data_spok119_0m _audit_creation_date 2018-09-21 _audit_creation_method ; Olex2 1.2-beta (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2016/6' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _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 '2(C7 H14 B10 N)' _chemical_formula_sum 'C14 H28 B20 N2' _chemical_formula_weight 440.58 _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' 'B' 'B' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 '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 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.5443(8) _cell_length_b 7.6742(10) _cell_length_c 21.996(3) _cell_angle_alpha 98.131(8) _cell_angle_beta 99.051(7) _cell_angle_gamma 90.522(7) _cell_volume 1244.3(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 5951 _cell_measurement_temperature 100 _cell_measurement_theta_max 68.050 _cell_measurement_theta_min 4.115 _shelx_estimated_absorpt_T_max 0.981 _shelx_estimated_absorpt_T_min 0.898 _exptl_absorpt_coefficient_mu 0.394 _exptl_absorpt_correction_T_max 0.7531 _exptl_absorpt_correction_T_min 0.6341 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1358 before and 0.0734 after correction. The Ratio of minimum to maximum transmission is 0.8420. The \l/2 correction factor is Not present.' _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.176 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 452 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0663 _diffrn_reflns_av_unetI/netI 0.0671 _diffrn_reflns_Laue_measured_fraction_full 0.976 _diffrn_reflns_Laue_measured_fraction_max 0.935 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 14151 _diffrn_reflns_point_group_measured_fraction_full 0.976 _diffrn_reflns_point_group_measured_fraction_max 0.935 _diffrn_reflns_theta_full 65.982 _diffrn_reflns_theta_max 65.982 _diffrn_reflns_theta_min 2.055 _diffrn_ambient_temperature 100.0 _diffrn_detector 'Bruker APEX2 area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 0.976 _diffrn_measured_fraction_theta_max 0.935 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\ms' _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3641 _reflns_number_total 4012 _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 V8.38A (?, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.38A (?, 2016)' _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 'ShelXS (Sheldrick, 2008)' _refine_diff_density_max 0.349 _refine_diff_density_min -0.405 _refine_diff_density_rms 0.090 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.549 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 326 _refine_ls_number_reflns 4012 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1309 _refine_ls_R_factor_gt 0.1231 _refine_ls_restrained_S_all 1.549 _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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3291 _refine_ls_wR_factor_ref 0.3435 _refine_special_details ; Refined as a 2-component twin. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.595(4) 0.405(4) 2. Fixed Uiso At 1.2 times of: All B(H) groups, All C(H) groups 3.a Aromatic/amide H refined with riding coordinates: C13(H13), C12(H12), C5(H5), C6(H6), C11(H11), C4(H4) 3.b Boron cage BH refined with riding coordinates: B14(H14), B7(H7), C1(H1), B18(H18), B6(H6A), B12(H12A), B9(H9), B10(H10), B19(H19), B4(H4A), B17(H17), B11(H11A), B15(H15), B1(H1A), B3(H3), C8(H8), B13(H13A), B16(H16), B20(H20), B8(H8A), B5(H5A), B2(H2) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _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 N2 N 0.8502(6) 0.6109(6) 0.0478(2) 0.0185(9) Uani 1 1 d . . . . . N1 N 1.0621(6) 0.1531(6) 0.4521(2) 0.0189(9) Uani 1 1 d . . . . . C9 C 0.6704(7) 0.7438(7) 0.1217(2) 0.0169(11) Uani 1 1 d . . . . . C13 C 1.0447(8) 0.3732(7) 0.0688(3) 0.0229(12) Uani 1 1 d . . . . . H13 H 1.130670 0.292641 0.055615 0.028 Uiso 1 1 calc R . . . . C12 C 0.9894(8) 0.3733(8) 0.1259(3) 0.0261(12) Uani 1 1 d . . . . . H12 H 1.036508 0.291043 0.152199 0.031 Uiso 1 1 calc R . . . . C3 C 1.0066(7) 0.2080(8) 0.3971(3) 0.0224(12) Uani 1 1 d . . . . . C14 C 0.9703(7) 0.4954(7) 0.0306(3) 0.0212(12) Uani 1 1 d . . . . . C2 C 1.1215(8) 0.3452(7) 0.3782(2) 0.0214(11) Uani 1 1 d . . . . . C7 C 0.9657(7) 0.0298(8) 0.4687(3) 0.0242(12) Uani 1 1 d . . . . . C5 C 0.7495(10) 0.0157(11) 0.3766(4) 0.046(2) Uani 1 1 d . . . . . H5 H 0.643432 -0.033936 0.350552 0.055 Uiso 1 1 calc R . . . . C10 C 0.7994(7) 0.6096(7) 0.1036(3) 0.0206(11) Uani 1 1 d . . . . . B14 B 0.7478(8) 0.9592(8) 0.1277(3) 0.0211(13) Uani 1 1 d . . . . . H14 H 0.886530 0.999730 0.121908 0.025 Uiso 1 1 calc R . . . . B7 B 1.0381(12) 0.4974(10) 0.3331(3) 0.0350(18) Uani 1 1 d . . . . . H7 H 0.893418 0.504965 0.312371 0.042 Uiso 1 1 calc R . . . . C6 C 0.8070(9) -0.0413(10) 0.4336(4) 0.0380(16) Uani 1 1 d . . . . . H6 H 0.738766 -0.127128 0.447898 0.046 Uiso 1 1 calc R . . . . C1 C 1.2920(10) 0.4269(9) 0.4298(3) 0.0323(15) Uani 