data_ps301 loop_ _publ_author_name _publ_author_address 'Samuel, P. P.' ; Institut f\"ur Anorganische Chemie Georg-August-Universit\"at G\"ottingen Tammannstr. 4, 37077 G\"ottingen (Germany) ; 'Yan Li' ; State Key Laboratory of Physical Chemistry of Solid Surfaces College of Chemistry and Chemical Engineering Xiamen University Xiamen, Fujian, 361005, China ; 'Roesky, H. W.' ; Institut f\"r Anorganische Chemie Georg-August-Universit\"at G\"ottingen Tammanstr. 4, 37077 G\"ottingen (Germany) ; 'Veniamin Chevelkov' ; Division of Solid-State NMR spectroscopy, Max Planck Institute for Biophysical Chemistry , Am Fassberg 11, D-37077, G\"ottingen, (Germany) ; 'Adam Lange' ; Division of Solid-State NMR spectroscopy, Max Planck Institute for Biophysical Chemistry , Am Fassberg 11, D-37077, G\"ottingen, (Germany) ; 'Burkhardt, A.' ; Deutsches Electronen-Synchrotron Notkestr. 85, 22607 Hamburg (Germany) ; 'Dittrich, B.' ; nstitut f\"ur Anorganische und Angewandte Chemie, Universit\"at Hamburg, Martin-Luther-King-Platz 6, D-20146 Hamburg, (Germany) ; _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H25 N2, F3 Ge' _chemical_formula_sum 'C15 H25 F3 Ge N2' _chemical_formula_weight 362.98 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ge' 'Ge' 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _cell_length_a 9.3477(11) _cell_length_b 10.5608(12) _cell_length_c 17.8086(19) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1758.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4869 _cell_measurement_theta_min 2.242 _cell_measurement_theta_max 26.46 #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APEX2 v2012.2 (Bruker AXS, 2012)' _computing_cell_refinement 'SAINT V8.32B' _computing_data_reduction 'SAINT V8.32B' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_publication_material 'enCIFer 1.4, CCDC, 2011' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Shelxle (Huebschle, 2013)' #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.367 _exptl_crystal_F_000 752 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.98 _exptl_crystal_size_mid 0.49 _exptl_crystal_size_min 0.21 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.766 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6604 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details ; SADABS version 2008/2, multi-scan. (G. M. Sheldrick, 2008) ; _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'INCOATEC Mo Microsource' _diffrn_measurement_device_type 'Bruker Smart APEX II Quazar' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15229 _diffrn_reflns_av_unetI/netI 0.0390 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.242 _diffrn_reflns_theta_max 27.546 _diffrn_reflns_theta_full 25.241 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 4054 _reflns_number_gt 3642 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.752 _reflns_Friedel_fraction_max 1.000 _reflns_Friedel_fraction_full 1.000 _diffrn_orient_matrix_UB_11 -2.2569629e-03 _diffrn_orient_matrix_UB_12 -7.5388779e-03 _diffrn_orient_matrix_UB_13 -5.5961803e-02 _diffrn_orient_matrix_UB_21 -1.0682275e-01 _diffrn_orient_matrix_UB_22 -4.5135273e-03 _diffrn_orient_matrix_UB_23 1.4008259e-03 _diffrn_orient_matrix_UB_31 -5.2944073e-03 _diffrn_orient_matrix_UB_32 9.4281070e-02 _diffrn_orient_matrix_UB_33 -4.4077407e-03 _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. ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; ADPs in the disordered parts of the molecule were restrained. The structure was refined as a 2-component inversion twin. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+0.0367P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.319(12) _chemical_absolute_configuration ? _refine_ls_number_reflns 4054 _refine_ls_number_parameters 256 _refine_ls_number_restraints 177 _refine_ls_R_factor_all 0.0360 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0587 _refine_ls_wR_factor_gt 0.0566 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_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 Ge1 Ge 0.83463(11) 0.38698(13) 0.42373(7) 0.02351(16) Uani 0.910(3) 1 d . U P A 1 F11 F 0.8974(3) 0.52208(19) 0.36899(12) 0.0344(6) Uani 0.910(3) 1 d . U P A 1 F12 F 0.7984(2) 0.30086(19) 0.33858(11) 0.0426(6) Uani 0.910(3) 1 d . U P A 1 F13 F 1.0136(2) 0.32518(19) 0.42697(12) 0.0319(5) Uani 0.910(3) 1 d . U P A 1 Ge2 Ge 0.8378(18) 0.3643(17) 0.4332(10) 0.055(4) Uani 0.090(3) 1 d . U P A 2 F21 F 0.718(3) 0.486(2) 0.4066(13) 0.052(5) Uani 0.090(3) 1 d . U P A 2 F22 F 0.7984(2) 0.30086(19) 0.33858(11) 0.0426(6) Uani 0.090(3) 1 d . U P A 2 F23 F 0.988(3) 0.475(3) 0.3935(13) 0.044(5) Uani 0.090(3) 1 d . U P A 2 N1 N 0.2073(2) 0.3942(3) 0.30377(12) 0.0217(5) Uani 1 1 d . U . . . H1 H 0.1425 0.3808 0.3387 0.026 Uiso 1 1 calc R U . . . N2 N 0.0166(3) 0.4368(2) 0.22890(13) 0.0220(5) Uani 1 1 d . U . . . H2 H -0.0246 0.4607 0.2710 0.039(10) Uiso 1 1 calc R . . . . C1 C 0.1546(3) 0.4116(2) 0.23551(14) 0.0169(6) Uani 1 1 d . U . . . C2 C 0.2479(3) 0.4029(3) 0.16814(15) 0.0178(6) Uani 1 1 d . U . . . C3 C 0.3094(3) 0.5119(3) 0.13916(16) 0.0227(7) Uani 1 1 d . U . . . H3 H 0.2938 0.5913 0.1628 0.027 Uiso 1 1 calc R U . . . C4 C 0.3943(3) 0.5039(3) 0.0752(2) 0.0303(7) Uani 1 1 d . U . . . H4 H 0.4378 0.5779 0.0554 0.036 Uiso 1 1 calc R U . . . C5 C 0.4153(3) 0.3885(4) 0.04053(17) 0.0339(7) Uani 1 1 d . U . . . H5 H 0.4728 0.3834 -0.0034 0.041 Uiso 1 1 calc R U . . . C6 C 0.3526(4) 0.2795(3) 0.06978(19) 0.0307(7) Uani 1 1 d . U . . . H6 H 0.3673 0.2001 0.0458 0.037 Uiso 1 1 calc R U . . . C7 C 0.2691(3) 0.2866(3) 0.13342(16) 0.0225(7) Uani 1 1 d . U . . . H7 H 0.2262 0.2124 0.1535 0.027 Uiso 1 1 calc R U . . . C8 C 0.3589(3) 0.3934(3) 0.33165(15) 0.0209(6) Uani 1 1 d . U . . . C12 C -0.0827(3) 0.4319(3) 0.16293(16) 0.0226(7) Uani 1 1 d . U . . . C13 C -0.0211(4) 0.4898(3) 0.09137(16) 0.0308(8) Uani 1 1 d . U . . . H13A H 0.0531 0.4339 0.0711 0.046 Uiso 1 1 calc R U . . . H13B H 0.0206 0.5727 0.1029 0.046 Uiso 1 1 calc R U . . . H13C H -0.0976 0.5000 0.0542 0.046 Uiso 1 1 calc R U . . . C14 C -0.1263(4) 0.2944(3) 0.15107(19) 0.0320(8) Uani 1 1 d . U . . . H14A H -0.2007 0.2899 0.1124 0.048 Uiso 1 1 calc R U . . . H14B H -0.1635 0.2596 0.1982 0.048 Uiso 1 1 calc R U . . . H14C H -0.0429 0.2451 0.1350 0.048 Uiso 1 1 calc R U . . . C15 C -0.2114(3) 0.5097(3) 0.18791(19) 0.0331(8) Uani 1 1 d . U . . . H15A H -0.2836 0.5098 0.1480 0.050 Uiso 1 1 calc R U . . . H15B H -0.1811 0.5968 0.1983 0.050 Uiso 1 1 calc R U . . . H15C H -0.2522 0.4724 0.2335 0.050 Uiso 1 1 calc R U . . . C9A C 0.4555(5) 0.3035(5) 0.2859(2) 0.0246(10) Uani 0.910(3) 1 d . U P A 1 H91A H 0.4728 0.3398 0.2361 0.037 Uiso 