data_cx1488 _audit_creation_date 2019-01-22 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2017/1' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C25 H30 B Br I2 N2 O3, C2 H7 O S' _chemical_formula_sum 'C27 H37 B Br I2 N2 O4 S' _chemical_formula_weight 830.16 _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' 'Br' 'Br' -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.3257 6.8362 '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' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 '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/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.8415(12) _cell_length_b 15.1909(13) _cell_length_c 16.2100(14) _cell_angle_alpha 90 _cell_angle_beta 109.352(6) _cell_angle_gamma 90 _cell_volume 3215.8(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9865 _cell_measurement_temperature 99.97 _cell_measurement_theta_max 64.020 _cell_measurement_theta_min 2.909 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 17.691 _exptl_absorpt_correction_T_max 0.7524 _exptl_absorpt_correction_T_min 0.5227 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1215 before and 0.0868 after correction. The Ratio of minimum to maximum transmission is 0.6947. The \l/2 correction factor is Not present.' _exptl_absorpt_special_details ? _exptl_crystal_colour pink _exptl_crystal_colour_primary pink _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description 'plate' _exptl_crystal_F_000 1628 _exptl_crystal_recrystallization_method 'The material was recrystallised from --- by as supplied' _exptl_crystal_size_max 0.253 _exptl_crystal_size_mid 0.249 _exptl_crystal_size_min 0.016 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0964 _diffrn_reflns_av_unetI/netI 0.0601 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 37392 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 64.016 _diffrn_reflns_theta_max 64.016 _diffrn_reflns_theta_min 3.384 _diffrn_ambient_temperature 99.97 _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker Kappa APEX CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'MX optics' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source microsource _diffrn_standards_number . _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 4410 _reflns_number_total 5323 _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, 2017)' _computing_data_collection 'APEX2 V2017.3 (Bruker, 2017)' _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XS (Sheldrick, 2008)' _refine_diff_density_max 2.078 _refine_diff_density_min -1.035 _refine_diff_density_rms 0.144 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 352 _refine_ls_number_reflns 5323 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0595 _refine_ls_R_factor_gt 0.0478 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0659P)^2^+9.5791P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1202 _refine_ls_wR_factor_ref 0.1276 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2.a Secondary CH2 refined with riding coordinates: C10(H10A,H10B), C11(H11A,H11B), C16(H16A,H16B), C18(H18A,H18B) 2.b Aromatic/amide H refined with riding coordinates: C21(H21), C22(H22), C24(H24), C25(H25) 2.c Idealised Me refined as rotating group: C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B, H15C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C26(H26A,H26B,H26C), C27(H27A, H27B,H27C) 