data_spok71_0m_a _audit_creation_date 2017-09-29 _audit_creation_method ; Olex2 1.2-beta (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _shelx_SHELXL_version_number '2016/6' _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. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C12 H18 B10 N2' _chemical_formula_sum 'C12 H18 B10 N2' _chemical_formula_weight 298.38 _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 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.6774(4) _cell_length_b 7.4665(3) _cell_length_c 20.6215(8) _cell_angle_alpha 90 _cell_angle_beta 104.1230(10) _cell_angle_gamma 90 _cell_volume 1594.31(11) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8238 _cell_measurement_temperature 100 _cell_measurement_theta_max 68.355 _cell_measurement_theta_min 4.303 _shelx_estimated_absorpt_T_max 0.901 _shelx_estimated_absorpt_T_min 0.881 _exptl_absorpt_coefficient_mu 0.465 _exptl_absorpt_correction_T_max 0.5210 _exptl_absorpt_correction_T_min 0.4338 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0756 before and 0.0530 after correction. The Ratio of minimum to maximum transmission is 0.8326. 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 1.243 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 616 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.23 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_unetI/netI 0.0354 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 11345 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 68.354 _diffrn_reflns_theta_min 4.302 _diffrn_ambient_temperature 100.15 _diffrn_detector 'Bruker Platinum135 CCD' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD Area Detector' _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device 'Fixed Chi Three-Circle Diffractometer' _diffrn_measurement_device_type 'Bruker D8 Platinum135' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'Multilayer Mirrors' _diffrn_radiation_probe X-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source 'Micro Focus Rotating Anode' _diffrn_source_type 'Bruker FR-591' _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2696 _reflns_number_total 2906 _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 'APEX3 v2016.1-0 (Bruker, 2016)' _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 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.248 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.047 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 254 _refine_ls_number_reflns 2906 _refine_ls_number_restraints 343 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0442 _refine_ls_restrained_S_all 0.986 _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^)+(0.0710P)^2^+0.5656P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1180 _refine_ls_wR_factor_ref 0.1217 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All B(H) groups, All C(H) groups, All C(H,H) groups 2. Restrained distances N2-C10 1.4 with sigma of 0.02 3. Rigid body (RIGU) restrains All non-hydrogen atoms with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002 4. Others Sof(H00C)=Sof(N2)=Sof(C10)=Sof(H0)=Sof(C10')=Sof(H0AA)=Sof(C9')=Sof(H1)=1- FVAR(1) Sof(N2')=Sof(C9)=Sof(H9)=Sof(C12)=Sof(H12)=Sof(H11)=Sof(C12')=Sof(H12')=FVAR(1) 5.a Aromatic/amide H refined with riding coordinates: C9(H9), C6(H6), C12(H12), C4(H4), C11(H11), C11(H00C), C7(H7), C12'(H12'), C5(H5), C10(H0), C10'(H0AA), C9'(H1) 5.b Boron cage BH refined with riding coordinates: B10(H10), B8(H8), B2(H2), B1(H1A), B7(H7A), B4(H4A), B9(H9A), B6(H6A), B5(H5A), B3(H3) ; _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 0.66159(10) 0.91869(16) 0.49541(5) 0.0255(3) Uani 1 1 d . U . . . N2' N 0.3332(13) 0.553(2) 0.2560(6) 0.0239(19) Uani 0.555(13) 1 d . U P A 1 C3 C 0.76079(12) 0.82187(17) 0.48586(6) 0.0197(3) Uani 1 1 d . U . . . C9 C 0.3049(10) 0.461(2) 0.3624(6) 0.0230(14) Uani 0.555(13) 1 d . U P A 1 H9 H 0.341260 0.423984 0.407112 0.028 Uiso 0.555(13) 1 calc R . P A 1 C8 C 0.38533(12) 0.51334(17) 0.31872(6) 0.0199(3) Uani 1 1 d . U . . . C1 C 0.72546(11) 0.68362(17) 0.43080(6) 0.0190(3) Uani 1 1 d . U . . . C2 C 0.53046(11) 0.52521(17) 0.34501(6) 0.0193(3) Uani 1 1 d . U . . . C6 C 0.80779(14) 1.07094(19) 0.58525(7) 0.0291(3) Uani 1 1 d . U . . . H6 H 0.821205 1.158915 0.619536 0.035 Uiso 1 1 calc R . . . . C12 C 0.2108(10) 0.544(3) 0.2301(6) 0.0276(16) Uani 0.555(13) 1 d . U P A 1 H12 H 0.177518 0.563171 0.183541 0.033 Uiso 0.555(13) 1 calc R . P A 1 C4 