data_cx1754_sq _audit_creation_date 2020-01-07 _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. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C36 H36 K0.5 N24 O12.5, Au Br4' _chemical_formula_sum 'C36 H36 Au Br4 K0.50 N24 O12.50' _chemical_formula_weight 1541.04 _chemical_melting_point ? _chemical_oxdiff_formula C36H36N24O12KAuBr4 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' 'Au' 'Au' -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 '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' 'O' 'O' 0.0106 0.0060 '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 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.3299(14) _cell_length_b 14.3772(11) _cell_length_c 15.9853(12) _cell_angle_alpha 66.228(7) _cell_angle_beta 88.468(7) _cell_angle_gamma 89.781(7) _cell_volume 3012.8(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 3543 _cell_measurement_temperature 100.01(12) _cell_measurement_theta_max 24.6240 _cell_measurement_theta_min 2.1240 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 5.200 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.74826 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.699 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 1497 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.0114 0 0 1 0.0114 5 -20 -7 0.0290 -20 0 -1 0.0559 14 14 6 0.0467 _exptl_crystal_recrystallization_method 'The material was recrystallised from --- by as supplied' _exptl_crystal_size_max 0.189 _exptl_crystal_size_mid 0.117 _exptl_crystal_size_min 0.023 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 -0.0047 -0.0008 -1.0000 -0.0375 0.0307 -0.0019 0.0047 0.0008 1.0000 0.0375 -0.0307 0.0019 4.8091 -19.5949 -6.9477 0.5826 0.6147 0.5317 -20.2049 -0.0903 -0.7972 0.2174 0.2274 -0.9492 14.1373 14.4984 5.8100 -0.6189 -0.6513 0.4392 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_unetI/netI 0.0996 _diffrn_reflns_Laue_measured_fraction_full 0.989 _diffrn_reflns_Laue_measured_fraction_max 0.932 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 15237 _diffrn_reflns_point_group_measured_fraction_full 0.989 _diffrn_reflns_point_group_measured_fraction_max 0.932 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.481 _diffrn_reflns_theta_min 2.094 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.01(12) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.932 _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 -4.00 64.00 0.50 193.88 -- 2.83 77.00 -60.00 136 2 \w -1.00 52.00 0.50 193.88 -- -3.30 77.00 0.00 106 3 \w -19.00 65.00 0.50 193.88 -- 2.83 77.00-120.00 168 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Single source at offset/far, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0120345000 _diffrn_orient_matrix_UB_12 -0.0460076000 _diffrn_orient_matrix_UB_13 0.0375716000 _diffrn_orient_matrix_UB_21 -0.0099433000 _diffrn_orient_matrix_UB_22 -0.0229541000 _diffrn_orient_matrix_UB_23 -0.0306166000 _diffrn_orient_matrix_UB_31 0.0469845000 _diffrn_orient_matrix_UB_32 -0.0162219000 _diffrn_orient_matrix_UB_33 0.0017399000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 7954 _reflns_number_total 15237 _reflns_special_details ; Structure factors included contributions from the .fab file. _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 'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)' _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 2.586 _refine_diff_density_min -1.493 _refine_diff_density_rms 0.221 