data_spok75_0m_a _audit_creation_date 2017-10-12 _audit_creation_method ; Olex2 1.2-beta (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _shelx_SHELXL_version_number '2014/7' _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_id_orcid ? _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 'C9 H25 B20 N' _chemical_formula_sum 'C9 H25 B20 N' _chemical_formula_weight 363.50 _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' 0.0033 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' 'B' 'B' 0.0013 0.0007 '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' _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 'tetragonal' _space_group_IT_number 122 _space_group_name_H-M_alt 'I -4 2 d' _space_group_name_Hall 'I -4 2bw' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y, -z+3/4' 'x+1/2, -y, -z+3/4' '-y+1/2, -x, z+3/4' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1, y+1/2, -z+5/4' 'x+1, -y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'y+1, x+1/2, z+5/4' _cell_length_a 14.9695(6) _cell_length_b 14.9695(6) _cell_length_c 19.0130(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4260.5(4) _cell_formula_units_Z 8 _cell_measurement_reflns_used 3572 _cell_measurement_temperature 100 _cell_measurement_theta_max 27.170 _cell_measurement_theta_min 2.721 _shelx_estimated_absorpt_T_max 0.986 _shelx_estimated_absorpt_T_min 0.983 _exptl_absorpt_coefficient_mu 0.051 _exptl_absorpt_correction_T_max 0.4915 _exptl_absorpt_correction_T_min 0.4383 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0984 before and 0.0814 after correction. The Ratio of minimum to maximum transmission is 0.8918. 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 1.133 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 1488 _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.28 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0667 _diffrn_reflns_av_unetI/netI 0.0585 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 11221 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.458 _diffrn_reflns_theta_min 1.731 _diffrn_ambient_temperature 100.0 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.804 _reflns_Friedel_fraction_full 0.999 _reflns_Friedel_fraction_max 0.997 _reflns_number_gt 2267 _reflns_number_total 2441 _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 v8.37A (Bruker, 2015)' _computing_data_collection ? _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _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 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.250 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.051 _refine_ls_abs_structure_details ; Flack x determined using 928 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.3(10) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 137 _refine_ls_number_reflns 2441 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0474 _refine_ls_restrained_S_all 1.073 _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^)+(0.0674P)^2^+1.8516P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1236 _refine_ls_wR_factor_ref 0.1292 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All B(H) groups, All C(H) groups 2.a Aromatic/amide H refined with riding coordinates: C4(H4), C5(H5) 2.b Boron cage BH refined with riding coordinates: C2(H2), B1(H1), B2(H2A), B3(H3), B4(H4A), B5(H5A), B6(H6), B7(H7), B8(H8), B9(H9), B10(H10) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _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 