data_sa3111 _audit_creation_date 2013-12-26 _audit_creation_method ; Olex2 1.2 (compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736) ; _shelxl_version_number 2013-4 _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122 ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C44 H44 N4 S6' _chemical_formula_sum 'C44 H44 N4 S6' _chemical_formula_weight 821.19 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.593(4) _cell_length_b 20.307(6) _cell_length_c 15.212(4) _cell_angle_alpha 90 _cell_angle_beta 92.886(7) _cell_angle_gamma 90 _cell_volume 4502(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 11456 _cell_measurement_temperature 173.1500 _cell_measurement_theta_max 27.4827 _cell_measurement_theta_min 1.6740 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 0.338 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.4434 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrystalClear (Rigaku Inc., 2007)' _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.211 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 1728 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.1222 _diffrn_reflns_av_unetI/netI 0.1024 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 33562 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.200 _diffrn_reflns_theta_min 1.397 _diffrn_ambient_temperature 173.1500 _diffrn_detector_area_resol_mean 28.5714 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device ; Saturn724+ (2x2 bin mode) ; _diffrn_measurement_device_details ; AFC10: Fixed Chi 2 circle ; _diffrn_measurement_device_type 'Saturn724+ CCD' _diffrn_measurement_method dtprofit.ref _diffrn_number_total 10537 _diffrn_orient_matrix_type d*Trek _diffrn_orient_matrix_UB_11 -0.0397 _diffrn_orient_matrix_UB_12 0.0226 _diffrn_orient_matrix_UB_13 0.0511 _diffrn_orient_matrix_UB_21 0.0152 _diffrn_orient_matrix_UB_22 0.0460 _diffrn_orient_matrix_UB_23 -0.0086 _diffrn_orient_matrix_UB_31 -0.0515 _diffrn_orient_matrix_UB_32 0.0096 _diffrn_orient_matrix_UB_33 -0.0398 _diffrn_radiation_detector CCD _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Sealed Tube' _diffrn_source_current 30.0000 _diffrn_source_power 1.5000 _diffrn_source_voltage 50.0000 _diffrn_special_details ; ? ; _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 5171 _reflns_number_total 8093 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution ; 'XL (Sheldrick, 2008)' ; _refine_diff_density_max 0.862 _refine_diff_density_min -0.359 _refine_diff_density_rms 0.105 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 491 _refine_ls_number_reflns 8093 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2000 _refine_ls_R_factor_gt 0.1463 _refine_ls_restrained_S_all 1.153 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1408P)^2^+13.5050P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3347 _refine_ls_wR_factor_ref 0.3692 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B), C9(H9A,H9B), C27(H27A,H27B), C28(H28A, H28B), C30(H30A,H30B), C31(H31A,H31B) 2.b Aromatic/amide H refined with riding coordinates: C12(H12), C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C34(H34), C35(H35), C37(H37), C38(H38), C40(H40), C41(H41), C43(H43), C44(H44) 2.c Idealised Me refined as rotating group: C7(H7A,H7B,H7C), C10(H10A,H10B,H10C), C29(H29A,H29B,H29C), C32(H32A,H32B,H32C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.82408(17) 0.57084(16) 0.38596(17) 0.0716(8) Uani 1 1 d . . . . . S2 S 0.5618(2) 0.76629(13) 0.57713(18) 0.0712(8) Uani 1 1 d . . . . . S3 S 0.37473(14) 0.63370(13) 0.89815(15) 0.0535(6) Uani 1 1 d . . . . . S4 S 0.71418(16) 0.54491(14) 1.12935(17) 0.0651(7) Uani 1 1 d . . . . . S5 S 1.0059(2) 0.73754(15) 0.97372(18) 0.0791(9) Uani 1 1 d . . . . . S6 S 1.17068(17) 0.62712(15) 0.62743(16) 0.0666(8) Uani 1 1 d . . . . . N1 N 0.9933(5) 0.6154(4) 0.5857(4) 0.0531(19) Uani 1 1 d . . . . . N2 N 0.9182(5) 0.6038(3) 0.5335(4) 0.0476(17) Uani 1 1 d . . . . . N3 N 0.5494(4) 0.6054(3) 0.9334(4) 0.0403(15) Uani 1 1 d . . . . . N4 N 0.6248(5) 0.5863(3) 0.9847(4) 0.0497(17) Uani 1 1 d . . . . . C1 C 1.0741(6) 0.6087(5) 0.5556(6) 0.055(2) Uani 1 1 d . . . . . C2 C 1.0898(6) 0.5855(5) 0.4690(6) 0.062(3) Uani 1 1 d . . . . . C3 C 1.0117(6) 0.5688(5) 0.4174(6) 