0.910(3) 1 calc R U P A 1 H92A H 0.4080 0.2212 0.2805 0.037 Uiso 0.910(3) 1 calc R U P A 1 H93A H 0.5468 0.2922 0.3120 0.037 Uiso 0.910(3) 1 calc R U P A 1 C10A C 0.3501(5) 0.3417(4) 0.4115(2) 0.0292(9) Uani 0.910(3) 1 d . U P A 1 H111 H 0.3112 0.2555 0.4104 0.044 Uiso 0.910(3) 1 calc R U P A 1 H121 H 0.2874 0.3960 0.4417 0.044 Uiso 0.910(3) 1 calc R U P A 1 H131 H 0.4459 0.3403 0.4338 0.044 Uiso 0.910(3) 1 calc R U P A 1 C11A C 0.4186(11) 0.5260(8) 0.3314(4) 0.0358(16) Uani 0.910(3) 1 d . U P A 1 H141 H 0.4228 0.5575 0.2797 0.054 Uiso 0.910(3) 1 calc R U P A 1 H151 H 0.5150 0.5255 0.3530 0.054 Uiso 0.910(3) 1 calc R U P A 1 H161 H 0.3567 0.5813 0.3613 0.054 Uiso 0.910(3) 1 calc R U P A 1 C9B C 0.422(5) 0.307(6) 0.306(3) 0.027(6) Uani 0.090(3) 1 d . U P A 2 H91B H 0.3545 0.2389 0.2943 0.040 Uiso 0.090(3) 1 calc R U P A 2 H92B H 0.4923 0.2769 0.3426 0.040 Uiso 0.090(3) 1 calc R U P A 2 H93B H 0.4708 0.3341 0.2602 0.040 Uiso 0.090(3) 1 calc R U P A 2 C10B C 0.339(6) 0.396(5) 0.420(3) 0.033(6) Uani 0.090(3) 1 d . U P A 2 H102 H 0.3102 0.4815 0.4361 0.050 Uiso 0.090(3) 1 calc R U P A 2 H112 H 0.4300 0.3743 0.4447 0.050 Uiso 0.090(3) 1 calc R U P A 2 H122 H 0.2656 0.3352 0.4352 0.050 Uiso 0.090(3) 1 calc R U P A 2 C11B C 0.418(13) 0.541(10) 0.313(5) 0.031(6) Uani 0.090(3) 1 d . U P A 2 H132 H 0.4236 0.5535 0.2588 0.046 Uiso 0.090(3) 1 calc R U P A 2 H142 H 0.5126 0.5529 0.3356 0.046 Uiso 0.090(3) 1 calc R U P A 2 H152 H 0.3510 0.6030 0.3347 0.046 Uiso 0.090(3) 1 calc R U P A 2 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 Ge1 0.0164(2) 0.0301(4) 0.0239(3) 0.0048(3) 0.0057(2) 0.0012(3) F11 0.0482(15) 0.0224(11) 0.0324(12) 0.0015(9) 0.0076(10) 0.0025(10) F12 0.0482(14) 0.0387(11) 0.0408(11) 0.0030(9) -0.0159(10) -0.0158(10) F13 0.0202(10) 0.0435(12) 0.0320(11) -0.0012(10) -0.0043(10) 0.0068(9) Ge2 0.060(5) 0.051(6) 0.053(5) 0.018(4) -0.012(4) -0.007(4) F21 0.045(9) 0.054(10) 0.058(12) -0.006(9) -0.018(9) 0.012(9) F22 0.0482(14) 0.0387(11) 0.0408(11) 0.0030(9) -0.0159(10) -0.0158(10) F23 0.043(9) 0.054(10) 0.036(9) -0.022(8) 0.015(8) -0.016(8) N1 0.0127(10) 0.0330(14) 0.0195(11) -0.0001(12) 0.0010(8) 0.0006(11) N2 0.0170(12) 0.0300(14) 0.0190(12) 0.0008(10) -0.0004(10) 0.0038(11) C1 0.0172(13) 0.0112(14) 0.0224(13) -0.0003(10) 0.0002(11) 0.0001(12) C2 0.0146(13) 0.0208(16) 0.0181(13) -0.0003(12) -0.0017(10) 0.0013(13) C3 0.0244(18) 0.0201(15) 0.0235(15) 0.0000(12) -0.0013(12) -0.0025(13) C4 0.0303(16) 0.0344(17) 0.0262(15) 0.0089(16) 0.0019(16) -0.0084(14) C5 0.0313(17) 0.047(2) 0.0230(15) -0.0011(17) 0.0097(13) 0.004(2) C6 0.0356(18) 0.0295(16) 0.0270(16) -0.0053(14) 0.0048(17) 0.0046(15) C7 0.0265(16) 0.0188(15) 0.0222(15) 0.0013(12) 0.0015(13) 0.0006(13) C8 0.0120(13) 0.0265(14) 0.0241(13) -0.0005(13) -0.0035(10) -0.0002(13) C12 0.0188(15) 0.0268(16) 0.0223(15) 0.0010(13) -0.0060(12) 0.0006(13) C13 0.0305(18) 0.0380(19) 0.0240(18) 0.0100(14) -0.0072(13) -0.0014(15) C14 0.033(2) 0.0298(17) 0.0337(18) 0.0003(14) -0.0039(14) -0.0055(15) C15 0.0217(17) 0.040(2) 0.0380(19) -0.0019(16) -0.0072(14) 0.0088(15) C9A 0.013(2) 0.033(2) 0.029(2) -0.0016(19) 0.0023(15) 0.0046(18) C10A 0.0196(18) 0.043(2) 0.025(2) 0.0008(19) -0.0027(15) 0.005(2) C11A 0.038(2) 0.024(3) 0.046(5) 0.002(3) -0.017(3) -0.004(2) C9B 0.009(11) 0.035(10) 0.035(12) -0.004(11) -0.009(11) 0.001(9) C10B 