N1 N 0.18705(15) 0.7500 0.6250 0.0116(5) Uani 1 2 d S T P . . C1 C 0.19404(13) 0.58937(14) 0.61732(12) 0.0118(4) Uani 1 1 d . . . . . C2 C 0.30251(13) 0.59810(15) 0.62331(14) 0.0163(5) Uani 1 1 d . . . . . H2 H 0.3341 0.6652 0.6309 0.020 Uiso 1 1 calc R . . . . C3 C 0.14050(14) 0.67384(13) 0.62179(12) 0.0118(4) Uani 1 1 d . . . . . C4 C 0.04750(14) 0.67001(15) 0.62158(12) 0.0144(5) Uani 1 1 d . . . . . H4 H 0.0170 0.6145 0.6192 0.017 Uiso 1 1 calc R . . . . C5 C 0.0011(2) 0.7500 0.6250 0.0155(6) Uani 1 2 d S T P . . H5 H -0.0624 0.7500 0.6250 0.019 Uiso 1 2 calc RS T P . . B1 B 0.25748(19) 0.57642(17) 0.54175(14) 0.0175(5) Uani 1 1 d . . . . . H1 H 0.2573 0.6234 0.4959 0.021 Uiso 1 1 calc R . . . . B2 B 0.35688(18) 0.52303(17) 0.57179(16) 0.0202(6) Uani 1 1 d . . . . . H2A H 0.4226 0.5348 0.5453 0.024 Uiso 1 1 calc R . . . . B3 B 0.3493(2) 0.50934(18) 0.66482(15) 0.0206(6) Uani 1 1 d . . . . . H3 H 0.4103 0.5121 0.6989 0.025 Uiso 1 1 calc R . . . . B4 B 0.2460(2) 0.55431(17) 0.69417(14) 0.0181(5) Uani 1 1 d . . . . . H4A H 0.2383 0.5870 0.7468 0.022 Uiso 1 1 calc R . . . . B5 B 0.16592(18) 0.50511(19) 0.56113(14) 0.0176(5) Uani 1 1 d . . . . . H5A H 0.1046 0.5047 0.5273 0.021 Uiso 1 1 calc R . . . . B6 B 0.26936(18) 0.45952(18) 0.53214(14) 0.0188(6) Uani 1 1 d . . . . . H6 H 0.2769 0.4280 0.4790 0.023 Uiso 1 1 calc R . . . . B7 B 0.32668(18) 0.41757(18) 0.60799(14) 0.0184(6) Uani 1 1 d . . . . . H7 H 0.3722 0.3584 0.6047 0.022 Uiso 1 1 calc R . . . . B8 B 0.2579(2) 0.43740(17) 0.68358(14) 0.0191(6) Uani 1 1 d . . . . . H8 H 0.2579 0.3913 0.7300 0.023 Uiso 1 1 calc R . . . . B9 B 0.15883(18) 0.49144(17) 0.65400(14) 0.0166(5) Uani 1 1 d . . . . . H9 H 0.0929 0.4821 0.6808 0.020 Uiso 1 1 calc R . . . . B10 B 0.20878(18) 0.40664(19) 0.60155(15) 0.0187(6) Uani 1 1 d . . . . . H10 H 0.1764 0.3399 0.5940 0.022 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 N1 0.0114(12) 0.0127(12) 0.0107(11) 0.0009(10) 0.000 0.000 C1 0.0102(9) 0.0108(10) 0.0143(11) -0.0002(9) 0.0000(8) -0.0023(8) C2 0.0103(10) 0.0128(10) 0.0259(12) 0.0009(10) -0.0024(10) -0.0001(8) C3 0.0130(10) 0.0134(10) 0.0091(9) -0.0003(8) -0.0002(8) 0.0000(8) C4 0.0123(10) 0.0181(11) 0.0127(10) -0.0005(9) 0.0000(8) -0.0031(8) C5 0.0101(13) 0.0220(16) 0.0145(14) -0.0039(13) 0.000 0.000 B1 0.0169(13) 0.0187(12) 0.0168(12) 0.0022(10) 0.0055(11) 0.0031(12) B2 0.0155(13) 0.0142(13) 0.0308(15) 0.0005(11) 0.0045(11) 0.0036(10) B3 0.0220(14) 0.0117(12) 0.0281(15) -0.0021(11) -0.0095(11) 0.0049(11) B4 0.0230(13) 0.0145(12) 0.0168(13) 0.0007(9) -0.0031(11) 0.0026(11) B5 0.0163(13) 0.0179(13) 0.0185(12) -0.0058(10) -0.0018(10) -0.0011(10) B6 0.0215(14) 0.0179(13) 0.0170(13) -0.0026(10) 0.0006(10) 0.0035(10) B7 0.0193(13) 0.0134(12) 0.0227(14) -0.0012(10) -0.0008(10) 0.0006(10) B8 0.0271(14) 0.0134(11) 0.0169(12) 0.0022(10) -0.0004(11) 0.0006(11) B9 0.0193(13) 0.0106(12) 0.0198(12) 0.0020(10) 0.0037(10) -0.0044(10) B10 0.0201(13) 0.0126(12) 0.0235(13) -0.0024(10) 0.0008(10) -0.0032(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 N1 C3 1.338(2) 14_465 ? N1 C3 1.338(2) . ? C1 C2 1.633(3) . ? C1 C3 1.499(3) . ? C1 B1 1.733(3) . ? C1 B4 1.736(3) . ? C1 B5 1.706(3) . ? C1 B9 1.707(3) . ? C2 H2 1.1200 . ? C2 B1 1.722(4) . ? C2 B2 1.698(4) . ? C2 B3 1.697(3) . ? C2 B4 1.721(4) . ? C3 C4 1.393(3) . ? C4 H4 0.9500 . ? C4 C5 1.386(3) . ? C5 C4 1.386(3) 14_465 ? C5 H5 0.9500 . ? B1 H1 1.1200 . ? B1 B2 1.783(4) . ? B1 