0.058(2) Uani 1 1 d . . . . . C4 C 0.9271(6) 0.5824(4) 0.4526(5) 0.054(2) Uani 1 1 d . . . . . C5 C 1.1875(7) 0.5837(6) 0.4397(6) 0.077(3) Uani 1 1 d . . . . . H5A H 1.2274 0.5676 0.4880 0.092 Uiso 1 1 calc R . . . . H5B H 1.1909 0.5527 0.3914 0.092 Uiso 1 1 calc R . . . . C6 C 1.2223(7) 0.6498(7) 0.4106(8) 0.093(4) Uani 1 1 d . . . . . H6A H 1.2156 0.6819 0.4572 0.112 Uiso 1 1 calc R . . . . H6B H 1.1861 0.6646 0.3591 0.112 Uiso 1 1 calc R . . . . C7 C 1.3228(9) 0.6449(10) 0.3888(11) 0.148(7) Uani 1 1 d . . . . . H7A H 1.3278 0.6201 0.3355 0.222 Uiso 1 1 calc GR . . . . H7B H 1.3567 0.6232 0.4361 0.222 Uiso 1 1 calc GR . . . . H7C H 1.3472 0.6883 0.3811 0.222 Uiso 1 1 calc GR . . . . C8 C 1.0135(8) 0.5307(5) 0.3264(7) 0.077(3) Uani 1 1 d . . . . . H8A H 1.0656 0.5011 0.3268 0.092 Uiso 1 1 calc R . . . . H8B H 0.9579 0.5049 0.3169 0.092 Uiso 1 1 calc R . . . . C9 C 1.0202(8) 0.5792(6) 0.2569(8) 0.090(4) Uani 1 1 d . . . . . H9A H 1.0746 0.6062 0.2667 0.108 Uiso 1 1 calc R . . . . H9B H 0.9667 0.6077 0.2538 0.108 Uiso 1 1 calc R . . . . C10 C 1.0260(13) 0.5360(8) 0.1666(8) 0.131(6) Uani 1 1 d . . . . . H10A H 1.0435 0.5641 0.1195 0.197 Uiso 1 1 calc GR . . . . H10B H 0.9671 0.5168 0.1516 0.197 Uiso 1 1 calc GR . . . . H10C H 1.0707 0.5016 0.1756 0.197 Uiso 1 1 calc GR . . . . C11 C 0.7470(6) 0.6234(5) 0.4419(6) 0.057(2) Uani 1 1 d . . . . . C12 C 0.7465(6) 0.6899(6) 0.4206(6) 0.066(3) Uani 1 1 d . . . . . H12 H 0.7845 0.7061 0.3783 0.079 Uiso 1 1 calc R . . . . C13 C 0.6877(6) 0.7323(5) 0.4638(5) 0.055(2) Uani 1 1 d . . . . . H13 H 0.6858 0.7769 0.4500 0.067 Uiso 1 1 calc R . . . . C14 C 0.6316(6) 0.7072(5) 0.5281(5) 0.055(2) Uani 1 1 d . . . . . C15 C 0.6374(7) 0.6409(4) 0.5512(6) 0.059(2) Uani 1 1 d . . . . . H15 H 0.6029 0.6246 0.5961 0.070 Uiso 1 1 calc R . . . . C16 C 0.6939(7) 0.6001(5) 0.5076(7) 0.071(3) Uani 1 1 d . . . . . H16 H 0.6967 0.5557 0.5225 0.085 Uiso 1 1 calc R . . . . C17 C 0.5378(6) 0.7451(4) 0.7514(5) 0.0452(19) Uani 1 1 d . . . . . H17 H 0.5838 0.7765 0.7604 0.054 Uiso 1 1 calc R . . . . C18 C 0.4937(6) 0.7185(4) 0.8233(6) 0.052(2) Uani 1 1 d . . . . . H18 H 0.5068 0.7342 0.8799 0.063 Uiso 1 1 calc R . . . . C19 C 0.4314(6) 0.6691(4) 0.8088(5) 0.0446(19) Uani 1 1 d . . . . . C20 C 0.4051(6) 0.6490(5) 0.7239(6) 0.059(2) Uani 1 1 d . . . . . H20 H 0.3613 0.6161 0.7153 0.071 Uiso 1 1 calc R . . . . C21 C 0.4442(7) 0.6779(5) 0.6516(6) 0.058(2) Uani 1 1 d . . . . . H21 H 0.4250 0.6661 0.5946 0.070 Uiso 1 1 calc R . . . . C22 C 0.5119(6) 0.7242(4) 0.6667(5) 0.052(2) Uani 1 1 d . . . . . C23 C 0.4684(5) 0.6032(4) 0.9662(5) 0.0450(19) Uani 1 1 d . . . . . C24 C 0.4501(6) 0.5775(4) 1.0500(5) 0.0443(19) Uani 1 1 d . . . . . C25 C 0.5269(5) 0.5558(4) 1.1017(5) 0.0424(19) Uani 1 1 d . . . . . C26 C 0.6120(6) 0.5653(4) 1.0661(6) 0.047(2) Uani 1 1 d . . . . . C27 C 0.3540(6) 0.5808(5) 1.0830(5) 0.053(2) Uani 1 1 d . . . . . H27A H 0.3103 0.5699 1.0351 0.063 Uiso 1 1 calc R . . . . H27B H 0.3481 0.5480 1.1289 0.063 Uiso 1 1 calc R . . . . C28 C 0.3310(7) 0.6473(5) 1.1188(7) 0.070(3) Uani 1 1 d . . . . . H28A H 0.3401 0.6804 1.0741 0.085 Uiso 1 1 calc R . . . . H28B H 0.3724 0.6571 1.1690 0.085 Uiso 1 1 calc R . . . . C29 C 0.2337(9) 0.6506(8) 1.1466(9) 0.116(5) Uani 1 1 d . . . . . H29A H 0.1924 0.6460 1.0958 0.174 Uiso 1 1 calc GR . . . . H29B H 0.2234 0.6922 1.1743 0.174 Uiso 1 1 calc GR . . . . H29C H 0.2231 0.6156 1.1873 0.174 Uiso 1 1 calc GR . . . . C30 C 0.5217(6) 0.5240(5) 1.1894(5) 0.051(2) Uani 1 1 d . . . . . H30A H 0.5714 0.4924 1.1966 0.061 Uiso 1 1 calc R . . . . H30B H 0.4645 0.4997 1.1903 0.061 Uiso 1 1 calc R . . . . C31 C 0.5271(8) 0.5714(5) 1.2685(6) 0.067(3) Uani 1 1 d . . . . . H31A H 0.4769 0.6027 1.2634 0.080 Uiso 1 1 calc R . . . . H31B H 0.5843 0.5957 1.2693 0.080 Uiso 1 1 calc R . . . . C32 C 0.5213(11) 0.5316(8) 1.3553(8) 0.113(5) Uani 1 1 d . . . . . H32A H 0.4669 0.5049 1.3524 0.169 Uiso 1 1 calc GR . . . . H32B H 0.5193 0.5614 1.4041 0.169 Uiso 1 1 calc GR . . . . H32C H 0.5743 0.5037 1.3631 0.169 Uiso 1 1 calc GR . . . . C33 C 0.7944(6) 0.5986(5) 1.0808(6) 0.054(2) Uani 1 1 d . . . . . C34 C 0.8401(6) 0.5789(5) 1.0090(6) 0.061(2) Uani 1 1 d . . . . . H34 H 0.8277 0.5380 0.9835 0.073 Uiso 1 1 calc R . . . . C35 C 