0.020(11) 0.057(14) 0.023(8) 0.009(11) -0.003(9) -0.001(13) C11B 0.033(11) 0.026(9) 0.034(14) -0.004(11) -0.007(13) -0.011(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 F13 1.796(2) . ? Ge1 F12 1.800(2) . ? Ge1 F11 1.825(2) . ? Ge2 F21 1.77(3) . ? Ge2 F23 1.96(3) . ? N1 C1 1.325(3) . ? N1 C8 1.502(3) . ? N2 C1 1.322(3) . ? N2 C12 1.498(3) . ? C1 C2 1.486(4) . ? C2 C3 1.386(4) . ? C2 C7 1.389(4) . ? C3 C4 1.390(4) . ? C4 C5 1.380(5) . ? C5 C6 1.393(5) . ? C6 C7 1.378(4) . ? C8 C9B 1.17(6) . ? C8 C11A 1.507(9) . ? C8 C10A 1.526(5) . ? C8 C9A 1.543(5) . ? C8 C10B 1.59(5) . ? C8 C11B 1.69(9) . ? C12 C15 1.523(4) . ? C12 C14 1.524(5) . ? C12 C13 1.526(4) . ? 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 F13 Ge1 F12 91.07(11) . . ? F13 Ge1 F11 90.10(12) . . ? F12 Ge1 F11 90.31(10) . . ? F21 Ge2 F23 85.7(14) . . ? C1 N1 C8 131.0(2) . . ? C1 N2 C12 131.8(2) . . ? N2 C1 N1 118.2(2) . . ? N2 C1 C2 120.9(2) . . ? N1 C1 C2 120.9(2) . . ? C3 C2 C7 120.6(2) . . ? C3 C2 C1 119.5(2) . . ? C7 C2 C1 119.8(2) . . ? C2 C3 C4 119.4(3) . . ? C5 C4 C3 120.1(3) . . ? C4 C5 C6 120.1(3) . . ? C7 C6 C5 120.0(3) . . ? C6 C7 C2 119.7(3) . . ? C9B C8 N1 110(3) . . ? N1 C8 C11A 110.1(4) . . ? N1 C8 C10A 105.0(3) . . ? C11A C8 C10A 110.9(4) . . ? N1 C8 C9A 112.4(3) . . ? C11A C8 C9A 110.7(5) . . ? C10A C8 C9A 107.7(3) . . ? C9B C8 C10B 117(3) . . ? N1 C8 C10B 103(2) . . ? C9B C8 C11B 119(5) . . ? N1 C8 C11B 104(4) . . ? C10B C8 C11B 102(4) . . ? N2 C12 C15 104.0(2) . . ? N2 C12 C14 107.9(2) . . ? C15 C12 C14 110.1(3) . . ? N2 C12 C13 114.1(2) . . ? C15 C12 C13 109.0(3) . . ? C14 C12 C13 111.5(3) . . ? _refine_diff_density_max 0.274 _refine_diff_density_min -0.190 _refine_diff_density_rms 0.050 _shelxl_version_number 2013-4 _shelx_res_file ; TITL solve in P2(1)2(1)2(1) CELL 0.7107 9.3477 10.5608 17.8086 90.000 90.000 90.000 ZERR 4.00 0.0011 0.0012 0.0019 0.0000 0.0000 0.0000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H N F Ge UNIT 60 100 8 12 4 L.S. 10 TEMP -173 BOND LIST 4 SIMU 0.01 f11 f21 f12 f22 f13 f23 ge1 ge2 EXYZ f12 f22 EADP f12 f22 ACTA TWIN FMAP 2 PLAN 20 DELU SIMU 0.005 C10A C10B C9A C9B C11A C11B WGHT 0.027700 0.036700 BASF 0.31923 FVAR 0.46501 0.90977 PART 1 GE1 5 0.834630 0.386978 0.423730 21.00000 0.01644 0.03013 = 0.02394 0.00476 0.00570 0.00123 F11 4 0.897422 0.522081 0.368986 21.00000 0.04822 0.02243 = 0.03243 0.00151 0.00765 0.00247 F12 4 0.798409 0.300864 0.338578 21.00000 0.04815 0.03874 = 0.04082 0.00298 -0.01587 -0.01582 F13 4 1.013572 0.325179 0.426970 21.00000 0.02015 0.04352 = 0.03196 -0.00120 -0.00434 0.00684 PART 2 GE2 5 0.837800 0.364301 0.433191 -21.00000 0.06023 0.05070 = 0.05325 0.01811 -0.01214 -0.00720 F21 4 0.717754 0.485611 0.406606 -21.00000 0.04459 0.05375 = 0.05771 -0.00565 -0.01803 0.01163 F22 4 0.798409 0.300864 0.338578 -21.00000 0.04815 0.03874 = 0.04082 0.00298 -0.01587 -0.01582 F23 4 0.988243 0.475444 0.393450 -21.00000 0.04329 0.05402 = 0.03619 -0.02190 0.01511 -0.01649 PART 0 N1 3 0.207316 0.394190 0.303771 11.00000 0.01269 0.03301 = 0.01949 -0.00014 0.00101 0.00065 AFIX 43 H1 2 0.142507 0.380766 0.338717 11.00000 -1.20000 AFIX 0 N2 3 0.016553 0.436756 0.228902 11.00000 0.01703 0.02997 = 0.01895 0.00080 -0.00045 0.00384 AFIX 43 H2 2 -0.024562 0.460714 0.271023 11.00000 0.03863 AFIX 0 C1 1 0.154551 0.411630 0.235506 11.00000 