#============================================================================== data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 12 _journal_issue 2 _journal_year 2021 _journal_page_first 179 _journal_page_last 186 #============================================================================== data_rb19036_twin1_hklf4 _audit_creation_date 2021-03-15 _audit_creation_method ; Olex2 1.3-ac4 (compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032) ; _shelx_SHELXL_version_number '2018/3' _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. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C21 H21 N4 S, 0.415(S12), 3(I3), 2(I2)' _chemical_formula_sum 'C21 H21 I13 N4 S5.98' _chemical_formula_weight 2170.84 _chemical_melting_point ? _chemical_oxdiff_formula C40H42N10S14I26 _chemical_oxdiff_usercomment 'Ibukun, dark red needles.' 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' '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' '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 7.5627(5) _cell_length_b 30.6764(19) _cell_length_c 20.8848(15) _cell_angle_alpha 90 _cell_angle_beta 91.632(6) _cell_angle_gamma 90 _cell_volume 4843.2(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6209 _cell_measurement_temperature 100.01(10) _cell_measurement_theta_max 77.6350 _cell_measurement_theta_min 3.5190 _shelx_estimated_absorpt_T_max 0.375 _shelx_estimated_absorpt_T_min 0.036 _exptl_absorpt_coefficient_mu 67.840 _exptl_absorpt_correction_T_max 0.462 _exptl_absorpt_correction_T_min 0.023 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.67a (Rigaku Oxford Diffraction, 2020) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'metallic dark violet' _exptl_crystal_colour_lustre metallic _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary violet _exptl_crystal_density_diffrn 2.977 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description needle _exptl_crystal_F_000 3839 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 0 0.0112 0 -1 0 0.0080 0 10 11 0.0165 0 -1 -1 0.0014 1 0 0 0.0807 -1 0 0 0.0655 _exptl_crystal_size_max 0.147 _exptl_crystal_size_mid 0.035 _exptl_crystal_size_min 0.018 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0.0019 0.9981 0.0211 -0.0136 0.0163 0.0455 -0.0019 -0.9981 -0.0211 0.0136 -0.0163 -0.0455 -0.0023 10.4825 11.2341 -0.9171 -0.0425 0.3496 0.0002 -0.9530 -1.0213 0.0834 0.0039 -0.0318 1.0014 -0.0388 0.0187 0.0326 -0.1865 0.0767 -1.0014 0.0388 -0.0187 -0.0326 0.1865 -0.0767 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_unetI/netI 0.0607 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.960 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 17906 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.960 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 81.470 _diffrn_reflns_theta_min 3.576 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.01(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 5.8140 _diffrn_detector_type 'Pilatus 200K' _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.960 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -42.00 25.00 0.50 6.17 -- -38.50 57.00 -30.00 134 2 \w -42.00 -6.00 0.50 6.17 -- -38.50 77.00 120.00 72 3 \w -89.00 -6.00 0.50 6.17 -- -38.50 125.00-180.00 166 4 \w -93.00 -67.00 0.50 6.17 -- -38.50 -37.00-150.00 52 5 \w -101.00 -27.00 0.50 6.17 -- -38.50 -57.00 30.00 148 6 \w -103.00 -49.00 0.50 6.17 -- -38.50 -37.00 120.00 108 7 \w 127.00 174.00 0.50 24.67 -- 111.00 50.00 0.00 94 8 \w 79.00 117.00 0.50 24.67 -- 111.00 -50.00-120.00 76 9 \w 42.00 68.00 0.50 24.67 -- 111.00 -12.00 0.00 52 10 \w 48.00 101.00 0.50 24.67 -- 111.00 -63.00 -30.00 106 11 \w 129.00 155.00 0.50 24.67 -- 111.00 37.00 150.00 52 12 \w 59.00 114.00 0.50 24.67 -- 111.00 -50.00 120.00 110 13 \w 69.00 103.00 0.50 24.67 -- 111.00 -37.00 60.00 68 14 \w 103.00 134.00 0.50 24.67 -- 111.00 111.00 90.00 62 15 \w 48.00 114.00 0.50 24.67 -- 111.00 -50.00 60.00 132 16 \w 96.00 125.00 0.50 24.67 -- 111.00 -63.00 60.00 58 17 \w 110.00 175.00 0.50 24.67 -- 111.00 50.00 90.00 130 18 \w 105.00 131.00 0.50 24.67 -- 111.00 -77.00 30.00 52 19 \w 48.00 106.00 0.50 24.67 -- 111.00 -37.00 -60.00 116 20 \w 46.00 74.00 0.50 24.67 -- 111.00 -37.00-150.00 56 21 \w 80.00 107.00 0.50 24.67 -- 111.00 -37.00-150.00 54 22 \w 42.00 101.00 0.50 24.67 -- 111.00 -25.00 30.00 118 23 \w 98.00 142.00 0.50 24.67 -- 111.00 63.00-150.00 88 24 \w 147.00 174.00 0.50 24.67 -- 111.00 63.00-150.00 54 25 \w 91.00 117.00 0.50 24.67 -- 111.00 -91.00 60.00 52 26 \w 83.00 145.00 0.50 24.67 -- 111.00 0.00 -90.00 124 27 \w 56.00 81.00 0.50 24.67 -- 111.00 -77.00-150.00 50 28 \w 104.00 129.00 0.50 24.67 -- 111.00 -77.00-150.00 50 29 \w 64.00 116.00 0.50 24.67 -- 111.00 -63.00 30.00 104 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Pilatus 200K' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0333734000 _diffrn_orient_matrix_UB_12 -0.0122272000 _diffrn_orient_matrix_UB_13 -0.0702213000 _diffrn_orient_matrix_UB_21 -0.1851568000 _diffrn_orient_matrix_UB_22 0.0170699000 _diffrn_orient_matrix_UB_23 -0.0197512000 _diffrn_orient_matrix_UB_31 0.0785435000 _diffrn_orient_matrix_UB_32 0.0456844000 _diffrn_orient_matrix_UB_33 -0.0114902000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 11295 _reflns_number_total 17906 _reflns_special_details ; _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. Completness statistics refer to single and composite reflections containing twin component 1 only. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.41.67a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.41.67a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.41.67a (Rigaku OD, 2020)' _computing_molecular_graphics 'Olex2 1.3-ac4 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-ac4 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _refine_diff_density_max 3.370 _refine_diff_density_min -3.073 _refine_diff_density_rms 0.579 _refine_ls_extinction_coef 0.00028(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 412 _refine_ls_number_reflns 17906 _refine_ls_number_restraints 192 _refine_ls_R_factor_all 0.1903 _refine_ls_R_factor_gt 0.1366 _refine_ls_restrained_S_all 1.034 _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^)+(0.1547P)^2^+453.6557P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3464 _refine_ls_wR_factor_ref 0.3926 _refine_special_details ; Refined as a 2-component twin. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.563(3) 0.437(3) 2. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 3. Uiso/Uaniso restraints and constraints Uanis(C8) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(S1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(S1E) \\sim Ueq, Uanis(S6E) \\sim Ueq, Uanis(S3E) \\sim Ueq, Uanis(S2E) \\sim Ueq, Uanis(S5E) \\sim Ueq, Uanis(S4E) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 4. Others Sof(S1E)=Sof(S2E)=Sof(S3E)=Sof(S4E)=Sof(S5E)=Sof(S6E)=FVAR(1) 5.a Aromatic/amide H refined with riding coordinates: C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19), C20(H20) 5.b Idealised Me refined as rotating group: C9(H9A,H9B,H9C), C15(H15A,H15B,H15C), C21(H21A,H21B,H21C) ; _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 S1 S 0.7294(15) 0.8930(3) 0.4816(5) 0.057(2) Uani 1 1 d . U . . . N1 N 0.895(4) 0.8468(10) 0.5712(16) 0.050(7) Uani 1 1 d . U . . . N2 N 0.806(5) 0.9846(12) 0.6957(17) 0.060(8) Uani 1 1 d . U . . . N3 N 0.659(4) 0.7902(10) 0.2805(14) 0.046(7) Uani 1 1 d . U . . . N4 N 1.095(4) 0.6952(10) 0.5304(15) 0.048(7) Uani 1 1 d . U . . . C1 C 0.819(5) 0.8868(11) 0.5577(15) 0.041(7) Uani 1 1 d . U . . . C2 C 0.797(5) 0.8431(12) 0.4652(17) 0.049(8) Uani 1 1 d . U . . . C3 C 0.886(5) 0.8229(11) 0.5129(16) 0.042(7) Uani 1 1 d . U . . . C4 C 0.815(5) 0.9197(10) 0.6062(15) 0.039(7) Uani 1 1 d . U . . . C5 C 0.875(5) 0.9138(13) 0.6678(19) 0.053(9) Uani 1 1 d . U . . . H5 H 0.920721 0.886263 0.680598 0.064 Uiso 1 1 calc R U . . . C6 C 0.869(7) 0.9460(16) 0.710(2) 0.069(12) Uani 1 1 d . U . . . H6 H 0.912041 0.940801 0.752728 0.083 Uiso 1 1 calc R U . . . C7 C 0.738(6) 0.9916(15) 0.635(2) 0.060(10) Uani 1 1 d . U . . . H7 H 0.690439 1.019389 0.624383 0.072 Uiso 1 1 calc R U . . . C8 C 0.737(5) 0.9597(14) 0.592(2) 0.055(9) Uani 1 1 d . U . . . H8 H 0.683451 0.964348 0.550530 0.066 Uiso 1 1 calc R U . . . C9 C 0.808(6) 1.0232(15) 0.741(2) 0.069(11) Uani 1 1 d . U . . . H9A H 0.759917 1.048910 0.718837 0.103 Uiso 1 1 calc R U . . . H9B H 0.929779 1.029114 0.755885 0.103 Uiso 1 1 calc R U . . . H9C H 0.735452 1.016579 0.778066 0.103 Uiso 1 1 calc R U . . . C10 C 0.745(5) 0.8230(13) 0.4002(19) 0.053(9) Uani 1 1 d . U . . . C11 C 0.770(4) 0.8491(12) 0.3439(16) 0.043(7) Uani 1 1 d . U . . . H11 H 0.819515 0.877503 0.347471 0.052 Uiso 1 1 calc R U . . . C12 C 0.719(5) 0.8317(13) 0.2824(18) 0.049(8) Uani 1 1 d . U . . . H12 H 0.727768 0.848693 0.244558 0.059 Uiso 1 1 calc R U . . . C13 C 0.631(6) 0.7665(14) 0.3351(19) 0.056(9) Uani 1 1 d . U . . . H13 H 0.576467 0.738761 0.331279 0.067 Uiso 1 1 calc R U . . . C14 C 0.678(5) 0.7808(11) 0.3922(17) 0.042(7) Uani 1 1 d . U . . . H14 H 0.666037 0.762358 0.428392 0.050 Uiso 1 1 calc R U . . . C15 C 0.611(5) 0.7716(12) 0.2156(19) 0.049(8) Uani 1 1 d . U . . . H15A H 0.545891 0.793471 0.190263 0.073 Uiso 1 1 calc R U . . . H15B H 0.537587 0.745664 0.220701 0.073 Uiso 1 1 calc R U . . . H15C H 0.719537 0.763652 0.193663 0.073 Uiso 1 1 calc R U . . . C16 C 0.961(5) 0.7781(12) 0.5184(17) 0.044(7) Uani 1 1 d . U . . . C17 C 1.032(5) 0.7557(13) 0.4650(19) 0.051(8) Uani 1 1 d . U . . . H17 H 1.028189 0.769642 0.424379 0.061 Uiso 1 1 calc R U . . . C18 C 1.104(5) 0.7161(12) 0.4699(17) 0.046(8) Uani 1 1 d . U . . . H18 H 1.157770 0.702490 0.434556 0.055 Uiso 1 1 calc R U . . . C19 C 1.041(5) 0.7138(13) 0.580(2) 0.053(9) Uani 1 1 d . U . . . H19 H 1.039535 0.698685 0.619969 0.064 Uiso 1 1 calc R U . . . C20 C 0.983(5) 0.7570(13) 0.5762(19) 0.050(8) Uani 1 1 d . U . . . H20 H 0.957583 0.772306 0.614463 0.061 Uiso 1 1 calc R U . . . C21 C 1.154(5) 0.6497(12) 0.5328(19) 0.049(8) Uani 1 1 d . U . . . H21A H 1.055919 0.630561 0.519616 0.073 Uiso 1 1 calc R U . . . H21B H 1.193550 0.642391 0.576604 0.073 Uiso 1 1 calc R U . . . H21C H 1.252390 0.645701 0.503764 0.073 Uiso 1 1 calc R U . . . I7 I 0.6180(3) 0.67604(8) 0.48356(12) 0.0531(6) Uani 1 1 d . . . . . I12 I 0.4829(3) 0.76291(9) 0.56317(12) 0.0553(6) Uani 1 1 d . . . A 1 I13 I 0.4021(4) 0.83472(10) 0.63615(14) 0.0646(7) Uani 1 1 d . . . A 1 S1E S 0.239(2) 0.5234(5) 0.4262(7) 0.069(4) Uani 0.83(2) 1 d . U P . . S2E S 0.374(2) 0.5524(5) 0.5024(7) 0.071(4) Uani 0.83(2) 1 d . U P . . S3E S 0.231(2) 0.5392(5) 0.5807(7) 0.070(4) Uani 0.83(2) 1 d . U P . . S4E S 0.308(2) 0.4788(6) 0.6100(9) 0.083(5) Uani 0.83(2) 1 d . U P . . S5E S 0.152(2) 0.4353(5) 0.5591(8) 0.076(4) Uani 0.83(2) 1 d . U P . . S6E S -0.071(2) 0.4290(5) 0.6091(7) 0.071(4) Uani 0.83(2) 1 d . U P . . I4 I 0.2550(4) 0.61683(10) -0.08644(14) 0.0661(8) Uani 1 1 d . . . B 1 I5 I 0.2515(4) 0.55991(9) 0.01993(12) 0.0577(6) Uani 1 1 d . . . B 1 I6 I 0.2479(4) 0.49443(9) 0.13270(12) 0.0582(7) Uani 1 1 d . . . B 1 I1 I 1.2352(4) 0.85140(10) 0.23217(14) 0.0620(7) Uani 1 1 d . . . . . I2 I 1.1178(3) 0.76256(9) 0.26817(12) 0.0536(6) Uani 1 1 d . . . . . I3 I 0.9687(4) 0.67869(9) 0.29867(13) 0.0611(7) Uani 1 1 d . . . . . I8 I 0.6730(4) 0.61338(9) 0.60445(12) 0.0574(6) Uani 1 1 d . . . . . I9 I 0.7068(4) 0.55786(9) 0.70996(14) 0.0641(7) Uani 1 1 d . . . . . I10 I 0.4876(4) 0.62461(11) 0.34102(17) 0.0730(8) Uani 1 1 d . . . . . I11 I 0.3737(4) 0.57099(9) 0.24188(13) 0.0610(7) Uani 1 1 d . . . . . 