data_Baran497 _audit_creation_date 2015-02-17 _audit_creation_method ; Olex2 1.2-beta (compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) ; _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. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C19 H26 O3 Si' _chemical_formula_sum 'C19 H26 O3 Si' _chemical_formula_weight 330.49 _chemical_absolute_configuration ad _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' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.2541 0.3302 '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 4 _space_group_name_H-M_alt 'P 1 21 1' _space_group_name_Hall 'P 2yb' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.0283(14) _cell_length_b 6.7122(9) _cell_length_c 14.1747(19) _cell_angle_alpha 90 _cell_angle_beta 101.993(6) _cell_angle_gamma 90 _cell_volume 933.3(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9874 _cell_measurement_temperature 100 _cell_measurement_theta_max 68.352 _cell_measurement_theta_min 3.188 _shelx_estimated_absorpt_T_max 0.961 _shelx_estimated_absorpt_T_min 0.838 _exptl_absorpt_coefficient_mu 1.202 _exptl_absorpt_correction_T_max 0.1665 _exptl_absorpt_correction_T_min 0.0631 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.1257 before and 0.0458 after correction. The Ratio of minimum to maximum transmission is 0.3790. The \l/2 correction factor is 0.00150. ; _exptl_absorpt_special_details ? _exptl_crystal_colour Colorless _exptl_crystal_colour_primary Colorless _exptl_crystal_density_diffrn 1.176 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description Block _exptl_crystal_F_000 356 _exptl_crystal_size_max 0.153 _exptl_crystal_size_mid 0.075 _exptl_crystal_size_min 0.033 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_unetI/netI 0.0154 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 24190 _diffrn_reflns_point_group_measured_fraction_full 0.984 _diffrn_reflns_point_group_measured_fraction_max 0.981 _diffrn_reflns_theta_full 68.000 _diffrn_reflns_theta_max 68.346 _diffrn_reflns_theta_min 3.187 _diffrn_ambient_temperature 100.0 _diffrn_detector 'Bruker APEX-II CCD' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD Area Detector' _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device 'Kappa Four-Circle Diffractometer' _diffrn_measurement_device_type 'Bruker X8 APEX II Cu' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'Double Bounce Multilayer Mirrors' _diffrn_radiation_probe X-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source 'Micro Focus Rotating Anode' _diffrn_source_type 'Bruker FR-591' _diffrn_standards_number 0 _reflns_Friedel_coverage 0.811 _reflns_Friedel_fraction_full 0.973 _reflns_Friedel_fraction_max 0.968 _reflns_number_gt 3294 _reflns_number_total 3355 _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 'SAINT v8.34A (Bruker, 2013)' _computing_data_collection 'APEX2 v2013.6-2 (Bruker, 2013)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'XT (Sheldrick, 2008)' _refine_diff_density_max 0.220 _refine_diff_density_min -0.113 _refine_diff_density_rms 0.030 _refine_ls_abs_structure_details ; Flack x determined using 1458 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.001(10) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 211 _refine_ls_number_reflns 3355 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0286 _refine_ls_R_factor_gt 0.0280 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+0.1548P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0730 _refine_ls_wR_factor_ref 0.0746 _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 Ternary CH refined with riding coordinates: C3(H3), C6(H6) 2.b Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C4(H4A,H4B), C7(H7A,H7B), C8(H8A,H8B) 2.c Aromatic/amide H refined with riding coordinates: C12(H12), C13(H13), C14(H14), C15(H15), C16(H16) 2.d X=CH2 refined with riding coordinates: C9(H9A,H9B) 2.e Idealised Me refined as rotating group: C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 Si1 Si 0.23862(6) 0.78212(10) 0.41781(4) 0.04255(17) Uani 1 1 d . . . . . O1 O 0.66239(15) 0.6510(3) 0.80606(12) 0.0491(4) Uani 1 1 d . . . . . O2 O 0.59505(14) 0.3344(2) 0.90449(10) 0.0364(3) Uani 1 1 d . . . . . O3 O 0.65091(17) 0.5621(3) 1.02224(11) 0.0472(4) Uani 1 1 d . . . . . C1 C 0.1585(2) 0.6798(4) 0.51704(15) 0.0405(5) Uani 1 1 d . . . . . H1A H 0.0596 0.7092 0.5014 0.049 Uiso 1 1 calc R . . . . H1B H 0.1693 0.5332 0.5191 0.049 Uiso 1 1 calc R . . . . C2 C 0.21889(19) 0.7639(4) 0.61572(14) 0.0358(4) Uani 1 1 d . . . . . C3 C 0.3323(2) 0.6419(3) 0.67623(14) 