2.d Idealised tetrahedral OH refined as rotating group: O4(H4) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary heavy _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 I1 I -0.19834(3) 0.41730(3) 0.48376(3) 0.03132(15) Uani 1 1 d . . . . . I2 I 0.58343(3) 0.19702(3) 0.80545(3) 0.03859(17) Uani 1 1 d . . . . . Br1 Br 0.28036(6) 0.63764(6) 1.00261(5) 0.0454(2) Uani 1 1 d . . . . . O1 O -0.0445(5) 0.2834(4) 0.3677(4) 0.0566(16) Uani 1 1 d . . . . . O2 O 0.1935(3) 0.2416(3) 0.4837(3) 0.0225(9) Uani 1 1 d . . . . . O3 O 0.1473(3) 0.1356(3) 0.5652(3) 0.0254(10) Uani 1 1 d . . . . . N1 N 0.0932(4) 0.2916(3) 0.5768(3) 0.0204(11) Uani 1 1 d . . . . . N2 N 0.2762(4) 0.2472(4) 0.6464(3) 0.0229(11) Uani 1 1 d . . . . . C1 C -0.0029(5) 0.3008(4) 0.5203(4) 0.0230(14) Uani 1 1 d . . . . . C2 C -0.0495(4) 0.3740(4) 0.5450(4) 0.0196(13) Uani 1 1 d . . . . . C3 C 0.0199(5) 0.4120(4) 0.6191(4) 0.0206(13) Uani 1 1 d . . . . . C4 C 0.1106(5) 0.3587(4) 0.6400(4) 0.0187(13) Uani 1 1 d . . . . . C5 C 0.2029(5) 0.3652(4) 0.7072(4) 0.0179(12) Uani 1 1 d . . . . . C6 C 0.2859(5) 0.3097(4) 0.7121(4) 0.0203(13) Uani 1 1 d . . . . . C7 C 0.3849(5) 0.3037(4) 0.7749(4) 0.0228(14) Uani 1 1 d . . . . . C8 C 0.4338(5) 0.2383(5) 0.7442(4) 0.0240(14) Uani 1 1 d . . . . . C9 C 0.3656(5) 0.2038(4) 0.6649(4) 0.0245(14) Uani 1 1 d . . . . . C10 C -0.0473(5) 0.2416(5) 0.4439(4) 0.0311(16) Uani 1 1 d . . . . . H10A H -0.007607 0.186083 0.452771 0.037 Uiso 1 1 calc R . . . . H10B H -0.118909 0.226961 0.438144 0.037 Uiso 1 1 calc R . . . . C11 C -0.0967(9) 0.2340(8) 0.2916(6) 0.073(3) Uani 1 1 d . . . . . H11A H -0.170976 0.232884 0.282938 0.087 Uiso 1 1 calc R . . . . H11B H -0.071293 0.172631 0.298570 0.087 Uiso 1 1 calc R . . . . C12 C -0.0791(8) 0.2753(8) 0.2138(7) 0.066(3) Uani 1 1 d . . . . . H12A H -0.124059 0.247584 0.160267 0.099 Uiso 1 1 calc GR . . . . H12B H -0.007497 0.266818 0.217808 0.099 Uiso 1 1 calc GR . . . . H12C H -0.094164 0.338383 0.212613 0.099 Uiso 1 1 calc GR . . . . C13 C 0.0019(5) 0.4931(4) 0.6639(4) 0.0251(14) Uani 1 1 d . . . . . H13A H 0.019564 0.481641 0.726696 0.038 Uiso 1 1 calc GR . . . . H13B H -0.070415 0.509955 0.639692 0.038 Uiso 1 1 calc GR . . . . H13C H 0.044640 0.541088 0.654830 0.038 Uiso 1 1 calc GR . . . . C14 C 0.4317(5) 0.3545(5) 0.8586(4) 0.0346(17) Uani 1 1 d . . . . . H14A H 0.450275 0.413650 0.845000 0.052 Uiso 1 1 calc GR . . . . H14B H 0.493145 0.323834 0.895462 0.052 Uiso 1 1 calc GR . . . . H14C H 0.382091 0.358928 0.889734 0.052 Uiso 1 1 calc GR . . . . C15 C 0.3846(6) 0.1316(5) 0.6099(5) 0.0362(17) Uani 1 1 d . . . . . H15A H 0.372187 0.074657 0.632891 0.054 Uiso 1 1 calc GR . . . . H15B H 0.455785 0.134370 0.610947 0.054 Uiso 1 1 calc GR . . . . H15C H 0.338427 0.138380 0.549577 0.054 Uiso 1 1 calc GR . . . . C16 C 0.2124(6) 0.3296(5) 0.4656(4) 0.0311(15) Uani 1 1 d . . . . . H16A H 0.274595 0.351587 0.511383 0.037 Uiso 1 1 calc R . . . . H16B H 0.153982 0.367165 0.465484 0.037 Uiso 1 1 calc R . . . . C17 C 0.2269(7) 0.3341(5) 0.3785(5) 0.0398(18) Uani 1 1 d . . . . . H17A H 0.167313 0.308319 0.334043 0.060 Uiso 1 1 calc GR . . . . H17B H 0.288638 0.301288 0.380591 0.060 Uiso 1 1 calc GR . . . . H17C H 0.234386 0.395736 0.363773 0.060 Uiso 1 1 calc GR . . . . C18 C 0.1286(8) 0.1017(5) 0.6401(5) 0.046(2) Uani 1 1 d . . . . . H18A H 0.068470 