B5 1.776(4) . ? B1 B6 1.768(4) . ? B2 H2A 1.1200 . ? B2 B3 1.784(4) . ? B2 B6 1.786(4) . ? B2 B7 1.780(4) . ? B3 H3 1.1200 . ? B3 B4 1.778(4) . ? B3 B7 1.780(4) . ? B3 B8 1.778(4) . ? B4 H4A 1.1200 . ? B4 B8 1.771(4) . ? B4 B9 1.781(4) . ? B5 H5A 1.1200 . ? B5 B6 1.780(4) . ? B5 B9 1.781(4) . ? B5 B10 1.782(4) . ? B6 H6 1.1200 . ? B6 B7 1.792(4) . ? B6 B10 1.786(4) . ? B7 H7 1.1200 . ? B7 B8 1.793(4) . ? B7 B10 1.777(4) . ? B8 H8 1.1200 . ? B8 B9 1.780(4) . ? B8 B10 1.785(4) . ? B9 H9 1.1200 . ? B9 B10 1.779(4) . ? B10 H10 1.1200 . ? 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 C3 N1 C3 117.2(2) 14_465 . ? C2 C1 B1 61.45(16) . . ? C2 C1 B4 61.34(16) . . ? C2 C1 B5 110.38(18) . . ? C2 C1 B9 110.33(18) . . ? C3 C1 C2 117.39(18) . . ? C3 C1 B1 115.73(18) . . ? C3 C1 B4 116.52(18) . . ? C3 C1 B5 121.81(18) . . ? C3 C1 B9 122.41(18) . . ? B1 C1 B4 114.75(17) . . ? B5 C1 B1 62.18(15) . . ? B5 C1 B4 114.46(18) . . ? B5 C1 B9 62.91(15) . . ? B9 C1 B1 114.32(17) . . ? B9 C1 B4 62.27(15) . . ? C1 C2 H2 120.0 . . ? C1 C2 B1 62.15(15) . . ? C1 C2 B2 112.53(19) . . ? C1 C2 B3 112.37(19) . . ? C1 C2 B4 62.29(15) . . ? B1 C2 H2 116.7 . . ? B2 C2 H2 117.7 . . ? B2 C2 B1 62.83(16) . . ? B2 C2 B4 115.80(18) . . ? B3 C2 H2 117.9 . . ? B3 C2 B1 115.65(18) . . ? B3 C2 B2 63.40(16) . . ? B3 C2 B4 62.67(16) . . ? B4 C2 H2 116.7 . . ? B4 C2 B1 116.15(17) . . ? N1 C3 C1 116.29(18) . . ? N1 C3 C4 123.8(2) . . ? C4 C3 C1 119.95(19) . . ? C3 C4 H4 121.1 . . ? C5 C4 C3 117.7(2) . . ? C5 C4 H4 121.1 . . ? C4 C5 C4 119.8(3) 14_465 . ? C4 C5 H5 120.1 . . ? C4 C5 H5 120.1 14_465 . ? C1 B1 H1 125.0 . . ? C1 B1 B2 104.00(18) . . ? C1 B1 B5 58.16(14) . . ? C1 B1 B6 104.57(18) . . ? C2 B1 C1 56.41(13) . . ? C2 B1 H1 125.7 . . ? C2 B1 B2 57.95(14) . . ? C2 B1 B5 103.22(18) . . ? C2 B1 B6 103.90(18) . . ? B2 B1 H1 122.2 . . ? B5 B1 H1 122.5 . . ? B5 B1 B2 107.95(18) . . ? B6 B1 H1 122.8 . . ? B6 B1 B2 60.37(15) . . ? B6 B1 B5 60.28(15) . . ? C2 B2 B1 59.22(14) . . ? C2 B2 H2A 125.2 . . ? C2 B2 B3 58.26(16) . . ? C2 B2 B6 104.14(18) . . ? C2 B2 B7 104.0(2) . . ? B1 B2 H2A 121.2 . . ? B1 B2 B3 108.44(19) . . ? B1 B2 B6 59.41(15) . . ? B3 B2 H2A 121.4 . . ? B3 B2 B6 108.1(2) . . ? B6 B2 H2A 122.6 . . ? B7 B2 B1 108.02(19) . . ? B7 B2 H2A 122.5 . . ? B7 B2 B3 59.92(15) . . ? B7 B2 B6 60.32(15) . . ? C2 B3 B2 58.34(15) . . ? C2 B3 H3 125.2 . . ? C2 B3 B4 59.32(14) . . ? C2 B3 B7 104.07(18) . . ? C2 B3 B8 104.45(19) . . ? B2 B3 H3 121.2 . . ? B4 B3 B2 108.83(19) . . ? B4 B3 H3 120.9 . . ? B4 B3 B7 108.5(2) . . ? B4 B3 B8 59.74(16) . . ? B7 B3 B2 59.94(15) . . ? B7 B3 H3 122.4 . . ? B8 B3 B2 108.49(19) . . ? B8 B3 H3 122.3 . . ? B8 B3 B7 60.51(15) . . ? C1 B4 B3 103.89(18) . . ? C1 B4 H4A 125.1 . . ? C1 B4 B8 104.37(18) . . ? C1 B4 B9 58.06(14) . . ? C2 B4 C1 56.37(12) . . ? C2 B4 B3 58.01(15) . . ? C2 B4 H4A 125.7 . . ? C2 B4 B8 103.76(19) . . ? C2 B4 B9 103.06(18) . . ? B3 B4 H4A 122.3 . . ? B3 B4 B9 107.64(18) . . ? B8 B4 B3 60.14(16) . . ? B8 B4 H4A 122.9 . . ? B8 B4 B9 60.18(16) . . ? B9 B4 H4A 122.6 . . ? C1 B5 B1 59.67(14) . . ? C1 B5 H5A 124.4 . . ? C1 B5 B6 105.24(18) . . ? C1 B5 B9 58.58(14) . . ? C1 B5 B10 104.64(18) . . ? B1 B5 H5A 121.1 . . ? B1 B5 B6 59.65(15) . . ? B1 B5 B9 108.71(19) . . ? B1 B5 B10 107.99(18) . . ? B6 B5 H5A 122.2 . . ? B6 B5 B9 108.35(19) . . ? B6 B5 B10 60.20(15) . . ? B9 B5 H5A 121.3 . . ? B9 B5 B10 59.91(16) . . ? B10 B5 H5A 122.5 . . ? B1 B6 B2 60.22(15) . . ? B1 B6 B5 