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 S1 0.063(6) 0.058(5) 0.049(5) 0.005(4) -0.001(4) -0.006(4) N1 0.048(11) 0.049(11) 0.055(12) 0.002(9) 0.016(10) -0.012(9) N2 0.054(12) 0.069(13) 0.056(12) -0.004(10) 0.006(10) 0.006(10) N3 0.042(11) 0.054(11) 0.043(11) 0.006(9) -0.004(9) -0.003(9) N4 0.043(11) 0.053(11) 0.048(11) 0.001(9) 0.001(9) 0.005(9) C1 0.044(12) 0.044(11) 0.036(11) 0.015(9) 0.003(9) 0.003(10) C2 0.052(13) 0.050(12) 0.044(12) 0.005(10) 0.002(10) -0.002(10) C3 0.039(11) 0.043(11) 0.042(11) -0.007(9) 0.008(9) -0.002(9) C4 0.043(12) 0.038(11) 0.038(11) 0.003(9) 0.003(9) -0.006(9) C5 0.052(13) 0.055(13) 0.051(13) 0.003(10) -0.005(10) -0.001(11) C6 0.069(16) 0.071(15) 0.068(15) 0.002(11) -0.002(11) -0.004(12) C7 0.056(14) 0.061(14) 0.063(14) 0.005(11) -0.007(11) 0.000(11) C8 0.048(13) 0.063(14) 0.055(13) 0.003(11) -0.003(10) 0.005(11) C9 0.06(2) 0.063(19) 0.08(2) -0.019(17) 0.012(17) 0.009(16) C10 0.052(13) 0.057(13) 0.049(13) -0.002(10) 0.001(10) -0.001(11) C11 0.036(11) 0.049(12) 0.045(12) -0.003(10) 0.006(10) -0.005(10) C12 0.046(12) 0.054(13) 0.046(12) 0.003(10) 0.000(10) 0.001(10) C13 0.055(14) 0.059(13) 0.053(13) -0.002(11) -0.006(11) 0.004(11) C14 0.043(12) 0.039(11) 0.045(12) -0.002(9) 0.007(10) 0.000(9) C15 0.032(14) 0.045(15) 0.069(18) 0.001(14) 0.011(13) -0.008(12) C16 0.040(12) 0.045(12) 0.047(12) 0.001(10) 0.002(10) -0.002(10) C17 0.049(13) 0.054(13) 0.049(12) 0.002(10) 0.000(10) -0.003(10) C18 0.042(12) 0.053(12) 0.043(12) -0.005(10) 0.011(10) 0.002(10) C19 0.053(13) 0.054(13) 0.052(13) 0.004(10) 0.002(10) -0.003(11) C20 0.045(13) 0.052(13) 0.055(13) -0.005(10) 0.003(10) 0.000(10) C21 0.043(16) 0.048(16) 0.056(17) 0.005(14) 0.012(13) 0.006(13) I7 0.0547(14) 0.0581(14) 0.0465(12) 0.0008(10) 0.0027(10) -0.0055(10) I12 0.0458(13) 0.0753(16) 0.0446(12) 0.0038(11) 0.0006(9) -0.0071(11) I13 0.0616(16) 0.0662(16) 0.0664(16) 0.0059(12) 0.0095(12) 0.0009(12) S1E 0.070(8) 0.072(7) 0.065(7) -0.010(6) 0.004(6) 0.000(6) S2E 0.072(8) 0.071(7) 0.069(7) 0.001(6) 0.000(6) 0.002(6) S3E 0.070(8) 0.067(7) 0.072(7) 0.006(6) 0.008(6) -0.007(6) S4E 0.081(9) 0.082(8) 0.084(8) 0.006(7) 0.004(7) -0.002(7) S5E 0.077(8) 0.082(8) 0.070(7) -0.011(6) -0.006(6) -0.002(6) S6E 0.067(7) 0.075(7) 0.070(7) 0.002(6) 0.004(6) 0.005(6) I4 0.0536(15) 0.0787(18) 0.0663(16) 0.0149(13) 0.0071(12) 0.0090(13) I5 0.0561(15) 0.0633(15) 0.0540(13) -0.0024(11) 0.0063(10) 0.0059(11) I6 0.0625(16) 0.0639(15) 0.0484(13) -0.0001(10) 0.0062(11) 0.0002(12) I1 0.0564(15) 0.0667(16) 0.0630(15) -0.0089(12) 0.0024(11) -0.0015(12) I2 0.0427(12) 0.0713(16) 0.0467(12) -0.0077(10) 0.0009(9) 0.0024(10) I3 0.0622(16) 0.0664(16) 0.0548(14) -0.0063(11) 0.0022(11) 0.0000(12) I8 0.0585(15) 0.0648(15) 0.0490(13) -0.0042(11) 0.0023(10) -0.0035(11) I9 0.0658(17) 0.0620(15) 0.0646(16) 0.0047(12) 0.0027(12) -0.0006(12) I10 0.0621(18) 0.0701(18) 0.086(2) 0.0047(15) -0.0055(14) -0.0082(14) I11 0.0520(14) 0.0687(16) 0.0623(15) 0.0120(12) 0.0022(11) -0.0008(12) _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 S1 C1 1.72(3) . ? S1 C2 1.65(4) . ? N1 C1 1.38(5) . ? N1 C3 1.42(5) . ? N2 C6 1.31(6) . ? N2 C7 1.36(5) . ? N2 C9 1.52(5) . ? N3 C12 1.35(5) . ? N3 C13 1.37(5) . ? N3 C15 1.50(5) . ? N4 C18 1.42(5) . ? N4 C19 1.27(5) . ? N4 C21 1.47(5) . ? C1 C4 1.43(5) . ? C2 C3 1.34(5) . ? C2 C10 1.53(5) . ? C3 C16 1.49(5) . ? C4 C5 1.36(5) . ? C4 C8 1.39(5) . ? C5 H5 0.9500 . ? C5 C6 1.33(6) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C7 C8 1.34(6) . ? C8 H8 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.44(5) . ? C10 C14 1.40(5) . ? C11 H11 0.9500 . ? C11 C12 1.43(5) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C13 C14 1.31(5) . ? C14 H14 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.43(5) . ? C16 C20 1.38(5) . ? C17 H17 0.9500 . ? C17 C18 1.33(5) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C19 C20 1.40(5) . ? C20 H20 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? I12 I13 2.757(4) . ? S1E S2E 2.06(2) . ? S1E S6E 2.06(2) 3_566 ? S2E S3E 2.03(2) . ? S3E S4E 2.03(2) . ? S4E S5E 2.06(2) . ? S5E S6E 2.02(2) . ? I4 I5 2.826(4) . ? I5 I6 3.096(4) . ? I1 I2 2.970(4) . ? I2 I3 2.888(4) . ? I8 I9 2.791(4) . ? I10 I11 2.763(5) . ? 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 C2 S1 C1 88.4(18) . . ? C1 N1 C3 106(3) . . ? C6 N2 C7 119(4) . . ? C6 N2 C9 124(4) . . ? C7 N2 C9 117(4) . . ? C12 N3 C13 122(3) . . ? C12 N3 C15 117(3) . . ? C13 N3 C15 121(3) . . ? C18 N4 C21 116(3) . . ? C19 N4 C18 124(3) . . ? C19 N4 C21 120(3) . . ? N1 C1 S1 116(3) . . ? N1 C1 C4 120(3) . . ? C4 C1 S1 124(2) . . ? C3 C2 S1 115(3) . . ? C3 C2 C10 126(4) . . ? C10 C2 S1 119(3) . . ? N1 C3 C16 114(3) . . ? C2 C3 N1 114(3) . . ? C2 C3 C16 132(3) . . ? C5 C4 C1 124(3) . . ? C5 C4 C8 117(3) . . ? C8 C4 C1 119(3) . . ? C4 C5 H5 119.5 . . ? C6 C5 C4 121(4) . . ? C6 C5 H5 119.5 . . ? N2 C6 C5 122(5) . . ? N2 C6 H6 118.8 . . ? C5 C6 H6 118.8 . . ? N2 C7 H7 119.7 . . ? C8 C7 N2 121(4) . . ? C8 C7 H7 119.7 . . ? C4 C8 H8 119.9 . . ? C7 C8 C4 120(4) . . ? C7 C8 H8 119.9 . . ? N2 C9 H9A 109.5 . . ? N2 C9 H9B 109.5 . . ? N2 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C2 118(3) . . ? C14 C10 C2 124(3) . . ? C14 C10 C11 118(3) . . ? C10 C11 H11 120.5 . . ? C12 C11 C10 119(3) . . ? C12 C11 H11 120.5 . . ? N3 C12 C11 117(3) . . ? N3 C12 H12 121.3 . . ? C11 C12 H12 121.3 . . ? N3 C13 H13 118.7 . . ? C14 C13 N3 123(4) . . ? C14 C13 H13 118.7 . . ? C10 C14 H14 119.9 . . ? C13 C14 C10 120(4) . . ? C13 C14 H14 119.9 . . ? N3 C15 H15A 109.5 . . ? N3 C15 H15B 109.5 . . ? N3 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C3 122(3) . . ? C20 C16 C3 122(3) . . ? C20 C16 C17 115(3) . . ? C16 C17 H17 118.6 . . ? C18 C17 C16 123(4) . . ? C18 C17 H17 118.6 . . ? N4 C18 H18 121.6 . . ? C17 C18 N4 117(3) . . ? C17 C18 H18 121.6 . . ? N4 C19 H19 120.5 . . ? N4 C19 C20 119(4) . . ? C20 C19 H19 120.5 . . ? C16 C20 C19 122(4) . . ? C16 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? N4 C21 H21A 109.5 . . ? N4 C21 H21B 109.5 . . ? N4 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? S6E S1E S2E 104.9(9) 3_566 . ? S3E S2E S1E 105.8(9) . . ? S2E S3E S4E 105.6(10) . . ? S3E S4E S5E 106.2(11) . . ? S6E S5E S4E 105.6(10) . . ? S5E S6E S1E 105.3(9) . 3_566 ? I4 I5 I6 177.70(13) . . ? I3 I2 I1 174.27(13) . . ? 