C 0.88621(13) 0.8426(2) 0.52414(7) 0.0286(3) Uani 1 1 d . U . . . H4 H 0.954593 0.771728 0.515899 0.034 Uiso 1 1 calc R . . . . C11 C 0.12426(12) 0.50358(19) 0.27241(7) 0.0278(3) Uani 1 1 d . U . . . H11 H 0.033462 0.504454 0.254352 0.033 Uiso 0.555(13) 1 calc R . P A 1 H00C H 0.032719 0.499061 0.258273 0.033 Uiso 0.445(13) 1 calc R . P A 2 C7 C 0.68602(14) 1.04080(19) 0.54439(7) 0.0285(3) Uani 1 1 d . U . . . H7 H 0.616114 1.110476 0.551494 0.034 Uiso 1 1 calc R . . . . C12' C 0.1724(9) 0.465(3) 0.3364(7) 0.0272(14) Uani 0.555(13) 1 d . U P A 1 H12' H 0.116012 0.441467 0.364581 0.033 Uiso 0.555(13) 1 calc R . P A 1 C5 C 0.90909(14) 0.9697(2) 0.57478(8) 0.0336(4) Uani 1 1 d . U . . . H5 H 0.993837 0.986728 0.602016 0.040 Uiso 1 1 calc R . . . . B10 B 0.58624(13) 0.5690(2) 0.42829(7) 0.0201(3) Uani 1 1 d . U . . . H10 H 0.523523 0.589688 0.463978 0.024 Uiso 1 1 calc R . . . . B8 B 0.75311(13) 0.7252(2) 0.35290(7) 0.0232(3) Uani 1 1 d . U . . . H8 H 0.801685 0.847957 0.339595 0.028 Uiso 1 1 calc R . . . . B2 B 0.62317(13) 0.6187(2) 0.29557(7) 0.0231(3) Uani 1 1 d . U . . . H2 H 0.584256 0.669873 0.243482 0.028 Uiso 1 1 calc R . . . . B1 B 0.59541(13) 0.73254(19) 0.36614(7) 0.0193(3) Uani 1 1 d . U . . . H1A H 0.538732 0.860199 0.360870 0.023 Uiso 1 1 calc R . . . . B7 B 0.60688(14) 0.3543(2) 0.39614(7) 0.0239(3) Uani 1 1 d . U . . . H7A H 0.557202 0.232999 0.409810 0.029 Uiso 1 1 calc R . . . . B4 B 0.73753(14) 0.4600(2) 0.45333(8) 0.0243(3) Uani 1 1 d . U . . . H4A H 0.776076 0.409760 0.505571 0.029 Uiso 1 1 calc R . . . . B9 B 0.84061(14) 0.5560(2) 0.40653(8) 0.0257(3) Uani 1 1 d . U . . . H9A H 0.947124 0.568488 0.428273 0.031 Uiso 1 1 calc R . . . . B6 B 0.77490(14) 0.5089(2) 0.32045(8) 0.0280(4) Uani 1 1 d . U . . . H6A H 0.837752 0.488266 0.284820 0.034 Uiso 1 1 calc R . . . . B5 B 0.63026(14) 0.3851(2) 0.31393(8) 0.0251(3) Uani 1 1 d . U . . . H5A H 0.595667 0.283247 0.273659 0.030 Uiso 1 1 calc R . . . . B3 B 0.76525(14) 0.3453(2) 0.38242(8) 0.0288(4) Uani 1 1 d . U . . . H3 H 0.821514 0.217312 0.387547 0.035 Uiso 1 1 calc R . . . . N2 N 0.3222(11) 0.474(3) 0.3615(7) 0.0273(18) Uani 0.445(13) 1 d D U P A 2 C10 C 0.1929(13) 0.456(4) 0.3402(9) 0.029(2) Uani 0.445(13) 1 d D U P A 2 H0 H 0.145463 0.411337 0.370247 0.034 Uiso 0.445(13) 1 calc R . P A 2 C10' C 0.1936(11) 0.552(3) 0.2327(8) 0.0257(17) Uani 0.445(13) 1 d . U P A 2 H0AA H 0.150255 0.590369 0.189029 0.031 Uiso 0.445(13) 1 calc R . P A 2 C9' C 0.336(2) 0.552(3) 0.2501(9) 0.024(2) Uani 0.445(13) 1 d . U P A 2 H1 H 0.387516 0.575115 0.219481 0.029 Uiso 0.445(13) 1 calc R . 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 N1 0.0227(5) 0.0281(6) 0.0251(6) -0.0038(4) 0.0044(4) 0.0038(4) N2' 0.0230(19) 0.024(4) 0.026(3) 0.003(2) 0.0081(17) -0.004(2) C3 0.0201(6) 0.0194(6) 0.0195(6) 0.0032(5) 0.0045(4) 0.0005(5) C9 0.017(3) 0.033(3) 0.022(2) -0.0011(17) 0.0090(19) -0.002(2) C8 0.0173(6) 0.0189(6) 0.0235(6) -0.0030(5) 0.0049(5) -0.0004(4) C1 0.0151(6) 0.0207(6) 0.0207(6) 0.0018(5) 0.0033(4) 0.0020(4) C2 0.0172(6) 0.0210(7) 0.0199(6) -0.0007(5) 0.0047(5) -0.0002(5) C6 0.0344(7) 0.0251(7) 0.0258(7) -0.0050(5) 0.0032(5) -0.0015(6) C12 0.023(3) 0.033(3) 0.028(2) -0.0001(18) 0.0084(19) 0.003(3) C4 0.0208(6) 0.0280(7) 0.0338(7) -0.0052(6) 0.0007(5) 0.0023(5) C11 0.0168(6) 0.0253(7) 0.0395(8) -0.0071(6) 0.0036(6) -0.0004(5) C7 0.0295(7) 0.0286(8) 0.0272(7) -0.0047(5) 0.0063(5) 0.0044(5) C12' 0.014(3) 0.033(3) 0.036(2) -0.0047(19) 0.0097(19) 0.004(3) C5 0.0255(7) 0.0334(8) 0.0361(8) -0.0086(6) -0.0035(6) -0.0010(6) B10 0.0182(6) 0.0211(7) 0.0205(7) 0.0019(5) 0.0035(5) -0.0012(5) B8 0.0202(7) 0.0281(8) 0.0225(7) -0.0019(6) 0.0076(5) -0.0029(6) B2 0.0205(7) 0.0286(8) 0.0218(7) -0.0024(6) 0.0080(5) -0.0036(6) B1 0.0177(6) 0.0211(7) 0.0184(6) 0.0009(5) 0.0031(5) -0.0003(5) B7 0.0227(7) 0.0197(7) 0.0272(7) 0.0009(6) 0.0021(5) 0.0010(5) B4 0.0220(7) 0.0198(8) 0.0286(8) 0.0015(5) 0.0010(6) 0.0028(5) B9 0.0166(7) 0.0262(8) 0.0331(8) -0.0066(6) 0.0040(6) 0.0030(5) B6 0.0192(7) 0.0339(9) 0.0325(8) -0.0106(6) 0.0095(6) -0.0023(6) B5 0.0197(7) 0.0267(8) 0.0295(7) -0.0068(6) 0.0074(5) 0.0009(6) B3 0.0208(7) 0.0252(8) 0.0377(8) -0.0075(6) 0.0018(6) 0.0038(6) N2 0.016(3) 0.037(4) 0.029(2) -0.002(2) 0.0061(18) -0.001(2) C10 0.020(3) 0.036(4) 0.033(3) -0.001(2) 0.012(3) 0.004(4) C10' 0.014(3) 0.025(3) 0.034(3) 0.000(3) -0.0024(19) 0.004(3) C9' 0.017(3) 0.031(6) 0.023(3) -0.003(3) 0.001(2) 0.002(3) _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 