0.9057(7) 0.6206(5) 0.9740(6) 0.067(3) Uani 1 1 d . . . . . H35 H 0.9365 0.6070 0.9251 0.081 Uiso 1 1 calc R . . . . C36 C 0.9250(6) 0.6808(5) 1.0107(6) 0.057(2) Uani 1 1 d . . . . . C37 C 0.8760(6) 0.6998(5) 1.0835(6) 0.059(2) Uani 1 1 d . . . . . H37 H 0.8865 0.7410 1.1086 0.071 Uiso 1 1 calc R . . . . C38 C 0.8148(6) 0.6600(5) 1.1172(6) 0.062(3) Uani 1 1 d . . . . . H38 H 0.7847 0.6735 1.1665 0.075 Uiso 1 1 calc R . . . . C39 C 1.0486(7) 0.7005(5) 0.8768(6) 0.059(2) Uani 1 1 d . . . . . C40 C 1.1048(7) 0.6481(5) 0.8794(6) 0.066(3) Uani 1 1 d . . . . . H40 H 1.1206 0.6280 0.9329 0.079 Uiso 1 1 calc R . . . . C41 C 1.1392(6) 0.6241(5) 0.8026(6) 0.059(2) Uani 1 1 d . . . . . H41 H 1.1758 0.5866 0.8045 0.071 Uiso 1 1 calc R . . . . C42 C 1.1201(5) 0.6550(5) 0.7240(5) 0.050(2) Uani 1 1 d . . . . . C43 C 1.0633(6) 0.7108(5) 0.7233(6) 0.059(2) Uani 1 1 d . . . . . H43 H 1.0495 0.7324 0.6703 0.070 Uiso 1 1 calc R . . . . C44 C 1.0281(6) 0.7340(5) 0.7982(6) 0.055(2) Uani 1 1 d . . . . . H44 H 0.9912 0.7714 0.7971 0.066 Uiso 1 1 calc R . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0592(15) 0.098(2) 0.0571(15) -0.0238(14) 0.0020(11) 0.0200(14) S2 0.0881(18) 0.0576(16) 0.0717(17) 0.0283(13) 0.0404(14) 0.0292(14) S3 0.0399(11) 0.0694(16) 0.0519(13) 0.0112(11) 0.0098(9) -0.0070(10) S4 0.0497(13) 0.0827(19) 0.0633(16) 0.0202(13) 0.0059(11) -0.0096(12) S5 0.0855(18) 0.083(2) 0.0716(18) -0.0352(15) 0.0345(14) -0.0430(16) S6 0.0568(14) 0.089(2) 0.0545(15) -0.0146(13) 0.0055(11) 0.0228(13) N1 0.063(5) 0.059(5) 0.037(4) 0.003(3) -0.001(3) 0.019(4) N2 0.059(4) 0.041(4) 0.043(4) 0.003(3) 0.012(3) 0.006(3) N3 0.040(3) 0.036(4) 0.046(4) -0.001(3) 0.019(3) -0.006(3) N4 0.060(4) 0.045(4) 0.044(4) -0.006(3) 0.000(3) -0.015(3) C1 0.048(5) 0.054(6) 0.064(6) 0.011(4) 0.013(4) 0.020(4) C2 0.064(6) 0.072(7) 0.051(5) 0.003(5) 0.013(4) 0.033(5) C3 0.060(5) 0.060(6) 0.053(5) -0.010(4) 0.004(4) 0.019(5) C4 0.075(6) 0.047(5) 0.040(5) -0.003(4) 0.003(4) 0.022(5) C5 0.073(7) 0.108(10) 0.050(6) -0.026(6) 0.003(5) 0.029(7) C6 0.062(7) 0.136(12) 0.083(8) 0.009(8) 0.024(6) 0.004(7) C7 0.083(9) 0.24(2) 0.126(13) -0.034(13) 0.056(9) -0.034(11) C8 0.075(7) 0.068(7) 0.089(8) 0.017(6) 0.012(6) 0.013(6) C9 0.072(7) 0.091(9) 0.107(9) 0.009(7) 0.012(6) 0.002(6) C10 0.195(17) 0.146(14) 0.054(8) -0.023(8) 0.010(9) 0.051(12) C11 0.054(5) 0.069(7) 0.048(5) 0.004(5) 0.006(4) 0.008(5) C12 0.062(6) 0.096(8) 0.040(5) 0.014(5) 0.010(4) 0.012(6) C13 0.043(4) 0.074(7) 0.049(5) 0.006(5) -0.004(4) 0.010(4) C14 0.047(5) 0.085(7) 0.032(4) 0.004(4) -0.002(4) 0.010(5) C15 0.074(6) 0.045(5) 0.057(6) 0.011(4) 0.015(5) 0.020(5) C16 0.096(8) 0.051(6) 0.066(6) 0.011(5) 0.004(6) 0.026(6) C17 0.056(5) 0.019(4) 0.060(5) 0.001(3) 0.002(4) 0.008(3) C18 0.078(6) 0.038(5) 0.042(5) -0.003(4) 0.009(4) -0.015(4) C19 0.054(5) 0.037(5) 0.044(5) -0.002(4) 0.012(4) -0.006(4) C20 0.050(5) 0.076(7) 0.049(6) 0.020(5) -0.008(4) -0.004(5) C21 0.071(6) 0.061(6) 0.043(5) 0.003(4) -0.001(4) 0.013(5) C22 0.070(6) 0.041(5) 0.045(5) 0.014(4) -0.002(4) 0.026(4) C23 0.049(5) 0.036(4) 0.050(5) -0.010(4) 0.000(4) -0.007(4) C24 0.056(5) 0.027(4) 0.051(5) -0.003(3) 0.011(4) -0.008(4) C25 0.041(4) 0.024(4) 0.064(5) 0.006(4) 0.018(4) -0.011(3) C26 0.057(5) 0.034(5) 0.050(5) 0.000(4) 0.006(4) -0.007(4) C27 0.046(5) 0.068(6) 0.044(5) 0.005(4) 0.003(4) -0.008(4) C28 0.079(7) 0.075(7) 0.060(6) 0.013(5) 0.036(5) 0.008(6) C29 0.106(10) 0.152(14) 0.092(10) -0.004(9) 0.029(8) 0.015(10) C30 0.055(5) 0.063(6) 0.035(4) 0.012(4) 0.002(4) -0.018(4) C31 0.089(7) 0.061(6) 0.053(6) 0.006(5) 0.017(5) -0.007(5) C32 0.137(12) 0.129(13) 0.073(8) -0.010(8) 0.010(8) -0.018(10) C33 0.040(4) 0.078(7) 0.044(5) 0.006(5) -0.003(4) -0.010(4) C34 0.056(5) 0.077(7) 0.049(5) -0.006(5) -0.007(4) -0.006(5) C35 0.066(6) 0.077(7) 0.061(6) -0.013(5) 0.027(5) -0.023(5) C36 0.038(4) 0.080(7) 0.053(5) -0.008(5) 0.006(4) -0.012(4) C37 0.052(5) 0.066(6) 0.060(6) -0.007(5) 0.016(4) -0.006(5) C38 0.036(4) 0.106(9) 0.045(5) -0.008(5) 0.004(4) -0.015(5) C39 0.066(6) 0.069(7) 0.045(5) -0.007(5) 0.020(4) -0.016(5) C40 0.075(6) 0.073(7) 0.051(6) -0.007(5) 0.002(5) 0.005(6) C41 0.061(6) 0.067(6) 0.049(6) 0.003(5) -0.007(4) 0.016(5) C42 0.030(4) 0.073(6) 0.048(5) -0.017(4) 0.011(3) -0.002(4) C43 