(3) 0.0909(5) 0.074(3) Uani 1.0 4 d . . . C(32) C 0.5483(6) 0.2524(3) 0.0994(5) 0.064(3) Uani 1.0 4 d . . . C(33) C 0.3847(6) 0.2593(3) 0.1022(4) 0.053(3) Uani 1.0 4 d . . . C(34) C 0.3051(7) 0.2859(3) 0.0961(5) 0.075(3) Uani 1.0 4 d . . . C(35) C 0.2168(7) 0.2687(4) 0.0801(5) 0.086(4) Uani 1.0 4 d . . . C(36) C 0.2032(7) 0.2257(4) 0.0687(5) 0.086(4) Uani 1.0 4 d . . . C(37) C 0.2807(6) 0.2002(3) 0.0743(5) 0.067(3) Uani 1.0 4 d . . . C(38) C 0.3706(6) 0.2158(3) 0.0921(4) 0.054(3) Uani 1.0 4 d . . . C(39) C 0.5540(6) 0.3525(3) 0.3836(6) 0.104(4) Uani 1.0 4 d . . . C(40) C 0.4919(7) 0.3206(3) 0.1434(6) 0.088(4) Uani 1.0 4 d . . . C(41) C 0.0211(5) 0.2328(3) 0.3035(4) 0.047(3) Uani 1.0 4 d . . . C(42) C -0.0494(5) 0.2087(3) 0.0884(4) 0.053(3) Uani 1.0 4 d . . . C(43) C -0.0577(6) 0.2500(3) 0.0541(5) 0.065(3) Uani 1.0 4 d . . . C(44) C -0.0422(6) 0.2867(3) 0.0995(6) 0.067(3) Uani 1.0 4 d . . . C(45) C -0.0144(5) 0.2840(3) 0.1879(5) 0.059(3) Uani 1.0 4 d . . . C(46) C 0.0047(5) 0.3175(3) 0.2461(6) 0.068(3) Uani 1.0 4 d . . . C(47) C 0.0318(5) 0.3081(3) 0.3275(6) 0.067(3) Uani 1.0 4 d . . . C(48) C 0.0380(5) 0.2665(3) 0.3577(5) 0.054(3) Uani 1.0 4 d . . . C(49) C -0.0210(5) 0.2053(2) 0.1714(5) 0.050(3) Uani 1.0 4 d . . . C(50) C -0.0042(5) 0.2426(2) 0.2192(5) 0.049(3) Uani 1.0 4 d . . . C(51) C -0.0053(5) 0.1696(2) 0.2330(5) 0.050(3) Uani 1.0 4 d . . . C(52) C 0.0209(5) 0.1863(2) 0.3100(5) 0.048(3) Uani 1.0 4 d . . . C(53) C -0.0162(5) 0.1242(2) 0.2073(4) 0.043(3) Uani 1.0 4 d . . . C(54) C -0.1012(5) 0.1034(2) 0.2024(4) 0.045(3) Uani 1.0 4 d . . . C(55) C -0.1801(6) 0.1240(2) 0.2166(4) 0.051(3) Uani 1.0 4 d . . . C(56) C -0.2599(6) 0.1026(3) 0.2147(5) 0.063(3) Uani 1.0 4 d . . . C(57) C -0.2667(6) 0.0594(3) 0.1965(5) 0.071(3) Uani 1.0 4 d . . . C(58) C -0.1951(6) 0.0381(3) 0.1800(5) 0.067(3) Uani 1.0 4 d . . . C(59) C -0.1075(5) 0.0592(3) 0.1822(4) 0.047(3) Uani 1.0 4 d . . . C(60) C 0.0478(6) 0.0597(3) 0.1640(4) 0.053(3) Uani 1.0 4 d . . . C(61) C 0.1223(7) 0.0391(3) 0.1426(6) 0.079(4) Uani 1.0 4 d . . . C(62) C 0.2012(7) 0.0601(3) 0.1452(6) 0.094(4) Uani 1.0 4 d . . . C(63) C 0.2153(6) 0.1026(3) 0.1715(6) 0.082(4) Uani 1.0 4 d . . . C(64) C 0.1460(6) 0.1233(3) 0.1911(5) 0.067(3) Uani 1.0 4 d . . . C(65) C 0.0590(5) 0.1035(3) 0.1885(4) 0.048(3) Uani 1.0 4 d . . . C(66) C 0.0489(5) 0.1643(3) 0.3921(4) 0.049(3) Uani 1.0 4 d . . . C(67) C -0.0307(5) 0.1369(3) 0.4084(4) 0.052(3) Uani 1.0 4 d . . . C(68) C -0.1059(6) 0.1552(3) 0.4261(5) 0.072(3) Uani 1.0 4 d . . . C(69) C -0.1804(7) 0.1331(4) 0.4383(5) 0.085(4) Uani 1.0 4 d . . . C(70) C -0.1792(8) 0.0899(5) 0.4326(6) 0.099(5) Uani 1.0 4 d . . . C(71) C -0.1035(7) 0.0699(3) 0.4156(5) 0.077(4) Uani 1.0 4 d . . . C(72) C -0.0252(6) 0.0926(3) 0.4030(4) 0.058(3) Uani 1.0 4 d . . . C(73) C 0.1373(6) 0.0940(3) 0.3957(5) 0.059(3) Uani 1.0 4 d . . . C(74) C 0.2201(7) 0.0724(3) 0.4006(5) 0.078(4) Uani 1.0 4 d . . . C(75) C 0.3028(7) 0.0961(4) 0.4095(6) 0.102(5) Uani 1.0 4 d . . . C(76) C 0.3071(7) 0.1387(4) 0.4170(6) 0.087(4) Uani 1.0 4 d . . . C(77) C 0.2236(6) 0.1593(3) 0.4137(5) 0.071(3) Uani 1.0 4 d . . . C(78) C 0.1380(5) 0.1386(3) 0.4012(4) 0.053(3) Uani 1.0 4 d . . . C(79) C -0.0426(6) -0.0077(2) 0.1461(5) 0.082(4) Uani 1.0 4 d . . . C(80) C 0.0495(7) 0.0264(3) 0.3737(5) 0.093(4) Uani 1.0 4 d . . . C(81) C 0.3987(10) 0.0724(6) -0.1157(9) 0.136(6) Uani 1.0 4 d . . . C(82) C 0.2763(8) -0.0795(4) 0.0686(7) 0.096(4) Uani 1.0 4 d . . . C(83) C 0.2600(8) -0.0738(4) 0.3069(6) 0.107(4) Uani 1.0 4 d . . . C(84) C 0.7208(7) 0.4260(3) 1.1563(6) 0.106(4) Uani 1.0 4 d . . . H(1) H 0.4354 0.0890 0.0837 0.075(3) Uiso 1.0 4 calc R . . H(2) H 0.4573 0.0181 0.1347 0.095(4) Uiso 1.0 4 calc R . . H(3) H 0.5017 0.0054 0.2734 0.102(4) Uiso 1.0 4 calc R . . H(4) H 0.5610 0.0383 0.4246 0.101(4) Uiso 1.0 4 calc R . . H(5) H 0.5966 0.0980 0.5009 0.102(4) Uiso 1.0 4 calc R . . H(6) H 0.5641 0.1677 0.4393 0.078(3) Uiso 1.0 4 calc R . . H(7) H 0.6799 0.1953 0.2709 0.074(3) Uiso 1.0 4 calc R . . H(8) H 0.8204 0.2299 0.2879 0.088(3) Uiso 1.0 4 calc R . . H(9) H 0.8409 0.2983 0.3424 0.100(4) Uiso 1.0 4 calc R . . H(10) H 0.7154 0.3351 0.3711 0.089(4) Uiso 1.0 4 calc R . . H(11) H 0.3869 0.3389 0.3718 0.087(4) Uiso 1.0 4 calc R . . H(12) H 0.2373 0.3091 0.3344 0.096(4) Uiso 1.0 4 calc R . . H(13) H 0.2147 0.2386 0.2850 0.084(3) Uiso 1.0 4 calc R . . H(14) H 0.331(5) 0.203(3) 0.260(4) 0.08(3) Uiso 1.0 4 d . . . H(15) H 0.5971 0.1557 0.0595 0.085(4) Uiso 1.0 4 calc R . . H(16) H 0.7403 0.1886 0.0505 0.112(5) Uiso 1.0 4 calc R . . H(17) H 0.7567 0.2600 0.0686 0.127(5) Uiso 1.0 4 calc R . . H(18) H 0.6413 0.3016 0.0967 0.087(4) Uiso 1.0 4 calc R . . H(19) H 0.3170 0.3156 0.1012 0.090(4) Uiso 1.0 4 calc R . . H(20) H 0.1680 0.2883 0.0818 0.105(4) Uiso 1.0 4 calc R . . H(21) H 0.1399 0.2155 0.0572 0.103(4) Uiso 1.0 4 calc R . . H(22) H 0.2686 0.1708 0.0638 0.080(3) Uiso 1.0 4 calc R . . H(23) H 0.5719 0.3522 0.4420 0.1287 Uiso 1.0 4 calc R . . H(24) H 0.4953 0.3670 0.3643 0.1287 Uiso 1.0 4 calc R . . H(25) H 0.6013 0.3668 0.3644 0.1287 Uiso 1.0 4 calc R . . H(26) H 0.559(6) 0.331(3) 0.185(5) 0.12(4) Uiso 1.0 4 d . . . H(27) H 0.5233 0.3337 0.1073 0.1017 Uiso 1.0 4 calc R . . H(28) H 0.4333 0.3346 0.1392 0.1017 Uiso 1.0 4 calc R . . H(29) H 0.445(4) 0.1680(17) 0.060(4) 0.034(18) Uiso 1.0 4 d . . . H(30) H -0.0679 0.1849 0.0532 0.064(3) Uiso 1.0 4 calc R . . H(31) H -0.073(4) 0.2563(15) -0.004(3) 0.026(15) Uiso 1.0 4 d . . . H(32) H -0.051(4) 0.3125(17) 0.073(3) 0.029(16) Uiso 1.0 4 d . . . H(33) H 0.0014 0.3466 0.2298 0.080(3) Uiso 1.0 4 calc R . . H(34) H 0.0488 0.3300 0.3674 0.078(3) Uiso 1.0 4 calc R . . H(35) H 0.0517 0.2605 0.4148 0.065(3) Uiso 1.0 4 calc R . . H(36) H -0.1763 0.1534 0.2306 0.061(3) Uiso 1.0 4 calc R . . H(37) H -0.3141 0.1162 0.2238 0.077(3) Uiso 1.0 4 calc R . . H(38) H -0.3241 0.0442 0.1907 0.086(3) Uiso 1.0 4 calc R . . H(39) H -0.1979 0.0081 0.1731 0.084(4) Uiso 1.0 4 calc R . . H(40) H 0.1172 0.0100 0.1267 0.101(4) Uiso 1.0 4 calc R . . H(41) H 0.2518 0.0463 0.1302 0.122(5) Uiso 1.0 4 calc R . . H(42) H 0.2701 0.1190 0.1725 0.102(4) Uiso 1.0 4 calc R . . H(43) H 0.159(4) 0.1553(19) 0.206(4) 0.046(18) Uiso 1.0 4 d . . . H(44) H -0.1107 0.1851 0.4329 0.0844 Uiso 1.0 4 calc R . . H(45) H -0.2340 0.1461 0.4498 0.1049 Uiso 1.0 4 calc R . . H(47) H -0.0983 0.0398 0.4122 0.0913 Uiso 1.0 4 calc R . . H(48) H 0.2212 0.0422 0.3999 0.0950 Uiso 1.0 4 calc R . . H(49) H 0.3598 0.0814 0.4107 0.1230 Uiso 1.0 4 calc R . . H(50) H 0.3654 0.1530 0.4206 0.1053 Uiso 1.0 4 calc R . . H(51) H 0.2253 0.1893 0.4212 0.085(4) Uiso 1.0 4 calc R . . H(52) H -0.0216 -0.0237 0.1954 0.0988 Uiso 1.0 4 calc R . . H(53) H -0.0045 -0.0144 0.1101 0.0989 Uiso 1.0 4 calc R . . H(54) H -0.1068 -0.0146 0.1202 0.0989 Uiso 1.0 4 calc R . . H(55) H 0.0763 0.0129 0.4250 0.1099 Uiso 1.0 4 calc R . . H(56) H 0.0853 0.0192 0.3362 0.1098 Uiso 1.0 4 calc R . . H(57) H -0.0140 0.0171 0.3524 0.1099 Uiso 1.0 4 calc R . . H(58) H 0.067(4) 0.1883(18) 0.438(4) 0.047(18) Uiso 1.0 4 d . . . H(59) H 0.2324 -0.0699 0.2497 0.1273 Uiso 1.0 4 calc R . . H(61) H -0.2290 0.0725 0.4407 0.1213 Uiso 1.0 4 calc R . . H(62) H 0.7307 0.4262 1.2143 0.1229 Uiso 1.0 4 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cl(1) 0.188(4) 0.139(3) 0.142(3) 0.052(3) 0.025(3) -0.021(3) Cl(2) 0.268(5) 0.163(4) 0.198(4) 0.032(4) 0.150(4) 0.020(3) Cl(3) 0.217(5) 0.127(3) 0.249(5) -0.040(3) 0.042(4) -0.020(3) Cl(4) 0.176(4) 0.120(3) 0.161(3) 0.028(3) 0.028(3) -0.028(3) Cl(5) 0.124(3) 0.155(3) 0.156(3) -0.008(3) -0.008(2) -0.006(3) Cl(6) 0.173(4) 0.119(3) 0.177(4) -0.033(3) 0.033(3) 0.005(3) S(1) 0.0761(16) 0.0738(17) 0.0911(17) 0.0091(15) 0.0018(14) -0.0137(15) S(2) 0.0875(17) 0.0581(14) 0.0654(14) -0.0007(14) 0.0199(12) 0.0007(12) F(1) 0.152(7) 0.224(9) 0.178(7) 0.046(6) 0.054(6) -0.081(7) F(2) 0.071(5) 0.430(14) 0.146(6) 0.026(7) 0.011(4) -0.066(8) F(3) 0.221(10) 0.236(11) 0.207(9) -0.116(9) 0.077(8) 0.013(8) F(4) 0.126(5) 0.240(8) 0.122(5) 0.032(6) 0.079(4) 0.028(6) F(5) 0.105(5) 0.172(7) 0.173(7) -0.040(5) 0.026(5) -0.028(6) F(6) 0.140(6) 0.170(7) 0.173(7) 0.083(6) 0.045(5) 0.071(6) O(1) 0.142(7) 0.076(5) 0.107(5) 0.027(5) -0.018(5) -0.033(4) O(2) 0.223(9) 0.090(6) 0.112(6) -0.045(6) 0.019(6) 0.032(5) O(3) 0.071(4) 0.107(5) 0.081(4) -0.010(4) -0.006(3) -0.006(4) O(4) 0.121(6) 0.071(4) 0.084(4) 0.017(4) 0.027(4) 0.018(4) O(5) 0.097(5) 0.083(4) 0.061(4) 0.000(4) 0.032(3) 0.004(3) O(6) 0.155(6) 0.067(4) 0.083(5) -0.025(4) 0.028(4) -0.019(4) N(1) 0.063(5) 0.035(4) 0.075(5) -0.007(4) 0.020(4) -0.011(3) N(2) 0.076(5) 0.047(5) 0.071(5) -0.011(4) 0.015(4) 0.005(4) N(3) 0.060(5) 0.039(4) 0.062(4) -0.002(4) 0.011(4) -0.007(3) N(4) 0.065(5) 0.051(5) 0.072(5) 0.002(4) 0.025(4) -0.007(4) C(1) 0.038(5) 0.038(5) 0.062(5) 0.001(4) 0.010(4) 0.003(4) C(2) 0.047(5) 0.061(6) 0.079(6) -0.001(5) 0.014(4) -0.004(5) C(3) 0.066(6) 0.048(6) 0.124(9) 0.007(5) 0.023(6) -0.014(6) C(4) 0.076(7) 0.054(7) 0.126(9) 0.004(5) 0.028(7) 0.033(6) C(5) 0.042(5) 0.060(6) 0.086(7) -0.002(5) 0.022(5) 0.015(5) C(6) 0.063(7) 0.102(9) 0.088(8) 0.015(6) 0.028(6) 0.040(6) C(7) 0.043(6) 0.129(9) 0.083(8) 0.008(6) 0.019(5) 0.045(7) C(8) 0.053(5) 0.088(7) 0.054(6) 0.006(5) 0.009(4) 0.003(5) C(9) 0.039(5) 0.052(5) 0.065(6) -0.004(4) 0.018(4) 0.010(4) C(10) 0.031(5) 0.056(6) 0.073(6) -0.002(4) 0.022(4) 0.007(5) C(11) 0.041(5) 0.043(5) 0.062(5) -0.005(4) 0.011(4) 0.003(4) C(12) 0.032(4) 0.050(5) 0.057(5) -0.008(4) 0.014(4) -0.001(4) C(13) 0.061(6) 0.047(5) 0.041(5) -0.005(4) 0.017(4) -0.001(4) C(14) 0.032(5) 0.052(5) 0.060(5) 0.003(4) 0.013(4) -0.000(4) C(15) 0.046(5) 0.065(6) 0.074(6) 0.000(5) 0.009(4) -0.005(4) C(16) 0.048(6) 0.060(6) 0.112(7) 0.001(5) 0.025(5) -0.008(5) C(17) 0.036(6) 0.072(7) 0.143(9) -0.021(5) 0.008(6) -0.005(6) C(18) 0.058(6) 0.060(6) 0.105(7) -0.010(5) 0.019(5) -0.009(5) C(19) 0.040(5) 0.054(6) 0.059(5) 0.002(4) 0.004(4) -0.009(4) C(20) 0.049(5) 0.060(6) 0.059(5) 0.009(5) 0.024(4) 0.000(4) C(21) 0.067(6) 0.069(6) 0.081(6) -0.000(6) 0.034(5) -0.011(5) C(22) 0.049(6) 0.083(7) 0.108(7) 0.012(5) 0.039(5) 0.010(6) C(23) 0.063(6) 0.072(7) 0.075(6) -0.005(6) 0.022(5) 0.010(5) C(24) 0.050(6) 0.064(6) 0.059(6) -0.000(5) 0.024(4) 0.004(5) C(25) 0.045(5) 0.056(5) 0.045(5) 0.006(4) 0.015(4) 0.002(4) C(26) 0.052(5) 0.043(5) 0.053(5) 0.003(4) 0.010(4) -0.002(4) C(27) 0.058(6) 0.069(6) 0.054(5) -0.008(5) 0.015(4) 0.009(4) C(28) 0.055(6) 0.091(7) 0.068(6) -0.000(6) 0.019(5) 0.017(5) C(29) 0.054(7) 0.147(10) 0.080(7) 0.022(8) 0.014(5) 0.045(8) C(30) 0.045(7) 0.191(13) 0.081(7) -0.010(9) 0.013(5) 0.037(9) C(31) 0.060(6) 0.075(7) 0.083(6) -0.022(6) 0.012(5) 0.024(5) C(32) 0.058(6) 0.078(7) 0.054(5) -0.005(5) 0.010(4) 0.008(5) C(33) 0.052(6) 0.053(6) 0.057(5) -0.006(5) 0.018(4) 0.005(4) C(34) 0.071(6) 0.063(6) 0.090(7) 0.016(6) 0.022(5) 0.017(5) C(35) 0.076(8) 0.094(8) 0.092(7) 0.021(7) 0.030(6) 0.020(6) C(36) 0.053(6) 0.116(9) 0.088(7) -0.013(7) 0.017(5) 0.003(6) C(37) 0.051(6) 0.068(6) 0.081(6) 0.001(5) 0.016(5) 0.001(5) C(38) 0.044(5) 0.066(6) 0.051(5) 0.008(5) 0.009(4) 0.009(4) C(39) 0.077(7) 0.086(7) 0.159(10) -0.019(6) 0.049(7) -0.043(7) C(40) 0.083(8) 0.062(7) 0.109(8) -0.017(6) 0.010(6) 0.014(5) C(41) 0.038(5) 0.051(5) 0.051(5) -0.008(4) 0.007(4) 0.000(4) C(42) 0.061(5) 0.050(5) 0.050(5) 0.002(4) 0.018(4) -0.001(4) C(43) 0.077(7) 0.064(6) 0.055(6) 0.016(5) 0.022(5) 0.013(5) C(44) 0.067(6) 0.061(7) 0.074(7) 0.005(5) 0.022(5) 0.034(6) C(45) 0.032(5) 0.060(6) 0.084(7) 0.002(4) 0.018(4) 0.008(5) C(46) 0.048(5) 0.043(5) 0.110(8) -0.007(4) 0.017(5) -0.010(5) C(47) 0.047(5) 0.062(6) 0.084(7) -0.006(5) 0.006(5) -0.017(5) C(48) 0.037(5) 0.052(5) 0.073(6) 0.000(4) 0.017(4) -0.010(5) C(49) 0.051(5) 0.039(5) 0.063(5) 0.006(4) 0.019(4) -0.002(4) C(50) 0.035(5) 0.041(5) 0.072(6) 0.003(4) 0.016(4) 0.005(4) C(51) 0.049(5) 0.036(5) 0.065(5) 0.003(4) 0.015(4) -0.001(4) C(52) 0.035(5) 0.049(5) 0.059(5) -0.001(4) 0.011(4) -0.002(4) C(53) 0.039(5) 0.043(5) 0.045(5) 0.002(4) 0.010(4) 0.007(4) C(54) 0.050(5) 0.042(5) 0.046(5) -0.004(4) 0.016(4) -0.002(4) C(55) 0.063(6) 0.036(5) 0.054(5) -0.004(4) 0.012(4) -0.004(4) C(56) 0.053(6) 0.063(6) 0.078(6) 0.002(5) 0.025(5) -0.005(5) C(57) 0.047(6) 0.070(7) 0.098(7) -0.013(5) 0.023(5) -0.009(5) C(58) 0.063(6) 0.048(5) 0.099(7) -0.018(5) 0.036(5) -0.008(5) C(59) 0.046(5) 0.051(5) 0.046(5) 0.002(4) 0.014(4) 0.001(4) C(60) 0.061(6) 0.048(5) 0.050(5) 0.007(4) 0.015(4) 0.002(4) C(61) 0.073(7) 0.046(6) 0.134(8) 0.011(5) 0.054(6) -0.013(5) C(62) 0.083(8) 0.080(8) 0.141(9) 0.018(6) 0.070(7) -0.009(6) C(63) 0.062(6) 0.058(7) 0.136(8) -0.002(5) 0.043(6) -0.002(6) C(64) 0.053(6) 0.051(6) 0.100(7) -0.004(5) 0.028(5) -0.006(5) C(65) 0.041(5) 0.048(5) 0.056(5) 0.007(4) 0.017(4) 0.001(4) C(66) 0.048(5) 0.052(5) 0.046(5) 0.002(4) 0.010(4) 0.006(4) C(67) 0.038(5) 0.068(6) 0.048(5) -0.006(5) 0.009(4) 0.005(4) C(68) 0.063(6) 0.089(7) 0.059(6) 0.012(6) 0.010(5) -0.007(5) C(69) 0.053(7) 0.139(10) 0.070(6) -0.002(7) 0.028(5) -0.015(7) C(70) 0.080(8) 0.144(11) 0.079(7) -0.042(8) 0.031(6) 0.013(7) C(71) 0.087(7) 0.079(7) 0.063(6) -0.021(6) 0.013(5) 0.010(5) C(72) 0.058(6) 0.055(6) 0.054(5) -0.016(5) 0.004(4) 0.007(4) C(73) 0.047(5) 0.063(6) 0.069(6) 0.022(5) 0.018(4) 0.005(4) C(74) 0.089(7) 0.063(6) 0.086(6) 0.006(6) 0.032(5) 0.014(5) C(75) 0.055(7) 0.143(11) 0.109(8) 0.032(8) 0.025(6) 0.003(8) C(76) 0.056(7) 0.101(8) 0.106(8) -0.006(7) 0.028(6) 0.006(7) C(77) 0.054(6) 0.093(7) 0.067(6) -0.014(6) 0.016(5) 0.016(5) C(78) 0.043(5) 0.059(6) 0.056(5) 0.007(5) 0.009(4) 0.011(4) C(79) 0.085(7) 0.044(5) 0.118(8) 0.001(5) 0.031(6) -0.019(5) C(80) 0.112(9) 0.065(7) 0.098(7) -0.004(6) 0.018(6) -0.000(5) C(81) 0.125(11) 0.164(14) 0.119(11) -0.037(12) 0.031(9) -0.056(11) C(82) 0.114(9) 0.083(8) 0.096(8) 0.015(8) 0.037(7) 0.013(7) C(83) 0.141(10) 0.092(8) 0.086(7) 0.002(8) 0.028(7) -0.006(6) C(84) 0.146(10) 0.070(7) 0.090(7) -0.024(7) 0.014(7) -0.016(6) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SIR92 (Altomare, et al., 1994)' _computing_structure_refinement 'CRYSTALS (Carruthers, et al., 1999)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cl(1) C(83) 1.712(11) yes . . Cl(2) C(83) 1.731(13) yes . . Cl(3) C(83) 1.681(11) yes . . Cl(4) C(84) 1.704(11) yes . . Cl(5) C(84) 1.731(10) yes . . Cl(6) C(84) 1.729(11) yes . . S(1) O(1) 1.409(7) yes . . S(1) O(2) 1.479(8) yes . . S(1) O(3) 1.417(5) yes . . S(1) C(81) 1.715(16) yes . . S(2) O(4) 1.409(6) yes . . S(2) O(5) 1.440(6) yes . . S(2) O(6) 1.425(6) yes . . S(2) C(82) 1.808(12) yes . . F(1) C(81) 1.305(18) yes . . F(2) C(81) 1.302(14) yes . . F(3) C(81) 1.399(19) yes . . F(4) C(82) 1.299(14) yes . . F(5) C(82) 1.306(13) yes . . F(6) C(82) 1.308(14) yes . . N(1) C(19) 1.381(11) yes . . N(1) C(20) 1.395(10) yes . . N(1) C(39) 1.510(10) yes . . N(2) C(32) 1.402(12) yes . . N(2) C(33) 1.385(11) yes . . N(2) C(40) 1.471(11) yes . . N(3) C(59) 1.334(11) yes . . N(3) C(60) 1.386(11) yes . . N(3) C(79) 1.493(9) yes . . N(4) C(72) 1.385(11) yes . . N(4) C(73) 1.412(11) yes . . N(4) C(80) 1.450(10) yes . . C(1) C(2) 1.367(10) yes . . C(1) C(10) 1.381(11) yes . . C(1) C(11) 1.477(10) yes . . C(2) C(3) 1.401(12) yes . . C(3) C(4) 1.371(15) yes . . C(4) C(5) 1.390(13) yes . . C(5) C(6) 1.391(14) yes . . C(5) C(10) 1.393(12) yes . . C(6) C(7) 1.313(15) yes . . C(7) C(8) 1.469(14) yes . . C(8) C(9) 1.357(11) yes . . C(9) C(10) 1.402(11) yes . . C(9) C(12) 1.488(10) yes . . C(11) C(12) 1.374(10) yes . . C(11) C(26) 1.528(10) yes . . C(12) C(13) 1.464(10) yes . . C(13) C(14) 1.393(10) yes . . C(13) C(25) 1.411(11) yes . . C(14) C(15) 1.436(11) yes . . C(14) C(19) 1.400(10) yes . . C(15) C(16) 1.336(11) yes . . C(16) C(17) 1.390(12) yes . . C(17) C(18) 1.368(13) yes . . C(18) C(19) 1.387(11) yes . . C(20) C(21) 1.400(12) yes . . C(20) C(25) 1.395(11) yes . . C(21) C(22) 1.358(12) yes . . C(22) C(23) 1.395(13) yes . . C(23) C(24) 1.347(13) yes . . C(24) C(25) 1.396(11) yes . . C(26) C(27) 1.477(12) yes . . C(26) C(38) 1.500(11) yes . . C(27) C(28) 1.402(13) yes . . C(27) C(32) 1.381(13) yes . . C(28) C(29) 1.358(14) yes . . C(29) C(30) 1.37(2) yes . . C(30) C(31) 1.344(16) yes . . C(31) C(32) 1.423(13) yes . . C(33) C(34) 1.415(12) yes . . C(33) C(38) 1.387(11) yes . . C(34) C(35) 1.361(14) yes . . C(35) C(36) 1.370(16) yes . . C(36) C(37) 1.372(13) yes . . C(37) C(38) 1.361(11) yes . . C(41) C(48) 1.378(10) yes . . C(41) C(50) 1.406(10) yes . . C(41) C(52) 1.466(10) yes . . C(42) C(43) 1.412(11) yes . . C(42) C(49) 1.355(10) yes . . C(43) C(44) 1.367(13) yes . . C(44) C(45) 1.440(12) yes . . C(45) C(46) 1.416(12) yes . . C(45) C(50) 1.397(10) yes . . C(46) C(47) 1.356(13) yes . . C(47) C(48) 1.394(11) yes . . C(49) C(50) 1.405(10) yes . . C(49) C(51) 1.503(10) yes . . C(51) C(52) 1.357(10) yes . . C(51) C(53) 1.489(9) yes . . C(52) C(66) 1.504(10) yes . . C(53) C(54) 1.387(10) yes . . C(53) C(65) 1.385(11) yes . . C(54) C(55) 1.401(11) yes . . C(54) C(59) 1.427(10) yes . . C(55) C(56) 1.340(12) yes . . C(56) C(57) 1.388(12) yes . . C(57) C(58) 1.334(13) yes . . C(58) C(59) 1.435(12) yes . . C(60) C(61) 1.396(13) yes . . C(60) C(65) 1.432(10) yes . . C(61) C(62) 1.321(14) yes . . C(62) C(63) 1.404(13) yes . . C(63) C(64) 1.320(13) yes . . C(64) C(65) 1.409(12) yes . . C(66) C(67) 1.531(11) yes . . C(66) C(78) 1.508(11) yes . . C(67) C(68) 1.346(12) yes . . C(67) C(72) 1.399(12) yes . . C(68) C(69) 1.354(14) yes . . C(69) C(70) 1.360(18) yes . . C(70) C(71) 1.370(16) yes . . C(71) C(72) 1.413(13) yes . . C(73) C(74) 1.372(13) yes . . C(73) C(78) 1.404(12) yes . . C(74) C(75) 1.395(15) yes . . C(75) C(76) 1.345(17) yes . . C(76) C(77) 1.371(14) yes . . C(77) C(78) 1.378(12) yes . . C(2) H(1) 0.950 no . . C(3) H(2) 0.950 no . . C(4) H(3) 0.950 no . . C(6) H(4) 0.950 no . . C(7) H(5) 0.950 no . . C(8) H(6) 0.950 no . . C(15) H(7) 0.950 no . . C(16) H(8) 0.950 no . . C(17) H(9) 0.950 no . . C(18) H(10) 0.950 no . . C(21) H(11) 0.950 no . . C(22) H(12) 0.950 no . . C(23) H(13) 0.950 no . . C(24) H(14) 0.95(7) no . . C(26) H(29) 0.92(6) no . . C(28) H(15) 0.950 no . . C(29) H(16) 0.950 no . . C(30) H(17) 0.950 no . . C(31) H(18) 0.950 no . . C(34) H(19) 0.950 no . . C(35) H(20) 0.950 no . . C(36) H(21) 0.950 no . . C(37) H(22) 0.950 no . . C(39) H(23) 0.950 no . . C(39) H(24) 0.950 no . . C(39) H(25) 0.950 no . . C(40) H(26) 1.10(8) no . . C(40) H(27) 0.950 no . . C(40) H(28) 0.950 no . . C(42) H(30) 0.950 no . . C(43) H(31) 0.97(5) no . . C(44) H(32) 0.92(6) no . . C(46) H(33) 0.950 no . . C(47) H(34) 0.950 no . . C(48) H(35) 0.950 no . . C(55) H(36) 0.950 no . . C(56) H(37) 0.950 no . . C(57) H(38) 0.950 no . . C(58) H(39) 0.950 no . . C(61) H(40) 0.950 no . . C(62) H(41) 0.950 no . . C(63) H(42) 0.950 no . . C(64) H(43) 1.04(6) no . . C(66) H(58) 1.07(6) no . . C(68) H(44) 0.950 no . . C(69) H(45) 0.950 no . . C(70) H(61) 0.950 no . . C(71) H(47) 0.950 no . . C(74) H(48) 0.950 no . . C(75) H(49) 0.950 no . . C(76) H(50) 0.950 no . . C(77) H(51) 0.950 no . . C(79) H(52) 0.950 no . . C(79) H(53) 0.950 no . . C(79) H(54) 0.950 no . . C(80) H(55) 0.950 no . . C(80) H(56) 0.950 no . . C(80) H(57) 0.950 no . . C(83) H(59) 0.950 no . . C(84) H(62) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O(1) S(1) O(2) 113.9(4) yes . . . O(1) S(1) O(3) 116.9(4) yes . . . O(1) S(1) C(81) 106.2(7) yes . . . O(2) S(1) O(3) 113.6(4) yes . . . O(2) S(1) C(81) 99.2(7) yes . . . O(3) S(1) C(81) 104.7(5) yes . . . O(4) S(2) O(5) 114.6(4) yes . . . O(4) S(2) O(6) 115.4(4) yes . . . O(4) S(2) C(82) 103.6(5) yes . . . O(5) S(2) O(6) 114.5(4) yes . . . O(5) S(2) C(82) 102.6(5) yes . . . O(6) S(2) C(82) 103.8(5) yes . . . C(19) N(1) C(20) 122.2(6) yes . . . C(19) N(1) C(39) 119.7(7) yes . . . C(20) N(1) C(39) 118.0(7) yes . . . C(32) N(2) C(33) 120.4(7) yes . . . C(32) N(2) C(40) 119.2(8) yes . . . C(33) N(2) C(40) 119.2(7) yes . . . C(59) N(3) C(60) 121.6(6) yes . . . C(59) N(3) C(79) 120.1(7) yes . . . C(60) N(3) C(79) 118.3(7) yes . . . C(72) N(4) C(73) 119.4(7) yes . . . C(72) N(4) C(80) 120.4(7) yes . . . C(73) N(4) C(80) 118.5(7) yes . . . C(2) C(1) C(10) 117.1(7) yes . . . C(2) C(1) C(11) 135.8(7) yes . . . C(10) C(1) C(11) 107.2(6) yes . . . C(1) C(2) C(3) 119.6(8) yes . . . C(2) C(3) C(4) 120.8(8) yes . . . C(3) C(4) C(5) 122.3(9) yes . . . C(4) C(5) C(6) 130.2(9) yes . . . C(4) C(5) C(10) 113.8(8) yes . . . C(6) C(5) C(10) 116.0(8) yes . . . C(5) C(6) C(7) 122.7(10) yes . . . C(6) C(7) C(8) 122.0(9) yes . . . C(7) C(8) C(9) 116.0(8) yes . . . C(8) C(9) C(10) 120.5(7) yes . . . C(8) C(9) C(12) 133.5(7) yes . . . C(10) C(9) C(12) 106.0(6) yes . . . C(1) C(10) C(5) 126.4(8) yes . . . C(1) C(10) C(9) 110.8(7) yes . . . C(5) C(10) C(9) 122.8(7) yes . . . C(1) C(11) C(12) 108.0(6) yes . . . C(1) C(11) C(26) 122.6(6) yes . . . C(12) C(11) C(26) 129.4(6) yes . . . C(9) C(12) C(11) 108.0(6) yes . . . C(9) C(12) C(13) 121.7(6) yes . . . C(11) C(12) C(13) 130.2(6) yes . . . C(12) C(13) C(14) 120.9(7) yes . . . C(12) C(13) C(25) 119.1(7) yes . . . C(14) C(13) C(25) 119.9(7) yes . . . C(13) C(14) C(15) 121.5(7) yes . . . C(13) C(14) C(19) 121.0(7) yes . . . C(15) C(14) C(19) 117.4(7) yes . . . C(14) C(15) C(16) 120.5(8) yes . . . C(15) C(16) C(17) 120.5(8) yes . . . C(16) C(17) C(18) 121.6(8) yes . . . C(17) C(18) C(19) 118.7(8) yes . . . N(1) C(19) C(14) 118.1(7) yes . . . N(1) C(19) C(18) 120.5(7) yes . . . C(14) C(19) C(18) 121.4(8) yes . . . N(1) C(20) C(21) 121.0(7) yes . . . N(1) C(20) C(25) 119.4(7) yes . . . C(21) C(20) C(25) 119.7(7) yes . . . C(20) C(21) C(22) 119.1(8) yes . . . C(21) C(22) C(23) 121.7(9) yes . . . C(22) C(23) C(24) 119.2(8) yes . . . C(23) C(24) C(25) 121.3(8) yes . . . C(13) C(25) C(20) 119.2(7) yes . . . C(13) C(25) C(24) 121.6(7) yes . . . C(20) C(25) C(24) 119.0(8) yes . . . C(11) C(26) C(27) 112.3(6) yes . . . C(11) C(26) C(38) 113.6(7) yes . . . C(27) C(26) C(38) 110.7(7) yes . . . C(26) C(27) C(28) 119.0(8) yes . . . C(26) C(27) C(32) 122.2(8) yes . . . C(28) C(27) C(32) 118.5(8) yes . . . C(27) C(28) C(29) 121.5(9) yes . . . C(28) C(29) C(30) 118.9(10) yes . . . C(29) C(30) C(31) 122.8(11) yes . . . C(30) C(31) C(32) 118.9(10) yes . . . N(2) C(32) C(27) 117.6(8) yes . . . N(2) C(32) C(31) 123.0(8) yes . . . C(27) C(32) C(31) 119.4(8) yes . . . N(2) C(33) C(34) 121.8(7) yes . . . N(2) C(33) C(38) 119.5(7) yes . . . C(34) C(33) C(38) 118.7(8) yes . . . C(33) C(34) C(35) 120.1(9) yes . . . C(34) C(35) C(36) 120.9(10) yes . . . C(35) C(36) C(37) 118.6(9) yes . . . C(36) C(37) C(38) 122.7(9) yes . . . C(26) C(38) C(33) 120.0(7) yes . . . C(26) C(38) C(37) 121.0(7) yes . . . C(33) C(38) C(37) 119.0(8) yes . . . C(48) C(41) C(50) 117.1(7) yes . . . C(48) C(41) C(52) 136.2(7) yes . . . C(50) C(41) C(52) 106.7(6) yes . . . C(43) C(42) C(49) 117.8(7) yes . . . C(42) C(43) C(44) 124.1(8) yes . . . C(43) C(44) C(45) 119.3(8) yes . . . C(44) C(45) C(46) 128.6(8) yes . . . C(44) C(45) C(50) 114.7(7) yes . . . C(46) C(45) C(50) 116.7(7) yes . . . C(45) C(46) C(47) 119.3(8) yes . . . C(46) C(47) C(48) 123.2(8) yes . . . C(41) C(48) C(47) 119.7(7) yes . . . C(42) C(49) C(50) 119.0(7) yes . . . C(42) C(49) C(51) 136.2(7) yes . . . C(50) C(49) C(51) 104.7(6) yes . . . C(41) C(50) C(45) 124.0(7) yes . . . C(41) C(50) C(49) 110.9(6) yes . . . C(45) C(50) C(49) 125.1(7) yes . . . C(49) C(51) C(52) 109.0(6) yes . . . C(49) C(51) C(53) 122.0(6) yes . . . C(52) C(51) C(53) 129.0(6) yes . . . C(41) C(52) C(51) 108.6(6) yes . . . C(41) C(52) C(66) 121.3(6) yes . . . C(51) C(52) C(66) 130.1(7) yes . . . C(51) C(53) C(54) 119.4(7) yes . . . C(51) C(53) C(65) 119.2(6) yes . . . C(54) C(53) C(65) 121.4(6) yes . . . C(53) C(54) C(55) 122.8(7) yes . . . C(53) C(54) C(59) 118.1(7) yes . . . C(55) C(54) C(59) 119.1(7) yes . . . C(54) C(55) C(56) 121.2(7) yes . . . C(55) C(56) C(57) 120.5(8) yes . . . C(56) C(57) C(58) 121.5(8) yes . . . C(57) C(58) C(59) 120.6(7) yes . . . N(3) C(59) C(54) 120.9(7) yes . . . N(3) C(59) C(58) 121.9(7) yes . . . C(54) C(59) C(58) 117.2(7) yes . . . N(3) C(60) C(61) 122.2(7) yes . . . N(3) C(60) C(65) 118.9(7) yes . . . C(61) C(60) C(65) 118.9(8) yes . . . C(60) C(61) C(62) 119.7(8) yes . . . C(61) C(62) C(63) 122.7(10) yes . . . C(62) C(63) C(64) 119.3(9) yes . . . C(63) C(64) C(65) 121.5(8) yes . . . C(53) C(65) C(60) 118.7(7) yes . . . C(53) C(65) C(64) 123.5(7) yes . . . C(60) C(65) C(64) 117.9(7) yes . . . C(52) C(66) C(67) 112.9(5) yes . . . C(52) C(66) C(78) 110.8(7) yes . . . C(67) C(66) C(78) 111.1(6) yes . . . C(66) C(67) C(68) 120.4(8) yes . . . C(66) C(67) C(72) 119.3(7) yes . . . C(68) C(67) C(72) 120.3(8) yes . . . C(67) C(68) C(69) 123.6(9) yes . . . C(68) C(69) C(70) 118.4(10) yes . . . C(69) C(70) C(71) 119.9(11) yes . . . C(70) C(71) C(72) 122.3(9) yes . . . N(4) C(72) C(67) 122.5(8) yes . . . N(4) C(72) C(71) 122.1(8) yes . . . C(67) C(72) C(71) 115.4(8) yes . . . N(4) C(73) C(74) 121.2(8) yes . . . N(4) C(73) C(78) 118.9(7) yes . . . C(74) C(73) C(78) 119.9(8) yes . . . C(73) C(74) C(75) 118.1(9) yes . . . C(74) C(75) C(76) 124.0(10) yes . . . C(75) C(76) C(77) 116.4(10) yes . . . C(76) C(77) C(78) 123.4(9) yes . . . C(66) C(78) C(73) 122.5(7) yes . . . C(66) C(78) C(77) 119.4(7) yes . . . C(73) C(78) C(77) 118.1(8) yes . . . S(1) C(81) F(1) 115.4(11) yes . . . S(1) C(81) F(2) 114.7(11) yes . . . S(1) C(81) F(3) 104.6(10) yes . . . F(1) C(81) F(2) 109.3(13) yes . . . F(1) C(81) F(3) 103.7(11) yes . . . F(2) C(81) F(3) 108.1(12) yes . . . S(2) C(82) F(4) 111.9(7) yes . . . S(2) C(82) F(5) 109.8(9) yes . . . S(2) C(82) F(6) 111.0(9) yes . . . F(4) C(82) F(5) 109.7(10) yes . . . F(4) C(82) F(6) 106.7(10) yes . . . F(5) C(82) F(6) 107.6(8) yes . . . Cl(1) C(83) Cl(2) 107.0(6) yes . . . Cl(1) C(83) Cl(3) 113.7(6) yes . . . Cl(2) C(83) Cl(3) 107.7(6) yes . . . Cl(4) C(84) Cl(5) 109.3(5) yes . . . Cl(4) C(84) Cl(6) 111.8(7) yes . . . Cl(5) C(84) Cl(6) 108.5(5) yes . . . C(1) C(2) H(1) 118.782 no . . . C(3) C(2) H(1) 121.596 no . . . C(2) C(3) H(2) 120.327 no . . . C(4) C(3) H(2) 118.789 no . . . C(3) C(4) H(3) 118.931 no . . . C(5) C(4) H(3) 118.757 no . . . C(5) C(6) H(4) 120.231 no . . . C(7) C(6) H(4) 117.014 no . . . C(6) C(7) H(5) 122.250 no . . . C(8) C(7) H(5) 115.380 no . . . C(7) C(8) H(6) 124.128 no . . . C(9) C(8) H(6) 119.627 no . . . C(14) C(15) H(7) 118.689 no . . . C(16) C(15) H(7) 120.826 no . . . C(15) C(16) H(8) 118.450 no . . . C(17) C(16) H(8) 120.962 no . . . C(16) C(17) H(9) 117.808 no . . . C(18) C(17) H(9) 120.592 no . . . C(17) C(18) H(10) 120.148 no . . . C(19) C(18) H(10) 121.199 no . . . C(20) C(21) H(11) 118.329 no . . . C(22) C(21) H(11) 122.464 no . . . C(21) C(22) H(12) 117.439 no . . . C(23) C(22) H(12) 120.771 no . . . C(22) C(23) H(13) 120.179 no . . . C(24) C(23) H(13) 120.474 no . . . C(23) C(24) H(14) 111(5) no . . . C(25) C(24) H(14) 127(5) no . . . C(11) C(26) H(29) 113(4) no . . . C(27) C(26) H(29) 96(4) no . . . C(38) C(26) H(29) 110(4) no . . . C(27) C(28) H(15) 117.000 no . . . C(29) C(28) H(15) 121.292 no . . . C(28) C(29) H(16) 123.551 no . . . C(30) C(29) H(16) 117.471 no . . . C(29) C(30) H(17) 119.170 no . . . C(31) C(30) H(17) 118.018 no . . . C(30) C(31) H(18) 121.215 no . . . C(32) C(31) H(18) 119.851 no . . . C(33) C(34) H(19) 116.521 no . . . C(35) C(34) H(19) 123.324 no . . . C(34) C(35) H(20) 114.758 no . . . C(36) C(35) H(20) 124.152 no . . . C(35) C(36) H(21) 117.360 no . . . C(37) C(36) H(21) 124.048 no . . . C(36) C(37) H(22) 116.475 no . . . C(38) C(37) H(22) 120.851 no . . . N(1) C(39) H(23) 109.484 no . . . N(1) C(39) H(24) 109.051 no . . . N(1) C(39) H(25) 109.876 no . . . H(23) C(39) H(24) 109.470 no . . . H(23) C(39) H(25) 109.471 no . . . H(24) C(39) H(25) 109.475 no . . . N(2) C(40) H(26) 121(5) no . . . N(2) C(40) H(27) 108.198 no . . . N(2) C(40) H(28) 110.401 no . . . H(26) C(40) H(27) 76.445 no . . . H(26) C(40) H(28) 123.444 no . . . H(27) C(40) H(28) 109.476 no . . . C(43) C(42) H(30) 119.337 no . . . C(49) C(42) H(30) 122.752 no . . . C(42) C(43) H(31) 125(3) no . . . C(44) C(43) H(31) 111(3) no . . . C(43) C(44) H(32) 119(4) no . . . C(45) C(44) H(32) 121(4) no . . . C(45) C(46) H(33) 121.850 no . . . C(47) C(46) H(33) 118.819 no . . . C(46) C(47) H(34) 120.667 no . . . C(48) C(47) H(34) 116.115 no . . . C(41) C(48) H(35) 118.120 no . . . C(47) C(48) H(35) 122.201 no . . . C(54) C(55) H(36) 119.634 no . . . C(56) C(55) H(36) 119.126 no . . . C(55) C(56) H(37) 122.043 no . . . C(57) C(56) H(37) 117.477 no . . . C(56) C(57) H(38) 121.727 no . . . C(58) C(57) H(38) 116.614 no . . . C(57) C(58) H(39) 120.840 no . . . C(59) C(58) H(39) 118.095 no . . . C(60) C(61) H(40) 120.734 no . . . C(62) C(61) H(40) 119.575 no . . . C(61) C(62) H(41) 120.015 no . . . C(63) C(62) H(41) 117.272 no . . . C(62) C(63) H(42) 125.030 no . . . C(64) C(63) H(42) 115.463 no . . . C(63) C(64) H(43) 116(4) no . . . C(65) C(64) H(43) 122(4) no . . . C(52) C(66) H(58) 108(3) no . . . C(67) C(66) H(58) 108(4) no . . . C(78) C(66) H(58) 106(3) no . . . C(67) C(68) H(44) 122.733 no . . . C(69) C(68) H(44) 113.605 no . . . C(68) C(69) H(45) 123.593 no . . . C(70) C(69) H(45) 117.994 no . . . C(69) C(70) H(61) 122.650 no . . . C(71) C(70) H(61) 117.453 no . . . C(70) C(71) H(47) 123.491 no . . . C(72) C(71) H(47) 114.166 no . . . C(73) C(74) H(48) 120.706 no . . . C(75) C(74) H(48) 121.156 no . . . C(74) C(75) H(49) 118.487 no . . . C(76) C(75) H(49) 117.496 no . . . C(75) C(76) H(50) 119.566 no . . . C(77) C(76) H(50) 123.872 no . . . C(76) C(77) H(51) 118.059 no . . . C(78) C(77) H(51) 118.535 no . . . N(3) C(79) H(52) 109.390 no . . . N(3) C(79) H(53) 109.688 no . . . N(3) C(79) H(54) 109.333 no . . . H(52) C(79) H(53) 109.468 no . . . H(52) C(79) H(54) 109.470 no . . . H(53) C(79) H(54) 109.477 no . . . N(4) C(80) H(55) 109.951 no . . . N(4) C(80) H(56) 109.369 no . . . N(4) C(80) H(57) 109.098 no . . . H(55) C(80) H(56) 109.467 no . . . H(55) C(80) H(57) 109.468 no . . . H(56) C(80) H(57) 109.474 no . . . Cl(1) C(83) H(59) 109.335 no . . . Cl(2) C(83) H(59) 109.622 no . . . Cl(3) C(83) H(59) 109.385 no . . . Cl(4) C(84) H(62) 108.893 no . . . Cl(5) C(84) H(62) 109.132 no . . . Cl(6) C(84) H(62) 109.244 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O(1) S(1) C(81) F(1) -175.7(9) no . . . . O(1) S(1) C(81) F(2) 55.8(13) no . . . . O(1) S(1) C(81) F(3) -62.4(8) no . . . . O(2) S(1) C(81) F(1) 66.0(10) no . . . . O(2) S(1) C(81) F(2) -62.5(12) no . . . . O(2) S(1) C(81) F(3) 179.3(7) no . . . . O(3) S(1) C(81) F(1) -51.5(11) no . . . . O(3) S(1) C(81) F(2) -179.9(10) no . . . . O(3) S(1) C(81) F(3) 61.8(9) no . . . . O(4) S(2) C(82) F(4) -62.1(8) no . . . . O(4) S(2) C(82) F(5) 60.0(8) no . . . . O(4) S(2) C(82) F(6) 178.8(7) no . . . . O(5) S(2) C(82) F(4) 178.3(7) no . . . . O(5) S(2) C(82) F(5) -59.5(8) no . . . . O(5) S(2) C(82) F(6) 59.3(8) no . . . . O(6) S(2) C(82) F(4) 58.8(8) no . . . . O(6) S(2) C(82) F(5) -179.1(7) no . . . . O(6) S(2) C(82) F(6) -60.3(8) no . . . . C(19) N(1) C(20) C(21) -177.5(6) no . . . . C(19) N(1) C(20) C(25) 3.3(10) no . . . . C(20) N(1) C(19) C(14) -2.5(9) no . . . . C(20) N(1) C(19) C(18) 176.6(6) no . . . . C(39) N(1) C(19) C(14) 179.9(6) no . . . . C(39) N(1) C(19) C(18) -1.1(10) no . . . . C(39) N(1) C(20) C(21) 0.1(9) no . . . . C(39) N(1) C(20) C(25) -179.1(6) no . . . . C(32) N(2) C(33) C(34) -158.8(6) no . . . . C(32) N(2) C(33) C(38) 22.7(10) no . . . . C(33) N(2) C(32) C(27) -21.7(9) no . . . . C(33) N(2) C(32) C(31) 159.3(6) no . . . . C(40) N(2) C(32) C(27) 171.4(6) no . . . . C(40) N(2) C(32) C(31) -7.6(10) no . . . . C(40) N(2) C(33) C(34) 8.1(10) no . . . . C(40) N(2) C(33) C(38) -170.4(6) no . . . . C(59) N(3) C(60) C(61) -176.4(6) no . . . . C(59) N(3) C(60) C(65) 6.4(9) no . . . . C(60) N(3) C(59) C(54) -3.0(9) no . . . . C(60) N(3) C(59) C(58) 176.7(5) no . . . . C(79) N(3) C(59) C(54) 179.1(5) no . . . . C(79) N(3) C(59) C(58) -1.1(9) no . . . . C(79) N(3) C(60) C(61) 1.5(9) no . . . . C(79) N(3) C(60) C(65) -175.7(5) no . . . . C(72) N(4) C(73) C(74) 161.6(6) no . . . . C(72) N(4) C(73) C(78) -19.0(9) no . . . . C(73) N(4) C(72) C(67) 19.9(9) no . . . . C(73) N(4) C(72) C(71) -161.9(6) no . . . . C(80) N(4) C(72) C(67) -175.4(6) no . . . . C(80) N(4) C(72) C(71) 2.8(9) no . . . . C(80) N(4) C(73) C(74) -3.3(10) no . . . . C(80) N(4) C(73) C(78) 176.1(6) no . . . . C(2) C(1) C(10) C(5) 0.7(11) no . . . . C(2) C(1) C(10) C(9) 179.8(6) no . . . . C(10) C(1) C(2) C(3) -0.8(10) no . . . . C(2) C(1) C(11) C(12) 179.1(8) no . . . . C(2) C(1) C(11) C(26) -2.3(13) no . . . . C(11) C(1) C(2) C(3) 179.1(7) no . . . . C(10) C(1) C(11) C(12) -1.0(8) no . . . . C(10) C(1) C(11) C(26) 177.6(6) no . . . . C(11) C(1) C(10) C(5) -179.2(6) no . . . . C(11) C(1) C(10) C(9) -0.1(8) no . . . . C(1) C(2) C(3) C(4) 0.8(12) no . . . . C(2) C(3) C(4) C(5) -0.8(14) no . . . . C(3) C(4) C(5) C(6) -178.9(8) no . . . . C(3) C(4) C(5) C(10) 0.6(13) no . . . . C(4) C(5) C(6) C(7) -179.1(9) no . . . . C(4) C(5) C(10) C(1) -0.6(12) no . . . . C(4) C(5) C(10) C(9) -179.6(7) no . . . . C(6) C(5) C(10) C(1) 179.0(7) no . . . . C(6) C(5) C(10) C(9) -0.0(11) no . . . . C(10) C(5) C(6) C(7) 1.5(13) no . . . . C(5) C(6) C(7) C(8) -1.4(14) no . . . . C(6) C(7) C(8) C(9) -0.2(12) no . . . . C(7) C(8) C(9) C(10) 1.5(11) no . . . . C(7) C(8) C(9) C(12) 179.3(7) no . . . . C(8) C(9) C(10) C(1) 179.4(6) no . . . . C(8) C(9) C(10) C(5) -1.5(11) no . . . . C(8) C(9) C(12) C(11) -179.7(8) no . . . . C(8) C(9) C(12) C(13) 1.9(12) no . . . . C(10) C(9) C(12) C(11) -1.6(8) no . . . . C(10) C(9) C(12) C(13) 179.9(6) no . . . . C(12) C(9) C(10) C(1) 1.0(8) no . . . . C(12) C(9) C(10) C(5) -179.8(6) no . . . . C(1) C(11) C(12) C(9) 1.6(8) no . . . . C(1) C(11) C(12) C(13) 179.8(6) no . . . . C(1) C(11) C(26) C(27) -113.2(7) no . . . . C(1) C(11) C(26) C(38) 120.2(7) no . . . . C(12) C(11) C(26) C(27) 65.0(10) no . . . . C(12) C(11) C(26) C(38) -61.6(10) no . . . . C(26) C(11) C(12) C(9) -176.8(7) no . . . . C(26) C(11) C(12) C(13) 1.5(13) no . . . . C(9) C(12) C(13) C(14) 84.1(9) no . . . . C(9) C(12) C(13) C(25) -92.3(7) no . . . . C(11) C(12) C(13) C(14) -94.0(8) no . . . . C(11) C(12) C(13) C(25) 89.6(10) no . . . . C(12) C(13) C(14) C(15) 6.1(10) no . . . . C(12) C(13) C(14) C(19) -177.2(6) no . . . . C(12) C(13) C(25) C(20) 178.0(5) no . . . . C(12) C(13) C(25) C(24) -5.3(9) no . . . . C(14) C(13) C(25) C(20) 1.5(9) no . . . . C(14) C(13) C(25) C(24) 178.3(6) no . . . . C(25) C(13) C(14) C(15) -177.6(6) no . . . . C(25) C(13) C(14) C(19) -0.8(10) no . . . . C(13) C(14) C(15) C(16) 177.3(6) no . . . . C(13) C(14) C(19) N(1) 1.3(10) no . . . . C(13) C(14) C(19) C(18) -177.8(6) no . . . . C(15) C(14) C(19) N(1) 178.1(6) no . . . . C(15) C(14) C(19) C(18) -0.9(10) no . . . . C(19) C(14) C(15) C(16) 