1.3361(17) . ? N1 C7 1.3382(18) . ? N2' C8 1.311(11) . ? N2' C12 1.287(16) . ? C3 C1 1.5126(17) . ? C3 C4 1.3873(18) . ? C9 H9 0.9500 . ? C9 C8 1.442(9) . ? C9 C12' 1.385(9) . ? C8 C2 1.5142(16) . ? C8 N2 1.269(10) . ? C8 C9' 1.413(17) . ? C1 B10 1.7052(18) . ? C1 B8 1.7307(18) . ? C1 B1 1.7136(17) . ? C1 B4 1.7292(19) . ? C1 B9 1.7237(18) . ? C2 B10 1.7063(18) . ? C2 B2 1.7319(18) . ? C2 B1 1.7087(18) . ? C2 B7 1.7279(19) . ? C2 B5 1.7247(18) . ? C6 H6 0.9500 . ? C6 C7 1.384(2) . ? C6 C5 1.379(2) . ? C12 H12 0.9500 . ? C12 C11 1.449(10) . ? C4 H4 0.9500 . ? C4 C5 1.388(2) . ? C11 H11 0.9500 . ? C11 H00C 0.9500 . ? C11 C12' 1.326(12) . ? C11 C10 1.456(15) . ? C11 C10' 1.283(14) . ? C7 H7 0.9500 . ? C12' H12' 0.9500 . ? C5 H5 0.9500 . ? B10 H10 1.1200 . ? B10 B1 1.790(2) . ? B10 B7 1.769(2) . ? B10 B4 1.7693(19) . ? B8 H8 1.1200 . ? B8 B2 1.776(2) . ? B8 B1 1.7712(19) . ? B8 B9 1.785(2) . ? B8 B6 1.785(2) . ? B2 H2 1.1200 . ? B2 B1 1.7715(19) . ? B2 B6 1.776(2) . ? B2 B5 1.783(2) . ? B1 H1A 1.1200 . ? B7 H7A 1.1200 . ? B7 B4 1.777(2) . ? B7 B5 1.788(2) . ? B7 B3 1.782(2) . ? B4 H4A 1.1200 . ? B4 B9 1.782(2) . ? B4 B3 1.781(2) . ? B9 H9A 1.1200 . ? B9 B6 1.777(2) . ? B9 B3 1.781(2) . ? B6 H6A 1.1200 . ? B6 B5 1.777(2) . ? B6 B3 1.789(2) . ? B5 H5A 1.1200 . ? B5 B3 1.780(2) . ? B3 H3 1.1200 . ? N2 C10 1.350(11) . ? C10 H0 0.9500 . ? C10' H0AA 0.9500 . ? C10' C9' 1.47(2) . ? C9' H1 0.9500 . ? 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 C7 117.67(11) . . ? C12 N2' C8 122.8(12) . . ? N1 C3 C1 114.74(11) . . ? N1 C3 C4 123.07(12) . . ? C4 C3 C1 122.18(11) . . ? C8 C9 H9 121.3 . . ? C12' C9 H9 121.3 . . ? C12' C9 C8 117.4(10) . . ? N2' C8 C9 120.2(8) . . ? N2' C8 C2 119.4(6) . . ? C9 C8 C2 120.4(5) . . ? N2 C8 C2 115.8(6) . . ? N2 C8 C9' 127.7(11) . . ? C9' C8 C2 116.5(9) . . ? C3 C1 B10 114.91(10) . . ? C3 C1 B8 120.44(10) . . ? C3 C1 B1 116.42(10) . . ? C3 C1 B4 117.94(10) . . ? C3 C1 B9 122.04(10) . . ? B10 C1 B8 113.99(9) . . ? B10 C1 B1 63.15(8) . . ? B10 C1 B4 62.01(8) . . ? B10 C1 B9 113.07(10) . . ? B1 C1 B8 61.89(8) . . ? B1 C1 B4 114.08(10) . . ? B1 C1 B9 113.07(10) . . ? B4 C1 B8 113.83(10) . . ? B9 C1 B8 62.24(8) . . ? B9 C1 B4 62.13(8) . . ? C8 C2 B10 116.55(10) . . ? C8 C2 B2 119.66(10) . . ? C8 C2 B1 117.42(10) . . ? C8 C2 B7 117.70(10) . . ? C8 C2 B5 120.17(10) . . ? B10 C2 B2 113.96(9) . . ? B10 C2 B1 63.23(8) . . ? B10 C2 B7 61.99(8) . . ? B10 C2 B5 113.24(10) . . ? B1 C2 B2 61.98(8) . . ? B1 C2 B7 114.30(9) . . ? B1 C2 B5 113.28(10) . . ? B7 C2 B2 113.84(10) . . ? B5 C2 B2 62.10(8) . . ? B5 C2 B7 62.36(8) . . ? C7 C6 H6 120.9 . . ? C5 C6 H6 120.9 . . ? C5 C6 C7 118.14(13) . . ? N2' C12 H12 120.2 . . ? N2' C12 C11 119.5(11) . . ? C11 C12 H12 120.2 . . ? C3 C4 H4 120.9 . . ? C3 C4 C5 118.21(13) . . ? C5 C4 H4 120.9 . . ? C12 C11 H11 120.2 . . ? C12' C11 C12 119.7(7) . . ? C12' C11 H11 120.2 . . ? C10 C11 H00C 121.7 . . ? C10' C11 H00C 121.7 . . ? C10' C11 C10 116.7(8) . . ? N1 C7 C6 123.45(13) . . ? N1 C7 H7 118.3 . . ? C6 C7 H7 118.3 . . ? C9 C12' H12' 119.9 . . ? C11 C12' C9 120.1(11) . . ? C11 C12' H12' 119.9 . . ? C6 C5 C4 119.46(13) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C1 B10 C2 102.38(9) . . ? C1 B10 H10 124.6 . . ? C1 B10 B1 58.65(7) . . ? C1 B10 B7 106.19(10) . . ? C1 B10 B4 59.66(8) . . ? C2 B10 H10 124.7 . . ? C2 B10 B1 58.45(7) . . ? C2 B10 B7 59.60(8) . . ? C2 B10 B4 105.98(10) . . ? B1 B10 H10 121.5 . . ? B7 B10 H10 121.4 . . ? B7 B10 B1 108.43(10) . . ? B7 B10 B4 60.29(8) . . ? B4 B10 H10 121.4 . . ? B4 B10 B1 108.48(10) . . ? C1 B8 H8 124.6 . . ? C1 B8 B2 104.79(9) . . ? C1 B8 B1 58.58(7) . . ? C1 B8 B9 58.69(8) . . ? C1 B8 B6 104.67(11) . . ? B2 B8 H8 122.4 . . ? B2 B8 B9 107.55(11) . . ? B2 B8 B6 59.84(8) . . ? B1 B8 H8 121.8 . . ? B1 B8 B2 59.92(8) . . ? B1 B8 B9 107.46(10) . . ? B1 B8 B6 107.56(10) . . ? B9 B8 H8 121.8 . . ? B6 B8 H8 122.6 . . ? B6 B8 B9 59.71(9) . . ? C2 B2 B8 104.74(9) . . ? C2 B2 H2 124.8 . . ? C2 B2 B1 58.37(7) . . ? C2 B2 B6 104.83(10) . . ? C2 B2 B5 58.75(8) . . ? B8 B2 H2 122.2 . . ? B8 B2 B6 60.33(8) . . ? B8 B2 B5 108.10(11) . . ? B1 B2 B8 59.91(8) . . ? B1 B2 H2 121.8 . . ? B1 B2 B6 107.93(10) . . ? B1 B2 B5 107.57(10) . . ? B6 B2 H2 122.2 . . ? B6 B2 B5 59.89(9) . . ? B5 B2 H2 121.6 . . ? C1 B1 B10 58.20(7) . . ? C1 B1 B8 59.53(7) . . ? C1 B1 B2 105.71(9) . . ? C1 B1 H1A 125.0 . . ? C2 B1 C1 101.93(9) . . ? C2 B1 B10 58.32(8) . . ? C2 B1 B8 105.93(10) . . ? C2 B1 B2 