1 1 d . . . . . H1 H 1.314264 0.384341 0.477035 0.039 Uiso 1 1 calc R . . . . B18 B 0.6268(9) 1.0798(9) 0.1814(3) 0.0254(14) Uani 1 1 d . . . . . H18 H 0.686499 1.202234 0.211902 0.031 Uiso 1 1 calc R . . . . C11 C 0.8654(8) 0.4933(8) 0.1447(3) 0.0217(12) Uani 1 1 d . . . . . H11 H 0.826938 0.496464 0.183967 0.026 Uiso 1 1 calc R . . . . B6 B 1.1727(8) 0.3264(8) 0.3041(3) 0.0201(12) Uani 1 1 d . . . . . H6A H 1.115731 0.222959 0.264504 0.024 Uiso 1 1 calc R . . . . B12 B 0.5175(9) 0.7108(9) 0.1694(3) 0.0245(14) Uani 1 1 d . . . . . H12A H 0.507592 0.589427 0.191706 0.029 Uiso 1 1 calc R . . . . B9 B 1.4041(14) 0.6314(13) 0.3497(4) 0.049(2) Uani 1 1 d . . . . . H9 H 1.500630 0.730761 0.339411 0.059 Uiso 1 1 calc R . . . . B10 B 1.2166(10) 0.5441(9) 0.2943(3) 0.0270(15) Uani 1 1 d . . . . . H10 H 1.189917 0.586506 0.247131 0.032 Uiso 1 1 calc R . . . . C4 C 0.8486(8) 0.1451(8) 0.3586(3) 0.0292(14) Uani 1 1 d . . . . . H4 H 0.809842 0.190327 0.320886 0.035 Uiso 1 1 calc R . . . . B19 B 0.5549(9) 1.0726(9) 0.1000(3) 0.0247(14) Uani 1 1 d . . . . . H19 H 0.566763 1.190649 0.076107 0.030 Uiso 1 1 calc R . . . . B4 B 1.3351(9) 0.2777(11) 0.3683(3) 0.0313(15) Uani 1 1 d . . . . . H4A H 1.384854 0.141767 0.371640 0.038 Uiso 1 1 calc R . . . . B17 B 0.4801(9) 0.9262(10) 0.2076(3) 0.0280(15) Uani 1 1 d . . . . . H17 H 0.442720 0.947847 0.255352 0.034 Uiso 1 1 calc R . . . . B11 B 0.4468(8) 0.7067(10) 0.0877(3) 0.0262(14) Uani 1 1 d . . . . . H11A H 0.391444 0.584037 0.056365 0.031 Uiso 1 1 calc R . . . . B15 B 0.3681(9) 0.9181(10) 0.0747(3) 0.0255(14) Uani 1 1 d . . . . . H15 H 0.260027 0.934062 0.034937 0.031 Uiso 1 1 calc R . . . . B1 B 1.1134(14) 0.5586(11) 0.4151(4) 0.042(2) Uani 1 1 d . . . . . H1A H 1.020348 0.605979 0.448506 0.050 Uiso 1 1 calc R . . . . B3 B 1.4725(12) 0.4659(12) 0.3965(4) 0.044(2) Uani 1 1 d . . . . . H3 H 1.615372 0.454486 0.418545 0.053 Uiso 1 1 calc R . . . . C8 C 0.5854(7) 0.8626(8) 0.0691(3) 0.0232(12) Uani 1 1 d . . . . . H8 H 0.623128 0.838963 0.021395 0.028 Uiso 1 1 calc R . . . . B13 B 0.7012(8) 0.8665(8) 0.1946(3) 0.0217(13) Uani 1 1 d . . . . . H13A H 0.809964 0.847155 0.233759 0.026 Uiso 1 1 calc R . . . . B16 B 0.3238(9) 0.8294(10) 0.1419(3) 0.0273(15) Uani 1 1 d . . . . . H16 H 0.184451 0.788352 0.146748 0.033 Uiso 1 1 calc R . . . . B20 B 0.3926(9) 1.0555(10) 0.1493(3) 0.0291(17) Uani 1 1 d . . . . . H20 H 0.298366 1.164121 0.159059 0.035 Uiso 1 1 calc R . . . . B8 B 1.1787(15) 0.6880(9) 0.3613(3) 0.045(2) Uani 1 1 d . . . . . H8A H 1.127689 0.823890 0.358898 0.054 Uiso 1 1 calc R . . . . B5 B 1.4019(10) 0.4067(12) 0.3148(3) 0.0360(17) Uani 1 1 d . . . . . H5A H 1.496539 0.357563 0.282299 0.043 Uiso 1 1 calc R . . . . B2 B 1.3430(16) 0.6367(11) 0.4252(3) 0.048(3) Uani 1 1 d . . . . . H2 H 1.401625 0.737161 0.465553 0.058 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 N2 0.015(2) 0.021(2) 0.020(2) 0.0066(17) 0.0007(16) -0.0010(17) N1 0.015(2) 0.020(2) 0.024(2) 0.0106(18) 0.0030(17) 0.0011(17) C9 0.014(2) 0.024(3) 0.015(2) 0.0105(19) 0.0008(19) 0.003(2) C13 0.022(3) 0.024(3) 0.024(3) 0.007(2) 0.003(2) 0.005(2) C12 0.025(3) 0.025(3) 0.029(3) 0.010(2) 0.000(2) 0.005(2) C3 0.018(3) 0.026(3) 0.025(3) 0.010(2) 0.007(2) 0.002(2) C14 0.019(3) 0.015(3) 0.028(3) 0.0047(19) 0.001(2) -0.002(2) C2 0.022(3) 0.025(3) 0.015(2) 0.004(2) -0.004(2) -0.005(2) C7 0.017(3) 0.029(3) 0.029(3) 0.017(2) 0.000(2) -0.001(2) C5 0.035(4) 0.054(5) 0.049(4) 0.036(4) -0.019(3) -0.019(3) C10 0.017(3) 0.020(3) 0.024(3) 0.009(2) -0.004(2) -0.005(2) B14 0.016(3) 0.023(3) 0.024(3) 0.008(2) 0.002(2) 0.002(2) B7 0.052(5) 0.032(4) 0.027(3) 0.017(3) 0.014(3) 0.014(3) C6 0.028(3) 0.043(4) 0.046(4) 0.027(3) -0.003(3) -0.006(3) C1 0.046(4) 0.031(3) 0.014(2) 0.000(2) -0.009(3) -0.027(3) B18 0.025(3) 0.031(3) 0.021(3) 0.009(2) -0.001(2) 0.012(3) C11 0.022(3) 0.023(3) 0.021(3) 0.006(2) 0.002(2) -0.001(2) B6 0.023(3) 0.022(3) 0.015(3) 0.001(2) 0.004(2) -0.013(2) B12 0.028(3) 0.031(4) 0.018(3) 0.012(2) 0.005(2) 0.008(3) B9 0.064(6) 0.055(5) 0.026(4) 0.014(4) -0.003(4) -0.035(4) B10 0.030(4) 0.028(4) 0.022(3) 0.006(2) -0.002(3) -0.019(3) C4 0.024(3) 0.034(3) 0.030(3) 0.019(2) -0.007(2) -0.004(2) B19 0.027(3) 0.029(3) 0.021(3) 0.011(2) 0.006(2) 0.009(3) B4 0.015(3) 0.048(4) 0.031(4) 0.011(3) 0.000(3) -0.008(3) B17 0.027(3) 0.039(4) 0.022(3) 0.010(3) 0.009(2) 0.012(3) B11 0.007(3) 0.041(4) 0.030(3) 0.013(3) -0.006(2) -0.003(3) B15 0.015(3) 0.039(4) 0.026(3) 0.013(3) 0.004(2) 0.007(3) B1 0.072(6) 0.033(4) 0.024(4) 0.007(3) 0.017(4) -0.006(4) B3 0.039(5) 0.050(5) 0.043(4) 0.022(4) -0.001(3) -0.022(4) C8 0.018(3) 0.026(3) 0.026(3) 0.012(2) -0.001(2) 0.003(2) B13 0.018(3) 0.025(3) 0.023(3) 0.012(2) -0.002(2) 0.005(2) B16 0.018(3) 0.039(4) 0.026(3) 0.011(3) 0.003(2) 0.008(3) B20 0.025(3) 0.050(4) 0.017(3) 0.017(3) 0.007(2) 0.023(3) B8 0.095(7) 0.015(3) 0.025(4) -0.001(3) 0.013(4) -0.007(4) B5 0.023(4) 0.059(5) 0.028(3) 0.015(3) 0.002(3) -0.009(3) B2 