0.4(10) no . . . . C(14) C(15) C(16) C(17) 0.0(11) no . . . . C(15) C(16) C(17) C(18) -0.0(13) no . . . . C(16) C(17) C(18) C(19) -0.5(12) no . . . . C(17) C(18) C(19) N(1) -178.1(7) no . . . . C(17) C(18) C(19) C(14) 1.0(11) no . . . . N(1) C(20) C(21) C(22) 178.7(6) no . . . . N(1) C(20) C(25) C(13) -2.7(9) no . . . . N(1) C(20) C(25) C(24) -179.5(6) no . . . . C(21) C(20) C(25) C(13) 178.1(6) no . . . . C(21) C(20) C(25) C(24) 1.2(10) no . . . . C(25) C(20) C(21) C(22) -2.1(10) no . . . . C(20) C(21) C(22) C(23) 1.9(12) no . . . . C(21) C(22) C(23) C(24) -0.9(12) no . . . . C(22) C(23) C(24) C(25) -0.0(12) no . . . . C(23) C(24) C(25) C(13) -176.9(7) no . . . . C(23) C(24) C(25) C(20) -0.2(11) no . . . . C(11) C(26) C(27) C(28) 72.6(8) no . . . . C(11) C(26) C(27) C(32) -100.9(7) no . . . . C(11) C(26) C(38) C(33) 101.5(7) no . . . . C(11) C(26) C(38) C(37) -76.0(8) no . . . . C(27) C(26) C(38) C(33) -25.9(9) no . . . . C(27) C(26) C(38) C(37) 156.6(6) no . . . . C(38) C(26) C(27) C(28) -159.4(6) no . . . . C(38) C(26) C(27) C(32) 27.2(9) no . . . . C(26) C(27) C(28) C(29) -175.1(6) no . . . . C(26) C(27) C(32) N(2) -4.9(10) no . . . . C(26) C(27) C(32) C(31) 174.1(6) no . . . . C(28) C(27) C(32) N(2) -178.4(6) no . . . . C(28) C(27) C(32) C(31) 0.6(10) no . . . . C(32) C(27) C(28) C(29) -1.4(10) no . . . . C(27) C(28) C(29) C(30) 1.3(11) no . . . . C(28) C(29) C(30) C(31) -0.4(13) no . . . . C(29) C(30) C(31) C(32) -0.3(13) no . . . . C(30) C(31) C(32) N(2) 179.2(7) no . . . . C(30) C(31) C(32) C(27) 0.2(11) no . . . . N(2) C(33) C(34) C(35) -178.9(6) no . . . . N(2) C(33) C(38) C(26) 2.9(10) no . . . . N(2) C(33) C(38) C(37) -179.6(6) no . . . . C(34) C(33) C(38) C(26) -175.7(6) no . . . . C(34) C(33) C(38) C(37) 1.8(10) no . . . . C(38) C(33) C(34) C(35) -0.4(11) no . . . . C(33) C(34) C(35) C(36) -0.8(12) no . . . . C(34) C(35) C(36) C(37) 0.5(13) no . . . . C(35) C(36) C(37) C(38) 1.1(12) no . . . . C(36) C(37) C(38) C(26) 175.3(7) no . . . . C(36) C(37) C(38) C(33) -2.2(11) no . . . . C(48) C(41) C(50) C(45) -1.0(10) no . . . . C(48) C(41) C(50) C(49) -178.9(6) no . . . . C(50) C(41) C(48) C(47) -1.6(10) no . . . . C(48) C(41) C(52) C(51) 177.6(8) no . . . . C(48) C(41) C(52) C(66) -3.6(12) no . . . . C(52) C(41) C(48) C(47) 179.6(7) no . . . . C(50) C(41) C(52) C(51) -1.3(8) no . . . . C(50) C(41) C(52) C(66) 177.5(6) no . . . . C(52) C(41) C(50) C(45) 178.2(6) no . . . . C(52) C(41) C(50) C(49) 0.3(8) no . . . . C(43) C(42) C(49) C(50) 2.0(11) no . . . . C(43) C(42) C(49) C(51) 177.9(8) no . . . . C(49) C(42) C(43) C(44) -2.5(12) no . . . . C(42) C(43) C(44) C(45) 0.9(13) no . . . . C(43) C(44) C(45) C(46) -179.7(7) no . . . . C(43) C(44) C(45) C(50) 1.0(11) no . . . . C(44) C(45) C(46) C(47) -178.9(7) no . . . . C(44) C(45) C(50) C(41) -179.1(6) no . . . . C(44) C(45) C(50) C(49) -1.4(11) no . . . . C(46) C(45) C(50) C(41) 1.6(10) no . . . . C(46) C(45) C(50) C(49) 179.2(6) no . . . . C(50) C(45) C(46) C(47) 0.3(10) no . . . . C(45) C(46) C(47) C(48) -2.9(12) no . . . . C(46) C(47) C(48) C(41) 3.6(11) no . . . . C(42) C(49) C(50) C(41) 177.8(6) no . . . . C(42) C(49) C(50) C(45) -0.1(11) no . . . . C(42) C(49) C(51) C(52) -177.8(8) no . . . . C(42) C(49) C(51) C(53) 3.8(13) no . . . . C(50) C(49) C(51) C(52) -1.5(8) no . . . . C(50) C(49) C(51) C(53) -180.0(6) no . . . . C(51) C(49) C(50) C(41) 0.7(8) no . . . . C(51) C(49) C(50) C(45) -177.2(6) no . . . . C(49) C(51) C(52) C(41) 1.7(8) no . . . . C(49) C(51) C(52) C(66) -176.9(6) no . . . . C(49) C(51) C(53) C(54) -96.1(8) no . . . . C(49) C(51) C(53) C(65) 83.6(8) no . . . . C(52) C(51) C(53) C(54) 85.8(9) no . . . . C(52) C(51) C(53) C(65) -94.5(9) no . . . . C(53) C(51) C(52) C(41) -180.0(7) no . . . . C(53) C(51) C(52) C(66) 1.4(13) no . . . . C(41) C(52) C(66) C(67) 119.6(7) no . . . . C(41) C(52) C(66) C(78) -115.1(7) no . . . . C(51) C(52) C(66) C(67) -61.9(10) no . . . . C(51) C(52) C(66) C(78) 63.4(10) no . . . . C(51) C(53) C(54) C(55) 3.3(9) no . . . . C(51) C(53) C(54) C(59) -176.4(5) no . . . . C(51) C(53) C(65) C(60) 179.8(5) no . . . . C(51) C(53) C(65) C(64) -0.9(9) no . . . . C(54) C(53) C(65) C(60) -0.4(9) no . . . . C(54) C(53) C(65) C(64) 178.8(6) no . . . . C(65) C(53) C(54) C(55) -176.4(6) no . . . . C(65) C(53) C(54) C(59) 3.8(9) no . . . . C(53) C(54) C(55) C(56) -177.2(6) no . . . . C(53) C(54) C(59) N(3) -2.2(9) no . . . . C(53) C(54) C(59) C(58) 178.1(5) no . . . . C(55) C(54) C(59) N(3) 178.0(6) no . . . . C(55) C(54) C(59) C(58) -1.7(9) no . . . . C(59) C(54) C(55) C(56) 2.5(9) no . . . . C(54) C(55) C(56) C(57) -1.5(10) no . . . . C(55) C(56) C(57) C(58) -0.4(11) no . . . . C(56) C(57) C(58) C(59) 1.2(11) no . . . . C(57) C(58) C(59) N(3) -179.9(7) no . . . . C(57) C(58) C(59) C(54) -0.1(10) no . . . . N(3) C(60) C(61) C(62) -177.1(6) no . . . . N(3) C(60) C(65) C(53) -4.7(9) no . . . . N(3) C(60) C(65) C(64) 176.0(5) no . . . . C(61) C(60) C(65) C(53) 178.1(6) no . . . . C(61) C(60) C(65) C(64) -1.2(9) no . . . . C(65) C(60) C(61) C(62) 0.1(11) no . . . . C(60) C(61) C(62) C(63) 2.0(13) no . . . . C(61) C(62) C(63) C(64) -3.0(14) no . . . . C(62) C(63) C(64) C(65) 1.7(13) no . . . . C(63) C(64) C(65) C(53) -179.0(7) no . . . . C(63) C(64) C(65) C(60) 0.3(11) no . . . . C(52) C(66) C(67) C(68) -73.4(8) no . . . . C(52) C(66) C(67) C(72) 105.3(7) no . . . . C(52) C(66) C(78) C(73) -105.5(7) no . . . . C(52) C(66) C(78) C(77) 73.2(7) no . . . . C(67) C(66) C(78) C(73) 20.8(9) no . . . . C(67) C(66) C(78) C(77) -160.5(6) no . . . . C(78) C(66) C(67) C(68) 161.4(5) no . . . . C(78) C(66) C(67) C(72) -19.8(8) no . . . . C(66) C(67) C(68) C(69) 177.6(6) no . . . . C(66) C(67) C(72) N(4) 0.8(9) no . . . . C(66) C(67) C(72) C(71) -177.4(5) no . . . . C(68) C(67) C(72) N(4) 179.6(6) no . . . . C(68) C(67) C(72) C(71) 1.3(9) no . . . . C(72) C(67) C(68) C(69) -1.2(10) no . . . . C(67) C(68) C(69) C(70) 0.2(11) no . . . . C(68) C(69) C(70) C(71) 0.5(12) no . . . . C(69) C(70) C(71) C(72) -0.3(12) no . . . . C(70) C(71) C(72) N(4) -178.9(7) no . . . . C(70) C(71) C(72) C(67) -0.6(10) no . . . . N(4) C(73) C(74) C(75) 178.3(6) no . . . . N(4) C(73) C(78) C(66) -2.5(10) no . . . . N(4) C(73) C(78) C(77) 178.8(6) no . . . . C(74) C(73) C(78) C(66) 177.0(6) no . . . . C(74) C(73) C(78) C(77) -1.8(10) no . . . . C(78) C(73) C(74) C(75) -1.2(11) no . . . . C(73) C(74) C(75) C(76) 3.0(13) no . . . . C(74) C(75) C(76) C(77) -1.6(14) no . . . . C(75) C(76) C(77) C(78) -1.7(12) no . . . . C(76) C(77) C(78) C(66) -175.5(7) no . . . . C(76) C(77) C(78) C(73) 3.3(11) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Cl(2) C(70) 3.540(11) no . 3_556 Cl(4) F(3) 3.521(10) no . 4_556 Cl(5) C(72) 3.533(7) no . 4_555 Cl(6) F(1) 3.534(8) no . 4_556 F(1) Cl(6) 3.534(8) no . 4_453 F(1) C(3) 3.242(12) no . 3_655 F(1) C(4) 3.344(14) no . 3_655 F(1) C(84) 3.591(11) no . 4_453 F(2) F(4) 3.150(9) no . 3_655 F(2) F(5) 3.549(11) no . 3_655 F(2) C(2) 3.427(12) no . . F(3) Cl(4) 3.521(10) no . 4_453 F(3) C(46) 3.370(14) no . 4_554 F(3) C(47) 3.293(13) no . 4_554 F(3) C(84) 3.593(12) no . 4_453 F(4) F(2) 3.150(9) no . 3_655 F(4) C(56) 3.593(10) no . 3_555 F(4) C(57) 3.272(11) no . 3_555 F(4) C(58) 3.271(10) no . 3_555 F(5) F(2) 3.549(11) no . 3_655 F(5) C(3) 3.551(11) no . . F(6) C(22) 3.582(12) no . 2_545 F(6) C(47) 3.321(11) no . 2_545 O(1) C(2) 3.367(9) no . . O(1) C(18) 3.229(10) no . 4_454 O(1) C(26) 3.578(9) no . . O(1) C(37) 3.370(11) no . . O(2) C(2) 3.524(10) no . . O(2) C(58) 3.467(10) no . 3_555 O(3) C(39) 3.554(11) no . 4_454 O(3) C(58) 3.599(10) no . 3_555 O(3) C(79) 3.436(10) no . 3_555 O(3) C(84) 3.123(11) no . 4_453 O(4) N(3) 2.943(8) no . 3_555 O(4) C(59) 3.298(9) no . 3_555 O(4) C(60) 3.404(8) no . 3_555 O(4) C(61) 3.286(10) no . . O(4) C(79) 3.002(9) no . 3_555 O(5) C(21) 3.399(10) no . 2_545 O(5) C(39) 3.450(10) no . 2_545 O(5) C(79) 3.561(10) no . . O(5) C(83) 2.999(10) no . . O(6) C(21) 3.420(10) no . 2_545 O(6) C(42) 3.345(9) no . 3_555 O(6) C(53) 3.454(8) no . 3_555 O(6) C(54) 3.406(9) no . 3_555 O(6) C(59) 3.530(9) no . 3_555 O(6) C(65) 3.561(8) no . 3_555 N(3) O(4) 2.943(8) no . 3_555 C(2) F(2) 3.427(12) no . . C(2) O(1) 3.367(9) no . . C(2) O(2) 3.524(10) no . . C(3) F(1) 3.242(12) no . 3_655 C(3) F(5) 3.551(11) no . . C(4) F(1) 3.344(14) no . 3_655 C(18) O(1) 3.229(10) no . 4_555 C(21) O(5) 3.399(10) no . 2_555 C(21) O(6) 3.420(10) no . 2_555 C(22) F(6) 3.582(12) no . 2_555 C(26) O(1) 3.578(9) no . . C(37) O(1) 3.370(11) no . . C(39) O(3) 3.554(11) no . 4_555 C(39) O(5) 3.450(10) no . 2_555 C(42) O(6) 3.345(9) no . 3_555 C(46) F(3) 3.370(14) no . 4_455 C(47) F(3) 3.293(13) no . 4_455 C(47) F(6) 3.321(11) no . 2_555 C(53) O(6) 3.454(8) no . 3_555 C(54) O(6) 3.406(9) no . 3_555 C(56) F(4) 3.593(10) no . 3_555 C(57) F(4) 3.272(11) no . 3_555 C(58) F(4) 3.271(10) no . 3_555 C(58) O(2) 3.467(10) no . 3_555 C(58) O(3) 3.599(10) no . 3_555 C(59) O(4) 3.298(9) no . 3_555 C(59) O(6) 3.530(9) no . 3_555 C(60) O(4) 3.404(8) no . 3_555 C(61) O(4) 3.286(10) no . . C(65) O(6) 3.561(8) no . 3_555 C(70) Cl(2) 3.540(11) no . 3_556 C(72) Cl(5) 3.533(7) no . 4_454 C(79) O(3) 3.436(10) no . 3_555 C(79) O(4) 3.002(9) no . 3_555 C(79) O(5) 3.561(10) no . . C(83) O(5) 2.999(10) no . . C(84) F(1) 3.591(11) no . 4_556 C(84) F(3) 3.593(12) no . 4_556 C(84) O(3) 3.123(11) no . 4_556 Cl(1) H(5) 2.9827 no . 3_656 Cl(1) H(12) 3.3784 no . 2_545 Cl(1) H(19) 3.3308 no . 2_545 Cl(1) H(20) 3.2584 no . 2_545 Cl(1) H(33) 3.1339 no . 2_545 Cl(2) H(19) 3.4209 no . 2_545 Cl(2) H(28) 3.1645 no . 2_545 Cl(2) H(55) 3.4882 no . . Cl(2) H(56) 3.2734 no . . Cl(2) H(61) 3.2918 no . 3_556 Cl(3) H(3) 3.3137 no . . Cl(3) H(5) 3.3024 no . 3_656 Cl(3) H(48) 3.0492 no . . Cl(4) H(18) 3.0606 no . 1_556 Cl(4) H(33) 3.5527 no . 1_656 Cl(5) H(26) 3.38(8) no . 1_556 Cl(5) H(27) 3.1385 no . 1_556 Cl(5) H(47) 3.5614 no . 2_556 Cl(5) H(55) 3.5770 no . 4_555 Cl(5) H(57) 3.2316 no . 2_556 Cl(6) H(3) 3.4723 no . 2_656 Cl(6) H(4) 3.5194 no . 2_656 Cl(6) H(47) 3.2599 no . 2_556 Cl(6) H(61) 3.3848 no . 2_556 S(1) H(1) 3.0412 no . . S(1) H(10) 3.0348 no . 4_454 S(1) H(25) 3.2852 no . 4_454 S(1) H(39) 3.2021 no . 3_555 S(1) H(54) 3.3165 no . 3_555 S(1) H(62) 3.2754 no . 4_453 S(2) H(11) 3.0121 no . 2_545 S(2) H(24) 3.3212 no . 2_545 S(2) H(40) 3.1362 no . . S(2) H(53) 3.3544 no . . S(2) H(59) 3.2493 no . . F(1) H(2) 2.7216 no . 3_655 F(1) H(3) 2.9725 no . 3_655 F(1) H(38) 2.8852 no . 3_555 F(1) H(39) 3.3208 no . 3_555 F(1) H(62) 2.9561 no . 4_453 F(2) H(1) 2.6376 no . . F(2) H(2) 3.3914 no . 3_655 F(2) H(15) 3.4476 no . . F(2) H(34) 3.5813 no . 4_554 F(3) H(9) 3.0542 no . 4_454 F(3) H(10) 3.3943 no . 4_454 F(3) H(33) 2.9816 no . 4_554 F(3) H(34) 2.8695 no . 4_554 F(3) H(62) 2.9556 no . 4_453 F(4) H(15) 3.1565 no . 3_655 F(4) H(16) 3.5821 no . 3_655 F(4) H(38) 3.4915 no . 3_555 F(5) H(2) 2.8896 no . . F(5) H(40) 3.4547 no . . F(5) H(41) 3.1146 no . . F(5) H(59) 2.9226 no . . F(6) H(11) 3.3723 no . 2_545 F(6) H(12) 2.7723 no . 2_545 F(6) H(16) 3.4526 no . 3_655 F(6) H(33) 3.5467 no . 2_545 F(6) H(34) 2.6265 no . 2_545 F(6) H(59) 3.2680 no . . O(1) H(1) 2.5123 no . . O(1) H(9) 3.5404 no . 4_454 O(1) H(10) 2.3691 no . 4_454 O(1) H(22) 2.6186 no . . O(1) H(23) 3.5127 no . 4_454 O(1) H(25) 3.0730 no . 4_454 O(1) H(29) 2.82(5) no . . O(2) H(1) 2.8827 no . . O(2) H(2) 3.1870 no . . O(2) H(39) 2.8150 no . 3_555 O(2) H(41) 3.1073 no . . O(2) H(54) 2.9594 no . 3_555 O(3) H(10) 2.8590 no . 4_454 O(3) H(25) 2.6368 no . 4_454 O(3) H(39) 2.6526 no . 3_555 O(3) H(52) 3.2749 no . 3_555 O(3) H(54) 2.7432 no . 3_555 O(3) H(62) 2.1869 no . 4_453 O(4) H(40) 2.4776 no . . O(4) H(41) 3.5582 no . . O(4) H(53) 2.8965 no . . O(4) H(53) 2.8597 no . 3_555 O(4) H(54) 2.7589 no . 3_555 O(5) H(11) 2.5338 no . 2_545 O(5) H(24) 2.5498 no . 2_545 O(5) H(40) 2.8801 no . . O(5) H(52) 3.3347 no . . O(5) H(53) 2.9135 no . . O(5) H(59) 2.1017 no . . O(6) H(11) 2.5964 no . 2_545 O(6) H(16) 3.3836 no . 3_655 O(6) H(23) 3.3247 no . 2_545 O(6) H(24) 3.1848 no . 2_545 O(6) H(30) 2.4206 no . 3_555 N(1) H(21) 3.4538 no . 4_555 N(2) H(44) 3.3092 no . 4_554 C(1) H(37) 2.9371 no . 1_655 C(1) H(42) 2.9827 no . . C(2) H(37) 3.4222 no . 1_655 C(2) H(38) 3.3170 no . 1_655 C(2) H(41) 3.1905 no . . C(2) H(42) 3.1405 no . . C(3) H(38) 2.9831 no . 1_655 C(3) H(41) 3.0516 no . . C(4) H(38) 3.0996 no . 1_655 C(5) H(37) 3.5307 no . 1_655 C(5) H(38) 3.5197 no . 1_655 C(5) H(49) 3.2492 no . . C(6) H(49) 2.9285 no . . C(6) H(61) 3.1026 no . 1_655 C(7) H(45) 3.2117 no . 1_655 C(7) H(49) 3.0184 no . . C(7) H(50) 3.3588 no . . C(7) H(61) 3.0844 no . 1_655 C(8) H(45) 2.9483 no . 1_655 C(8) H(49) 3.4791 no . . C(8) H(50) 2.8973 no . . C(9) H(37) 3.3305 no . 1_655 C(9) H(45) 3.5621 no . 1_655 C(9) H(50) 3.2306 no . . C(10) H(37) 2.9797 no . 1_655 C(10) H(42) 3.4874 no . . C(11) H(37) 3.2825 no . 1_655 C(11) H(42) 3.3161 no . . C(12) H(37) 3.5189 no . 1_655 C(15) H(36) 3.3144 no . 1_655 C(15) H(37) 3.5592 no . 1_655 C(15) H(44) 3.4997 no . 1_655 C(15) H(45) 3.5887 no . 1_655 C(16) H(36) 3.2724 no . 1_655 C(16) H(44) 3.0437 no . 1_655 C(18) H(22) 3.5453 no . 4_555 C(20) H(31) 3.17(6) no . 4_555 C(21) H(30) 3.3436 no . 4_555 C(21) H(31) 3.21(5) no . 4_555 C(22) H(31) 3.36(5) no . 4_555 C(23) H(31) 3.44(5) no . 4_555 C(23) H(51) 3.0338 no . . C(24) H(31) 3.38(5) no . 4_555 C(24) H(50) 3.2087 no . . C(24) H(51) 3.4645 no . . C(25) H(31) 3.25(6) no . 4_555 C(27) H(35) 3.1477 no . 4_554 C(28) H(34) 3.3294 no . 4_554 C(28) H(35) 3.0501 no . 4_554 C(28) H(37) 3.3370 no . 1_655 C(29) H(34) 3.5302 no . 4_554 C(29) H(35) 2.9567 no . 4_554 C(29) H(36) 3.4028 no . 1_655 C(30) H(35) 2.9530 no . 4_554 C(30) H(51) 3.3402 no . 4_554 C(30) H(58) 3.27(6) no . 4_554 C(31) H(35) 3.0628 no . 4_554 C(31) H(58) 2.80(6) no . 4_554 C(32) H(35) 3.1536 no . 4_554 C(32) H(58) 3.36(6) no . 4_554 C(33) H(44) 3.3635 no . 4_554 C(34) H(44) 3.4261 no . 4_554 C(34) H(45) 3.1985 no . 4_554 C(35) H(6) 3.4361 no . 4_454 C(36) H(23) 3.4747 no . 4_454 C(36) H(43) 3.39(6) no . . C(37) H(10) 3.4855 no . 4_454 C(37) H(42) 3.0684 no . . C(37) H(43) 3.50(6) no . . C(39) H(21) 3.5728 no . 4_555 C(40) H(44) 3.4730 no . 4_554 C(41) H(8) 2.8813 no . 1_455 C(41) H(9) 3.5422 no . 1_455 C(41) H(13) 2.9386 no . . C(42) H(16) 3.0401 no . 1_455 C(42) H(17) 3.2019 no . 1_455 C(42) H(21) 2.9643 no . . C(43) H(16) 3.5182 no . 1_455 C(43) H(17) 2.8090 no . 1_455 C(43) H(20) 3.4310 no . . C(43) H(21) 3.0791 no . . C(44) H(17) 2.9708 no . 1_455 C(44) H(20) 3.1717 no . . C(44) H(50) 3.5159 no . 4_454 C(45) H(17) 3.5019 no . 1_455 C(45) H(20) 3.5911 no . . C(46) H(9) 3.2906 no . 1_455 C(46) H(12) 3.3447 no . . C(47) H(9) 2.8884 no . 1_455 C(47) H(12) 2.9800 no . . C(48) H(8) 3.2956 no . 1_455 C(48) H(9) 2.9990 no . 1_455 C(48) H(12) 3.3264 no . . C(48) H(13) 3.2639 no . . C(49) H(8) 3.5050 no . 1_455 C(49) H(16) 3.5864 no . 1_455 C(49) H(21) 3.4326 no . . C(50) H(8) 3.1113 no . 1_455 C(50) H(13) 3.1033 no . . C(51) H(8) 3.4952 no . 1_455 C(52) H(8) 3.1715 no . 1_455 C(52) H(13) 3.4007 no . . C(55) H(7) 3.3232 no . 1_455 C(55) H(8) 3.5362 no . 1_455 C(55) H(16) 3.4043 no . 1_455 C(56) H(7) 3.2548 no . 1_455 C(56) H(15) 3.3318 no . 1_455 C(63) H(22) 3.0409 no . . C(64) H(22) 3.4792 no . . C(66) H(18) 3.5224 no . 4_455 C(67) H(27) 3.3650 no . 4_455 C(68) H(8) 3.2807 no . 1_455 C(68) H(19) 3.5510 no . 4_455 C(68) H(27) 3.1566 no . 4_455 C(68) H(28) 3.5007 no . 4_455 C(69) H(7) 3.5919 no . 1_455 C(69) H(19) 3.1938 no . 4_455 C(69) H(28) 3.5049 no . 4_455 C(76) H(14) 3.42(8) no . . C(76) H(32) 3.27(5) no . 4_555 C(77) H(13) 3.2839 no . . C(77) H(17) 3.5815 no . 4_455 C(81) H(1) 3.3023 no . . C(81) H(62) 3.2444 no . 4_453 C(82) H(59) 3.2979 no . . C(83) H(5) 3.4464 no . 3_656 H(1) S(1) 3.0412 no . . H(1) F(2) 2.6376 no . . H(1) O(1) 2.5123 no . . H(1) O(2) 2.8827 no . . H(1) C(81) 3.3023 no . . H(1) H(41) 3.2815 no . . H(1) H(42) 3.3052 no . . H(2) F(1) 2.7216 no . 3_655 H(2) F(2) 3.3914 no . 3_655 H(2) F(5) 2.8896 no . . H(2) O(2) 3.1870 no . . H(2) H(38) 3.1942 no . 1_655 H(2) H(41) 3.1185 no . . H(3) Cl(3) 3.3137 no . . H(3) Cl(6) 3.4723 no . 2_646 H(3) F(1) 2.9725 no . 3_655 H(3) H(38) 3.4402 no . 1_655 H(4) Cl(6) 3.5194 no . 2_646 H(4) H(49) 3.1928 no . . H(4) H(61) 3.1998 no . 1_655 H(5) Cl(1) 2.9827 no . 3_656 H(5) Cl(3) 3.3024 no . 3_656 H(5) C(83) 3.4464 no . 3_656 H(5) H(45) 3.2112 no . 1_655 H(5) H(49) 3.4355 no . . H(5) H(61) 3.0928 no . 1_655 H(6) C(35) 3.4361 no . 4_555 H(6) H(20) 2.8382 no . 4_555 H(6) H(31) 3.4072 no . 4_555 H(6) H(32) 3.2208 no . 4_555 H(6) H(45) 2.9926 no . 1_655 H(6) H(50) 2.8800 no . . H(7) C(55) 3.3232 no . 1_655 H(7) C(56) 3.2548 no . 1_655 H(7) C(69) 3.5919 no . 1_655 H(7) H(36) 2.7174 no . 1_655 H(7) H(37) 2.6156 no . 1_655 H(7) H(44) 3.5374 no . 1_655 H(7) H(45) 3.3262 no . 1_655 H(8) C(41) 2.8813 no . 1_655 H(8) C(48) 3.2956 no . 1_655 H(8) C(49) 3.5050 no . 1_655 H(8) C(50) 3.1113 no . 1_655 H(8) C(51) 3.4952 no . 1_655 H(8) C(52) 3.1715 no . 1_655 H(8) C(55) 3.5362 no . 1_655 H(8) C(68) 3.2807 no . 1_655 H(8) H(36) 2.5961 no . 1_655 H(8) H(44) 2.7689 no . 1_655 H(9) F(3) 3.0542 no . 4_555 H(9) O(1) 3.5404 no . 4_555 H(9) C(41) 3.5422 no . 1_655 H(9) C(46) 3.2906 no . 1_655 H(9) C(47) 2.8884 no . 1_655 H(9) C(48) 2.9990 no . 1_655 H(9) H(34) 3.1218 no . 1_655 H(9) H(35) 3.2286 no . 1_655 H(10) S(1) 3.0348 no . 