0.01722 0.01115 = 0.02242 -0.00026 0.00022 0.00008 C2 1 0.247877 0.402923 0.168142 11.00000 0.01456 0.02083 = 0.01814 -0.00030 -0.00173 0.00126 C3 1 0.309438 0.511888 0.139155 11.00000 0.02435 0.02007 = 0.02355 -0.00004 -0.00127 -0.00246 AFIX 43 H3 2 0.293785 0.591347 0.162774 11.00000 -1.20000 AFIX 0 C4 1 0.394267 0.503852 0.075227 11.00000 0.03032 0.03442 = 0.02625 0.00892 0.00190 -0.00840 AFIX 43 H4 2 0.437823 0.577916 0.055379 11.00000 -1.20000 AFIX 0 C5 1 0.415350 0.388495 0.040525 11.00000 0.03130 0.04749 = 0.02298 -0.00109 0.00970 0.00364 AFIX 43 H5 2 0.472774 0.383417 -0.003385 11.00000 -1.20000 AFIX 0 C6 1 0.352561 0.279460 0.069777 11.00000 0.03565 0.02954 = 0.02696 -0.00526 0.00484 0.00462 AFIX 43 H6 2 0.367310 0.200145 0.045829 11.00000 -1.20000 AFIX 0 C7 1 0.269083 0.286608 0.133423 11.00000 0.02653 0.01876 = 0.02224 0.00133 0.00151 0.00057 AFIX 43 H7 2 0.226244 0.212362 0.153461 11.00000 -1.20000 AFIX 0 C8 1 0.358942 0.393437 0.331652 11.00000 0.01197 0.02652 = 0.02413 -0.00047 -0.00351 -0.00018 C12 1 -0.082663 0.431947 0.162931 11.00000 0.01879 0.02684 = 0.02226 0.00102 -0.00597 0.00062 C13 1 -0.021136 0.489834 0.091374 11.00000 0.03051 0.03803 = 0.02396 0.01004 -0.00724 -0.00145 AFIX 137 H13A 2 0.053103 0.433943 0.071096 11.00000 -1.50000 H13B 2 0.020573 0.572732 0.102874 11.00000 -1.50000 H13C 2 -0.097571 0.500004 0.054196 11.00000 -1.50000 AFIX 0 C14 1 -0.126335 0.294357 0.151068 11.00000 0.03263 0.02980 = 0.03371 0.00032 -0.00391 -0.00554 AFIX 137 H14A 2 -0.200688 0.289894 0.112363 11.00000 -1.50000 H14B 2 -0.163481 0.259592 0.198218 11.00000 -1.50000 H14C 2 -0.042920 0.245112 0.134996 11.00000 -1.50000 AFIX 0 C15 1 -0.211363 0.509688 0.187914 11.00000 0.02166 0.03974 = 0.03801 -0.00187 -0.00715 0.00882 AFIX 137 H15A 2 -0.283592 0.509832 0.148028 11.00000 -1.50000 H15B 2 -0.181140 0.596817 0.198253 11.00000 -1.50000 H15C 2 -0.252175 0.472440 0.233537 11.00000 -1.50000 AFIX 0 PART 1 C9A 1 0.455462 0.303473 0.285898 21.00000 0.01252 0.03268 = 0.02866 -0.00158 0.00227 0.00460 AFIX 137 H91A 2 0.472820 0.339849 0.236099 21.00000 -1.50000 H92A 2 0.408047 0.221215 0.280484 21.00000 -1.50000 H93A 2 0.546824 0.292214 0.312050 21.00000 -1.50000 AFIX 0 C10A 1 0.350054 0.341691 0.411519 21.00000 0.01963 0.04336 = 0.02454 0.00078 -0.00273 0.00504 AFIX 137 H111 2 0.311187 0.255529 0.410375 21.00000 -1.50000 H121 2 0.287381 0.396016 0.441655 21.00000 -1.50000 H131 2 0.445886 0.340295 0.433818 21.00000 -1.50000 AFIX 0 C11A 1 0.418578 0.526035 0.331372 21.00000 0.03789 0.02351 = 0.04603 0.00243 -0.01669 -0.00373 AFIX 137 H141 2 0.422841 0.557514 0.279654 21.00000 -1.50000 H151 2 0.515009 0.525479 0.352961 21.00000 -1.50000 H161 2 0.356658 0.581326 0.361318 21.00000 -1.50000 AFIX 0 PART 2 C9B 1 0.421748 0.307276 0.306125 -21.00000 0.00944 0.03479 = 0.03544 -0.00398 -0.00936 0.00059 AFIX 137 H91B 2 0.354513 0.238937 0.294276 -21.00000 -1.50000 H92B 2 0.492305 0.276898 0.342623 -21.00000 -1.50000 H93B 2 0.470834 0.334097 0.260174 -21.00000 -1.50000 AFIX 0 C10B 1 0.339295 0.396406 0.420455 -21.00000 0.01962 0.05654 = 0.02293 0.00858 -0.00336 -0.00114 AFIX 137 H102 2 0.310160 0.481528 0.436148 -21.00000 -1.50000 H112 2 0.430020 0.374296 0.444715 -21.00000 -1.50000 H122 2 0.265615 0.335222 0.435153 -21.00000 -1.50000 AFIX 0 C11B 1 0.417697 0.541170 0.313262 -21.00000 