data_spok41_a _audit_creation_date 2016-09-01 _audit_creation_method ; Olex2 1.2-beta (compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221) ; _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C20 H28 B20 F4 N2' _chemical_formula_sum 'C20 H28 B20 F4 N2' _chemical_formula_weight 588.64 _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' 'F' 'F' 0.0171 0.0103 '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 '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 7.2661(12) _cell_length_b 15.0779(18) _cell_length_c 13.2917(16) _cell_angle_alpha 90 _cell_angle_beta 90.604(5) _cell_angle_gamma 90 _cell_volume 1456.1(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4128 _cell_measurement_temperature 100 _cell_measurement_theta_max 28.26 _cell_measurement_theta_min 3.067 _shelx_estimated_absorpt_T_max 0.979 _shelx_estimated_absorpt_T_min 0.973 _exptl_absorpt_coefficient_mu 0.086 _exptl_absorpt_correction_T_max 0.3343 _exptl_absorpt_correction_T_min 0.2814 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0458 before and 0.0413 after correction. The Ratio of minimum to maximum transmission is 0.8418. The \l/2 correction factor is 0.00150. ; _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 596 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.25 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_unetI/netI 0.0348 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 13668 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.296 _diffrn_reflns_theta_min 2.702 _diffrn_ambient_temperature 100 _diffrn_detector 'Bruker APEX CCD' _diffrn_detector_area_resol_mean 8.0 _diffrn_detector_type 'CCD Area Detector' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device 'Kappa Four-Circle Diffractometer' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe X-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed tube' _diffrn_source_type fine-focus _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2981 _reflns_number_total 3596 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_collection 'APEX2 v2013.6-2 (Bruker, 2013)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.368 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.059 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 208 _refine_ls_number_reflns 3596 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_gt 0.0489 _refine_ls_restrained_S_all 1.076 _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^)+(0.0595P)^2^+0.8870P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1211 _refine_ls_wR_factor_ref 0.1274 _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: C6(H6), C7(H7), C4(H4), C5(H5) 2.b Boron cage BH refined with riding coordinates: B9(H9), B4(H4A), B6(H6A), B10(H10), B5(H5A), B8(H8), B1(H1), B3(H3), B2(H2), B7(H7A) ; _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 F2 F 0.32651(12) 0.34415(6) 0.52787(7) 0.0159(2) Uani 1 1 d . . . . . F1 F 0.18170(12) 0.45497(6) 0.40762(7) 0.0162(2) Uani 1 1 d . . . . . N1 N 0.4107(2) 0.48113(9) 0.75317(10) 0.0182(3) Uani 1 1 d . . . . . C9 C 0.4179(2) 0.42082(10) 0.51766(11) 0.0110(3) Uani 1 1 d . . . . . C8 C 0.5795(2) 0.43747(10) 0.57159(11) 0.0109(3) Uani 1 1 d . . . . . C10 C 0.3402(2) 0.48067(10) 0.45080(11) 0.0118(3) Uani 1 1 d . . . . . C1 C 0.6704(2) 0.37060(10) 0.64027(11) 0.0107(3) Uani 1 1 d . . . . . C2 C 0.6212(2) 0.35751(10) 0.76559(11) 0.0122(3) Uani 1 1 d . . . . . C6 C 0.2146(2) 0.52447(11) 0.88853(13) 0.0193(3) Uani 1 1 d . . . . . H6 H 0.1222 0.5631 0.9132 0.023 Uiso 1 1 calc R . . . . C7 C 0.2804(2) 0.53371(11) 0.79151(13) 0.0212(4) Uani 1 1 d . . . . . H7 H 0.2308 0.5795 0.7503 0.025 Uiso 1 1 calc R . . . . C3 C 0.4768(2) 0.41671(10) 0.81155(11) 0.0132(3) Uani 1 1 d . . . . . C4 C 0.4205(2) 0.40225(12) 0.90967(12) 0.0188(3) Uani 1 1 d . . . . . H4 H 0.4721 0.3558 0.9491 0.023 Uiso 1 1 calc R . . . . C5 C 0.2863(2) 0.45797(12) 0.94829(12) 0.0215(4) Uani 1 1 d . . . . . H5 H 0.2444 0.4503 1.0152 0.026 Uiso 1 1 calc R . . . . B9 B 0.9938(2) 0.32339(12) 0.74200(13) 0.0150(3) Uani 1 1 d . . . . . H9 H 1.1402 0.3392 0.7621 0.018 Uiso 1 1 calc R . . . . B4 B 0.5494(2) 0.27679(11) 0.68214(13) 0.0137(3) Uani 1 1 d . . . . . H4A H 0.4014 0.2632 0.6633 0.016 Uiso 1 1 calc R . . . . B6 B 0.7176(3) 0.19229(12) 0.69128(13) 0.0158(3) Uani 1 1 d . . . . . H6A H 0.6816 0.1210 0.6777 0.019 Uiso 1 1 calc R . . . . B10 B 0.8837(3) 0.22432(12) 0.78434(14) 0.0167(4) Uani 1 1 d . . . . . H10 H 0.9579 0.1743 0.8320 0.020 Uiso 1 1 calc R . . . . B5 B 0.9338(3) 0.23774(12) 0.65455(14) 0.0168(4) Uani 1 1 d . . . . . H5A H 1.0411 0.1965 0.6168 0.020 Uiso 1 1 calc R . . . . B8 B 0.8158(2) 0.32937(12) 0.83222(13) 0.0146(3) Uani 1 1 d . . . . . H8 H 0.8434 0.3492 0.9122 0.017 Uiso 1 1 calc R . . . . B1 B 0.8247(2) 0.40775(12) 0.73267(13) 0.0129(3) Uani 1 1 d . . . . . H1 H 0.8555 0.4795 0.7468 0.015 Uiso 1 1 calc R . . . . B3 B 0.7275(2) 0.27000(11) 0.59077(13) 0.0139(3) Uani 1 1 d . . . . . H3 H 0.6969 0.2506 0.5110 0.017 Uiso 1 1 calc R . . . . B2 B 0.8990(2) 0.35057(12) 