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.410 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 746 _refine_ls_number_reflns 15237 _refine_ls_number_restraints 1758 _refine_ls_R_factor_all 0.2244 _refine_ls_R_factor_gt 0.1468 _refine_ls_restrained_S_all 1.373 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3994 _refine_ls_wR_factor_ref 0.4354 _refine_special_details ; Diffuse, disordered solvent molecules could not be adequately modeled. The bypass procedure in Platon (Spek, 1990) was used to remove the electronic contribution from these solvents. The total potential solvent accessible void volume was 573 Ang^3^ and the electron count / cell = 152. As the exact solvent content is not known, the reported formula reflects only the atoms used in the refinement.The crystal under investigation was found to be non-merohedrally twinned. The orientation matrices for the two components were identified using the program CrysAlisPro (Rigaku Oxford Diffraction, 2019). The exact twin matrix identified by the integration program was found to be (-1.0008 -0.0002 -0.0005 -0.0007 -1.0006 -0.0034 0.8910 0.0538 0.9990). The second domain is rotated from first domain by 180 \% about the reciprocal lattice c axis. An hklf5 file which was used in all refinements; The twin fraction refined to a value of 0.315(3). Distance restraints were imposed on the C-N bonds. The enhanced rigid-bond restraint (SHELX keyword RIGU) was applied globally. (Acta Cryst. A68 (2012) 448-451) Restraints on similar amplitudes separated by less than 1.7 Ang. were also imposed globally. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.685(3) 0.315(3) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 3. Restrained distances N15-C23 \\sim N16-C24 \\sim N18-C24 \\sim N22-C31 \\sim N21-C31 \\sim N21-C29 \\sim N22-C30 \\sim N22-C33 \\sim N24-C33 \\sim N24-C34 \\sim N23-C34 \\sim N23-C32 \\sim N19-C29 \\sim N20-C30 \\sim N20-C28 \\sim N18- C27 \\sim N18-C25 \\sim N17-C25 \\sim N17-C23 \\sim N17-C26 \\sim N16-C21 \\sim N14-C21 \\sim N14-C19 ~ N13-C19 \\sim N13-C20 \\sim N15-C20 \\sim N15-C22 \\sim N16-C22 \\sim N20-C27 \\sim N19-C26 \\sim N21-C32 with sigma of 0.01 4. Uiso/Uaniso restraints and constraints All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(Au2) \\sim Ueq, Uanis(Br5) \\sim Ueq, Uanis(Br6) \\sim Ueq, Uanis(Br7) \\sim Ueq, Uanis(Br8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 5. Rigid body (RIGU) restrains All non-hydrogen atoms with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 6. Others Fixed Sof: O13(0.5) Au1(0.66667) Br1(0.66667) Br2(0.66667) Br3(0.66667) Br4(0.66667) Au2(0.33333) Br5(0.33333) Br6(0.33333) Br7(0.33333) Br8(0.33333) 7.a Free rotating group: Au2(Br5,Br6,Br7,Br8) 7.b Ternary CH refined with riding coordinates: C1(H1), C4(H4), C7(H7), C10(H10), C13(H13), C16(H16), C19(H19), C22(H22), C25(H25), C28(H28), C31(H31), C34(H34) 7.c Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C3(H3A,H3B), C8(H8A,H8B), C9(H9A,H9B), C14(H14A,H14B), C15(H15A, H15B), C23(H23A,H23B), C24(H24A,H24B), C29(H29A,H29B), C30(H30A,H30B), C35(H35A,H35B), C36(H36A,H36B) ; _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 K1 K 1.000000 1.000000 0.500000 0.088(2) Uani 1 2 d S TU P . . O1 O 0.7878(10) 0.6969(10) 0.2937(10) 0.070(3) Uani 1 1 d . U . . . O2 O 1.0402(10) 0.3637(10) 0.2852(12) 0.081(4) Uani 1 1 d . U . . . O3 O 0.9715(10) 0.8381(10) 0.2886(10) 0.070(3) Uani 1 1 d . U . . . O4 O 1.2145(9) 0.4968(9) 0.2941(9) 0.062(3) Uani 1 1 d . U . . . O5 O 