0.100(8) 0.025(4) 0.014(3) 0.000(3) -0.006(4) -0.025(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 N2 C14 1.333(7) . ? N2 C10 1.343(7) . ? N1 C3 1.343(7) . ? N1 C7 1.314(8) . ? C9 C10 1.480(7) . ? C9 B14 1.728(8) . ? C9 B12 1.717(8) . ? C9 B11 1.738(8) . ? C9 C8 1.630(6) . ? C9 B13 1.721(8) . ? C13 C12 1.385(9) . ? C13 C14 1.408(8) . ? C12 C11 1.388(9) . ? C3 C2 1.501(8) . ? C3 C4 1.388(9) . ? C14 C14 1.494(12) 2_765 ? C2 B7 1.701(8) . ? C2 C1 1.631(7) . ? C2 B6 1.720(8) . ? C2 B4 1.734(9) . ? C2 B1 1.728(10) . ? C7 C7 1.526(10) 2_756 ? C7 C6 1.381(10) . ? C5 C6 1.392(10) . ? C5 C4 1.375(10) . ? C10 C11 1.399(7) . ? B14 B18 1.771(9) . ? B14 B19 1.772(8) . ? B14 C8 1.711(8) . ? B14 B13 1.803(9) . ? B7 B6 1.775(9) . ? B7 B10 1.763(10) . ? B7 B1 1.798(11) . ? B7 B8 1.777(12) . ? C1 B4 1.719(10) . ? C1 B1 1.710(12) . ? C1 B3 1.688(11) . ? C1 B2 1.673(9) . ? B18 B19 1.779(9) . ? B18 B17 1.821(10) . ? B18 B13 1.783(8) . ? B18 B20 1.794(9) . ? B6 B10 1.750(8) . ? B6 B4 1.802(9) . ? B6 B5 1.799(10) . ? B12 B17 1.791(10) . ? B12 B11 1.787(9) . ? B12 B13 1.787(10) . ? B12 B16 1.797(8) . ? B9 B10 1.773(10) . ? B9 B3 1.776(12) . ? B9 B8 1.806(16) . ? B9 B5 1.784(13) . ? B9 B2 1.787(12) . ? B10 B8 1.775(10) . ? B10 B5 1.798(11) . ? B19 B15 1.799(10) . ? B19 C8 1.691(9) . ? B19 B20 1.773(9) . ? B4 B3 1.750(11) . ? B4 B5 1.767(10) . ? B17 B13 1.789(9) . ? B17 B16 1.782(10) . ? B17 B20 1.781(8) . ? B11 B15 1.778(9) . ? B11 C8 1.717(9) . ? B11 B16 1.792(10) . ? B15 C8 1.717(8) . ? B15 B16 1.787(9) . ? B15 B20 1.802(10) . ? B1 B8 1.772(11) . ? B1 B2 1.798(15) . ? B3 B5 1.783(12) . ? B3 B2 1.747(15) . ? B16 B20 1.785(11) . ? B8 B2 1.813(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 C14 N2 C10 118.4(4) . . ? C7 N1 C3 118.3(5) . . ? C10 C9 B14 114.7(4) . . ? C10 C9 B12 123.0(4) . . ? C10 C9 B11 117.3(5) . . ? C10 C9 C8 117.0(4) . . ? C10 C9 B13 121.6(4) . . ? B14 C9 B11 114.5(4) . . ? B12 C9 B14 114.9(4) . . ? B12 C9 B11 62.3(3) . . ? B12 C9 B13 62.7(4) . . ? C8 C9 B14 61.2(3) . . ? C8 C9 B12 110.4(4) . . ? C8 C9 B11 61.2(3) . . ? C8 C9 B13 110.7(4) . . ? B13 C9 B14 63.0(4) . . ? B13 C9 B11 114.2(4) . . ? C12 C13 C14 118.4(5) . . ? C13 C12 C11 120.1(5) . . ? N1 C3 C2 117.3(5) . . ? N1 C3 C4 122.7(6) . . ? C4 C3 C2 120.0(5) . . ? N2 C14 C13 122.3(5) . . ? N2 C14 C14 117.2(6) . 2_765 ? C13 C14 C14 120.5(6) . 2_765 ? C3 C2 B7 123.4(5) . . ? C3 C2 C1 116.3(4) . . ? C3 C2 B6 121.2(5) . . ? C3 C2 B4 114.2(5) . . ? C3 C2 B1 117.1(5) . . ? B7 C2 B6 62.5(4) . . ? B7 C2 B4 114.6(5) . . ? B7 C2 B1 63.3(4) . . ? C1 C2 B7 111.1(5) . . ? C1 C2 B6 111.2(5) . . ? C1 C2 B4 61.4(4) . . ? C1 C2 B1 61.1(5) . . ? B6 C2 B4 62.9(4) . . ? B6 C2 B1 115.1(4) . . ? B1 C2 B4 114.6(5) . . ? N1 C7 C7 116.6(7) . 2_756 ? N1 C7 C6 123.2(5) . . ? C6 C7 C7 120.1(7) . 2_756 ? C4 C5 C6 119.0(6) . . ? N2 C10 C9 116.6(4) . . ? N2 C10 C11 123.6(5) . . ? C11 C10 C9 119.8(5) . . ? C9 B14 B18 104.7(4) . . ? C9 B14 B19 103.9(4) . . ? C9 B14 B13 58.3(3) . . ? B18 B14 B19 60.3(3) . . ? B18 B14 B13 59.9(3) . . ? B19 B14 B13 107.2(4) . . ? C8 B14 C9 56.6(3) . . ? C8 B14 B18 104.3(4) . . ? C8 B14 B19 58.1(3) . . ? C8 B14 B13 103.3(4) . . ? C2 B7 B6 59.3(3) . . ? C2 B7 B10 103.9(5) . . ? C2 B7 B1 59.1(4) . . ? C2 B7 B8 104.4(6) . . ? B6 B7 B1 109.0(5) . . ? B6 B7 B8 108.2(6) . . ? B10 B7 B6 59.3(4) . . ? B10 B7 B1 107.5(6) . . ? B10 B7 B8 60.2(5) . . ? B8 B7 B1 59.4(4) . . ? C7 C6 C5 118.4(7) . . ? C2 C1 B4 62.3(3) . . ? C2 C1 B1 62.3(4) . . ? C2 C1 B3 111.7(5) . . ? C2 C1 B2 113.1(5) . . ? B1 C1 B4 116.3(5) . . ? B3 C1 B4 61.8(5) . . ? B3 C1 B1 116.1(5) . . ? B2 C1 B4 114.7(5) . . ? B2 C1 B1 64.2(6) . . ? B2 C1 B3 62.6(6) . . ? B14 B18 B19 59.9(3) . . ? B14 B18 B17 108.3(5) . . ? B14 B18 B13 61.0(3) . . ? B14 B18 B20 107.8(5) . . ? B19 B18 B17 106.7(5) . . ? B19 B18 B13 107.8(5) . . ? B19 B18 B20 59.5(4) . . ? B13 B18 B17 59.5(4) . . ? B13 B18 B20 106.9(5) . . ? B20 B18 B17 59.0(4) . . ? C12 C11 C10 117.3(5) . . ? C2 B6 B7 58.2(3) . . ? C2 B6 B10 103.7(4) . . ? C2 B6 B4 58.9(3) . . ? C2 B6 B5 104.4(4) . . ? B7 B6 B4 107.8(5) . . ? B7 B6 B5 109.1(5) . . ? B10 B6 B7 60.0(4) . . ? B10 B6 B4 106.9(5) . . ? B10 B6 B5 60.9(4) . . ? B5 B6 B4 58.8(4) . . ? C9 B12 B17 104.9(5) . . ? C9 B12 B11 59.4(3) . . ? C9 B12 B13 58.8(4) . . ? C9 B12 B16 105.1(4) . . ? B17 B12 B16 59.6(4) . . ? B11 B12 B17 108.0(4) . . ? B11 B12 B13 108.7(4) . . ? B11 B12 B16 60.0(3) . . ? B13 B12 B17 60.0(4) . . ? B13 B12 B16 107.7(4) . . ? B10 B9 B3 107.4(6) . . ? B10 B9 B8 59.4(5) . . ? B10 B9 B5 60.7(4) . . ? B10 B9 B2 107.6(6) . . ? B3 B9 B8 107.3(6) . . ? B3 B9 B5 60.1(5) . . ? B3 B9 B2 58.7(5) . . ? B5 B9 B8 108.8(6) . . ? B5 B9 B2 108.0(5) . . ? B2 B9 B8 60.6(5) . . ? B7 B10 B9 109.5(5) . . ? B7 B10 B8 60.3(5) . . ? B7 B10 B5 109.7(5) . . ? B6 B10 B7 60.7(4) . . ? B6 B10 B9 109.2(5) . . ? B6 B10 B8 109.4(5) . . ? B6 B10 B5 60.9(4) . . ? B9 B10 B8 61.2(6) . . ? B9 B10 B5 59.9(5) . . ? B8 B10 B5 109.6(5) . . ? C5 