0.62202(13) 0.0137(3) Uani 1 1 d . . . . . H2 H 0.9823 0.3844 0.5629 0.016 Uiso 1 1 calc R . . . . B7 B 0.6462(3) 0.24903(12) 0.80129(13) 0.0158(4) Uani 1 1 d . . . . . H7A H 0.5624 0.2161 0.8608 0.019 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 F2 0.0173(5) 0.0127(4) 0.0177(5) 0.0041(3) -0.0046(4) -0.0061(3) F1 0.0135(4) 0.0163(5) 0.0187(5) 0.0044(4) -0.0073(3) -0.0058(4) N1 0.0221(7) 0.0150(7) 0.0175(7) 0.0027(5) 0.0050(5) 0.0050(5) C9 0.0133(7) 0.0090(6) 0.0109(7) -0.0004(5) 0.0023(5) -0.0016(5) C8 0.0126(7) 0.0108(7) 0.0092(7) 0.0005(5) 0.0011(5) 0.0020(5) C10 0.0087(6) 0.0140(7) 0.0125(7) -0.0005(5) -0.0017(5) -0.0008(5) C1 0.0117(7) 0.0108(7) 0.0095(7) 0.0002(5) 0.0000(5) 0.0004(5) C2 0.0146(7) 0.0116(7) 0.0105(7) 0.0010(5) -0.0010(5) 0.0002(5) C6 0.0155(7) 0.0206(8) 0.0219(8) -0.0071(6) 0.0041(6) 0.0013(6) C7 0.0246(8) 0.0171(8) 0.0222(8) 0.0007(6) 0.0040(7) 0.0047(7) C3 0.0116(6) 0.0154(7) 0.0127(7) -0.0017(6) -0.0005(5) -0.0019(6) C4 0.0181(7) 0.0242(8) 0.0141(7) 0.0018(6) 0.0005(6) 0.0006(6) C5 0.0218(8) 0.0304(9) 0.0126(7) -0.0021(7) 0.0037(6) -0.0001(7) B9 0.0142(8) 0.0170(9) 0.0138(8) -0.0004(6) -0.0022(6) 0.0038(6) B4 0.0169(8) 0.0107(8) 0.0134(8) 0.0021(6) -0.0007(6) -0.0014(6) B6 0.0203(8) 0.0117(8) 0.0153(8) 0.0003(6) -0.0031(7) 0.0022(7) B10 0.0190(8) 0.0152(8) 0.0158(8) 0.0014(7) -0.0027(7) 0.0027(7) B5 0.0186(9) 0.0157(9) 0.0161(8) -0.0006(7) -0.0033(7) 0.0042(7) B8 0.0165(8) 0.0145(8) 0.0127(8) 0.0009(6) -0.0035(6) 0.0020(6) B1 0.0110(7) 0.0147(8) 0.0129(8) -0.0010(6) -0.0011(6) 0.0001(6) B3 0.0165(8) 0.0118(8) 0.0134(8) -0.0016(6) -0.0013(6) 0.0032(6) B2 0.0118(8) 0.0164(8) 0.0128(8) -0.0001(6) -0.0010(6) 0.0025(6) B7 0.0205(9) 0.0133(8) 0.0135(8) 0.0030(6) -0.0018(7) 0.0012(7) _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 F2 C9 1.3407(16) . ? F1 C10 1.3388(17) . ? N1 C7 1.340(2) . ? N1 C3 1.330(2) . ? C9 C8 1.392(2) . ? C9 C10 1.383(2) . ? C8 C10 1.399(2) 3_666 ? C8 C1 1.508(2) . ? C10 C8 1.399(2) 3_666 ? C1 C2 1.719(2) . ? C1 B4 1.759(2) . ? C1 B1 1.747(2) . ? C1 B3 1.706(2) . ? C1 B2 1.708(2) . ? C2 C3 1.512(2) . ? C2 B4 1.724(2) . ? C2 B8 1.713(2) . ? C2 B1 1.722(2) . ? C2 B7 1.712(2) . ? C6 H6 0.9500 . ? C6 C7 1.387(2) . ? C6 C5 1.378(2) . ? C7 H7 0.9500 . ? C3 C4 1.388(2) . ? C4 H4 0.9500 . ? C4 C5 1.390(2) . ? C5 H5 0.9500 . ? B9 H9 1.1200 . ? B9 B10 1.788(3) . ? B9 B5 1.788(3) . ? B9 B8 1.775(2) . ? B9 B1 1.772(2) . ? B9 B2 1.778(2) . ? B4 H4A 1.1200 . ? B4 B6 1.769(2) . ? B4 B3 1.787(2) . ? B4 B7 1.776(2) . ? B6 H6A 