0.03250 0.02613 = 0.03415 -0.00418 -0.00712 -0.01125 AFIX 137 H132 2 0.423582 0.553490 0.258808 -21.00000 -1.50000 H142 2 0.512620 0.552915 0.335560 -21.00000 -1.50000 H152 2 0.351037 0.602970 0.334731 -21.00000 -1.50000 PART 0 AFIX 0 HKLF 4 REM solve in P2(1)2(1)2(1) REM R1 = 0.0281 for 3642 Fo > 4sig(Fo) and 0.0360 for all 4054 data REM 256 parameters refined using 177 restraints END WGHT 0.0277 0.0367 REM Highest difference peak 0.274, deepest hole -0.190, 1-sigma level 0.050 Q1 1 0.7710 0.3593 0.3681 11.00000 0.05 0.27 Q2 1 0.8338 0.3949 0.3535 11.00000 0.05 0.26 Q3 1 0.8424 0.3921 0.4876 11.00000 0.05 0.25 Q4 1 0.8337 0.4909 0.3950 11.00000 0.05 0.24 Q5 1 -0.0496 0.4772 0.1293 11.00000 0.05 0.22 Q6 1 0.3451 0.2923 0.1139 11.00000 0.05 0.21 Q7 1 0.1162 0.3573 0.0744 11.00000 0.05 0.20 Q8 1 0.4150 0.3418 0.0688 11.00000 0.05 0.20 Q9 1 0.2344 0.3581 0.1474 11.00000 0.05 0.20 Q10 1 0.8255 0.2896 0.3958 11.00000 0.05 0.20 Q11 1 0.2879 0.2737 0.4205 11.00000 0.05 0.19 Q12 1 0.2230 0.2608 0.1400 11.00000 0.05 0.19 Q13 1 0.8155 0.4814 0.4563 11.00000 0.05 0.19 Q14 1 0.2865 0.3972 0.3184 11.00000 0.05 0.19 Q15 1 1.0192 0.3945 0.3864 11.00000 0.05 0.19 Q16 1 0.9054 0.2995 0.4486 11.00000 0.05 0.18 Q17 1 0.7394 0.4115 0.3205 11.00000 0.05 0.18 Q18 1 0.2780 0.2936 0.0915 11.00000 0.05 0.18 Q19 1 0.8048 0.2954 0.4581 11.00000 0.05 0.18 Q20 1 0.7784 0.3203 0.3152 11.00000 0.05 0.18 ; _shelx_res_checksum 82062 _shelx_hkl_file ; -1 0 0 1.48817 1.32838 1 1 0 0 -1.5213 1.19424 1 -1 0 0 -0.5081 0.86495 2 -2 0 0 837.351 23.7612 2 -2 0 0 828.035 26.6987 1 -3 0 0 -3.5006 2.91522 1 -3 0 0 -3.8390 1.90007 2 -4 0 0 340.049 13.0807 1 -4 0 0 339.971 10.9748 2 -5 0 0 0.82803 3.67461 1 -6 0 0 1515.13 49.6993 1 -7 0 0 1.55997 4.65046 1 -8 0 0 36.1902 6.79643 1 -9 0 0 -1.7433 6.08416 1 -10 0 0 58.0575 9.59854 3 -10 0 0 57.2739 8.93833 1 -11 0 0 4.13627 7.80841 1 -11 0 0 -5.3327 8.82217 3 -12 0 0 160.083 15.8012 3 -12 0 0 177.975 15.1352 1 0 1 0 -2.1703 0.92152 1 0 1 0 -1.9262 1.06123 3 0 1 0 -3.1641 0.93715 2 0 -1 0 -2.1749 0.92307 1 1 -1 0 18.3888 2.04314 1 -1 1 0 15.8778 2.06053 1 -1 -1 0 13.0259 1.83809 1 -1 1 0 13.8606 2.12977 3 1 1 0 12.4128 1.75941 1 -1 1 0 11.5930 1.71177 2 -2 1 0 5286.55 164.363 1 -2 1 0 4987.23 147.813 2 -2 -1 0 5151.09 145.048 2 -2 -1 0 5129.36 163.559 1 -2 1 0 5418.16 167.996 3 -3 1 0 34.9227 3.72721 3 -3 1 0 24.9643 3.46498 1 -3 1 0 33.0696 3.07391 2 -3 -1 0 29.2790 2.06595 2 -4 1 0 865.693 26.1926 2 -4 1 0 870.028 29.4385 1 -4 1 0 908.095 30.2785 3 -4 -1 0 894.949 29.3742 1 -5 1 0 479.944 15.6753 2 -5 1 0 481.067 18.5565 3 -5 1 0 498.500 18.1873 1 -5 -1 0 493.206 17.9477 1 -6 1 0 23.3022 4.86182 3 -6 1 0 20.3152 4.75287 1 -6 -1 0 22.1680 4.85723 1 -7 1 0 171.549 11.1485 3 -7 -1 0 177.165 10.3630 1 -7 1 0 177.036 11.0662 1 -8 1 0 193.640 12.2061 1 -8 1 0 203.953 13.2938 3 -8 -1 0 220.106 12.7248 1 -9 1 0 32.3802 7.33223 1 -9 1 0 9.31162 7.11263 3 -9 -1 0 10.1327 6.55302 1 -10 -1 0 93.7151 10.4116 1 -10 1 0 107.907 11.6190 3 -10 1 0 102.357 10.9079 1 -11 1 0 53.4731 10.7456 3 -11 -1 0 77.9598 10.2540 1 -11 -1 0 59.2123 11.1299 3 -11 1 0 85.7084 10.9103 1 -12 -1 0 47.9134 10.2924 1 -12 1 0 50.0067 11.7707 3 -12 1 0 56.2778 10.8489 1 -12 -1 0 29.9854 11.4742 3 0 2 0 1708.13 48.6996 2 0 2 0 1788.11 55.4323 3 0 -2 0 1711.69 54.4111 1 0 2 0 1717.59 54.3983 1 -1 2 0 1782.25 