0.131708 0.647264 0.055 Uiso 1 1 calc R . . . . H18B H 0.188510 0.113734 0.692715 0.055 Uiso 1 1 calc R . . . . C19 C 0.1098(9) 0.0066(6) 0.6320(6) 0.059(3) Uani 1 1 d . . . . . H19A H 0.056140 -0.005996 0.576258 0.088 Uiso 1 1 calc GR . . . . H19B H 0.087719 -0.013707 0.680310 0.088 Uiso 1 1 calc GR . . . . H19C H 0.172906 -0.023921 0.634094 0.088 Uiso 1 1 calc GR . . . . C20 C 0.2178(4) 0.4336(4) 0.7767(4) 0.0187(13) Uani 1 1 d . . . . . C21 C 0.2688(5) 0.5109(4) 0.7740(4) 0.0270(15) Uani 1 1 d . . . . . H21 H 0.292112 0.522400 0.726102 0.032 Uiso 1 1 calc R . . . . C22 C 0.2862(6) 0.5718(5) 0.8406(5) 0.0311(16) Uani 1 1 d . . . . . H22 H 0.321099 0.625225 0.838487 0.037 Uiso 1 1 calc R . . . . C23 C 0.2527(5) 0.5548(5) 0.9101(4) 0.0268(15) Uani 1 1 d . . . . . C24 C 0.2014(5) 0.4778(5) 0.9144(4) 0.0233(14) Uani 1 1 d . . . . . H24 H 0.178629 0.466564 0.962554 0.028 Uiso 1 1 calc R . . . . C25 C 0.1839(5) 0.4172(4) 0.8468(4) 0.0211(13) Uani 1 1 d . . . . . H25 H 0.148360 0.364148 0.848562 0.025 Uiso 1 1 calc R . . . . B1 B 0.1769(6) 0.2253(5) 0.5653(4) 0.0246(16) Uani 1 1 d . . . . . S1 S 0.5185(2) 0.56626(19) 0.3760(2) 0.0685(7) Uani 1 1 d . . . . . O4 O 0.5926(5) 0.5080(5) 0.4391(6) 0.080(2) Uani 1 1 d . . . . . H4 H 0.566618 0.457798 0.437881 0.119 Uiso 1 1 calc GR . . . . C26 C 0.3986(8) 0.5115(9) 0.3428(9) 0.083(4) Uani 1 1 d . . . . . H26A H 0.379082 0.498186 0.394329 0.124 Uiso 1 1 calc GR . . . . H26B H 0.403934 0.456597 0.312892 0.124 Uiso 1 1 calc GR . . . . H26C H 0.346588 0.549456 0.302959 0.124 Uiso 1 1 calc GR . . . . C27 C 0.4847(10) 0.6520(7) 0.4378(9) 0.081(3) Uani 1 1 d . . . . . H27A H 0.543841 0.690590 0.463185 0.121 Uiso 1 1 calc GR . . . . H27B H 0.464207 0.625731 0.484654 0.121 Uiso 1 1 calc GR . . . . H27C H 0.427682 0.686344 0.399124 0.121 Uiso 1 1 calc GR . . . . 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 I1 0.0227(2) 0.0316(3) 0.0333(2) 0.00292(19) 0.00067(17) -0.00025(17) I2 0.0289(2) 0.0474(3) 0.0342(3) -0.0114(2) 0.00332(18) 0.0147(2) Br1 0.0492(5) 0.0522(6) 0.0395(4) -0.0292(4) 0.0210(4) -0.0127(4) O1 0.063(4) 0.059(4) 0.040(3) -0.007(3) 0.007(3) -0.007(3) O2 0.036(2) 0.018(2) 0.0138(19) -0.0027(17) 0.0100(17) 0.0020(19) O3 0.039(3) 0.024(3) 0.017(2) 0.0007(19) 0.0127(19) 0.001(2) N1 0.028(3) 0.019(3) 0.015(2) -0.006(2) 0.008(2) -0.002(2) N2 0.031(3) 0.024(3) 0.015(2) -0.001(2) 0.009(2) 0.007(2) C1 0.023(3) 0.027(4) 0.018(3) 0.002(3) 0.005(2) -0.002(3) C2 0.015(3) 0.026(4) 0.014(3) 0.004(3) 0.000(2) 0.002(3) C3 0.025(3) 0.022(3) 0.013(3) 0.002(2) 0.003(2) 0.001(3) C4 0.028(3) 0.018(3) 0.014(3) 0.002(2) 0.012(2) -0.002(3) C5 0.027(3) 0.015(3) 0.014(3) 0.004(2) 0.010(2) 0.000(2) C6 0.026(3) 0.024(4) 0.013(3) 0.001(2) 0.008(2) 0.001(3) C7 0.023(3) 0.030(4) 0.017(3) -0.002(3) 0.008(2) 0.002(3) C8 0.020(3) 0.029(4) 0.020(3) 0.005(3) 0.002(2) 0.007(3) C9 0.031(3) 0.028(4) 0.015(3) 0.001(3) 0.009(3) 0.004(3) C10 0.035(4) 0.032(4) 0.021(3) -0.003(3) 0.002(3) 0.000(3) C11 0.085(8) 0.085(8) 0.042(5) -0.015(5) 0.013(5) -0.018(6) C12 0.073(7) 0.069(7) 0.055(6) -0.006(5) 0.020(5) 0.008(6) C13 0.027(3) 0.028(4) 0.020(3) 0.000(3) 0.007(3) 0.009(3) C14 0.026(3) 0.042(5) 0.028(3) -0.013(3) -0.002(3) 0.007(3) C15 0.036(4) 0.043(5) 0.029(4) -0.010(3) 0.011(3) 0.011(3) C16 0.045(4) 0.028(4) 0.023(3) -0.002(3) 0.015(3) 0.000(3) C17 0.059(5) 0.034(4) 0.034(4) 0.003(3) 