59.66(8) . . ? C2 B1 H1A 124.8 . . ? B10 B1 H1A 121.8 . . ? B8 B1 B10 108.01(10) . . ? B8 B1 B2 60.17(8) . . ? B8 B1 H1A 121.5 . . ? B2 B1 B10 108.07(10) . . ? B2 B1 H1A 121.6 . . ? C2 B7 B10 58.40(8) . . ? C2 B7 H7A 124.7 . . ? C2 B7 B4 104.73(10) . . ? C2 B7 B5 58.73(8) . . ? C2 B7 B3 104.84(10) . . ? B10 B7 H7A 121.9 . . ? B10 B7 B4 59.87(8) . . ? B10 B7 B5 107.34(10) . . ? B10 B7 B3 107.67(10) . . ? B4 B7 H7A 122.4 . . ? B4 B7 B5 107.68(10) . . ? B4 B7 B3 60.04(8) . . ? B5 B7 H7A 121.8 . . ? B3 B7 H7A 122.4 . . ? B3 B7 B5 59.80(8) . . ? C1 B4 B10 58.33(7) . . ? C1 B4 B7 104.81(10) . . ? C1 B4 H4A 124.6 . . ? C1 B4 B9 58.78(8) . . ? C1 B4 B3 105.08(11) . . ? B10 B4 B7 59.83(8) . . ? B10 B4 H4A 122.0 . . ? B10 B4 B9 107.33(10) . . ? B10 B4 B3 107.72(10) . . ? B7 B4 H4A 122.3 . . ? B7 B4 B9 107.92(11) . . ? B7 B4 B3 60.13(8) . . ? B9 B4 H4A 121.7 . . ? B3 B4 H4A 122.2 . . ? B3 B4 B9 60.01(9) . . ? C1 B9 B8 59.07(8) . . ? C1 B9 B4 59.09(8) . . ? C1 B9 H9A 124.3 . . ? C1 B9 B6 105.29(10) . . ? C1 B9 B3 105.29(10) . . ? B8 B9 H9A 121.0 . . ? B4 B9 B8 108.72(10) . . ? B4 B9 H9A 121.2 . . ? B6 B9 B8 60.13(9) . . ? B6 B9 B4 108.42(10) . . ? B6 B9 H9A 122.1 . . ? B6 B9 B3 60.35(9) . . ? B3 B9 B8 108.63(11) . . ? B3 B9 B4 59.97(9) . . ? B3 B9 H9A 122.1 . . ? B8 B6 H6A 121.6 . . ? B8 B6 B3 108.32(11) . . ? B2 B6 B8 59.83(8) . . ? B2 B6 B9 107.88(10) . . ? B2 B6 H6A 121.6 . . ? B2 B6 B5 60.24(8) . . ? B2 B6 B3 108.31(10) . . ? B9 B6 B8 60.16(8) . . ? B9 B6 H6A 121.9 . . ? B9 B6 B3 59.94(9) . . ? B5 B6 B8 107.98(10) . . ? B5 B6 B9 107.61(11) . . ? B5 B6 H6A 121.9 . . ? B5 B6 B3 59.88(9) . . ? B3 B6 H6A 121.5 . . ? C2 B5 B2 59.15(8) . . ? C2 B5 B7 58.91(8) . . ? C2 B5 B6 105.11(10) . . ? C2 B5 H5A 124.4 . . ? C2 B5 B3 105.10(10) . . ? B2 B5 B7 108.58(10) . . ? B2 B5 H5A 121.2 . . ? B7 B5 H5A 121.3 . . ? B6 B5 B2 59.87(9) . . ? B6 B5 B7 108.36(11) . . ? B6 B5 H5A 122.2 . . ? B6 B5 B3 60.40(9) . . ? B3 B5 B2 108.42(11) . . ? B3 B5 B7 59.96(9) . . ? B3 B5 H5A 122.1 . . ? B7 B3 B6 108.05(10) . . ? B7 B3 H3 121.7 . . ? B4 B3 B7 59.82(8) . . ? B4 B3 B9 60.02(8) . . ? B4 B3 B6 107.96(11) . . ? B4 B3 H3 121.7 . . ? B9 B3 B7 107.69(11) . . ? B9 B3 B6 59.71(9) . . ? B9 B3 H3 122.1 . . ? B6 B3 H3 121.8 . . ? B5 B3 B7 60.24(8) . . ? B5 B3 B4 107.86(10) . . ? B5 B3 B9 107.30(11) . . ? B5 B3 B6 59.72(9) . . ? B5 B3 H3 122.0 . . ? C8 N2 C10 118.2(12) . . ? C11 C10 H0 119.2 . . ? N2 C10 C11 121.5(13) . . ? N2 C10 H0 119.2 . . ? C11 C10' H0AA 117.8 . . ? C11 C10' C9' 124.4(14) . . ? C9' C10' H0AA 117.8 . . ? C8 C9' C10' 110.8(17) . . ? C8 C9' H1 124.6 . . ? C10' C9' H1 124.6 . . ? _shelx_res_file ; TITL spok71_0m_a.res in P2(1)/n spok71_0m_a.res created by SHELXL-2016/6 at 13:08:12 on 29-Sep-2017 REM Old TITL spok71_0m in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.122, Rweak 0.003, Alpha 0.024, Orientation as input REM Formula found by SHELXT: C13 B10 N CELL 1.54178 10.6774 7.4665 20.6215 90 104.123 90 ZERR 4 0.0004 0.0003 0.0008 0 0.001 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H B N UNIT 48 72 40 8 DFIX 1.4 N2 C10 RIGU 0.002 0.002 L.S. 10 PLAN 20 SIZE 0.23 0.26 0.28 TEMP -173 BOND $H LIST 6 fmap 2 ACTA REM REM REM WGHT 0.071000 0.565600 FVAR 0.64576 0.55510 N1 4 0.661590 0.918689 0.495414 11.00000 0.02271 0.02815 = 0.02506 -0.00375 0.00445 0.00379 PART 1 N2' 4 0.333170 0.553358 0.256042 21.00000 0.02303 0.02386 = 0.02602 0.00344 0.00806 -0.00373 PART 0 C3 1 0.760789 0.821866 0.485862 11.00000 0.02013 0.01938 = 0.01950 0.00315 0.00449 0.00051 PART 1 C9 1 0.304855 0.460606 0.362359 21.00000 0.01658 0.03294 = 0.02186 -0.00107 0.00899 -0.00170 AFIX 43 H9 2 0.341260 0.423984 0.407112 21.00000 -1.20000 AFIX 0 PART 0 C8 1 0.385335 0.513344 0.318721 11.00000 0.01730 0.01886 = 0.02350 -0.00304 0.00493 -0.00043 C1 1 0.725464 0.683621 0.430804 11.00000 0.01512 0.02070 = 0.02069 0.00176 0.00332 0.00196 C2 1 0.530456 0.525214 0.345011 11.00000 0.01717 0.02103 = 0.01991 -0.00073 0.00471 -0.00018 C6 1 0.807789 1.070939 0.585249 11.00000 0.03441 0.02505 = 0.02578 -0.00500 0.00316 -0.00147 AFIX 43 H6 2 0.821205 1.158915 0.619536 11.00000 -1.20000 AFIX 0 PART 1 C12 1 0.210831 0.543878 0.230102 21.00000 0.02256 0.03303 = 0.02830 -0.00012 0.00844 0.00302 AFIX 43 H12 2 0.177518 0.563171 0.183541 21.00000 -1.20000 AFIX 0 PART 0 C4 1 0.886210 0.842599 0.524136 11.00000 0.02079 0.02796 = 0.03382 -0.00516 0.00072 0.00228 AFIX 43 H4 2 0.954593 0.771728 0.515899 11.00000 -1.20000 AFIX 0 C11 1 0.124265 