4_555 H(10) F(3) 3.3943 no . 4_555 H(10) O(1) 2.3691 no . 4_555 H(10) O(3) 2.8590 no . 4_555 H(10) C(37) 3.4855 no . 4_555 H(10) H(22) 3.1397 no . 4_555 H(11) S(2) 3.0121 no . 2_555 H(11) F(6) 3.3723 no . 2_555 H(11) O(5) 2.5338 no . 2_555 H(11) O(6) 2.5964 no . 2_555 H(11) H(30) 3.0467 no . 4_555 H(12) Cl(1) 3.3784 no . 2_555 H(12) F(6) 2.7723 no . 2_555 H(12) C(46) 3.3447 no . . H(12) C(47) 2.9800 no . . H(12) C(48) 3.3264 no . . H(12) H(34) 3.0302 no . . H(13) C(41) 2.9386 no . . H(13) C(48) 3.2639 no . . H(13) C(50) 3.1033 no . . H(13) C(52) 3.4007 no . . H(13) C(77) 3.2839 no . . H(13) H(43) 2.9517 no . . H(13) H(51) 2.7412 no . . H(14) C(76) 3.42(8) no . . H(14) H(42) 3.0429 no . . H(14) H(43) 2.87(9) no . . H(14) H(50) 3.0539 no . . H(14) H(51) 3.4929 no . . H(15) F(2) 3.4476 no . . H(15) F(4) 3.1565 no . 3_655 H(15) C(56) 3.3318 no . 1_655 H(15) H(34) 3.1588 no . 4_554 H(15) H(35) 3.5304 no . 4_554 H(15) H(37) 2.9992 no . 1_655 H(16) F(4) 3.5821 no . 3_655 H(16) F(6) 3.4526 no . 3_655 H(16) O(6) 3.3836 no . 3_655 H(16) C(42) 3.0401 no . 1_655 H(16) C(43) 3.5182 no . 1_655 H(16) C(49) 3.5864 no . 1_655 H(16) C(55) 3.4043 no . 1_655 H(16) H(30) 2.7984 no . 1_655 H(16) H(35) 3.4721 no . 4_554 H(16) H(36) 3.1580 no . 1_655 H(17) C(42) 3.2019 no . 1_655 H(17) C(43) 2.8090 no . 1_655 H(17) C(44) 2.9708 no . 1_655 H(17) C(45) 3.5019 no . 1_655 H(17) C(77) 3.5815 no . 4_554 H(17) H(30) 3.5462 no . 1_655 H(17) H(31) 3.0682 no . 1_655 H(17) H(32) 3.2415 no . 1_655 H(17) H(35) 3.4659 no . 4_554 H(17) H(51) 2.8858 no . 4_554 H(17) H(58) 3.4595 no . 4_554 H(18) Cl(4) 3.0606 no . 1_554 H(18) C(66) 3.5224 no . 4_554 H(18) H(35) 3.5776 no . 4_554 H(18) H(51) 3.5064 no . 4_554 H(18) H(58) 2.6219 no . 4_554 H(19) Cl(1) 3.3308 no . 2_555 H(19) Cl(2) 3.4209 no . 2_555 H(19) C(68) 3.5510 no . 4_554 H(19) C(69) 3.1938 no . 4_554 H(19) H(44) 3.2835 no . 4_554 H(19) H(45) 2.7397 no . 4_554 H(20) Cl(1) 3.2584 no . 2_555 H(20) C(43) 3.4310 no . . H(20) C(44) 3.1717 no . . H(20) C(45) 3.5911 no . . H(20) H(6) 2.8382 no . 4_454 H(20) H(31) 3.5793 no . . H(20) H(32) 3.2656 no . . H(20) H(45) 3.5995 no . 4_554 H(21) N(1) 3.4538 no . 4_454 H(21) C(39) 3.5728 no . 4_454 H(21) C(42) 2.9643 no . . H(21) C(43) 3.0791 no . . H(21) C(49) 3.4326 no . . H(21) H(23) 2.8745 no . 4_454 H(21) H(30) 3.1759 no . . H(21) H(31) 3.2696 no . . H(21) H(43) 3.0982 no . . H(22) O(1) 2.6186 no . . H(22) C(18) 3.5453 no . 4_454 H(22) C(63) 3.0409 no . . H(22) C(64) 3.4792 no . . H(22) H(10) 3.1397 no . 4_454 H(22) H(23) 3.1452 no . 4_454 H(22) H(42) 2.4468 no . . H(22) H(43) 3.2632 no . . H(23) O(1) 3.5127 no . 4_555 H(23) O(6) 3.3247 no . 2_555 H(23) C(36) 3.4747 no . 4_555 H(23) H(21) 2.8745 no . 4_555 H(23) H(22) 3.1452 no . 4_555 H(23) H(30) 3.3331 no . 4_555 H(24) S(2) 3.3212 no . 2_555 H(24) O(5) 2.5498 no . 2_555 H(24) O(6) 3.1848 no . 2_555 H(25) S(1) 3.2852 no . 4_555 H(25) O(1) 3.0730 no . 4_555 H(25) O(3) 2.6368 no . 4_555 H(26) Cl(5) 3.38(8) no . 1_554 H(27) Cl(5) 3.1385 no . 1_554 H(27) C(67) 3.3650 no . 4_554 H(27) C(68) 3.1566 no . 4_554 H(27) H(44) 3.1270 no . 4_554 H(27) H(58) 3.1529 no . 4_554 H(28) Cl(2) 3.1645 no . 2_555 H(28) C(68) 3.5007 no . 4_554 H(28) C(69) 3.5049 no . 4_554 H(28) H(44) 3.4225 no . 4_554 H(28) H(45) 3.5227 no . 4_554 H(29) O(1) 2.82(5) no . . H(30) O(6) 2.4206 no . 3_555 H(30) C(21) 3.3436 no . 4_454 H(30) H(11) 3.0467 no . 4_454 H(30) H(16) 2.7984 no . 1_455 H(30) H(17) 3.5462 no . 1_455 H(30) H(21) 3.1759 no . . H(30) H(23) 3.3331 no . 4_454 H(31) C(20) 3.17(6) no . 4_454 H(31) C(21) 3.21(5) no . 4_454 H(31) C(22) 3.36(5) no . 4_454 H(31) C(23) 3.44(5) no . 4_454 H(31) C(24) 3.38(5) no . 4_454 H(31) C(25) 3.25(6) no . 4_454 H(31) H(6) 3.4072 no . 4_454 H(31) H(17) 3.0682 no . 1_455 H(31) H(20) 3.5793 no . . H(31) H(21) 3.2696 no . . H(31) H(50) 3.1516 no . 4_454 H(31) H(51) 3.3586 no . 4_454 H(32) C(76) 3.27(5) no . 4_454 H(32) H(6) 3.2208 no . 4_454 H(32) H(17) 3.2415 no . 1_455 H(32) H(20) 3.2656 no . . H(32) H(50) 2.7604 no . 4_454 H(32) H(51) 3.5787 no . 4_454 H(33) Cl(1) 3.1339 no . 2_555 H(33) Cl(4) 3.5527 no . 1_454 H(33) F(3) 2.9816 no . 4_455 H(33) F(6) 3.5467 no . 2_555 H(34) F(2) 3.5813 no . 4_455 H(34) F(3) 2.8695 no . 4_455 H(34) F(6) 2.6265 no . 2_555 H(34) C(28) 3.3294 no . 4_455 H(34) C(29) 3.5302 no . 4_455 H(34) H(9) 3.1218 no . 1_455 H(34) H(12) 3.0302 no . . H(34) H(15) 3.1588 no . 4_455 H(35) C(27) 3.1477 no . 4_455 H(35) C(28) 3.0501 no . 4_455 H(35) C(29) 2.9567 no . 4_455 H(35) C(30) 2.9530 no . 4_455 H(35) C(31) 3.0628 no . 4_455 H(35) C(32) 3.1536 no . 4_455 H(35) H(9) 3.2286 no . 1_455 H(35) H(15) 3.5304 no . 4_455 H(35) H(16) 3.4721 no . 4_455 H(35) H(17) 3.4659 no . 4_455 H(35) H(18) 3.5776 no . 4_455 H(36) C(15) 3.3144 no . 1_455 H(36) C(16) 3.2724 no . 1_455 H(36) C(29) 3.4028 no . 1_455 H(36) H(7) 2.7174 no . 1_455 H(36) H(8) 2.5961 no . 1_455 H(36) H(16) 3.1580 no . 1_455 H(37) C(1) 2.9371 no . 1_455 H(37) C(2) 3.4222 no . 1_455 H(37) C(5) 3.5307 no . 1_455 H(37) C(9) 3.3305 no . 1_455 H(37) C(10) 2.9797 no . 1_455 H(37) C(11) 3.2825 no . 1_455 H(37) C(12) 3.5189 no . 1_455 H(37) C(15) 3.5592 no . 1_455 H(37) C(28) 3.3370 no . 1_455 H(37) H(7) 2.6156 no . 1_455 H(37) H(15) 2.9992 no . 1_455 H(38) F(1) 2.8852 no . 3_555 H(38) F(4) 3.4915 no . 3_555 H(38) C(2) 3.3170 no . 1_455 H(38) C(3) 2.9831 no . 1_455 H(38) C(4) 3.0996 no . 1_455 H(38) C(5) 3.5197 no . 1_455 H(38) H(2) 3.1942 no . 1_455 H(38) H(3) 3.4402 no . 1_455 H(39) S(1) 3.2021 no . 3_555 H(39) F(1) 3.3208 no . 3_555 H(39) O(2) 2.8150 no . 3_555 H(39) O(3) 2.6526 no . 3_555 H(39) H(62) 3.3074 no . 2_546 H(40) S(2) 3.1362 no . . H(40) F(5) 3.4547 no . . H(40) O(4) 2.4776 no . . H(40) O(5) 2.8801 no . . H(40) H(59) 3.4037 no . . H(41) F(5) 3.1146 no . . H(41) O(2) 3.1073 no . . H(41) O(4) 3.5582 no . . H(41) C(2) 3.1905 no . . H(41) C(3) 3.0516 no . . H(41) H(1) 3.2815 no . . H(41) H(2) 3.1185 no . . H(42) C(1) 2.9827 no . . H(42) C(2) 3.1405 no . . H(42) C(10) 3.4874 no . . H(42) C(11) 3.3161 no . . H(42) C(37) 3.0684 no . . H(42) H(1) 3.3052 no . . H(42) H(14) 3.0429 no . . H(42) H(22) 2.4468 no . . H(43) C(36) 3.39(6) no . . H(43) C(37) 3.50(6) no . . H(43) H(13) 2.9517 no . . H(43) H(14) 2.87(9) no . . H(43) H(21) 3.0982 no . . H(43) H(22) 3.2632 no . . H(44) N(2) 3.3092 no . 4_455 H(44) C(15) 3.4997 no . 1_455 H(44) C(16) 3.0437 no . 1_455 H(44) C(33) 3.3635 no . 4_455 H(44) C(34) 3.4261 no . 4_455 H(44) C(40) 3.4730 no . 4_455 H(44) H(7) 3.5374 no . 1_455 H(44) H(8) 2.7689 no . 1_455 H(44) H(19) 3.2835 no . 4_455 H(44) H(27) 3.1270 no . 4_455 H(44) H(28) 3.4225 no . 4_455 H(45) C(7) 3.2117 no . 1_455 H(45) C(8) 2.9483 no . 1_455 H(45) C(9) 3.5621 no . 1_455 H(45) C(15) 3.5887 no . 1_455 H(45) C(34) 3.1985 no . 4_455 H(45) H(5) 3.2112 no . 1_455 H(45) H(6) 2.9926 no . 1_455 H(45) H(7) 3.3262 no . 1_455 H(45) H(19) 2.7397 no . 4_455 H(45) H(20) 3.5995 no . 4_455 H(45) H(28) 3.5227 no . 4_455 H(47) Cl(5) 3.5614 no . 2_546 H(47) Cl(6) 3.2599 no . 2_546 H(47) H(55) 3.1495 no . 3_556 H(48) Cl(3) 3.0492 no . . H(49) C(5) 3.2492 no . . H(49) C(6) 2.9285 no . . H(49) C(7) 3.0184 no . . H(49) C(8) 3.4791 no . . H(49) H(4) 3.1928 no . . H(49) H(5) 3.4355 no . . H(50) C(7) 3.3588 no . . H(50) C(8) 2.8973 no . . H(50) C(9) 3.2306 no . . H(50) C(24) 3.2087 no . . H(50) C(44) 3.5159 no . 4_555 H(50) H(6) 2.8800 no . . H(50) H(14) 3.0539 no . . H(50) H(31) 3.1516 no . 4_555 H(50) H(32) 2.7604 no . 4_555 H(51) C(23) 3.0338 no . . H(51) C(24) 3.4645 no . . H(51) C(30) 3.3402 no . 4_455 H(51) H(13) 2.7412 no . . H(51) H(14) 3.4929 no . . H(51) H(17) 2.8858 no . 4_455 H(51) H(18) 3.5064 no . 4_455 H(51) H(31) 3.3586 no . 4_555 H(51) H(32) 3.5787 no . 4_555 H(52) O(3) 3.2749 no . 3_555 H(52) O(5) 3.3347 no . . H(53) S(2) 3.3544 no . . H(53) O(4) 2.8965 no . . H(53) O(4) 2.8597 no . 3_555 H(53) O(5) 2.9135 no . . H(54) S(1) 3.3165 no . 3_555 H(54) O(2) 2.9594 no . 3_555 H(54) O(3) 2.7432 no . 3_555 H(54) O(4) 2.7589 no . 3_555 H(55) Cl(2) 3.4882 no . . H(55) Cl(5) 3.5770 no . 4_454 H(55) H(47) 3.1495 no . 3_556 H(56) Cl(2) 3.2734 no . . H(57) Cl(5) 3.2316 no . 2_546 H(58) C(30) 3.27(6) no . 4_455 H(58) C(31) 2.80(6) no . 4_455 H(58) C(32) 3.36(6) no . 4_455 H(58) H(17) 3.4595 no . 4_455 H(58) H(18) 2.6219 no . 4_455 H(58) H(27) 3.1529 no . 4_455 H(59) S(2) 3.2493 no . . H(59) F(5) 2.9226 no . . H(59) F(6) 3.2680 no . . H(59) O(5) 2.1017 no . . H(59) C(82) 3.2979 no . . H(59) H(40) 3.4037 no . . H(61) Cl(2) 3.2918 no . 3_556 H(61) Cl(6) 3.3848 no . 2_546 H(61) C(6) 3.1026 no . 1_455 H(61) C(7) 3.0844 no . 1_455 H(61) H(4) 3.1998 no . 1_455 H(61) H(5) 3.0928 no . 1_455 H(62) S(1) 3.2754 no . 4_556 H(62) F(1) 2.9561 no . 4_556 H(62) F(3) 2.9556 no . 4_556 H(62) O(3) 2.1869 no . 4_556 H(62) C(81) 3.2444 no . 4_556 H(62) H(39) 3.3074 no . 2_556 #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 975888' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data__060121tt #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C41 H30 Cl2 N2 O2' _chemical_formula_moiety 'C41 H30 Cl2 N2 O2' _chemical_formula_weight 653.61 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,+Y,1/2-Z 3 -X,-Y,-Z 4 +X,-Y,1/2+Z 5 1/2+X,1/2+Y,+Z 6 1/2-X,1/2+Y,1/2-Z 7 1/2-X,1/2-Y,-Z 8 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 33.637(17) _cell_length_b 11.993(6) _cell_length_c 15.904(8) _cell_angle_alpha 90.0000 _cell_angle_beta 97.925(9) _cell_angle_gamma 90.0000 _cell_volume 6355(6) _cell_formula_units_Z 8 _cell_measurement_reflns_used 7725 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 27.10 _cell_measurement_temperature 153 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.020 _exptl_crystal_density_diffrn 1.366 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2720.00 _exptl_absorpt_coefficient_mu 0.245 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.944 _exptl_absorpt_correction_T_max 0.995 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 153 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_reflns_number 28173 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_theta_max 27.10 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6973 _reflns_number_gt 3047 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0759 _refine_ls_wR_factor_ref 0.1462 _refine_ls_number_restraints ? _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 6973 _refine_ls_number_parameters 458 _refine_ls_goodness_of_fit_ref 1.202 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0001Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 1.470 _refine_diff_density_min -0.712 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.1484 0.1585 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Cl(1) Cl 0.08172(6) -0.33257(12) 0.27847(12) 0.1026(7) Uani 1.0 8 d . . . Cl(2) Cl 0.01943(11) -0.3335(3) 0.1195(3) 0.1197(15) Uani 0.5000 8 d . . . Cl(3) Cl 0.05302(16) -0.4135(3) 0.1348(3) 0.1333(18) Uani 0.5000 8 d . . . O(1) O 0.17018(8) 0.1504(2) 0.19234(15) 0.0349(9) Uani 1.0 8 d . . . O(2) O 0.18054(8) 0.0652(2) 0.25917(15) 0.0335(8) Uani 1.0 8 d . . . N(1) N 0.20184(9) 0.4059(3) 0.1723(2) 0.0336(10) Uani 1.0 8 d . . . N(2) N 0.18081(11) -0.2078(3) 0.2511(2) 0.0427(12) Uani 1.0 8 d . . . C(1) C 0.08348(11) 0.2563(3) 0.3014(3) 0.0269(11) Uani 1.0 8 d . . . C(2) C 0.07374(12) 0.3657(3) 0.3105(3) 0.0351(13) Uani 1.0 8 d . . . C(3) C 0.03823(12) 0.3903(4) 0.3466(3) 0.0401(14) Uani 1.0 8 d . . . C(4) C 0.01374(12) 0.3098(4) 0.3715(3) 0.0388(14) Uani 1.0 8 d . . . C(5) C 0.02326(11) 0.1958(4) 0.3619(3) 0.0317(12) Uani 1.0 8 d . . . C(6) C 0.00197(12) 0.1010(4) 0.3852(3) 0.0373(13) Uani 1.0 8 d . . . C(7) C 0.01634(12) -0.0047(4) 0.3733(3) 0.0412(14) Uani 1.0 8 d . . . C(8) C 0.05288(12) -0.0239(4) 0.3406(3) 0.0366(13) Uani 1.0 8 d . . . C(9) C 0.07396(11) 0.0662(3) 0.3178(3) 0.0266(11) Uani 1.0 8 d . . . C(10) C 0.05820(11) 0.1732(3) 0.3282(3) 0.0266(11) Uani 1.0 8 d . . . C(11) C 0.11699(11) 0.1958(3) 0.2707(2) 0.0253(11) Uani 1.0 8 d . . . C(12) C 0.11185(11) 0.0851(3) 0.2827(2) 0.0239(11) Uani 1.0 8 d . . . C(13) C 0.15101(11) 0.2446(3) 0.2309(3) 0.0256(11) Uani 1.0 8 d . . . C(14) C 0.13717(12) 0.3136(3) 0.1529(3) 0.0292(12) Uani 1.0 8 d . . . C(15) C 0.09990(12) 0.2965(4) 0.1037(3) 0.0386(13) Uani 1.0 8 d . . . C(16) C 0.08905(13) 0.3535(4) 0.0282(3) 0.0488(15) Uani 1.0 8 d . . . C(17) C 0.11584(13) 0.4292(4) 0.0015(3) 0.0445(14) Uani 1.0 8 d . . . C(18) C 0.15272(12) 0.4474(4) 0.0478(3) 0.0368(13) Uani 1.0 8 d . . . C(19) C 0.16409(12) 0.3893(3) 0.1246(3) 0.0312(12) Uani 1.0 8 d . . . C(20) C 0.20777(11) 0.3817(3) 0.2594(3) 0.0312(12) Uani 1.0 8 d . . . C(21) C 0.23824(12) 0.4313(4) 0.3152(3) 0.0365(13) Uani 1.0 8 d . . . C(22) C 0.24237(12) 0.4075(4) 0.4006(3) 0.0417(14) Uani 1.0 8 d . . . C(23) C 0.21629(12) 0.3355(4) 0.4330(3) 0.0360(13) Uani 1.0 8 d . . . C(24) C 0.18630(12) 0.2850(4) 0.3782(3) 0.0329(12) Uani 1.0 8 d . . . C(25) C 0.18145(11) 0.3060(3) 0.2915(3) 0.0262(11) Uani 1.0 8 d . . . C(26) C 0.23282(12) 0.4658(4) 0.1336(3) 0.0463(15) Uani 1.0 8 d . . . C(27) C 0.14290(11) -0.0003(3) 0.2678(3) 0.0290(11) Uani 1.0 8 d . . . C(28) C 0.13148(11) -0.0723(3) 0.1909(3) 0.0290(12) Uani 1.0 8 d . . . C(29) C 0.10179(12) -0.0416(4) 0.1259(3) 0.0325(12) Uani 1.0 8 d . . . C(30) C 0.09257(13) -0.1056(4) 0.0537(3) 0.0397(14) Uani 1.0 8 d . . . C(31) C 0.11414(14) -0.2017(4) 0.0457(3) 0.0452(15) Uani 1.0 8 d . . . C(32) C 0.14378(14) -0.2351(4) 0.1089(3) 0.0438(14) Uani 1.0 8 d . . . C(33) C 0.15265(13) -0.1719(4) 0.1833(3) 0.0361(13) Uani 1.0 8 d . . . C(34) C 0.17759(12) -0.1710(4) 0.3336(3) 0.0343(13) Uani 1.0 8 d . . . C(35) C 0.19417(13) -0.2314(4) 0.4053(3) 0.0444(14) Uani 1.0 8 d . . . C(36) C 0.19170(13) -0.1903(4) 0.4854(3) 0.0449(15) Uani 1.0 8 d . . . C(37) C 0.17261(12) -0.0913(4) 0.4962(3) 0.0388(13) Uani 1.0 8 d . . . C(38) C 0.15591(11) -0.0312(4) 0.4262(3) 0.0318(12) Uani 1.0 8 d . . . C(39) C 0.15790(11) -0.0694(3) 0.3446(3) 0.0283(11) Uani 1.0 8 d . . . C(40) C 0.20743(15) -0.3013(4) 0.2397(3) 0.0641(18) Uani 1.0 8 d . . . C(41) C 0.0520 -0.2960 0.2000 0.300(8) Uani 1.0 8 d . . . H(1) H 0.0903 0.4231 0.2930 0.0418(16) Uiso 1.0 8 calc R . . H(2) H 0.0314 0.4663 0.3533 0.0482(17) Uiso 1.0 8 calc R . . H(3) H -0.0097 0.3297 0.3953 0.0471(17) Uiso 1.0 8 calc R . . H(4) H -0.0219 0.1107 0.4100 0.0448(16) Uiso 1.0 8 calc R . . H(5) H 0.0010 -0.0669 0.3872 0.0497(17) Uiso 1.0 8 calc R . . H(6) H 0.0625 -0.0975 0.3344 0.0438(16) Uiso 1.0 8 calc R . . H(7) H 0.0817 0.2455 0.1235 0.0461(17) Uiso 1.0 8 calc R . . H(8) H 0.0638 0.3398 -0.0049 0.0572(18) Uiso 1.0 8 calc R . . H(9) H 0.1086 0.4696 -0.0497 0.0525(17) Uiso 1.0 8 calc R . . H(10) H 0.1709 0.4993 0.0288 0.0445(17) Uiso 1.0 8 calc R . . H(11) H 0.2559 0.4823 0.2936 0.0433(16) Uiso 1.0 8 calc R . . H(12) H 0.2637 0.4404 0.4377 0.0489(17) Uiso 1.0 8 calc R . . H(13) H 0.2189 0.3209 0.4922 0.0423(16) Uiso 1.0 8 calc R . . H(14) H 0.1684 0.2351 0.4001 0.0396(16) Uiso 1.0 8 calc R . . H(15) H 0.0875 0.0256 0.1316 0.0390 Uiso 1.0 8 calc R . . H(16) H 0.0715 -0.0844 0.0106 0.0469 Uiso 1.0 8 calc R . . H(17) H 0.1085 -0.2450 -0.0046 0.0543 Uiso 1.0 8 calc R . . H(18) H 0.1585 -0.3013 0.1023 0.0528 Uiso 1.0 8 calc R . . H(19) H 0.2066 -0.3014 0.3988 0.0525 Uiso 1.0 8 calc R . . H(20) H 0.2034 -0.2313 0.5337 0.0530 Uiso 1.0 8 calc R . . H(21) H 0.1713 -0.0640 0.5519 0.0462 Uiso 1.0 8 calc R . . H(22) H 0.1426 0.0371 0.4337 0.0378 Uiso 1.0 8 calc R . . H(23) H 0.2310 0.4457 0.0754 0.0569 Uiso 1.0 8 calc R . . H(24) H 0.2290 0.5439 0.1382 0.0569 Uiso 1.0 8 calc R . . H(25) H 0.2586 0.4461 0.1620 0.0569 Uiso 1.0 8 calc R . . H(26) H 0.2339 -0.2832 0.2652 0.0777 Uiso 1.0 8 calc R . . H(27) H 0.1986 -0.3663 0.2657 0.0776 Uiso 1.0 8 calc R . . H(28) H 0.2074 -0.3145 0.1808 0.0776 Uiso 1.0 8 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cl(1) 0.1263(16) 0.0529(9) 0.1291(15) -0.0091(10) 0.0202(12) 0.0266(10) Cl(2) 0.078(3) 0.089(3) 0.171(4) -0.042(2) -0.055(3) 0.062(3) Cl(3) 0.208(5) 0.091(3) 0.108(3) -0.074(4) 0.048(4) -0.002(3) O(1) 0.0418(18) 0.0316(16) 0.0314(16) 0.0048(14) 0.0056(14) 0.0059(13) O(2) 0.0359(17) 0.0311(16) 0.0334(16) 0.0012(13) 0.0044(13) 0.0069(13) N(1) 0.026(2) 0.037(2) 0.038(2) -0.0045(16) 0.0081(17) 0.0060(17) N(2) 0.049(3) 0.039(3) 0.039(3) 0.0203(19) 0.0035(19) 0.0029(18) C(1) 0.023(3) 0.033(3) 0.024(2) 0.0003(18) 0.0008(17) 0.0030(18) C(2) 0.034(3) 0.031(3) 0.040(3) -0.000(2) 0.002(2) 0.001(2) C(3) 0.042(3) 0.039(3) 0.039(3) 0.011(3) 0.006(3) -0.006(2) C(4) 0.032(3) 0.047(3) 0.039(3) 0.007(3) 0.010(2) -0.001(3) C(5) 0.027(3) 0.039(3) 0.028(3) -0.000(2) 0.0012(18) 0.000(2) C(6) 0.025(3) 0.050(3) 0.037(3) -0.005(2) 0.0042(19) 0.000(3) C(7) 0.037(3) 0.045(3) 0.043(3) -0.014(3) 0.008(3) 0.002(3) C(8) 0.040(3) 0.033(3) 0.037(3) -0.001(2) 0.006(3) -0.002(2) C(9) 0.024(3) 0.031(3) 0.024(2) 0.0000(18) 0.0016(18) 0.0016(18) C(10) 0.026(3) 0.032(3) 0.022(2) -0.0004(19) 0.0024(17) -0.0005(18) C(11) 0.020(2) 0.031(3) 0.023(2) -0.0031(18) 0.0009(17) 0.0023(18) C(12) 0.022(2) 0.030(3) 0.0189(19) 0.0027(18) -0.0005(16) 0.0011(17) C(13) 0.020(3) 0.027(2) 0.029(2) 0.0028(17) 0.0036(18) 0.0008(18) C(14) 0.032(3) 0.028(3) 0.028(3) 0.0027(19) 0.0059(19) 0.0010(18) C(15) 0.032(3) 0.049(3) 0.035(3) -0.001(3) 0.003(2) 0.012(3) C(16) 0.032(3) 0.068(4) 0.043(3) -0.002(3) -0.007(3) 0.017(3) C(17) 0.046(3) 0.051(3) 0.034(3) 0.008(3) -0.002(3) 