C4 C3 118.3(5) . . ? B14 B19 B18 59.8(3) . . ? B14 B19 B15 109.4(4) . . ? B14 B19 B20 108.6(4) . . ? B18 B19 B15 109.5(5) . . ? C8 B19 B14 59.2(3) . . ? C8 B19 B18 104.8(4) . . ? C8 B19 B15 58.8(4) . . ? C8 B19 B20 104.7(5) . . ? B20 B19 B18 60.7(4) . . ? B20 B19 B15 60.6(4) . . ? C2 B4 B6 58.2(3) . . ? C2 B4 B3 104.1(6) . . ? C2 B4 B5 105.2(5) . . ? C1 B4 C2 56.4(4) . . ? C1 B4 B6 103.5(5) . . ? C1 B4 B3 58.2(5) . . ? C1 B4 B5 105.1(6) . . ? B3 B4 B6 108.2(5) . . ? B3 B4 B5 60.9(4) . . ? B5 B4 B6 60.5(4) . . ? B12 B17 B18 107.1(4) . . ? B13 B17 B18 59.2(4) . . ? B13 B17 B12 59.9(4) . . ? B16 B17 B18 108.0(4) . . ? B16 B17 B12 60.4(4) . . ? B16 B17 B13 108.3(4) . . ? B20 B17 B18 59.7(4) . . ? B20 B17 B12 107.8(5) . . ? B20 B17 B13 107.2(4) . . ? B20 B17 B16 60.1(4) . . ? C9 B11 B12 58.3(3) . . ? C9 B11 B15 104.8(5) . . ? C9 B11 B16 104.4(5) . . ? B12 B11 B16 60.3(4) . . ? B15 B11 B12 108.4(5) . . ? B15 B11 B16 60.1(4) . . ? C8 B11 C9 56.3(3) . . ? C8 B11 B12 103.4(5) . . ? C8 B11 B15 58.8(4) . . ? C8 B11 B16 103.8(5) . . ? B19 B15 B20 59.0(4) . . ? B11 B15 B19 107.3(4) . . ? B11 B15 B16 60.4(4) . . ? B11 B15 B20 107.5(4) . . ? C8 B15 B19 57.4(4) . . ? C8 B15 B11 58.8(3) . . ? C8 B15 B16 104.0(4) . . ? C8 B15 B20 102.5(5) . . ? B16 B15 B19 106.9(5) . . ? B16 B15 B20 59.6(4) . . ? C2 B1 B7 57.6(4) . . ? C2 B1 B8 103.5(5) . . ? C2 B1 B2 102.8(6) . . ? C1 B1 C2 56.6(4) . . ? C1 B1 B7 103.1(5) . . ? C1 B1 B8 103.7(6) . . ? C1 B1 B2 56.9(5) . . ? B8 B1 B7 59.7(4) . . ? B8 B1 B2 61.0(5) . . ? B2 B1 B7 107.6(6) . . ? C1 B3 B9 104.6(7) . . ? C1 B3 B4 60.0(4) . . ? C1 B3 B5 105.7(6) . . ? C1 B3 B2 58.2(5) . . ? B9 B3 B5 60.2(5) . . ? B4 B3 B9 108.2(6) . . ? B4 B3 B5 60.0(4) . . ? B2 B3 B9 61.0(5) . . ? B2 B3 B4 109.5(6) . . ? B2 B3 B5 109.8(6) . . ? C9 C8 B14 62.2(3) . . ? C9 C8 B19 112.2(4) . . ? C9 C8 B11 62.5(3) . . ? C9 C8 B15 112.7(4) . . ? B14 C8 B11 116.5(4) . . ? B14 C8 B15 116.5(5) . . ? B19 C8 B14 62.8(4) . . ? B19 C8 B11 115.4(5) . . ? B19 C8 B15 63.7(4) . . ? B15 C8 B11 62.4(4) . . ? C9 B13 B14 58.7(3) . . ? C9 B13 B18 104.5(4) . . ? C9 B13 B12 58.6(3) . . ? C9 B13 B17 104.8(4) . . ? B18 B13 B14 59.2(3) . . ? B18 B13 B12 109.0(4) . . ? B18 B13 B17 61.3(4) . . ? B12 B13 B14 107.9(4) . . ? B12 B13 B17 60.1(4) . . ? B17 B13 B14 108.2(4) . . ? B17 B16 B12 60.1(4) . . ? B17 B16 B11 108.2(4) . . ? B17 B16 B15 108.9(5) . . ? B17 B16 B20 59.9(4) . . ? B11 B16 B12 59.7(3) . . ? B15 B16 B12 107.6(4) . . ? B15 B16 B11 59.6(4) . . ? B20 B16 B12 107.3(5) . . ? B20 B16 B11 107.6(5) . . ? B20 B16 B15 60.6(4) . . ? B18 B20 B15 108.7(4) . . ? B19 B20 B18 59.8(4) . . ? B19 B20 B17 108.7(4) . . ? B19 B20 B15 60.4(4) . . ? B19 B20 B16 108.2(5) . . ? B17 B20 B18 61.2(4) . . ? B17 B20 B15 108.3(5) . . ? B17 B20 B16 60.0(4) . . ? B16 B20 B18 109.1(4) . . ? B16 B20 B15 59.7(4) . . ? B7 B8 B9 107.4(6) . . ? B7 B8 B2 107.8(5) . . ? B9 B8 B2 59.2(5) . . ? B10 B8 B7 59.5(4) . . ? B10 B8 B9 59.3(5) . . ? B10 B8 B2 106.4(6) . . ? B1 B8 B7 60.9(4) . . ? B1 B8 B9 108.1(6) . . ? B1 B8 B10 108.2(5) . . ? B1 B8 B2 60.2(5) . . ? B9 B5 B6 106.5(6) . . ? B9 B5 B10 59.3(5) . . ? B10 B5 B6 58.2(4) . . ? B4 B5 B6 60.7(4) . . ? B4 B5 B9 107.1(6) . . ? B4 B5 B10 106.4(5) . . ? B4 B5 B3 59.1(4) . . ? B3 B5 B6 106.9(5) . . ? B3 B5 B9 59.7(5) . . ? B3 B5 B10 106.0(6) . . ? C1 B2 B9 104.7(6) . . ? C1 B2 B1 58.9(5) . . ? C1 B2 B3 59.1(5) . . ? C1 B2 B8 103.5(6) . . ? B9 B2 B1 107.8(6) . . ? B9 B2 B8 60.2(5) . . ? B1 B2 B8 58.8(5) . . ? B3 B2 B9 60.3(5) . . ? B3 B2 B1 108.9(6) . . ? B3 B2 B8 108.2(5) . . ? _shelx_res_file ; TITL spok119_0m in P-1 spok119_0m.res created by SHELXL-2016/6 at 11:08:33 on 21-Sep-2018 REM Best SHELXD solution FINAL CC 54.98 REM Fragments: 15 14 CELL 1.54178 7.5443 7.6742 21.9959 98.1311 99.0509 90.5222 ZERR 2 0.0008 0.001 0.0026 0.008 0.0065 0.0068 LATT 1 SFAC C H B N UNIT 28 56 40 4 L.S. 4 PLAN 20 SIZE 0.05 0.25 0.28 TEMP -173.15 list 4 acta BOND fmap 2 TWIN -1 0 0 0 -1 0 0.925 0.819 1 2 OMIT -3 132 REM REM REM WGHT 0.200000 BASF 0.40534 FVAR 0.70949 N2 4 0.850221 0.610880 0.047817 11.00000 0.01510 0.02108 = 0.01958 0.00660 0.00070 -0.00096 N1 4 1.062088 0.153083 0.452063 11.00000 0.01482 0.01992 = 0.02411 0.01057 0.00300 0.00105 C9 1 0.670449 0.743811 0.121688 11.00000 0.01379 0.02379 = 0.01496 0.01047 0.00084 0.00328 C13 1 1.044673 0.373213 0.068752 11.00000 0.02156 0.02362 = 0.02440 0.00706 0.00252 0.00501 AFIX 43 H13 2 1.130670 0.292641 0.055615 11.00000 -1.20000 AFIX 0 C12 1 0.989443 0.373291 0.125876 11.00000 0.02490 0.02459 = 0.02935 0.01018 0.00034 0.00464 AFIX 43 H12 2 1.036508 0.291043 0.152199 11.00000 -1.20000 AFIX 0 C3 1 1.006592 0.207974 0.397076 11.00000 0.01848 0.02634 = 0.02537 0.00995 0.00668 0.00166 C14 1 0.970334 0.495405 0.030599 11.00000 0.01934 0.01549 = 0.02840 0.00474 0.00116 -0.00173 C2 1 1.121524 0.345170 0.378222 11.00000 0.02247 0.02497 = 0.01485 0.00375 -0.00350 -0.00463 C7 1 0.965723 0.029836 0.468730 