1.1200 . ? B6 B10 1.786(3) . ? B6 B5 1.786(3) . ? B6 B3 1.779(3) . ? B6 B7 1.776(3) . ? B10 H10 1.1200 . ? B10 B5 1.778(3) . ? B10 B8 1.779(3) . ? B10 B7 1.782(3) . ? B5 H5A 1.1200 . ? B5 B3 1.782(3) . ? B5 B2 1.773(3) . ? B8 H8 1.1200 . ? B8 B1 1.776(2) . ? B8 B7 1.773(3) . ? B1 H1 1.1200 . ? B1 B2 1.793(2) . ? B3 H3 1.1200 . ? B3 B2 1.786(3) . ? B2 H2 1.1200 . ? B7 H7A 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 C7 117.56(14) . . ? F2 C9 C8 121.28(13) . . ? F2 C9 C10 115.38(13) . . ? C10 C9 C8 123.34(14) . . ? C9 C8 C10 113.64(13) . 3_666 ? C9 C8 C1 123.56(13) . . ? C10 C8 C1 122.55(13) 3_666 . ? F1 C10 C9 115.47(13) . . ? F1 C10 C8 121.55(13) . 3_666 ? C9 C10 C8 122.98(14) . 3_666 ? C8 C1 C2 124.71(11) . . ? C8 C1 B4 120.81(12) . . ? C8 C1 B1 119.02(12) . . ? C8 C1 B3 117.89(12) . . ? C8 C1 B2 116.91(12) . . ? C2 C1 B4 59.42(9) . . ? C2 C1 B1 59.58(9) . . ? B1 C1 B4 110.78(11) . . ? B3 C1 C2 109.00(11) . . ? B3 C1 B4 62.08(10) . . ? B3 C1 B1 113.52(12) . . ? B3 C1 B2 63.07(10) . . ? B2 C1 C2 109.25(11) . . ? B2 C1 B4 113.13(12) . . ? B2 C1 B1 62.52(10) . . ? C1 C2 B4 61.45(9) . . ? C1 C2 B1 61.01(9) . . ? C3 C2 C1 118.43(12) . . ? C3 C2 B4 118.04(12) . . ? C3 C2 B8 120.65(12) . . ? C3 C2 B1 116.39(12) . . ? C3 C2 B7 121.62(12) . . ? B8 C2 C1 110.53(11) . . ? B8 C2 B4 113.60(12) . . ? B8 C2 B1 62.25(10) . . ? B1 C2 B4 113.71(11) . . ? B7 C2 C1 110.84(11) . . ? B7 C2 B4 62.25(10) . . ? B7 C2 B8 62.33(10) . . ? B7 C2 B1 113.69(12) . . ? C7 C6 H6 120.8 . . ? C5 C6 H6 120.8 . . ? C5 C6 C7 118.50(15) . . ? N1 C7 C6 123.10(16) . . ? N1 C7 H7 118.4 . . ? C6 C7 H7 118.4 . . ? N1 C3 C2 116.33(13) . . ? N1 C3 C4 123.70(15) . . ? C4 C3 C2 119.97(14) . . ? C3 C4 H4 121.1 . . ? C3 C4 C5 117.83(16) . . ? C5 C4 H4 121.1 . . ? C6 C5 C4 119.31(15) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? B10 B9 H9 122.0 . . ? B10 B9 B5 59.64(10) . . ? B5 B9 H9 122.2 . . ? B8 B9 H9 121.7 . . ? B8 B9 B10 59.90(10) . . ? B8 B9 B5 107.55(12) . . ? B8 B9 B2 108.42(12) . . ? B1 B9 H9 121.4 . . ? B1 B9 B10 108.04(12) . . ? B1 B9 B5 107.99(12) . . ? B1 B9 B8 60.08(10) . . ? B1 B9 B2 60.66(10) . . ? B2 B9 H9 121.5 . . ? B2 B9 B10 107.73(13) . . ? B2 B9 B5 59.61(10) . . ? C1 B4 H4A 123.9 . . ? C1 B4 B6 104.68(12) . . ? C1 B4 B3 57.52(9) . . ? C1 B4 B7 106.07(12) . . ? C2 B4 C1 59.12(9) . . ? C2 B4 H4A 123.8 . . ? C2 B4 B6 105.07(12) . . ? C2 B4 B3 105.13(12) . . ? C2 B4 B7 58.55(9) . . ? B6 B4 H4A 123.0 . . ? B6 B4 B3 60.02(10) . . ? B6 B4 B7 60.14(10) . . ? B3 B4 H4A 122.6 . . ? B7 B4 H4A 121.8 . . ? B7 B4 B3 108.02(12) . . ? B4 B6 H6A 121.3 . . ? B4 B6 B10 108.32(12) . . ? B4 B6 B5 108.30(12) . . ? B4 B6 B3 60.50(10) . . ? B4 B6 B7 60.13(10) . . ? B10 B6 H6A 121.8 . . ? B10 B6 B5 59.72(10) . . ? B5 B6 H6A 121.9 . . ? B3 B6 H6A 121.5 . . ? B3 B6 B10 108.04(13) . . ? B3 B6 B5 59.97(10) . . ? B7 B6 H6A 121.7 . . ? B7 B6 B10 60.04(10) . . ? B7 B6 B5 107.78(13) . . ? B7 B6 B3 108.39(12) . . ? B9 B10 H10 121.8 . . ? B6 B10 B9 108.01(12) . . ? B6 B10 H10 121.8 . . ? B5 B10 B9 60.19(10) . . ? B5 B10 B6 60.17(10) . . ? B5 B10 H10 121.6 . . ? B5 B10 B8 107.82(12) . . ? B5 B10 B7 107.89(13) . . ? B8 B10 B9 59.70(10) . . ? B8 B10 B6 107.49(12) . . ? B8 B10 H10 122.1 . . ? B8 B10 B7 59.72(10) . . ? B7 B10 B9 107.58(12) . . ? B7 B10 B6 59.72(10) . . ? B7 B10 H10 122.0 . . ? B9 B5 H5A 121.8 . . ? B6 B5 B9 107.96(12) . . ? B6 B5 H5A 121.8 . . ? B10 B5 B9 60.17(10) . . ? B10 B5 B6 60.12(10) . . ? B10 B5 H5A 121.4 . . ? B10 B5 B3 108.23(13) . . ? B3 B5 B9 108.06(12) . . ? B3 B5 B6 59.81(10) . . ? B3 B5 H5A 121.6 . . ? B2 B5 B9 59.92(10) . . ? B2 B5 B6 108.13(12) . . ? B2 B5 B10 108.40(12) . . ? B2 B5 H5A 121.5 . . ? B2 B5 B3 60.32(10) . . ? C2 B8 B9 105.45(12) . . ? C2 B8 B10 105.44(12) . . ? C2 B8 H8 124.2 . . ? C2 B8 B1 59.11(9) . . ? C2 B8 B7 58.80(10) . . ? B9 B8 B10 60.40(10) . . ? B9 B8 H8 122.0 . . ? B9 B8 B1 59.86(10) . . ? B10 B8 H8 122.0 . . ? B1 B8 B10 108.27(12) . . ? B1 B8 H8 121.4 . . ? B7 B8 B9 108.54(12) . . ? B7 B8 B10 60.23(10) . . ? B7 B8 H8 121.3 . . ? B7 B8 B1 108.22(12) . . ? C1 B1 B9 104.98(12) . . ? C1 B1 B8 106.39(12) . . ? C1 B1 H1 123.6 . . ? C1 B1 B2 57.70(9) . . ? C2 B1 C1 59.40(9) . . ? C2 B1 B9 105.24(12) . . ? C2 B1 B8 58.64(9) . . ? C2 B1 H1 123.6 . . ? C2 B1 B2 105.29(12) . . ? B9 B1 B8 60.05(10) . . ? B9 B1 H1 123.0 . . ? B9 B1 B2 59.84(10) . . ? B8 B1 H1 121.8 . . ? B8 B1 B2 107.75(12) . . ? B2 B1 H1 122.7 . . ? C1 B3 B4 60.40(9) . . ? C1 B3 B6 106.50(12) . . ? C1 B3 B5 105.44(12) . . ? C1 B3 H3 123.4 . . ? C1 B3 B2 58.52(9) . . ? B4 B3 H3 121.3 . . ? B6 B3 B4 59.48(10) . . ? B6 B3 B5 60.23(10) . . ? B6 B3 H3 122.0 . . ? B6 B3 B2 107.88(12) . . ? B5 B3 B4 107.70(12) . . ? B5 B3 H3 122.5 . . ? B5 B3 B2 59.59(10) . . ? B2 B3 B4 108.15(12) . . ? B2 B3 H3 121.9 . . ? C1 B2 B9 106.34(12) . . ? C1 B2 B5 105.75(12) . . ? C1 B2 B1 59.79(9) . . ? C1 B2 B3 58.42(9) . . ? C1 B2 H2 123.6 . . ? B9 B2 B1 59.49(10) . . ? B9 B2 B3 108.32(12) . . ? B9 B2 H2 121.8 . . ? B5 B2 B9 60.47(10) . . ? B5 B2 B1 107.74(12) . . ? B5 B2 B3 