50.3220 2 -1 2 0 1704.82 55.4475 1 -1 -2 0 1703.53 55.3514 1 1 2 0 1773.07 57.1544 3 -1 2 0 1933.27 57.7597 3 -2 2 0 140.088 6.73066 1 -2 2 0 146.025 7.05286 3 -2 -2 0 140.573 6.35238 1 -2 2 0 143.286 6.31809 2 -3 -2 0 1627.43 52.0352 1 -3 2 0 1699.73 52.3093 1 -3 2 0 1679.80 53.6100 3 -3 2 0 1566.09 47.1382 2 -4 -2 0 64.4914 5.27837 1 -4 2 0 58.4326 5.14152 1 -4 2 0 41.8992 4.91985 3 -4 2 0 58.8256 4.43976 2 -5 -2 0 1322.96 43.0212 1 -5 2 0 1318.48 43.2241 1 -5 2 0 1288.02 44.1826 3 -5 2 0 1315.95 38.6559 2 -6 2 0 23.4919 5.26664 1 -6 -2 0 32.3198 5.14464 1 -6 2 0 19.7547 5.21067 3 -7 2 0 210.020 12.1054 3 -7 -2 0 212.719 11.3904 1 -7 2 0 197.216 11.6744 1 -8 2 0 7.29989 6.40150 3 -8 2 0 22.4552 6.44018 1 -8 -2 0 7.50006 5.81443 1 -9 2 0 214.112 13.8012 1 -9 2 0 214.201 15.0006 3 -9 -2 0 219.405 13.3615 1 -10 2 0 51.6189 9.07910 1 -10 -2 0 37.6941 8.55131 1 -10 2 0 33.3384 8.98359 3 -11 2 0 114.029 12.9880 3 -11 -2 0 119.381 12.1018 1 -11 2 0 146.609 13.0067 1 -12 2 0 29.4760 9.96258 1 -12 -2 0 22.6746 9.41575 1 -12 2 0 9.88671 10.5046 3 0 3 0 -0.1027 2.26610 1 0 3 0 -4.0891 2.27875 2 0 3 0 0.58993 2.56621 3 -1 -3 0 59.6332 4.33554 1 -1 3 0 74.9607 5.02004 3 -1 3 0 55.2429 4.58775 1 1 3 0 76.9307 5.33276 3 -1 3 0 55.3749 4.46911 2 -2 -3 0 27.0590 3.24662 1 -2 3 0 20.8285 3.24477 2 -2 -3 0 28.7045 1.80736 2 -2 3 0 28.2041 3.67508 1 -2 3 0 32.3560 3.58594 3 -3 3 0 39.2812 4.04469 2 -3 -3 0 47.2904 4.44683 1 -3 3 0 36.0963 4.50536 3 -3 3 0 53.5267 4.84381 1 -4 3 0 82.4071 6.10741 2 -4 3 0 81.3231 7.12826 3 -4 3 0 99.4047 7.06762 1 -4 -3 0 89.1455 6.48823 1 -5 3 0 668.646 24.7146 1 -5 3 0 703.673 22.3840 2 -5 3 0 739.179 25.5521 3 -5 -3 0 697.167 24.5464 1 -6 3 0 115.991 8.92156 1 -6 3 0 129.872 9.54036 3 -6 -3 0 142.192 8.86715 1 -7 -3 0 95.7142 8.26877 1 -7 3 0 100.914 8.67721 3 -7 3 0 98.4890 8.35573 1 -8 3 0 325.205 15.8600 1 -8 -3 0 298.902 15.0310 1 -8 3 0 313.001 16.4785 3 -9 3 0 66.3173 8.71633 1 -9 3 0 64.5556 9.32240 3 -9 -3 0 71.9227 8.71351 1 -10 -3 0 264.179 16.0154 1 -10 3 0 235.189 17.5567 3 -10 3 0 280.164 16.3918 1 -11 -3 0 37.2520 9.35074 1 -11 3 0 47.4958 9.99366 1 -11 3 0 55.3273 11.0105 3 0 4 0 353.672 12.5618 1 0 4 0 350.375 13.1068 3 0 4 0 334.650 11.4066 2 -1 4 0 376.739 13.7991 1 -1 -4 0 378.962 13.8420 1 -1 4 0 390.428 12.9706 2 -1 4 0 397.904 14.3249 3 1 4 0 382.937 14.5095 3 -2 4 0 504.067 17.3529 1 -2 4 0 468.848 15.9226 2 -2 -4 0 503.197 17.1090 1 2 4 0 465.674 17.9407 3 -2 4 0 502.129 17.6414 3 -3 4 0 22.6009 4.00001 2 -3 4 0 42.7765 4.73443 1 -3 4 0 20.9276 4.00863 3 -3 -4 0 30.9014 4.11638 1 -4 -4 0 254.263 10.8046 1 -4 4 0 252.521 10.5624 2 -4 4 0 248.209 11.3754 3 -4 4 0 229.705 10.9779 1 -5 4 0 17.9512 4.89795 3 -5 4 0 13.8427 4.20848 2 -5 4 0 9.12430 4.54467 1 -5 -4 0 13.7049 4.41398 1 -6 4 0 1020.22 36.7369 3 -6 -4 0 1031.62 35.4030 1 -6 4 0 1057.68 35.9368 1 -7 4 0 8.08350 5.81316 1 -7 -4 0 10.5985 5.65118 1 -7 4 0 0.71130 5.72340 3 -8 4 0 28.8586 7.76427 3 -8 -4 0 56.0963 7.61869 1 -8 4 0 39.2793 7.67031 1 -9 4 0 122.498 10.8281 1 -9 -4 0 137.380 11.4574 1 -9 4 0 110.615 11.4559 3 -10 -4 0 226.389 15.5238 1 -10 4 0 234.328 15.8368 1 -10 4 0 225.209 17.6963 3 -11 4 0 1.76507 10.0300 3 -11 4 0 2.61216 8.60100 1 -11 -4 0 0.36635 7.32579 1 0 5 0 2.99923 3.02452 1 0 5 0 4.44033 3.42971 3 1 5 0 6.82405 3.74926 3 -1 5 0 8.51287 