0.067(6) 0.057(6) 0.051(5) 0.001(4) 0.003(4) 0.004(5) C44 0.048(5) 0.055(6) 0.064(6) -0.027(5) 0.015(4) -0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C4 1.786(9) . ? S1 C11 1.796(9) . ? S2 C14 1.764(9) . ? S2 C22 1.794(9) . ? S3 C19 1.778(8) . ? S3 C23 1.784(8) . ? S4 C26 1.782(9) . ? S4 C33 1.788(9) . ? S5 C36 1.762(9) . ? S5 C39 1.794(9) . ? S6 C1 1.779(10) . ? S6 C42 1.770(8) . ? N1 N2 1.341(9) . ? N1 C1 1.294(11) . ? N2 C4 1.318(10) . ? N3 N4 1.373(9) . ? N3 C23 1.307(10) . ? N4 C26 1.331(10) . ? C1 C2 1.428(13) . ? C2 C3 1.394(13) . ? C2 C5 1.516(13) . ? C3 C4 1.398(12) . ? C3 C8 1.587(14) . ? C5 C6 1.510(17) . ? C6 C7 1.523(15) . ? C8 C9 1.453(15) . ? C9 C10 1.636(17) . ? C11 C12 1.390(14) . ? C11 C16 1.379(13) . ? C12 C13 1.403(13) . ? C13 C14 1.401(12) . ? C14 C15 1.392(13) . ? C15 C16 1.365(13) . ? C17 C18 1.405(11) . ? C17 C22 1.392(12) . ? C18 C19 1.364(11) . ? C19 C20 1.389(12) . ? C20 C21 1.394(12) . ? C21 C22 1.375(13) . ? C23 C24 1.415(11) . ? C24 C25 1.407(11) . ? C24 C27 1.515(11) . ? C25 C26 1.393(11) . ? C25 C30 1.487(11) . ? C27 C28 1.500(13) . ? C28 C29 1.504(15) . ? C30 C31 1.540(13) . ? C31 C32 1.554(15) . ? C33 C34 1.368(13) . ? C33 C38 1.389(13) . ? C34 C35 1.402(13) . ? C35 C36 1.367(13) . ? C36 C37 1.404(12) . ? C37 C38 1.326(12) . ? C39 C40 1.343(14) . ? C39 C44 1.396(13) . ? C40 C41 1.384(13) . ? C41 C42 1.367(12) . ? C42 C43 1.403(12) . ? C43 C44 1.358(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 S1 C11 100.5(4) . . ? C14 S2 C22 105.2(4) . . ? C19 S3 C23 102.2(4) . . ? C26 S4 C33 100.5(4) . . ? C36 S5 C39 104.7(4) . . ? C42 S6 C1 103.1(4) . . ? C1 N1 N2 120.3(7) . . ? C4 N2 N1 119.6(7) . . ? C23 N3 N4 119.1(7) . . ? C26 N4 N3 118.3(7) . . ? N1 C1 S6 118.0(7) . . ? N1 C1 C2 123.5(9) . . ? C2 C1 S6 118.5(7) . . ? C1 C2 C5 118.5(9) . . ? C3 C2 C1 115.8(8) . . ? C3 C2 C5 125.7(8) . . ? C2 C3 C4 116.7(8) . . ? C2 C3 C8 124.2(8) . . ? C4 C3 C8 118.9(8) . . ? N2 C4 S1 116.9(7) . . ? N2 C4 C3 123.6(8) . . ? C3 C4 S1 119.4(7) . . ? C6 C5 C2 113.5(9) . . ? C5 C6 C7 110.3(12) . . ? C9 C8 C3 108.0(9) . . ? C8 C9 C10 104.8(11) . . ? C12 C11 S1 117.6(7) . . ? C16 C11 S1 121.8(8) . . ? C16 C11 C12 120.5(9) . . ? C11 C12 C13 118.9(9) . . ? C14 C13 C12 119.8(9) . . ? C13 C14 S2 114.7(8) . . ? C15 C14 S2 125.4(7) . . ? C15 C14 C13 119.8(9) . . ? C16 C15 C14 119.7(9) . . ? C15 C16 C11 121.2(9) . . ? C22 C17 C18 119.3(8) . . ? C19 C18 C17 119.1(8) . . ? C18 C19 S3 120.4(6) . . ? C18 C19 C20 121.1(8) . . ? C20 C19 S3 118.3(6) . . ? C19 C20 C21 120.4(9) . . ? C22 C21 C20 118.4(8) . . ? C17 C22 S2 117.1(7) . . ? C21 C22 S2 121.0(7) . . ? C21 C22 C17 121.5(8) . . ? N3 C23 S3 116.6(6) . . ? N3 C23 C24 124.9(8) . . ? C24 C23 S3 118.5(6) . . ? C23 C24 C27 120.2(8) . . ? C25 C24 C23 115.9(7) . . ? C25 C24 C27 123.6(7) . . ? C24 C25 C30 124.2(7) . . ? C26 C25 C24 116.1(7) . . ? C26 C25 C30 119.7(8) . . ? N4 C26 S4 115.1(6) . . ? N4 C26 C25 125.1(8) . . ? C25 C26 S4 119.7(7) . . ? C28 C27 C24 112.7(7) . . ? C27 C28 C29 111.9(10) . . ? C25 C30 C31 115.3(7) . . ? C30 C31 C32 109.7(9) . . ? C34 C33 S4 120.4(8) . . ? C34 C33 C38 118.6(9) . . ? C38 C33 S4 120.9(7) . . ? C33 C34 C35 119.6(9) . . ? C36 C35 C34 121.1(9) . . ? C35 C36 S5 125.7(7) . . ? C35 C36 C37 117.7(9) . . ? C37 C36 S5 116.6(7) . . ? C38 C37 C36 121.1(10) . . ? C37 C38 C33 121.9(9) . . ? C40 C39 S5 123.0(8) . . ? C40 C39 C44 121.0(8) . . ? C44 C39 S5 115.6(8) . . ? C39 C40 C41 120.1(9) . . ? C42 C41 C40 120.7(9) . . ? C41 C42 S6 120.2(7) . . ? C41 C42 C43 118.2(8) . . ? C43 C42 S6 121.5(7) . . ? C44 C43 C42 121.5(9) . . ? C43 C44 C39 118.5(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S1 C11 C12 C13 -179.4(6) . . . . ? S1 C11 C16 C15 178.2(8) . . . . ? S2 C14 C15 C16 179.7(8) . . . . ? S3 C19 C20 C21 176.6(7) . . . . ? S3 C23 C24 C25 -178.4(6) . . . . ? S3 C23 C24 C27 -4.4(10) . . . . ? S4 C33 C34 C35 -177.3(7) . . . . ? S4 C33 C38 C37 178.2(7) . . . . ? S5 C36 C37 C38 -178.7(7) . . . . ? S5 C39 C40 C41 -176.5(8) . . . . ? S5 C39 C44 C43 176.0(7) . . . . ? S6 C1 C2 C3 176.9(7) . . . . ? S6 C1 C2 C5 -5.5(13) . . . . ? S6 C42 C43 C44 -176.8(7) . . . . ? N1 N2 C4 S1 -177.9(6) . . . . ? N1 N2 C4 C3 2.0(13) . . . . ? N1 C1 C2 C3 -1.3(14) . . . . ? N1 C1 C2 C5 