0.014(3) C(18) 0.039(3) 0.034(3) 0.038(3) 0.004(2) 0.009(3) 0.009(2) C(19) 0.030(3) 0.034(3) 0.030(3) 0.004(2) 0.004(2) 0.0011(19) C(20) 0.026(3) 0.031(3) 0.036(3) 0.0015(19) 0.002(2) 0.0001(19) C(21) 0.028(3) 0.035(3) 0.045(3) -0.006(2) 0.001(2) -0.001(3) C(22) 0.033(3) 0.046(3) 0.044(3) -0.002(3) -0.004(3) -0.010(3) C(23) 0.035(3) 0.044(3) 0.027(3) 0.008(3) -0.003(2) -0.007(2) C(24) 0.031(3) 0.038(3) 0.030(3) -0.003(2) 0.0045(19) -0.002(2) C(25) 0.023(3) 0.026(2) 0.030(3) 0.0036(18) 0.0021(18) 0.0000(18) C(26) 0.040(3) 0.049(3) 0.053(3) -0.002(3) 0.019(3) 0.007(3) C(27) 0.029(3) 0.031(3) 0.027(3) 0.0003(19) 0.0043(19) 0.0046(19) C(28) 0.031(3) 0.030(3) 0.026(3) 0.0001(19) 0.0045(19) -0.0006(19) C(29) 0.036(3) 0.035(3) 0.026(3) 0.000(2) 0.0040(19) -0.0009(19) C(30) 0.042(3) 0.044(3) 0.031(3) -0.011(3) -0.002(2) -0.000(2) C(31) 0.062(4) 0.041(3) 0.032(3) -0.014(3) 0.006(3) -0.012(3) C(32) 0.062(4) 0.029(3) 0.042(3) 0.000(3) 0.009(3) -0.009(3) C(33) 0.047(3) 0.030(3) 0.032(3) -0.000(2) 0.007(2) -0.001(2) C(34) 0.036(3) 0.036(3) 0.030(3) 0.001(2) 0.002(2) 0.005(2) C(35) 0.044(3) 0.037(3) 0.050(3) 0.006(3) 0.000(3) 0.014(3) C(36) 0.051(3) 0.044(3) 0.038(3) -0.007(3) -0.002(3) 0.017(3) C(37) 0.041(3) 0.046(3) 0.029(3) -0.007(3) 0.001(2) 0.006(2) C(38) 0.030(3) 0.036(3) 0.029(3) -0.0003(19) 0.0013(19) 0.0044(19) C(39) 0.026(3) 0.029(3) 0.029(3) 0.0002(18) 0.0016(18) 0.0054(19) C(40) 0.080(4) 0.042(3) 0.072(4) 0.021(3) 0.016(3) -0.004(3) C(41) 0.44(3) 0.290(16) 0.137(10) -0.090(15) -0.082(12) 0.104(10) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution SIR97 _computing_structure_refinement 'CRYSTALS (Carruthers, et al., 1999)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cl(1) C(41) 1.5509(19) yes . . Cl(2) Cl(3) 1.477(6) yes . . Cl(2) C(41) 1.629(4) yes . . Cl(3) C(41) 1.753(4) yes . . O(1) O(2) 1.481(4) yes . . O(1) C(13) 1.475(5) yes . . O(2) C(27) 1.513(5) yes . . N(1) C(19) 1.400(5) yes . . N(1) C(20) 1.402(5) yes . . N(1) C(26) 1.469(6) yes . . N(2) C(33) 1.401(5) yes . . N(2) C(34) 1.403(6) yes . . N(2) C(40) 1.461(6) yes . . C(1) C(2) 1.365(6) yes . . C(1) C(10) 1.415(6) yes . . C(1) C(11) 1.478(6) yes . . C(2) C(3) 1.425(6) yes . . C(3) C(4) 1.363(6) yes . . C(4) C(5) 1.417(6) yes . . C(5) C(6) 1.421(6) yes . . C(5) C(10) 1.384(6) yes . . C(6) C(7) 1.378(6) yes . . C(7) C(8) 1.418(6) yes . . C(8) C(9) 1.368(6) yes . . C(9) C(10) 1.407(6) yes . . C(9) C(12) 1.477(6) yes . . C(11) C(12) 1.356(5) yes . . C(11) C(13) 1.501(6) yes . . C(12) C(27) 1.505(6) yes . . C(13) C(14) 1.510(5) yes . . C(13) C(25) 1.500(5) yes . . C(14) C(15) 1.399(6) yes . . C(14) C(19) 1.399(6) yes . . C(15) C(16) 1.386(6) yes . . C(16) C(17) 1.386(7) yes . . C(17) C(18) 1.370(6) yes . . C(18) C(19) 1.413(6) yes . . C(20) C(21) 1.393(6) yes . . C(20) C(25) 1.413(6) yes . . C(21) C(22) 1.377(6) yes . . C(22) C(23) 1.380(6) yes . . C(23) C(24) 1.379(6) yes . . C(24) C(25) 1.388(6) yes . . C(27) C(28) 1.502(5) yes . . C(27) C(39) 1.504(5) yes . . C(28) C(29) 1.384(5) yes . . C(28) C(33) 1.404(6) yes . . C(29) C(30) 1.381(6) yes . . C(30) C(31) 1.377(6) yes . . C(31) C(32) 1.375(6) yes . . C(32) C(33) 1.402(6) yes . . C(34) C(35) 1.400(6) yes . . C(34) C(39) 1.409(6) yes . . C(35) C(36) 1.379(7) yes . . C(36) C(37) 1.372(6) yes . . C(37) C(38) 1.380(6) yes . . C(38) C(39) 1.387(6) yes . . C(2) H(1) 0.950 no . . C(3) H(2) 0.950 no . . C(4) H(3) 0.950 no . . C(6) H(4) 0.950 no . . C(7) H(5) 0.950 no . . C(8) H(6) 0.950 no . . C(15) H(7) 0.950 no . . C(16) H(8) 0.950 no . . C(17) H(9) 0.950 no . . C(18) H(10) 0.950 no . . C(21) H(11) 0.950 no . . C(22) H(12) 0.950 no . . C(23) H(13) 0.950 no . . C(24) H(14) 0.950 no . . C(26) H(23) 0.950 no . . C(26) H(24) 0.950 no . . C(26) H(25) 0.950 no . . C(29) H(15) 0.950 no . . C(30) H(16) 0.950 no . . C(31) H(17) 0.950 no . . C(32) H(18) 0.950 no . . C(35) H(19) 0.950 no . . C(36) H(20) 0.950 no . . C(37) H(21) 0.950 no . . C(38) H(22) 0.950 no . . C(40) H(26) 0.950 no . . C(40) H(27) 0.950 no . . C(40) H(28) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cl(3) Cl(2) C(41) 68.5(3) yes . . . Cl(2) Cl(3) C(41) 59.9(3) yes . . . O(2) O(1) C(13) 107.7(3) yes . . . O(1) O(2) C(27) 107.8(3) yes . . . C(19) N(1) C(20) 120.0(4) yes . . . C(19) N(1) C(26) 119.1(3) yes . . . C(20) N(1) C(26) 120.2(3) yes . . . C(33) N(2) C(34) 119.5(4) yes . . . C(33) N(2) C(40) 120.1(4) yes . . . C(34) N(2) C(40) 119.0(4) yes . . . C(2) C(1) C(10) 118.8(4) yes . . . C(2) C(1) C(11) 135.4(4) yes . . . C(10) C(1) C(11) 105.7(3) yes . . . C(1) C(2) C(3) 117.9(4) yes . . . C(2) C(3) C(4) 123.0(4) yes . . . C(3) C(4) C(5) 119.8(4) yes . . . C(4) C(5) C(6) 128.0(4) yes . . . C(4) C(5) C(10) 116.6(4) yes . . . C(6) C(5) C(10) 115.4(4) yes . . . C(5) C(6) C(7) 120.1(4) yes . . . C(6) C(7) C(8) 122.6(4) yes . . . C(7) C(8) C(9) 118.4(4) yes . . . C(8) C(9) C(10) 118.1(4) yes . . . C(8) C(9) C(12) 136.6(4) yes . . . C(10) C(9) C(12) 105.3(3) yes . . . C(1) C(10) C(5) 123.8(4) yes . . . C(1) C(10) C(9) 110.8(4) yes . . . C(5) C(10) C(9) 125.4(4) yes . . . C(1) C(11) C(12) 108.5(4) yes . . . C(1) C(11) C(13) 127.4(3) yes . . . C(12) C(11) C(13) 124.1(4) yes . . . C(9) C(12) C(11) 109.6(4) yes . . . C(9) C(12) C(27) 127.5(4) yes . . . C(11) C(12) C(27) 122.7(4) yes . . . O(1) C(13) C(11) 106.2(3) yes . . . O(1) C(13) C(14) 100.5(3) yes . . . O(1) C(13) C(25) 110.2(3) yes . . . C(11) C(13) C(14) 113.2(3) yes . . . C(11) C(13) C(25) 114.3(3) yes . . . C(14) C(13) C(25) 111.4(3) yes . . . C(13) C(14) C(15) 122.0(4) yes . . . C(13) C(14) C(19) 118.7(4) yes . . . C(15) C(14) C(19) 119.0(4) yes . . . C(14) C(15) C(16) 121.4(4) yes . . . C(15) C(16) C(17) 118.9(4) yes . . . C(16) C(17) C(18) 121.2(4) yes . . . C(17) C(18) C(19) 120.2(4) yes . . . N(1) C(19) C(14) 119.8(4) yes . . . N(1) C(19) C(18) 121.0(4) yes . . . C(14) C(19) C(18) 119.2(4) yes . . . N(1) C(20) C(21) 122.2(4) yes . . . N(1) C(20) C(25) 118.7(3) yes . . . C(21) C(20) C(25) 119.1(4) yes . . . C(20) C(21) C(22) 120.4(4) yes . . . C(21) C(22) C(23) 121.0(4) yes . . . C(22) C(23) C(24) 119.0(4) yes . . . C(23) C(24) C(25) 121.6(4) yes . . . C(13) C(25) C(20) 119.3(4) yes . . . C(13) C(25) C(24) 121.7(4) yes . . . C(20) C(25) C(24) 118.8(4) yes . . . O(2) C(27) C(12) 105.6(3) yes . . . O(2) C(27) C(28) 110.4(3) yes . . . O(2) C(27) C(39) 99.7(3) yes . . . C(12) C(27) C(28) 114.5(3) yes . . . C(12) C(27) C(39) 114.1(4) yes . . . C(28) C(27) C(39) 111.3(3) yes . . . C(27) C(28) C(29) 122.1(4) yes . . . C(27) C(28) C(33) 118.9(4) yes . . . C(29) C(28) C(33) 118.9(4) yes . . . C(28) C(29) C(30) 122.0(4) yes . . . C(29) C(30) C(31) 118.7(4) yes . . . C(30) C(31) C(32) 121.0(4) yes . . . C(31) C(32) C(33) 120.6(4) yes . . . N(2) C(33) C(28) 119.5(4) yes . . . N(2) C(33) C(32) 121.7(4) yes . . . C(28) C(33) C(32) 118.7(4) yes . . . N(2) C(34) C(35) 121.7(4) yes . . . N(2) C(34) C(39) 119.1(4) yes . . . C(35) C(34) C(39) 119.2(4) yes . . . C(34) C(35) C(36) 120.0(4) yes . . . C(35) C(36) C(37) 120.9(4) yes . . . C(36) C(37) C(38) 119.7(4) yes . . . C(37) C(38) C(39) 121.1(4) yes . . . C(27) C(39) C(34) 119.1(4) yes . . . C(27) C(39) C(38) 121.6(4) yes . . . C(34) C(39) C(38) 119.1(4) yes . . . Cl(1) C(41) Cl(2) 147.48(15) yes . . . Cl(1) C(41) Cl(3) 100.70(16) yes . . . Cl(2) C(41) Cl(3) 51.6(2) yes . . . C(1) C(2) H(1) 120.388 no . . . C(3) C(2) H(1) 121.673 no . . . C(2) C(3) H(2) 118.250 no . . . C(4) C(3) H(2) 118.748 no . . . C(3) C(4) H(3) 120.414 no . . . C(5) C(4) H(3) 119.774 no . . . C(5) C(6) H(4) 119.722 no . . . C(7) C(6) H(4) 120.193 no . . . C(6) C(7) H(5) 118.639 no . . . C(8) C(7) H(5) 118.802 no . . . C(7) C(8) H(6) 120.926 no . . . C(9) C(8) H(6) 120.659 no . . . C(14) C(15) H(7) 118.609 no . . . C(16) C(15) H(7) 119.951 no . . . C(15) C(16) H(8) 120.212 no . . . C(17) C(16) H(8) 120.875 no . . . C(16) C(17) H(9) 119.682 no . . . C(18) C(17) H(9) 119.097 no . . . C(17) C(18) H(10) 120.481 no . . . C(19) C(18) H(10) 119.298 no . . . C(20) C(21) H(11) 119.168 no . . . C(22) C(21) H(11) 120.457 no . . . C(21) C(22) H(12) 119.425 no . . . C(23) C(22) H(12) 119.535 no . . . C(22) C(23) H(13) 120.568 no . . . C(24) C(23) H(13) 120.396 no . . . C(23) C(24) H(14) 119.377 no . . . C(25) C(24) H(14) 119.027 no . . . N(1) C(26) H(23) 109.270 no . . . N(1) C(26) H(24) 109.732 no . . . N(1) C(26) H(25) 109.395 no . . . H(23) C(26) H(24) 109.474 no . . . H(23) C(26) H(25) 109.481 no . . . H(24) C(26) H(25) 109.476 no . . . C(28) C(29) H(15) 118.542 no . . . C(30) C(29) H(15) 119.461 no . . . C(29) C(30) H(16) 120.731 no . . . C(31) C(30) H(16) 120.516 no . . . C(30) C(31) H(17) 119.221 no . . . C(32) C(31) H(17) 119.806 no . . . C(31) C(32) H(18) 119.984 no . . . C(33) C(32) H(18) 119.458 no . . . C(34) C(35) H(19) 120.052 no . . . C(36) C(35) H(19) 119.938 no . . . C(35) C(36) H(20) 119.405 no . . . C(37) C(36) H(20) 119.677 no . . . C(36) C(37) H(21) 119.853 no . . . C(38) C(37) H(21) 120.394 no . . . C(37) C(38) H(22) 119.740 no . . . C(39) C(38) H(22) 119.177 no . . . N(2) C(40) H(26) 109.035 no . . . N(2) C(40) H(27) 109.961 no . . . N(2) C(40) H(28) 109.413 no . . . H(26) C(40) H(27) 109.472 no . . . H(26) C(40) H(28) 109.465 no . . . H(27) C(40) H(28) 109.480 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 Cl(3) Cl(2) C(41) Cl(1) -36.7(4) no . . . . Cl(3) Cl(2) C(41) Cl(3) 0.0(2) no . . . . C(41) Cl(2) Cl(3) C(41) 0.000(12) no . . . . Cl(2) Cl(3) C(41) Cl(1) 160.9(2) no . . . . Cl(2) Cl(3) C(41) Cl(2) 0.00(19) no . . . . O(2) O(1) C(13) C(11) -53.9(3) no . . . . O(2) O(1) C(13) C(14) -172.0(2) no . . . . O(2) O(1) C(13) C(25) 70.4(3) no . . . . C(13) O(1) O(2) C(27) 80.4(3) no . . . . O(1) O(2) C(27) C(12) -54.1(3) no . . . . O(1) O(2) C(27) C(28) 70.1(3) no . . . . O(1) O(2) C(27) C(39) -172.6(2) no . . . . C(19) N(1) C(20) C(21) -156.4(3) no . . . . C(19) N(1) C(20) C(25) 22.4(5) no . . . . C(20) N(1) C(19) C(14) -23.3(5) no . . . . C(20) N(1) C(19) C(18) 157.0(3) no . . . . C(26) N(1) C(19) C(14) 166.7(3) no . . . . C(26) N(1) C(19) C(18) -12.9(5) no . . . . C(26) N(1) C(20) C(21) 13.4(5) no . . . . C(26) N(1) C(20) C(25) -167.8(3) no . . . . C(33) N(2) C(34) C(35) 156.3(4) no . . . . C(33) N(2) C(34) C(39) -25.1(6) no . . . . C(34) N(2) C(33) C(28) 23.4(6) no . . . . C(34) N(2) C(33) C(32) -154.1(4) no . . . . C(40) N(2) C(33) C(28) -170.5(4) no . . . . C(40) N(2) C(33) C(32) 12.1(6) no . . . . C(40) N(2) C(34) C(35) -10.0(6) no . . . . C(40) N(2) C(34) C(39) 168.7(4) no . . . . C(2) C(1) C(10) C(5) 1.5(5) no . . . . C(2) C(1) C(10) C(9) -177.1(3) no . . . . C(10) C(1) C(2) C(3) -0.3(5) no . . . . C(2) C(1) C(11) C(12) 175.3(4) no . . . . C(2) C(1) C(11) C(13) -6.1(6) no . . . . C(11) C(1) C(2) C(3) -177.7(4) no . . . . C(10) C(1) C(11) C(12) -2.3(4) no . . . . C(10) C(1) C(11) C(13) 176.3(3) no . . . . C(11) C(1) C(10) C(5) 179.6(3) no . . . . C(11) C(1) C(10) C(9) 1.0(4) no . . . . C(1) C(2) C(3) C(4) -0.4(6) no . . . . C(2) C(3) C(4) C(5) -0.0(6) no . . . . C(3) C(4) C(5) C(6) 178.9(3) no . . . . C(3) C(4) C(5) C(10) 1.1(5) no . . . . C(4) C(5) C(6) C(7) -178.2(4) no . . . . C(4) C(5) C(10) C(1) -1.9(5) no . . . . C(4) C(5) C(10) C(9) 176.5(3) no . . . . C(6) C(5) C(10) C(1) -180.0(3) no . . . . C(6) C(5) C(10) C(9) -1.5(5) no . . . . C(10) C(5) C(6) C(7) -0.4(5) no . . . . C(5) C(6) C(7) C(8) 2.1(6) no . . . . C(6) C(7) C(8) C(9) -1.9(6) no . . . . C(7) C(8) C(9) C(10) 0.1(5) no . . . . C(7) C(8) C(9) C(12) 179.7(4) no . . . . C(8) C(9) C(10) C(1) -179.7(3) no . . . . C(8) C(9) C(10) C(5) 1.7(5) no . . . . C(8) C(9) C(12) C(11) 178.3(4) no . . . . C(8) C(9) C(12) C(27) -6.4(7) no . . . . C(10) C(9) C(12) C(11) -2.1(4) no . . . . C(10) C(9) C(12) C(27) 173.3(3) no . . . . C(12) C(9) C(10) C(1) 0.6(4) no . . . . C(12) C(9) C(10) C(5) -178.0(3) no . . . . C(1) C(11) C(12) C(9) 2.7(4) no . . . . C(1) C(11) C(12) C(27) -172.9(3) no . . . . C(1) C(11) C(13) O(1) -166.0(3) no . . . . C(1) C(11) C(13) C(14) -56.7(5) no . . . . C(1) C(11) C(13) C(25) 72.3(4) no . . . . C(12) C(11) C(13) O(1) 12.4(5) no . . . . C(12) C(11) C(13) C(14) 121.8(4) no . . . . C(12) C(11) C(13) C(25) -109.3(4) no . . . . C(13) C(11) C(12) C(9) -176.0(3) no . . . . C(13) C(11) C(12) C(27) 8.4(5) no . . . . C(9) C(12) C(27) O(2) -162.0(3) no . . . . C(9) C(12) C(27) C(28) 76.4(5) no . . . . C(9) C(12) C(27) C(39) -53.6(5) no . . . . C(11) C(12) C(27) O(2) 12.7(5) no . . . . C(11) C(12) C(27) C(28) -108.9(4) no . . . . C(11) C(12) C(27) C(39) 121.2(4) no . . . . O(1) C(13) C(14) C(15) 87.8(4) no . . . . O(1) C(13) C(14) C(19) -85.8(4) no . . . . O(1) C(13) C(25) C(20) 78.9(4) no . . . . O(1) C(13) C(25) C(24) -96.8(4) no . . . . C(11) C(13) C(14) C(15) -25.0(5) no . . . . C(11) C(13) C(14) C(19) 161.4(3) no . . . . C(11) C(13) C(25) C(20) -161.6(3) no . . . . C(11) C(13) C(25) C(24) 22.8(5) no . . . . C(14) C(13) C(25) C(20) -31.7(5) no . . . . C(14) C(13) C(25) C(24) 152.6(3) no . . . . C(25) C(13) C(14) C(15) -155.5(3) no . . . . C(25) C(13) C(14) C(19) 30.9(5) no . . . . C(13) C(14) C(15) C(16) -174.1(3) no . . . . C(13) C(14) C(19) N(1) -5.0(6) no . . . . C(13) C(14) C(19) C(18) 174.7(3) no . . . . C(15) C(14) C(19) N(1) -178.8(4) no . . . . C(15) C(14) C(19) C(18) 0.9(6) no . . . . C(19) C(14) C(15) C(16) -0.5(6) no . . . . C(14) C(15) C(16) C(17) -0.2(6) no . . . . C(15) C(16) C(17) C(18) 0.7(7) no . . . . C(16) C(17) C(18) C(19) -0.4(7) no . . . . C(17) C(18) C(19) N(1) 179.3(4) no . . . . C(17) C(18) C(19) C(14) -0.4(6) no . . . . N(1) C(20) C(21) C(22) 178.3(3) no . . . . N(1) C(20) C(25) C(13) 6.6(5) no . . . . N(1) C(20) C(25) C(24) -177.6(3) no . . . . C(21) C(20) C(25) C(13) -174.5(3) no . . . . C(21) C(20) C(25) C(24) 1.3(6) no . . . . C(25) C(20) C(21) C(22) -0.6(6) no . . . . C(20) C(21) C(22) C(23) -0.8(6) no . . . . C(21) C(22) C(23) C(24) 1.5(6) no . . . . C(22) C(23) C(24) C(25) -0.8(6) no . . . . C(23) C(24) C(25) C(13) 175.1(4) no . . . . C(23) C(24) C(25) C(20) -0.6(6) no . . . . O(2) C(27) C(28) C(29) -99.8(4) no . . . . O(2) C(27) C(28) C(33) 77.7(4) no . . . . O(2) C(27) C(39) C(34) -86.2(4) no . . . . O(2) C(27) C(39) C(38) 88.2(4) no . . . . C(12) C(27) C(28) C(29) 19.1(5) no . . . . C(12) C(27) C(28) C(33) -163.3(3) no . . . . C(12) C(27) C(39) C(34) 161.8(3) no . . . . C(12) C(27) C(39) C(38) -23.8(5) no . . . . C(28) C(27) C(39) C(34) 30.3(5) no . . . . C(28) C(27) C(39) C(38) -155.3(3) no . . . . C(39) C(27) C(28) C(29) 150.4(4) no . . . . C(39) C(27) C(28) C(33) -32.0(5) no . . . . C(27) C(28) C(29) C(30) 177.1(4) no . . . . C(27) C(28) C(33) N(2) 6.8(6) no . . . . C(27) C(28) C(33) C(32) -175.7(4) no . . . . C(29) C(28) C(33) N(2) -175.6(4) no . . . . C(29) C(28) C(33) C(32) 1.9(6) no . . . . C(33) C(28) C(29) C(30) -0.5(6) no . . . . C(28) C(29) C(30) C(31) -1.2(6) no . . . . C(29) C(30) C(31) C(32) 1.3(7) no . . . . C(30) C(31) C(32) C(33) 0.2(7) no . . . . C(31) C(32) C(33) N(2) 175.6(4) no . . . . C(31) C(32) C(33) C(28) -1.8(7) no . . . . N(2) C(34) C(35) C(36) 177.6(4) no . . . . N(2) C(34) C(39) C(27) -3.3(6) no . . . . N(2) C(34) C(39) C(38) -177.9(3) no . . . . C(35) C(34) C(39) C(27) 175.3(4) no . . . . C(35) C(34) C(39) C(38) 0.8(6) no . . . . C(39) C(34) C(35) C(36) -1.1(6) no . . . . C(34) C(35) C(36) C(37) 1.0(7) no . . . . C(35) C(36) C(37) C(38) -0.6(7) no . . . . C(36) C(37) C(38) C(39) 0.3(6) no . . . . C(37) C(38) C(39) C(27) -174.8(4) no . . . . C(37) C(38) C(39) C(34) -0.4(6) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Cl(1) C(33) 3.563(5) no . . Cl(3) C(16) 3.566(7) no . 1_545 O(1) C(36) 3.499(6) no . 4_554 O(1) C(37) 3.210(5) no . 4_554 O(2) C(21) 3.512(6) no . 6_545 O(2) C(26) 3.384(5) no . 6_545 N(2) C(21) 3.479(6) no . 6_545 C(16) Cl(3) 3.566(7) no . 1_565 C(18) C(36) 3.546(6) no . 4_554 C(19) C(36) 3.468(6) no . 4_554 C(20) C(40) 3.598(7) no . 6_555 C(21) O(2) 3.512(6) no . 6_555 C(21) N(2) 3.479(6) no . 6_555 C(21) C(40) 3.530(6) no . 1_565 C(21) C(40) 3.510(7) no . 6_555 C(23) C(23) 3.543(6) no . 7_556 C(26) O(2) 3.384(5) no . 6_555 C(26) C(34) 3.408(6) no . 6_555 C(26) C(35) 3.525(6) no . 6_555 C(26) C(40) 3.432(6) no . 1_565 C(30) C(38) 3.540(6) no . 4_554 C(33) Cl(1) 3.563(5) no . . C(34) C(26) 3.408(6) no . 6_545 C(35) C(26) 3.525(6) no . 6_545 C(36) O(1) 3.499(6) no . 4_555 C(36) C(18) 3.546(6) no . 4_555 C(36) C(19) 3.468(6) no . 4_555 C(37) O(1) 3.210(5) no . 4_555 C(38) C(30) 3.540(6) no . 4_555 C(40) C(20) 3.598(7) no . 6_545 C(40) C(21) 3.530(6) no . 1_545 C(40) C(21) 3.510(7) no . 6_545 C(40) C(26) 3.432(6) no . 1_545 Cl(1) H(1) 2.9507 no . 1_545 Cl(1) H(2) 3.2647 no . 1_545 Cl(1) H(6) 3.0521 no . . Cl(1) H(8) 3.5792 no . 4_555 Cl(1) H(9) 3.2103 no . 4_555 Cl(2) H(2) 3.0131 no . 2_545 Cl(2) H(3) 3.5661 no . 4_554 Cl(2) H(5) 3.2690 no . 2_555 Cl(2) H(8) 3.1238 no . 3_555 Cl(3) H(1) 3.2975 no . 1_545 Cl(3) H(2) 3.2129 no . 2_545 Cl(3) H(3) 3.4126 no . 2_545 O(1) H(11) 3.1840 no . 6_545 O(1) H(20) 3.0560 no . 4_554 O(1) H(21) 2.4676 no . 4_554 O(1) H(26) 3.3024 no . 6_555 O(2) H(11) 2.5991 no . 6_545 O(2) H(21) 3.2686 no . 4_554 O(2) H(24) 3.2600 no . 6_545 O(2) H(25) 2.6641 no . 6_545 O(2) H(26) 3.4713 no . 6_555 N(1) H(20) 3.0472 no . 4_554 N(1) H(26) 3.1967 no . 6_555 N(1) H(27) 3.1189 no . 1_565 N(1) H(28) 3.3595 no . 1_565 N(2) H(11) 3.2636 no . 6_545 N(2) H(25) 2.9493 no . 6_545 C(1) H(17) 3.0881 no . 4_555 C(2) H(9) 3.0820 no . 