0.024(4) -0.003(4) C18 0.082(6) 0.034(5) 0.038(4) -0.004(4) 0.041(4) -0.009(4) C19 0.110(8) 0.037(5) 0.046(5) 0.003(4) 0.049(6) -0.013(5) C20 0.019(3) 0.024(4) 0.013(3) 0.001(2) 0.006(2) 0.003(2) C21 0.042(4) 0.023(4) 0.024(3) -0.007(3) 0.022(3) -0.011(3) C22 0.040(4) 0.026(4) 0.033(4) -0.006(3) 0.020(3) -0.011(3) C23 0.028(3) 0.033(4) 0.021(3) -0.011(3) 0.010(3) -0.002(3) C24 0.028(3) 0.032(4) 0.013(3) -0.003(3) 0.011(2) 0.000(3) C25 0.027(3) 0.020(3) 0.020(3) 0.006(3) 0.013(3) 0.000(3) B1 0.027(4) 0.030(4) 0.017(3) -0.007(3) 0.008(3) 0.003(3) S1 0.0560(14) 0.0636(17) 0.0871(18) 0.0074(14) 0.0252(13) 0.0010(12) O4 0.050(4) 0.051(4) 0.122(7) -0.004(4) 0.007(4) 0.003(3) C26 0.051(6) 0.096(10) 0.087(8) -0.014(7) 0.002(5) 0.002(6) C27 0.083(8) 0.051(7) 0.108(9) -0.003(6) 0.032(7) 0.004(6) _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 I1 C2 2.075(6) . ? I2 C8 2.075(6) . ? Br1 C23 1.897(6) . ? O1 C10 1.401(9) . ? O1 C11 1.420(11) . ? O2 C16 1.411(8) . ? O2 B1 1.438(8) . ? O3 C18 1.418(8) . ? O3 B1 1.423(9) . ? N1 C1 1.349(8) . ? N1 C4 1.409(8) . ? N1 B1 1.591(9) . ? N2 C6 1.399(8) . ? N2 C9 1.346(8) . ? N2 B1 1.590(9) . ? C1 C2 1.408(9) . ? C1 C10 1.489(9) . ? C2 C3 1.392(9) . ? C3 C4 1.436(9) . ? C3 C13 1.493(9) . ? C4 C5 1.380(9) . ? C5 C6 1.406(9) . ? C5 C20 1.496(9) . ? C6 C7 1.414(9) . ? C7 C8 1.384(9) . ? C7 C14 1.507(9) . ? C8 C9 1.419(9) . ? C9 C15 1.491(9) . ? C11 C12 1.498(15) . ? C16 C17 1.491(9) . ? C18 C19 1.465(11) . ? C20 C21 1.379(9) . ? C20 C25 1.389(8) . ? C21 C22 1.381(10) . ? C22 C23 1.378(9) . ? C23 C24 1.381(10) . ? C24 C25 1.389(9) . ? S1 O4 1.479(8) . ? S1 C26 1.772(12) . ? S1 C27 1.796(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 O1 C11 111.8(7) . . ? C16 O2 B1 116.9(5) . . ? C18 O3 B1 118.8(5) . . ? C1 N1 C4 108.1(5) . . ? C1 N1 B1 125.4(5) . . ? C4 N1 B1 126.0(5) . . ? C6 N2 B1 127.5(5) . . ? C9 N2 C6 108.2(5) . . ? C9 N2 B1 124.2(5) . . ? N1 C1 C2 109.4(5) . . ? N1 C1 C10 122.9(6) . . ? C2 C1 C10 127.7(6) . . ? C1 C2 I1 126.2(4) . . ? C3 C2 I1 125.0(5) . . ? C3 C2 C1 108.8(5) . . ? C2 C3 C4 105.6(5) . . ? C2 C3 C13 125.7(6) . . ? C4 C3 C13 128.6(5) . . ? N1 C4 C3 108.1(5) . . ? C5 C4 N1 121.0(6) . . ? C5 C4 C3 130.8(6) . . ? C4 C5 C6 121.8(5) . . ? C4 C5 C20 120.3(5) . . ? C6 C5 C20 117.9(5) . . ? N2 C6 C5 119.6(5) . . ? N2 C6 C7 109.3(5) . . ? C5 C6 C7 131.1(6) . . ? C6 C7 C14 129.9(6) . . ? C8 C7 C6 105.0(5) . . ? C8 C7 C14 125.1(6) . . ? C7 C8 I2 125.1(5) . . ? C7 C8 C9 109.5(5) . . ? C9 C8 I2 125.5(5) . . ? N2 C9 C8 107.9(5) . . ? N2 C9 C15 123.9(6) . . ? C8 C9 C15 128.1(6) . . ? O1 C10 C1 109.6(6) . . ? O1 C11 C12 109.4(9) . . ? O2 C16 C17 109.5(6) . . ? O3 C18 C19 111.1(6) . . ? C21 C20 C5 120.9(5) . . ? C21 C20 C25 119.6(6) . . ? C25 C20 C5 119.5(6) . . ? C20 C21 C22 120.3(6) . . ? C23 C22 C21 119.6(6) . . ? C22 C23 Br1 119.1(5) . . ? C22 C23 C24 121.2(6) . . ? C24 C23 Br1 119.7(5) . . ? C23 C24 C25 118.7(5) . . ? C20 C25 C24 120.6(6) . . ? O2 B1 N1 110.1(5) . . ? O2 B1 N2 111.5(5) . . ? O3 B1 O2 107.3(5) . . ? O3 B1 N1 112.7(5) . . ? O3 B1 N2 111.7(6) . . ? N2 B1 N1 103.6(5) . . ? O4 S1 C26 107.1(6) . . ? O4 S1 C27 107.3(6) . . ? C26 S1 C27 96.8(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag I1 C2 C3 C4 177.7(4) . . . . ? I1 C2 C3 C13 -4.0(9) . . . . ? I2 C8 C9 N2 179.9(4) . . . . ? I2 C8 C9 C15 0.9(10) . . . . ? Br1 C23 C24 C25 -178.7(5) . . . . ? N1 C1 C2 I1 -178.3(4) . . . . ? N1 C1 C2 C3 0.3(7) . . . . ? N1 C1 C10 O1 -101.2(7) . . . . ? N1 C4 C5 C6 4.8(9) . . . . ? N1 C4 C5 C20 -176.4(5) . . . . ? N2 C6 C7 C8 1.3(7) . . . . ? N2 C6 C7 C14 -178.1(7) . . . . ? C1 N1 C4 C3 -1.0(6) . . . . ? C1 N1 C4 C5 179.3(5) . . . . ? C1 N1 B1 O2 56.9(8) . . . . ? C1 N1 B1 O3 -62.9(8) . . . . ? C1 N1 B1 N2 176.2(5) . . . . ? C1 C2 C3 C4 -0.9(7) . . . . ? C1 C2 C3 C13 177.4(6) . . . . ? C2 C1 C10 O1 77.3(8) . . . . ? C2 C3 C4 N1 1.1(6) . . . . ? C2 C3 C4 C5 -179.2(6) . . . . ? C3 C4 C5 C6 -174.8(6) . . . . ? C3 C4 C5 C20 4.0(10) . . . . ? C4 N1 C1 C2 0.4(7) . . . . ? C4 N1 C1 C10 179.3(6) . . . . ? C4 N1 B1 O2 -113.4(6) . . . . ? C4 N1 B1 O3 126.8(6) . . . . ? C4 N1 B1 N2 5.9(8) . . . . ? C4 C5 C6 N2 1.3(9) . . . . ? C4 C5 C6 C7 -178.6(6) . . . . ? C4 C5 C20 C21 -99.8(7) . . . . ? C4 C5 C20 C25 83.1(7) . . . . ? C5 C6 C7 C8 -178.8(6) . . . . ? C5 C6 C7 C14 1.8(12) . . . . ? C5 C20 C21 C22 -177.0(6) . . . . ? C5 C20 C25 C24 176.8(6) . . . . ? C6 N2 C9 C8 0.6(7) . . . . ? C6 N2 C9 C15 179.7(6) . . . . ? C6 N2 B1 O2 118.8(6) . . . . ? C6 N2 B1 O3 -121.1(6) . . . . ? C6 N2 B1 N1 0.5(8) . . . . ? C6 C5 C20 C21 79.0(8) . . . . ? C6 C5 C20 C25 -98.1(7) . . . . ? C6 C7 C8 I2 179.4(4) . . . . ? C6 C7 C8 C9 -1.0(7) . . . . ? C7 C8 C9 N2 0.3(8) . . . . ? C7 C8 C9 C15 -178.8(7) . . . . ? C9 N2 C6 C5 178.9(5) . . . . ? C9 N2 C6 C7 -1.2(7) . . . . ? C9 N2 B1 O2 -64.4(8) . . . . ? C9 N2 B1 O3 55.7(8) . . . . ? C9 N2 B1 N1 177.3(5) . . . . ? C10 O1 C11 C12 -172.3(8) . . . . ? C10 C1 C2 I1 3.0(10) . . . . ? C10 C1 C2 C3 -178.5(6) . . . . ? C11 O1 C10 C1 -173.1(8) . . . . ? C13 C3 C4 N1 -177.1(6) . . . . ? C13 C3 C4 C5 2.5(11) . . . . ? C14 C7 C8 I2 -1.1(10) . . . . ? C14 C7 C8 C9 178.5(7) . . . . ? C16 O2 B1 O3 173.1(5) . . . . ? C16 O2 B1 N1 50.1(7) . . . . ? C16 O2 B1 N2 -64.3(7) . . . . ? C18 O3 B1 O2 178.4(6) . . . . ? C18 O3 B1 N1 -60.2(8) . . . . ? C18 O3 B1 N2 55.9(8) . . . . ? C20 C5 C6 N2 -177.5(5) . . . . ? C20 C5 C6 C7 2.6(10) . . . . ? C20 C21 C22 C23 0.3(11) . . . . ? C21 C20 C25 C24 -0.4(9) . . . . ? C21 C22 C23 Br1 178.3(6) . . . . ? C21 C22 C23 C24 -0.3(11) . . . . ? C22 C23 C24 C25 0.0(10) . . . . ? C23 C24 C25 C20 0.4(9) . . . . ? C25 C20 C21 C22 0.1(10) . . . . ? B1 O2 C16 C17 -179.5(6) . . . . ? B1 O3 C18 C19 -174.0(8) . . . . ? B1 N1 C1 C2 -171.4(6) . . . . ? B1 N1 C1 C10 7.4(10) . . . . ? B1 N1 C4 C3 170.8(5) . . . . ? B1 N1 C4 C5 -8.9(9) . . . . ? B1 N2 C6 C5 -3.9(9) . . . . ? B1 N2 C6 C7 176.0(6) . . . . ? B1 N2 C9 C8 -176.8(6) . . . . ? B1 N2 C9 C15 2.3(10) . . . . ? _shelx_res_file ; TITL cx1488 in P21/c #14 cx1488.res created by SHELXL-2017/1 at 13:03:58 on 22-Jan-2019 REM reset to P21/c #14 CELL 1.54178 13.8415 15.1909 16.21 90 109.352 90 ZERR 4 0.0012 0.0013 0.0014 0 0.0059 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H B Br I N O S UNIT 108 148 4 4 8 8 16 4 L.S. 4 0 0 PLAN 20 TEMP -173.18 BOND fmap 2 53 acta wpdb -2 conf REM REM REM WGHT 0.065900 9.579100 FVAR 0.06138 I1 5 -0.198341 0.417303 0.483756 11.00000 0.02265 0.03156 = 0.03334 0.00292 0.00067 -0.00025 I2 5 0.583426 0.197021 0.805451 11.00000 0.02888 0.04740 = 0.03417 -0.01143 0.00332 0.01471 BR1 4 0.280359 0.637642 1.002607 11.00000 0.04916 0.05225 = 0.03946 -0.02921 0.02101 -0.01268 O1 7 -0.044463 0.283377 0.367696 11.00000 0.06317 0.05869 = 0.04039 -0.00700 0.00707 -0.00710 O2 7 0.193536 0.241635 0.483734 11.00000 0.03645 0.01849 = 0.01382 -0.00274 0.00999 0.00197 O3 7 0.147325 0.135600 0.565246 11.00000 0.03853 0.02354 = 0.01672 0.00068 0.01272 0.00077 N1 6 0.093214 0.291586 0.576770 11.00000 0.02833 0.01865 = 0.01506 -0.00596 0.00817 -0.00221 N2 6 0.276165 0.247151 0.646421 11.00000 0.03053 0.02387 = 0.01503 -0.00068 0.00856 0.00744 C1 1 -0.002903 0.300834 0.520308 11.00000 0.02267 0.02711 = 0.01813 0.00208 0.00517 -0.00239 C2 1 -0.049547 0.373987 0.544955 11.00000 0.01504 0.02626 = 0.01413 0.00436 0.00011 0.00223 C3 1 0.019947 0.411997 0.619118 11.00000 0.02499 0.02158 = 0.01308 0.00189 0.00332 0.00056 C4 1 0.110600 0.358711 0.640014 11.00000 0.02840 0.01809 = 0.01361 0.00219 0.01217 -0.00217 C5 1 0.202888 0.365165 0.707192 11.00000 0.02749 0.01462 = 0.01400 0.00355 0.00993 -0.00009 C6 1 0.285881 0.309653 0.712076 11.00000 0.02584 0.02361 = 0.01291 0.00079 0.00826 0.00056 C7 1 0.384880 0.303723 0.774900 11.00000 0.02318 0.03000 = 0.01654 -0.00224 0.00835 0.00248 C8 1 0.433787 0.238330 0.744195 11.00000 0.02006 0.02906 = 0.01977 0.00521 0.00229 0.00713 C9 1 0.365634 0.203824 0.664914 11.00000 0.03133 0.02756 = 0.01532 0.00107 0.00867 0.00409 C10 1 -0.047262 0.241569 0.443903 11.00000 0.03529 0.03205 = 0.02071 -0.00309 0.00217 0.00015 AFIX 23 H10A 2 -0.007607 0.186083 0.452771 11.00000 -1.20000 H10B 2 -0.118909 0.226961 0.438144 11.00000 -1.20000 AFIX 0 C11 1 -0.096743 0.234019 0.291607 11.00000 0.08479 0.08543 = 0.04171 -0.01466 0.01266 -0.01823 AFIX 23 H11A 2 -0.170976 0.232884 0.282938 11.00000 -1.20000 H11B 2 -0.071293 0.172631 0.298570 11.00000 -1.20000 AFIX 0 C12 1 -0.079089 0.275269 0.213848 11.00000 0.07324 0.06879 = 0.05500 -0.00645 0.01976 0.00795 AFIX 137 H12A 2 -0.124059 0.247584 0.160267 11.00000 -1.50000 H12B 2 -0.007497 0.266818 0.217808 11.00000 -1.50000 H12C 2 -0.094164 0.338383 0.212613 11.00000 -1.50000 AFIX 0 C13 1 0.001881 0.493145 0.663936 11.00000 0.02655 0.02758 = 0.02038 0.00032 0.00686 0.00873 AFIX 137 H13A 2 0.019564 0.481641 0.726696 11.00000 -1.50000 H13B 2 -0.070415 0.509955 0.639692 11.00000 -1.50000 H13C 2 0.044640 0.541088 0.654830 11.00000 -1.50000 AFIX 0 C14 1 0.431692 0.354473 0.858595 11.00000 0.02617 0.04174 = 0.02765 -0.01322 -0.00206 0.00746 AFIX 137 H14A 2 0.450275 0.413650 0.845000 11.00000 -1.50000 H14B 2 0.493145 0.323834 0.895462 11.00000 -1.50000 H14C 2 0.382091 0.358928 0.889734 11.00000 -1.50000 AFIX 0 C15 1 0.384637 0.131618 0.609863 11.00000 0.03627 0.04323 = 0.02905 -0.00993 0.01084 0.01138 AFIX 137 H15A 2 0.372187 0.074657 0.632891 11.00000 -1.50000 H15B 2 0.455785 0.134370 0.610947 11.00000 -1.50000 H15C 2 0.338427 0.138380 0.549577 11.00000 -1.50000 AFIX 0 C16 1 0.212441 0.329577 0.465563 11.00000 0.04537 0.02757 = 0.02301 -0.00214 0.01502 0.00004 AFIX 23 H16A 2 0.274595 0.351587 0.511383 11.00000 -1.20000 H16B 2 0.153982 0.367165 0.465484 11.00000 -1.20000 AFIX 0 C17 1 0.226936 0.334119 0.378538 11.00000 0.05855 0.03374 = 0.03376 0.00292 0.02409 -0.00254 AFIX 137 H17A 2 0.167313 0.308319 0.334043 11.00000 -1.50000 H17B 2 0.288638 0.301288 0.380591 11.00000 -1.50000 H17C 2 0.234386 0.395736 0.363773 11.00000 -1.50000 AFIX 0 C18 1 0.128646 0.101677 0.640051 11.00000 0.08176 0.03358 = 0.03774 -0.00424 0.04125 -0.00932 AFIX 23 H18A 2 0.068470 0.131708 0.647264 11.00000 -1.20000 