176.4(9) . . . . ? N2 N1 C1 S6 178.2(6) . . . . ? N2 N1 C1 C2 -3.6(14) . . . . ? N3 N4 C26 S4 -177.4(5) . . . . ? N3 N4 C26 C25 5.7(12) . . . . ? N3 C23 C24 C25 2.9(12) . . . . ? N3 C23 C24 C27 176.9(8) . . . . ? N4 N3 C23 S3 176.1(5) . . . . ? N4 N3 C23 C24 -5.1(12) . . . . ? C1 S6 C42 C41 122.1(8) . . . . ? C1 S6 C42 C43 -61.0(8) . . . . ? C1 N1 N2 C4 3.2(12) . . . . ? C1 C2 C3 C4 6.0(13) . . . . ? C1 C2 C3 C8 -168.9(9) . . . . ? C1 C2 C5 C6 -79.9(12) . . . . ? C2 C3 C4 S1 173.2(7) . . . . ? C2 C3 C4 N2 -6.7(14) . . . . ? C2 C3 C8 C9 -89.1(12) . . . . ? C2 C5 C6 C7 175.8(10) . . . . ? C3 C2 C5 C6 97.4(13) . . . . ? C3 C8 C9 C10 177.7(10) . . . . ? C4 S1 C11 C12 84.4(8) . . . . ? C4 S1 C11 C16 -91.7(9) . . . . ? C4 C3 C8 C9 96.0(11) . . . . ? C5 C2 C3 C4 -171.4(10) . . . . ? C5 C2 C3 C8 13.6(16) . . . . ? C8 C3 C4 S1 -11.6(12) . . . . ? C8 C3 C4 N2 168.5(8) . . . . ? C11 S1 C4 N2 21.6(8) . . . . ? C11 S1 C4 C3 -158.4(8) . . . . ? C11 C12 C13 C14 0.8(13) . . . . ? C12 C11 C16 C15 2.3(15) . . . . ? C12 C13 C14 S2 179.7(7) . . . . ? C12 C13 C14 C15 2.7(13) . . . . ? C13 C14 C15 C16 -3.7(14) . . . . ? C14 S2 C22 C17 113.7(7) . . . . ? C14 S2 C22 C21 -72.7(8) . . . . ? C14 C15 C16 C11 1.2(15) . . . . ? C16 C11 C12 C13 -3.2(14) . . . . ? C17 C18 C19 S3 179.6(6) . . . . ? C17 C18 C19 C20 -5.7(13) . . . . ? C18 C17 C22 S2 173.5(6) . . . . ? C18 C17 C22 C21 -0.1(12) . . . . ? C18 C19 C20 C21 1.8(14) . . . . ? C19 S3 C23 N3 -8.1(7) . . . . ? C19 S3 C23 C24 173.1(6) . . . . ? C19 C20 C21 C22 3.0(13) . . . . ? C20 C21 C22 S2 -177.1(7) . . . . ? C20 C21 C22 C17 -3.7(13) . . . . ? C22 S2 C14 C13 -171.4(6) . . . . ? C22 S2 C14 C15 5.4(9) . . . . ? C22 C17 C18 C19 4.9(12) . . . . ? C23 S3 C19 C18 -59.3(8) . . . . ? C23 S3 C19 C20 125.9(7) . . . . ? C23 N3 N4 C26 0.9(10) . . . . ? C23 C24 C25 C26 3.2(11) . . . . ? C23 C24 C25 C30 -176.6(7) . . . . ? C23 C24 C27 C28 -79.7(10) . . . . ? C24 C25 C26 S4 175.6(6) . . . . ? C24 C25 C26 N4 -7.7(12) . . . . ? C24 C25 C30 C31 -90.6(10) . . . . ? C24 C27 C28 C29 176.8(9) . . . . ? C25 C24 C27 C28 93.9(10) . . . . ? C25 C30 C31 C32 -179.7(9) . . . . ? C26 S4 C33 C34 -88.1(8) . . . . ? C26 S4 C33 C38 94.8(8) . . . . ? C26 C25 C30 C31 89.6(10) . . . . ? C27 C24 C25 C26 -170.6(8) . . . . ? C27 C24 C25 C30 9.6(13) . . . . ? C30 C25 C26 S4 -4.6(11) . . . . ? C30 C25 C26 N4 172.1(8) . . . . ? C33 S4 C26 N4 28.5(7) . . . . ? C33 S4 C26 C25 -154.4(7) . . . . ? C33 C34 C35 C36 0.1(15) . . . . ? C34 C33 C38 C37 1.0(14) . . . . ? C34 C35 C36 S5 179.7(7) . . . . ? C34 C35 C36 C37 -1.0(15) . . . . ? C35 C36 C37 C38 1.9(14) . . . . ? C36 S5 C39 C40 -72.2(9) . . . . ? C36 S5 C39 C44 114.7(7) . . . . ? C36 C37 C38 C33 -1.9(15) . . . . ? C38 C33 C34 C35 -0.1(13) . . . . ? C39 S5 C36 C35 3.5(10) . . . . ? C39 S5 C36 C37 -175.9(7) . . . . ? C39 C40 C41 C42 3.0(15) . . . . ? C40 C39 C44 C43 2.6(14) . . . . ? C40 C41 C42 S6 175.8(7) . . . . ? C40 C41 C42 C43 -1.2(14) . . . . ? C41 C42 C43 C44 0.1(13) . . . . ? C42 S6 C1 N1 -2.9(9) . . . . ? C42 S6 C1 C2 178.8(8) . . . . ? C42 C43 C44 C39 -0.8(14) . . . . ? C44 C39 C40 C41 -3.7(15) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.236 0.386 0.246 102 42 ' ' 2 0.236 0.114 0.746 102 42 ' ' 3 0.764 0.886 0.254 102 42 ' ' 4 0.764 0.614 0.754 102 43 ' ' _shelx_res_file ; TITL sa3111 in P2(1)/c CELL 0.71073 14.5934 20.307 15.2121 90 92.886 90 ZERR 4 0.0044 0.0062 0.0038 0 0.007 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N S UNIT 176 176 16 24 L.S. 4 PLAN 20 BOND fmap 2 MORE -1 ACTA CONF OMIT -2 50.4 OMIT 0 2 1 OMIT 1 1 0 OMIT 1 1 1 OMIT -1 1 1 OMIT 0 1 1 OMIT 4 6 5 REM D:/D/SXRD/sa(3100-3199)/sa3111/sa3111.hkl WGHT 0.140800 13.505000 FVAR 27.89580 S1 4 0.824081 0.570842 0.385964 11.00000 0.05923 0.09832 = 0.05708 -0.02378 0.00204 0.01998 S2 4 0.561820 0.766285 0.577132 11.00000 0.08814 0.05759 = 0.07166 0.02829 0.04038 0.02920 S3 4 0.374731 0.633696 0.898151 11.00000 0.03985 0.06942 = 0.05192 0.01124 0.00979 -0.00699 S4 4 0.714180 0.544906 1.129353 11.00000 0.04965 0.08270 = 0.06333 0.02022 0.00594 -0.00961 S5 4 1.005920 0.737535 0.973716 11.00000 0.08550 0.08315 = 0.07160 -0.03515 0.03448 -0.04304 S6 4 1.170684 0.627123 0.627430 11.00000 0.05681 0.08860 = 0.05453 -0.01460 0.00555 0.02277 