0.0341(4) Uani 1 1 d . . . . . H3 H 0.3850 0.5794 0.6313 0.041 Uiso 1 1 calc R . . . . C4 C 0.43362(19) 0.7665(4) 0.75036(14) 0.0375(4) Uani 1 1 d . . . . . H4A H 0.4757 0.8705 0.7165 0.045 Uiso 1 1 calc R . . . . H4B H 0.3846 0.8331 0.7954 0.045 Uiso 1 1 calc R . . . . C5 C 0.5427(2) 0.6326(3) 0.80581(15) 0.0375(5) Uani 1 1 d . . . . . C6 C 0.4874(2) 0.4637(3) 0.85790(15) 0.0350(4) Uani 1 1 d . . . . . H6 H 0.4402 0.5206 0.9074 0.042 Uiso 1 1 calc R . . . . C7 C 0.3865(2) 0.3401(3) 0.78649(15) 0.0373(5) Uani 1 1 d . . . . . H7A H 0.3449 0.2380 0.8217 0.045 Uiso 1 1 calc R . . . . H7B H 0.4350 0.2707 0.7419 0.045 Uiso 1 1 calc R . . . . C8 C 0.2747(2) 0.4729(3) 0.72864(15) 0.0364(5) Uani 1 1 d . . . . . H8A H 0.2205 0.5309 0.7728 0.044 Uiso 1 1 calc R . . . . H8B H 0.2127 0.3903 0.6807 0.044 Uiso 1 1 calc R . . . . C9 C 0.1736(2) 0.9315(4) 0.64676(16) 0.0449(5) Uani 1 1 d . . . . . H9A H 0.1013 1.0024 0.6068 0.054 Uiso 1 1 calc R . . . . H9B H 0.2134 0.9810 0.7090 0.054 Uiso 1 1 calc R . . . . C10 C 0.6718(2) 0.4045(3) 0.98737(14) 0.0361(5) Uani 1 1 d . . . . . C11 C 0.7821(2) 0.2630(4) 1.03004(13) 0.0359(4) Uani 1 1 d . . . . . C12 C 0.8859(2) 0.3343(3) 1.10386(15) 0.0393(5) Uani 1 1 d . . . . . H12 H 0.8829 0.4674 1.1262 0.047 Uiso 1 1 calc R . . . . C13 C 0.9929(2) 0.2113(4) 1.14431(16) 0.0442(6) Uani 1 1 d . . . . . H13 H 1.0649 0.2607 1.1931 0.053 Uiso 1 1 calc R . . . . C14 C 0.9950(2) 0.0168(4) 1.11373(16) 0.0464(6) Uani 1 1 d . . . . . H14 H 1.0684 -0.0679 1.1419 0.056 Uiso 1 1 calc R . . . . C15 C 0.8904(2) -0.0565(4) 1.04194(17) 0.0444(5) Uani 1 1 d . . . . . H15 H 0.8915 -0.1915 1.0221 0.053 Uiso 1 1 calc R . . . . C16 C 0.7848(2) 0.0676(4) 0.99946(15) 0.0397(5) Uani 1 1 d . . . . . H16 H 0.7143 0.0188 0.9494 0.048 Uiso 1 1 calc R . . . . C17 C 0.2018(3) 1.0545(4) 0.40372(19) 0.0514(6) Uani 1 1 d . . . . . H17A H 0.1030 1.0753 0.3860 0.077 Uiso 1 1 calc GR . . . . H17B H 0.2446 1.1085 0.3530 0.077 Uiso 1 1 calc GR . . . . H17C H 0.2384 1.1227 0.4647 0.077 Uiso 1 1 calc GR . . . . C18 C 0.4266(3) 0.7388(4) 0.4479(2) 0.0562(7) Uani 1 1 d . . . . . H18A H 0.4641 0.7891 0.5129 0.084 Uiso 1 1 calc GR . . . . H18B H 0.4693 0.8089 0.4013 0.084 Uiso 1 1 calc GR . . . . H18C H 0.4450 0.5957 0.4454 0.084 Uiso 1 1 calc GR . . . . C19 C 0.1672(4) 0.6454(5) 0.30370(19) 0.0675(8) Uani 1 1 d . . . . . H19A H 0.1808 0.5019 0.3143 0.101 Uiso 1 1 calc GR . . . . H19B H 0.2138 0.6889 0.2530 0.101 Uiso 1 1 calc GR . . . . H19C H 0.0695 0.6737 0.2839 0.101 Uiso 1 1 calc GR . . . . 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 Si1 0.0532(3) 0.0392(3) 0.0349(3) 0.0041(3) 0.0083(2) -0.0030(3) O1 0.0329(8) 0.0584(10) 0.0544(9) 0.0101(8) 0.0054(7) -0.0018(7) O2 0.0369(7) 0.0380(8) 0.0324(7) 0.0000(6) 0.0027(6) 0.0049(6) O3 0.0498(9) 0.0468(9) 0.0413(8) -0.0097(7) 0.0005(7) 0.0112(7) C1 0.0398(11) 0.0411(12) 0.0377(11) 0.0052(9) 0.0013(8) -0.0047(9) C2 0.0341(9) 0.0386(11) 0.0343(9) 0.0062(10) 0.0060(8) -0.0025(9) C3 0.0349(10) 0.0352(11) 0.0322(10) -0.0006(8) 0.0070(8) 0.0006(9) C4 0.0351(10) 0.0362(11) 0.0396(10) 0.0008(10) 0.0038(8) -0.0027(9) C5 0.0365(11) 0.0392(12) 0.0357(11) -0.0041(9) 0.0053(8) -0.0009(9) C6 0.0327(10) 0.0382(11) 0.0331(10) 0.0009(8) 0.0049(8) 0.0051(9) C7 0.0390(10) 0.0370(11) 0.0341(10) 0.0035(8) 0.0035(8) -0.0011(8) C8 0.0352(10) 0.0390(11) 0.0338(10) 0.0021(8) 0.0043(8) -0.0038(9) C9 0.0436(12) 0.0470(13) 0.0414(12) 0.0039(10) 0.0029(9) 0.0077(10) C10 0.0353(10) 0.0413(12) 0.0315(10) 0.0003(9) 0.0067(8) -0.0001(9) C11 0.0356(10) 0.0426(11) 0.0312(9) 0.0034(9) 0.0109(7) 0.0035(10) C12 0.0402(11) 0.0446(13) 0.0336(10) 0.0044(8) 0.0089(8) -0.0005(9) C13 0.0362(11) 0.0585(15) 0.0369(11) 0.0067(10) 0.0051(9) 0.0007(10) C14 0.0416(11) 0.0571(15) 0.0423(13) 0.0144(11) 0.0132(9) 0.0123(10) C15 0.0510(13) 0.0421(12) 0.0436(12) 0.0060(10) 0.0180(10) 0.0095(10) C16 0.0415(11) 0.0447(12) 0.0348(11) 0.0011(9) 0.0120(9) 0.0026(10) C17 0.0644(15) 0.0435(13) 0.0489(13) 0.0093(11) 0.0177(11) 0.0011(12) C18 0.0601(15) 0.0547(17) 0.0597(15) 0.0096(12) 0.0263(12) 0.0038(12) C19 0.107(2) 0.0533(16) 0.0382(13) 0.0025(12) 0.0054(14) -0.0084(16) _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 Si1 C1 1.888(2) . ? Si1 C17 1.868(3) . ? Si1 C18 1.867(3) . ? Si1 C19 1.868(3) . ? O1 C5 1.206(3) . ? O2 C6 1.434(2) . ? O2 C10 1.348(2) . ? O3 C10 1.204(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1 C2 1.513(3) . ? C2 C3 1.515(3) . ? C2 C9 1.322(3) . ? C3 H3 1.0000 . ? C3 C4 1.546(3) . ? C3 C8 1.534(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C4 C5 1.505(3) . ? C5 C6 1.519(3) . ? C6 H6 1.0000 . ? C6 C7 1.520(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.531(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9500 . ? C9 H9B 0.9500 . ? C10 C11 1.488(3) . ? C11 C12 1.398(3) . ? C11 C16 1.383(3) . ? C12 H12 0.9500 . ? C12 C13 1.380(3) . ? C13 H13 0.9500 . ? C13 C14 1.377(4) . ? C14 H14 0.9500 . ? C14 C15 1.390(4) . ? C15 H15 0.9500 . ? C15 C16 1.383(3) . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? 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 C17 Si1 C1 109.28(11) . . ? C18 Si1 C1 109.81(11) . . ? C18 Si1 C17 110.17(13) . . ? C18 Si1 C19 107.99(15) . . ? C19 Si1 C1 108.68(13) . . ? C19 Si1 C17 110.88(13) . . ? C10 O2 C6 115.39(16) . . ? Si1 C1 H1A 108.8 . . ? Si1 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? C2 C1 Si1 113.71(15) . . ? C2 C1 H1A 108.8 . . ? C2 C1 H1B 108.8 . . ? C1 C2 C3 115.53(19) . . ? C9 C2 C1 121.7(2) . . ? C9 C2 C3 122.74(19) . . ? C2 C3 H3 107.5 . . ? C2 C3 C4 113.74(18) . . ? C2 C3 C8 111.10(16) . . ? C4 C3 H3 107.5 . . ? C8 C3 H3 107.5 . . ? C8 C3 C4 109.35(17) . . ? C3 C4 H4A 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C5 C4 C3 109.62(19) . . ? C5 C4 H4A 109.7 . . ? C5 C4 H4B 109.7 . . ? O1 C5 C4 123.7(2) . . ? O1 C5 C6 122.6(2) . . ? C4 C5 C6 113.59(17) . . ? O2 C6 C5 111.04(16) . . ? O2 C6 H6 109.2 . . ? O2 C6 C7 108.05(16) . . ? C5 C6 H6 109.2 . . ? C5 C6 C7 110.08(17) . . ? C7 C6 H6 109.2 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? C6 C7 C8 110.57(17) . . ? H7A C7 H7B 108.1 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? C3 C8 H8A 109.1 . . ? C3 C8 H8B 109.1 . . ? C7 C8 C3 112.48(17) . . ? C7 C8 H8A 109.1 . . ? C7 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? C2 C9 H9A 120.0 . . ? C2 C9 H9B 120.0 . . ? H9A C9 H9B 120.0 . . ? O2 C10 C11 111.90(18) . . ? O3 C10 O2 123.22(19) . . ? O3 C10 C11 124.88(19) . . ? C12 C11 C10 117.5(2) . . ? C16 C11 C10 122.63(19) . . ? C16 C11 C12 119.9(2) . . ? C11 C12 H12 120.0 . . ? C13 C12 C11 120.0(2) . . ? C13 C12 H12 120.0 . . ? C12 C13 H13 120.1 . . ? C14 C13 C12 119.8(2) . . ? C14 C13 H13 120.1 . . ? C13 C14 H14 119.8 . . ? C13 C14 C15 120.5(2) . . ? C15 C14 H14 119.8 . . ? C14 C15 H15 120.1 . . ? C16 C15 C14 119.9(2) . . ? C16 C15 H15 120.1 . . ? C11 C16 H16 120.1 . . ? C15 C16 C11 119.8(2) . . ? C15 C16 H16 120.1 . . ? Si1 C17 H17A 109.5 . . ? Si1 C17 H17B 109.5 . . ? Si1 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? _shelx_res_file ; baran497.res created by SHELXL-2014/7 TITL Baran497 in P21 #4 REM SHELXT solution in P2(1) REM R1 0.103, Rweak 0.033, Alpha 0.002, Orientation as input REM Flack x = 0.101 ( 0.007 ) from Parsons' quotients REM Formula found by SHELXT: C18 O4 Si CELL 1.54178 10.0283 6.7122 14.1747 90 101.993 90 ZERR 2 0.0014 0.0009 0.0019 0 0.006 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H O Si UNIT 38 52 6 2 L.S. 10 PLAN 20 SIZE 0.153 0.075 0.033 TEMP -173.15 BOND $H fmap 2 53 ACTA 136 REM REM REM WGHT 0.042400 0.154800 FVAR 1.24530 SI1 4 0.238616 0.782118 0.417809 11.00000 0.05318 0.03916 = 0.03493 0.00406 0.00828 -0.00300 O1 3 0.662392 0.650993 0.806064 11.00000 0.03293 0.05845 = 0.05445 0.01014 0.00536 -0.00184 O2 3 0.595049 0.334441 0.904487 11.00000 0.03689 0.03802 = 0.03243 0.00001 0.00271 0.00488 O3 3 0.650914 0.562066 1.022243 11.00000 0.04975 0.04679 = 0.04130 -0.00973 0.00053 0.01125 C1 1 0.158464 0.679830 0.517040 11.00000 0.03983 0.04106 = 0.03771 0.00523 0.00134 -0.00466 AFIX 23 H1A 2 0.059575 0.709208 0.501415 11.00000 -1.20000 H1B 2 0.169346 0.533201 0.519144 11.00000 -1.20000 AFIX 0 C2 1 0.218893 0.763945 0.615722 11.00000 0.03414 0.03856 = 0.03434 0.00615 0.00598 -0.00253 C3 1 0.332303 0.641947 0.676234 11.00000 0.03488 0.03523 = 0.03222 -0.00059 0.00704 0.00059 AFIX 13 H3 2 0.384961 0.579429 0.631319 11.00000 -1.20000 AFIX 0 C4 1 0.433624 0.766473 0.750356 11.00000 0.03515 0.03617 = 0.03959 0.00081 0.00384 -0.00273 AFIX 23 H4A 2 0.475671 0.870528 0.716494 11.00000 -1.20000 H4B 2 0.384559 0.833120 0.795383 11.00000 -1.20000 AFIX 0 C5 1 0.542731 0.632577 0.805814 11.00000 0.03653 0.03920 = 0.03573 -0.00410 0.00525 -0.00091 C6 1 0.487400 0.463655 0.857902 11.00000 0.03273 0.03821 = 0.03311 0.00087 0.00494 0.00512 AFIX 13 H6 2 0.440205 0.520649 0.907373 11.00000 -1.20000 AFIX 0 C7 1 0.386500 0.340118 0.786492 11.00000 0.03902 0.03703 = 0.03414 0.00354 0.00350 -0.00107 AFIX 23 H7A 2 0.344852 0.237971 0.821693 11.00000 -1.20000 H7B 2 0.434981 0.270749 0.741915 11.00000 -1.20000 AFIX 0 C8 1 0.274653 0.472905 0.728644 11.00000 