1.0610(10) 0.8136(9) 0.5073(11) 0.072(3) Uani 1 1 d . U . . . O6 O 1.3155(10) 0.4658(9) 0.4993(11) 0.072(3) Uani 1 1 d . U . . . O7 O 0.2540(11) 0.8706(10) 0.7121(11) 0.077(4) Uani 1 1 d . U . . . O8 O 0.5945(11) 1.1180(9) 0.7036(10) 0.068(3) Uani 1 1 d . U . . . O9 O 0.3931(11) 0.6939(12) 0.7089(11) 0.078(4) Uani 1 1 d . U . . . O10 O 0.7335(11) 0.9378(10) 0.7184(14) 0.091(4) Uani 1 1 d . U . . . O11 O 0.4705(9) 0.6835(10) 0.5031(11) 0.070(3) Uani 1 1 d . U . . . O12 O 0.8134(10) 0.9383(9) 0.4993(12) 0.073(3) Uani 1 1 d . U . . . O13 O 1.011(2) 0.970(2) 0.683(3) 0.094(9) Uani 0.5 1 d . U . . . N1 N 0.7225(11) 0.4322(11) 0.4239(13) 0.059(3) Uani 1 1 d . U . . . N2 N 0.8196(11) 0.2945(11) 0.4209(13) 0.065(3) Uani 1 1 d . U . . . N3 N 0.7837(12) 0.5438(12) 0.2757(12) 0.062(2) Uani 1 1 d . U . . . N4 N 0.8847(12) 0.4127(12) 0.2770(13) 0.065(3) Uani 1 1 d . U . . . N5 N 0.8903(12) 0.6560(12) 0.2016(12) 0.063(2) Uani 1 1 d . U . . . N6 N 0.9895(11) 0.5214(11) 0.1932(11) 0.058(2) Uani 1 1 d . U . . . N7 N 1.0231(12) 0.7640(12) 0.1945(13) 0.066(2) Uani 1 1 d . U . . . N8 N 1.1214(11) 0.6244(11) 0.1981(11) 0.058(2) Uani 1 1 d . U . . . N9 N 1.1260(12) 0.7967(11) 0.2827(12) 0.063(2) Uani 1 1 d . U . . . N10 N 1.2288(11) 0.6661(11) 0.2755(12) 0.061(2) Uani 1 1 d . U . . . N11 N 1.1845(11) 0.7764(11) 0.4283(13) 0.063(2) Uani 1 1 d . U . . . N12 N 1.2869(11) 0.6372(11) 0.4278(12) 0.060(2) Uani 1 1 d . U . . . N13 N 0.3014(12) 1.0186(9) 0.7224(12) 0.071(3) Uani 1 1 d D U . . . N14 N 0.4311(9) 1.1221(10) 0.7209(11) 0.063(3) Uani 1 1 d D U . . . N15 N 0.3675(11) 0.8778(8) 0.8094(12) 0.071(2) Uani 1 1 d D U . . . N16 N 0.5101(9) 0.9791(9) 0.8009(10) 0.064(3) Uani 1 1 d D U . . . N17 N 0.4766(9) 0.7517(11) 0.8049(10) 0.062(2) Uani 1 1 d D U . . . N18 N 0.6097(10) 0.8452(9) 0.8138(11) 0.065(2) Uani 1 1 d D U . . . N19 N 0.5563(10) 0.6796(11) 0.7268(11) 0.066(2) Uani 1 1 d D U . . . N20 N 0.6909(10) 0.7821(10) 0.7202(11) 0.067(2) Uani 1 1 d D U . . . N21 N 0.6048(9) 0.6870(10) 0.5796(9) 0.062(2) Uani 1 1 d D U . . . N22 N 0.7422(11) 0.7815(9) 0.5803(9) 0.068(2) Uani 1 1 d D U . . . N23 N 0.6095(9) 0.7521(11) 0.4283(11) 0.063(2) Uani 1 1 d D U . . . N24 N 0.7413(11) 0.8538(9) 0.4264(11) 0.066(2) Uani 1 1 d D U . . . C1 C 0.7280(13) 0.3222(13) 0.4437(15) 0.060(3) Uani 1 1 d . U . . . H1 H 0.676813 0.297838 0.418193 0.072 Uiso 1 1 calc R . . . . C2 C 0.6966(14) 0.5028(14) 0.3334(15) 0.064(3) Uani 1 1 d . U . . . H2A H 0.660936 0.558218 0.337833 0.077 Uiso 1 1 calc R . . . . H2B H 0.658027 0.468448 0.305548 0.077 Uiso 1 1 calc R . . . . C3 C 0.8464(15) 0.3071(14) 0.3291(16) 0.066(3) Uani 1 1 d . U . . . H3A H 0.792522 0.296307 0.298496 0.079 Uiso 1 1 calc R . . . . H3B H 0.893307 0.257459 0.331295 0.079 Uiso 1 1 calc R . . . . C4 C 0.8287(14) 0.4989(14) 0.2246(15) 0.063(2) Uani 1 1 d . U . . . H4 H 0.786289 0.483866 0.184497 0.075 Uiso 1 1 calc R . . . . C5 C 0.8173(15) 0.6361(14) 0.2619(15) 0.062(3) Uani 1 1 d . U . . . C6 C 0.9759(15) 0.4251(15) 0.2551(15) 0.065(3) Uani 1 1 d . U . . . C7 C 0.9090(14) 0.5789(14) 0.1681(15) 0.061(2) Uani 1 1 d . U . . . H7 H 0.900051 0.604347 0.102054 0.074 Uiso 1 1 calc R . . . . C8 C 0.9358(15) 0.7497(14) 0.1587(16) 0.066(3) Uani 1 1 d . U . . . H8A H 0.893362 0.801858 0.159898 0.079 Uiso 1 1 calc R . . . . H8B H 0.946850 0.761599 0.095019 0.079 Uiso 1 1 calc R . . . . C9 C 1.0792(14) 0.5651(14) 0.1586(14) 0.062(2) Uani 1 1 d . U . . . H9A H 1.121388 0.510149 0.164168 0.075 Uiso 1 1 calc R . . . . H9B H 1.073758 