0.503577 0.272406 11.00000 0.01676 0.02530 = 0.03952 -0.00707 0.00358 -0.00036 PART 1 AFIX 43 H11 2 0.033462 0.504454 0.254352 21.00000 -1.20000 AFIX 43 PART 0 PART 2 H00C 2 0.032719 0.499061 0.258273 -21.00000 -1.20000 AFIX 0 PART 0 C7 1 0.686015 1.040803 0.544390 11.00000 0.02950 0.02855 = 0.02722 -0.00465 0.00629 0.00443 AFIX 43 H7 2 0.616114 1.110476 0.551494 11.00000 -1.20000 AFIX 0 PART 1 C12' 1 0.172433 0.465472 0.336437 21.00000 0.01436 0.03287 = 0.03622 -0.00469 0.00974 0.00416 AFIX 43 H12' 2 0.116012 0.441467 0.364581 21.00000 -1.20000 AFIX 0 PART 0 C5 1 0.909091 0.969652 0.574779 11.00000 0.02552 0.03339 = 0.03611 -0.00856 -0.00353 -0.00104 AFIX 43 H5 2 0.993837 0.986728 0.602016 11.00000 -1.20000 AFIX 0 B10 3 0.586237 0.568970 0.428290 11.00000 0.01821 0.02108 = 0.02051 0.00185 0.00348 -0.00118 AFIX 153 H10 2 0.523523 0.589688 0.463978 11.00000 -1.20000 AFIX 0 B8 3 0.753112 0.725160 0.352904 11.00000 0.02016 0.02805 = 0.02254 -0.00194 0.00759 -0.00289 AFIX 153 H8 2 0.801685 0.847957 0.339595 11.00000 -1.20000 AFIX 0 B2 3 0.623170 0.618727 0.295569 11.00000 0.02054 0.02858 = 0.02176 -0.00243 0.00797 -0.00357 AFIX 153 H2 2 0.584256 0.669873 0.243482 11.00000 -1.20000 AFIX 0 B1 3 0.595406 0.732541 0.366139 11.00000 0.01771 0.02114 = 0.01844 0.00093 0.00308 -0.00034 AFIX 153 H1A 2 0.538732 0.860199 0.360870 11.00000 -1.20000 AFIX 0 B7 3 0.606882 0.354316 0.396136 11.00000 0.02272 0.01970 = 0.02724 0.00088 0.00214 0.00103 AFIX 153 H7A 2 0.557202 0.232999 0.409810 11.00000 -1.20000 AFIX 0 B4 3 0.737527 0.460042 0.453333 11.00000 0.02198 0.01976 = 0.02855 0.00149 0.00099 0.00279 AFIX 153 H4A 2 0.776076 0.409760 0.505571 11.00000 -1.20000 AFIX 0 B9 3 0.840609 0.555963 0.406526 11.00000 0.01660 0.02624 = 0.03306 -0.00655 0.00403 0.00298 AFIX 153 H9A 2 0.947124 0.568488 0.428273 11.00000 -1.20000 AFIX 0 B6 3 0.774899 0.508883 0.320446 11.00000 0.01923 0.03391 = 0.03250 -0.01062 0.00948 -0.00227 AFIX 153 H6A 2 0.837752 0.488266 0.284820 11.00000 -1.20000 AFIX 0 B5 3 0.630257 0.385078 0.313927 11.00000 0.01967 0.02671 = 0.02954 -0.00675 0.00736 0.00087 AFIX 153 H5A 2 0.595667 0.283247 0.273659 11.00000 -1.20000 AFIX 0 B3 3 0.765246 0.345304 0.382419 11.00000 0.02083 0.02519 = 0.03765 -0.00753 0.00182 0.00375 AFIX 153 H3 2 0.821514 0.217312 0.387547 11.00000 -1.20000 AFIX 0 PART 2 N2 4 0.322223 0.473523 0.361475 -21.00000 0.01645 0.03656 = 0.02914 -0.00225 0.00612 -0.00080 C10 1 0.192857 0.455892 0.340239 -21.00000 0.02018 0.03564 = 0.03329 -0.00054 0.01246 0.00435 AFIX 43 H0 2 0.145463 0.411337 0.370247 -21.00000 -1.20000 AFIX 0 C10' 1 0.193588 0.552004 0.232660 -21.00000 0.01375 0.02520 = 0.03393 -0.00042 -0.00241 0.00426 AFIX 43 H0AA 2 0.150255 0.590369 0.189029 -21.00000 -1.20000 AFIX 0 C9' 1 0.335951 0.552108 0.250148 -21.00000 0.01713 0.03115 = 0.02307 -0.00313 0.00142 0.00153 AFIX 43 H1 2 0.387516 0.575115 0.219481 -21.00000 -1.20000 AFIX 0 HKLF 4 REM spok71_0m_a.res in P2(1)/n REM R1 = 0.0442 for 2696 Fo > 4sig(Fo) and 0.0472 for all 2906 data REM 254 parameters refined using 343 restraints END WGHT 0.0701 0.5655 REM Highest difference peak 0.248, deepest hole -0.324, 1-sigma level 0.047 Q1 1 0.5161 0.6376 0.4461 11.00000 0.05 0.25 Q2 1 0.8074 0.8440 0.3633 11.00000 0.05 0.23 Q3 1 0.4612 0.5267 0.3323 11.00000 0.05 0.22 Q4 1 0.5294 0.2932 0.4069 11.00000 0.05 0.22 Q5 1 0.5207 0.8176 0.3743 11.00000 0.05 0.22 Q6 1 0.7669 0.4750 0.5091 11.00000 0.05 0.21 Q7 1 0.6994 0.3737 0.4117 11.00000 0.05 0.20 Q8 1 0.7447 0.7576 0.4574 11.00000 0.05 0.20 Q9 1 0.5516 0.6946 0.2603 11.00000 0.05 0.19 Q10 1 0.7831 0.4409 0.4205 11.00000 0.05 0.18 Q11 1 0.6394 0.6621 0.4180 11.00000 0.05 0.17 Q12 1 0.6606 0.3411 0.3667 11.00000 0.05 0.17 Q13 1 0.9188 0.6197 0.4258 11.00000 0.05 0.16 Q14 1 0.5586 0.3433 0.2658 11.00000 0.05 0.16 Q15 1 0.7805 0.6013 0.4323 11.00000 0.05 0.16 Q16 1 0.6518 0.4419 0.4339 11.00000 0.05 0.16 Q17 1 0.6451 0.7070 0.3325 11.00000 0.05 0.15 Q18 1 0.6589 0.6213 0.4350 11.00000 0.05 0.15 Q19 1 0.7975 0.2196 0.4134 11.00000 0.05 0.15 Q20 1 0.7134 0.6310 0.3174 11.00000 0.05 0.14 ; _shelx_res_checksum 19077 _shelx_hkl_file ; 1 0 0 0.35623 0.10105 6 1 0 0 0.07892 0.10184 2 2 0 0 8785.41 407.932 2 2 0 0 7612.03 407.885 6 3 0 0 -0.0642 0.22634 6 3 0 0 0.22492 0.26457 2 4 0 0 726.164 37.4470 6 4 0 0 773.438 37.4756 2 5 0 0 -0.2813 0.23589 2 5 0 0 0.19325 0.35666 6 6 0 0 21.2748 1.41384 2 7 0 0 0.08799 0.45858 2 -8 0 0 103.820 5.60257 5 8 0 0 108.160 5.70215 7 -8 0 0 