0.03524 0.03898 = 0.03375 0.00211 0.00433 -0.00381 AFIX 23 H8A 2 0.220491 0.530876 0.772831 11.00000 -1.20000 H8B 2 0.212722 0.390317 0.680659 11.00000 -1.20000 AFIX 0 C9 1 0.173636 0.931454 0.646761 11.00000 0.04364 0.04703 = 0.04139 0.00394 0.00286 0.00766 AFIX 93 H9A 2 0.101333 1.002358 0.606791 11.00000 -1.20000 H9B 2 0.213407 0.980957 0.709041 11.00000 -1.20000 AFIX 0 C10 1 0.671781 0.404525 0.987374 11.00000 0.03529 0.04130 = 0.03153 0.00028 0.00673 -0.00010 C11 1 0.782094 0.263038 1.030038 11.00000 0.03557 0.04257 = 0.03123 0.00341 0.01088 0.00347 C12 1 0.885936 0.334306 1.103856 11.00000 0.04017 0.04458 = 0.03359 0.00443 0.00888 -0.00053 AFIX 43 H12 2 0.882877 0.467357 1.126161 11.00000 -1.20000 AFIX 0 C13 1 0.992896 0.211285 1.144310 11.00000 0.03617 0.05854 = 0.03691 0.00675 0.00510 0.00073 AFIX 43 H13 2 1.064904 0.260672 1.193126 11.00000 -1.20000 AFIX 0 C14 1 0.994952 0.016811 1.113727 11.00000 0.04157 0.05709 = 0.04233 0.01437 0.01316 0.01227 AFIX 43 H14 2 1.068351 -0.067926 1.141883 11.00000 -1.20000 AFIX 0 C15 1 0.890399 -0.056461 1.041942 11.00000 0.05100 0.04214 = 0.04362 0.00605 0.01805 0.00951 AFIX 43 H15 2 0.891497 -0.191538 1.022106 11.00000 -1.20000 AFIX 0 C16 1 0.784805 0.067621 0.999465 11.00000 0.04145 0.04473 = 0.03482 0.00114 0.01203 0.00255 AFIX 43 H16 2 0.714290 0.018779 0.949405 11.00000 -1.20000 AFIX 0 C17 1 0.201757 1.054537 0.403717 11.00000 0.06438 0.04349 = 0.04888 0.00932 0.01769 0.00108 AFIX 137 H17A 2 0.102973 1.075252 0.385985 11.00000 -1.50000 H17B 2 0.244606 1.108546 0.353038 11.00000 -1.50000 H17C 2 0.238356 1.122731 0.464737 11.00000 -1.50000 AFIX 0 C18 1 0.426583 0.738812 0.447927 11.00000 0.06012 0.05471 = 0.05971 0.00965 0.02631 0.00383 AFIX 137 H18A 2 0.464080 0.789061 0.512940 11.00000 -1.50000 H18B 2 0.469323 0.808898 0.401261 11.00000 -1.50000 H18C 2 0.445013 0.595744 0.445388 11.00000 -1.50000 AFIX 0 C19 1 0.167167 0.645431 0.303705 11.00000 0.10676 0.05325 = 0.03825 0.00254 0.00544 -0.00838 AFIX 137 H19A 2 0.180760 0.501942 0.314349 11.00000 -1.50000 H19B 2 0.213788 0.688912 0.252981 11.00000 -1.50000 H19C 2 0.069471 0.673728 0.283923 11.00000 -1.50000 AFIX 0 HKLF 4 REM Baran497 in P21 #4 REM R1 = 0.0280 for 3294 Fo > 4sig(Fo) and 0.0286 for all 3355 data REM 211 parameters refined using 1 restraints END WGHT 0.0424 0.1546 REM Highest difference peak 0.220, deepest hole -0.113, 1-sigma level 0.030 Q1 1 0.2013 0.7286 0.3551 11.00000 0.05 0.22 Q2 1 0.2168 0.7415 0.4802 11.00000 0.05 0.20 Q3 1 0.3401 0.7773 0.4143 11.00000 0.05 0.18 Q4 1 0.2181 0.9350 0.4126 11.00000 0.05 0.17 Q5 1 0.8031 0.2884 1.0778 11.00000 0.05 0.15 Q6 1 0.2368 0.8821 0.6158 11.00000 0.05 0.14 Q7 1 0.3837 0.7130 0.7188 11.00000 0.05 0.14 Q8 1 0.1535 0.7931 0.6468 11.00000 0.05 0.14 Q9 1 0.8493 0.3160 1.0412 11.00000 0.05 0.13 Q10 1 0.1971 0.7662 0.5678 11.00000 0.05 0.13 Q11 1 0.3324 0.4005 0.7572 11.00000 0.05 0.13 Q12 1 0.3013 0.5623 0.6987 11.00000 0.05 0.11 Q13 1 0.2805 0.7220 0.6415 11.00000 0.05 0.11 Q14 1 0.8634 0.0199 0.9901 11.00000 0.05 0.11 Q15 1 0.7594 0.3330 1.0161 11.00000 0.05 0.11 Q16 1 0.6003 0.6064 0.7796 11.00000 0.05 0.11 Q17 1 0.9585 -0.0358 1.0643 11.00000 0.05 0.11 Q18 1 0.5956 0.3134 0.9527 11.00000 0.05 0.11 Q19 1 0.6193 0.7019 0.8487 11.00000 0.05 0.11 Q20 1 0.6646 0.3336 0.8798 11.00000 0.05 0.10 ; _shelx_res_checksum 85707 _shelx_hkl_file ; 1 0 0 896.664 29.2628 36 1 0 0 924.302 29.2431 43 1 0 0 864.374 29.3482 35 1 0 0 898.358 29.3377 36 1 0 0 844.583 29.2160 29 -1 0 0 902.675 29.3000 43 -1 0 0 823.217 29.3432 2 -1 0 0 899.645 29.4404 11 -1 0 0 935.337 29.2425 29 -1 0 0 855.722 29.3615 32 -1 0 0 904.794 29.3489 35 -1 0 0 908.561 29.2773 36 -1 0 0 906.079 29.2231 38 1 0 0 869.833 29.4093 11 2 0 0 2888.13 93.8371 36 2 0 0 2614.61 93.6063 29 -2 0 0 2905.17 93.6742 38 -2 0 0 2831.01 93.7684 43 -2 0 0 2929.37 93.6723 29 -2 0 0 2916.06 93.8715 35 2 0 0 2767.68 93.6886 36 -2 0 0 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72.8807 4.39422 3 -4 4 10 64.5236 3.53384 24 4 4 -10 69.3476 4.11533 23 -4 4 10 67.2294 4.14601 44 -3 -4 10 189.282 8.43346 7 3 -4 -10 190.320 7.54455 25 3 -4 -10 183.152 7.33927 5 3 -4 -10 184.417 6.82330 14 3 -4 -10 174.135 7.31233 42 -3 -4 10 166.665 6.99441 28 3 -4 -10 177.567 9.16765 39 -3 -4 10 178.577 8.22997 15 -3 -4 10 185.046 7.89525 13 3 -4 -10 179.963 6.77741 10 3 4 -10 182.104 7.52320 23 3 4 -10 176.636 8.12593 39 -3 4 10 189.760 7.88367 24 3 4 -10 195.777 7.70704 3 2 -4 -10 130.768 5.24539 14 -2 -4 10 128.954 6.73637 7 2 -4 -10 130.282 6.05359 25 2 -4 -10 134.579 5.24797 10 2 -4 -10 