0.606787 0.093848 0.075 Uiso 1 1 calc R . . . . C10 C 1.1206(14) 0.7334(13) 0.1676(15) 0.063(2) Uani 1 1 d . U . . . H10 H 1.135794 0.768821 0.102184 0.075 Uiso 1 1 calc R . . . . C11 C 1.0307(15) 0.8017(14) 0.2609(16) 0.064(2) Uani 1 1 d . U . . . C12 C 1.1903(13) 0.5865(13) 0.2591(13) 0.053(3) Uani 1 1 d . U . . . C13 C 1.1830(14) 0.7594(14) 0.2233(15) 0.063(2) Uani 1 1 d . U . . . H13 H 1.228224 0.811246 0.185425 0.076 Uiso 1 1 calc R . . . . C14 C 1.1604(15) 0.8423(14) 0.3389(15) 0.067(3) Uani 1 1 d . U . . . H14A H 1.113694 0.889145 0.343550 0.080 Uiso 1 1 calc R . . . . H14B H 1.215309 0.882240 0.308649 0.080 Uiso 1 1 calc R . . . . C15 C 1.3123(14) 0.6464(14) 0.3342(15) 0.062(3) Uani 1 1 d . U . . . H15A H 1.341883 0.584110 0.337886 0.075 Uiso 1 1 calc R . . . . H15B H 1.356999 0.701523 0.306313 0.075 Uiso 1 1 calc R . . . . C16 C 1.2727(14) 0.7239(13) 0.4522(15) 0.062(3) Uani 1 1 d . U . . . H16 H 1.324693 0.772355 0.427897 0.074 Uiso 1 1 calc R . . . . C17 C 1.1351(14) 0.7616(14) 0.5112(16) 0.065(3) Uani 1 1 d . U . . . C18 C 1.2938(11) 0.5502(12) 0.5031(15) 0.050(3) Uani 1 1 d . U . . . C19 C 0.3620(12) 1.0512(12) 0.7743(12) 0.070(3) Uani 1 1 d D U . . . H19 H 0.327800 1.074259 0.816299 0.084 Uiso 1 1 calc R . . . . C20 C 0.2993(15) 0.9137(9) 0.7422(15) 0.072(3) Uani 1 1 d D U . . . C21 C 0.5213(11) 1.0805(9) 0.7359(12) 0.063(3) Uani 1 1 d D U . . . C22 C 0.4140(10) 0.9580(11) 0.8225(15) 0.069(3) Uani 1 1 d D U . . . H22 H 0.406274 0.943200 0.887715 0.082 Uiso 1 1 calc R . . . . C23 C 0.3997(12) 0.7772(10) 0.8485(13) 0.066(3) Uani 1 1 d D U . . . H23A H 0.348122 0.732481 0.851214 0.080 Uiso 1 1 calc R . . . . H23B H 0.416268 0.762439 0.911019 0.080 Uiso 1 1 calc R . . . . C24 C 0.5871(12) 0.9204(12) 0.8459(13) 0.067(2) Uani 1 1 d D U . . . H24A H 0.640780 0.964762 0.836690 0.080 Uiso 1 1 calc R . . . . H24B H 0.572892 0.888338 0.911052 0.080 Uiso 1 1 calc R . . . . C25 C 0.5683(11) 0.7475(10) 0.8382(14) 0.066(2) Uani 1 1 d D U . . . H25 H 0.571971 0.704508 0.903602 0.079 Uiso 1 1 calc R . . . . C26 C 0.4647(11) 0.7042(13) 0.7441(12) 0.065(2) Uani 1 1 d D U . . . C27 C 0.6828(13) 0.8622(12) 0.7488(13) 0.069(3) Uani 1 1 d D U . . . C28 C 0.6283(13) 0.7039(12) 0.7752(13) 0.067(2) Uani 1 1 d D U . . . H28 H 0.662327 0.642786 0.813067 0.080 Uiso 1 1 calc R . . . . C29 C 0.5658(14) 0.6284(12) 0.6678(10) 0.067(2) Uani 1 1 d D U . . . H29A H 0.504585 0.604317 0.660629 0.081 Uiso 1 1 calc R . . . . H29B H 0.604540 0.569154 0.696954 0.081 Uiso 1 1 calc R . . . . C30 C 0.7679(12) 0.7684(15) 0.6693(10) 0.067(2) Uani 1 1 d D U . . . H30A H 0.792675 0.700687 0.700924 0.081 Uiso 1 1 calc R . . . . H30B H 0.816585 0.817003 0.664733 0.081 Uiso 1 1 calc R . . . . C31 C 0.7009(10) 0.7060(12) 0.5567(14) 0.065(2) Uani 1 1 d D U . . . H31 H 0.736461 0.642701 0.581005 0.078 Uiso 1 1 calc R . . . . C32 C 0.5482(11) 0.7041(12) 0.5039(10) 0.061(3) Uani 1 1 d D U . . . C33 C 0.7715(13) 0.8693(11) 0.5034(10) 0.066(2) Uani 1 1 d D U . . . C34 C 0.7055(10) 0.7555(10) 0.4465(15) 0.063(2) Uani 1 1 d D U . . . H34 H 0.744687 0.716733 0.420992 0.076 Uiso 1 1 calc R . . . . C35 C 0.5785(14) 0.7702(13) 0.3365(14) 0.061(3) Uani 1 1 d . U . . . H35A H 0.623210 0.740681 0.307762 0.074 Uiso 1 1 calc R . . . . H35B H 0.518920 0.736355 0.341497 0.074 Uiso 1 1 calc R . . . . C36 C 0.7779(15) 0.9167(15) 0.3401(16) 0.070(4) Uani 1 1 d . U . . . H36A H 0.807503 0.875388 0.311812 0.084 Uiso 1 1 calc R . . . . H36B H 0.824863 0.961554 0.346459 0.084 Uiso 1 1 calc R . . . . Au1 Au 0.52184(11) 0.67760(9) 0.09867(7) 0.0697(5) Uani 0.6667 1 d . U . . . Br1 Br 0.3687(3) 0.5978(2) 0.1076(2) 0.0861(10) Uani 0.6667 1 d . U . . . Br2 Br 0.5948(3) 0.5281(2) 0.0927(3) 0.0869(11) Uani 0.6667 1 d . U . . . Br3 Br 0.6725(3) 0.7581(3) 0.0838(3) 0.1007(13) Uani 0.6667 1 d . U . . . Br4 Br 0.4478(3) 0.8290(3) 0.0985(3) 0.0911(11) Uani 0.6667 1 d . U . . . Au2 Au 0.9688(4) 1.0065(5) 0.0029(5) 0.137(2) Uani 0.3333 1 d . U . A -1 Br5 Br 0.8482(6) 0.9655(7) -0.0803(8) 0.222(6) Uani 0.3333 1 d G U . A -1 Br6 Br 1.0844(6) 0.9480(6) -0.0771(5) 0.144(3) Uani 0.3333 1 d G U . A -1 Br7 Br 1.0929(6) 1.0445(6) 0.0845(5) 0.146(4) Uani 0.3333 1 d G U . A -1 Br8 Br 0.8514(7) 1.0600(9) 0.0878(9) 0.275(8) Uani 0.3333 1 d G U . A -1 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 K1 0.069(4) 0.068(4) 0.133(6) -0.045(4) -0.023(5) -0.003(3) O1 0.067(8) 0.062(5) 0.085(8) -0.034(6) 0.002(6) -0.002(5) O2 0.044(5) 0.053(5) 0.129(11) -0.018(6) -0.012(6) -0.009(4) O3 0.047(5) 0.068(7) 0.093(7) -0.031(6) -0.010(5) 0.011(5) O4 0.048(7) 0.047(3) 0.083(8) -0.017(4) -0.005(6) 0.001(4) O5 0.052(5) 0.058(5) 0.095(7) -0.019(5) 0.005(5) -0.003(4) O6 0.077(8) 0.050(4) 0.092(8) -0.033(5) -0.013(8) 0.004(5) O7 0.073(8) 0.050(6) 0.110(9) -0.035(6) -0.010(7) -0.011(5) O8 0.073(5) 0.045(5) 0.085(8) -0.025(5) -0.003(5) -0.005(4) O9 0.059(5) 0.095(9) 0.088(8) -0.046(7) -0.009(6) -0.002(5) O10 0.064(7) 0.054(5) 0.148(11) -0.035(6) 0.006(7) -0.007(5) O11 0.056(4) 0.069(7) 0.089(7) -0.036(6) -0.012(4) -0.008(4) O12 0.058(4) 0.055(4) 0.112(7) -0.038(5) -0.011(6) -0.002(3) O13 0.09(2) 0.064(15) 0.139(11) -0.053(12) -0.045(15) 0.023(15) N1 0.038(6) 0.046(4) 0.090(6) -0.026(4) -0.007(4) -0.007(4) N2 0.041(6) 0.053(5) 0.099(6) -0.028(4) -0.001(5) -0.003(4) N3 0.048(5) 0.058(4) 0.081(5) -0.029(4) -0.007(4) 0.001(3) N4 0.049(4) 0.054(4) 0.091(6) -0.028(4) -0.006(4) -0.001(3) N5 0.050(4) 0.059(4) 0.077(6) -0.025(4) -0.005(4) 0.002(3) N6 0.050(4) 0.058(4) 0.068(6) -0.028(3) -0.008(4) 0.000(3) N7 0.049(4) 0.058(4) 0.086(5) -0.024(4) -0.008(4) 0.003(3) N8 0.046(4) 0.051(3) 0.067(5) -0.016(3) -0.003(4) 0.000(3) N9 0.046(4) 0.052(5) 0.089(5) -0.025(4) -0.008(4) 0.004(3) N10 0.046(5) 0.050(3) 0.083(5) -0.022(4) -0.008(4) 0.002(3) N11 0.046(5) 0.051(5) 0.091(5) -0.027(4) -0.006(4) -0.004(4) N12 0.041(5) 0.050(4) 0.088(5) -0.026(4) -0.012(4) -0.004(4) N13 0.072(6) 0.042(4) 0.098(7) -0.025(4) -0.013(5) -0.008(3) N14 0.070(5) 0.040(4) 0.085(7) -0.029(4) -0.012(5) -0.004(3) N15 0.071(5) 0.044(3) 0.093(6) -0.024(4) -0.006(4) -0.007(3) N16 0.069(4) 0.043(4) 0.077(6) -0.022(4) -0.011(4) -0.004(3) N17 0.058(4) 0.048(4) 0.076(5) -0.019(4) -0.006(3) -0.007(3) N18 0.058(5) 0.053(4) 0.083(5) -0.024(4) -0.016(4) -0.002(3) N19 0.060(4) 0.052(5) 0.084(4) -0.026(4) -0.010(4) -0.003(3) N20 0.054(5) 0.057(4) 0.090(5) -0.028(4) -0.014(4) 0.000(3) N21 0.057(4) 0.049(5) 0.087(4) -0.033(4) -0.014(3) -0.002(4) N22 0.057(5) 0.056(4) 0.094(4) -0.034(3) -0.014(4) -0.005(4) N23 0.051(4) 0.053(5) 0.087(4) -0.029(4) -0.013(4) 0.002(4) N24 0.055(5) 0.051(4) 0.094(4) -0.029(3) -0.012(4) 0.000(4) C1 0.035(6) 0.047(4) 0.097(7) -0.028(5) -0.003(5) -0.008(4) C2 0.047(5) 0.057(5) 0.088(6) -0.027(4) -0.006(4) 0.001(4) C3 0.046(6) 0.053(4) 0.099(6) -0.029(4) -0.002(5) 0.001(4) C4 0.050(4) 0.059(3) 0.081(5) -0.029(3) -0.008(4) 0.002(3) C5 0.051(5) 0.059(4) 0.078(6) -0.030(4) -0.005(4) -0.001(4) C6 0.048(4) 0.059(4) 0.083(7) -0.024(4) -0.010(4) -0.003(3) C7 0.052(4) 0.061(3) 0.071(5) -0.026(3) -0.008(4) 