60.07(16) . . ? B1 B6 H6 121.3 . . ? B1 B6 B7 108.16(19) . . ? B1 B6 B10 108.12(19) . . ? B2 B6 H6 122.1 . . ? B2 B6 B7 59.70(15) . . ? B2 B6 B10 107.25(19) . . ? B5 B6 B2 107.66(18) . . ? B5 B6 H6 121.9 . . ? B5 B6 B7 107.56(19) . . ? B5 B6 B10 59.96(15) . . ? B7 B6 H6 122.0 . . ? B10 B6 H6 122.0 . . ? B10 B6 B7 59.55(15) . . ? B2 B7 B6 59.98(15) . . ? B2 B7 H7 121.7 . . ? B2 B7 B8 107.99(19) . . ? B3 B7 B2 60.14(16) . . ? B3 B7 B6 108.02(19) . . ? B3 B7 H7 121.9 . . ? B3 B7 B8 59.68(16) . . ? B6 B7 H7 121.6 . . ? B6 B7 B8 108.19(19) . . ? B8 B7 H7 121.7 . . ? B10 B7 B2 107.89(19) . . ? B10 B7 B3 107.6(2) . . ? B10 B7 B6 60.08(15) . . ? B10 B7 H7 121.9 . . ? B10 B7 B8 59.99(16) . . ? B3 B8 B7 59.81(15) . . ? B3 B8 H8 122.1 . . ? B3 B8 B9 107.63(17) . . ? B3 B8 B10 107.35(19) . . ? B4 B8 B3 60.12(16) . . ? B4 B8 B7 108.22(19) . . ? B4 B8 H8 121.3 . . ? B4 B8 B9 60.19(16) . . ? B4 B8 B10 108.23(19) . . ? B7 B8 H8 122.0 . . ? B9 B8 B7 107.49(18) . . ? B9 B8 H8 121.9 . . ? B9 B8 B10 59.87(15) . . ? B10 B8 B7 59.56(15) . . ? B10 B8 H8 122.0 . . ? C1 B9 B4 59.67(13) . . ? C1 B9 B5 58.51(15) . . ? C1 B9 B8 105.19(17) . . ? C1 B9 H9 124.5 . . ? C1 B9 B10 104.71(18) . . ? B4 B9 B5 108.71(18) . . ? B4 B9 H9 121.1 . . ? B5 B9 H9 121.2 . . ? B8 B9 B4 59.64(15) . . ? B8 B9 B5 108.40(19) . . ? B8 B9 H9 122.2 . . ? B10 B9 B4 108.04(19) . . ? B10 B9 B5 60.07(15) . . ? B10 B9 B8 60.18(15) . . ? B10 B9 H9 122.4 . . ? B5 B10 B6 59.84(15) . . ? B5 B10 B8 108.17(18) . . ? B5 B10 H10 121.8 . . ? B6 B10 H10 121.4 . . ? B7 B10 B5 108.1(2) . . ? B7 B10 B6 60.38(15) . . ? B7 B10 B8 60.45(16) . . ? B7 B10 B9 108.25(19) . . ? B7 B10 H10 121.4 . . ? B8 B10 B6 108.79(19) . . ? B8 B10 H10 121.3 . . ? B9 B10 B5 60.02(16) . . ? B9 B10 B6 108.14(19) . . ? B9 B10 B8 59.95(15) . . ? B9 B10 H10 121.7 . . ? _shelx_res_file ; spok75_0m_a.res created by SHELXL-2014/7 TITL spok75_0m_a.res in I-42d REM Old TITL spok75_0m in I-42d REM SHELXT solution in I-42d REM R1 0.122, Rweak 0.013, Alpha 0.002, Orientation as input REM Flack x = -0.373 ( 1.606 ) from Parsons' quotients REM Formula found by SHELXT: C7 B22 N CELL 0.71073 14.9695 14.9695 19.013 90 90 90 ZERR 8 0.0006 0.0006 0.001 0 0 0 LATT -2 SYMM -X,-Y,+Z SYMM +Y,-X,-Z SYMM -Y,+X,-Z SYMM 0.5-X,+Y,0.75-Z SYMM 0.5+X,-Y,0.75-Z SYMM 0.5-Y,-X,0.75+Z SYMM 0.5+Y,+X,0.75+Z SFAC C H B N UNIT 72 200 160 8 L.S. 6 PLAN 8 SIZE 0.28 0.3 0.33 TEMP -173.15 BOND $H LIST 6 fmap 2 ACTA REM REM REM WGHT 0.067400 1.851600 FVAR 0.20135 N1 4 0.187049 0.750000 0.625000 10.50000 0.01137 0.01270 = 0.01071 0.00093 0.00000 0.00000 C1 1 0.194044 0.589369 0.617320 11.00000 0.01023 0.01076 = 0.01426 -0.00017 0.00001 -0.00227 C2 1 0.302508 0.598101 0.623315 11.00000 0.01034 0.01276 = 0.02588 0.00094 -0.00242 -0.00013 AFIX 153 H2 2 0.334101 0.665240 0.630871 11.00000 -1.20000 AFIX 0 C3 1 0.140502 0.673836 0.621786 11.00000 0.01299 0.01339 = 0.00911 -0.00025 -0.00017 0.00001 C4 1 0.047499 0.670014 0.621575 11.00000 0.01231 0.01806 = 0.01269 -0.00053 -0.00001 -0.00308 AFIX 43 H4 2 0.016956 0.614469 0.619166 11.00000 -1.20000 AFIX 0 C5 1 0.001061 0.750000 0.625000 10.50000 0.01014 0.02197 = 0.01451 -0.00391 0.00000 0.00000 AFIX 43 H5 2 -0.062401 0.750001 0.624998 10.50000 -1.20000 AFIX 0 B1 3 0.257481 0.576416 0.541752 11.00000 0.01692 0.01867 = 0.01683 0.00224 0.00551 0.00306 AFIX 153 H1 2 0.257295 0.623404 0.495911 11.00000 -1.20000 AFIX 0 B2 3 0.356877 0.523033 0.571791 11.00000 0.01552 0.01415 = 0.03079 0.00049 