4_565 C(2) H(17) 3.3410 no . 4_555 C(3) H(9) 3.1735 no . 4_565 C(3) H(17) 3.5615 no . 4_555 C(4) H(7) 3.3121 no . 2_555 C(4) H(17) 3.5936 no . 4_555 C(5) H(16) 2.9918 no . 4_555 C(5) H(17) 3.3755 no . 4_555 C(6) H(7) 3.2911 no . 2_555 C(6) H(15) 3.1170 no . 2_555 C(6) H(16) 2.8627 no . 4_555 C(7) H(15) 3.5005 no . 2_555 C(7) H(16) 2.8689 no . 4_555 C(8) H(16) 2.9870 no . 4_555 C(9) H(16) 3.0869 no . 4_555 C(10) H(16) 3.0639 no . 4_555 C(10) H(17) 3.0712 no . 4_555 C(14) H(20) 3.2723 no . 4_554 C(15) H(3) 3.0631 no . 2_555 C(15) H(4) 3.4254 no . 2_555 C(16) H(3) 3.0964 no . 2_555 C(18) H(18) 3.1346 no . 1_565 C(18) H(20) 3.1287 no . 4_554 C(19) H(20) 2.8222 no . 4_554 C(20) H(26) 2.8516 no . 6_555 C(20) H(27) 3.0407 no . 1_565 C(21) H(26) 3.5134 no . 1_565 C(21) H(26) 3.0763 no . 6_555 C(21) H(27) 2.8289 no . 1_565 C(21) H(28) 3.4661 no . 6_555 C(22) H(10) 3.5416 no . 4_565 C(22) H(13) 3.3902 no . 7_556 C(22) H(21) 3.4526 no . 7_556 C(22) H(23) 3.3565 no . 4_565 C(22) H(28) 3.4971 no . 6_555 C(23) H(10) 3.0370 no . 4_565 C(23) H(13) 2.9951 no . 7_556 C(23) H(18) 3.5541 no . 4_555 C(23) H(23) 3.4565 no . 4_565 C(23) H(24) 3.5403 no . 4_565 C(24) H(17) 3.4506 no . 4_555 C(25) H(26) 3.2832 no . 6_555 C(26) H(12) 3.5975 no . 4_564 C(26) H(13) 3.3948 no . 4_564 C(26) H(20) 3.3138 no . 4_554 C(26) H(26) 3.5030 no . 6_555 C(26) H(27) 3.2353 no . 1_565 C(26) H(28) 2.9011 no . 1_565 C(27) H(25) 3.4092 no . 6_545 C(28) H(21) 3.1897 no . 4_554 C(29) H(4) 3.2332 no . 2_555 C(29) H(5) 3.4501 no . 2_555 C(29) H(21) 3.0366 no . 4_554 C(29) H(22) 3.5190 no . 4_554 C(30) H(5) 3.4400 no . 2_555 C(30) H(21) 3.3430 no . 4_554 C(30) H(22) 2.8329 no . 4_554 C(31) H(14) 3.1638 no . 4_554 C(31) H(22) 2.9064 no . 4_554 C(32) H(10) 3.5952 no . 1_545 C(32) H(13) 3.4901 no . 4_554 C(32) H(14) 3.5309 no . 4_554 C(33) H(11) 3.5637 no . 6_545 C(34) H(23) 3.5048 no . 6_545 C(34) H(25) 2.5589 no . 6_545 C(35) H(20) 3.4762 no . 7_546 C(35) H(23) 3.2755 no . 6_545 C(35) H(25) 2.9452 no . 6_545 C(36) H(12) 3.4962 no . 7_556 C(36) H(23) 3.5576 no . 4_555 C(36) H(23) 3.3246 no . 6_545 C(36) H(25) 3.4722 no . 6_545 C(37) H(12) 2.8893 no . 7_556 C(38) H(12) 3.4012 no . 7_556 C(38) H(16) 3.5835 no . 4_555 C(38) H(25) 3.3809 no . 6_545 C(39) H(25) 2.8323 no . 6_545 C(40) H(11) 3.1221 no . 1_545 C(40) H(24) 2.6275 no . 1_545 C(40) H(25) 3.4730 no . 6_545 C(41) H(5) 3.4601 no . 2_555 C(41) H(6) 3.1863 no . . H(1) Cl(1) 2.9507 no . 1_565 H(1) Cl(3) 3.2975 no . 1_565 H(1) H(9) 2.8051 no . 4_565 H(2) Cl(1) 3.2647 no . 1_565 H(2) Cl(2) 3.0131 no . 2_565 H(2) Cl(3) 3.2129 no . 2_565 H(2) H(8) 3.3174 no . 4_565 H(2) H(9) 2.9340 no . 4_565 H(3) Cl(2) 3.5661 no . 4_555 H(3) Cl(3) 3.4126 no . 2_565 H(3) C(15) 3.0631 no . 2_555 H(3) C(16) 3.0964 no . 2_555 H(3) H(7) 2.6021 no . 2_555 H(3) H(8) 2.6917 no . 2_555 H(4) C(15) 3.4254 no . 2_555 H(4) C(29) 3.2332 no . 2_555 H(4) H(5) 3.2477 no . 3_556 H(4) H(7) 2.5766 no . 2_555 H(4) H(8) 3.5208 no . 2_555 H(4) H(15) 2.4360 no . 2_555 H(4) H(16) 3.2290 no . 2_555 H(4) H(16) 3.3389 no . 4_555 H(5) Cl(2) 3.2690 no . 2_555 H(5) C(29) 3.4501 no . 2_555 H(5) C(30) 3.4400 no . 2_555 H(5) C(41) 3.4601 no . 2_555 H(5) H(4) 3.2477 no . 3_556 H(5) H(15) 3.1527 no . 2_555 H(5) H(16) 3.1195 no . 2_555 H(5) H(16) 3.3876 no . 4_555 H(6) Cl(1) 3.0521 no . . H(6) C(41) 3.1863 no . . H(6) H(16) 3.5313 no . 4_555 H(7) C(4) 3.3121 no . 2_555 H(7) C(6) 3.2911 no . 2_555 H(7) H(3) 2.6021 no . 2_555 H(7) H(4) 2.5766 no . 2_555 H(8) Cl(1) 3.5792 no . 4_554 H(8) Cl(2) 3.1238 no . 3_555 H(8) H(2) 3.3174 no . 4_564 H(8) H(3) 2.6917 no . 2_555 H(8) H(4) 3.5208 no . 2_555 H(9) Cl(1) 3.2103 no . 4_554 H(9) C(2) 3.0820 no . 4_564 H(9) C(3) 3.1735 no . 4_564 H(9) H(1) 2.8051 no . 4_564 H(9) H(2) 2.9340 no . 4_564 H(9) H(17) 3.4979 no . 1_565 H(10) C(22) 3.5416 no . 4_564 H(10) C(23) 3.0370 no . 4_564 H(10) C(32) 3.5952 no . 1_565 H(10) H(13) 2.8029 no . 4_564 H(10) H(18) 2.7191 no . 1_565 H(10) H(19) 3.4690 no . 4_554 H(10) H(20) 3.3934 no . 4_554 H(10) H(28) 3.3937 no . 1_565 H(11) O(1) 3.1840 no . 6_555 H(11) O(2) 2.5991 no . 6_555 H(11) N(2) 3.2636 no . 6_555 H(11) C(33) 3.5637 no . 6_555 H(11) C(40) 3.1221 no . 1_565 H(11) H(21) 3.3657 no . 7_556 H(11) H(26) 2.9274 no . 1_565 H(11) H(26) 3.3502 no . 6_555 H(11) H(27) 2.6421 no . 1_565 H(11) H(28) 3.3190 no . 1_565 H(12) C(26) 3.5975 no . 4_565 H(12) C(36) 3.4962 no . 7_556 H(12) C(37) 2.8893 no . 7_556 H(12) C(38) 3.4012 no . 7_556 H(12) H(13) 3.3510 no . 7_556 H(12) H(21) 2.6271 no . 7_556 H(12) H(22) 3.5235 no . 7_556 H(12) H(23) 2.9216 no . 4_565 H(12) H(24) 3.5487 no . 4_565 H(13) C(22) 3.3902 no . 7_556 H(13) C(23) 2.9951 no . 7_556 H(13) C(26) 3.3948 no . 4_565 H(13) C(32) 3.4901 no . 4_555 H(13) H(10) 2.8029 no . 4_565 H(13) H(12) 3.3510 no . 7_556 H(13) H(13) 2.6816 no . 7_556 H(13) H(18) 2.8674 no . 4_555 H(13) H(23) 3.0980 no . 4_565 H(13) H(24) 2.8126 no . 4_565 H(13) H(28) 3.0776 no . 4_555 H(14) C(31) 3.1638 no . 4_555 H(14) C(32) 3.5309 no . 4_555 H(14) H(17) 2.6851 no . 4_555 H(14) H(18) 3.3720 no . 4_555 H(15) C(6) 3.1170 no . 2_555 H(15) C(7) 3.5005 no . 2_555 H(15) H(4) 2.4360 no . 2_555 H(15) H(5) 3.1527 no . 2_555 H(15) H(21) 3.2806 no . 4_554 H(16) C(5) 2.9918 no . 4_554 H(16) C(6) 2.8627 no . 4_554 H(16) C(7) 2.8689 no . 4_554 H(16) C(8) 2.9870 no . 4_554 H(16) C(9) 3.0869 no . 4_554 H(16) C(10) 3.0639 no . 4_554 H(16) C(38) 3.5835 no . 4_554 H(16) H(4) 3.2290 no . 2_555 H(16) H(4) 3.3389 no . 4_554 H(16) H(5) 3.1195 no . 2_555 H(16) H(5) 3.3876 no . 4_554 H(16) H(6) 3.5313 no . 4_554 H(16) H(22) 2.8881 no . 4_554 H(17) C(1) 3.0881 no . 4_554 H(17) C(2) 3.3410 no . 4_554 H(17) C(3) 3.5614 no . 4_554 H(17) C(4) 3.5936 no . 4_554 H(17) C(5) 3.3755 no . 4_554 H(17) C(10) 3.0712 no . 4_554 H(17) C(24) 3.4506 no . 4_554 H(17) H(9) 3.4979 no . 1_545 H(17) H(14) 2.6851 no . 4_554 H(17) H(22) 2.9667 no . 4_554 H(18) C(18) 3.1346 no . 1_545 H(18) C(23) 3.5541 no . 4_554 H(18) H(10) 2.7191 no . 1_545 H(18) H(13) 2.8674 no . 4_554 H(18) H(14) 3.3720 no . 4_554 H(18) H(24) 3.0021 no . 1_545 H(19) H(10) 3.4690 no . 4_555 H(19) H(20) 3.0942 no . 7_546 H(19) H(23) 3.3050 no . 4_555 H(19) H(25) 3.3822 no . 6_545 H(20) O(1) 3.0560 no . 4_555 H(20) N(1) 3.0472 no . 4_555 H(20) C(14) 3.2723 no . 4_555 H(20) C(18) 3.1287 no . 4_555 H(20) C(19) 2.8222 no . 4_555 H(20) C(26) 3.3138 no . 4_555 H(20) C(35) 3.4762 no . 7_546 H(20) H(10) 3.3934 no . 4_555 H(20) H(19) 3.0942 no . 7_546 H(20) H(20) 3.4763 no . 7_546 H(20) H(23) 2.7832 no . 4_555 H(20) H(26) 3.5850 no . 7_546 H(21) O(1) 2.4676 no . 4_555 H(21) O(2) 3.2686 no . 4_555 H(21) C(22) 3.4526 no . 7_556 H(21) C(28) 3.1897 no . 4_555 H(21) C(29) 3.0366 no . 4_555 H(21) C(30) 3.3430 no . 4_555 H(21) H(11) 3.3657 no . 7_556 H(21) H(12) 2.6271 no . 7_556 H(21) H(15) 3.2806 no . 4_555 H(22) C(29) 3.5190 no . 4_555 H(22) C(30) 2.8329 no . 4_555 H(22) C(31) 2.9064 no . 4_555 H(22) H(12) 3.5235 no . 7_556 H(22) H(16) 2.8881 no . 4_555 H(22) H(17) 2.9667 no . 4_555 H(23) C(22) 3.3565 no . 4_564 H(23) C(23) 3.4565 no . 4_564 H(23) C(34) 3.5048 no . 6_555 H(23) C(35) 3.2755 no . 6_555 H(23) C(36) 3.5576 no . 4_554 H(23) C(36) 3.3246 no . 6_555 H(23) H(12) 2.9216 no . 4_564 H(23) H(13) 3.0980 no . 4_564 H(23) H(19) 3.3050 no . 4_554 H(23) H(20) 2.7832 no . 4_554 H(23) H(28) 3.4753 no . 1_565 H(24) O(2) 3.2600 no . 6_555 H(24) C(23) 3.5403 no . 4_564 H(24) C(40) 2.6275 no . 1_565 H(24) H(12) 3.5487 no . 4_564 H(24) H(13) 2.8126 no . 4_564 H(24) H(18) 3.0021 no . 1_565 H(24) H(26) 2.8833 no . 1_565 H(24) H(27) 2.6254 no . 1_565 H(24) H(28) 2.0015 no . 1_565 H(25) O(2) 2.6641 no . 6_555 H(25) N(2) 2.9493 no . 6_555 H(25) C(27) 3.4092 no . 6_555 H(25) C(34) 2.5589 no . 6_555 H(25) C(35) 2.9452 no . 6_555 H(25) C(36) 3.4722 no . 6_555 H(25) C(38) 3.3809 no . 6_555 H(25) C(39) 2.8323 no . 6_555 H(25) C(40) 3.4730 no . 6_555 H(25) H(19) 3.3822 no . 6_555 H(25) H(26) 2.9819 no . 6_555 H(25) H(27) 3.5738 no . 1_565 H(25) H(28) 3.3818 no . 1_565 H(26) O(1) 3.3024 no . 6_545 H(26) O(2) 3.4713 no . 6_545 H(26) N(1) 3.1967 no . 6_545 H(26) C(20) 2.8516 no . 6_545 H(26) C(21) 3.5134 no . 1_545 H(26) C(21) 3.0763 no . 6_545 H(26) C(25) 3.2832 no . 6_545 H(26) C(26) 3.5030 no . 6_545 H(26) H(11) 2.9274 no . 1_545 H(26) H(11) 3.3502 no . 6_545 H(26) H(20) 3.5850 no . 7_546 H(26) H(24) 2.8833 no . 1_545 H(26) H(25) 2.9819 no . 6_545 H(27) N(1) 3.1189 no . 1_545 H(27) C(20) 3.0407 no . 1_545 H(27) C(21) 2.8289 no . 1_545 H(27) C(26) 3.2353 no . 1_545 H(27) H(11) 2.6421 no . 1_545 H(27) H(24) 2.6254 no . 1_545 H(27) H(25) 3.5738 no . 1_545 H(28) N(1) 3.3595 no . 1_545 H(28) C(21) 3.4661 no . 6_545 H(28) C(22) 3.4971 no . 6_545 H(28) C(26) 2.9011 no . 1_545 H(28) H(10) 3.3937 no . 1_545 H(28) H(11) 3.3190 no . 1_545 H(28) H(13) 3.0776 no . 4_554 H(28) H(23) 3.4753 no . 1_545 H(28) H(24) 2.0015 no . 1_545 H(28) H(25) 3.3818 no . 1_545 #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 975889' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data__060121km #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C247 H195 Cl3 N12' _chemical_formula_moiety 'C247 H195 Cl3 N12' _chemical_formula_weight 3437.70 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3:H' _symmetry_space_group_name_Hall '-R 3' _symmetry_Int_Tables_number 148 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -Y,+X-Y,+Z 3 -X+Y,-X,+Z 4 -X,-Y,-Z 5 +Y,-X+Y,-Z 6 +X-Y,+X,-Z 7 2/3+X,1/3+Y,1/3+Z 8 2/3-Y,1/3+X-Y,1/3+Z 9 2/3-X+Y,1/3-X,1/3+Z 10 2/3-X,1/3-Y,1/3-Z 11 2/3+Y,1/3-X+Y,1/3-Z 12 2/3+X-Y,1/3+X,1/3-Z 13 1/3+X,2/3+Y,2/3+Z 14 1/3-Y,2/3+X-Y,2/3+Z 15 1/3-X+Y,2/3-X,2/3+Z 16 1/3-X,2/3-Y,2/3-Z 17 1/3+Y,2/3-X+Y,2/3-Z 18 1/3+X-Y,2/3+X,2/3-Z #------------------------------------------------------------------------------ _cell_length_a 36.2356 _cell_length_b 36.2356 _cell_length_c 11.6336 _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 120.0000 _cell_volume 13228.6540 _cell_formula_units_Z 3 _cell_measurement_reflns_used 4006 _cell_measurement_theta_min 3.13 _cell_measurement_theta_max 27.48 _cell_measurement_temperature 95 #------------------------------------------------------------------------------ _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.294 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5436.00 _exptl_absorpt_coefficient_mu 0.119 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.882 _exptl_absorpt_correction_T_max 0.988 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 95 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type 'Rigaku Mercury70' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_reflns_number 37068 _diffrn_reflns_av_R_equivalents 0.0567 _diffrn_reflns_theta_max 27.47 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -47 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6700 _reflns_number_gt 3521 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.0985 _refine_ls_number_restraints ? _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 6700 _refine_ls_number_parameters 423 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[1.0000\s(Fo^2^)]/(4Fo^2^)' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 0.810 _refine_diff_density_min -0.462 _refine_ls_extinction_method 'Larson (1970) Crystallographic Computing eq. 22' _refine_ls_extinction_coef 267(23) 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.1484 0.1585 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Cl(1) Cl 0.0598(5) 0.0283(7) 0.5991(11) 0.929(15) Uiso 0.5000 18 d . . . N(1) N 0.28351(6) 0.28429(6) 1.16970(16) 0.0269(6) Uani 1.0 18 d . . . N(2) N 0.20388(6) 0.20207(6) 0.49357(16) 0.0278(6) Uani 1.0 18 d . . . C(1) C 0.14295(7) 0.18120(7) 0.9791(2) 0.0245(7) Uani 1.0 18 d . . . C(2) C 0.12457(7) 0.17401(7) 1.0866(2) 0.0295(8) Uani 1.0 18 d . . . C(3) C 0.07986(8) 0.14657(8) 1.0964(3) 0.0335(8) Uani 1.0 18 d . . . C(4) C 0.05450(8) 0.12737(8) 1.0022(3) 0.0360(8) Uani 1.0 18 d . . . C(5) C 0.07258(8) 0.13451(8) 0.8895(3) 0.0313(8) Uani 1.0 18 d . . . C(6) C 0.05126(9) 0.11879(9) 0.7830(3) 0.0414(9) Uani 1.0 18 d . . . C(7) C 0.07418(9) 0.12952(9) 0.6829(3) 0.0454(10) Uani 1.0 18 d . . . C(8) C 0.11908(8) 0.15611(8) 0.6803(3) 0.0354(9) Uani 1.0 18 d . . . C(9) C 0.14031(8) 0.17189(7) 0.7819(2) 0.0264(7) Uani 1.0 18 d . . . C(10) C 0.11633(7) 0.16081(7) 0.8838(2) 0.0259(7) Uani 1.0 18 d . . . C(11) C 0.18644(7) 0.20730(7) 0.93211(19) 0.0241(7) Uani 1.0 18 d . . . C(12) C 0.18525(7) 0.20113(7) 0.81617(19) 0.0240(7) Uani 1.0 18 d . . . C(13) C 0.22462(7) 0.23661(7) 1.00291(19) 0.0246(7) Uani 1.0 18 d . . . C(14) C 0.22028(7) 0.27081(7) 1.06746(19) 0.0234(7) Uani 1.0 18 d . . . C(15) C 0.18813(7) 0.28030(8) 1.0467(2) 0.0273(7) Uani 1.0 18 d . . . C(16) C 0.18688(7) 0.31314(8) 1.1044(2) 0.0290(8) Uani 1.0 18 d . . . C(17) C 0.21855(8) 0.33724(8) 1.1820(2) 0.0310(8) Uani 1.0 18 d . . . C(18) C 0.25115(7) 0.32888(8) 1.2029(2) 0.0282(7) Uani 1.0 18 d . . . C(19) C 0.25179(7) 0.29510(8) 1.14758(19) 0.0244(7) Uani 1.0 18 d . . . C(20) C 0.27094(7) 0.24069(8) 1.16592(19) 0.0249(7) Uani 1.0 18 d . . . C(21) C 0.28844(8) 0.22293(7) 1.23770(19) 0.0266(7) Uani 1.0 18 d . . . C(22) C 0.27458(8) 0.17952(8) 1.2313(2) 0.0301(8) Uani 1.0 18 d . . . C(23) C 0.24290(8) 0.15372(7) 1.1561(2) 0.0280(7) Uani 1.0 18 d . . . C(24) C 0.22547(7) 0.17148(7) 1.08296(19) 0.0247(7) Uani 1.0 18 d . . . C(25) C 0.23947(7) 0.21472(7) 1.08678(19) 0.0226(7) Uani 1.0 18 d . . . C(26) C 0.22284(7) 0.21897(7) 0.73506(19) 0.0254(7) Uani 1.0 18 d . . . C(27) C 0.22408(7) 0.25183(7) 0.6520(2) 0.0249(7) Uani 1.0 18 d . . . C(28) C 0.23351(8) 0.29134(8) 0.6923(2) 0.0331(8) Uani 1.0 18 d . . . C(29) C 0.23616(8) 0.32298(8) 0.6191(3) 0.0344(8) Uani 1.0 18 d . . . C(30) C 0.23024(8) 0.31480(8) 0.5039(2) 0.0328(8) Uani 1.0 18 d . . . C(31) C 0.22065(8) 0.27535(8) 0.4611(2) 0.0309(8) Uani 1.0 18 d . . . C(32) C 0.21650(8) 0.24310(7) 0.5343(2) 0.0254(7) Uani 1.0 18 d . . . C(33) C 0.21476(8) 0.17586(8) 0.5550(2) 0.0256(7) Uani 1.0 18 d . . . C(34) C 0.21514(8) 0.14164(7) 0.5010(2) 0.0288(8) Uani 1.0 18 d . . . C(35) C 0.22701(8) 0.11650(8) 0.5612(2) 0.0318(8) Uani 1.0 18 d . . . C(36) C 0.23861(8) 0.12446(8) 0.6764(2) 0.0308(8) Uani 1.0 18 d . . . C(37) C 0.23746(8) 0.15793(8) 0.7305(2) 0.0291(8) Uani 1.0 18 d . . . C(38) C 0.22526(7) 0.18361(8) 0.6714(2) 0.0258(7) Uani 1.0 18 d . . . C(39) C 0.31900(8) 0.31279(8) 1.2440(2) 0.0350(8) Uani 1.0 18 d . . . C(40) C 0.18603(8) 0.18915(8) 0.37863(18) 0.0317(8) Uani 1.0 18 d . . . C(41) C 0.0000 0.0000 0.9437(8) 0.162(5) Uiso 1.0 6 d . . . C(42) C 0.0000 0.0000 0.7036(18) 0.304(8) Uiso 1.0 6 d . . . C(43) C 0.0000 0.0000 0.5000 0.292(11) Uiso 1.0 3 d . . . C(44) C -0.0122(10) 0.0092(11) 0.8469(15) 0.184(10) Uiso 0.3330 18 d . . . H(1) H 0.1416 0.1872 1.1526 0.0342(13) Uiso 1.0 18 calc R . . H(2) H 0.0671 0.1413 1.1704 0.0386(14) Uiso 1.0 18 calc R . . H(3) H 0.0246 0.1093 1.0115 0.0443(14) Uiso 1.0 18 calc R . . H(4) H 0.0212 0.1007 0.7814 0.0561(15) Uiso 1.0 18 calc R . . H(5) H 0.0594 0.1188 0.6124 0.0604(16) Uiso 1.0 18 calc R . . H(6) H 0.1342 0.1630 0.6096 0.0455(14) Uiso 1.0 18 calc R . . H(7) H 0.1667 0.2639 0.9919 0.0329(13) Uiso 1.0 18 calc R . . H(8) H 0.1644 0.3189 1.0907 0.0341(13) Uiso 1.0 18 calc R . . H(9) H 0.2180 0.3598 1.2218 0.0339(13) Uiso 1.0 18 calc R . . H(10) H 0.2734 0.3463 1.2548 0.0322(13) Uiso 1.0 18 calc R . . H(11) H 0.3100 0.2404 1.2911 0.0327(13) Uiso 1.0 18 calc R . . H(12) H 0.2871 0.1677 1.2798 0.0358(13) Uiso 1.0 18 calc R . . H(13) H 0.2331 0.1240 1.1540 0.0317(13) Uiso 1.0 18 calc R . . H(14) H 0.2038 0.1539 1.0300 0.0305(13) Uiso 1.0 18 calc R . . H(15) H 0.2384 0.2972 0.7722 0.0388(14) Uiso 1.0 18 calc R . . H(16) H 0.2421 0.3498 0.6487 0.0394(14) Uiso 1.0 18 calc R . . H(17) H 0.2324 0.3362 0.4528 0.0378(14) Uiso 1.0 18 calc R . . H(18) H 0.2172 0.2701 0.3807 0.0372(14) Uiso 1.0 18 calc R . . H(19) H 0.2071 0.1358 0.4224 0.0345(13) Uiso 1.0 18 calc R . . H(20) H 0.2272 0.0933 0.5236 0.0373(14) Uiso 1.0 18 calc R . . H(21) H 0.2471 0.1073 0.7175 0.0358(13) Uiso 1.0 18 calc R . . H(22) H 0.2453 0.1637 0.8091 0.0355(13) Uiso 1.0 18 calc R . . H(23) H 0.2474 0.2513 0.9501 0.0302 Uiso 1.0 18 calc R . . H(24) H 0.2478 0.2331 0.7811 0.0309 Uiso 1.0 18 calc R . . H(25) H 0.3294 0.3415 1.2212 0.0438 Uiso 1.0 18 calc R . . H(26) H 0.3412 0.3061 1.2377 0.0439 Uiso 1.0 18 calc R . . H(27) H 0.3095 0.3092 1.3215 0.0439 Uiso 1.0 18 calc R . . H(28) H 0.2083 0.1958 0.3252 0.0371 Uiso 1.0 18 calc R . . H(29) H 0.1666 0.1593 0.3777 0.0371 Uiso 1.0 18 calc R . . H(30) H 0.1715 0.2039 0.3581 0.0373 Uiso 1.0 18 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 N(1) 0.0245(12) 0.0309(13) 0.0257(12) 0.0142(11) 0.0045(10) -0.0024(10) N(2) 0.0303(13) 0.0286(12) 0.0210(11) 0.0122(11) 0.0017(10) -0.0026(10) C(1) 0.0242(14) 0.0216(14) 0.0233(14) 0.0081(12) -0.0011(11) -0.0012(11) C(2) 0.0273(15) 0.0289(15) 0.0295(15) 0.0119(13) 0.0016(12) 0.0001(12) C(3) 0.0367(16) 0.0290(15) 0.0318(16) 0.0141(13) -0.0056(13) 0.0021(12) C(4) 0.0316(16) 0.0276(15) 0.0518(18) 0.0170(13) -0.0012(14) 0.0022(14) C(5) 0.0319(16) 0.0247(15) 0.0364(16) 0.0133(13) 0.0001(13) 0.0006(12) C(6) 0.0492(19) 0.0489(19) 0.0420(17) 0.0365(16) 0.0039(15) -0.0007(15) C(7) 0.059(2) 0.055(2) 0.0377(17) 0.0399(18) 0.0070(15) -0.0017(15) C(8) 0.0432(18) 0.0409(17) 0.0296(16) 0.0267(15) 0.0037(13) -0.0003(13) C(9) 0.0289(15) 0.0251(14) 