H18B 2 0.188510 0.113734 0.692715 11.00000 -1.20000 AFIX 0 C19 1 0.109792 0.006647 0.632013 11.00000 0.10983 0.03714 = 0.04638 0.00279 0.04898 -0.01297 AFIX 137 H19A 2 0.056140 -0.005996 0.576258 11.00000 -1.50000 H19B 2 0.087719 -0.013707 0.680310 11.00000 -1.50000 H19C 2 0.172906 -0.023921 0.634094 11.00000 -1.50000 AFIX 0 C20 1 0.217849 0.433599 0.776670 11.00000 0.01904 0.02418 = 0.01315 0.00084 0.00552 0.00288 C21 1 0.268834 0.510946 0.773991 11.00000 0.04199 0.02312 = 0.02403 -0.00676 0.02184 -0.01099 AFIX 43 H21 2 0.292112 0.522400 0.726102 11.00000 -1.20000 AFIX 0 C22 1 0.286227 0.571849 0.840587 11.00000 0.04040 0.02585 = 0.03311 -0.00645 0.02027 -0.01131 AFIX 43 H22 2 0.321099 0.625225 0.838487 11.00000 -1.20000 AFIX 0 C23 1 0.252705 0.554756 0.910121 11.00000 0.02765 0.03266 = 0.02137 -0.01131 0.00985 -0.00247 C24 1 0.201446 0.477835 0.914373 11.00000 0.02831 0.03239 = 0.01267 -0.00297 0.01145 -0.00045 AFIX 43 H24 2 0.178629 0.466564 0.962554 11.00000 -1.20000 AFIX 0 C25 1 0.183895 0.417237 0.846792 11.00000 0.02658 0.02004 = 0.02050 0.00574 0.01313 0.00045 AFIX 43 H25 2 0.148360 0.364148 0.848562 11.00000 -1.20000 AFIX 0 B1 3 0.176875 0.225311 0.565334 11.00000 0.02675 0.03037 = 0.01698 -0.00668 0.00776 0.00265 S1 8 0.518457 0.566258 0.375990 11.00000 0.05602 0.06359 = 0.08705 0.00742 0.02523 0.00101 O4 7 0.592574 0.507973 0.439140 11.00000 0.04959 0.05133 = 0.12219 -0.00434 0.00729 0.00281 AFIX 147 H4 2 0.566618 0.457798 0.437881 11.00000 -1.50000 AFIX 0 C26 1 0.398623 0.511505 0.342837 11.00000 0.05081 0.09561 = 0.08705 -0.01352 0.00200 0.00234 AFIX 137 H26A 2 0.379082 0.498186 0.394329 11.00000 -1.50000 H26B 2 0.403934 0.456597 0.312892 11.00000 -1.50000 H26C 2 0.346588 0.549456 0.302959 11.00000 -1.50000 AFIX 0 C27 1 0.484714 0.651966 0.437754 11.00000 0.08293 0.05069 = 0.10848 -0.00306 0.03164 0.00381 AFIX 137 H27A 2 0.543841 0.690590 0.463185 11.00000 -1.50000 H27B 2 0.464207 0.625731 0.484654 11.00000 -1.50000 H27C 2 0.427682 0.686344 0.399124 11.00000 -1.50000 AFIX 0 HKLF 4 REM cx1488 in P21/c #14 REM R1 = 0.0478 for 4410 Fo > 4sig(Fo) and 0.0595 for all 5323 data REM 352 parameters refined using 0 restraints END WGHT 0.0659 9.5690 REM Highest difference peak 2.078, deepest hole -1.035, 1-sigma level 0.144 Q1 1 0.2224 0.6650 0.9615 11.00000 0.05 2.08 Q2 1 0.6076 0.2461 0.7757 11.00000 0.05 1.75 Q3 1 -0.1790 0.3767 0.4549 11.00000 0.05 1.31 Q4 1 -0.1581 0.4542 0.4807 11.00000 0.05 1.05 Q5 1 0.5318 0.1541 0.7919 11.00000 0.05 0.94 Q6 1 0.5233 0.1901 0.8265 11.00000 0.05 0.90 Q7 1 0.4999 0.5039 0.3987 11.00000 0.05 0.80 Q8 1 -0.2402 0.4506 0.4631 11.00000 0.05 0.76 Q9 1 0.6031 0.5329 0.3767 11.00000 0.05 0.73 Q10 1 -0.2558 0.3997 0.4973 11.00000 0.05 0.56 Q11 1 -0.0055 0.4170 0.5548 11.00000 0.05 0.55 Q12 1 0.5012 0.2324 0.7627 11.00000 0.05 0.53 Q13 1 0.4184 0.5334 0.2813 11.00000 0.05 0.51 Q14 1 0.6567 0.2368 0.8549 11.00000 0.05 0.49 Q15 1 0.4396 0.0473 0.6756 11.00000 0.05 0.48 Q16 1 0.4649 0.5607 0.4160 11.00000 0.05 0.47 Q17 1 0.4546 0.1172 0.6677 11.00000 0.05 0.45 Q18 1 0.6371 0.1855 0.7688 11.00000 0.05 0.44 Q19 1 0.6344 0.1605 0.8036 11.00000 0.05 0.44 Q20 1 0.4421 0.1752 0.7404 11.00000 0.05 0.43 ; _shelx_res_checksum 73327 _shelx_hkl_file ; -1 0 0 11.29 1.12 -1 0 0 11.32 1.07 -1 0 0 9.81 1.02 1 0 0 10.09 1.10 1 0 0 8.92 1.01 2 0 0 86.03 8.04 -2 0 0 85.65 8.04 2 