11.00000 0.01723 0.02879 = 0.02910 0.01681 -0.00009 -0.00103 C5 1 0.749499 0.015735 0.376610 11.00000 0.03482 0.05407 = 0.04910 0.03583 -0.01910 -0.01891 AFIX 43 H5 2 0.643432 -0.033936 0.350552 11.00000 -1.20000 AFIX 0 C10 1 0.799388 0.609630 0.103587 11.00000 0.01703 0.01988 = 0.02433 0.00912 -0.00383 -0.00456 B14 3 0.747841 0.959166 0.127651 11.00000 0.01624 0.02347 = 0.02439 0.00814 0.00180 0.00212 AFIX 153 H14 2 0.886530 0.999730 0.121908 11.00000 -1.20000 AFIX 0 B7 3 1.038088 0.497421 0.333090 11.00000 0.05240 0.03213 = 0.02688 0.01745 0.01358 0.01391 AFIX 153 H7 2 0.893418 0.504965 0.312371 11.00000 -1.20000 AFIX 0 C6 1 0.807041 -0.041289 0.433557 11.00000 0.02798 0.04280 = 0.04578 0.02652 -0.00341 -0.00589 AFIX 43 H6 2 0.738766 -0.127128 0.447898 11.00000 -1.20000 AFIX 0 C1 1 1.291987 0.426856 0.429837 11.00000 0.04619 0.03117 = 0.01368 0.00043 -0.00907 -0.02681 AFIX 153 H1 2 1.314264 0.384341 0.477035 11.00000 -1.20000 AFIX 0 B18 3 0.626777 1.079827 0.181403 11.00000 0.02458 0.03131 = 0.02077 0.00926 -0.00079 0.01173 AFIX 153 H18 2 0.686499 1.202234 0.211902 11.00000 -1.20000 AFIX 0 C11 1 0.865420 0.493348 0.144738 11.00000 0.02227 0.02279 = 0.02066 0.00639 0.00246 -0.00101 AFIX 43 H11 2 0.826938 0.496464 0.183967 11.00000 -1.20000 AFIX 0 B6 3 1.172661 0.326434 0.304112 11.00000 0.02262 0.02178 = 0.01547 0.00058 0.00406 -0.01298 AFIX 153 H6A 2 1.115731 0.222959 0.264504 11.00000 -1.20000 AFIX 0 B12 3 0.517485 0.710834 0.169383 11.00000 0.02751 0.03098 = 0.01798 0.01167 0.00512 0.00768 AFIX 153 H12A 2 0.507592 0.589427 0.191706 11.00000 -1.20000 AFIX 0 B9 3 1.404064 0.631370 0.349704 11.00000 0.06383 0.05505 = 0.02649 0.01436 -0.00316 -0.03484 AFIX 153 H9 2 1.500630 0.730761 0.339411 11.00000 -1.20000 AFIX 0 B10 3 1.216604 0.544118 0.294314 11.00000 0.02968 0.02826 = 0.02153 0.00623 -0.00179 -0.01860 AFIX 153 H10 2 1.189917 0.586506 0.247131 11.00000 -1.20000 AFIX 0 C4 1 0.848586 0.145128 0.358645 11.00000 0.02399 0.03406 = 0.03000 0.01940 -0.00729 -0.00351 AFIX 43 H4 2 0.809842 0.190327 0.320886 11.00000 -1.20000 AFIX 0 B19 3 0.554924 1.072590 0.100047 11.00000 0.02659 0.02914 = 0.02120 0.01096 0.00575 0.00869 AFIX 153 H19 2 0.566763 1.190649 0.076107 11.00000 -1.20000 AFIX 0 B4 3 1.335080 0.277674 0.368291 11.00000 0.01518 0.04795 = 0.03077 0.01061 -0.00033 -0.00751 AFIX 153 H4A 2 1.384854 0.141767 0.371640 11.00000 -1.20000 AFIX 0 B17 3 0.480088 0.926224 0.207612 11.00000 0.02686 0.03900 = 0.02175 0.01023 0.00888 0.01223 AFIX 153 H17 2 0.442720 0.947847 0.255352 11.00000 -1.20000 AFIX 0 B11 3 0.446759 0.706656 0.087738 11.00000 0.00722 0.04056 = 0.03014 0.01272 -0.00572 -0.00263 AFIX 153 H11A 2 0.391444 0.584037 0.056365 11.00000 -1.20000 AFIX 0 B15 3 0.368132 0.918126 0.074750 11.00000 0.01492 0.03898 = 0.02553 0.01302 0.00394 0.00730 AFIX 153 H15 2 0.260027 0.934062 0.034937 11.00000 -1.20000 AFIX 0 B1 3 1.113370 0.558604 0.415144 11.00000 0.07217 0.03299 = 0.02427 0.00670 0.01731 -0.00650 AFIX 153 H1A 2 1.020348 0.605979 0.448506 11.00000 -1.20000 AFIX 0 B3 3 1.472469 0.465913 0.396500 11.00000 0.03949 0.05032 = 0.04346 0.02169 -0.00108 -0.02197 AFIX 153 H3 2 1.615372 0.454486 0.418545 11.00000 -1.20000 AFIX 0 C8 1 0.585423 0.862639 0.069068 11.00000 0.01795 0.02612 = 0.02643 0.01201 -0.00130 0.00301 AFIX 153 H8 2 0.623128 0.838963 0.021395 11.00000 -1.20000 AFIX 0 B13 3 0.701166 0.866459 0.194571 11.00000 0.01789 0.02549 = 0.02262 0.01215 -0.00184 0.00511 AFIX 153 H13A 2 0.809964 0.847155 0.233759 11.00000 -1.20000 AFIX 0 B16 3 0.323788 0.829351 0.141879 11.00000 0.01819 0.03927 = 0.02634 0.01107 0.00346 0.00802 AFIX 153 H16 2 0.184451 0.788352 0.146748 11.00000 -1.20000 AFIX 0 B20 3 0.392610 1.055518 0.149304 11.00000 0.02508 0.05043 = 0.01687 0.01664 0.00682 0.02316 AFIX 153 H20 2 0.298366 1.164121 0.159059 11.00000 -1.20000 AFIX 0 B8 3 1.178743 0.688042 0.361285 11.00000 0.09504 0.01477 = 0.02503 -0.00095 0.01314 -0.00724 AFIX 153 H8A 2 1.127689 0.823890 0.358898 11.00000 -1.20000 AFIX 0 B5 3 1.401860 0.406682 0.314849 11.00000 0.02274 0.05925 = 0.02779 0.01549 0.00206 -0.00940 AFIX 153 H5A 2 1.496539 0.357563 0.282299 11.00000 -1.20000 AFIX 0 B2 3 1.343020 0.636654 0.425216 11.00000 0.09974 0.02480 = 0.01440 -0.00017 -0.00589 -0.02459 AFIX 153 H2 2 1.401625 0.737161 0.465553 11.00000 -1.20000 AFIX 0 HKLF 4 REM spok119_0m in P-1 REM R1 = 0.1231 for 3641 Fo > 4sig(Fo) and 0.1309 for all 4012 data REM 326 parameters refined using 0 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.349, deepest hole -0.405, 1-sigma level 0.090 Q1 1 0.9629 0.5075 0.4219 11.00000 0.05 0.35 Q2 1 0.1911 0.6926 0.1309 11.00000 0.05 0.35 Q3 1 0.9982 0.1697 0.0550 11.00000 0.05 0.31 Q4 1 0.8987 0.2049 0.1312 11.00000 0.05 0.31 Q5 1 1.0614 0.4730 0.4377 11.00000 0.05 0.31 Q6 1 0.8608 0.4973 0.1955 11.00000 0.05 0.31 Q7 1 1.3347 0.8771 0.3626 11.00000 0.05 0.30 Q8 1 0.2259 0.6837 0.0013 11.00000 0.05 0.30 Q9 1 0.5470 0.9860 0.1903 11.00000 