0.002(3) C8 0.050(4) 0.058(4) 0.084(6) -0.022(4) -0.008(4) 0.002(3) C9 0.051(4) 0.059(5) 0.072(6) -0.021(4) -0.007(4) 0.001(3) C10 0.049(4) 0.052(3) 0.080(5) -0.018(3) -0.006(3) 0.002(3) C11 0.046(4) 0.055(6) 0.087(5) -0.024(4) -0.007(4) 0.004(4) C12 0.041(5) 0.048(3) 0.066(6) -0.018(3) 0.000(4) 0.001(3) C13 0.048(4) 0.050(3) 0.087(5) -0.023(3) -0.006(4) 0.005(3) C14 0.053(6) 0.055(6) 0.091(5) -0.028(4) -0.007(4) 0.000(4) C15 0.048(5) 0.048(5) 0.086(5) -0.022(4) -0.010(4) 0.000(4) C16 0.045(5) 0.048(4) 0.091(6) -0.025(4) -0.006(5) -0.006(4) C17 0.046(5) 0.057(6) 0.091(5) -0.029(5) -0.005(5) -0.007(4) C18 0.024(6) 0.047(4) 0.082(5) -0.030(4) -0.015(5) -0.008(4) C19 0.070(4) 0.043(3) 0.095(6) -0.025(4) -0.013(4) -0.005(3) C20 0.073(6) 0.043(4) 0.100(7) -0.026(4) -0.011(5) -0.009(4) C21 0.069(5) 0.041(4) 0.078(7) -0.023(4) -0.010(5) -0.004(3) C22 0.069(4) 0.044(3) 0.090(6) -0.024(4) -0.008(4) -0.004(3) C23 0.064(5) 0.043(4) 0.087(6) -0.021(4) 0.001(5) -0.009(4) C24 0.069(5) 0.046(4) 0.080(6) -0.018(4) -0.009(5) -0.004(4) C25 0.061(4) 0.054(4) 0.083(5) -0.026(4) -0.011(3) -0.004(3) C26 0.060(4) 0.054(5) 0.079(5) -0.023(4) -0.011(4) -0.002(4) C27 0.057(6) 0.054(4) 0.092(6) -0.026(4) -0.011(4) -0.003(4) C28 0.059(4) 0.056(4) 0.086(5) -0.028(4) -0.012(3) -0.003(3) C29 0.060(6) 0.056(5) 0.087(4) -0.030(4) -0.013(4) -0.001(5) C30 0.055(5) 0.057(6) 0.094(4) -0.034(4) -0.011(4) -0.008(4) C31 0.056(4) 0.053(4) 0.089(4) -0.030(4) -0.015(4) -0.003(4) C32 0.054(4) 0.049(6) 0.086(4) -0.034(5) -0.012(4) -0.002(4) C33 0.053(5) 0.052(4) 0.097(4) -0.034(4) -0.011(4) 0.001(4) C34 0.051(4) 0.051(4) 0.089(4) -0.029(4) -0.015(4) 0.003(4) C35 0.048(8) 0.050(7) 0.086(4) -0.026(6) -0.013(5) 0.003(6) C36 0.055(8) 0.058(6) 0.095(5) -0.027(5) -0.013(5) -0.005(6) Au1 0.1041(11) 0.0606(7) 0.0374(5) -0.0117(5) -0.0160(7) -0.0006(6) Br1 0.101(2) 0.0637(17) 0.076(2) -0.0124(16) 0.030(2) -0.0077(16) Br2 0.083(2) 0.0655(17) 0.088(2) -0.0050(17) -0.020(2) 0.0143(16) Br3 0.104(3) 0.090(2) 0.088(2) -0.0102(19) -0.058(2) -0.0010(18) Br4 0.137(3) 0.083(2) 0.0628(19) -0.0393(18) -0.002(2) 0.002(2) Au2 0.197(7) 0.0559(19) 0.112(2) 0.0132(16) 0.008(4) -0.015(4) Br5 0.207(10) 0.093(7) 0.244(12) 0.064(6) -0.084(10) -0.047(7) Br6 0.229(10) 0.081(5) 0.075(5) 0.017(3) -0.007(6) 0.007(6) Br7 0.230(10) 0.088(6) 0.083(6) 0.005(4) 0.005(6) -0.015(7) Br8 0.238(12) 0.245(15) 0.244(14) -0.005(10) 0.118(11) 0.027(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 K1 O5 2.774(13) . ? K1 O5 2.774(13) 2_776 ? K1 O12 2.823(13) 2_776 ? K1 O12 2.823(13) . ? K1 O13 2.79(4) . ? K1 O13 2.79(4) 2_776 ? O1 C5 1.24(2) . ? O2 C6 1.24(2) . ? O3 C11 1.16(2) . ? O4 C12 1.233(19) . ? O5 C17 1.28(2) . ? O6 C18 1.275(19) . ? O7 C20 1.139(19) . ? O8 C21 1.19(2) . ? O9 C26 1.22(2) . ? O10 C27 1.23(2) . ? O11 C32 1.155(18) . ? O12 C33 1.140(18) . ? N1 C1 1.48(2) . ? N1 C2 1.45(3) . ? N1 C18 1.31(3) 2_766 ? N2 C1 1.45(2) . ? N2 C3 1.45(3) . ? N2 C17 1.26(2) 2_766 ? N3 C2 1.50(3) . ? N3 C4 1.38(3) . ? N3 C5 1.34(2) . ? N4 C3 1.50(3) . ? N4 C4 1.44(2) . ? N4 C6 1.34(3) . ? N5 C5 1.35(3) . ? N5 C7 1.43(2) . ? N5 C8 1.40(3) . ? N6 C6 1.35(2) . ? N6 C7 1.39(2) . ? N6 C9 1.43(3) . ? N7 C8 1.44(3) . ? N7 C10 1.56(3) . ? N7 C11 1.38(3) . ? N8 C9 1.40(2) . ? N8 C10 1.44(2) . ? N8 C12 1.36(2) . ? N9 C11 1.41(3) . ? N9 C13 1.49(3) . ? N9 C14 1.41(3) . ? N10 C12 1.39(2) . ? N10 C13 1.43(2) . ? N10 C15 1.50(2) . ? N11 C14 1.41(3) . ? N11 C16 1.45(2) . ? N11 C17 1.42(3) . ? N12 C15 1.48(3) . ? N12 C16 