130.083 7.69606 39 -2 -4 10 130.504 5.54832 17 -2 -4 10 125.474 5.58891 40 -2 -4 10 120.093 5.34272 28 -2 -4 10 134.825 6.24314 13 -2 -4 10 122.998 6.56302 15 2 -4 -10 128.700 5.47043 5 2 4 -10 125.035 5.78024 23 -2 4 10 127.216 6.17823 24 2 4 -10 125.481 5.78674 44 2 4 -10 124.336 6.35707 39 2 4 -10 126.468 6.10369 3 -2 4 10 124.009 5.33203 4 -1 -4 10 385.899 14.0649 20 -1 -4 10 376.676 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6.95290 1.42074 40 1 -4 10 7.43596 1.65917 20 -1 4 -10 4.16180 2.90505 39 -1 4 -10 3.97462 1.62302 30 1 4 10 4.02623 1.47756 4 -1 4 -10 4.91280 1.79711 44 1 4 10 5.92824 1.53600 24 1 4 10 3.76993 1.45289 8 1 4 10 3.17764 1.31129 13 2 -4 10 31.6047 3.37546 20 2 -4 10 32.9315 2.73809 40 -2 -4 -10 27.9830 2.97534 5 -2 -4 -10 27.0303 3.42600 25 -2 -4 -10 25.8049 1.84570 10 2 -4 10 31.6659 2.51044 17 -2 4 -10 28.1380 2.39603 44 2 4 10 28.3021 2.26583 13 2 4 10 28.1671 2.26810 15 -2 4 -10 28.3534 3.75261 39 2 4 10 25.2860 2.07191 4 2 4 10 31.7230 2.53196 8 -2 4 -10 23.3024 2.00552 30 2 4 10 29.1081 2.36520 24 -3 -4 -10 17.4112 1.42642 10 -3 -4 -10 15.4695 2.55762 25 -3 -4 -10 12.7680 2.03292 5 3 -4 10 15.4850 1.99362 17 3 -4 10 20.2800 1.78695 40 3 -4 10 19.1570 2.21714 20 3 4 10 15.8745 1.77338 24 3 4 10 17.9230 2.11672 8 -3 4 -10 18.4633 1.85849 30 -3 4 -10 19.0642 2.83482 39 3 4 10 17.9756 1.51623 13 -3 4 -10 17.8580 1.83761 44 3 4 10 18.4704 2.14355 4 3 4 10 19.5837 1.97047 15 4 -4 10 28.1893 1.87604 40 -4 -4 -10 34.4121 3.17662 25 4 -4 10 32.4155 2.46275 20 -4 -4 -10 32.4076 1.90714 10 4 -4 10 28.8970 2.16451 17 -4 -4 -10 33.3866 2.26826 5 4 4 10 31.4237 2.38530 4 4 4 10 32.5189 2.00852 8 4 4 10 28.0743 2.32542 34 4 4 10 31.1401 1.91104 15 4 4 10 30.3119 1.78272 13 -4 4 -10 33.7147 2.01998 44 5 -4 10 10.8295 1.25297 17 -5 -4 -10 10.1535 1.43436 25 -5 -4 -10 9.99867 1.26436 5 5 -4 10 11.8545 1.40279 20 5 4 10 9.55908 1.47202 8 5 4 10 9.01992 1.26759 34 5 4 10 8.59899 0.92160 13 5 4 10 8.15270 1.16122 15 6 -4 10 16.1419 1.37299 17 -6 -4 -10 12.5095 1.25264 5 6 4 10 11.7823 0.98931 15 7 -5 -10 4.48954 1.53057 14 7 -5 -10 9.10132 1.17675 42 -7 -5 10 9.95133 1.55681 7 -7 5 10 9.03275 0.96277 7 7 5 -10 10.8346 1.26657 3 7 5 -10 5.62958 1.11745 22 7 5 -10 9.70630 1.27573 13 6 -5 -10 31.6616 1.64430 14 6 -5 -10 34.0382 1.98466 42 -6 -5 10 28.4906 2.56841 7 6 -5 -10 32.5674 2.07429 5 6 -5 -10 31.1615 3.68234 31 6 5 -10 29.3761 3.14629 13 6 5 -10 28.0125 2.23859 22 6 5 -10 38.8613 2.19751 3 6 5 -10 30.6151 2.02936 23 -5 -5 10 32.9397 3.36136 7 -5 -5 10 30.7558 2.12267 28 5 -5 -10 32.0774 2.60034 25 5 -5 -10 30.3095 1.93527 5 5 -5 -10 25.8435 2.66852 39 5 -5 -10 28.5430 2.06235 42 5 5 -10 30.1973 2.16853 3 5 5 -10 27.5420 2.36930 34 5 5 -10 27.0551 2.48364 22 5 5 -10 28.2776 2.01311 23 -5 5 10 25.6004 2.40099 44 4 -5 -10 125.999 6.81235 39 4 -5 -10 132.269 5.31592 25 4 -5 -10 125.726 5.31104 42 4 -5 -10 137.173 4.95027 14 -4 -5 10 133.391 6.13749 15 -4 -5 10 141.838 6.48703 7 -4 -5 10 133.001 5.38067 28 4 -5 -10 129.804 5.11997 5 4 5 -10 144.916 6.21827 22 -4 5 10 131.572 5.53402 24 -4 5 10 110.850 5.86680 44 4 5 -10 145.257 5.76344 3 4 5 -10 131.198 6.13178 34 -3 -5 10 47.2086 2.68104 28 3 -5 -10 51.9512 2.43331 14 3 -5 -10 56.9639 3.39302 25 3 -5 -10 51.0411 4.03773 39 -3 -5 10 54.0609 3.97896 15 3 -5 -10 54.9868 2.45127 10 3 -5 -10 49.5051 3.45063 42 3 -5 -10 49.8343 2.69844 5 -3 -5 10 55.1737 3.96175 7 3 5 -10 51.3276 3.80721 34 3 5 -10 52.0777 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7.38543 40 1 -2 14 213.032 8.94487 24 1 2 14 202.567 7.37196 20 -1 2 -14 200.650 7.56817 23 1 2 14 206.199 8.12355 24 -1 2 -14 198.784 8.20913 39 1 2 14 207.687 7.44444 13 1 2 14 192.713 7.57775 8 1 2 14 210.164 8.10112 4 1 2 14 198.063 7.27455 33 1 2 14 187.814 8.06840 19 2 -2 14 45.1875 2.52868 20 -2 -2 -14 45.3370 2.24918 5 2 -2 14 43.5438 3.20908 4 2 -2 14 46.4823 2.36945 40 2 -2 14 38.3990 2.53993 15 2 -2 14 42.9521 3.06796 24 -2 2 -14 42.6552 2.91465 44 2 2 14 37.5112 2.63475 4 2 2 14 44.6124 2.13318 13 2 2 14 38.8005 2.19569 20 2 2 14 38.2798 2.76214 19 2 2 14 43.6115 2.29965 15 -2 2 -14 41.2170 2.23425 23 2 2 14 42.1977 2.98341 24 2 2 14 45.5190 2.81893 8 3 -2 14 4.02221 1.17559 15 3 -2 14 8.50716 1.13678 20 3 -2 14 5.12125 0.90127 40 -3 -2 -14 6.21736 0.95323 5 3 2 14 5.51619 0.77634 13 3 2 14 6.84219 1.02186 15 3 2 14 7.66178 1.29633 4 3 2 14 6.93843 0.93647 20 3 2 14 6.85684 0.81710 33 3 2 14 6.49167 1.07583 8 4 2 14 10.4215 1.48307 15 7 -3 -14 56.1231 2.72736 5 -7 -3 14 74.4303 3.23766 7 -7 3 14 60.9736 2.73830 7 6 -3 -14 7.37962 