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 S1 C1 C4 C5 175(3) . . . . ? S1 C1 C4 C8 -1(5) . . . . ? S1 C2 C3 N1 5(4) . . . . ? S1 C2 C3 C16 177(3) . . . . ? S1 C2 C10 C11 48(5) . . . . ? S1 C2 C10 C14 -133(4) . . . . ? N1 C1 C4 C5 -4(5) . . . . ? N1 C1 C4 C8 -180(3) . . . . ? N1 C3 C16 C17 -153(3) . . . . ? N1 C3 C16 C20 20(5) . . . . ? N2 C7 C8 C4 -4(7) . . . . ? N3 C13 C14 C10 6(6) . . . . ? N4 C19 C20 C16 9(6) . . . . ? C1 S1 C2 C3 -2(3) . . . . ? C1 S1 C2 C10 175(3) . . . . ? C1 N1 C3 C2 -5(4) . . . . ? C1 N1 C3 C16 -179(3) . . . . ? C1 C4 C5 C6 179(4) . . . . ? C1 C4 C8 C7 -178(4) . . . . ? C2 S1 C1 N1 -2(3) . . . . ? C2 S1 C1 C4 179(3) . . . . ? C2 C3 C16 C17 34(6) . . . . ? C2 C3 C16 C20 -153(4) . . . . ? C2 C10 C11 C12 -179(3) . . . . ? C2 C10 C14 C13 178(4) . . . . ? C3 N1 C1 S1 4(4) . . . . ? C3 N1 C1 C4 -177(3) . . . . ? C3 C2 C10 C11 -136(4) . . . . ? C3 C2 C10 C14 42(6) . . . . ? C3 C16 C17 C18 178(4) . . . . ? C3 C16 C20 C19 175(4) . . . . ? C4 C5 C6 N2 0(7) . . . . ? C5 C4 C8 C7 6(6) . . . . ? C6 N2 C7 C8 -1(7) . . . . ? C7 N2 C6 C5 2(7) . . . . ? C8 C4 C5 C6 -5(6) . . . . ? C9 N2 C6 C5 -176(4) . . . . ? C9 N2 C7 C8 177(4) . . . . ? C10 C2 C3 N1 -171(3) . . . . ? C10 C2 C3 C16 1(7) . . . . ? C10 C11 C12 N3 -4(5) . . . . ? C11 C10 C14 C13 -3(6) . . . . ? C12 N3 C13 C14 -7(6) . . . . ? C13 N3 C12 C11 6(5) . . . . ? C14 C10 C11 C12 3(5) . . . . ? C15 N3 C12 C11 -178(3) . . . . ? C15 N3 C13 C14 177(4) . . . . ? C16 C17 C18 N4 4(6) . . . . ? C17 C16 C20 C19 -11(6) . . . . ? C18 N4 C19 C20 1(6) . . . . ? C19 N4 C18 C17 -8(6) . . . . ? C20 C16 C17 C18 4(6) . . . . ? C21 N4 C18 C17 173(3) . . . . ? C21 N4 C19 C20 -179(4) . . . . ? _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL rb19036_twin1_hklf4_a.res in P2(1)/c rb19036_twin1_hklf4.res created by SHELXL-2018/3 at 16:37:33 on 15-Mar-2021 REM Old TITL RB19036_twin1_hklf4 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.227, Rweak 0.059, Alpha 0.077 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C18 C6 S7 I13 CELL 1.54184 7.5627 30.6764 20.8848 90 91.632 90 ZERR 4 0.0005 0.0019 0.0015 0 0.006 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H I N S UNIT 84 84 52 16 23.92 EQIV $1 1+X,+Y,+Z EQIV $2 2-X,0.5+Y,1.5-Z EQIV $3 +X,1.5-Y,-0.5+Z EQIV $4 1-X,0.5+Y,1.5-Z EQIV $5 1-X,1-Y,1-Z EQIV $6 +X,1.5-Y,0.5+Z ISOR 0.01 0.02 C8 C6 N1 C2 N3 C7 C4 C10 C21 C17 N2 C18 C20 C1 C15 C12 C19 = C9 C5 C16 N4 C13 C3 C11 C14 S1 ISOR 0.01 0.02 S1E S6E S3E S2E S5E S4E L.S. 30 PLAN 5 SIZE 0.018 0.035 0.147 TEMP -173.14(10) CONF RTAB BOND I7 I8 RTAB BOND I7 I10 RTAB BOND I7 I12 RTAB BOND I7 H14 RTAB BOND H21c I7_$1 RTAB BOND H9b I9_$2 RTAB BOND H12 I9_$3 RTAB BOND C15 I12_$3 RTAB BOND H9c S4E_$4 RTAB BOND I8 S2E RTAB BOND I9 I6_$5 RTAB BOND I13 I11_$6 RTAB BOND I10 S4E_$5 RTAB BOND I6 I11 MPLA 4 C5 > C8 C4 C1 N2 C9 MPLA 4 C11 > C14 C10 C2 N3 C15 MPLA 4 C17 > C20 C16 C3 N4 C21 MPLA 5 S1 N1 C1 C2 C3 MPLA 6 C4 > C8 N2 C9 MPLA 5 S1 N1 C1 C2 C3 MPLA 6 C10 > C14 N3 C15 MPLA 5 S1 N1 C1 C2 C3 MPLA 6 C16 > C20 N4 C21 LIST 6 MORE -1 BOND $H fmap 2 acta OMIT 3 -1 8 OMIT 4 0 6 OMIT 3 0 6 OMIT 3 -6 -4 OMIT 3 -2 7 OMIT 6 -2 6 OMIT -1 8 4 REM REM REM WGHT 0.154700 453.655701 EXTI 0.000281 BASF 0.43653 FVAR 0.35820 0.83054 S1 5 0.729370 0.892998 0.481575 11.00000 0.06292 0.05820 = 0.04906 0.00495 -0.00058 -0.00554 N1 4 0.894562 0.846766 0.571199 11.00000 0.04792 0.04901 = 0.05525 0.00165 0.01554 -0.01180 N2 4 0.805823 0.984570 0.695690 11.00000 0.05366 0.06928 = 0.05643 -0.00384 0.00603 0.00561 N3 4 0.659262 0.790156 0.280458 11.00000 0.04153 0.05419 = 0.04289 0.00573 -0.00391 -0.00315 N4 4 1.095170 0.695201 0.530425 11.00000 0.04272 0.05266 = 0.04818 0.00147 0.00117 0.00465 C1 1 0.818619 0.886769 0.557660 11.00000 0.04391 0.04424 = 0.03596 0.01530 0.00331 0.00308 C2 1 0.797128 0.843062 0.465175 11.00000 0.05176 0.04969 = 0.04416 0.00531 0.00174 -0.00158 C3 1 0.885698 0.822950 0.512902 11.00000 0.03923 0.04347 = 0.04245 -0.00656 0.00833 -0.00156 C4 1 0.815343 0.919730 0.606177 11.00000 0.04266 0.03796 = 0.03764 0.00278 0.00282 -0.00568 C5 1 0.874589 0.913822 0.667804 11.00000 0.05234 0.05547 = 0.05074 0.00347 -0.00455 -0.00110 AFIX 43 H5 2 0.920721 0.886263 0.680598 11.00000 -1.20000 AFIX 0 C6 1 0.868838 0.945989 0.710253 11.00000 0.06852 0.07055 = 0.06801 0.00205 -0.00173 -0.00418 AFIX 43 H6 2 0.912041 0.940801 0.752728 11.00000 -1.20000 AFIX 0 C7 1 0.737820 0.991620 0.635421 11.00000 0.05567 0.06138 = 0.06255 0.00482 -0.00701 0.00024 AFIX 43 H7 2 0.690439 1.019389 0.624383 11.00000 -1.20000 AFIX 0 C8 1 0.737283 0.959676 0.591611 11.00000 0.04778 0.06255 = 0.05494 0.00298 -0.00310 0.00503 AFIX 43 H8 2 0.683451 0.964348 0.550530 11.00000 -1.20000 AFIX 0 C9 1 0.807930 1.023221 0.741151 11.00000 0.06284 0.06268 = 0.08153 -0.01907 0.01195 0.00892 AFIX 137 H9A 2 0.759917 1.048910 0.718837 11.00000 -1.50000 H9B 2 0.929779 1.029114 0.755885 11.00000 -1.50000 H9C 2 0.735452 1.016579 0.778066 11.00000 -1.50000 AFIX 0 C10 1 0.744615 0.823001 0.400161 11.00000 0.05223 0.05698 = 0.04936 -0.00192 0.00087 -0.00110 C11 1 0.769949 0.849123 0.343873 11.00000 0.03612 0.04895 = 0.04542 -0.00315 0.00607 -0.00483 AFIX 43 H11 2 0.819515 0.877503 0.347471 11.00000 -1.20000 AFIX 0 C12 1 0.719435 0.831747 0.282426 11.00000 0.04643 0.05390 = 0.04607 0.00321 0.00017 0.00056 AFIX 43 H12 2 0.727768 0.848693 0.244558 11.00000 -1.20000 AFIX 0 C13 1 0.631454 0.766521 0.335082 11.00000 0.05543 0.05858 = 0.05335 -0.00232 -0.00586 0.00386 AFIX 43 H13 2 0.576467 0.738761 0.331279 11.00000 -1.20000 AFIX 0 C14 1 0.677813 0.780774 0.392192 11.00000 0.04314 0.03862 = 0.04456 -0.00236 0.00682 0.00027 AFIX 43 H14 2 0.666037 0.762358 0.428392 11.00000 -1.20000 AFIX 0 C15 1 0.611406 0.771623 0.215631 11.00000 0.03171 0.04541 = 0.06909 0.00089 0.01093 -0.00751 AFIX 137 H15A 2 0.545891 0.793471 0.190263 11.00000 -1.50000 H15B 2 0.537587 0.745664 0.220701 11.00000 -1.50000 H15C 2 0.719537 0.763652 0.193663 11.00000 -1.50000 AFIX 0 C16 1 0.960541 0.778104 0.518371 11.00000 0.03976 0.04505 = 0.04736 0.00131 0.00163 -0.00160 C17 1 1.031924 0.755725 0.465031 11.00000 0.04861 0.05444 = 0.04915 