1.46(2) . ? N12 C18 1.35(2) . ? N13 C19 1.421(8) . ? N13 C20 1.411(8) . ? N13 C36 1.57(2) 2_676 ? N14 C19 1.418(8) . ? N14 C21 1.408(8) . ? N14 C35 1.46(2) 2_676 ? N15 C20 1.407(8) . ? N15 C22 1.422(8) . ? N15 C23 1.407(8) . ? N16 C21 1.415(8) . ? N16 C22 1.415(8) . ? N16 C24 1.412(8) . ? N17 C23 1.413(8) . ? N17 C25 1.422(8) . ? N17 C26 1.409(8) . ? N18 C24 1.405(8) . ? N18 C25 1.424(8) . ? N18 C27 1.406(8) . ? N19 C26 1.408(8) . ? N19 C28 1.43(2) . ? N19 C29 1.415(8) . ? N20 C27 1.403(8) . ? N20 C28 1.418(8) . ? N20 C30 1.413(8) . ? N21 C29 1.420(8) . ? N21 C31 1.413(8) . ? N21 C32 1.412(8) . ? N22 C30 1.416(8) . ? N22 C31 1.422(8) . ? N22 C33 1.416(8) . ? N23 C32 1.409(8) . ? N23 C34 1.419(8) . ? N23 C35 1.46(2) . ? N24 C33 1.414(8) . ? N24 C34 1.412(8) . ? N24 C36 1.40(3) . ? C1 C16 1.52(3) 2_766 ? C4 C7 1.61(3) . ? C10 C13 1.43(3) . ? C19 C22 1.46(2) . ? C25 C28 1.61(3) . ? C31 C34 1.61(3) . ? Au1 Br1 2.453(4) . ? Au1 Br2 2.422(4) . ? Au1 Br3 2.414(5) . ? Au1 Br4 2.416(4) . ? Au2 Br5 2.4218 . ? Au2 Br6 2.4144 . ? Au2 Br7 2.4217 . ? Au2 Br8 2.4439 . ? 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 O5 K1 O5 180.0(5) . 2_776 ? O5 K1 O12 89.8(4) 2_776 2_776 ? O5 K1 O12 90.2(4) 2_776 . ? O5 K1 O12 90.2(4) . 2_776 ? O5 K1 O12 89.8(4) . . ? O5 K1 O13 100.9(6) . . ? O5 K1 O13 79.1(6) 2_776 . ? O5 K1 O13 100.9(6) 2_776 2_776 ? O5 K1 O13 79.1(6) . 2_776 ? O12 K1 O12 180.0 . 2_776 ? O13 K1 O12 80.5(8) . 2_776 ? O13 K1 O12 80.5(8) 2_776 . ? O13 K1 O12 99.5(8) . . ? O13 K1 O12 99.5(8) 2_776 2_776 ? O13 K1 O13 180.0 . 2_776 ? C17 O5 K1 142.5(12) . . ? C33 O12 K1 140.2(13) . . ? C2 N1 C1 119.1(16) . . ? C18 N1 C1 113.0(16) 2_766 . ? C18 N1 C2 122.5(15) 2_766 . ? C3 N2 C1 122.3(17) . . ? C17 N2 C1 114.3(19) 2_766 . ? C17 N2 C3 121.6(18) 2_766 . ? C4 N3 C2 124.8(16) . . ? C5 N3 C2 120.5(17) . . ? C5 N3 C4 114.2(19) . . ? C4 N4 C3 124.1(16) . . ? C6 N4 C3 119.1(16) . . ? C6 N4 C4 114.1(17) . . ? C5 N5 C7 115.1(17) . . ? C5 N5 C8 125.5(18) . . ? C8 N5 C7 118.3(19) . . ? C6 N6 C7 114.8(18) . . ? C6 N6 C9 124.1(16) . . ? C7 N6 C9 121.0(16) . . ? C8 N7 C10 124.6(17) . . ? C11 N7 C8 124.0(18) . . ? C11 N7 C10 111.3(16) . . ? C9 N8 C10 128.3(16) . . ? C12 N8 C9 121.2(15) . . ? C12 N8 C10 108.6(15) . . ? C11 N9 C13 110.7(17) . . ? C14 N9 C11 121.8(18) . . ? C14 N9 C13 126.2(17) . . ? C12 N10 C13 110.4(15) . . ? C12 N10 C15 119.1(14) . . ? C13 N10 C15 130.3(15) . . ? C14 N11 C16 124.6(18) . . ? C14 N11 C17 127.0(17) . . ? C17 N11 C16 107.7(16) . . ? C16 N12 C15 124.0(16) . . ? C18 N12 C15 123.5(16) . . ? C18 N12 C16 111.0(17) . . ? C19 N13 C36 125.8(14) . 2_676 ? C20 N13 C19 117.1(13) . . ? C20 N13 C36 115.9(13) . 2_676 ? C19 N14 C35 129.0(15) . 2_676 ? C21 N14 C19 112.1(13) . . ? C21 N14 C35 118.5(13) . 2_676 ? C20 N15 C22 112.5(13) . . ? C23 N15 C20 125.0(13) . . ? C23 N15 C22 121.6(14) . . ? C22 N16 C21 109.3(12) . . ? C24 N16 C21 121.5(14) . . ? C24 N16 C22 128.2(15) . . ? C23 N17 C25 120.7(16) . . ? C26 N17 C23 121.7(14) . . ? C26 N17 C25 115.5(14) . . ? C24 N18 C25 129.0(16) . . ? C24 N18 C27 119.8(14) . . ? C27 N18 C25 111.2(14) . . ? C26 N19 C28 116.1(14) . . ? C26 N19 C29 116.2(15) . . ? C29 N19 C28 127.7(16) . . ? C27 N20 C28 107.6(14) . . ? C27 N20 C30 124.4(14) . . ? C30 N20 C28 124.9(15) . . ? C31 N21 C29 126.2(15) . . ? C32 N21 C29 117.2(14) . . ? C32 N21 C31 114.1(13) . . ? C30 N22 C31 125.6(15) . . ? C30 N22 C33 120.3(13) . . ? C33 N22 C31 113.3(13) . . ? C32 N23 C34 117.2(15) . . ? C32 N23 C35 119.2(13) . . ? C34 N23 C35 121.3(17) . . ? C34 N24 C33 114.6(14) . . ? C36 N24 C33 118.5(14) . . ? C36 N24 C34 122.7(17) . . ? N1 C1 C16 101.0(16) . 