60.09(10) . . ? B5 B2 H2 122.1 . . ? B1 B2 H2 121.8 . . ? B3 B2 B1 107.61(12) . . ? B3 B2 H2 121.8 . . ? C2 B7 B4 59.20(9) . . ? C2 B7 B6 105.25(12) . . ? C2 B7 B10 105.36(12) . . ? C2 B7 B8 58.87(10) . . ? C2 B7 H7A 124.2 . . ? B4 B7 B10 108.16(12) . . ? B4 B7 H7A 121.4 . . ? B6 B7 B4 59.73(10) . . ? B6 B7 B10 60.24(10) . . ? B6 B7 H7A 122.3 . . ? B10 B7 H7A 122.1 . . ? B8 B7 B4 108.27(12) . . ? B8 B7 B6 108.17(13) . . ? B8 B7 B10 60.06(10) . . ? B8 B7 H7A 121.4 . . ? _shelx_res_file ; spok41_a.res created by SHELXL-2014/7 TITL spok41_a.res in P2(1)/n REM Old TITL spok41 in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.110, Rweak 0.006, Alpha 0.034, Orientation as input REM Formula found by SHELXT: C10 B10 N F2 CELL 0.71073 7.2661 15.0779 13.2917 90 90.604 90 ZERR 2 0.0012 0.0018 0.0016 0 0.005 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H B F N UNIT 40 56 40 8 4 L.S. 10 PLAN 20 SIZE 0.25 0.29 0.32 TEMP -173.15 BOND $H LIST 6 fmap 2 ACTA OMIT 1 1 4 OMIT 2 2 2 OMIT 1 2 0 OMIT 1 1 3 REM REM REM WGHT 0.059500 0.887000 FVAR 0.28864 F2 4 0.326513 0.344151 0.527871 11.00000 0.01730 0.01269 = 0.01771 0.00409 -0.00459 -0.00614 F1 4 0.181698 0.454969 0.407623 11.00000 0.01354 0.01634 = 0.01870 0.00444 -0.00725 -0.00578 N1 5 0.410681 0.481134 0.753167 11.00000 0.02210 0.01504 = 0.01748 0.00267 0.00503 0.00496 C9 1 0.417875 0.420824 0.517663 11.00000 0.01327 0.00904 = 0.01086 -0.00035 0.00232 -0.00156 C8 1 0.579480 0.437471 0.571590 11.00000 0.01262 0.01075 = 0.00920 0.00051 0.00109 0.00199 C10 1 0.340227 0.480671 0.450801 11.00000 0.00873 0.01398 = 0.01251 -0.00055 -0.00175 -0.00082 C1 1 0.670363 0.370599 0.640275 11.00000 0.01172 0.01080 = 0.00949 0.00020 -0.00002 0.00044 C2 1 0.621216 0.357510 0.765593 11.00000 0.01457 0.01164 = 0.01048 0.00103 -0.00096 0.00021 C6 1 0.214612 0.524465 0.888528 11.00000 0.01546 0.02061 = 0.02192 -0.00712 0.00414 0.00125 AFIX 43 H6 2 0.122207 0.563101 0.913217 11.00000 -1.20000 AFIX 0 C7 1 0.280415 0.533711 0.791511 11.00000 0.02457 0.01708 = 0.02216 0.00074 0.00402 0.00470 AFIX 43 H7 2 0.230751 0.579495 0.750310 11.00000 -1.20000 AFIX 0 C3 1 0.476793 0.416714 0.811547 11.00000 0.01162 0.01538 = 0.01271 -0.00166 -0.00048 -0.00194 C4 1 0.420530 0.402252 0.909672 11.00000 0.01806 0.02419 = 0.01414 0.00177 0.00053 0.00063 AFIX 43 H4 2 0.472107 0.355777 0.949137 11.00000 -1.20000 AFIX 0 C5 1 0.286312 0.457968 0.948290 11.00000 0.02175 0.03038 = 0.01258 -0.00210 0.00370 -0.00014 AFIX 43 H5 2 0.244418 0.450297 1.015193 11.00000 -1.20000 AFIX 0 B9 3 0.993769 0.323388 0.742004 11.00000 0.01425 0.01703 = 0.01381 -0.00037 -0.00217 0.00377 AFIX 153 H9 2 1.140242 0.339153 0.762076 11.00000 -1.20000 AFIX 0 B4 3 0.549368 0.276785 0.682144 11.00000 0.01693 0.01066 = 0.01345 0.00207 -0.00070 -0.00142 AFIX 153 H4A 2 0.401408 0.263226 0.663343 11.00000 -1.20000 AFIX 0 B6 3 0.717635 0.192288 0.691275 11.00000 0.02028 0.01169 = 0.01526 0.00028 -0.00313 0.00217 AFIX 153 H6A 2 0.681625 0.121035 0.677671 11.00000 -1.20000 AFIX 0 B10 3 0.883720 0.224316 0.784338 11.00000 0.01903 0.01517 = 0.01584 0.00136 -0.00267 0.00265 AFIX 153 H10 2 0.957890 0.174265 0.832018 11.00000 -1.20000 AFIX 0 B5 3 0.933817 0.237741 0.654555 11.00000 0.01855 0.01570 = 0.01611 -0.00064 -0.00325 0.00419 AFIX 153 H5A 2 1.041068 0.196453 0.616839 11.00000 -1.20000 AFIX 0 B8 3 0.815751 0.329372 0.832219 11.00000 0.01646 0.01449 = 0.01271 0.00086 -0.00347 0.00202 AFIX 153 H8 2 0.843354 0.349213 0.912165 11.00000 -1.20000 AFIX 0 B1 3 0.824681 0.407753 0.732669 11.00000 0.01097 0.01466 = 0.01295 -0.00100 -0.00109 0.00008 AFIX 153 H1 2 0.855458 0.479499 0.746751 11.00000 -1.20000 AFIX 0 B3 3 0.727540 0.269999 0.590770 11.00000 0.01647 0.01177 = 0.01342 -0.00163 -0.00127 0.00321 AFIX 153 H3 2 0.696870 0.250642 0.510988 11.00000 -1.20000 AFIX 0 B2 3 0.898995 0.350574 0.622018 11.00000 0.01179 0.01636 = 0.01283 -0.00014 -0.00098 0.00250 AFIX 153 H2 2 0.982346 0.384375 0.562882 11.00000 -1.20000 AFIX 0 B7 3 0.646236 0.249027 0.801287 11.00000 0.02050 0.01331 = 0.01352 0.00305 -0.00180 0.00123 AFIX 153 H7A 2 0.562359 0.216097 0.860826 11.00000 -1.20000 AFIX 0 HKLF 4 REM spok41_a.res in P2(1)/n REM R1 = 0.0489 for 2981 Fo > 4sig(Fo) and 0.0605 for all 3596 data REM 208 parameters refined using 0 restraints END WGHT 0.0598 0.9191 REM Highest difference peak 0.368, deepest hole -0.261, 1-sigma level 0.059 Q1 1 0.7965 0.3791 0.6433 11.00000 0.05 0.37 Q2 1 0.1553 0.3372 0.5207 11.00000 0.05 0.37 Q3 1 0.2969 0.4392 0.3982 11.00000 0.05 0.36 Q4 1 0.2527 0.5212 0.8415 11.00000 0.05 0.33 Q5 1 0.4217 0.2973 0.6720 11.00000 0.05 0.33 Q6 1 0.7940 0.2619 0.8007 11.00000 0.05 0.32 Q7 1 0.5375 0.3866 0.7829 11.00000 0.05 0.32 Q8 1 0.5355 0.2420 0.8409 11.00000 0.05 0.32 Q9 1 0.4070 0.4440 0.4621 11.00000 0.05 0.32 Q10 1 0.4422 0.4062 0.8575 11.00000 0.05 0.31 Q11 1 0.9159 0.4106 0.5779 11.00000 0.05 0.30 Q12 1 0.2753 0.5007 0.9182 11.00000 0.05 0.30 Q13 1 0.3668 0.4600 0.5029 11.00000 0.05 0.30 Q14 1 0.6827 0.2830 0.5267 11.00000 0.05 0.29 Q15 1 0.8684 0.3601 