0.00220 0.00014 -0.00324 AFIX 43 H17 2 1.028189 0.769642 0.424379 11.00000 -1.20000 AFIX 0 C18 1 1.103662 0.716085 0.469870 11.00000 0.04192 0.05296 = 0.04298 -0.00501 0.01095 0.00203 AFIX 43 H18 2 1.157770 0.702490 0.434556 11.00000 -1.20000 AFIX 0 C19 1 1.040768 0.713849 0.580323 11.00000 0.05262 0.05417 = 0.05245 0.00417 0.00172 -0.00348 AFIX 43 H19 2 1.039535 0.698685 0.619969 11.00000 -1.20000 AFIX 0 C20 1 0.982609 0.757044 0.576192 11.00000 0.04463 0.05231 = 0.05464 -0.00471 0.00299 -0.00044 AFIX 43 H20 2 0.957583 0.772306 0.614463 11.00000 -1.20000 AFIX 0 C21 1 1.154145 0.649692 0.532799 11.00000 0.04315 0.04785 = 0.05590 0.00506 0.01188 0.00589 AFIX 137 H21A 2 1.055919 0.630561 0.519616 11.00000 -1.50000 H21B 2 1.193550 0.642391 0.576604 11.00000 -1.50000 H21C 2 1.252390 0.645701 0.503764 11.00000 -1.50000 AFIX 0 I7 3 0.617956 0.676042 0.483565 11.00000 0.05472 0.05813 = 0.04648 0.00079 0.00265 -0.00546 PART 1 I12 3 0.482862 0.762907 0.563170 11.00000 0.04583 0.07531 = 0.04461 0.00375 0.00055 -0.00708 I13 3 0.402130 0.834719 0.636153 11.00000 0.06156 0.06622 = 0.06638 0.00588 0.00952 0.00087 PART 0 S1E 5 0.239210 0.523391 0.426202 21.00000 0.06960 0.07168 = 0.06540 -0.01010 0.00411 0.00004 S2E 5 0.373748 0.552364 0.502355 21.00000 0.07164 0.07057 = 0.06945 0.00067 -0.00040 0.00238 S3E 5 0.230611 0.539157 0.580684 21.00000 0.07020 0.06731 = 0.07192 0.00565 0.00758 -0.00679 S4E 5 0.307981 0.478834 0.610024 21.00000 0.08144 0.08249 = 0.08444 0.00601 0.00439 -0.00184 S5E 5 0.151705 0.435253 0.559074 21.00000 0.07690 0.08181 = 0.07015 -0.01112 -0.00646 -0.00195 S6E 5 -0.071026 0.429046 0.609065 21.00000 0.06661 0.07543 = 0.07044 0.00199 0.00415 0.00532 PART 1 I4 3 0.255005 0.616829 -0.086442 11.00000 0.05359 0.07870 = 0.06625 0.01491 0.00705 0.00898 I5 3 0.251535 0.559914 0.019931 11.00000 0.05612 0.06328 = 0.05401 -0.00236 0.00633 0.00585 I6 3 0.247878 0.494426 0.132696 11.00000 0.06249 0.06393 = 0.04836 -0.00011 0.00617 0.00024 PART 0 I1 3 1.235221 0.851402 0.232170 11.00000 0.05638 0.06671 = 0.06304 -0.00895 0.00238 -0.00149 I2 3 1.117809 0.762565 0.268173 11.00000 0.04275 0.07132 = 0.04672 -0.00771 0.00086 0.00242 I3 3 0.968680 0.678693 0.298667 11.00000 0.06223 0.06636 = 0.05484 -0.00635 0.00215 -0.00004 I8 3 0.672953 0.613377 0.604450 11.00000 0.05850 0.06475 = 0.04899 -0.00415 0.00231 -0.00348 I9 3 0.706824 0.557859 0.709958 11.00000 0.06581 0.06195 = 0.06462 0.00470 0.00269 -0.00057 I10 3 0.487596 0.624608 0.341019 11.00000 0.06212 0.07006 = 0.08638 0.00474 -0.00555 -0.00823 I11 3 0.373683 0.570992 0.241882 11.00000 0.05205 0.06870 = 0.06230 0.01199 0.00217 -0.00079 HKLF 5 REM rb19036_twin1_hklf4_a.res in P2(1)/c REM wR2 = 0.3926, GooF = S = 1.039, Restrained GooF = 1.034 for all data REM R1 = 0.1366 for 11295 Fo > 4sig(Fo) and 0.1903 for all 17906 data REM 412 parameters refined using 192 restraints END WGHT 0.1585 446.9935 REM Highest difference peak 3.370, deepest hole -3.073, 1-sigma level 0.579 Q1 1 0.4696 0.7999 0.5659 11.00000 0.05 3.37 Q2 1 0.2227 0.5610 -0.0444 11.00000 0.05 2.92 Q3 1 0.4947 0.7232 0.5606 11.00000 0.05 2.87 Q4 1 0.2484 0.6501 -0.0812 11.00000 0.05 2.85 Q5 1 0.9753 0.6438 0.3003 11.00000 0.05 2.78 ; _shelx_res_checksum 53382 _shelx_hkl_file ; 0 0 2 1161.27 43.2452 -2 0 0 2 1161.27 43.2452 1 0 0 4 10070.4 123.000 -2 0 0 4 10070.4 123.000 1 0 0 6 14915.7 174.374 -2 0 0 6 14915.7 174.374 1 0 0 8 18765.8 223.105 -2 0 0 8 18765.8 223.105 1 0 0 10 867.080 124.908 -2 0 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42.0637 31.3193 1 6 15 -16 72.4261 47.1813 -2 6 15 -16 72.4261 47.1813 1 6 15 -15 120.423 52.1769 1 6 15 -15 278.091 42.3920 -2 6 15 -15 278.091 42.3920 1 6 15 -14 51.8479 52.9490 1 6 -15 -14 183.278 48.0704 -2 6 -15 -14 183.278 48.0704 1 6 15 -13 47.1489 23.4929 -2 6 15 -13 47.1489 23.4929 1 6 15 -12 28.3271 55.5690 -2 6 15 -12 28.3271 55.5690 1 6 -15 -11 4.85305 58.8827 -2 6 -15 -11 4.85305 58.8827 1 6 -15 -10 225.799 74.2017 -2 6 -15 -10 225.799 74.2017 1 6 -15 -9 453.117 80.0651 -2 6 -15 -9 453.117 80.0651 1 6 -15 -8 1334.23 90.6317 -2 6 -15 -8 1334.23 90.6317 1 6 -15 -7 102.744 31.5532 -2 6 -15 -7 102.744 31.5532 1 6 -15 -6 127.946 94.1383 -2 6 -15 -6 127.946 94.1383 1 6 -15 -5 623.055 100.199 -2 6 -15 -5 623.055 100.199 1 6 -15 -4 2099.85 90.7368 -2 6 -15 -4 2099.85 90.7368 1 6 -15 -3 81.1157 75.1824 -2 6 -15 -3 81.1157 75.1824 1 6 -15 -2 242.397 67.5196 -2 6 -15 -2 242.397 67.5196 1 6 -15 -1 1581.79 75.8582 -2 6 -15 -1 1581.79 75.8582 1 6 15 0 1695.61 75.7481 -2 6 15 0 1695.61 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89.5144 44.6445 2 2 -9 -19 41.3858 48.2893 2 2 -9 -18 115.589 56.2107 2 2 -9 -17 707.919 42.5293 2 2 -9 -16 553.703 52.0385 2 2 -9 -15 110.610 39.3612 2 2 -9 -14 296.161 33.8094 2 2 -9 -13 7350.48 46.5422 2 2 -9 10 1367.59 77.7709 2 2 -9 11 3447.78 96.1400 2 -2 9 -12 438.772 35.5554 2 -2 9 -13 96.5808 35.9151 2 -2 9 -14 2604.37 47.5235 2 -2 9 -15 84.7185 39.7660 2 -2 9 -16 894.840 44.1444 2 -2 9 -17-25.0564 55.0564 2 2 9 18-17.5269 36.9669 2 -2 9 -19 1071.24 43.2695 2 -2 9 -20 174.502 60.9995 2 -2 9 -21 42.0826 31.7475 2 -2 9 -22 12.4278 28.5803 2 -2 9 -23 120.981 22.7974 2 -2 -9 -24 5.31823 17.6172 2 -2 -9 -25 50.6031 13.2735 2 2 10 -25-5.90912 24.2573 2 -2 10 24 2.94835 15.3204 2 2 10 -23 39.7825 34.9853 2 2 -10 -22-32.3305 29.6562 2 2 -10 -21-27.4029 32.5824 2 2 -10 -20 156.507 38.1464 2 2 -10 -19 2186.25 69.3527 2 2 -10 -18 153.314 55.6792 2 -2 10 17 176.399 51.9047 2 2 -10 -16 1537.72 57.3773 2 2 -10 -15 804.257 42.7401 2 2 -10 -14 116.559 30.2212 2 2 -10 -13-17.6780 24.4018 2 2 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11 -18-28.7471 39.7337 2 -2 11 -19 176.094 51.5377 2 -2 11 -20-45.8804 55.2757 2 -2 11 -21 37.6520 41.6352 2 -2 11 -22 47.9262 29.4824 2 -2 11 -23 63.6406 26.5405 2 -2 11 -24 27.0690 22.3023 2 2 12 -24 13.3097 15.7197 2 -2 12 23 17.3300 22.9706 2 2 -12 -22 446.388 33.7873 2 2 -12 -21 4.12332 35.2063 2 2 -12 -20 94.1266 37.9788 2 2 -12 -19 180.552 28.9762 2 2 -12 -18 466.388 