0.05 0.29 Q10 1 1.0617 0.2736 0.3892 11.00000 0.05 0.29 Q11 1 0.5208 0.0258 0.3622 11.00000 0.05 0.29 Q12 1 1.1660 0.1525 0.4225 11.00000 0.05 0.28 Q13 1 0.6664 1.2921 0.0614 11.00000 0.05 0.28 Q14 1 1.1549 1.0371 0.3536 11.00000 0.05 0.28 Q15 1 0.8199 0.3875 0.2490 11.00000 0.05 0.28 Q16 1 0.6150 1.0794 0.0681 11.00000 0.05 0.27 Q17 1 1.1881 0.2066 0.2867 11.00000 0.05 0.27 Q18 1 0.8728 0.5226 0.3467 11.00000 0.05 0.27 Q19 1 0.9309 0.2516 0.1605 11.00000 0.05 0.27 Q20 1 1.4973 0.0974 0.4198 11.00000 0.05 0.27 ; _shelx_res_checksum 7084 _shelx_hkl_file ; -1 0 0 347.867 21.4596 2 -2 0 0 154.706 10.7210 2 2 0 0 150.079 9.83523 10 -3 0 0 11.4354 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-2 5 -22 0.08223 2.09689 3 2 -5 22 2.09305 2.17603 8 5 4 -22 2.79591 1.86971 15 -5 -4 22 -0.6936 1.64492 12 4 4 -22 40.4367 4.42894 15 -4 -4 22 50.6769 5.23236 12 3 4 -22 17.9211 3.19688 15 -3 -4 22 24.7975 3.98939 12 2 4 -22 27.1527 4.05753 15 2 4 -22 24.0156 4.03791 3 -2 -4 22 22.3630 3.85105 12 1 4 -22 5.10292 2.75681 3 -1 -4 22 4.68677 3.00822 12 -1 -4 22 6.66473 2.93557 8 0 4 -22 103.716 8.59249 3 0 -4 22 107.980 8.18486 12 0 -4 22 114.315 9.10949 8 -1 4 -22 69.2838 6.65470 3 1 -4 22 69.6200 6.02132 12 1 -4 22 76.3634 7.05995 8 -2 4 -22 28.7321 4.04019 3 -2 4 -22 26.9117 3.44712 14 2 -4 22 15.6617 3.21611 8 3 -4 22 0.74348 2.01108 8 5 3 -22 18.5224 2.82275 15 -5 -3 22 15.3530 2.92592 12 4 3 -22 94.1282 6.69771 15 -4 -3 22 79.9319 6.82282 12 3 3 -22 0.09008 3.95440 13 3 3 -22 6.11193 2.65846 15 -3 -3 22 2.75174 3.03021 12 -2 -3 22 4.77981 3.02481 12 -2 -3 22 5.10091 2.87887 8 1 3 -22 26.1276 4.19462 3 -1 -3 22 29.6557 5.31735 12 -1 -3 22 25.3095 4.07708 8 0 3 -22 17.9482 3.85191 3 0 -3 22 7.31712 3.26386 8 0 -3 22 9.72908 3.08413 12 -1 3 -22 17.7918 3.61588 14 -1 3 -22 13.9945 3.75358 3 1 -3 22 12.4867 3.37265 8 1 -3 22 14.5165 3.01268 12 -2 3 -22 14.2355 3.11652 14 -2 3 -22 13.9317 3.50326 3 2 -3 22 8.87111 3.13471 8 -3 3 -22 0.44802 1.98328 3 -3 3 -22 1.07715 2.25207 14 3 -3 22 1.18124 2.33499 8 6 2 -22 10.6287 2.11295 15 5 2 -22 1.46942 3.20326 13 5 2 -22 8.09458 2.54339 15 4 2 -22 45.4493 4.83321 15 -4 -2 22 40.6626 4.61529 12 3 2 -22 5.08674 2.66265 3 -3 -2 22 4.51475 2.86602 12 1 2 -22 7.74325 3.32429 3 -1 -2 22 7.14181 2.99738 8 -1 -2 22 10.8678 3.25034 12 0 2 -22 2.93762 3.31108 3 0 2 -22 7.50633 3.02306 14 0 -2 22 2.26550 2.97381 8 0 -2 22 4.33471 2.94764 12 -1 2 -22 3.29195 3.11128 14 -1 2 -22 2.46520 3.57351 3 1 -2 22 3.52956 3.02995 8 1 -2 22 3.84224 2.57169 12 -2 2 -22 32.2042 5.42994 14 -2 2 -22 38.6473 5.57600 3 2 -2 22 35.5180 5.64070 8 2 -2 22 28.9851 4.54536 12 -3 2 -22 3.11926 2.70590 14 3 -2 22 0.50167 2.39598 8 -6 -1 22 19.4920 3.48115 9 -5 -1 22 47.1999 5.16389 9 4 1 -22 51.4719 5.54134 3 3 1 -22 7.59462 3.26562 3 -3 -1 22 2.90302 2.71051 12 2 1 -22 63.9707 7.18513 3 -2 -1 22 72.6292 6.73075 12 1 1 -22 2.87217 3.34435 14 1 1 -22 4.82350 3.82282 3 -1 -1 22 1.75471 3.10692 12 0 1 -22 2.27939 3.60809 3 0 1 -22 3.84204 3.12769 14 0 -1 22 8.65490 3.14201 12 0 -1 22 3.74761 2.82540 8 -1 1 -22 80.3444 7.02919 14 -1 1 -22 83.2467 7.57498 3 1 -1 22 72.7431 7.36719 8 1 -1 22 70.6439 6.73104 12 -2 1 -22 29.0467 5.24927 3 -2 1 -22 26.7100 4.79630 14 2 -1 22 25.2716 4.23108 12 2 -1 22 23.5896 4.93240 8 -3 1 -22 15.4451 3.08081 14 3 -1 22 13.9914 2.72229 12 3 -1 22 11.2456 2.83606 8 -6 0 22 4.26603 2.03737 9 -5 0 22 72.3802 6.48088 9 4 0 -22 58.4885 6.14567 3 -4 0 22 57.8765 6.10925 9 3 0 -22 66.4222 6.86236 3 -3 0 22 77.7537 10.5164 9 -3 0 22 55.3361 5.77887 12 2 0 -22 9.19072 4.16924 3 -2 0 22 7.61512 3.05148 12 1 0 -22 4.23838 3.18158 14 1 0 -22 2.85206 3.49628 3 -1 0 22 1.19891 3.05114 12 0 0 -22 4.57248 3.80980 3 0 0 -22 5.29526 3.21176 14 0 0 22 1.36167 2.91340 12 -1 0 -22 33.1867 5.39782 3 -1 0 -22 30.4927 5.12225 14 1 0 22 24.4746 4.79047 8 1 0 22 25.3175 4.58747 12 -2 0 -22 4.44992 2.68734 14 2 0 22 2.82796 2.54609 8 2 0 22 1.79923 2.57954 12 -3 0 -22 29.0450 4.25137 14 3 0 22 26.1535 4.10935 12 3 0 22 22.0623 4.48591 8 5 -1 -22 11.9436 3.03722 3 -5 1 22 12.1895 2.79640 9 4 -1 -22 37.8183 5.17402 3 -4 1 22 37.3072 5.45975 9 3 -1 -22 120.186 9.31960 3 -3 1 22 116.538 9.50023 9 2 -1 -22 80.2044 6.95782 14 2 -1 -22 87.3407 7.85124 3 -2 1 22 77.2950 6.73311 12 1 -1 -22 81.9159 7.18789 14 1 -1 -22 74.6560 7.72251 3 -1 1 22 73.7036 6.71408 12 0 -1 -22 5.45698 3.19900 14 0 -1 -22 3.63317 3.46319 3 0 1 22 4.74952 2.95038 12 -1 -1 -22 112.727 8.21625 14 -1 -1 -22 99.4745 8.23534 3 1 1 22 103.617 8.00463 12 -2 -1 -22 16.0977 2.97604 14 -2 -1 -22 13.4252 3.29157 1 2 1 22 18.4498 3.30370 12 2 1 22 12.4854 3.01005 8 -3 -1 -22 30.8221 4.54050 1 -3 -1 -22 36.0716 3.98857 14 3 1 22 37.9272 4.39526 8 3 1 22 34.0311 4.18083 12 5 -2 -22 50.4779 4.58968 3 -5 2 22 45.4579 4.97546 9 4 -2 -22 22.9457 4.39071 3 -4 2 22 28.1224 5.01694 9 3 -2 -22 -0.9384 2.84729 3 3 -2 -22 -1.4234 3.20601 14 -3 2 22 1.39408 3.20755 9 2 -2 -22 37.8266 5.60077 