0 0 77.91 8.12 -2 0 0 80.42 8.10 3 0 0 116.49 11.54 -3 0 0 120.55 11.64 -3 0 0 122.17 11.55 3 0 0 115.43 11.65 4 0 0 36.28 4.01 -4 0 0 40.45 3.98 -4 0 0 37.47 3.81 -5 0 0 344.24 33.76 5 0 0 349.37 33.78 6 0 0 84.33 8.03 -6 0 0 73.58 8.17 -6 0 0 78.46 7.96 7 0 0 18.98 2.53 -7 0 0 21.42 2.41 -7 0 0 18.44 2.56 -7 0 0 16.48 2.10 -8 0 0 65.79 6.97 8 0 0 69.48 7.29 -8 0 0 74.44 7.20 -9 0 0 12.86 2.03 -9 0 0 12.36 1.65 9 0 0 10.94 2.30 -9 0 0 10.14 1.73 -9 0 0 13.36 2.06 -10 0 0 153.51 16.20 -10 0 0 171.22 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80.37 9.65 -5 -8 0 88.01 8.98 -5 -8 0 93.09 8.90 -6 8 0 3.05 1.01 6 8 0 2.80 1.66 6 -8 0 3.36 1.36 -6 -8 0 1.99 0.91 6 -8 0 1.51 1.21 -6 -8 0 3.26 1.09 -6 -8 0 4.07 1.63 -6 -8 0 2.20 1.30 -6 -8 0 4.38 1.30 -7 8 0 4.17 1.15 7 8 0 4.15 1.98 -7 -8 0 4.97 1.96 7 -8 0 5.99 1.68 -7 -8 0 2.44 1.43 -7 -8 0 5.08 1.58 -7 -8 0 3.47 1.11 -7 -8 0 4.25 1.05 7 -8 0 4.32 1.47 -8 8 0 9.29 1.67 8 8 0 13.06 2.80 -8 8 0 9.80 1.94 -8 -8 0 14.77 1.92 -8 -8 0 10.75 1.79 -8 -8 0 14.72 3.10 8 -8 0 8.18 2.07 -9 8 0 11.75 1.85 -9 8 0 10.43 1.92 9 8 0 11.87 2.74 -9 8 0 9.24 1.58 -9 8 0 9.63 1.64 9 -8 0 8.93 2.09 -9 -8 0 8.64 1.57 -9 -8 0 7.45 2.13 10 8 0 13.82 2.98 -10 8 0 12.30 2.01 -10 8 0 10.00 1.97 -10 8 0 11.89 1.84 -10 8 0 11.35 1.99 -10 -8 0 13.00 2.95 -10 -8 0 16.40 2.05 10 -8 0 11.22 2.40 -11 8 0 7.52 1.53 -11 8 0 5.18 1.26 11 8 0 9.08 2.29 -11 8 0 9.96 1.60 -11 8 0 8.11 1.39 -11 -8 0 8.46 1.60 11 -8 0 7.73 1.74 12 8 0 9.65 2.14 -12 8 0 7.17 1.44 -12 8 0 7.91 1.52 -12 8 0 8.53 1.48 -12 8 0 7.99 1.34 -12 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0 21.58 4.38 -4 -10 0 25.52 3.38 4 -10 0 21.81 3.16 -4 -10 0 24.76 3.14 4 -10 0 22.20 2.98 5 10 0 81.04 9.33 -5 10 0 98.65 9.00 -5 -10 0 82.52 9.15 5 -10 0 97.20 9.16 5 -10 0 77.96 10.29 -5 -10 0 69.40 8.93 5 -10 0 98.20 9.00 -5 -10 0 92.29 9.28 -5 -10 0 79.32 8.81 -6 10 0 7.22 1.49 6 10 0 5.64 1.94 -6 -10 0 5.99 2.78 6 -10 0 5.73 1.51 -6 -10 0 5.53 1.27 6 -10 0 5.00 1.05 -6 -10 0 3.47 1.63 -7 10 0 0.77 0.84 7 10 0 0.84 1.72 7 -10 0 0.69 0.77 7 -10 0 2.17 1.30 -7 -10 0 0.96 1.00 -7 -10 0 2.34 1.63 8 10 0 9.26 2.64 -8 10 0 7.76 1.62 -8 10 0 9.63 1.48 -8 -10 0 5.93 2.25 8 -10 0 8.41 1.87 -8 -10 0 7.93 1.54 9 10 0 3.14 2.40 -9 10 0 2.52 1.10 -9 10 0 2.21 0.85 -9 10 0 2.34 1.01 -9 -10 0 1.11 0.95 9 -10 0 2.61 1.29 9 -10 0 3.45 2.33 -9 -10 0 0.84 1.50 -10 10 0 17.01 2.44 -10 10 0 20.05 2.67 -10 10 0 24.23 2.56 10 10 0 14.58 3.22 10 -10 0 25.83 2.83 -10 -10 0 16.71 3.44 -10 -10 0 18.83 2.57 11 10 0 6.13 1.98 -11 10 0 5.18 1.14 -11 10 0 3.32 1.16 -11 10 0 4.78 1.02 -11 -10 0 4.57 1.05 -12 10 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0.82 -7 -4 18 4.84 0.84 -7 -4 18 3.95 1.13 -8 4 18 0.46 0.56 -8 -4 18 0.44 0.92 -4 -5 18 1.32 0.61 -4 -5 18 -0.65 1.04 -4 -5 18 1.61 0.92 -5 -5 18 1.52 0.95 -5 -5 18 1.56 1.15 -5 -5 18 2.36 0.68 -6 -5 18 1.25 1.04 -6 -5 18 -0.01 0.55 -6 -5 18 -1.00 0.93 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 15954 _olex2_date_sample_data_collection 2019-01-18 _olex2_date_sample_submission 2019-01-17 _olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems' _olex2_exptl_crystal_mounting_method 'The crystal was mounted on a MITIGEN holder with Paratone oil' _olex2_submission_original_sample_id cx1488 _olex2_submission_special_instructions 'No special instructions were received'