1.13943 18 6 -3 -14 7.62501 0.99044 5 6 -3 -14 6.24018 1.03109 14 -6 -3 14 3.89643 1.46129 7 -6 -3 14 7.03396 1.11213 15 6 3 -14 1.20645 0.98633 23 6 3 -14 4.16753 1.30551 22 -6 3 14 4.59631 1.00268 7 5 -3 -14 31.1311 1.87127 5 5 -3 -14 29.9001 1.89642 14 -5 -3 14 31.4002 2.68456 13 -5 -3 14 28.5993 2.12830 15 -5 -3 14 26.6136 2.17837 7 5 3 -14 25.6708 1.91626 23 5 3 -14 25.4752 1.95800 22 -5 3 14 21.2217 1.75315 7 4 -3 -14 107.340 5.74771 39 -4 -3 14 122.353 5.33880 15 4 -3 -14 124.285 4.76057 14 -4 -3 14 121.656 5.01985 13 4 -3 -14 127.506 4.88516 5 -4 -3 14 110.876 5.10548 7 -4 3 14 124.750 4.84696 7 4 3 -14 117.890 5.41710 22 -4 3 14 112.994 5.13110 24 4 3 -14 125.807 4.92959 23 -4 3 14 115.579 5.27938 19 4 3 -14 107.803 4.61401 3 3 -3 -14 161.766 7.34656 39 -3 -3 14 173.298 6.69672 13 -3 -3 14 166.446 6.80979 15 -3 -3 14 172.261 7.86851 24 3 -3 -14 185.425 6.51617 5 3 -3 -14 163.209 6.22358 14 3 3 -14 175.064 7.27488 39 -3 3 14 156.516 7.01040 19 3 3 -14 185.470 6.75753 3 -3 3 14 196.561 7.42949 24 2 -3 -14 148.174 6.89777 39 2 -3 -14 159.880 6.03455 5 -2 -3 14 163.864 6.63635 15 -2 -3 14 153.852 6.03448 13 -2 -3 14 143.295 7.34640 24 2 3 -14 153.242 5.90233 3 -2 3 14 152.195 6.32207 24 -2 3 14 145.213 6.35922 19 2 3 -14 150.755 6.07352 23 2 3 -14 151.940 6.68789 39 -1 -3 14 26.8479 2.36187 15 1 -3 -14 24.6985 1.98702 5 1 -3 -14 23.2324 2.59173 39 -1 -3 14 25.6269 3.18941 24 -1 -3 14 24.4132 1.83846 40 -1 3 14 28.4999 1.95931 8 -1 3 14 30.8430 1.97551 13 -1 3 14 21.5029 1.94482 4 -1 3 14 30.8154 2.36770 24 -1 3 14 28.2596 2.46388 19 1 3 -14 25.7881 1.80913 23 1 3 -14 27.7017 2.38270 39 1 3 -14 27.9426 2.05315 3 0 -3 -14 158.611 6.04506 5 0 -3 -14 179.325 7.60417 39 0 -3 14 157.455 6.03594 40 0 -3 14 157.722 6.37089 15 0 -3 14 158.753 7.35863 24 0 3 -14 147.863 5.60843 23 0 3 14 155.480 5.86575 8 0 3 14 145.598 5.91779 4 0 3 -14 147.810 6.24861 39 0 3 14 151.545 5.64371 13 0 3 14 136.992 6.05846 24 1 -3 14 16.8482 1.46914 40 1 -3 14 15.7356 1.63059 15 1 -3 14 15.1151 1.46324 20 -1 -3 -14 16.0723 1.55664 5 1 3 14 15.7294 1.56949 8 1 3 14 13.8678 1.19247 20 1 3 14 17.1161 1.35196 15 1 3 14 17.2884 1.39327 13 1 3 14 16.9634 1.66580 4 2 -3 14 27.1523 1.74426 20 -2 -3 -14 26.4829 1.66881 5 2 -3 14 28.4521 1.64214 40 2 -3 14 27.3466 1.75031 15 2 3 14 26.7584 1.43691 20 2 3 14 27.8017 1.76529 15 2 3 14 23.1670 1.61374 8 2 3 14 27.4828 2.15109 4 2 3 14 22.9422 1.44047 13 -5 -4 14 26.9854 2.13959 15 5 -4 -14 29.6656 1.61181 5 5 -4 -14 29.1325 1.55553 14 -4 -4 14 8.09603 1.30109 15 4 -4 -14 10.6273 1.21215 5 4 -4 -14 11.1664 1.42965 14 -4 4 14 8.68763 1.09669 7 4 4 -14 5.49624 0.92644 3 -3 -4 14 70.6428 3.16345 15 3 -4 -14 68.5123 2.67499 14 3 -4 -14 57.8821 2.74822 5 3 4 -14 71.1659 3.13255 3 -3 4 14 69.8756 3.07045 7 3 4 -14 73.6810 3.40838 22 -3 4 14 71.3281 3.50156 24 2 -4 -14 84.4189 3.19607 5 -2 -4 14 70.2047 3.36483 15 -2 4 14 89.9738 4.16974 24 2 4 -14 94.4423 4.16860 22 1 -4 -14 110.801 4.27634 5 -1 -4 14 115.193 4.63016 15 -1 4 14 116.708 4.56225 13 -1 4 14 121.343 5.06275 24 1 4 -14 122.960 4.70551 3 1 4 -14 121.489 4.91418 22 0 -4 -14 6.30580 0.97052 5 0 -4 14 4.72825 1.00505 15 0 4 -14 2.77010 0.98916 3 0 4 14 3.42349 1.29368 24 0 4 14 5.54107 1.07771 4 0 4 14 3.31895 0.72764 13 -1 -4 -14 125.320 4.77244 5 -1 4 -14 89.4673 3.58316 3 -7 0 15 84.4108 3.70085 1 7 0 -15 84.1494 3.66895 18 -7 0 15 82.8209 3.79864 7 -6 0 15 61.0509 3.40374 7 -6 0 15 56.4815 3.31284 13 6 0 -15 53.1930 2.88725 18 -5 0 15 22.6204 2.05634 19 5 0 -15 29.0333 2.87686 39 -5 0 15 21.9472 2.60843 13 5 0 -15 19.2387 1.87194 18 5 0 -15 21.8628 1.77740 23 -5 0 15 22.1922 2.40795 7 -4 0 15 80.6322 3.89765 13 4 0 -15 81.8219 4.29029 39 4 0 -15 81.7771 3.73407 18 -4 0 15 81.9310 4.66529 24 -4 0 15 79.8403 3.81998 7 -4 0 15 80.7879 4.26358 19 4 0 -15 75.2749 3.47412 23 -3 0 15 22.7497 1.99702 15 -3 0 15 23.8110 2.78783 24 -3 0 15 21.9365 2.23689 19 3 0 -15 22.7302 2.37112 23 3 0 -15 24.5442 2.71457 39 -3 0 15 22.6110 2.12286 13 2 0 -15 -0.1377 1.33982 39 2 0 -15 -0.0571 1.58903 23 -2 0 15 0.21685 1.44691 13 -2 0 15 -0.2647 1.79183 19 -2 0 15 1.03745 1.63353 24 -2 0 15 1.23404 1.19681 15 -1 0 15 1.55254 1.01156 13 -1 0 15 -0.0255 1.57689 15 -1 0 15 1.11944 1.22965 4 1 0 -15 2.59694 1.47168 39 -1 0 15 0.26802 1.79257 19 1 0 -15 3.15984 1.18402 23 -1 0 15 1.91664 1.66829 24 0 0 15 0.51394 1.11807 15 0 0 15 1.05551 1.53851 24 0 0 -15 0.26830 1.35576 39 0 0 15 0.74455 1.20948 19 0 0 15 -0.3401 1.69803 4 0 0 15 0.51419 0.87723 13 0 0 -15 -0.8579 1.49868 23 -1 0 -15 99.7630 3.88993 23 -1 0 -15 