3 2 -2 -22 30.8563 4.86194 14 -2 2 22 39.3237 6.12428 9 1 -2 -22 9.18318 3.25415 14 1 -2 -22 10.5665 3.72213 3 -1 2 22 13.3227 3.04979 12 0 -2 -22 37.3582 5.50805 3 0 -2 -22 38.9954 5.53806 14 0 2 22 37.7502 4.95662 12 -1 -2 -22 9.27083 3.12852 1 -1 -2 -22 9.36698 2.75028 14 1 2 22 7.20973 2.87895 12 -2 -2 -22 22.1016 3.79917 14 -2 -2 -22 31.7167 4.44458 1 2 2 22 27.4773 4.49955 12 4 -3 -22 3.74278 2.10526 3 -4 3 22 1.31319 2.31671 9 3 -3 -22 1.56365 2.65717 3 3 -3 -22 4.39499 2.09703 14 -3 3 22 1.17064 2.65814 9 2 -3 -22 14.3834 3.28528 3 2 -3 -22 11.5997 2.77515 14 -2 3 22 10.1565 3.11805 9 1 -3 -22 15.1862 3.13689 14 1 -3 -22 13.3003 3.27925 3 -1 3 22 11.5738 3.04471 9 0 3 22 3.24277 2.45149 12 1 3 22 7.98013 2.42245 12 -1 4 22 2.62440 2.06068 9 -3 -5 23 62.1748 5.20937 12 -3 -5 23 60.8988 6.33020 8 2 5 -23 26.8365 3.32491 15 -2 -5 23 36.4354 4.14375 12 -2 -5 23 28.7301 4.35150 8 1 5 -23 21.3566 3.41936 3 -1 -5 23 23.3174 3.63605 12 -1 -5 23 20.3983 3.15458 8 0 5 -23 78.7620 6.35880 3 0 -5 23 85.3977 6.42368 12 0 -5 23 96.6238 7.09239 8 -1 5 -23 12.9339 2.32487 3 1 -5 23 10.6507 2.55379 8 4 4 -23 27.9908 3.50663 15 -4 -4 23 33.1306 3.81027 12 3 4 -23 14.3764 2.64292 15 -3 -4 23 18.5173 3.06560 12 2 4 -23 13.3111 2.69385 3 -2 -4 23 16.3718 3.24365 12 -2 -4 23 8.53277 2.70499 8 1 4 -23 18.0787 3.24332 3 -1 -4 23 23.2349 4.27602 12 -1 -4 23 21.1025 4.80188 8 0 4 -23 10.9766 3.25945 3 0 -4 23 7.51912 2.85982 8 0 -4 23 10.1730 2.59134 12 -1 4 -23 153.293 9.90991 3 1 -4 23 148.532 10.3091 8 1 -4 23 113.316 10.9694 12 -2 4 -23 8.75163 2.30687 14 -2 4 -23 7.37032 2.11286 3 2 -4 23 6.88307 2.57658 8 5 3 -23 46.4570 3.87874 15 4 3 -23 31.8377 3.61489 15 -4 -3 23 33.5817 4.06643 12 -3 -3 23 22.3698 3.47032 12 2 3 -23 9.98977 2.88807 3 -2 -3 23 10.6973 3.21633 12 -1 -3 23 55.5638 5.67051 12 -1 -3 23 48.1550 5.92702 8 0 3 -23 75.0564 6.87886 3 0 -3 23 72.8961 6.51913 12 0 -3 23 72.4598 7.04320 8 -1 3 -23 34.2785 5.31134 3 -1 3 -23 40.1995 4.45225 14 1 -3 23 32.1149 4.43988 12 1 -3 23 36.6162 5.57141 8 -2 3 -23 5.81481 2.31146 14 -2 3 -23 5.03079 2.61633 3 2 -3 23 1.22596 2.72160 8 5 2 -23 3.08703 2.35177 15 -4 -2 23 1.40027 2.10325 12 3 2 -23 3.89179 2.58064 3 -3 -2 23 1.99781 2.64534 12 1 2 -23 4.37931 3.26954 3 -1 -2 23 10.7080 3.06885 12 0 2 -23 57.7658 6.61998 3 0 2 -23 63.4884 5.60971 14 0 -2 23 51.8080 5.93847 12 0 -2 23 54.5194 6.37423 8 -1 2 -23 15.7349 3.62715 14 -1 2 -23 12.4028 3.91703 3 1 -2 23 9.63622 3.10414 8 1 -2 23 13.7678 2.98770 12 -2 2 -23 8.95364 3.16721 3 -2 2 -23 14.1924 3.29474 14 2 -2 23 22.8946 3.63906 12 2 -2 23 26.3230 4.85538 8 -3 2 -23 12.9490 2.41246 14 3 -2 23 9.69711 2.36540 8 -5 -1 23 7.27972 2.64505 9 4 1 -23 46.2724 5.00630 3 3 1 -23 8.69927 3.30673 3 -3 -1 23 5.94151 2.63906 12 2 1 -23 39.2777 6.06203 3 -2 -1 23 35.4803 5.24810 12 1 1 -23 51.9842 6.43857 3 -1 -1 23 53.5420 5.78267 12 0 1 -23 4.07559 2.96197 14 0 1 -23 1.19226 3.20083 3 0 -1 23 1.43792 3.21497 8 0 -1 23 2.35283 2.59955 12 -1 1 -23 153.449 10.6871 3 -1 1 -23 152.946 10.2449 14 1 -1 23 137.882 10.0633 12 1 -1 23 128.232 10.3282 8 -2 1 -23 16.4813 3.44493 14 -2 1 -23 18.1937 3.43962 3 2 -1 23 12.6277 2.70392 12 2 -1 23 12.5696 2.75296 8 -3 1 -23 30.5657 3.93295 14 3 -1 23 28.5895 4.41096 8 -5 0 23 42.3601 4.80192 9 4 0 -23 127.697 9.25293 3 -4 0 23 125.557 9.40824 9 3 0 -23 111.907 9.43684 3 -3 0 23 125.872 9.53538 12 2 0 -23 82.0787 7.28936 3 -2 0 23 67.8021 6.24543 12 1 0 -23 30.8651 5.83391 3 1 0 -23 28.8644 5.07155 14 -1 0 23 31.1343 3.96773 12 0 0 -23 0.25008 3.42995 3 0 0 -23 2.46695 3.12944 14 0 0 23 1.43680 2.58969 12 -1 0 -23 5.84712 3.38154 3 -1 0 -23 6.74151 3.05769 14 1 0 23 9.05955 2.78608 12 -2 0 -23 48.8345 4.76481 14 2 0 23 49.1127 4.95086 12 2 0 23 41.1390 4.99524 8 -3 0 -23 17.5165 3.26965 14 -5 1 23 19.0257 4.12461 9 4 -1 -23 8.70223 3.26193 3 -4 1 23 5.02217 2.89575 9 3 -1 -23 61.2193 6.42896 3 -3 1 23 54.4926 6.39825 9 2 -1 -23 27.1417 4.77887 14 2 -1 -23 34.1128 4.90283 3 -2 1 23 23.4429 3.35688 12 1 -1 -23 139.806 9.78967 14 1 -1 -23 141.862 10.2464 3 -1 1 23 123.468 9.44685 12 0 -1 -23 23.3903 3.69538 14 0 -1 -23 26.0005 4.31412 3 0 1 23 21.5543 3.27732 12 -1 -1 -23 36.8965 4.84553 14 1 1 23 33.3808 4.71204 12 -2 -1 -23 92.7170 6.89541 14 2 1 23 92.8850 7.08682 12 4 -2 -23 6.61702 2.63445 3 -4 2 23 2.77254 2.70419 9 3 -2 -23 2.98152 2.89947 3 -3 2 23 0.88268 3.00749 9 2 -2 -23 28.9485 5.12253 3 2 -2 -23 31.1623 4.59092 14 -2 2 23 34.5195 5.36911 9 1 -2 -23 90.6561 7.05247 14 1 -2 -23 81.2988 7.15461 3 -1 2 23 75.6773 6.35882 12 0 -2 -23 62.7670 5.63951 14 0 -2 -23 53.8157 5.77469 3 0 2 23 57.0857 5.37026 12 -1 -2 -23 11.4619 2.70289 14 1 2 23 12.5378 3.00206 12 3 -3 -23 6.50295 2.24131 3 -3 3 23 2.78676 2.32725 9 2 -3 -23 7.91354 2.32950 14 2 -3 -23 8.60931 2.75632 3 -2 3 23 1.73634 2.45606 9 1 -3 -23 47.1059 5.05903 14 1 -3 -23 51.6551 5.00360 3 0 -3 -23 21.1638 2.87652 14 -1 -5 24 36.5014 3.91524 12 -1 -5 24 