N1 3 0.993263 0.615430 0.585655 11.00000 0.06305 0.05885 = 0.03720 0.00339 -0.00050 0.01860 N2 3 0.918159 0.603824 0.533477 11.00000 0.05905 0.04140 = 0.04340 0.00319 0.01235 0.00555 N3 3 0.549431 0.605370 0.933373 11.00000 0.03987 0.03624 = 0.04643 -0.00088 0.01936 -0.00558 N4 3 0.624794 0.586252 0.984720 11.00000 0.06019 0.04484 = 0.04384 -0.00592 -0.00013 -0.01457 C1 1 1.074113 0.608667 0.555636 11.00000 0.04790 0.05357 = 0.06352 0.01075 0.01285 0.01973 C2 1 1.089847 0.585510 0.469050 11.00000 0.06377 0.07189 = 0.05095 0.00273 0.01254 0.03322 C3 1 1.011721 0.568751 0.417409 11.00000 0.06022 0.05961 = 0.05297 -0.00950 0.00414 0.01891 C4 1 0.927125 0.582410 0.452573 11.00000 0.07516 0.04716 = 0.04028 -0.00313 0.00276 0.02180 C5 1 1.187545 0.583658 0.439742 11.00000 0.07282 0.10825 = 0.04970 -0.02575 0.00275 0.02928 AFIX 23 H5A 2 1.227439 0.567607 0.487993 11.00000 -1.20000 H5B 2 1.190923 0.552722 0.391428 11.00000 -1.20000 AFIX 0 C6 1 1.222268 0.649830 0.410627 11.00000 0.06200 0.13642 = 0.08260 0.00904 0.02397 0.00390 AFIX 23 H6A 2 1.215648 0.681870 0.457173 11.00000 -1.20000 H6B 2 1.186080 0.664638 0.359148 11.00000 -1.20000 AFIX 0 C7 1 1.322766 0.644902 0.388808 11.00000 0.08299 0.24010 = 0.12639 -0.03396 0.05572 -0.03380 AFIX 137 H7A 2 1.327759 0.620143 0.335503 11.00000 -1.50000 H7B 2 1.356717 0.623150 0.436070 11.00000 -1.50000 H7C 2 1.347161 0.688307 0.381101 11.00000 -1.50000 AFIX 0 C8 1 1.013462 0.530681 0.326404 11.00000 0.07521 0.06773 = 0.08857 0.01733 0.01247 0.01257 AFIX 23 H8A 2 1.065635 0.501068 0.326797 11.00000 -1.20000 H8B 2 0.957903 0.504892 0.316855 11.00000 -1.20000 AFIX 0 C9 1 1.020155 0.579243 0.256852 11.00000 0.07219 0.09114 = 0.10679 0.00890 0.01164 0.00193 AFIX 23 H9A 2 1.074622 0.606161 0.266656 11.00000 -1.20000 H9B 2 0.966664 0.607661 0.253806 11.00000 -1.20000 AFIX 0 C10 1 1.025964 0.535961 0.166584 11.00000 0.19459 0.14639 = 0.05366 -0.02312 0.00959 0.05077 AFIX 137 H10A 2 1.043510 0.564059 0.119545 11.00000 -1.50000 H10B 2 0.967101 0.516789 0.151618 11.00000 -1.50000 H10C 2 1.070688 0.501641 0.175624 11.00000 -1.50000 AFIX 0 C11 1 0.746981 0.623410 0.441916 11.00000 0.05360 0.06913 = 0.04801 0.00372 0.00571 0.00790 C12 1 0.746499 0.689947 0.420580 11.00000 0.06153 0.09646 = 0.03960 0.01426 0.01030 0.01236 AFIX 43 H12 2 0.784541 0.706121 0.378339 11.00000 -1.20000 AFIX 0 C13 1 0.687651 0.732293 0.463847 11.00000 0.04336 0.07374 = 0.04863 0.00642 -0.00416 0.00953 AFIX 43 H13 2 0.685829 0.776890 0.449962 11.00000 -1.20000 AFIX 0 C14 1 0.631606 0.707184 0.528072 11.00000 0.04749 0.08513 = 0.03204 0.00359 -0.00151 0.00975 C15 1 0.637408 0.640949 0.551196 11.00000 0.07433 0.04510 = 0.05743 0.01122 0.01493 0.02011 AFIX 43 H15 2 0.602942 0.624613 0.596130 11.00000 -1.20000 AFIX 0 C16 1 0.693911 0.600076 0.507631 11.00000 0.09561 0.05081 = 0.06556 0.01124 0.00393 0.02568 AFIX 43 H16 2 0.696668 0.555680 0.522538 11.00000 -1.20000 AFIX 0 C17 1 0.537827 0.745142 0.751433 11.00000 0.05585 0.01926 = 0.06039 0.00075 0.00233 0.00840 AFIX 43 H17 2 0.583847 0.776460 0.760409 11.00000 -1.20000 AFIX 0 C18 1 0.493699 0.718457 0.823255 11.00000 0.07819 0.03790 = 0.04164 -0.00258 0.00933 -0.01550 AFIX 43 H18 2 0.506803 0.734232 0.879892 11.00000 -1.20000 AFIX 0 C19 1 0.431368 0.669094 0.808806 11.00000 0.05424 0.03691 = 0.04369 -0.00200 0.01165 -0.00590 C20 1 0.405146 0.649003 0.723944 11.00000 0.05034 0.07613 = 0.04889 0.01999 -0.00800 -0.00379 AFIX 43 H20 2 0.361272 0.616107 0.715339 11.00000 -1.20000 AFIX 0 C21 1 0.444234 0.677879 0.651611 11.00000 0.07118 0.06070 = 0.04297 0.00310 -0.00064 0.01309 AFIX 43 H21 2 0.425000 0.666101 0.594551 11.00000 -1.20000 AFIX 0 C22 1 0.511914 0.724194 0.666698 11.00000 0.06969 0.04060 = 0.04468 0.01396 -0.00168 0.02582 C23 1 0.468435 0.603196 0.966222 11.00000 0.04943 0.03580 = 0.04953 -0.01045 -0.00019 -0.00666 C24 1 0.450112 0.577540 1.050029 11.00000 0.05583 0.02665 = 0.05139 -0.00276 0.01143 -0.00820 C25 1 0.526923 0.555789 1.101682 11.00000 0.04075 0.02397 = 0.06396 0.00565 0.01764 -0.01076 C26 1 0.612012 0.565298 1.066070 11.00000 0.05673 0.03422 = 0.05040 0.00044 0.00643 -0.00656 C27 1 0.354000 0.580752 1.083028 11.00000 0.04587 0.06799 = 0.04440 0.00463 0.00289 -0.00777 AFIX 23 H27A 2 0.310260 