29.0166 2 2 12 -17 820.848 34.8018 2 2 12 -16 145.829 27.9781 2 2 -12 -15 138.275 26.6038 2 2 -12 -14 363.288 26.8396 2 2 -12 -13 1956.77 30.6060 2 2 12 9-11.3402 73.5009 2 2 -12 10 9781.98 135.755 2 -2 12 -11 1115.11 30.9341 2 -2 12 -12-30.3809 25.8236 2 -2 12 -13 1567.47 33.3435 2 -2 12 -14 947.425 32.7257 2 -2 12 -15 862.833 34.1802 2 -2 12 -16-30.6364 28.7126 2 -2 12 -17 18.5302 33.6651 2 -2 12 -18 76.5174 39.3036 2 -2 12 -19 143.730 62.0072 2 -2 12 -20 45.2718 56.2568 2 -2 12 -21 28.7415 33.4957 2 -2 12 -22 19.5242 32.7409 2 -2 12 -23-48.4979 24.1268 2 -2 12 -24 24.2324 19.5036 2 2 13 -24 41.8580 19.9615 2 -2 13 23 93.6090 20.7544 2 2 -13 -22-15.2143 28.7422 2 2 -13 -21 94.5852 33.7738 2 2 -13 -20 353.910 35.5086 2 2 -13 -19 55.8090 26.6468 2 2 -13 -18-1.42346 24.5739 2 2 13 -17 241.534 28.4790 2 2 13 -16 144.478 27.4331 2 2 -13 -15 145.505 25.2833 2 2 -13 -14 1431.09 30.8631 2 -2 13 13 1957.10 31.1267 2 2 13 9 292.711 76.5237 2 -2 13 -10 783.309 33.9042 2 -2 13 -11 1489.67 32.5145 2 2 13 12 361.208 29.1823 2 -2 13 -13 1431.80 32.3375 2 -2 13 -14-66.3915 26.1882 2 -2 13 -15-104.292 28.1330 2 -2 13 -16-30.7564 28.6152 2 -2 13 -17 373.447 30.1020 2 -2 13 -18 341.664 29.7138 2 -2 13 -19 3.60192 30.9516 2 -2 13 -20 26.6487 34.2970 2 -2 13 -21 94.9623 44.8325 2 -2 13 -22-13.0198 30.4090 2 -2 13 -23 0.37005 16.6856 2 2 13 24-7.29926 17.6465 2 2 14 -24 40.3734 15.3363 2 2 14 -23 125.337 17.8147 2 -2 14 22 20.1818 18.6206 2 2 -14 -21 12.2111 29.1327 2 2 -14 -20 133.173 33.9252 2 2 -14 -19 149.030 26.5693 2 2 -14 -18 536.537 24.0971 2 2 14 -17 548.220 27.5565 2 2 14 -16 2.54813 26.7263 2 2 -14 -15 255.162 26.9865 2 2 14 -14 203.023 25.2097 2 -2 14 13 205.777 24.6248 2 2 14 9 6671.41 178.181 2 -2 14 -10-61.9404 21.7454 2 2 14 11-14.0916 28.2894 2 2 14 12 2451.23 34.4616 2 -2 14 -13 34.0244 29.7170 2 -2 14 -14 1485.42 36.6007 2 -2 14 -15 1401.96 35.0446 2 -2 14 -16 1312.70 34.0787 2 -2 14 -17 861.749 33.6533 2 -2 14 -18 102.606 27.6290 2 -2 14 -19 225.110 29.7479 2 -2 14 -20 52.1905 32.8410 2 -2 14 -21 4.76998 29.2842 2 -2 14 -22 4.44501 21.4462 2 -2 14 -23 23.4498 16.9854 2 2 15 -23 33.4640 23.1985 2 -2 15 22 20.8547 21.1677 2 -2 15 21 30.1776 21.9717 2 2 -15 -20 301.527 34.2365 2 2 -15 -19 365.340 36.0953 2 2 -15 -18 243.544 22.7573 2 2 15 -17 235.705 26.1973 2 2 15 -16 299.547 26.3409 2 2 15 -15 265.786 27.9649 2 2 15 -14 995.325 26.3826 2 2 15 -13 1604.62 26.1707 2 2 15 9 693.173 41.7102 2 -2 15 -10 53.1078 22.7965 2 -2 15 -11 325.417 26.4304 2 2 15 12 357.476 28.5829 2 2 15 13 26.6126 31.6281 2 -2 15 -14 36.5160 31.9628 2 -2 15 -15 96.3129 35.6624 2 -2 15 -16 624.546 35.3690 2 -2 15 -17 5.28896 31.8572 2 -2 15 -18 192.135 30.9122 2 -2 15 -19 187.766 27.0532 2 -2 15 -20 162.962 22.9973 2 -2 15 -21 230.626 33.7057 2 -2 15 -22 19.9759 21.9774 2 -2 15 -23 24.4799 14.7737 2 2 16 -23 9.07398 19.1933 2 2 16 -22 22.6385 28.2861 2 -2 16 21 44.4087 18.5842 2 2 -16 -20 205.978 24.5358 2 2 16 -19 97.5515 33.7332 2 2 -16 -18 32.9019 21.5132 2 2 16 -17 92.2369 25.7099 2 2 16 -16 157.546 25.8362 2 2 16 -15 680.825 26.4009 2 2 16 -14 1042.68 26.2233 2 2 -16 -13 430.613 22.0187 2 2 16 9 2686.86 36.4729 2 -2 16 -10 133.322 23.3135 2 -2 16 -11 17.9886 25.9640 2 2 16 12 326.694 27.6135 2 2 16 13 209.249 30.9119 2 -2 16 -14 104.191 35.5263 2 -2 16 -15 140.416 34.7246 2 -2 16 -16 141.879 35.5301 2 -2 16 -17 374.120 34.7212 2 -2 16 -18 1093.07 32.8735 2 -2 16 -19 183.050 26.9111 2 -2 16 -20-11.0841 23.4315 2 -2 16 -21 516.730 33.9150 2 -2 16 -22 28.0701 19.0312 2 -2 -16 -23-5.15624 25.8951 2 2 17 -23 21.7251 20.9444 2 2 17 -22 91.1396 25.0664 2 2 -17 -21 24.4479 21.9273 2 2 -17 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4.56298 31.1891 2 2 20 -20 60.6070 29.2886 2 2 20 -19 200.430 40.4601 2 2 -20 -18 444.770 25.1365 2 2 20 -17 81.4662 22.5217 2 2 20 -16-17.9258 26.9522 2 2 20 -15 136.026 28.1193 2 2 20 -14 19.6001 26.4855 2 2 20 -13 55.8471 27.3712 2 2 20 9 1508.18 32.0604 2 -2 20 -10 679.471 28.8461 2 -2 20 -11 1149.92 31.2647 2 -2 20 -12 38.1123 23.5121 2 -2 20 -13-10.5462 25.1179 2 -2 20 -14 584.863 31.1775 2 -2 20 -15 225.616 28.9568 2 -2 20 -16 24.4515 27.6487 2 -2 20 -17 255.827 26.5979 2 -2 20 -18 74.5038 22.4396 2 -2 20 -19 49.1061 21.8764 2 -2 20 -20-2.23496 20.4155 2 2 21 -21 19.7491 27.3545 2 2 21 -20 110.221 39.3254 2 -2 21 19 3.18278 25.6389 2 2 21 -18 104.271 34.5553 2 2 21 -17 88.3288 25.1284 2 2 21 -16 219.184 27.2881 2 2 21 -15 411.377 28.1831 2 2 21 -14 88.3185 27.7288 2 2 21 -13 626.548 29.5877 2 -2 21 12 55.8950 27.8690 2 2 21 9 799.355 28.6143 2 -2 21 -10 313.752 31.2381 2 -2 21 -11 121.985 30.3437 2 -2 21 -12 184.957 27.0302 2 -2 21 -13 405.272 32.0010 2 -2 21 -14 242.093 28.7177 2 -2 21 -15 17.2186 26.7078 2 -2 21 -16-13.9796 24.9230 2 -2 21 -17 41.9390 24.0277 2 -2 21 -18 52.2773 32.0959 2 -2 21 -19 253.339 27.7496 2 2 21 20-3.67581 26.0472 2 -2 22 19 105.930 23.3950 2 -2 22 17 51.6491 26.7787 2 -2 22 16 98.9354 27.9557 2 2 22 -15 21.2327 25.9246 2 2 22 -14 254.524 27.5176 2 2 22 -13 1931.65 34.9006 2 -2 22 12 188.094 28.8624 2 2 22 3-3.49648 56.0276 2 2 22 4 1287.62 69.9130 2 2 22 5 360.014 32.4949 2 2 22 6 92.8410 30.5249 2 2 22 7-77.3012 26.4812 2 2 22 8 280.629 31.1528 2 2 22 9 119.536 31.1001 2 -2 22 -10 658.192 32.4608 2 -2 22 -11 220.880 30.3185 2 -2 22 -12 840.849 29.9856 2 -2 22 -13 173.597 30.6577 2 -2 22 -14-12.4935 33.2145 2 -2 22 -15 290.882 33.5090 2 -2 22 -16 26.8131 30.0542 2 -2 22 -17 64.6637 28.3647 2 -2 22 -18-58.1444 32.3603 2 -2 22 -19 85.4290 27.4551 2 2 22 20 80.9301 28.7954 2 -2 23 19 0.32209 21.6461 2 -2 23 17 88.3816 25.3668 2 2 23 -16 393.873 25.7713 2 -2 23 15 50.4503 27.3203 2 -2 23 14 161.331 28.6895 2 2 23 -13 131.793 27.4087 2 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58.5049 2 2 24 0 1962.83 220.380 2 2 24 1 24.7789 174.198 2 2 24 2 137.912 169.410 2 2 24 3 1927.25 54.4015 2 2 24 4 146.940 43.4748 2 2 24 5 1826.67 35.5492 2 2 24 6 38.9555 23.9991 2 2 24 7 25.0880 26.0133 2 2 24 8 259.615 26.7124 2 -2 24 -10 190.711 56.1572 