80.1397 5.83377 39 1 0 15 91.7560 3.74253 13 1 0 15 95.0562 4.04147 15 1 0 15 91.3920 4.84035 24 1 0 15 83.9631 4.37834 4 1 0 15 84.9004 3.83764 20 -2 0 -15 -0.2937 0.81389 23 2 0 15 1.25366 1.42764 24 2 0 15 0.94177 1.12525 4 2 0 15 0.76114 0.94346 15 2 0 15 0.96255 0.71852 20 3 0 15 76.9350 3.37853 15 3 0 15 89.3593 4.03481 4 -7 -1 15 84.5923 3.81890 13 -7 -1 15 88.8548 4.05566 7 7 -1 -15 81.7045 3.36816 16 7 -1 -15 87.1129 3.69564 18 -7 1 15 83.9709 3.64466 7 6 -1 -15 38.9224 2.42158 18 -6 -1 15 37.6974 2.55881 7 -6 -1 15 42.7220 2.96235 13 6 1 -15 32.0267 2.40100 18 -6 1 15 42.0781 2.44373 7 6 1 -15 40.7458 2.16826 23 5 -1 -15 4.49019 2.16126 39 -5 -1 15 6.86466 1.35687 7 -5 -1 15 8.54312 1.52816 13 5 -1 -15 6.71865 1.36679 18 -5 1 15 5.74284 1.20895 7 5 1 -15 5.71328 1.24235 23 -5 1 15 4.47404 1.36756 19 -5 1 15 8.21738 1.34933 13 -4 -1 15 6.90282 1.35271 15 4 -1 -15 8.32092 1.80737 39 -4 -1 15 6.25382 1.84044 13 -4 -1 15 8.12215 1.36660 7 -4 -1 15 5.79783 1.68209 24 -4 1 15 10.3520 1.49478 13 -4 1 15 8.99824 1.66880 24 4 1 -15 11.6151 1.63622 23 4 1 -15 9.85100 1.69581 39 -4 1 15 9.11973 1.41676 7 -4 1 15 9.74920 1.64951 19 3 -1 -15 43.5677 3.40154 39 -3 -1 15 46.1668 2.79679 13 3 -1 -15 42.5943 2.40008 23 -3 -1 15 47.7337 2.78134 15 -3 -1 15 40.7269 3.45428 24 -3 1 15 47.5244 3.10974 19 3 1 -15 52.3506 2.84615 23 -3 1 15 48.8817 3.38675 24 -3 1 15 51.4803 2.91397 13 3 1 -15 48.7708 3.21174 39 -2 -1 15 82.2014 5.12352 24 2 -1 -15 75.6231 3.41127 23 -2 -1 15 73.3439 3.70582 13 -2 -1 15 80.5183 4.13600 15 2 -1 -15 77.7701 4.83961 39 2 1 -15 86.4109 4.89827 39 -2 1 15 86.7873 4.45411 19 -2 1 15 91.4471 5.12116 24 2 1 -15 87.2350 4.25544 23 -2 1 15 90.2130 4.28479 13 -1 -1 15 2.23200 2.33481 24 1 -1 -15 2.21942 1.48174 39 -1 -1 15 0.29661 1.62478 15 -1 -1 15 3.19505 1.07253 13 -1 -1 15 2.67405 1.84864 4 1 -1 -15 0.87425 1.06841 23 1 1 -15 2.68313 1.60978 23 -1 1 15 1.40309 1.60286 4 -1 1 15 1.21595 1.31704 13 1 1 -15 0.51786 1.14430 39 -1 1 15 1.81139 1.06241 15 -1 1 15 0.64117 1.34552 19 -1 1 15 2.25651 2.02443 24 0 -1 -15 135.722 5.19041 23 0 -1 -15 128.667 5.96742 39 0 -1 15 129.303 5.13198 40 0 -1 15 125.909 5.09527 13 0 -1 15 135.254 6.05804 4 0 -1 15 142.715 5.53566 15 0 -1 15 131.981 6.31983 24 0 1 15 145.946 6.10305 4 0 1 -15 146.110 5.52041 23 0 1 15 117.481 6.07826 24 0 1 15 140.798 5.43483 13 0 1 15 141.390 6.11573 19 0 1 -15 135.097 6.26692 39 0 1 15 145.716 5.59197 15 1 -1 15 178.384 7.19213 4 1 -1 15 158.553 6.27582 20 1 -1 15 158.365 6.16522 40 -1 -1 -15 177.849 6.30504 23 1 -1 15 175.355 6.70081 15 1 -1 15 162.240 7.10324 24 1 1 15 165.715 6.88299 24 1 1 15 157.262 6.07932 20 1 1 15 164.309 6.25775 15 1 1 15 172.897 6.21005 13 -1 1 -15 170.739 6.18828 23 1 1 15 158.649 6.92457 19 2 -1 15 47.4600 2.95800 4 -2 -1 -15 47.9467 2.28086 23 2 -1 15 43.3957 2.28829 40 2 -1 15 48.9154 2.41112 20 2 1 15 47.2723 2.38424 20 2 1 15 38.4309 1.87521 13 2 1 15 48.0482 3.05273 4 -2 1 -15 41.2028 2.10179 23 2 1 15 41.6595 2.56470 24 2 1 15 43.6573 2.24286 15 3 1 15 1.11115 0.78931 15 -7 2 15 0.81829 1.29138 7 6 -2 -15 31.1244 1.62587 5 6 -2 -15 28.0893 1.96362 18 -6 -2 15 31.0825 2.04896 13 -6 -2 15 29.9049 1.99795 7 -6 2 15 24.1515 1.84269 7 6 2 -15 27.9296 1.71392 23 5 -2 -15 31.8631 1.81255 5 -5 -2 15 30.2043 2.36056 15 -5 -2 15 31.2371 2.44672 7 5 -2 -15 32.5097 2.21227 18 -5 -2 15 34.8731 2.71728 13 5 2 -15 31.8325 1.97169 23 5 2 -15 26.0666 1.85889 22 -5 2 15 28.2715 1.94852 7 -4 -2 15 42.6732 3.18873 24 -4 -2 15 51.6512 3.10045 15 -4 -2 15 53.9749 3.32579 7 4 -2 -15 42.2658 2.22629 5 4 -2 -15 45.9574 2.36957 14 -4 -2 15 46.3957 2.74391 13 -4 2 15 46.7415 2.87040 19 -4 2 15 51.2331 2.82475 7 -4 2 15 48.0496 2.94822 13 4 2 -15 51.9214 2.66474 23 -4 2 15 40.8847 2.81608 24 3 -2 -15 10.9885 1.84914 39 -3 -2 15 9.36702 1.95098 15 3 -2 -15 9.97333 1.50833 5 -3 -2 15 9.99426 2.48922 24 -3 -2 15 8.53927 1.68744 13 3 2 -15 5.06647 1.72189 39 3 2 -15 10.6571 1.55719 23 -3 2 15 7.07577 1.78742 24 -3 2 15 7.86376 1.55563 19 -3 2 15 7.41476 1.27944 13 -2 -2 15 13.3453 1.86322 15 -2 -2 15 12.5694 1.66179 13 2 -2 -15 11.8011 2.02015 39 2 -2 -15 13.3786 1.42186 5 -2 -2 15 12.6713 2.64575 24 2 2 -15 13.1712 1.63909 23 -2 2 15 10.4134 1.65457 19 2 2 -15 11.4843 1.71048 39 -2 2 15 10.9783 1.63660 13 -2 2 15 11.6967 1.88608 24 -1 -2 15 100.712 3.91247 40 -1 -2 15 88.8478 3.89290 13 -1 -2 15 107.111 5.57492 24 -1 -2 15 96.8495 4.37751 15 1 -2 -15 93.4352 3.82318 5 -1 2 15 103.686 4.72602 24 1 2 -15 93.0776 4.67976 39 1 2 -15 95.5647 4.07855 3 1 2 -15 106.632 4.19246 23 -1 2 15 