0.569920 1.035083 11.00000 -1.20000 H27B 2 0.348068 0.548037 1.128854 11.00000 -1.20000 AFIX 0 C28 1 0.331038 0.647272 1.118799 11.00000 0.07876 0.07542 = 0.06039 0.01303 0.03550 0.00841 AFIX 23 H28A 2 0.340060 0.680390 1.074105 11.00000 -1.20000 H28B 2 0.372422 0.657114 1.168977 11.00000 -1.20000 AFIX 0 C29 1 0.233692 0.650586 1.146563 11.00000 0.10576 0.15182 = 0.09192 -0.00391 0.02893 0.01536 AFIX 137 H29A 2 0.192395 0.646002 1.095787 11.00000 -1.50000 H29B 2 0.223426 0.692223 1.174288 11.00000 -1.50000 H29C 2 0.223112 0.615647 1.187338 11.00000 -1.50000 AFIX 0 C30 1 0.521709 0.524029 1.189372 11.00000 0.05492 0.06324 = 0.03525 0.01156 0.00244 -0.01798 AFIX 23 H30A 2 0.571386 0.492445 1.196570 11.00000 -1.20000 H30B 2 0.464545 0.499723 1.190277 11.00000 -1.20000 AFIX 0 C31 1 0.527057 0.571362 1.268536 11.00000 0.08874 0.06084 = 0.05261 0.00635 0.01671 -0.00667 AFIX 23 H31A 2 0.476903 0.602692 1.263353 11.00000 -1.20000 H31B 2 0.584284 0.595704 1.269329 11.00000 -1.20000 AFIX 0 C32 1 0.521331 0.531558 1.355349 11.00000 0.13713 0.12878 = 0.07284 -0.01041 0.01019 -0.01832 AFIX 137 H32A 2 0.466905 0.504933 1.352427 11.00000 -1.50000 H32B 2 0.519251 0.561425 1.404126 11.00000 -1.50000 H32C 2 0.574298 0.503731 1.363118 11.00000 -1.50000 AFIX 0 C33 1 0.794419 0.598640 1.080766 11.00000 0.04040 0.07806 = 0.04364 0.00568 -0.00339 -0.01001 C34 1 0.840070 0.578866 1.008970 11.00000 0.05562 0.07712 = 0.04925 -0.00550 -0.00676 -0.00602 AFIX 43 H34 2 0.827684 0.537996 0.983470 11.00000 -1.20000 AFIX 0 C35 1 0.905652 0.620562 0.974031 11.00000 0.06611 0.07713 = 0.06130 -0.01332 0.02675 -0.02252 AFIX 43 H35 2 0.936492 0.607035 0.925138 11.00000 -1.20000 AFIX 0 C36 1 0.924998 0.680764 1.010654 11.00000 0.03846 0.07973 = 0.05298 -0.00792 0.00599 -0.01193 C37 1 0.875953 0.699801 1.083516 11.00000 0.05158 0.06594 = 0.06030 -0.00721 0.01599 -0.00596 AFIX 43 H37 2 0.886506 0.741042 1.108611 11.00000 -1.20000 AFIX 0 C38 1 0.814815 0.659959 1.117168 11.00000 0.03559 0.10633 = 0.04532 -0.00804 0.00436 -0.01530 AFIX 43 H38 2 0.784747 0.673458 1.166538 11.00000 -1.20000 AFIX 0 C39 1 1.048647 0.700542 0.876848 11.00000 0.06643 0.06852 = 0.04516 -0.00699 0.01953 -0.01553 C40 1 1.104826 0.648145 0.879437 11.00000 0.07457 0.07276 = 0.05072 -0.00750 0.00152 0.00516 AFIX 43 H40 2 1.120631 0.627952 0.932941 11.00000 -1.20000 AFIX 0 C41 1 1.139239 0.624149 0.802619 11.00000 0.06076 0.06689 = 0.04898 0.00328 -0.00689 0.01599 AFIX 43 H41 2 1.175792 0.586611 0.804495 11.00000 -1.20000 AFIX 0 C42 1 1.120069 0.655044 0.723983 11.00000 0.03028 0.07340 = 0.04755 -0.01711 0.01084 -0.00181 C43 1 1.063335 0.710821 0.723259 11.00000 0.06700 0.05731 = 0.05144 0.00095 0.00311 0.00439 AFIX 43 H43 2 1.049530 0.732383 0.670304 11.00000 -1.20000 AFIX 0 C44 1 1.028125 0.734026 0.798182 11.00000 0.04773 0.05549 = 0.06419 -0.02651 0.01511 -0.00792 AFIX 43 H44 2 0.991191 0.771368 0.797100 11.00000 -1.20000 AFIX 0 HKLF 4 REM sa3111 in P2(1)/c REM R1 = 0.1463 for 5171 Fo > 4sig(Fo) and 0.2000 for all 8093 data REM 491 parameters refined using 0 restraints END WGHT 0.1408 13.5157 REM Highest difference peak 0.862, deepest hole -0.359, 1-sigma level 0.105 Q1 1 0.6665 0.5744 1.1151 11.00000 0.05 0.86 Q2 1 0.7626 0.5488 0.3651 11.00000 0.05 0.83 Q3 1 0.9314 0.7655 0.9296 11.00000 0.05 0.82 Q4 1 0.4827 0.7375 0.5224 11.00000 0.05 0.77 Q5 1 0.3139 0.6310 0.8754 11.00000 0.05 0.70 Q6 1 1.1169 0.6258 0.6044 11.00000 0.05 0.69 Q7 1 0.6221 0.7056 0.4162 11.00000 0.05 0.43 Q8 1 0.7837 0.5994 0.9937 11.00000 0.05 0.42 Q9 1 0.8375 0.5616 0.4173 11.00000 0.05 0.42 Q10 1 0.3909 0.6013 0.8987 11.00000 0.05 0.41 Q11 1 0.7432 0.5544 1.1273 11.00000 0.05 0.39 Q12 1 0.5759 0.6185 0.5187 11.00000 0.05 0.38 Q13 1 0.8655 0.5905 0.5249 11.00000 0.05 0.38 Q14 1 0.7658 0.6631 1.0838 11.00000 0.05 0.37 Q15 1 0.8340 0.6365 0.9463 11.00000 0.05 0.37 Q16 1 0.5913 0.6878 0.4967 11.00000 0.05 0.36 Q17 1 0.9511 0.5605 0.4035 11.00000 0.05 0.36 Q18 1 0.3351 0.6368 0.7169 11.00000 0.05 0.36 Q19 1 1.0639 0.6261 0.5632 11.00000 0.05 0.36 Q20 1 1.1539 0.5831 0.6348 11.00000 0.05 0.35 ; _shelx_res_checksum 53759 _shelx_hkl_file ; 0 0 417523368 107240 -0.00503 0.01490 0.99554-0.99554 0.09411 0.09305 996915 104.49 -2.07 1.0000 0 0 -416197687 