107.822 5.64045 4 -9 0 0 0.10216 0.43035 4 9 0 0 0.03398 0.48086 7 -9 0 0 0.81948 0.64625 5 -10 0 0 27.5915 1.87567 4 10 0 0 25.6656 1.68695 5 10 0 0 26.9199 1.80322 7 11 0 0 0.28495 0.41183 5 -11 0 0 0.08618 0.43484 4 11 0 0 -0.4668 0.44070 7 12 0 0 14.8594 1.10357 7 0 -1 0 -0.0542 0.21868 6 0 -1 0 -0.0218 0.12666 2 -1 -1 0 1673.58 88.9678 2 -1 -1 0 1890.83 88.9668 6 1 -1 0 1798.53 88.9585 2 -2 -1 0 6.57206 0.59309 2 2 -1 0 6.78967 0.44871 2 2 -1 0 7.20395 0.62269 6 2 1 0 6.65569 0.46927 6 3 -1 0 133.202 6.38197 2 3 -1 0 115.754 6.49225 6 3 1 0 128.675 6.36693 6 4 -1 0 66.2862 3.48304 2 4 -1 0 71.0061 3.63857 6 4 1 0 62.2367 3.42954 6 4 1 0 68.0841 3.60187 2 5 -1 0 678.845 35.5486 2 5 -1 0 743.898 35.7096 6 5 1 0 710.284 35.6626 2 6 -1 0 159.587 7.93656 6 6 -1 0 133.466 7.67490 2 6 1 0 155.958 7.86903 2 7 1 0 5.39760 0.87099 2 8 -1 0 12.3162 0.99980 5 8 -1 0 13.5784 1.30436 7 -8 -1 0 14.8066 1.27915 4 -8 -1 0 11.6000 1.25401 5 -8 -1 0 12.4664 1.29507 1 8 1 0 14.2755 1.15216 7 8 1 0 13.6908 1.31232 2 -9 -1 0 131.075 7.15605 4 -9 -1 0 135.432 7.08026 5 9 -1 0 141.103 7.15387 7 9 -1 0 127.008 7.00396 5 9 1 0 144.812 7.16913 7 -10 -1 0 2.41119 0.83716 5 -10 -1 0 3.13725 0.80730 4 10 -1 0 1.39770 0.73604 7 10 -1 0 3.27015 0.50775 5 10 1 0 1.70076 0.75118 7 11 -1 0 8.63630 0.96462 7 -11 -1 0 9.17548 0.95337 4 11 1 0 8.04723 0.88337 5 11 1 0 10.4674 1.18437 7 12 -1 0 1.38786 0.44689 7 -12 -1 0 1.56802 0.51850 4 12 1 0 1.42589 0.35712 5 12 1 0 1.16793 0.44632 7 0 -2 0 9638.76 488.784 6 0 -2 0 9999.99 488.577 2 -1 -2 0 239.193 12.2952 6 -1 -2 0 262.277 12.2624 2 1 -2 0 242.339 12.3418 6 1 -2 0 228.935 12.1616 2 2 -2 0 373.420 19.0782 6 -2 -2 0 404.717 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16.2829 1.19789 1 8 -2 -20 16.8979 1.09386 5 8 2 -20 16.8425 1.24456 1 7 -2 -20 10.4858 1.03674 1 7 -2 -20 9.59644 1.03373 5 7 2 -20 9.99122 1.02165 1 6 -2 -20 35.4267 2.26849 1 6 -2 -20 32.3536 1.94428 5 6 2 -20 34.7667 2.07105 1 5 -2 -20 1.18242 0.62144 5 5 -2 -20 0.96419 0.79370 1 5 2 -20 2.87498 0.76076 1 4 -2 -20 48.3896 2.85611 5 4 -2 -20 52.1411 2.96611 1 4 2 -20 50.7365 2.89495 1 -4 2 20 53.5546 2.98400 3 3 -2 -20 4.45448 0.74939 1 -3 2 20 4.95994 0.83811 3 2 -2 -20 156.479 7.70027 1 -2 2 20 148.229 7.80245 3 2 2 -20 136.467 7.57600 4 1 -2 -20 6.85013 0.83753 1 -1 -2 20 3.87499 0.90500 3 -1 2 20 5.38264 1.03579 3 1 2 -20 7.11848 0.84394 4 0 -2 -20 2.33045 0.85564 1 0 -2 20 2.23167 0.65833 3 0 2 -20 2.14612 0.54638 4 0 2 20 3.38052 0.73100 3 1 -2 20 5.09110 0.77711 3 -1 -2 -20 4.39120 0.86510 1 1 2 20 5.93181 0.82915 3 -1 2 -20 4.56486 0.78988 4 -2 -2 -20 65.9309 3.63571 1 2 -2 20 67.0678 3.74223 3 2 2 20 68.2945 3.75622 3 -2 2 -20 68.2232 3.70589 4 3 -2 20 7.67346 0.92874 3 -3 2 -20 8.55757 0.83944 4 3 2 20 8.69501 0.93223 3 4 -2 20 0.78381 0.47283 3 4 2 20 0.11205 0.39484 3 -4 2 -20 0.22182 0.39041 4 8 -3 -20 24.8347 1.37642 5 8 -3 -20 22.3264 1.46876 1 8 3 -20 22.6212 1.39551 1 7 -3 -20 0.15223 0.49028 1 7 -3 -20 -0.1969 0.39852 5 7 3 -20 0.47886 0.39418 1 6 -3 -20 65.6788 3.54727 1 6 -3 -20 66.4369 3.45933 5 6 3 -20 62.5219 3.47492 1 5 -3 -20 44.3712 2.64742 1 5 -3 -20 42.5789 2.41116 5 -4 -3 20 1.62401 0.45729 4 4 -3 -20 1.71124 0.60293 1 4 -3 -20 1.28014 0.47480 5 3 -3 -20 28.0067 1.73913 5 3 -3 -20 29.6516 2.08281 1 -3 -3 20 30.1493 1.90660 4 -3 3 20 28.6110 1.96987 3 2 -3 -20 8.85534 0.86095 5 2 -3 -20 8.23163 1.04101 1 -2 3 20 8.33074 1.18019 3 1 -3 -20 5.44614 0.73019 5 1 -3 -20 6.03174 0.80174 1 1 3 -20 4.53031 0.85498 4 -1 3 20 4.77195 0.81745 3 0 -3 20 5.40828 0.88431 3 0 -3 -20 8.49660 0.88670 1 0 3 -20 6.25141 0.73772 4 0 3 20 5.64270 1.00289 3 -1 -3 -20 1.36430 0.80450 1 1 -3 20 1.72177 0.61280 3 -1 3 -20 1.64732 0.54522 4 1 3 20 1.19041 0.61690 3 -2 -3 -20 14.6504 1.14648 1 2 -3 20 15.1251 1.38298 3 2 3 20 16.7123 1.25284 3 -2 3 -20 15.5096 1.31812 4 -3 -3 -20 13.4925 0.91424 1 3 -3 20 10.0836 1.00923 3 -3 3 -20 14.6019 1.00542 4 3 3 20 13.1809 0.98337 3 7 -4 -20 23.6900 1.38205 5 6 -4 -20 9.06139 0.77907 5 6 -4 -20 9.26577 0.82502 1 -6 -4 20 8.60775 0.72501 4 5 -4 -20 10.9976 0.98194 1 5 -4 -20 11.0883 0.92224 5 -5 -4 20 11.4992 0.89753 4 -4 -4 20 239.184 12.0892 4 4 -4 -20 236.886 12.0447 5 4 -4 -20 239.585 12.1126 1 3 -4 -20 2.16369 0.50633 5 3 -4 -20 1.95042 0.59642 1 -3 -4 20 1.08961 0.47091 4 2 -4 -20 19.9163 1.31204 5 2 -4 -20 21.0231 1.45245 1 -2 4 20 20.0809 1.51951 3 1 -4 -20 1.27712 0.57713 1 1 -4 -20 0.56751 0.44129 5 -1 4 20 1.74944 0.63395 3 1 