0.0253(14) 0.0135(12) 0.0022(12) -0.0014(11) C(10) 0.0276(14) 0.0225(14) 0.0282(14) 0.0130(12) 0.0008(12) -0.0011(11) C(11) 0.0246(14) 0.0249(14) 0.0207(13) 0.0108(12) 0.0004(11) -0.0027(11) C(12) 0.0234(14) 0.0228(13) 0.0222(13) 0.0089(11) -0.0002(11) -0.0021(11) C(13) 0.0284(14) 0.0275(14) 0.0198(13) 0.0153(12) 0.0010(11) 0.0009(11) C(14) 0.0233(14) 0.0251(14) 0.0190(13) 0.0098(12) -0.0019(11) -0.0003(11) C(15) 0.0253(14) 0.0336(15) 0.0233(14) 0.0149(12) -0.0016(11) -0.0020(12) C(16) 0.0279(15) 0.0265(15) 0.0309(15) 0.0124(13) -0.0041(12) 0.0016(12) C(17) 0.0268(15) 0.0324(16) 0.0250(14) 0.0081(13) -0.0017(12) 0.0048(12) C(18) 0.0244(14) 0.0337(15) 0.0228(14) 0.0119(12) 0.0004(11) -0.0006(12) C(19) 0.0238(14) 0.0285(14) 0.0196(13) 0.0121(12) -0.0012(11) 0.0005(11) C(20) 0.0263(14) 0.0284(14) 0.0205(13) 0.0141(12) 0.0014(11) 0.0024(11) C(21) 0.0288(15) 0.0280(14) 0.0256(14) 0.0161(12) 0.0032(12) -0.0025(12) C(22) 0.0331(16) 0.0274(15) 0.0287(14) 0.0144(13) -0.0009(12) -0.0053(12) C(23) 0.0256(14) 0.0244(14) 0.0291(15) 0.0088(12) 0.0036(12) 0.0004(12) C(24) 0.0241(14) 0.0286(14) 0.0241(14) 0.0152(12) 0.0036(11) 0.0015(11) C(25) 0.0250(14) 0.0249(14) 0.0192(13) 0.0135(12) 0.0010(11) 0.0024(11) C(26) 0.0275(14) 0.0280(14) 0.0219(13) 0.0147(12) -0.0009(11) -0.0044(11) C(27) 0.0245(14) 0.0253(14) 0.0248(14) 0.0124(12) 0.0002(11) -0.0023(11) C(28) 0.0314(16) 0.0381(16) 0.0273(15) 0.0155(14) 0.0041(12) -0.0021(13) C(29) 0.0267(15) 0.0329(16) 0.0389(16) 0.0113(13) 0.0054(13) -0.0030(13) C(30) 0.0312(16) 0.0323(16) 0.0309(15) 0.0128(13) -0.0057(13) -0.0047(13) C(31) 0.0358(16) 0.0335(16) 0.0238(14) 0.0175(13) -0.0011(12) -0.0003(12) C(32) 0.0253(14) 0.0264(14) 0.0252(14) 0.0134(12) -0.0012(11) -0.0021(11) C(33) 0.0270(14) 0.0273(14) 0.0234(14) 0.0141(12) -0.0014(11) -0.0024(12) C(34) 0.0350(15) 0.0304(15) 0.0212(13) 0.0164(13) 0.0016(12) 0.0003(12) C(35) 0.0277(15) 0.0317(16) 0.0335(16) 0.0129(13) 0.0025(13) 0.0050(13) C(36) 0.0292(15) 0.0270(15) 0.0327(15) 0.0116(13) -0.0053(12) -0.0055(12) C(37) 0.0307(15) 0.0351(16) 0.0236(14) 0.0180(13) -0.0006(12) -0.0028(12) C(38) 0.0250(14) 0.0272(14) 0.0236(14) 0.0118(12) 0.0019(11) 0.0003(11) C(39) 0.0333(16) 0.0413(17) 0.0350(16) 0.0220(14) 0.0073(13) -0.0012(13) C(40) 0.0400(17) 0.0293(15) 0.0233(14) 0.0153(13) 0.0024(12) -0.0010(12) #============================================================================== _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'CRYSTALS (Carruthers, et al., 1999)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cl(1) C(42) 2.237(18) yes . . Cl(1) C(43) 2.203(15) yes . . N(1) C(19) 1.411(4) yes . . N(1) C(20) 1.409(4) yes . . N(1) C(39) 1.463(3) yes . . N(2) C(32) 1.402(4) yes . . N(2) C(33) 1.394(4) yes . . N(2) C(40) 1.457(3) yes . . C(1) C(2) 1.379(4) yes . . C(1) C(10) 1.412(3) yes . . C(1) C(11) 1.479(3) yes . . C(2) C(3) 1.420(3) yes . . C(3) C(4) 1.375(4) yes . . C(4) C(5) 1.430(4) yes . . C(5) C(6) 1.420(4) yes . . C(5) C(10) 1.384(4) yes . . C(6) C(7) 1.369(4) yes . . C(7) C(8) 1.417(4) yes . . C(8) C(9) 1.370(4) yes . . C(9) C(10) 1.404(4) yes . . C(9) C(12) 1.486(3) yes . . C(11) C(12) 1.364(4) yes . . C(11) C(13) 1.500(3) yes . . C(12) C(26) 1.511(4) yes . . C(13) C(14) 1.523(4) yes . . C(13) C(25) 1.516(4) yes . . C(14) C(15) 1.391(5) yes . . C(14) C(19) 1.394(3) yes . . C(15) C(16) 1.387(5) yes . . C(16) C(17) 1.376(3) yes . . C(17) C(18) 1.380(5) yes . . C(18) C(19) 1.393(5) yes . . C(20) C(21) 1.386(5) yes . . C(20) C(25) 1.400(3) yes . . C(21) C(22) 1.394(4) yes . . C(22) C(23) 1.373(3) yes . . C(23) C(24) 1.394(4) yes . . C(24) C(25) 1.385(4) yes . . C(26) C(27) 1.516(4) yes . . C(26) C(38) 1.520(4) yes . . C(27) C(28) 1.377(4) yes . . C(27) C(32) 1.401(4) yes . . C(28) C(29) 1.393(5) yes . . C(29) C(30) 1.366(4) yes . . C(30) C(31) 1.384(4) yes . . C(31) C(32) 1.392(4) yes . . C(33) C(34) 1.396(5) yes . . C(33) C(38) 1.397(4) yes . . C(34) C(35) 1.378(5) yes . . C(35) C(36) 1.391(4) yes . . C(36) C(37) 1.385(5) yes . . C(37) C(38) 1.394(5) yes . . C(41) C(41) 1.310(13) yes . 4_557 C(41) C(44) 1.31(3) yes . . C(41) C(44) 1.31(3) yes . 2_555 C(41) C(44) 1.31(3) yes . 3_555 C(42) C(44) 1.80(3) yes . . C(42) C(44) 1.80(3) yes . 2_555 C(42) C(44) 1.80(3) yes . 3_555 C(44) C(44) 1.17(6) yes . 2_555 C(44) C(44) 1.17(6) yes . 3_555 C(2) H(1) 0.950 no . . C(3) H(2) 0.950 no . . C(4) H(3) 0.950 no . . C(6) H(4) 0.950 no . . C(7) H(5) 0.950 no . . C(8) H(6) 0.950 no . . C(13) H(23) 0.950 no . . C(15) H(7) 0.950 no . . C(16) H(8) 0.950 no . . C(17) H(9) 0.950 no . . C(18) H(10) 0.950 no . . C(21) H(11) 0.950 no . . C(22) H(12) 0.950 no . . C(23) H(13) 0.950 no . . C(24) H(14) 0.950 no . . C(26) H(24) 0.950 no . . C(28) H(15) 0.950 no . . C(29) H(16) 0.950 no . . C(30) H(17) 0.950 no . . C(31) H(18) 0.950 no . . C(34) H(19) 0.950 no . . C(35) H(20) 0.950 no . . C(36) H(21) 0.950 no . . C(37) H(22) 0.950 no . . C(39) H(25) 0.950 no . . C(39) H(26) 0.950 no . . C(39) H(27) 0.950 no . . C(40) H(28) 0.950 no . . C(40) H(29) 0.950 no . . C(40) H(30) 0.950 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C(42) Cl(1) C(43) 64.5(6) yes . . . C(19) N(1) C(20) 117.00(18) yes . . . C(19) N(1) C(39) 117.5(3) yes . . . C(20) N(1) C(39) 119.2(3) yes . . . C(32) N(2) C(33) 119.7(2) yes . . . C(32) N(2) C(40) 120.6(3) yes . . . C(33) N(2) C(40) 118.9(3) yes . . . C(2) C(1) C(10) 118.32(19) yes . . . C(2) C(1) C(11) 135.7(2) yes . . . C(10) C(1) C(11) 105.9(2) yes . . . C(1) C(2) C(3) 118.7(2) yes . . . C(2) C(3) C(4) 122.0(3) yes . . . C(3) C(4) C(5) 120.6(3) yes . . . C(4) C(5) C(6) 128.2(3) yes . . . C(4) C(5) C(10) 115.6(3) yes . . . C(6) C(5) C(10) 116.2(3) yes . . . C(5) C(6) C(7) 119.8(3) yes . . . C(6) C(7) C(8) 122.6(3) yes . . . C(7) C(8) C(9) 118.6(3) yes . . . C(8) C(9) C(10) 118.1(3) yes . . . C(8) C(9) C(12) 135.7(3) yes . . . C(10) C(9) C(12) 106.18(19) yes . . . C(1) C(10) C(5) 124.8(3) yes . . . C(1) C(10) C(9) 110.49(19) yes . . . C(5) C(10) C(9) 124.7(3) yes . . . C(1) C(11) C(12) 108.95(18) yes . . . C(1) C(11) C(13) 124.1(2) yes . . . C(12) C(11) C(13) 126.95(19) yes . . . C(9) C(12) C(11) 108.38(19) yes . . . C(9) C(12) C(26) 124.7(2) yes . . . C(11) C(12) C(26) 126.83(19) yes . . . C(11) C(13) C(14) 114.4(3) yes . . . C(11) C(13) C(25) 115.2(2) yes . . . C(14) C(13) C(25) 108.45(19) yes . . . C(13) C(14) C(15) 123.7(2) yes . . . C(13) C(14) C(19) 117.3(3) yes . . . C(15) C(14) C(19) 118.9(3) yes . . . C(14) C(15) C(16) 121.2(2) yes . . . C(15) C(16) C(17) 119.2(3) yes . . . C(16) C(17) C(18) 120.7(3) yes . . . C(17) C(18) C(19) 120.3(2) yes . . . N(1) C(19) C(14) 118.1(3) yes . . . N(1) C(19) C(18) 122.2(2) yes . . . C(14) C(19) C(18) 119.7(3) yes . . . N(1) C(20) C(21) 122.36(19) yes . . . N(1) C(20) C(25) 118.2(3) yes . . . C(21) C(20) C(25) 119.5(3) yes . . . C(20) C(21) C(22) 120.1(2) yes . . . C(21) C(22) C(23) 120.6(3) yes . . . C(22) C(23) C(24) 119.5(3) yes . . . C(23) C(24) C(25) 120.6(2) yes . . . C(13) C(25) C(20) 117.0(3) yes . . . C(13) C(25) C(24) 123.10(19) yes . . . C(20) C(25) C(24) 119.7(3) yes . . . C(12) C(26) C(27) 113.6(3) yes . . . C(12) C(26) C(38) 111.30(18) yes . . . C(27) C(26) C(38) 111.1(2) yes . . . C(26) C(27) C(28) 119.6(2) yes . . . C(26) C(27) C(32) 121.3(3) yes . . . C(28) C(27) C(32) 119.1(3) yes . . . C(27) C(28) C(29) 121.8(3) yes . . . C(28) C(29) C(30) 118.9(3) yes . . . C(29) C(30) C(31) 120.6(3) yes . . . C(30) C(31) C(32) 120.8(3) yes . . . N(2) C(32) C(27) 119.6(3) yes . . . N(2) C(32) C(31) 121.6(3) yes . . . C(27) C(32) C(31) 118.8(3) yes . . . N(2) C(33) C(34) 120.4(3) yes . . . N(2) C(33) C(38) 120.1(3) yes . . . C(34) C(33) C(38) 119.5(3) yes . . . C(33) C(34) C(35) 120.2(3) yes . . . C(34) C(35) C(36) 121.0(3) yes . . . C(35) C(36) C(37) 118.7(3) yes . . . C(36) C(37) C(38) 121.3(3) yes . . . C(26) C(38) C(33) 121.1(3) yes . . . C(26) C(38) C(37) 119.6(3) yes . . . C(33) C(38) C(37) 119.3(3) yes . . . C(41) C(41) C(44) 149.1(18) yes 4_557 . . C(41) C(41) C(44) 149.1(18) yes 4_557 . 2_555 C(41) C(41) C(44) 149.1(18) yes 4_557 . 3_555 C(44) C(41) C(44) 53(3) yes . . 2_555 C(44) C(41) C(44) 53(3) yes . . 3_555 C(44) C(41) C(44) 53(3) yes 2_555 . 3_555 Cl(1) C(42) Cl(1) 93.3(10) yes . . 2_555 Cl(1) C(42) Cl(1) 93.3(10) yes . . 3_555 Cl(1) C(42) C(44) 133.7(11) yes . . . Cl(1) C(42) C(44) 129.0(11) yes . . 2_555 Cl(1) C(42) C(44) 101.1(14) yes . . 3_555 Cl(1) C(42) Cl(1) 93.3(10) yes 2_555 . 3_555 Cl(1) C(42) C(44) 101.1(14) yes 2_555 . . Cl(1) C(42) C(44) 133.7(11) yes 2_555 . 2_555 Cl(1) C(42) C(44) 129.0(11) yes 2_555 . 3_555 Cl(1) C(42) C(44) 129.0(11) yes 3_555 . . Cl(1) C(42) C(44) 101.1(14) yes 3_555 . 2_555 Cl(1) C(42) C(44) 133.7(11) yes 3_555 . 3_555 C(44) C(42) C(44) 37.8(18) yes . . 2_555 C(44) C(42) C(44) 37.8(18) yes . . 3_555 C(44) C(42) C(44) 37.8(18) yes 2_555 . 3_555 Cl(1) C(43) Cl(1) 95.1(8) yes . . 2_555 Cl(1) C(43) Cl(1) 95.1(8) yes . . 3_555 Cl(1) C(43) Cl(1) 180.0(11) yes . . 4_556 Cl(1) C(43) Cl(1) 84.9(8) yes . . 5_556 Cl(1) C(43) Cl(1) 84.9(8) yes . . 6_556 Cl(1) C(43) Cl(1) 95.1(8) yes 2_555 . 3_555 Cl(1) C(43) Cl(1) 84.9(8) yes 2_555 . 4_556 Cl(1) C(43) Cl(1) 180.0(11) yes 2_555 . 5_556 Cl(1) C(43) Cl(1) 84.9(8) yes 2_555 . 6_556 Cl(1) C(43) Cl(1) 84.9(8) yes 3_555 . 4_556 Cl(1) C(43) Cl(1) 84.9(8) yes 3_555 . 5_556 Cl(1) C(43) Cl(1) 180.0(11) yes 3_555 . 6_556 Cl(1) C(43) Cl(1) 95.1(8) yes 4_556 . 5_556 Cl(1) C(43) Cl(1) 95.1(8) yes 4_556 . 6_556 Cl(1) C(43) Cl(1) 95.1(8) yes 5_556 . 6_556 C(41) C(44) C(42) 127(3) yes . . . C(41) C(44) C(44) 64(2) yes . . 2_555 C(41) C(44) C(44) 64(2) yes . . 3_555 C(42) C(44) C(44) 71.1(18) yes . . 2_555 C(42) C(44) C(44) 71.1(18) yes . . 3_555 C(44) C(44) C(44) 60(3) yes 2_555 . 3_555 C(1) C(2) H(1) 120.463 no . . . C(3) C(2) H(1) 120.871 no . . . C(2) C(3) H(2) 118.979 no . . . C(4) C(3) H(2) 119.013 no . . . C(3) C(4) H(3) 120.041 no . . . C(5) C(4) H(3) 119.327 no . . . C(5) C(6) H(4) 119.972 no . . . C(7) C(6) H(4) 120.218 no . . . C(6) C(7) H(5) 118.759 no . . . C(8) C(7) H(5) 118.652 no . . . C(7) C(8) H(6) 120.882 no . . . C(9) C(8) H(6) 120.488 no . . . C(11) C(13) H(23) 106.036 no . . . C(14) C(13) H(23) 106.087 no . . . C(25) C(13) H(23) 105.899 no . . . C(14) C(15) H(7) 119.042 no . . . C(16) C(15) H(7) 119.714 no . . . C(15) C(16) H(8) 120.441 no . . . C(17) C(16) H(8) 120.363 no . . . C(16) C(17) H(9) 119.728 no . . . C(18) C(17) H(9) 119.610 no . . . C(17) C(18) H(10) 120.066 no . . . C(19) C(18) H(10) 119.668 no . . . C(20) C(21) H(11) 119.886 no . . . C(22) C(21) H(11) 120.030 no . . . C(21) C(22) H(12) 119.512 no . . . C(23) C(22) H(12) 119.843 no . . . C(22) C(23) H(13) 120.022 no . . . C(24) C(23) H(13) 120.497 no . . . C(23) C(24) H(14) 120.082 no . . . C(25) C(24) H(14) 119.361 no . . . C(12) C(26) H(24) 106.828 no . . . C(27) C(26) H(24) 106.871 no . . . C(38) C(26) H(24) 106.713 no . . . C(27) C(28) H(15) 119.001 no . . . C(29) C(28) H(15) 119.222 no . . . C(28) C(29) H(16) 120.586 no . . . C(30) C(29) H(16) 120.546 no . . . C(29) C(30) H(17) 119.819 no . . . C(31) C(30) H(17) 119.621 no . . . C(30) C(31) H(18) 120.023 no . . . C(32) C(31) H(18) 119.138 no . . . C(33) C(34) H(19) 119.627 no . . . C(35) C(34) H(19) 120.159 no . . . C(34) C(35) H(20) 119.547 no . . . C(36) C(35) H(20) 119.460 no . . . C(35) C(36) H(21) 120.858 no . . . C(37) C(36) H(21) 120.407 no . . . C(36) C(37) H(22) 119.619 no . . . C(38) C(37) H(22) 119.118 no . . . N(1) C(39) H(25) 109.629 no . . . N(1) C(39) H(26) 109.352 no . . . N(1) C(39) H(27) 109.433 no . . . H(25) C(39) H(26) 109.472 no . . . H(25) C(39) H(27) 109.466 no . . . H(26) C(39) H(27) 109.475 no . . . N(2) C(40) H(28) 109.531 no . . . N(2) C(40) H(29) 109.450 no . . . N(2) C(40) H(30) 109.418 no . . . H(28) C(40) H(29) 109.470 no . . . H(28) C(40) H(30) 109.472 no . . . H(29) C(40) H(30) 109.486 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C(42) Cl(1) C(43) Cl(1) 47.8(5) no . . . 2_555 C(42) Cl(1) C(43) Cl(1) -47.8(5) no . . . 3_555 C(42) Cl(1) C(43) Cl(1) -132.2(5) no . . . 5_556 C(42) Cl(1) C(43) Cl(1) 132.2(5) no . . . 6_556 C(43) Cl(1) C(42) Cl(1) -46.7(6) no . . . 2_555 C(43) Cl(1) C(42) Cl(1) 46.7(6) no . . . 3_555 C(43) Cl(1) C(42) C(44) -155.4(6) no . . . . C(43) Cl(1) C(42) C(44) 153.8(5) no . . . 2_555 C(43) Cl(1) C(42) C(44) -177.5(3) no . . . 3_555 C(19) N(1) C(20) C(21) -145.6(2) no . . . . C(19) N(1) C(20) C(25) 34.1(3) no . . . . C(20) N(1) C(19) C(14) -34.7(3) no . . . . C(20) N(1) C(19) C(18) 145.25(19) no . . . . C(39) N(1) C(19) C(14) 173.31(16) no . . . . C(39) N(1) C(19) C(18) -6.7(3) no . . . . C(39) N(1) C(20) C(21) 5.9(4) no . . . . C(39) N(1) C(20) C(25) -174.43(19) no . . . . C(32) N(2) C(33) C(34) -159.3(2) no . . . . C(32) N(2) C(33) C(38) 20.9(3) no . . . . C(33) N(2) C(32) C(27) -25.5(4) no . . . . C(33) N(2) C(32) C(31) 156.3(3) no . . . . C(40) N(2) C(32) C(27) 165.1(2) no . . . . C(40) N(2) C(32) C(31) -13.1(4) no . . . . C(40) N(2) C(33) C(34) 10.3(3) no . . . . C(40) N(2) C(33) C(38) -169.47(18) no . . . . C(2) C(1) C(10) C(5) 1.4(5) no . . . . C(2) C(1) C(10) C(9) 179.7(3) no . . . . C(10) C(1) C(2) C(3) -0.1(4) no . . . . C(2) C(1) C(11) C(12) 179.5(4) no . . . . C(2) C(1) C(11) C(13) -2.4(6) no . . . . C(11) C(1) C(2) C(3) 178.2(3) no . . . . C(10) C(1) C(11) C(12) -2.0(3) no . . . . C(10) C(1) C(11) C(13) 176.0(3) no . . . . C(11) C(1) C(10) C(5) -177.4(3) no . . . . C(11) C(1) C(10) C(9) 0.9(4) no . . . . C(1) C(2) C(3) C(4) -0.5(5) no . . . . C(2) C(3) C(4) C(5) -0.0(5) no . . . . C(3) C(4) C(5) C(6) -177.4(3) no . . . . C(3) C(4) C(5) C(10) 1.1(5) no . . . . C(4) C(5) C(6) C(7) 179.4(3) no . . . . C(4) C(5) C(10) C(1) -1.9(5) no . . . . C(4) C(5) C(10) C(9) -180(47895) no . . . . C(6) C(5) C(10) C(1) 176.9(3) no . . . . C(6) C(5) C(10) C(9) -1.3(5) no . . . . C(10) C(5) C(6) C(7) 0.8(5) no . . . . C(5) C(6) C(7) C(8) -0.0(6) no . . . . C(6) C(7) C(8) C(9) -0.4(6) no . . . . C(7) C(8) C(9) C(10) 0.0(5) no . . . . C(7) C(8) C(9) C(12) -177.1(3) no . . . . C(8) C(9) C(10) C(1) -177.5(3) no . . . . C(8) C(9) C(10) C(5) 0.9(5) no . . . . C(8) C(9) C(12) C(11) 175.6(4) no . . . . C(8) C(9) C(12) C(26) -6.8(6) no . . . . C(10) C(9) C(12) C(11) -1.7(4) no . . . . C(10) C(9) C(12) C(26) 175.9(3) no . . . . C(12) C(9) C(10) C(1) 0.4(4) no . . . . C(12) C(9) C(10) C(5) 178.7(3) no . . . . C(1) C(11) C(12) C(9) 2.3(4) no . . . . C(1) C(11) C(12) C(26) -175.2(3) no . . . . C(1) C(11) C(13) C(14) -57.6(4) no . . . . C(1) C(11) C(13) C(25) 69.1(4) no . . . . C(12) C(11) C(13) C(14) 120.1(3) no . . . . C(12) C(11) C(13) C(25) -113.2(3) no . . . . C(13) C(11) C(12) C(9) -175.7(3) no . . . . C(13) C(11) C(12) C(26) 6.7(5) no . . . . C(9) C(12) C(26) C(27) 70.8(4) no . . . . C(9) C(12) C(26) C(38) -55.5(4) no . . . . C(11) C(12) C(26) C(27) -112.0(3) no . . . . C(11) C(12) C(26) C(38) 121.7(3) no . . . . C(11) C(13) C(14) C(15) -12.4(3) no . . . . C(11) C(13) C(14) C(19) 170.90(16) no . . . . C(11) C(13) C(25) C(20) -171.0(2) no . . . . C(11) C(13) C(25) C(24) 13.4(4) no . . . . C(14) C(13) C(25) C(20) -41.4(3) no . . . . C(14) C(13) C(25) C(24) 143.02(19) no . . . . C(25) C(13) C(14) C(15) -142.51(18) no . . . . C(25) C(13) C(14) C(19) 40.8(3) no . . . . C(13) C(14) C(15) C(16) -176.97(17) no . . . . C(13) C(14) C(19) N(1) -4.8(3) no . . . . C(13) C(14) C(19) C(18) 175.24(16) no . . . . C(15) C(14) C(19) N(1) 178.38(17) no . . . . C(15) C(14) C(19) C(18) -1.6(3) no . . . . C(19) C(14) C(15) C(16) -0.3(3) no . . . . C(14) C(15) C(16) C(17) 1.3(4) no . . . . C(15) C(16) C(17) C(18) -0.3(4) no . . . . C(16) C(17) C(18) C(19) -1.7(4) no . . . . C(17) C(18) C(19) N(1) -177.37(18) no . . . . C(17) C(18) C(19) C(14) 2.6(3) no . . . . N(1) C(20) C(21) C(22) 179.4(2) no . . . . N(1) C(20) C(25) C(13) 6.1(4) no . . . . N(1) C(20) C(25) C(24) -178.16(19) no . . . . C(21) C(20) C(25) C(13) -174.2(2) no . . . . C(21) C(20) C(25) C(24) 1.5(4) no . . . . C(25) C(20) C(21) C(22) -0.3(4) no . . . . C(20) C(21) C(22) C(23) -1.5(4) no . . . . C(21) C(22) C(23) C(24) 2.1(4) no . . . . C(22) C(23) C(24) C(25) -0.8(4) no . . . . C(23) C(24) C(25) C(13) 174.5(2) no . . . . C(23) C(24) C(25) C(20) -1.0(4) no . . . . C(12) C(26) C(27) C(28) 70.7(3) no . . . . C(12) C(26) C(27) C(32) -110.4(3) no . . . . C(12) C(26) C(38) C(33) 107.1(3) no . . . . C(12) C(26) C(38) C(37) -71.8(3) no . . . . C(27) C(26) C(38) C(33) -20.5(3) no . . . . C(27) C(26) C(38) C(37) 160.60(17) no . . . . C(38) C(26) C(27) C(28) -162.91(18) no . . . . C(38) C(26) C(27) C(32) 16.0(3) no . . . . C(26) C(27) C(28) C(29) 178.3(2) no . . . . C(26) C(27) C(32) N(2) 5.6(4) no . . . . C(26) C(27) C(32) C(31) -176.1(2) no . . . . C(28) C(27) C(32) N(2) -175.4(3) no . . . . C(28) C(27) C(32) C(31) 2.9(4) no . . . . C(32) C(27) C(28) C(29) -0.7(4) no . . . . C(27) C(28) C(29) C(30) -1.6(4) no . . . . C(28) C(29) C(30) C(31) 1.7(4) no . . . . C(29) C(30) C(31) C(32) 0.5(4) no . . . . C(30) C(31) C(32) N(2) 175.4(3) no . . . . C(30) C(31) C(32) C(27) -2.8(4) no . . . . N(2) C(33) C(34) C(35) 178.27(18) no . . . . N(2) C(33) C(38) C(26) 3.3(3) no . . . . N(2) C(33) C(38) C(37) -177.84(17) no . . . . C(34) C(33) C(38) C(26) -176.54(18) no . . . . C(34) C(33) C(38) C(37) 2.4(3) no . . . . C(38) C(33) C(34) C(35) -1.9(4) no . . . . C(33) C(34) C(35) C(36) 0.3(4) no . . . . C(34) C(35) C(36) C(37) 0.9(4) no . . . . C(35) C(36) C(37) C(38) -0.4(4) no . . . . C(36) C(37) C(38) C(26) 177.73(18) no . . . . C(36) C(37) C(38) C(33) -1.2(4) no . . . . C(41) C(41) C(44) C(42) -180(284400) no 4_557 . . . C(41) C(41) C(44) C(44) -146.1(15) no 4_557 . . 