110105 -0.84781 0.83807 0.52796-0.52796-0.04972-0.13740 693856 104.49 2.07 1.0000 0 0 -418055058 163382 -0.53228 0.52235 0.84401-0.84401-0.06566-0.12162 1118399 104.49 2.07 1.0000 0 0 416700734 143464 -0.65337 0.66337 0.74599-0.74599 0.12877 0.05844 807617 104.49 -2.07 1.0000 0 0 611425480 451459 0.29418-0.27960 0.94748-0.94748 0.12543 0.1552530661510 -70.62 2.21 1.0000 0 0 -610021388 419409 -0.96633 0.95198 0.24053-0.24053-0.09129-0.1893828336782 -70.62 -2.21 1.0000 0 0 -611476038 493367 -0.49602 0.48111 0.86072-0.86072-0.11453-0.1663830749382 -70.62 -2.21 1.0000 0 0 611184714 481625 -0.67786 0.69286 0.71355-0.71355 0.17702 0.1038130266240 -70.62 2.21 1.0000 0 0 -8 1151317 241793 -0.45721 0.43736 0.87418-0.87418-0.16355-0.21097 6478865 48.13 2.91 1.0000 0 0 8 1335039 224758 -0.69989 0.71989 0.67782-0.67782 0.22514 0.14930 6894937 48.13 -2.91 1.0000 0 0 -10 489525 69618 -0.41592 0.39111 0.88417-0.88417-0.21268-0.25546 65349 -30.69 -4.59 1.0000 0 0 10 423378 56345 -0.71928 0.74426 0.63880-0.63880 0.27303 0.19493 98991 -30.69 4.59 1.0000 0 0 -12 749913 82641 -0.37192 0.34214 0.89053-0.89053-0.26196-0.29981 140119 18.57 6.55 1.0000 0 0 -14 287870 197863 -0.32500 0.29026 0.89297-0.89297-0.31139-0.34401 800000 -10.81 -7.30 1.0000 0 0 -16 16818 79449 -0.27540 0.23584 0.89102-0.89102-0.36086-0.38788 99183 5.05 5.59 1.0000 0 0 -18 69126 88355 -0.22176 0.17726 0.88442-0.88442-0.41063-0.43171 104064 -1.42 -2.43 1.0000 0 1 1 8874 8057 -0.96709 0.96948 0.23731-0.20228-0.09169 0.13847 13166 -0.67 -0.11 1.0000 0 -1 -1 10580 7896 -0.98286 0.98044 0.15412-0.18913-0.10114 0.05437 15222 -0.67 0.11 1.0000 0 1 -1 5751 4401 -0.97129 0.96901-0.19551 0.23051-0.13551 0.08876 6435 -0.22 0.65 1.0000 0 -1 1 11439 7233 -0.94320 0.94548-0.30022 0.26522-0.14222 0.18896 12600 -0.22 -0.65 1.0000 0 -1 -1 1303 7427 0.06165-0.06412 0.77948-0.81451-0.62338 0.57658 3193 -0.67 0.11 1.0000 0 1 1 24244 10138 -0.01310 0.01557 0.81797-0.78294-0.57510 0.62190 31071 -0.67 -0.11 1.0000 0 1 -1 432 9978 -0.75620 0.75371 0.52197-0.48693 0.39457-0.44137 -12445 -0.22 0.65 1.0000 0 -1 1 27917 12060 -0.76385 0.76635 0.47714-0.51217 0.43457-0.38778 29940 -0.22 -0.65 1.0000 0 1 2 59361 16812 -0.89644 0.90130 0.43849-0.40346-0.06411 0.15767 5016 -5.65 0.34 1.0000 0 -1 -2 163310 15328 -0.96763 0.96284 0.23501-0.27004-0.09197-0.00157 53522 -5.65 -0.34 1.0000 0 1 -2 161281 10214 -0.91918 0.91495-0.36480 0.39980-0.14840 0.05495 42640 6.39 0.14 1.0000 0 -1 2 203762 24945 -0.74811 0.75230-0.64526 0.61025-0.15480 0.24823 65719 6.39 -0.14 1.0000 0 -1 -2 69863 14141 -0.26290 0.25795 0.88990-0.92494-0.37276 0.27917 8364 -5.65 -0.34 1.0000 0 1 2 220018 37109 -0.37374 0.37870 0.89034-0.85529-0.25998 0.35361 87890 -5.65 0.34 1.0000 0 1 -2 175418 23319 -0.70410 0.69910 0.67009-0.63504 0.23497-0.32858 50054 6.39 0.14 1.0000 0 -1 2 233813 41846 -0.73485 0.73985 0.59950-0.63454 0.31712-0.22353 83234 6.39 -0.14 1.0000 0 1 -3 232949 72262 0.38597-0.39326 0.91285-0.87781 0.13311-0.27345 242009 0.29 -1.09 1.0000 0 1 3 123724 57345 -0.79360 0.80089 0.60739-0.57235-0.03562 0.17596 135819 0.55 -0.04 1.0000 0 -1 -3 187335 63782 -0.96256 0.95539 0.25587-0.29090-0.08937-0.05096 202148 0.55 0.04 1.0000 0 1 -3 158955 51182 -0.86960 0.86325-0.46960 0.50461-0.15250 0.01231 166263 0.29 -1.09 1.0000 0 -1 -3 153604 61967 -0.35659 0.34914 0.89179-0.92684-0.27845 0.13801 167044 0.55 0.04 1.0000 0 1 3 187399 86626 -0.49668 0.50414 0.86045-0.82538-0.11366 0.25412 202220 0.55 -0.04 1.0000 0 1 -3 236085 85503 -0.66147 0.65397 0.73596-0.70091 0.14423-0.28465 245213 0.29 -1.09 1.0000 0 -1 3 166284 89703 -0.71914 0.72663 0.63913-0.67417 0.27265-0.13226 173654 0.29 1.09 1.0000 0 1 -4 153616 8730 -0.03104 0.02116 0.99536-0.96029 0.09099-0.27816 25042 -7.65 0.07 1.0000 0 1 4 228756 41189 -0.66750 0.67729 0.74456-0.70957-0.00729 0.19436 65586 7.29 -0.41 1.0000 0 -1 -4 163598 21465 -0.96736 0.95779 0.23617-0.27120-0.09183-0.09528 33079 7.29 0.41 1.0000 0 1 -4 130910 12201 -0.84809 0.83964-0.50711 0.54211-0.15350-0.03340 16414 -7.65 0.07 1.0000 0 -1 -4 166248 52223 -0.38931 0.37938 0.88851-0.92356-0.24284 0.05558 34278 7.29 0.41 1.0000 0 1 4 93204 58817 -0.55836 0.56830 0.82910-0.79403-0.02843 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