31.4722 4.14447 8 -3 -4 24 9.06647 2.53605 12 2 4 -24 -0.2276 2.00050 3 -2 -4 24 0.27985 2.00896 8 -2 -4 24 -0.1775 2.43926 12 1 4 -24 43.5291 4.54781 3 -1 -4 24 42.3293 4.50136 12 -1 -4 24 35.8654 4.86345 8 0 4 -24 54.8250 5.23839 3 0 -4 24 55.4395 5.62422 8 0 -4 24 51.9462 4.87048 12 -1 4 -24 5.57316 2.39880 3 1 -4 24 4.32714 2.46943 8 -4 -3 24 1.64903 1.91668 12 -3 -3 24 8.86878 2.59108 12 2 3 -24 1.80867 2.42995 3 -2 -3 24 1.19136 2.68965 12 1 3 -24 10.1399 3.11902 3 -1 -3 24 9.48250 2.76335 8 -1 -3 24 13.2193 3.07669 12 0 3 -24 37.9555 5.09676 3 0 -3 24 36.8455 4.78816 12 0 -3 24 42.3210 5.45708 8 -1 3 -24 42.6568 5.06961 3 -1 3 -24 39.7575 3.95142 14 1 -3 24 43.1153 4.59683 12 1 -3 24 40.2908 5.14949 8 -2 3 -24 8.51487 2.22609 3 2 -3 24 6.25397 2.37057 8 -4 -2 24 16.4933 3.05319 12 -3 -2 24 8.66191 2.54551 12 2 2 -24 0.04399 2.68547 3 -2 -2 24 0.56789 2.63351 12 1 2 -24 29.8993 4.35592 3 -1 -2 24 21.0327 3.62811 12 0 2 -24 26.2362 4.75592 14 0 2 -24 26.3122 5.21877 3 -1 2 -24 72.1700 6.37277 3 -1 2 -24 62.5087 5.68374 14 1 -2 24 67.2984 5.89272 12 1 -2 24 59.2648 6.30411 8 -2 2 -24 2.16519 2.24138 14 -2 2 -24 1.97669 2.24590 3 2 -2 24 1.94244 2.07100 8 2 -2 24 1.97770 1.99237 12 4 1 -24 10.6126 2.64286 3 3 1 -24 40.1944 5.55003 3 -3 -1 24 52.6283 4.81436 12 2 1 -24 6.45476 3.26269 3 -2 -1 24 7.77826 2.66514 12 1 1 -24 107.828 8.34082 3 -1 -1 24 94.3450 7.76199 12 0 1 -24 23.7346 4.01157 14 0 1 -24 17.1729 3.75555 3 0 -1 24 13.6635 3.10557 12 -1 1 -24 19.3545 3.18673 14 -1 1 -24 11.9146 3.70140 3 1 -1 24 9.55750 2.78610 12 1 -1 24 8.32089 2.38580 8 -2 1 -24 80.5545 6.09011 14 2 -1 24 73.3854 5.91656 12 2 -1 24 65.2371 5.99578 8 4 0 -24 17.6778 3.43238 3 3 0 -24 15.3873 3.68873 3 2 0 -24 3.31221 3.33856 3 -2 0 24 3.95792 2.31635 12 1 0 -24 8.51494 2.78998 14 1 0 -24 7.14450 3.58155 3 -1 0 24 8.49819 2.67282 12 0 0 -24 2.89814 2.67049 14 0 0 -24 2.05829 3.26214 3 0 0 24 1.87880 2.51360 12 -1 0 -24 4.77723 3.23743 3 -1 0 -24 8.64283 2.87660 14 1 0 24 3.83002 2.39834 12 -2 0 -24 77.7470 6.15505 14 2 0 24 79.7458 6.10728 12 4 -1 -24 19.1774 3.02644 3 -4 1 24 12.3703 2.93174 9 3 -1 -24 18.5938 3.45645 3 2 -1 -24 7.43546 2.61129 14 2 -1 -24 13.0879 3.44636 3 -2 1 24 10.5641 2.31001 12 1 -1 -24 12.3919 2.80251 14 1 -1 -24 13.9444 3.68559 3 -1 1 24 12.1230 2.47595 12 0 -1 -24 -0.6011 2.66993 14 0 -1 -24 0.41118 2.89389 3 0 1 24 1.24913 2.37023 12 -1 -1 -24 1.16824 2.35717 14 1 1 24 3.13530 2.39929 12 3 -2 -24 13.2584 2.68757 3 -3 2 24 7.86806 2.56153 9 2 -2 -24 3.63889 2.65410 3 2 -2 -24 2.57628 2.07445 14 1 -2 -24 58.2070 5.66092 3 1 -2 -24 57.3008 4.95299 14 -1 2 24 50.4981 4.72854 12 0 -2 -24 17.1493 2.81999 14 0 2 24 18.4614 2.74424 12 -2 -4 25 6.47014 2.21741 12 1 4 -25 18.0180 3.04443 3 -1 -4 25 16.6876 2.55948 12 -1 -4 25 13.9281 2.49747 8 -3 -3 25 14.8871 2.58421 12 2 3 -25 2.20013 1.99393 3 -2 -3 25 4.32817 2.41928 12 1 3 -25 48.8140 4.72782 3 -1 -3 25 42.2378 5.03988 8 -1 -3 25 43.8843 4.72386 12 0 3 -25 10.2275 2.73012 3 0 -3 25 11.0198 2.76882 12 0 -3 25 8.70442 2.43209 8 -1 3 -25 19.5845 2.94616 3 1 -3 25 15.3306 2.60040 8 3 2 -25 1.15875 2.09729 3 -3 -2 25 0.09763 2.08988 12 2 2 -25 13.1801 2.85337 3 -2 -2 25 13.9418 2.78088 12 1 2 -25 9.01251 3.10410 3 -1 -2 25 10.5834 2.71038 12 0 -2 25 8.47969 2.83553 12 3 1 -25 25.2108 4.08761 3 -3 -1 25 21.8176 3.19988 12 2 1 -25 0.39951 2.85338 3 -2 -1 25 2.46143 2.12756 12 1 1 -25 32.6285 4.98967 3 -1 -1 25 28.9605 4.38107 12 0 1 -25 0.48220 3.18705 3 0 1 -25 2.15114 2.37121 14 0 -1 25 -0.8397 2.38224 12 -1 1 -25 27.8838 3.86116 14 -1 1 -25 27.2440 4.08320 3 1 -1 25 23.4957 3.54302 12 3 0 -25 23.6331 4.31168 3 2 0 -25 53.8829 5.48144 3 -2 0 25 42.4903 4.34764 12 1 0 -25 7.08738 2.18916 14 1 0 -25 3.36206 2.98474 3 -1 0 25 5.77427 2.26459 12 0 0 -25 4.34683 2.27698 14 0 0 -25 1.21503 2.90281 3 0 0 25 5.46281 2.15784 12 -1 0 -25 0.00177 5.14936 3 -1 0 -25 8.80123 2.49169 14 1 0 25 7.92709 2.44182 12 3 -1 -25 25.3698 4.14341 3 2 -1 -25 69.3356 6.16102 3 1 -1 -25 23.6433 3.33745 14 1 -1 -25 21.3182 4.07570 3 -1 1 25 23.4088 3.41537 12 0 -1 -25 21.6153 3.29016 14 0 -1 -25 13.1310 2.95970 3 0 1 25 19.3008 3.01940 12 2 2 -26 18.1432 3.38433 3 -2 -2 26 16.8682 2.59858 12 1 2 -26 6.47955 2.55281 3 -1 -2 26 6.16367 2.29569 12 0 2 -26 3.45303 2.38660 3 0 -2 26 3.57364 2.11747 12 2 1 -26 25.5446 3.99915 3 -2 -1 26 21.0719 3.20089 12 1 1 -26 9.49655 2.81382 3 -1 -1 26 9.34378 2.35137 12 0 1 -26 19.7571 4.07298 3 0 -1 26 13.8035 2.44812 12 2 0 -26 78.8154 6.24089 3 1 0 -26 8.57783 2.62537 3 -1 0 26 7.75530 1.87701 12 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7531 _exptl_absorpt_correction_T_min 0.6341 _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 1.54181 7.539 7.658 21.971 98.152 99.051 90.482 ) ; _shelx_hkl_checksum 9830 _olex2_submission_special_instructions 'No special instructions were received' loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.595(4) 2 0.405(4)