0.00451 0.00365 AFIX 153 H2A 2 0.422625 0.534828 0.545255 11.00000 -1.20000 AFIX 0 B3 3 0.349340 0.509336 0.664820 11.00000 0.02197 0.01166 = 0.02812 -0.00213 -0.00948 0.00489 AFIX 153 H3 2 0.410299 0.512148 0.698902 11.00000 -1.20000 AFIX 0 B4 3 0.245958 0.554308 0.694166 11.00000 0.02301 0.01455 = 0.01685 0.00065 -0.00311 0.00260 AFIX 153 H4A 2 0.238322 0.586988 0.746815 11.00000 -1.20000 AFIX 0 B5 3 0.165922 0.505111 0.561126 11.00000 0.01631 0.01786 = 0.01851 -0.00576 -0.00178 -0.00108 AFIX 153 H5A 2 0.104627 0.504697 0.527349 11.00000 -1.20000 AFIX 0 B6 3 0.269362 0.459518 0.532138 11.00000 0.02145 0.01793 = 0.01698 -0.00263 0.00056 0.00346 AFIX 153 H6 2 0.276897 0.427998 0.479044 11.00000 -1.20000 AFIX 0 B7 3 0.326679 0.417575 0.607988 11.00000 0.01927 0.01335 = 0.02268 -0.00116 -0.00079 0.00056 AFIX 153 H7 2 0.372235 0.358374 0.604667 11.00000 -1.20000 AFIX 0 B8 3 0.257893 0.437400 0.683577 11.00000 0.02709 0.01340 = 0.01689 0.00216 -0.00043 0.00063 AFIX 153 H8 2 0.257936 0.391317 0.729984 11.00000 -1.20000 AFIX 0 B9 3 0.158825 0.491435 0.654004 11.00000 0.01934 0.01059 = 0.01985 0.00199 0.00371 -0.00442 AFIX 153 H9 2 0.092874 0.482063 0.680825 11.00000 -1.20000 AFIX 0 B10 3 0.208776 0.406639 0.601551 11.00000 0.02009 0.01259 = 0.02347 -0.00236 0.00083 -0.00324 AFIX 153 H10 2 0.176375 0.339877 0.594047 11.00000 -1.20000 AFIX 0 HKLF 4 REM spok75_0m_a.res in I-42d REM R1 = 0.0474 for 2267 Fo > 4sig(Fo) and 0.0525 for all 2441 data REM 137 parameters refined using 0 restraints END WGHT 0.0675 1.8459 REM Highest difference peak 0.250, deepest hole -0.261, 1-sigma level 0.051 Q1 1 0.2418 0.6112 0.7276 11.00000 0.05 0.25 Q2 1 0.2531 0.6404 0.5211 11.00000 0.05 0.24 Q3 1 0.4157 0.5514 0.5654 11.00000 0.05 0.22 Q4 1 0.3999 0.5439 0.6935 11.00000 0.05 0.19 Q5 1 0.1733 0.6371 0.6198 11.00000 0.05 0.18 Q6 1 0.1083 0.5338 0.5365 11.00000 0.05 0.17 Q7 1 0.1020 0.5076 0.6842 11.00000 0.05 0.16 Q8 1 0.2759 0.5006 0.6935 11.00000 0.05 0.15 ; _shelx_res_checksum 29023 _shelx_hkl_file ; 1 -1 0 0.10 0.10 1 -1 0 0.10 0.10 -1 1 0 0.00 0.10 -1 1 0 0.10 0.10 0 -2 0 162.48 13.80 -2 0 0 149.88 13.70 2 -2 0 5449.95 493.65 2 -2 0 6123.29 493.15 -2 2 0 5475.35 493.15 -2 2 0 5477.95 493.65 -1 3 0 4.80 0.60 1 -3 0 4.70 0.80 1 -3 0 6.20 0.60 -3 -1 0 5.70 0.70 -1 3 0 4.50 0.80 -3 1 0 4.30 0.60 3 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139.09 13.40 -4 11 -3 141.09 12.70 4 -11 -3 145.59 13.00 -4 11 -3 143.59 12.70 4 -11 3 167.08 13.60 -11 -4 3 138.69 13.00 -4 11 3 138.39 12.60 -11 -2 -3 43.90 4.20 2 -11 -3 45.30 4.40 2 -11 -3 55.39 5.00 -11 -2 3 45.90 4.60 2 -11 3 41.30 4.90 11 0 -3 0.70 0.80 -11 0 -3 1.40 0.60 0 -11 -3 1.90 0.80 0 -11 -3 1.10 0.60 11 0 3 1.50 0.60 -11 0 3 1.10 0.70 0 -11 3 1.00 0.80 0 -11 3 1.70 0.50 -2 -11 -3 45.50 4.20 -11 2 -3 50.49 4.60 11 -2 -3 46.90 4.80 -2 -11 -3 43.40 4.70 -2 -11 3 48.40 4.30 11 -2 3 43.90 4.50 -2 -11 3 45.20 4.30 -4 -11 -3 141.59 13.00 11 -4 -3 133.99 13.10 11 -4 3 139.19 12.90 -4 -11 3 145.49 12.50 -6 -11 -3 24.00 3.10 11 -6 -3 31.00 3.30 11 -6 -3 31.10 3.60 -6 -11 3 29.10 2.60 11 -6 3 27.80 3.30 11 -8 -3 78.19 6.80 -8 -11 -3 66.49 6.30 11 -8 -3 64.79 6.90 -8 -11 3 66.59 6.00 11 -8 3 57.99 6.60 -10 -11 -3 3.40 0.90 11 -10 -3 4.10 1.60 11 -10 -3 3.40 1.40 11 -10 3 6.10 1.70 11 -12 -3 5.80 1.70 11 -12 -3 5.70 1.80 11 -12 3 8.60 2.10 9 -12 -3 4.50 1.50 9 -12 -3 5.20 1.50 9 -12 3 5.40 1.60 7 -12 -3 30.10 3.50 7 -12 -3 26.60 3.80 -7 12 -3 28.80 3.10 7 -12 