3.49783 1 -1 5 0 2.62627 3.23568 3 -1 5 0 5.71969 3.50928 2 -1 -5 0 5.16358 3.49297 1 2 5 0 574.938 21.4545 3 -2 -5 0 572.570 20.3594 1 -2 5 0 573.770 20.5064 1 -2 5 0 593.346 21.0142 3 -2 5 0 620.033 19.1708 2 -3 -5 0 69.8982 5.89488 1 -3 -5 0 66.9941 3.30890 2 -3 5 0 70.7525 5.58471 3 -3 5 0 73.1814 5.89887 1 -3 5 0 59.6377 5.52894 2 -4 5 0 137.910 8.42489 3 -4 5 0 139.527 8.45989 2 -4 5 0 117.639 8.34266 1 -4 -5 0 126.665 7.80100 1 -5 -5 0 428.379 16.9040 1 -5 5 0 407.856 17.3851 3 -5 5 0 424.226 17.2269 1 -6 5 0 9.30610 5.30299 1 -6 5 0 9.42900 5.50606 3 -6 -5 0 5.20575 4.88407 1 -7 5 0 341.916 17.8695 3 -7 5 0 388.302 17.4217 1 -7 -5 0 393.251 17.1591 1 -8 -5 0 60.4638 7.94511 1 -8 5 0 59.6974 8.80975 1 -8 5 0 53.9974 8.83192 3 -9 5 0 4.18089 7.85477 3 -9 5 0 -1.1847 7.40755 1 -9 -5 0 2.15975 6.43016 1 -10 5 0 25.3722 9.04234 1 -10 -5 0 24.6021 7.85416 1 -10 5 0 19.3905 9.40198 3 -11 5 0 186.434 15.1840 1 -11 -5 0 158.200 13.4717 1 0 6 0 25.4852 4.09953 1 0 6 0 18.3763 4.21624 3 -1 6 0 2.13188 3.64072 3 -1 -6 0 5.72289 3.69926 1 1 6 0 4.21134 3.38646 1 -1 6 0 5.07349 3.67399 1 1 6 0 5.85089 4.01748 3 2 6 0 215.350 11.0652 3 -2 -6 0 211.264 9.96873 1 -2 6 0 227.541 10.1825 1 -2 6 0 200.573 10.3110 3 -3 6 0 967.236 32.6723 3 -3 -6 0 951.913 31.7554 1 -3 6 0 926.466 31.9126 1 -3 -6 0 917.180 27.1447 2 -4 -6 0 73.9271 6.49550 1 -4 6 0 88.8575 7.23923 1 -4 6 0 78.6444 6.81172 3 -5 -6 0 143.269 9.18452 1 -5 6 0 131.017 9.84417 3 -5 6 0 128.726 9.68148 1 -6 6 0 76.4243 8.12597 3 -6 -6 0 70.2924 7.58696 1 -6 6 0 72.3515 8.02845 1 -7 -6 0 34.8615 7.02483 1 -7 6 0 27.4327 7.39310 1 -7 6 0 43.0432 7.72352 3 -8 6 0 10.0228 7.33650 1 -8 -6 0 12.6292 6.48275 1 -8 6 0 2.87735 6.93128 3 -9 6 0 230.911 16.0978 1 -9 -6 0 233.781 14.4164 1 -9 6 0 214.814 16.2581 3 -10 -6 0 104.681 10.7358 1 -10 6 0 85.7063 11.7121 1 0 7 0 2.15383 4.02280 1 0 7 0 -1.8852 4.09880 3 1 7 0 76.5208 6.88211 3 -1 -7 0 72.3816 6.58498 1 -1 7 0 63.5690 6.12760 1 -1 7 0 96.6233 7.89568 3 -2 7 0 863.345 29.4611 1 2 7 0 826.002 30.6332 3 -2 -7 0 876.183 29.4996 1 -2 7 0 843.780 30.1016 3 -3 -7 0 26.7220 5.00704 1 -3 7 0 28.0985 5.22034 3 -3 7 0 21.3571 5.15743 1 -3 -7 0 26.3028 3.13695 2 -4 7 0 118.206 9.49031 3 -4 -7 0 119.782 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25.0428 1 0 -1 -4 787.092 25.2274 1 -1 1 4 1948.21 63.1332 1 1 1 -4 1998.66 57.2409 2 1 -1 4 2043.56 62.9260 1 -1 -1 -4 2030.58 63.3864 1 -1 1 4 2061.56 65.5542 3 1 1 -4 1949.48 62.4946 1 -1 -1 -4 2064.53 57.3942 2 1 1 4 2055.79 65.0105 3 -1 -1 4 2010.37 62.5727 1 -1 1 -4 2036.12 62.9715 1 -1 1 -4 2102.25 57.4374 2 1 -1 -4 2037.02 58.8988 2 2 1 -4 1555.30 49.1472 1 -2 -1 -4 1522.34 44.7787 2 2 1 -4 1693.63 44.8475 2 -2 1 4 1464.00 49.5633 1 -2 -1 -4 1625.27 49.9500 1 -2 1 4 1639.60 51.7408 3 -2 -1 4 1499.32 49.1448 1 2 1 4 1600.21 50.9904 3 -2 1 -4 1586.45 49.6700 1 -2 1 -4 1588.20 45.0829 2 2 -1 -4 1582.64 45.2371 2 -3 -1 -4 507.180 15.6883 2 -3 1 4 489.582 19.0513 3 -3 -1 -4 501.835 18.1776 1 -3 1 4 479.565 17.8144 1 3 1 -4 489.687 15.5989 2 -3 1 -4 540.411 16.2380 2 3 -1 -4 534.630 16.3277 2 -3 -1 4 562.317 17.6108 1 -3 1 -4 558.081 18.0847 1 4 1 -4 507.285 15.7804 2 -4 1 4 481.246 19.7756 3 -4 -1 -4 504.682 15.8272 2 -4 -1 -4 492.733 18.4880 1 -4 1 4 492.287 18.4458 1 -4 1 -4 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