2 -2 24 -11 726.327 59.0898 2 -2 24 -12-45.2350 51.0810 2 -2 24 -13 1049.34 56.6192 2 -2 24 -14 158.915 29.1767 2 -2 24 -15-4.80716 35.7565 2 -2 24 -16 40.8761 34.5751 2 -2 24 -17 37.7612 31.6846 2 2 24 18-50.9311 36.7803 2 2 24 19-14.2450 29.9138 2 2 25 -19 1.05287 24.9567 2 -2 25 18 15.4001 20.6551 2 2 25 -17 15.3780 23.2407 2 2 25 -16 169.175 23.1296 2 -2 25 15 40.3809 27.0367 2 -2 25 14 47.7747 27.4293 2 2 25 -13 646.874 28.6736 2 -2 25 12 351.674 25.4916 2 2 25 -11 176.862 66.0681 2 2 25 -10 753.289 69.2965 2 2 25 -9 517.852 66.4419 2 2 25 -8-30.5783 58.2110 2 2 25 0 43.5171 176.542 2 2 25 1 524.436 182.265 2 2 25 2 96.9980 169.219 2 2 25 3 1111.71 74.6983 2 2 25 4 439.819 34.2275 2 2 25 5 236.203 32.6582 2 2 25 6 225.681 23.8452 2 2 25 7 91.5416 25.1587 2 2 25 8 265.167 26.0721 2 -2 25 -10 217.142 56.6906 2 -2 25 -11 6.77378 51.8138 2 -2 25 -12 195.063 51.1607 2 -2 25 -13 133.630 49.1287 2 -2 25 -14-19.7934 35.9910 2 -2 25 -15 47.4292 34.9401 2 -2 25 -16 39.2419 32.5832 2 2 25 17 24.3907 40.3317 2 2 25 18-74.8390 33.0872 2 2 25 19 12.5855 24.3565 2 2 26 -18-21.7173 26.3798 2 2 26 -17-40.6226 37.9916 2 -2 26 16 116.714 23.0096 2 -2 26 15 464.989 43.0275 2 2 26 -13 460.751 66.5579 2 2 26 -12 216.129 64.2210 2 -2 26 11 516.962 37.7319 2 -2 26 10 100.003 29.9159 2 -2 26 9 214.805 31.2264 2 -2 26 8-1.70545 26.8614 2 -2 26 7 177.136 31.5123 2 -2 26 6 16.9668 30.7841 2 -2 26 5 715.051 41.7989 2 -2 26 4 1192.99 55.1650 2 -2 26 3 261.867 69.2466 2 2 26 3 1289.31 82.6667 2 2 26 4 84.8947 30.9301 2 2 26 5-42.6352 31.1652 2 2 26 6 511.253 25.2178 2 2 26 7-67.0291 22.7055 2 2 26 8 287.982 26.5192 2 2 26 14 50.0313 49.8042 2 2 26 15 411.267 49.1205 2 2 26 16 16.0907 43.5187 2 2 26 17 359.189 38.7572 2 2 26 18 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40.6120 2 2 28 4 311.764 30.7586 2 2 28 5-2.97293 25.5015 2 2 28 6 151.942 27.7068 2 2 28 7-8.07230 23.0920 2 2 28 8-33.9879 28.2123 2 2 28 9 114.658 47.0765 2 2 28 16 17.5782 33.3671 2 2 28 17 6.29909 26.0255 2 -2 29 17-34.8588 16.9130 2 -2 29 16 106.912 27.8395 2 2 29 -13 41.6189 34.5637 2 2 29 -12 19.9709 38.6795 2 2 29 -11 157.019 27.6078 2 -2 29 10-8.03948 39.5292 2 -2 29 9 483.135 30.1503 2 -2 29 8 130.197 26.4577 2 -2 29 7 74.5399 24.6199 2 -2 29 6 144.811 34.0275 2 -2 29 5 227.913 35.0386 2 -2 29 4 158.889 42.7673 2 -2 29 3 268.679 61.3749 2 2 29 3-43.8600 29.6936 2 2 29 4 294.084 27.7653 2 2 29 5-11.3076 23.0468 2 2 29 6-19.4543 26.5923 2 2 29 7 176.263 27.9798 2 2 29 8 552.955 29.5722 2 2 29 9 261.119 44.6317 2 -2 29 -10 201.177 96.9876 2 -2 30 16 38.5109 20.4015 2 -2 30 11 344.295 36.8545 2 -2 30 10 199.493 25.3965 2 -2 30 9 18.3498 29.9627 2 -2 30 8 148.231 28.9195 2 -2 30 7 119.304 24.2384 2 -2 30 6 233.392 26.8614 2 -2 30 5 1.42516 32.4930 2 -2 30 4-38.4983 49.7052 2 -2 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7-65.8404 29.4493 2 7 -18 8 14.6019 23.8582 2 7 -18 9 94.8035 39.8964 2 7 -18 10 149.466 44.9187 2 7 18 11 52.8490 33.0071 2 7 18 12 7.03603 24.6095 2 -7 18 -13 33.5693 26.6489 2 7 19 -10 49.5225 50.1422 2 7 19 -9 276.619 24.9282 2 7 19 -8 53.1500 29.0853 2 7 19 -7 76.4305 35.6658 2 7 19 3 121.955 111.990 2 7 19 4-1.73194 106.967 2 7 19 5 39.1229 100.115 2 7 -19 6 43.7468 49.5844 2 7 -19 7-2.19817 47.5871 2 7 -19 8 40.0110 45.9820 2 7 -19 9 148.155 43.5386 2 7 -19 10 14.9393 37.0797 2 7 -19 11-65.3830 30.0682 2 -7 19 -12-44.1934 28.9593 2 7 20 -8 64.9906 54.2393 2 7 20 4 61.0092 95.9699 2 7 20 5 85.8600 85.5726 2 7 -20 6 121.874 45.3083 2 7 -20 7-36.4989 41.6907 2 7 -20 8 17.8576 40.3694 2 7 -20 9 82.3668 37.7298 2 7 -20 10 14.8423 30.8480 2 7 -20 11 0.25337 24.3311 2 7 21 -11 57.7521 29.7096 2 7 21 5 54.9863 78.3451 2 7 -21 6-10.2944 40.0568 2 7 -21 7-2.55910 37.6644 2 7 -21 8-19.4749 35.5483 2 7 -21 9-5.80379 30.9202 2 7 -21 10-10.4309 24.1749 2 7 -21 11-38.8949 25.2218 2 7 22 -10 11.1227 27.8179 2 7 22 -9-25.2767 35.6711 2 7 -22 6 45.0302 22.7273 2 7 -22 7 4.68694 20.1000 2 7 -22 8 28.2446 17.8838 2 7 -22 9 30.4138 23.7747 2 7 -22 10-10.3748 17.1305 2 7 23 -9 29.8577 25.9470 2 7 23 -8 61.8330 33.4370 2 7 23 -7 46.5918 39.4627 2 7 -23 6 14.5476 18.7370 2 7 -23 7 76.3452 18.9362 2 7 -23 8 27.6040 22.3865 2 -7 23 -9 13.6547 22.9980 2 7 24 -7 0.80563 29.4194 2 7 24 -6-26.9326 33.6981 2 7 24 -5-13.0550 39.3776 2 7 -24 6 81.5194 25.5072 2 7 -24 7-21.9228 20.0339 2 7 25 -6 54.2212 24.3227 2 7 25 -5 17.9608 29.3373 2 7 25 -4 4.89779 32.1477 2 -7 25 -6 5.50969 24.1107 2 7 26 -3 52.4672 23.9569 2 8 -1 -13-4.53122 43.7840 2 8 -1 5 182.880 98.2377 2 8 1 7-34.9594 29.4757 2 8 1 13 184.834 15.4854 2 8 -2 -13 42.2988 43.2259 2 8 -2 5 317.748 107.430 2 8 -2 6 28.3543 90.7382 2 8 3 -13-13.0768 58.0466 2 8 -4 5 12.9746 103.334 2 8 -4 6 224.733 103.522 2 8 -4 8-95.5406 47.5958 2 8 5 5 49.8153 86.5839 2 8 5 6 196.414 69.9033 2 8 -5 7 261.200 93.7071 2 8 -5 8 207.240 90.5329 2 8 -5 9 187.951 83.7834 2 8 -5 10 35.8756 78.0139 2 8 5 13-58.2953 42.9661 2 8 6 -12 94.6229 70.3240 2 8 6 5 739.584 78.2057 2 8 6 6 37.4731 66.5945 2 8 -6 7 135.268 66.2244 2 8 -6 8 105.752 81.2969 2 8 6 12 15.4589 56.1743 2 8 6 13 45.1093 38.1482 2 8 7 -12-18.5086 60.7865 2 8 7 5 1081.68 78.4476 2 8 7 6 152.397 64.5357 2 8 7 7 324.791 90.6923 2 8 -7 8 304.398 94.6363 2 8 -7 9-47.4467 72.8460 2 8 7 11-90.9280 63.1544 2 8 7 12-69.6302 47.4350 2 8 7 13 4.14296 32.8873 2 8 8 -12-14.3864 50.4143 2 8 8 -11 70.1409 82.5646 2 8 -8 5-4.13914 200.184 2 8 -8 6 225.968 156.518 2 8 8 7-147.227 89.0998 2 8 8 8-26.5578 70.7476 2 8 8 9-79.7508 55.8712 2 8 8 10-20.4613 29.9331 2 8 8 11-81.5598 54.3209 2 8 8 12-41.4142 41.5071 2 8 8 13-76.1610 26.5715 2 8 9 -11-12.3278 64.8927 2 8 9 -10 144.207 81.3497 2 8 -9 5 991.028 239.947 2 8 -9 6 296.176 176.242 2 8 -9 7-57.0637 134.397 2 8 -9 8-19.2715 103.129 2 8 -9 9-19.3841 79.6821 2 8 -9 10 14.0167 52.1178 2 8 10 -11 38.4552 51.5596 2 8 10 -10 50.0820 77.5773 2 8 10 5 553.164 111.981 2 8 -10 6 91.6506 208.400 2 8 -10 7 72.1683 147.339 2 8 -10 8 60.3075 112.279 2 8 -10 9 270.377 90.5528 2 8 -10 10-16.7012 58.5671 