3 27.90 3.90 -12 -7 3 23.00 3.20 -7 12 3 30.40 3.60 5 -12 -3 107.49 9.70 5 -12 3 107.59 10.30 -12 -5 3 98.49 9.60 3 -12 -3 8.70 1.40 -12 -3 -3 7.50 0.90 3 -12 -3 6.80 1.60 -12 -3 3 8.40 1.40 3 -12 3 5.30 1.80 -12 -1 -3 17.90 2.00 1 -12 -3 21.20 2.90 1 -12 -3 19.00 2.10 -12 -1 3 18.30 2.40 12 1 3 16.70 2.00 1 -12 3 15.80 2.80 -12 1 -3 16.50 2.10 -1 -12 -3 19.00 2.80 12 -1 -3 21.60 2.80 -1 -12 -3 19.30 2.00 12 -1 3 21.10 2.30 -1 -12 3 16.40 2.70 -3 -12 -3 9.90 1.70 12 -3 -3 11.10 2.00 -3 -12 -3 7.80 0.90 12 -3 3 7.30 1.50 -3 -12 3 8.30 1.10 12 -5 -3 95.79 10.00 -5 -12 -3 107.89 9.80 -5 -12 3 106.99 9.30 12 -5 3 102.59 9.80 12 -7 -3 25.70 3.40 -7 -12 -3 24.00 3.00 12 -7 -3 30.70 3.90 -7 -12 3 27.20 2.50 12 -7 3 25.10 3.40 12 -9 -3 5.70 1.70 12 -9 -3 7.20 1.90 -9 -12 -3 8.90 1.40 12 -9 3 9.90 2.00 12 -11 -3 8.90 2.00 12 -11 -3 4.30 1.80 12 -11 3 4.60 1.60 12 -13 -3 3.00 1.80 12 -13 -3 0.50 1.20 12 -13 3 2.30 1.60 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3.10 11 -14 3 14.40 2.90 9 -14 -3 27.40 3.70 9 -14 -3 31.50 4.30 -9 14 -3 21.40 3.10 9 -14 3 32.70 4.40 -7 14 -3 11.80 1.70 7 -14 -3 12.60 2.50 7 -14 -3 14.00 2.20 7 -14 3 12.60 2.60 5 -14 -3 2.70 1.00 5 -14 -3 1.70 1.40 5 -14 3 0.90 1.10 3 -14 -3 10.00 1.70 3 -14 -3 10.90 2.20 3 -14 3 9.70 2.10 1 -14 -3 23.90 3.40 1 -14 -3 22.60 2.60 1 -14 3 24.60 3.60 -1 -14 -3 26.80 2.80 -1 -14 -3 33.90 3.60 14 -1 -3 26.10 3.50 14 -1 3 24.70 2.90 -1 -14 3 27.60 3.90 -3 -14 -3 11.10 1.30 -3 -14 -3 8.10 1.90 14 -3 -3 10.60 2.10 14 -3 3 10.70 1.80 -3 -14 3 11.00 2.20 -5 -14 -3 1.50 1.00 14 -5 -3 2.30 1.30 14 -5 3 2.70 1.10 -5 -14 3 3.00 1.30 14 -7 -3 6.40 1.80 -7 -14 -3 10.30 1.80 14 -7 3 11.00 2.00 -9 -14 -3 28.30 3.40 14 -9 -3 26.80 4.20 14 -9 3 35.90 4.30 14 -11 -3 21.60 3.70 14 -11 3 20.90 3.50 14 -13 -3 26.30 4.30 14 -13 3 25.80 4.20 12 -15 -3 23.30 4.00 12 -15 3 27.70 4.30 10 -15 -3 17.00 3.30 10 -15 -3 18.50 2.90 10 -15 3 14.00 3.10 8 -15 -3 46.10 4.90 8 -15 -3 51.79 5.60 8 -15 3 34.10 5.40 6 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36.10 5.20 -3 -16 -3 4.90 1.60 16 -3 -3 3.00 1.60 -3 -16 3 8.10 2.10 16 -3 3 2.20 1.20 16 -5 -3 14.80 2.90 -5 -16 -3 15.30 2.60 16 -5 3 18.20 2.70 -5 -16 3 17.20 3.00 16 -7 -3 44.50 5.00 -7 -16 -3 40.50 4.40 16 -7 3 35.10 4.80 -7 -16 3 38.20 5.10 16 -9 -3 3.80 1.90 16 -9 3 3.40 1.60 -9 -16 3 8.70 2.00 8 -17 -3 10.40 2.20 8 -17 -3 11.10 2.60 8 -17 3 7.30 2.50 6 -17 -3 23.60 3.30 6 -17 -3 23.20 4.00 6 -17 3 21.40 3.80 4 -17 -3 25.00 3.20 4 -17 -3 23.40 3.90 4 -17 3 25.20 4.10 2 -17 -3 27.20 3.50 2 -17 -3 23.50 3.70 2 -17 3 23.10 3.90 0 -17 -3 44.70 5.00 0 -17 3 37.00 5.40 -2 -17 -3 30.80 4.10 17 -2 -3 23.10 3.70 -2 -17 3 29.20 4.30 -4 -17 -3 31.60 4.20 17 -4 -3 30.40 4.20 -4 -17 3 26.70 4.20 17 -6 -3 21.10 3.60 -6 -17 -3 24.50 3.30 17 -6 3 18.50 3.10 -6 -17 3 26.00 3.80 17 -8 -3 8.40 2.40 -8 -17 3 9.30 2.30 17 -8 3 7.80 2.20 5 -18 -3 6.50 1.80 5 -18 -3 6.20 2.30 5 -18 3 5.70 2.50 3 -18 -3 43.20 5.40 3 -18 3 33.20 5.20 1 -18 -3 24.50 3.80 1 -18 3 23.00 3.80 -1 -18 -3 22.30 3.60 -1 -18 3 22.50 3.90 18 -3 -3 31.80 4.60 -3 -18 -3 32.70 4.70 -3 -18 3 46.40 5.50 -5 -18 -3 9.90 2.20 18 -5 -3 4.60 2.20 -5 -18 3 8.70 2.30 2 -19 -3 21.40 3.70 2 -19 3 16.20 3.50 0 -19 -3 5.90 2.00 0 -19 3 4.30 2.10 -2 -19 -3 13.80 2.90 -2 -19 3 17.50 3.30 0 0 -4 9029.10 833.02 0 0 4 9999.00 832.92 1 1 -4 -0.10 0.40 1 -1 -4 0.30 0.50 1 -1 -4 0.60 0.40 -1 -1 -4 -0.20 0.30 -1 1 -4 -0.10 0.30 1 -1 4 -0.30 0.40 1 1 4 0.20 0.30 -1 1 4 0.10 0.40 -1 -1 4 -0.10 0.40 -1 1 4 0.30 0.40 0 -2 -4 145.49 14.30 2 0 -4 148.49 14.30 2 0 -4 169.78 14.40 0 2 -4 169.38 14.30 0 -2 -4 182.18 14.30 0 -2 4 163.48 14.30 -2 0 4 145.69 14.30 -2 0 4 142.19 14.30 0 2 4 187.58 14.30 0 2 4 159.68 14.30 2 -2 -4 181.18 17.60 2 2 -4 174.78 17.50 -2 -2 -4 198.58 17.50 -2 2 -4 213.38 17.70 2 2 4 202.18 17.50 -2 -2 4 216.78 17.60 -2 2 4 234.28 17.70 -2 2 4 175.68 17.60 3 1 -4 47.00 4.30 1 -3 -4 46.20 4.30 1 -3 -4 44.60 4.40 -1 3 -4 42.10 4.30 -1 3 4 46.80 4.30 -3 -1 4 59.19 4.50 -3 -1 4 50.79 4.40 1 -3 4 46.00 4.30 -1 3 4 42.90 4.40 -1 -3 -4 44.90 4.30 3 -1 -4 46.20 4.40 1 3 -4 47.60 4.30 3 -1 -4 56.19 4.60 -1 -3 -4 48.40 4.40 -3 1 4 43.10 4.40 -3 1 4 45.60 4.40 1 3 4 45.80 4.30 -1 -3 4 50.29 4.40 3 -3 -4 0.00 0.40 3 -3 -4 -0.10 0.30 3 3 -4 0.10 0.20 -3 -3 -4 -0.10 0.20 -3 -3 4 0.40 0.30 -3 3 4 -0.40 0.30 -3 3 4 -0.10 0.40 3 3 4 -0.20 0.20 4 2 -4 16.60 1.80 2 -4 -4 19.50 1.90 -2 4 -4 18.00 1.90 2 -4 -4 19.20 2.00 -2 4 4 17.20 2.00 -4 -2 4 22.70 2.00 -2 4 4 17.80 1.90 -4 -2 4 16.20 1.80 0 -4 -4 338.47 27.60 0 4 -4 297.07 27.60 0 -4 -4 368.86 27.70 4 0 -4 297.17 27.80 0 -4 4 296.97 27.60 0 4 4 300.27 27.70 0 4 4 311.17 27.50 -4 0 4 302.97 27.70 -4 0 4 311.37 27.70 2 4 -4 17.20 1.50 -2 -4 -4 17.60 1.70 4 -2 -4 15.20 1.90 4 -2 -4 15.80 1.80 -2 -4 4 18.30 1.70 -4 2 4 16.90 1.80 2 4 4 17.40 1.70 -4 2 4 16.20 1.80 4 -4 -4 3.60 0.90 -4 -4 -4 5.00 0.60 4 -4 -4 5.20 0.90 -4 4 4 5.90 1.00 -4 -4 4 5.70 0.70 4 -4 4 4.80 1.00 -4 4 4 4.70 0.90 -3 5 -4 72.59 7.40 -3 5 -4 78.89 7.40 3 -5 -4 87.19 7.50 3 -5 -4 101.69 7.70 -3 5 4 82.09 7.40 -3 5 4 81.19 7.60 -5 -3 4 73.49 7.30 -1 5 -4 5.40 0.80 1 -5 -4 5.20 0.80 1 -5 -4 4.00 0.90 -1 5 -4 5.40 0.70 5 1 -4 5.30 0.80 -1 5 4 5.10 0.70 -5 -1 4 4.80 0.80 5 1 4 5.40 0.50 -1 5 4 5.40 1.00 -5 -1 4 5.30 0.90 5 -1 -4 5.30 0.90 -1 -5 -4 5.70 0.70 -1 -5 -4 5.10 0.90 5 -1 -4 5.30 1.00 1 5 -4 5.60 0.50 5 -1 4 5.20 0.80 -1 -5 4 6.10 0.80 -5 1 4 7.30 1.10 1 5 4 5.30 0.90 -5 1 4 4.00 0.80 -3 -5 -4 90.79 7.30 5 -3 -4 76.49 7.60 5 -3 -4 71.59 7.40 5 -3 4 80.79 7.50 -3 -5 4 90.89 7.30 -5 3 4 69.99 7.40 -5 3 4 82.09 7.60 -5 -5 -4 0.00 0.20 5 -5 -4 0.50 0.40 5 -5 -4 -0.90 0.50 -5 5 -4 0.10 0.50 -5 5 4 0.20 0.40 -5 -5 4 0.00 0.30 5 -5 4 0.50 0.60 -5 5 4 -0.20 0.50 4 -6 -4 41.90 4.20 4 -6 -4 46.30 4.10 -4 6 -4 38.50 3.90 -4 6 4 37.10 4.10 -6 -4 4 46.40 3.90 4 -6 4 34.80 4.20 -4 6 4 41.40 4.00 -2 6 -4 252.87 19.90 6 2 -4 227.58 19.80 -2 6 -4 201.28 19.80 2 -6 -4 213.68 20.10 2 -6 -4 214.88 19.90 -6 -2 4 264.77 20.10 -2 6 4 227.18 20.10 -2 6 4 216.08 19.80 -6 -2 4 207.48 19.90 6 0 -4 555.84 51.89 0 6 -4 596.64 51.59 0 6 -4 630.94 51.59 0 -6 -4 583.74 51.69 0 -6 -4 568.74 51.89 6 0 4 583.84 51.69 0 6 4 593.64 51.89 0 -6 4 620.74 51.79 -6 0 4 564.74 51.89 6 -2 -4 259.57 21.70 -2 -6 -4 254.67 21.50 6 -2 -4 269.37 21.60 -6 2 4 283.67 21.70 -6 2 4 228.98 21.50 -2 -6 4 220.48 21.30 2 6 4 214.98 21.50 6 -2 4 218.48 21.50 6 -4 -4 55.29 4.40 6 -4 -4 40.20 4.40 -4 -6 -4 42.10 4.10 -6 4 -4 56.19 4.40 6 -4 4 36.20 4.20 -4 -6 4 47.50 4.00 -6 4 4 38.70 4.20 -6 4 4 39.10 4.30 6 -6 -4 129.29 12.30 -6 -6 -4 123.89 12.00 -6 6 -4 119.89 12.20 6 -6 -4 147.69 12.60 -6 6 4 147.19 12.40 -6 6 4 122.29 12.50 6 -6 4 165.48 12.70 -6 -6 4 143.39 12.10 5 -7 -4 13.50 1.80 -7 -5 -4 12.40 1.10 -5 7 -4 12.90 1.70 -7 -5 -4 12.70 1.10 5 -7 -4 12.40 2.00 -5 7 4 12.90 1.70 -7 -5 4 13.10 1.40 5 -7 4 11.60 1.90 3 -7 -4 29.10 3.00 -3 7 -4 25.80 2.90 3 -7 -4 26.80 3.10 -3 7 -4 28.30 2.90 -7 -3 4 28.00 3.00 -7 -3 4 35.00 2.90 -3 7 4 33.50 2.90 -3 7 4 26.70 3.10 3 -7 4 29.40 3.30 1 -7 -4 81.49 6.80 -1 7 -4 66.69 6.40 -1 7 -4 67.99 6.30 1 -7 -4 64.19 6.50 7 1 -4 68.09 6.50 -7 -1 4 85.79 6.60 -1 7 4 65.89 6.70 7 1 4 74.79 6.30 -7 -1 4 69.09 6.60 -1 -7 -4 69.29 6.00 7 -1 -4 61.29 6.20 7 -1 -4 66.99 6.40 -1 -7 -4 60.69 6.20 -7 1 4 64.29 6.20 -1 -7 4 73.69 6.10 -7 1 4 69.19 6.30 1 7 4 67.49 6.30 7 -1 4 65.99 6.10 7 -3 -4 27.10 3.00 7 -3 -4 26.90 3.20 -3 -7 -4 29.30 3.00 -7 3 4 30.00 3.10 -7 3 4 28.70 3.10 7 -3 4 34.80 3.10 -3 -7 4 29.10 2.80 -5 -7 -4 12.00 1.30 7 -5 -4 10.70 1.60 7 -5 -4 12.70 1.90 -7 5 -4 9.90 1.50 -5 -7 4 11.90 1.20 7 -5 4 9.90 1.70 -7 5 4 11.80 1.80 -7 5 4 10.40 1.60 -7 7 -4 0.30 0.60 -7 -7 -4 0.30 0.30 7 -7 -4 -0.60 0.70 7 -7 -4 0.80 0.70 -7 -7 4 0.00 0.40 -7 7 4 -1.00 0.50 7 -7 4 0.40 0.80 6 -8 -4 147.19 13.70 -6 8 -4 155.18 13.60 -8 -6 -4 146.09 13.20 -8 -6 -4 147.59 13.20 6 -8 4 127.29 13.80 -6 8 4 170.88 13.70 -8 -6 4 159.68 13.40 4 -8 -4 100.59 8.40 -4 8 -4 97.29 7.90 4 -8 -4 79.09 8.00 -4 8 -4 83.09 7.90 -4 8 4 85.29 7.90 -8 -4 4 77.49 8.00 -8 -4 4 84.89 7.90 4 -8 4 85.89 8.30 -2 8 -4 69.69 6.30 2 -8 -4 69.29 6.60 -2 8 -4 65.49 6.20 2 -8 -4 69.39 6.40 -8 -2 4 72.79 6.40 -2 8 4 67.19 6.70 -2 8 4 70.19 6.20 -8 -2 4 67.69 6.50 0 -8 -4 131.09 12.80 8 0 -4 143.79 12.90 0 -8 -4 143.89 12.60 8 0 -4 128.49 12.70 0 8 4 135.49 12.90 8 0 4 133.99 12.50 -8 0 4 163.58 12.80 0 -8 4 151.98 12.70 8 -2 -4 70.99 6.80 8 -2 -4 81.69 7.10 -2 -8 -4 68.99 6.90 -2 -8 -4 76.09 6.50 -8 2 4 70.79 6.90 -8 2 4 75.19 6.90 8 -2 4 70.49 6.80 -2 -8 4 73.19 6.60 8 -4 -4 101.19 8.50 -4 -8 -4 83.39 8.30 8 -4 -4 109.09 8.70 -8 4 4 87.09 8.50 8 -4 4 86.59 8.40 -4 -8 4 86.49 8.10 8 -6 -4 145.99 13.00 8 -6 -4 148.99 13.20 -6 -8 -4 139.39 12.80 8 -6 4 132.49 13.10 -6 -8 4 144.99 12.60 -8 -8 -4 43.50 4.10 8 -8 -4 42.20 4.50 8 -8 -4 52.99 4.90 8 -8 4 55.49 4.90 -8 -8 4 38.20 4.10 -7 9 -4 142.59 11.00 7 -9 -4 117.79 11.20 7 -9 -4 115.99 11.00 -9 -7 -4 113.09 10.50 -9 -7 -4 114.89 10.50 -7 9 4 112.99 10.90 7 -9 4 110.49 11.20 -9 -7 4 126.69 10.70 -5 9 -4 63.89 5.80 5 -9 -4 53.79 6.00 -5 9 -4 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2.60 1.60 0 5 -23 1.60 1.60 5 -2 -23 12.20 2.80 -5 2 -23 14.30 3.00 -2 -5 -23 14.60 3.10 2 5 -23 10.90 2.50 -4 -5 -23 2.00 1.90 5 -4 -23 3.30 1.90 4 5 -23 1.80 1.60 -5 4 -23 2.10 1.70 -6 -3 -23 7.50 2.50 6 3 -23 10.00 2.40 3 -6 -23 11.10 2.70 -3 6 -23 12.60 2.60 -1 6 -23 9.60 2.40 -6 -1 -23 13.20 2.90 6 1 -23 9.50 2.30 1 -6 -23 7.10 2.40 -6 1 -23 6.50 2.20 1 6 -23 7.50 2.00 -1 -6 -23 9.60 2.60 6 -1 -23 8.10 2.30 -6 3 -23 14.20 3.00 -3 -6 -23 10.70 2.80 6 -3 -23 13.00 2.90 3 6 -23 8.70 2.20 -7 0 -23 10.90 2.80 0 0 -24 34.80 4.90 -1 1 -24 -0.50 1.50 1 -1 -24 -0.50 1.50 -1 -1 -24 -0.60 1.50 1 1 -24 -0.20 1.60 2 0 -24 11.20 2.70 -2 0 -24 11.00 2.80 0 -2 -24 10.20 2.60 0 2 -24 7.50 2.40 2 2 -24 16.50 3.20 -2 -2 -24 21.30 3.80 2 -2 -24 17.00 3.40 -2 2 -24 32.20 4.30 1 -3 -24 15.60 3.20 -3 -1 -24 16.80 3.50 -1 3 -24 26.40 3.70 3 1 -24 19.00 3.40 -3 1 -24 26.60 4.00 -1 -3 -24 24.90 3.90 1 3 -24 18.60 3.30 3 -1 -24 13.00 3.20 3 3 -24 -0.80 1.40 3 -3 -24 -2.30 1.30 -3 3 -24 1.20 1.60 -3 -3 -24 2.70 1.90 -4 -2 -24 4.70 2.10 4 0 -24 -1.80 1.30 0 4 -24 0.70 1.60 0 -4 -24 2.00 1.70 -4 0 -24 -0.90 1.50 -4 2 -24 5.70 2.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 9929 _olex2_submission_special_instructions 'No special instructions were received'