87.6261 4.29773 4 -1 2 15 106.672 4.17875 13 0 -2 15 79.8892 3.23247 40 0 -2 -15 78.6847 3.17058 5 0 -2 -15 78.4088 3.19305 23 0 -2 15 68.0321 4.22195 24 0 -2 15 77.3004 3.60251 15 0 2 15 82.5866 4.08168 4 0 2 15 85.6864 3.72553 8 0 2 -15 83.5025 3.55567 23 0 2 15 77.4284 3.63150 15 0 2 15 81.6491 4.14400 24 0 2 -15 74.2373 4.36997 39 0 2 15 100.067 5.00056 19 0 2 15 84.0200 3.66442 13 1 -2 15 52.0128 2.55096 15 -1 -2 -15 39.5174 2.18793 23 1 -2 15 50.8821 3.16704 24 1 -2 15 48.8336 2.34804 20 1 -2 15 46.7798 2.43792 40 1 2 15 50.5447 2.47014 15 -1 2 -15 48.8404 2.47513 23 1 2 15 47.8557 2.57896 8 1 2 15 53.4900 3.21523 24 1 2 15 50.9709 2.45214 20 1 2 15 55.5459 2.90094 4 1 2 15 53.5238 2.37188 13 2 -2 15 22.8656 1.85533 15 2 -2 15 27.4163 1.98058 20 2 -2 15 21.6741 1.37365 40 2 2 15 22.6441 1.39438 13 2 2 15 21.5574 1.42942 15 2 2 15 17.8463 2.36624 4 5 -3 -15 50.9406 2.52044 14 -5 -3 15 57.0833 2.62403 15 -5 3 15 56.9478 2.60313 7 4 -3 -15 28.7050 1.66597 5 -4 -3 15 22.5797 1.90962 15 4 -3 -15 30.2824 1.96160 14 -4 -3 15 31.4360 2.09375 13 -4 3 15 25.8397 1.65627 7 4 3 -15 23.1880 2.11684 22 4 3 -15 25.2556 1.68185 23 -3 -3 15 69.5374 3.35788 15 3 -3 -15 81.6889 3.07316 5 -3 -3 15 67.3876 3.12707 13 3 3 -15 72.4275 3.37449 22 3 3 -15 69.3769 2.97458 3 -3 3 15 69.3684 3.42973 24 2 -3 -15 25.2623 1.67995 5 -2 3 15 48.2535 2.94550 24 -2 3 15 41.5090 2.21208 13 2 3 -15 40.5748 2.15029 23 2 3 -15 34.9839 2.00409 3 1 -3 -15 39.6346 2.11693 5 -1 -3 15 44.5047 2.50909 15 -1 3 15 47.2520 2.98307 24 1 3 -15 45.7474 2.28717 3 0 -3 15 67.5592 2.71591 40 0 -3 15 59.8063 2.93226 15 0 -3 -15 64.8119 2.63299 5 0 3 15 75.3040 3.01941 13 0 3 -15 77.0846 3.12513 3 0 3 15 64.8761 3.47438 4 0 3 15 74.1237 3.61376 24 1 3 15 10.7539 0.98002 13 -1 3 -15 13.7005 1.52363 3 -6 0 16 6.16691 1.29039 7 -5 0 16 87.1918 3.56922 7 -5 0 16 82.6042 3.53651 13 5 0 -16 72.4642 3.36424 18 4 0 -16 1.85066 0.99295 23 -4 0 16 2.87957 1.59589 24 -4 0 16 0.79169 1.01791 13 -3 0 16 107.747 5.37994 24 3 0 -16 113.112 4.46879 23 -3 0 16 117.489 4.88707 13 -2 0 16 60.4363 3.12919 13 -2 0 16 59.7465 3.54425 24 -2 0 16 57.3161 2.82202 15 2 0 -16 58.6131 2.79594 23 -1 0 16 51.0947 3.19877 24 -1 0 16 39.2108 2.35870 13 1 0 -16 54.7816 2.49235 23 -1 0 16 47.7378 2.53984 15 0 0 16 22.0289 2.15561 24 0 0 16 21.1924 1.70645 15 0 0 16 20.4080 1.83536 4 0 0 16 19.0223 1.36509 13 1 0 16 13.0303 1.30810 15 -5 -1 16 24.4147 1.84858 13 5 -1 -16 20.6066 1.59163 18 -5 1 16 22.6823 1.90105 7 5 1 -16 27.1529 2.00545 23 -4 -1 16 88.9184 3.95647 13 4 -1 -16 87.8359 3.73790 18 -4 -1 16 91.4174 4.66603 24 -4 1 16 86.9867 3.66727 13 -4 1 16 79.5628 3.89249 24 -3 -1 16 14.0772 2.06402 24 -3 -1 16 14.5990 1.47949 13 -3 -1 16 15.8371 1.57925 15 -3 1 16 14.2067 1.54932 13 -3 1 16 16.0974 2.51940 24 -2 -1 16 48.2271 3.19705 24 -2 -1 16 48.8493 2.54501 15 -2 -1 16 39.6028 2.40044 13 2 -1 -16 47.7551 2.25404 23 -2 1 16 54.7885 3.63390 24 2 1 -16 52.6695 2.60797 23 -2 1 16 49.2563 2.87997 13 -1 -1 16 1.39575 1.00751 15 -1 -1 16 0.54277 1.33059 24 1 -1 -16 0.08886 1.11826 23 -1 -1 16 0.95803 0.63711 13 1 1 -16 0.25090 0.93619 23 -1 1 16 0.73011 0.79859 13 -1 1 16 1.44879 1.22284 24 -1 1 16 0.30561 1.14546 15 0 -1 -16 54.2867 2.40934 23 0 -1 16 55.1113 2.67820 15 0 -1 16 46.9607 3.13388 24 0 -1 16 51.2975 2.94288 4 0 1 16 48.2425 2.97007 24 0 1 16 52.6587 2.91552 4 0 1 16 49.2636 2.31274 13 0 1 -16 51.7118 2.42229 23 0 1 16 42.7965 2.32442 15 1 -1 16 47.9538 2.34616 15 1 1 16 41.3307 2.29823 13 1 1 16 47.9279 2.15958 15 -5 -2 16 87.1148 3.58354 13 -4 -2 16 42.7376 2.08722 15 -4 -2 16 48.8640 2.53731 13 4 -2 -16 36.0362 2.15426 18 4 2 -16 49.5675 2.40202 23 -3 -2 16 40.1925 2.18133 13 -3 -2 16 48.7759 3.19632 24 -3 -2 16 43.0704 2.33305 15 -3 2 16 42.7263 2.63933 24 -3 2 16 37.8208 2.19067 13 -2 -2 16 2.33756 1.01612 15 -2 -2 16 2.79488 0.89685 13 -2 -2 16 3.11058 1.41904 24 -2 2 16 2.56577 0.83623 13 2 2 -16 0.97482 1.00654 23 -2 2 16 3.21847 1.51768 24 -1 2 16 69.6804 2.87963 13 -1 2 16 61.6887 3.58972 24 0 -2 16 56.0879 2.63491 15 0 2 16 64.3760 2.67859 13 -3 0 17 63.8393 2.87147 13 -2 0 17 13.7188 1.74264 13 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details 'SADABS 2014/4' _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_max 0.1665 _exptl_absorpt_correction_T_min 0.0631 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 1.54184 10.039 6.706 14.165 90.006 102.008 89.965 ) ; _shelx_hkl_checksum 85511 _shelx_SHELXL_version_number '2014/7' _olex2_submission_special_instructions 'No special instructions were received'