4 -20 2.22042 0.74141 4 0 -4 -20 7.69167 0.69343 5 0 -4 -20 6.23658 0.73248 1 0 4 -20 5.53431 0.69591 4 0 4 20 7.22711 0.92693 3 -1 -4 -20 20.1725 1.32600 1 1 -4 20 17.1212 1.22695 3 -1 4 -20 17.5399 1.28437 4 1 4 20 21.7334 1.37131 3 2 -4 20 -0.1330 0.36050 3 -2 -4 -20 0.36222 0.41648 1 2 4 20 0.05541 0.46771 3 -2 4 -20 0.27739 0.39110 4 -5 -5 20 46.3905 2.47563 4 5 -5 -20 46.5686 2.48036 5 4 -5 -20 42.5439 2.29514 5 3 -5 -20 3.12642 0.52109 1 3 -5 -20 2.58515 0.44223 5 2 -5 -20 0.71397 0.39762 5 2 -5 -20 0.58976 0.48065 1 2 5 -20 1.57064 0.45366 4 -2 5 20 1.56255 0.55854 3 1 -5 -20 0.60177 0.48116 1 1 -5 -20 0.57662 0.36459 5 -1 5 20 0.98997 0.49888 3 1 5 -20 0.51164 0.41440 4 0 -5 -20 19.6809 1.18167 5 0 -5 -20 21.0127 1.28815 1 0 5 20 19.9958 1.32764 3 0 5 -20 21.1074 1.26626 4 9 0 -21 22.1604 1.39500 1 8 0 -21 -0.2604 0.47003 1 7 0 -21 21.7542 1.51124 1 6 0 -21 0.44617 0.73770 1 5 0 -21 1.34587 0.59734 1 4 0 -21 0.39130 0.78467 1 3 0 -21 138.775 7.24735 1 2 0 -21 0.51641 0.53483 1 -2 0 21 0.04683 0.75455 3 1 0 -21 24.5619 1.62799 1 -1 0 21 24.9674 1.74413 3 0 0 21 0.67338 0.57764 3 1 0 21 321.357 16.3321 3 2 0 21 0.34672 0.51171 3 3 0 21 70.3296 3.79888 3 9 -1 -21 3.07094 0.49725 1 9 1 -21 3.82886 0.54444 1 8 -1 -21 110.842 5.87342 1 8 1 -21 115.677 5.90468 1 7 -1 -21 33.3911 2.15540 1 7 1 -21 33.4574 2.04975 1 6 -1 -21 38.3267 2.32756 1 6 1 -21 39.4541 2.32717 1 5 -1 -21 35.7086 2.27687 1 5 1 -21 39.1270 2.40718 1 4 -1 -21 28.1867 1.85677 1 4 1 -21 28.5091 1.96864 1 3 -1 -21 53.5356 2.98894 1 -3 1 21 50.3988 3.05527 3 3 1 -21 51.7970 3.01882 1 2 -1 -21 12.0570 1.43364 1 -2 -1 21 11.5707 1.05538 3 -2 1 21 12.1485 1.41704 3 -1 -1 21 3.93949 0.68346 3 1 -1 -21 5.70771 0.74926 1 -1 1 21 4.47303 0.96103 3 0 -1 21 1.61581 0.82861 3 0 -1 -21 2.64096 0.59796 1 0 1 21 1.93775 0.63528 3 1 -1 21 3.31116 0.67852 3 1 1 21 2.98414 0.67012 3 -1 1 -21 4.82001 0.61112 4 2 -1 21 19.8883 1.57304 3 -2 1 -21 17.2321 1.20946 4 2 1 21 20.0793 1.41882 3 3 -1 21 0.65800 0.50183 3 3 1 21 0.30140 0.50230 3 -3 1 -21 0.46552 0.37339 4 8 -2 -21 8.90856 0.84191 1 8 -2 -21 9.05815 0.72695 5 8 2 -21 11.0707 0.87454 1 7 -2 -21 23.9839 1.55511 1 7 -2 -21 23.3349 1.48114 5 7 2 -21 23.8811 1.52880 1 6 -2 -21 58.3679 3.16299 1 6 -2 -21 52.0691 2.90316 5 6 2 -21 53.9554 3.01271 1 5 -2 -21 159.824 7.70618 5 5 -2 -21 142.718 7.74523 1 5 2 -21 146.438 7.73066 1 4 -2 -21 0.11719 0.76167 1 -4 2 21 -0.1043 0.66727 3 3 -2 -21 333.187 16.8575 1 -3 2 21 330.967 16.8855 3 2 -2 -21 107.266 5.43519 1 -2 2 21 96.6737 5.45368 3 1 -2 -21 -0.8807 0.52553 1 -1 -2 21 0.16587 0.51713 3 -1 2 21 0.48231 0.58738 3 1 2 -21 0.46204 0.42378 4 0 -2 -21 -0.2718 0.76442 1 0 -2 21 0.14832 0.75973 3 0 2 21 0.91296 0.81282 3 0 2 -21 0.44061 0.57758 4 -1 -2 -21 9.63891 1.14399 1 1 -2 21 8.98158 1.22646 3 -1 2 -21 9.79885 0.88952 4 1 2 21 8.60859 1.07608 3 -2 -2 -21 91.2855 5.21623 1 2 -2 21 108.290 5.32076 3 -2 2 -21 95.9865 5.21441 4 2 2 21 106.935 5.33845 3 3 -2 21 9.13044 0.96114 3 3 2 21 12.8069 0.95713 3 -3 2 -21 13.2462 0.87970 4 7 -3 -21 46.8580 2.68604 1 7 -3 -21 53.0150 2.62747 5 7 3 -21 48.1837 2.67970 1 6 -3 -21 31.8272 1.87094 1 6 -3 -21 30.1569 1.74508 5 5 -3 -21 2.90756 0.78635 1 5 -3 -21 1.63682 0.59183 5 4 -3 -21 2.97307 0.81533 1 4 -3 -21 3.04442 0.48579 5 -4 3 21 3.93344 0.85240 3 3 -3 -21 150.531 7.83854 5 3 -3 -21 152.241 7.94895 1 -3 3 21 160.122 8.00627 3 3 3 -21 151.510 7.90063 4 2 -3 -21 10.6024 1.06268 1 -2 3 21 9.81849 1.08785 3 2 3 -21 10.5365 0.95727 4 1 -3 -21 7.52724 0.83676 1 -1 3 21 7.28477 0.99504 3 1 3 -21 7.54491 0.82956 4 0 -3 -21 3.25091 0.62922 1 0 -3 21 1.87115 0.67793 3 0 3 -21 2.91682 0.55624 4 0 3 21 2.52265 0.65516 3 -1 -3 -21 91.8508 4.87419 1 1 -3 21 93.7314 4.89641 3 -1 3 -21 93.3980 4.86439 4 1 3 21 93.6282 4.96461 3 2 -3 21 4.90039 0.60496 3 2 3 21 3.58801 0.55351 3 6 -4 -21 12.9089 0.90543 1 6 -4 -21 12.1247 0.87296 5 5 -4 -21 2.20460 0.48564 1 5 -4 -21 1.16218 0.36680 5 4 -4 -21 0.28543 0.40526 5 4 -4 -21 1.06415 0.70357 1 -4 4 21 0.93391 0.49514 3 3 -4 -21 3.81945 0.47729 5 3 -4 -21 4.33108 0.61663 1 3 4 -21 3.38061 0.54526 4 -3 4 21 2.48987 0.59613 3 2 -4 -21 20.3145 1.47667 1 2 -4 -21 18.2829 1.15891 5 -2 4 21 17.3977 1.36533 3 2 4 -21 19.4528 1.27149 4 1 -4 -21 6.99892 0.67850 1 1 -4 -21 2.43309 0.43856 5 1 4 -21 4.58628 0.57560 4 -1 4 21 4.15113 0.64836 3 0 -4 -21 24.3258 1.49660 1 0 4 21 23.2188 1.52761 3 0 4 -21 23.7688 1.45419 4 -1 -4 -21 0.27445 0.43132 1 -1 4 -21 1.30211 