0.7656 11.00000 0.05 0.28 Q16 1 0.3251 0.4262 0.9235 11.00000 0.05 0.27 Q17 1 0.6416 0.4705 0.5492 11.00000 0.05 0.27 Q18 1 0.2093 0.4783 0.9095 11.00000 0.05 0.26 Q19 1 0.6245 0.3974 0.6091 11.00000 0.05 0.26 Q20 1 0.7950 0.4654 0.7493 11.00000 0.05 0.26 ; _shelx_res_checksum 11179 _shelx_hkl_file ; -1 0 0 1.23 0.18 -1 0 0 1.30 0.19 -1 0 0 0.93 0.14 1 0 0 1.01 0.15 1 0 0 1.05 0.20 -2 0 0 223.53 6.94 2 0 0 253.04 6.95 -2 0 0 232.26 7.03 2 0 0 242.82 7.04 -2 0 0 234.67 7.00 -3 0 0 0.40 0.25 -3 0 0 0.81 0.36 -3 0 0 -0.02 0.22 3 0 0 0.46 0.34 3 0 0 0.45 0.24 -4 0 0 59.36 2.05 -4 0 0 60.90 2.19 -4 0 0 60.32 2.21 -5 0 0 0.69 0.43 -5 0 0 0.89 0.49 -6 0 0 7.43 0.91 -6 0 0 5.16 0.77 -7 0 0 -0.39 0.55 -7 0 0 -0.43 0.57 -8 0 0 45.92 2.41 -8 0 0 46.64 2.29 -9 0 0 -0.32 0.71 -9 0 0 -1.16 0.70 0 -1 0 -0.15 0.04 0 1 0 -0.16 0.03 1 -1 0 630.74 18.26 -1 -1 0 623.70 18.22 -1 -1 0 629.64 18.23 1 -1 0 655.98 18.24 -1 -1 0 628.33 18.23 -1 -1 0 651.99 18.23 -1 1 0 590.58 18.35 -1 1 0 618.14 18.24 1 1 0 650.36 18.23 1 1 0 663.44 18.23 1 1 0 625.88 18.34 2 -1 0 66.18 2.09 -2 -1 0 63.26 2.05 -2 -1 0 62.25 2.10 -2 -1 0 65.64 2.11 -2 -1 0 62.53 2.09 2 -1 0 65.95 1.97 2 1 0 66.01 2.05 2 1 0 65.14 2.10 -2 1 0 63.00 2.04 -2 1 0 61.12 2.10 -3 -1 0 3.47 0.40 -3 -1 0 3.51 0.47 -3 -1 0 2.97 0.42 3 -1 0 3.66 0.34 -3 1 0 2.79 0.45 3 1 0 3.12 0.39 -3 1 0 2.98 0.40 -4 -1 0 16.98 0.98 -4 -1 0 17.87 1.02 -4 -1 0 16.64 0.90 4 -1 0 18.03 0.81 -4 1 0 18.04 1.03 -4 1 0 19.29 0.96 -5 -1 0 63.80 2.32 -5 -1 0 66.15 2.48 -5 -1 0 66.10 2.47 -5 1 0 62.16 2.46 -5 1 0 65.37 2.40 -6 -1 0 0.13 0.50 -6 -1 0 -0.19 0.52 -6 1 0 0.35 0.53 -6 1 0 -0.19 0.46 -7 -1 0 6.54 0.99 -7 -1 0 6.44 0.94 -7 1 0 5.58 0.95 -7 1 0 7.06 0.92 -8 -1 0 0.85 0.68 -8 -1 0 -0.47 0.68 -8 1 0 0.06 0.57 -8 1 0 0.58 0.72 -9 -1 0 0.77 0.69 -9 -1 0 0.61 0.76 -9 1 0 -0.31 0.75 -9 1 0 -0.36 0.62 0 -2 0 106.32 3.11 0 -2 0 105.52 3.10 0 -2 0 105.09 3.06 0 2 0 105.04 3.10 -1 -2 0 3.75 0.32 -1 -2 0 3.58 0.33 -1 -2 0 3.60 0.29 -1 -2 0 3.57 0.30 -1 2 0 2.54 0.27 -1 2 0 2.41 0.20 1 2 0 3.17 0.30 -2 -2 0 120.96 3.77 -2 -2 0 126.37 3.77 2 -2 0 123.30 3.77 -2 -2 0 122.92 3.75 -2 -2 0 123.25 3.77 2 -2 0 121.22 3.58 2 2 0 126.30 3.77 -2 2 0 118.65 3.66 -2 2 0 114.13 3.76 2 2 0 124.56 3.74 -3 -2 0 1.03 0.38 3 -2 0 1.47 0.23 -3 -2 0 0.74 0.32 -3 -2 0 0.79 0.37 -3 2 0 1.34 0.31 -3 2 0 1.07 0.38 4 -2 0 2.02 0.29 -4 -2 0 0.83 0.35 -4 -2 0 0.76 0.33 -4 -2 0 0.81 0.41 -4 2 0 1.24 0.36 -4 2 0 1.17 0.43 -5 -2 0 4.23 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