2 8 10 12-57.8090 29.7512 2 8 11 -10-16.7906 61.0617 2 8 11 -9-2.73149 70.3668 2 8 11 4-74.4171 113.892 2 8 11 5-53.9713 89.8166 2 8 11 6 154.879 88.8475 2 8 11 7 58.5085 70.7694 2 8 11 8-48.0534 60.3850 2 8 11 9 9.31088 56.4525 2 8 11 10 69.2661 37.9007 2 8 11 11 20.0952 35.5172 2 8 12 -10 79.3385 41.1567 2 8 12 -9 116.667 70.4613 2 8 12 4 142.607 97.5785 2 8 12 5 228.301 90.6436 2 8 -12 6 133.687 70.7703 2 8 12 7 57.7965 46.1924 2 8 12 8 105.621 53.6202 2 8 12 9-12.6228 43.6152 2 8 -12 10-1.71705 32.7750 2 8 13 -9-7.66041 33.4605 2 8 13 -8 47.2865 63.0319 2 8 13 4 151.380 83.3690 2 -8 13 -5 63.4056 52.7666 2 -8 13 -6 42.4504 47.1991 2 8 -13 7 96.5690 40.9283 2 8 -13 8-5.87204 33.8517 2 8 -13 9-3.49651 36.1557 2 8 -13 10 50.1827 27.4264 2 8 14 -7 22.7618 43.4421 2 8 14 -6 86.8798 55.9062 2 8 14 4 83.6924 72.4639 2 -8 14 -5 16.7483 44.4270 2 -8 14 -6 47.4465 41.8454 2 8 -14 7 66.3850 34.7451 2 8 -14 8 15.0817 29.9042 2 8 -14 9 25.0637 24.1546 2 8 15 -5-78.5289 30.6385 2 8 15 4-21.1596 58.8235 2 8 -15 5 14.8446 34.8319 2 -8 15 -6 14.9595 35.6015 2 -8 15 -7 24.4093 30.1295 2 8 -15 8 151.600 36.4624 2 8 -15 9 96.7101 47.7989 2 8 16 -2-2.99536 21.5884 2 8 16 3 127.589 46.2161 2 8 16 4 79.3390 38.4541 2 8 -16 5-51.9004 22.9450 2 8 -16 6-48.1987 36.7264 2 -8 16 -7 56.6269 41.7566 2 -8 16 -8-3.89102 38.6717 2 8 -16 9 58.9937 35.2026 2 8 -17 5-53.4766 33.5341 2 8 -17 6-43.4415 31.0684 2 -8 17 -7-11.2362 36.1199 2 8 18 -9-34.3261 22.9673 2 8 18 -8-4.65258 31.0407 2 8 18 -7-24.9218 36.2304 2 8 18 -6 17.5945 41.1128 2 8 18 -5-1.38273 45.6895 2 8 -18 5 52.9185 29.7112 2 8 -18 6 73.7253 27.1954 2 8 -18 7-16.2143 38.1653 2 8 19 -8 18.5129 22.0039 2 8 19 -7 56.7092 30.5859 2 8 19 -6 27.3679 34.0130 2 8 19 -5 57.8788 37.6801 2 8 -19 5-50.7677 23.4638 2 8 -19 6 3.68787 32.9491 2 8 20 -6 19.3729 25.6737 2 8 20 -5 31.8292 30.1860 2 8 20 -4-24.6090 33.5012 2 8 -20 5 0.52668 27.7006 2 8 21 -5-0.32920 21.2526 2 8 21 -4 24.7396 25.3859 2 9 0 -8 105.176 71.3940 2 9 1 -10 8.41079 30.9377 2 9 -1 -9 66.1322 41.1172 2 9 -1 -8 1.37642 51.6022 2 9 -1 -7-9.78415 53.1844 2 9 -1 -6 132.966 73.0887 2 9 1 5-11.5484 18.8769 2 9 2 -10-34.4717 28.8570 2 9 -2 -9 7.84225 36.7318 2 9 -2 -8-89.7523 50.4737 2 9 2 -7 264.245 84.9301 2 9 -3 -9 56.6264 31.3761 2 9 -3 -8 182.194 50.2341 2 9 -3 -7 98.0776 51.8970 2 9 3 -6 1.58790 78.5316 2 9 -4 -9-44.7471 25.7773 2 9 -4 -8 6.16526 41.6445 2 9 -4 -7-0.91754 45.2873 2 9 4 -6-177.998 70.8163 2 9 4 -5 101.246 75.2601 2 9 -4 4 86.4951 81.1057 2 9 -4 5 28.9732 72.6180 2 9 -5 -8 3.85251 41.8352 2 9 -5 -7-39.0388 65.0740 2 9 5 -6-37.8104 68.7625 2 9 5 -5-28.9279 70.1774 2 9 5 4 328.818 126.955 2 9 5 5 99.0919 116.264 2 9 5 6 30.7035 85.6107 2 9 5 7 19.7074 56.9760 2 9 5 8-22.4688 36.9162 2 9 6 4 1.94926 107.334 2 9 6 5-150.126 89.7250 2 9 6 6-14.6198 64.6424 2 9 6 7 41.6946 46.6245 2 9 7 -8 7.41344 40.7378 2 9 7 -7-61.9496 51.0529 2 9 7 4 46.5416 91.7573 2 9 7 5 129.480 70.8507 2 9 7 6 58.2325 54.4350 2 9 7 7-2.74224 36.7397 2 9 8 -7 12.0801 44.9023 2 9 8 -6 165.004 52.4796 2 9 8 -5 37.0424 53.1255 2 9 8 -4 117.906 58.2459 2 9 9 -6 27.6541 42.7641 2 9 9 -5 15.7236 45.7896 2 9 9 -4 34.3146 48.8399 2 9 9 -3 99.6492 51.9263 2 9 9 4-69.3655 56.0207 2 9 9 5-12.0125 45.2533 2 9 9 6-31.2112 32.4373 2 9 10 -4 20.2056 41.5297 2 9 10 -3-16.7667 42.8333 2 9 10 -2 24.2875 43.5695 2 9 10 4 11.9200 42.6431 2 9 11 -2 30.0583 34.6428 2 9 11 -1 15.6936 33.7226 2 0 0 0 0.00000 0.00000 0 TITL RB19036_twin1_hklf4 in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 1.54184 7.559157 30.640518 20.869728 89.9435 91.5647 90.1108 ZERR 2.00 0.000366 0.001330 0.000957 0.0036 0.0038 0.0037 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N S I UNIT 80.00 84.00 20.00 28.00 52.00 REM CrysAlisPro recorded range (K): Min=100.0; max=100.0; aver:100.0 TEMP -173 TREF HKLF 5 BASF 0.42220 END ; _shelx_hkl_checksum 68578 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.290 _oxdiff_exptl_absorpt_empirical_full_min 0.284 _oxdiff_twin_integration_method simultaneous _oxdiff_twin_items 2 loop_ _twin_individual_id _twin_individual_mass_fraction_refined _oxdiff_twin_reflns_isolated _oxdiff_twin_reflns_overlapped _twin_individual_twin_lattice_type _twin_individual_twin_matrix_11 _twin_individual_twin_matrix_12 _twin_individual_twin_matrix_13 _twin_individual_twin_matrix_21 _twin_individual_twin_matrix_22 _twin_individual_twin_matrix_23 _twin_individual_twin_matrix_31 _twin_individual_twin_matrix_32 _twin_individual_twin_matrix_33 1 0.563(3) 13236 20951 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 2 0.437(3) 13156 20951 nmt 1.0015 0.0015 -0.0025 -0.0379 0.9985 -0.0450 0.0190 0.0210 1.0007 _twin_special_details ; Component 2 rotated by 1.8859\% around [0.63 -0.58 -0.52] (reciprocal) or [0.99 -0.05 -0.10] (direct) ; # start Validation Reply Form _vrf_PLAT084_rb19036_twin1_hklf4 ; PROBLEM: High wR2 Value (i.e. > 0.25) ................... 0.39 Report RESPONSE: Small dark needles of the title compound were impossible to assess with optical microscopy. Twinning was detected in CrysAlisPro and a two- component twin model integrated. Nevertheless the data quality is still not optimal. A view of the final map shows that all the residual peaks and holes are associated with the heavy iodine atoms. ; _vrf_PLAT342_rb19036_twin1_hklf4 ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.05125 Ang. RESPONSE: Small dark needles of the title compound were impossible to assess with optical microscopy. Twinning was detected in CrysAlisPro and a two- component twin model integrated. Nevertheless the data quality is still not optimal. A view of the final map shows that all the residual peaks and holes are associated with the heavy iodine atoms. ; _vrf_PLAT434_rb19036_twin1_hklf4 ; PROBLEM: Short Inter HL..HL Contact I6 ..I11 3.39 Ang. RESPONSE: Contacts refined as 3.3909(40) Ang for I6...I11; 3.3174(38) Ang for I7...I12 and 3.4867(42) Ang for I7...I10. Contacts are discussed in the publication. ; # end Validation Reply Form