0.39520 4 1 4 21 0.50692 0.42498 3 8 0 -22 29.2841 1.76366 1 7 0 -22 0.14492 0.50004 1 6 0 -22 72.2667 3.91000 1 5 0 -22 -0.0667 0.51670 1 4 0 -22 49.1426 2.80966 1 3 0 -22 0.32933 0.69779 1 -2 0 22 27.5909 1.76255 3 2 0 -22 27.6665 1.73037 1 -1 0 22 0.36416 0.55395 3 0 0 22 24.1462 1.64098 3 1 0 22 -0.4650 0.49529 3 2 0 22 71.3989 3.85344 3 3 0 22 -0.4302 0.41393 3 8 -1 -22 16.2637 1.16713 1 8 1 -22 17.7815 1.16577 1 7 -1 -22 1.32420 0.51315 1 7 1 -22 1.64129 0.49693 1 6 -1 -22 8.98933 0.97734 1 6 1 -22 8.86453 0.90086 1 5 -1 -22 0.06281 0.51358 1 5 1 -22 0.36979 0.49759 1 4 -1 -22 44.7381 2.57139 1 4 1 -22 43.8904 2.62271 1 3 -1 -22 3.22614 0.65933 1 -3 1 22 3.07886 0.60626 3 3 1 -22 2.07362 0.65643 1 2 -1 -22 16.2181 1.23676 1 -2 1 22 13.3918 1.20550 3 1 -1 -22 18.0360 1.27163 1 -1 -1 22 16.6749 1.24870 3 -1 1 22 15.5937 1.30620 3 0 -1 22 5.22058 0.88880 3 0 -1 -22 4.77561 0.76233 1 0 1 22 6.26907 0.81487 3 1 -1 22 115.956 6.02155 3 1 1 22 113.827 6.02946 3 2 -1 22 31.5997 1.96510 3 2 1 22 35.0776 2.08993 3 7 -2 -22 1.80768 0.52827 1 7 2 -22 3.47504 0.48782 1 6 -2 -22 0.78163 0.72406 1 6 2 -22 0.10778 0.37818 1 5 -2 -22 3.25672 0.62792 1 5 2 -22 1.40456 0.43112 1 4 -2 -22 0.56151 0.53190 1 3 -2 -22 0.68948 0.78687 1 -3 2 22 0.48961 0.54567 3 2 -2 -22 146.687 7.69580 1 -2 2 22 150.838 7.74943 3 1 -2 -22 18.8016 1.32232 1 -1 -2 22 15.1942 1.33515 3 -1 2 22 18.2319 1.36682 3 0 -2 -22 84.1892 4.43964 1 0 -2 22 85.1219 4.51102 3 0 2 -22 78.9023 4.40980 4 0 2 22 89.1338 4.53960 3 1 -2 22 2.68618 0.70445 3 -1 -2 -22 2.01326 0.49038 1 1 2 22 3.59188 0.62200 3 -1 2 -22 1.56699 0.39800 4 2 -2 22 143.956 8.10787 3 2 2 22 173.894 8.14663 3 6 -3 -22 76.6922 4.33549 5 6 -3 -22 93.3962 4.44467 1 5 -3 -22 14.4771 1.21114 1 5 -3 -22 19.1785 1.05623 5 4 -3 -22 106.777 6.06353 5 4 -3 -22 132.152 6.17591 1 -4 3 22 115.152 6.11648 3 3 -3 -22 2.18737 0.58067 1 -3 3 22 2.51783 0.57116 3 2 -3 -22 0.22140 0.54017 1 2 3 -22 -0.8400 0.37022 4 -2 3 22 -0.3647 0.71957 3 1 -3 -22 3.68035 0.61379 1 -1 3 22 4.01289 0.66953 3 1 3 -22 2.72912 0.61436 4 0 -3 -22 2.78626 0.55384 1 0 -3 22 2.61403 0.43363 3 0 3 -22 3.47983 0.48773 4 0 3 22 1.59480 0.51780 3 -1 -3 -22 0.81577 0.40475 1 1 -3 22 0.46358 0.31817 3 -1 3 -22 0.38135 0.33860 4 1 3 22 0.88966 0.47127 3 4 -4 -22 11.7156 0.73488 5 4 -4 -22 11.1954 0.85214 1 -4 4 22 9.83554 0.81024 3 3 -4 -22 5.19890 0.58084 1 3 -4 -22 2.92008 0.39549 5 -3 4 22 4.84854 0.61676 3 3 4 -22 4.67130 0.51692 4 2 -4 -22 1.67550 0.46273 1 2 4 -22 1.22524 0.39237 4 -2 4 22 1.07541 0.48877 3 7 0 -23 -0.0678 0.43039 1 6 0 -23 0.43020 0.67580 1 5 0 -23 2.91141 0.54784 1 4 0 -23 -0.4400 0.44291 1 3 0 -23 0.52945 0.50423 1 -2 0 23 0.48597 0.61736 3 2 0 -23 0.27257 0.42217 1 -1 0 23 21.8943 1.44249 3 0 0 23 0.11443 0.46891 3 1 0 23 6.96081 0.80607 3 7 -1 -23 11.3989 0.93396 1 7 1 -23 11.4687 0.88797 1 5 -1 -23 29.3600 1.85202 1 5 1 -23 32.1840 1.82591 1 4 -1 -23 0.95655 0.55926 1 4 1 -23 0.59763 0.57278 1 3 -1 -23 136.952 7.11042 1 2 -1 -23 0.05740 0.67852 1 -2 1 23 0.87909 0.45681 3 -1 -1 23 57.4336 3.42738 3 1 -1 -23 68.6884 3.42344 1 -1 1 23 65.1911 3.47708 3 0 -1 23 20.5174 1.36327 3 0 1 23 21.4513 1.53576 3 1 -1 23 -0.2323 0.44689 3 1 1 23 -0.2385 0.41052 3 6 -2 -23 0.99915 0.45735 1 6 2 -23 0.55499 0.32543 1 5 -2 -23 13.5307 1.04955 1 4 -2 -23 44.6177 2.51255 1 3 -2 -23 2.30899 0.56412 1 -3 2 23 2.11024 0.48555 3 2 -2 -23 11.7315 1.25275 1 -2 2 23 12.9640 1.02842 3 1 -2 -23 2.96579 0.50868 1 -1 2 23 2.65417 0.56522 3 0 -2 23 55.8253 2.93559 3 0 -2 -23 53.0621 2.89255 1 5 -3 -23 2.05430 0.43219 1 4 -3 -23 0.54039 0.44370 1 3 -3 -23 8.16929 0.84259 1 -3 3 23 7.72712 0.76359 3 2 -3 -23 3.89305 0.54395 1 -1 3 23 58.8187 3.15814 3 5 0 -24 0.25332 0.41287 1 4 0 -24 4.64439 0.57231 1 3 0 -24 -0.0502 0.35224 1 -1 0 24 -0.2210 0.34850 3 0 0 24 5.07032 0.61876 3 5 -1 -24 12.5974 1.04711 1 5 1 -24 15.1954 0.94499 1 4 -1 -24 0.51954 0.46203 1 3 -1 -24 40.2391 2.25880 1 2 -1 -24 12.4543 0.95642 1 -2 1 24 15.3366 0.97573 3 -1 -1 24 0.93632 0.61439 3 -1 1 24 0.63816 0.40858 3 4 -2 -24 41.2849 2.26566 1 3 -2 -24 82.6835 4.30607 1 2 -2 -24 1.60300 0.46724 1 -2 2 24 2.82717 0.45816 3 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 0.5210 _exptl_absorpt_correction_T_min 0.4338 _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 1.54182 10.678 7.471 20.626 89.990 104.122 89.983 ) ; _shelx_hkl_checksum 82351 _olex2_submission_special_instructions 'No special instructions were received'