2_555 C(41) C(41) C(44) C(44) 146.1(13) no 4_557 . . 3_555 C(44) C(41) C(41) C(44) 180(509344) no . . 4_557 4_557 C(44) C(41) C(41) C(44) -60(3) no . . 4_557 5_557 C(44) C(41) C(41) C(44) 60(3) no . . 4_557 6_557 C(41) C(41) C(44) C(42) -180(509346) no 4_557 . 2_555 . C(41) C(41) C(44) C(44) -146.1(15) no 4_557 . 2_555 3_555 C(41) C(41) C(44) C(44) 146.1(13) no 4_557 . 2_555 . C(44) C(41) C(41) C(44) 60(3) no 2_555 . 4_557 4_557 C(44) C(41) C(41) C(44) 180(509344) no 2_555 . 4_557 5_557 C(44) C(41) C(41) C(44) -60(3) no 2_555 . 4_557 6_557 C(41) C(41) C(44) C(42) 180.0 no 4_557 . 3_555 . C(41) C(41) C(44) C(44) -146.1(15) no 4_557 . 3_555 . C(41) C(41) C(44) C(44) 146.1(13) no 4_557 . 3_555 2_555 C(44) C(41) C(41) C(44) -60(3) no 3_555 . 4_557 4_557 C(44) C(41) C(41) C(44) 60(3) no 3_555 . 4_557 5_557 C(44) C(41) C(41) C(44) 180(509344) no 3_555 . 4_557 6_557 C(44) C(41) C(44) C(42) 34(2) no . . 2_555 . C(44) C(41) C(44) C(44) 68(3) no . . 2_555 3_555 C(44) C(41) C(44) C(44) 0.0(16) no . . 2_555 . C(44) C(41) C(44) C(42) -34(3) no 2_555 . . . C(44) C(41) C(44) C(44) -0.0(18) no 2_555 . . 2_555 C(44) C(41) C(44) C(44) -68(3) no 2_555 . . 3_555 C(44) C(41) C(44) C(42) -34(3) no . . 3_555 . C(44) C(41) C(44) C(44) 0.0(18) no . . 3_555 . C(44) C(41) C(44) C(44) -68(3) no . . 3_555 2_555 C(44) C(41) C(44) C(42) 34(2) no 3_555 . . . C(44) C(41) C(44) C(44) 68(3) no 3_555 . . 2_555 C(44) C(41) C(44) C(44) 0.0(16) no 3_555 . . 3_555 C(44) C(41) C(44) C(42) 34(2) no 2_555 . 3_555 . C(44) C(41) C(44) C(44) 68(3) no 2_555 . 3_555 . C(44) C(41) C(44) C(44) 0.0(16) no 2_555 . 3_555 2_555 C(44) C(41) C(44) C(42) -34(3) no 3_555 . 2_555 . C(44) C(41) C(44) C(44) 0.0(18) no 3_555 . 2_555 3_555 C(44) C(41) C(44) C(44) -68(3) no 3_555 . 2_555 . Cl(1) C(42) C(44) C(41) -69(3) no . . . . Cl(1) C(42) C(44) C(44) -100.8(17) no . . . 2_555 Cl(1) C(42) C(44) C(44) -37(3) no . . . 3_555 Cl(1) C(42) C(44) C(41) 82(3) no . . 2_555 . Cl(1) C(42) C(44) C(44) 50(3) no . . 2_555 3_555 Cl(1) C(42) C(44) C(44) 114.0(14) no . . 2_555 . Cl(1) C(42) C(44) C(41) -174(2) no . . 3_555 . Cl(1) C(42) C(44) C(44) 153.7(13) no . . 3_555 . Cl(1) C(42) C(44) C(44) -142.5(15) no . . 3_555 2_555 Cl(1) C(42) C(44) C(41) -174(2) no 2_555 . . . Cl(1) C(42) C(44) C(44) 153.7(13) no 2_555 . . 2_555 Cl(1) C(42) C(44) C(44) -142.5(15) no 2_555 . . 3_555 Cl(1) C(42) C(44) C(41) -69(3) no 2_555 . 2_555 . Cl(1) C(42) C(44) C(44) -100.8(17) no 2_555 . 2_555 3_555 Cl(1) C(42) C(44) C(44) -37(3) no 2_555 . 2_555 . Cl(1) C(42) C(44) C(41) 82(3) no 2_555 . 3_555 . Cl(1) C(42) C(44) C(44) 50(3) no 2_555 . 3_555 . Cl(1) C(42) C(44) C(44) 114.0(14) no 2_555 . 3_555 2_555 Cl(1) C(42) C(44) C(41) 82(3) no 3_555 . . . Cl(1) C(42) C(44) C(44) 50(3) no 3_555 . . 2_555 Cl(1) C(42) C(44) C(44) 114.0(14) no 3_555 . . 3_555 Cl(1) C(42) C(44) C(41) -174(2) no 3_555 . 2_555 . Cl(1) C(42) C(44) C(44) 153.7(13) no 3_555 . 2_555 3_555 Cl(1) C(42) C(44) C(44) -142.5(15) no 3_555 . 2_555 . Cl(1) C(42) C(44) C(41) -69(3) no 3_555 . 3_555 . Cl(1) C(42) C(44) C(44) -100.8(17) no 3_555 . 3_555 . Cl(1) C(42) C(44) C(44) -37(3) no 3_555 . 3_555 2_555 C(44) C(42) C(44) C(41) -32(2) no . . 2_555 . C(44) C(42) C(44) C(44) -64(3) no . . 2_555 3_555 C(44) C(42) C(44) C(44) 0.0(15) no . . 2_555 . C(44) C(42) C(44) C(41) 32(3) no 2_555 . . . C(44) C(42) C(44) C(44) 0.0(18) no 2_555 . . 2_555 C(44) C(42) C(44) C(44) 64(3) no 2_555 . . 3_555 C(44) C(42) C(44) C(41) 32(3) no . . 3_555 . C(44) C(42) C(44) C(44) 0.0(18) no . . 3_555 . C(44) C(42) C(44) C(44) 64(3) no . . 3_555 2_555 C(44) C(42) C(44) C(41) -32(2) no 3_555 . . . C(44) C(42) C(44) C(44) -64(3) no 3_555 . . 2_555 C(44) C(42) C(44) C(44) 0.0(15) no 3_555 . . 3_555 C(44) C(42) C(44) C(41) -32(2) no 2_555 . 3_555 . C(44) C(42) C(44) C(44) -64(3) no 2_555 . 3_555 . C(44) C(42) C(44) C(44) 0.0(15) no 2_555 . 3_555 2_555 C(44) C(42) C(44) C(41) 32(3) no 3_555 . 2_555 . C(44) C(42) C(44) C(44) 0.0(18) no 3_555 . 2_555 3_555 C(44) C(42) C(44) C(44) 64(3) no 3_555 . 2_555 . C(41) C(44) C(44) C(41) 0.00(13) no . . 2_555 . C(41) C(44) C(44) C(42) -151.9(18) no . . 2_555 . C(41) C(44) C(44) C(44) -73.4(12) no . . 2_555 3_555 C(41) C(44) C(44) C(41) 0.00(13) no . . 3_555 . C(41) C(44) C(44) C(42) 151.9(18) no . . 3_555 . C(41) C(44) C(44) C(44) 73.4(12) no . . 3_555 2_555 C(42) C(44) C(44) C(41) 151.9(18) no . . 2_555 . C(42) C(44) C(44) C(42) 0.00(14) no . . 2_555 . C(42) C(44) C(44) C(44) 78.6(10) no . . 2_555 3_555 C(42) C(44) C(44) C(41) -151.9(18) no . . 3_555 . C(42) C(44) C(44) C(42) 0.00(14) no . . 3_555 . C(42) C(44) C(44) C(44) -78.6(10) no . . 3_555 2_555 C(44) C(44) C(44) C(41) -73.4(16) no 2_555 . 3_555 . C(44) C(44) C(44) C(42) 78.6(14) no 2_555 . 3_555 . C(44) C(44) C(44) C(44) 0.0(10) no 2_555 . 3_555 2_555 C(44) C(44) C(44) C(41) 73.4(16) no 3_555 . 2_555 . C(44) C(44) C(44) C(42) -78.6(14) no 3_555 . 2_555 . C(44) C(44) C(44) C(44) 0.0(10) no 3_555 . 2_555 3_555 loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Cl(1) C(7) 3.57(3) no . . C(6) C(44) 3.53(3) no . . C(6) C(44) 3.53(3) no . 3_555 C(7) Cl(1) 3.57(3) no . . C(10) C(23) 3.600(4) no . 6_557 C(16) C(21) 3.559(4) no . 15_554 C(16) C(22) 3.478(4) no . 15_554 C(18) C(30) 3.566(4) no . 1_556 C(18) C(31) 3.445(4) no . 1_556 C(20) C(29) 3.550(4) no . 8_555 C(21) C(16) 3.559(4) no . 8_555 C(22) C(16) 3.478(4) no . 8_555 C(23) C(10) 3.600(4) no . 5_557 C(29) C(20) 3.550(4) no . 15_554 C(30) C(18) 3.566(4) no . 1_554 C(31) C(18) 3.445(4) no . 1_554 C(31) C(35) 3.475(5) no . 6_556 C(35) C(31) 3.475(5) no . 5_556 C(41) C(44) 2.53(3) no . 5_557 C(41) C(44) 2.53(3) no . 6_557 C(44) C(6) 3.53(3) no . . C(44) C(6) 3.53(3) no . 2_555 Cl(1) H(4) 3.0832 no . 3_555 Cl(1) H(5) 3.2919 no . . Cl(1) H(5) 3.1733 no . 3_555 Cl(1) H(5) 3.0792 no . 5_556 N(1) H(15) 3.3888 no . 8_555 N(1) H(18) 3.2904 no . 1_556 N(1) H(26) 3.3535 no . 15_554 N(1) H(27) 3.1496 no . 15_554 N(1) H(28) 3.4986 no . 1_556 N(2) H(20) 3.1006 no . 6_556 C(1) H(3) 3.0780 no . 5_557 C(1) H(13) 3.1221 no . 6_557 C(2) H(3) 3.2098 no . 5_557 C(2) H(4) 3.4442 no . 5_557 C(2) H(21) 3.3251 no . 6_557 C(2) H(30) 3.4922 no . 1_556 C(3) H(3) 3.1847 no . 5_557 C(3) H(4) 3.2134 no . 5_557 C(3) H(14) 3.1460 no . 6_557 C(4) H(3) 3.0722 no . 5_557 C(4) H(14) 2.8809 no . 6_557 C(5) H(3) 2.9607 no . 5_557 C(5) H(13) 3.1678 no . 6_557 C(5) H(14) 3.1499 no . 6_557 C(6) H(29) 3.4351 no . 6_556 C(7) H(19) 3.1151 no . 6_556 C(7) H(29) 3.3820 no . 6_556 C(8) H(13) 3.5554 no . 6_557 C(8) H(19) 3.3209 no . 6_556 C(8) H(20) 3.3420 no . 6_556 C(9) H(2) 3.5997 no . 5_557 C(9) H(13) 3.0438 no . 6_557 C(10) H(3) 2.9091 no . 5_557 C(10) H(13) 2.7943 no . 6_557 C(11) H(13) 3.5154 no . 6_557 C(12) H(13) 3.5043 no . 6_557 C(13) H(16) 3.5667 no . 8_555 C(13) H(26) 3.1964 no . 15_554 C(14) H(11) 2.9813 no . 15_554 C(14) H(26) 3.1491 no . 15_554 C(15) H(11) 2.9418 no . 15_554 C(15) H(12) 3.4355 no . 15_554 C(15) H(13) 3.4184 no . 6_557 C(15) H(21) 3.1513 no . 6_557 C(16) H(11) 2.9607 no . 15_554 C(16) H(12) 2.7872 no . 15_554 C(16) H(21) 2.9734 no . 6_557 C(16) H(22) 3.4977 no . 6_557 C(17) H(11) 2.9720 no . 15_554 C(17) H(12) 3.1851 no . 15_554 C(17) H(17) 3.1930 no . 1_556 C(17) H(18) 3.3380 no . 1_556 C(17) H(21) 3.2938 no . 6_557 C(18) H(11) 2.9820 no . 15_554 C(18) H(17) 3.0279 no . 1_556 C(18) H(18) 2.7763 no . 1_556 C(19) H(11) 3.0123 no . 15_554 C(19) H(18) 2.9343 no . 1_556 C(19) H(26) 3.1943 no . 15_554 C(19) H(27) 3.2475 no . 15_554 C(20) H(15) 3.2206 no . 8_555 C(20) H(16) 2.9248 no . 8_555 C(20) H(28) 2.7452 no . 1_556 C(21) H(15) 3.0000 no . 8_555 C(21) H(16) 3.1333 no . 8_555 C(21) H(28) 2.7523 no . 1_556 C(22) H(8) 3.4827 no . 8_555 C(22) H(16) 3.3139 no . 8_555 C(22) H(19) 3.0921 no . 1_556 C(22) H(28) 2.9532 no . 1_556 C(23) H(7) 3.0481 no . 5_557 C(23) H(16) 3.3287 no . 8_555 C(23) H(19) 3.2962 no . 1_556 C(23) H(28) 3.1107 no . 1_556 C(24) H(16) 3.1133 no . 8_555 C(24) H(28) 3.1067 no . 1_556 C(25) H(16) 2.8977 no . 8_555 C(25) H(28) 2.9433 no . 1_556 C(26) H(10) 3.5167 no . 8_554 C(27) H(10) 3.4270 no . 8_554 C(27) H(20) 3.5686 no . 6_556 C(27) H(25) 3.4374 no . 8_554 C(28) H(25) 3.3428 no . 8_554 C(28) H(26) 3.1970 no . 15_554 C(29) H(8) 3.0299 no . 16_556 C(29) H(23) 3.5797 no . 15_554 C(29) H(25) 3.3425 no . 8_554 C(30) H(8) 3.1173 no . 16_556 C(30) H(10) 3.2192 no . 1_554 C(30) H(20) 3.3590 no . 6_556 C(30) H(22) 3.5516 no . 15_554 C(30) H(24) 3.5821 no . 15_554 C(30) H(25) 3.3808 no . 8_554 C(31) H(10) 3.3325 no . 1_554 C(31) H(20) 2.7339 no . 6_556 C(31) H(21) 3.3085 no . 6_556 C(31) H(25) 3.4631 no . 8_554 C(31) H(27) 3.2492 no . 1_554 C(32) H(10) 3.5491 no . 8_554 C(32) H(20) 2.8326 no . 6_556 C(32) H(25) 3.5254 no . 8_554 C(33) H(9) 3.0924 no . 8_554 C(33) H(10) 3.5305 no . 8_554 C(34) H(5) 3.5215 no . 5_556 C(34) H(9) 2.9489 no . 8_554 C(34) H(12) 3.4429 no . 1_554 C(35) H(6) 3.4712 no . 5_556 C(35) H(9) 2.8093 no . 8_554 C(35) H(18) 3.4363 no . 5_556 C(35) H(30) 2.8835 no . 5_556 C(36) H(1) 3.2044 no . 5_557 C(36) H(2) 3.5357 no . 5_557 C(36) H(9) 2.8274 no . 8_554 C(36) H(18) 3.3807 no . 5_556 C(36) H(30) 2.9446 no . 5_556 C(37) H(2) 3.4781 no . 5_557 C(37) H(9) 2.9834 no . 8_554 C(37) H(17) 3.1239 no . 8_555 C(38) H(9) 3.1314 no . 8_554 C(38) H(10) 3.3133 no . 8_554 C(38) H(17) 3.5684 no . 8_555 C(39) H(15) 3.2233 no . 8_555 C(39) H(18) 3.5804 no . 1_556 C(39) H(23) 3.2654 no . 8_555 C(39) H(27) 3.3001 no . 15_554 C(40) H(1) 3.0665 no . 1_554 C(40) H(20) 3.0616 no . 6_556 C(40) H(21) 3.4622 no . 6_556 C(42) H(4) 3.4544 no . . C(42) H(4) 3.4544 no . 2_555 C(42) H(4) 3.4544 no . 3_555 C(44) H(3) 3.3744 no . 6_557 C(44) H(4) 3.0068 no . . C(44) H(4) 3.3002 no . 2_555 H(1) C(36) 3.2044 no . 6_557 H(1) C(40) 3.0665 no . 1_556 H(1) H(4) 3.4961 no . 5_557 H(1) H(21) 2.6727 no . 6_557 H(1) H(28) 3.0379 no . 1_556 H(1) H(29) 3.1019 no . 1_556 H(1) H(30) 2.5691 no . 1_556 H(2) C(9) 3.5997 no . 6_557 H(2) C(36) 3.5357 no . 6_557 H(2) C(37) 3.4781 no . 6_557 H(2) H(4) 3.0893 no . 5_557 H(2) H(14) 3.5151 no . 6_557 H(2) H(22) 3.5426 no . 6_557 H(3) C(1) 3.0780 no . 6_557 H(3) C(2) 3.2098 no . 6_557 H(3) C(3) 3.1847 no . 6_557 H(3) C(4) 3.0722 no . 6_557 H(3) C(5) 2.9607 no . 6_557 H(3) C(10) 2.9091 no . 6_557 H(3) C(44) 3.3744 no . 5_557 H(3) H(14) 3.1081 no . 6_557 H(4) Cl(1) 3.0832 no . 2_555 H(4) C(2) 3.4442 no . 6_557 H(4) C(3) 3.2134 no . 6_557 H(4) C(42) 3.4544 no . . H(4) C(44) 3.0068 no . . H(4) C(44) 3.3002 no . 3_555 H(4) H(1) 3.4961 no . 6_557 H(4) H(2) 3.0893 no . 6_557 H(4) H(29) 3.2533 no . 6_556 H(5) Cl(1) 3.2919 no . . H(5) Cl(1) 3.1733 no . 2_555 H(5) Cl(1) 3.0792 no . 6_556 H(5) C(34) 3.5215 no . 6_556 H(5) H(19) 3.0338 no . 6_556 H(5) H(29) 3.1393 no . 6_556 H(6) C(35) 3.4712 no . 6_556 H(6) H(19) 3.3933 no . 6_556 H(6) H(20) 2.7993 no . 6_556 H(7) C(23) 3.0481 no . 6_557 H(7) H(11) 3.4658 no . 15_554 H(7) H(13) 2.4808 no . 6_557 H(7) H(21) 3.4866 no . 6_557 H(8) C(22) 3.4827 no . 15_554 H(8) C(29) 3.0299 no . 16_556 H(8) C(30) 3.1173 no . 16_556 H(8) H(11) 3.5073 no . 15_554 H(8) H(12) 2.6309 no . 15_554 H(8) H(16) 2.7471 no . 16_556 H(8) H(17) 2.9118 no . 16_556 H(8) H(21) 3.1964 no . 6_557 H(8) H(22) 3.0779 no . 6_557 H(9) C(33) 3.0924 no . 15_555 H(9) C(34) 2.9489 no . 15_555 H(9) C(35) 2.8093 no . 15_555 H(9) C(36) 2.8274 no . 15_555 H(9) C(37) 2.9834 no . 15_555 H(9) C(38) 3.1314 no . 15_555 H(9) H(11) 3.5202 no . 15_554 H(9) H(12) 3.3009 no . 15_554 H(9) H(17) 2.9454 no . 1_556 H(9) H(19) 3.4957 no . 15_555 H(9) H(20) 3.2928 no . 15_555 H(9) H(21) 3.3091 no . 15_555 H(9) H(22) 3.5312 no . 15_555 H(10) C(26) 3.5167 no . 15_555 H(10) C(27) 3.4270 no . 15_555 H(10) C(30) 3.2192 no . 1_556 H(10) C(31) 3.3325 no . 1_556 H(10) C(32) 3.5491 no . 15_555 H(10) C(33) 3.5305 no . 15_555 H(10) C(38) 3.3133 no . 15_555 H(10) H(11) 3.5120 no . 15_554 H(10) H(17) 2.6652 no . 1_556 H(10) H(18) 2.8781 no . 1_556 H(10) H(24) 3.2158 no . 15_555 H(11) C(14) 2.9813 no . 8_555 H(11) C(15) 2.9418 no . 8_555 H(11) C(16) 2.9607 no . 8_555 H(11) C(17) 2.9720 no . 8_555 H(11) C(18) 2.9820 no . 8_555 H(11) C(19) 3.0123 no . 8_555 H(11) H(7) 3.4658 no . 8_555 H(11) H(8) 3.5073 no . 8_555 H(11) H(9) 3.5202 no . 8_555 H(11) H(10) 3.5120 no . 8_555 H(11) H(15) 2.8589 no . 8_555 H(11) H(23) 3.5597 no . 8_555 H(11) H(28) 3.2229 no . 1_556 H(12) C(15) 3.4355 no . 8_555 H(12) C(16) 2.7872 no . 8_555 H(12) C(17) 3.1851 no . 8_555 H(12) C(34) 3.4429 no . 1_556 H(12) H(8) 2.6309 no . 8_555 H(12) H(9) 3.3009 no . 8_555 H(12) H(19) 3.0241 no . 1_556 H(12) H(28) 3.5175 no . 1_556 H(13) C(1) 3.1221 no . 5_557 H(13) C(5) 3.1678 no . 5_557 H(13) C(8) 3.5554 no . 5_557 H(13) C(9) 3.0438 no . 5_557 H(13) C(10) 2.7943 no . 5_557 H(13) C(11) 3.5154 no . 5_557 H(13) C(12) 3.5043 no . 5_557 H(13) C(15) 3.4184 no . 5_557 H(13) H(7) 2.4808 no . 5_557 H(13) H(19) 3.3495 no . 1_556 H(14) C(3) 3.1460 no . 5_557 H(14) C(4) 2.8809 no . 5_557 H(14) C(5) 3.1499 no . 5_557 H(14) H(2) 3.5151 no . 5_557 H(14) H(3) 3.1081 no . 5_557 H(15) N(1) 3.3888 no . 15_554 H(15) C(20) 3.2206 no . 15_554 H(15) C(21) 3.0000 no . 15_554 H(15) C(39) 3.2233 no . 15_554 H(15) H(11) 2.8589 no . 15_554 H(15) H(26) 2.4277 no . 15_554 H(16) C(13) 3.5667 no . 15_554 H(16) C(20) 2.9248 no . 15_554 H(16) C(21) 3.1333 no . 15_554 H(16) C(22) 3.3139 no . 15_554 H(16) C(23) 3.3287 no . 15_554 H(16) C(24) 3.1133 no . 15_554 H(16) C(25) 2.8977 no . 15_554 H(16) H(8) 2.7471 no . 16_556 H(16) H(22) 3.1588 no . 15_554 H(16) H(23) 3.1125 no . 15_554 H(16) H(24) 3.5327 no . 15_554 H(17) C(17) 3.1930 no . 1_554 H(17) C(18) 3.0279 no . 1_554 H(17) C(37) 3.1239 no . 15_554 H(17) C(38) 3.5684 no . 15_554 H(17) H(8) 2.9118 no . 16_556 H(17) H(9) 2.9454 no . 1_554 H(17) H(10) 2.6652 no . 1_554 H(17) H(22) 2.8133 no . 15_554 H(17) H(24) 3.0625 no . 15_554 H(18) N(1) 3.2904 no . 1_554 H(18) C(17) 3.3380 no . 1_554 H(18) C(18) 2.7763 no . 1_554 H(18) C(19) 2.9343 no . 1_554 H(18) C(35) 3.4363 no . 6_556 H(18) C(36) 3.3807 no . 6_556 H(18) C(39) 3.5804 no . 1_554 H(18) H(10) 2.8781 no . 1_554 H(18) H(20) 2.8425 no . 6_556 H(18) H(21) 2.7436 no . 6_556 H(18) H(27) 2.9872 no . 1_554 H(19) C(7) 3.1151 no . 5_556 H(19) C(8) 3.3209 no . 5_556 H(19) C(22) 3.0921 no . 1_554 H(19) C(23) 3.2962 no . 1_554 H(19) H(5) 3.0338 no . 5_556 H(19) H(6) 3.3933 no . 5_556 H(19) H(9) 3.4957 no . 8_554 H(19) H(12) 3.0241 no . 1_554 H(19) H(13) 3.3495 no . 1_554 H(20) N(2) 3.1006 no . 5_556 H(20) C(8) 3.3420 no . 5_556 H(20) C(27) 3.5686 no . 5_556 H(20) C(30) 3.3590 no . 5_556 H(20) C(31) 2.7339 no . 5_556 H(20) C(32) 2.8326 no . 5_556 H(20) C(40) 3.0616 no . 5_556 H(20) H(6) 2.7993 no . 5_556 H(20) H(9) 3.2928 no . 8_554 H(20) H(18) 2.8425 no . 5_556 H(20) H(29) 3.4197 no . 5_556 H(20) H(30) 2.3699 no . 5_556 H(21) C(2) 3.3251 no . 5_557 H(21) C(15) 3.1513 no . 5_557 H(21) C(16) 2.9733 no . 5_557 H(21) C(17) 3.2938 no . 5_557 H(21) C(31) 3.3085 no . 5_556 H(21) C(40) 3.4622 no . 5_556 H(21) H(1) 2.6727 no . 5_557 H(21) H(7) 3.4866 no . 5_557 H(21) H(8) 3.1964 no . 5_557 H(21) H(9) 3.3091 no . 8_554 H(21) H(18) 2.7436 no . 5_556 H(21) H(30) 2.5179 no . 5_556 H(22) C(16) 3.4977 no . 5_557 H(22) C(30) 3.5516 no . 8_555 H(22) H(2) 3.5426 no . 5_557 H(22) H(8) 3.0779 no . 5_557 H(22) H(9) 3.5312 no . 8_554 H(22) H(16) 3.1588 no . 8_555 H(22) H(17) 2.8133 no . 8_555 H(23) C(29) 3.5797 no . 8_555 H(23) C(39) 3.2654 no . 15_554 H(23) H(11) 3.5597 no . 15_554 H(23) H(16) 3.1125 no . 8_555 H(23) H(25) 3.4322 no . 15_554 H(23) H(26) 2.4402 no . 15_554 H(23) H(27) 3.5556 no . 15_554 H(24) C(30) 3.5821 no . 8_555 H(24) H(10) 3.2158 no . 8_554 H(24) H(16) 3.5327 no . 8_555 H(24) H(17) 3.0625 no . 8_555 H(24) H(26) 3.2396 no . 15_554 H(25) C(27) 3.4374 no . 15_555 H(25) C(28) 3.3428 no . 15_555 H(25) C(29) 3.3425 no . 15_555 H(25) C(30) 3.3808 no . 15_555 H(25) C(31) 3.4631 no . 15_555 H(25) C(32) 3.5254 no . 15_555 H(25) H(23) 3.4322 no . 8_555 H(25) H(27) 2.7606 no . 15_554 H(26) N(1) 3.3535 no . 8_555 H(26) C(13) 3.1964 no . 8_555 H(26) C(14) 3.1491 no . 8_555 H(26) C(19) 3.1943 no . 8_555 H(26) C(28) 3.1970 no . 8_555 H(26) H(15) 2.4277 no . 8_555 H(26) H(23) 2.4402 no . 8_555 H(26) H(24) 3.2396 no . 8_555 H(26) H(27) 3.5333 no . 15_554 H(27) N(1) 3.1496 no . 8_555 H(27) C(19) 3.2475 no . 8_555 H(27) C(31) 3.2492 no . 1_556 H(27) C(39) 3.3001 no . 8_555 H(27) H(18) 2.9872 no . 1_556 H(27) H(23) 3.5556 no . 8_555 H(27) H(25) 2.7606 no . 8_555 H(27) H(26) 3.5333 no . 8_555 H(28) N(1) 3.4986 no . 1_554 H(28) C(20) 2.7452 no . 1_554 H(28) C(21) 2.7523 no . 1_554 H(28) C(22) 2.9532 no . 1_554 H(28) C(23) 3.1107 no . 1_554 H(28) C(24) 3.1067 no . 1_554 H(28) C(25) 2.9433 no . 1_554 H(28) H(1) 3.0379 no . 1_554 H(28) H(11) 3.2229 no . 1_554 H(28) H(12) 3.5175 no . 1_554 H(29) C(6) 3.4351 no . 5_556 H(29) C(7) 3.3820 no . 5_556 H(29) H(1) 3.1019 no . 1_554 H(29) H(4) 3.2533 no . 5_556 H(29) H(5) 3.1393 no . 5_556 H(29) H(20) 3.4197 no . 6_556 H(30) C(2) 3.4922 no . 1_554 H(30) C(35) 2.8835 no . 6_556 H(30) C(36) 2.9446 no . 6_556 H(30) H(1) 2.5691 no . 1_554 H(30) H(20) 2.3699 no . 6_556 H(30) H(21) 2.5179 no . 6_556 #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 975890'