2_766 ? N2 C1 N1 111.9(16) . . ? N2 C1 C16 102.3(15) . 2_766 ? N1 C2 N3 109.1(15) . . ? N2 C3 N4 109.4(16) . . ? N3 C4 N4 114.3(19) . . ? N3 C4 C7 104.5(15) . . ? N4 C4 C7 100.3(16) . . ? O1 C5 N3 129(2) . . ? O1 C5 N5 123.8(19) . . ? N3 C5 N5 107.4(17) . . ? O2 C6 N4 129.0(19) . . ? O2 C6 N6 123(2) . . ? N4 C6 N6 107.8(16) . . ? N5 C7 C4 98.8(16) . . ? N6 C7 N5 119.8(17) . . ? N6 C7 C4 102.6(15) . . ? N5 C8 N7 118.1(16) . . ? N8 C9 N6 118.5(18) . . ? N8 C10 N7 107.9(16) . . ? C13 C10 N7 103.0(17) . . ? C13 C10 N8 107.6(15) . . ? O3 C11 N7 126.6(19) . . ? O3 C11 N9 126(2) . . ? N7 C11 N9 107.0(18) . . ? O4 C12 N8 125.7(17) . . ? O4 C12 N10 125.9(16) . . ? N8 C12 N10 108.3(14) . . ? N10 C13 N9 111.8(18) . . ? N10 C13 C10 104.3(15) . . ? C10 C13 N9 107.8(17) . . ? N9 C14 N11 116.7(16) . . ? N12 C15 N10 111.8(17) . . ? N11 C16 N12 116.9(16) . . ? N11 C16 C1 104.9(17) . 2_766 ? N12 C16 C1 104.3(15) . 2_766 ? O5 C17 N11 118.7(19) . . ? N2 C17 O5 130(2) 2_766 . ? N2 C17 N11 110.7(18) 2_766 . ? O6 C18 N1 127.6(18) . 2_766 ? O6 C18 N12 122.6(19) . . ? N1 C18 N12 109.8(14) 2_766 . ? N13 C19 C22 100.7(13) . . ? N14 C19 N13 113.9(15) . . ? N14 C19 C22 104.1(14) . . ? O7 C20 N13 129.1(14) . . ? O7 C20 N15 130.1(13) . . ? N15 C20 N13 100.8(12) . . ? O8 C21 N14 130.0(13) . . ? O8 C21 N16 123.9(13) . . ? N14 C21 N16 106.0(12) . . ? N15 C22 C19 107.5(13) . . ? N16 C22 N15 122.1(15) . . ? N16 C22 C19 108.3(13) . . ? N15 C23 N17 117.6(15) . . ? N18 C24 N16 112.1(14) . . ? N17 C25 N18 113.3(13) . . ? N17 C25 C28 102.5(14) . . ? N18 C25 C28 101.8(14) . . ? O9 C26 N17 128.5(14) . . ? O9 C26 N19 127.7(15) . . ? N19 C26 N17 103.6(13) . . ? O10 C27 N18 125.4(14) . . ? O10 C27 N20 122.8(16) . . ? N20 C27 N18 111.8(14) . . ? N19 C28 C25 101.5(13) . . ? N20 C28 N19 115.2(16) . . ? N20 C28 C25 107.2(13) . . ? N19 C29 N21 115.4(14) . . ? N20 C30 N22 111.5(15) . . ? N21 C31 N22 115.6(14) . . ? N21 C31 C34 104.5(13) . . ? N22 C31 C34 103.6(13) . . ? O11 C32 N21 129.1(16) . . ? O11 C32 N23 127.7(14) . . ? N23 C32 N21 103.3(12) . . ? O12 C33 N22 130.2(16) . . ? O12 C33 N24 124.3(15) . . ? N24 C33 N22 105.4(12) . . ? N23 C34 C31 100.0(15) . . ? N24 C34 N23 114.8(13) . . ? N24 C34 C31 102.4(14) . . ? N14 C35 N23 112.4(15) 2_676 . ? N24 C36 N13 110.6(18) . 2_676 ? Br2 Au1 Br1 89.01(13) . . ? Br3 Au1 Br1 177.89(14) . . ? Br3 Au1 Br2 90.72(15) . . ? Br3 Au1 Br4 89.62(16) . . ? Br4 Au1 Br1 90.57(15) . . ? Br4 Au1 Br2 177.79(12) . . ? Br5 Au2 Br8 90.9 . . ? Br6 Au2 Br5 89.1 . . ? Br6 Au2 Br7 89.1 . . ? Br6 Au2 Br8 178.1 . . ? Br7 Au2 Br5 178.2 . . ? Br7 Au2 Br8 90.9 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C1 H1 O9 0.98 2.25 3.11(3) 146.6 2_666 yes C3 H3A O7 0.97 2.56 3.23(2) 126.3 2_666 yes C14 H14B O10 0.97 2.55 3.28(2) 132.0 2_776 yes C16 H16 O8 0.98 2.34 3.19(3) 145.8 2_776 yes C30 H30A O2 0.97 2.55 3.26(2) 130.8 2_766 yes C31 H31 O4 0.98 2.31 3.19(2) 149.0 2_766 yes C36 H36A O3 0.97 2.46 3.20(3) 133.2 . yes _shelx_res_file ; TITL twin_twin1_hklf4 in P-1 twin_twin1_hklf5_sq.res created by SHELXL-2017/1 at 12:40:47 on 07-Jan-2020 REM P-1 (#2 in standard setting) CELL 0.71073 14.329904 14.377221 15.985301 66.2279 88.4679 89.7814 ZERR 2 0.001394 0.001052 0.001151 0.0069 0.0069 0.0069 LATT 1 SFAC C H Au Br K N O UNIT 72 72 2 8 1 48 25 EQIV $1 1-X,1-Y,1-Z EQIV $2 2-X,2-Y,1-Z EQIV $3 2-X,1-Y,1-Z SADI 0.01 N15 C23 N16 C24 N18 C24 N22 C31 N21 C31 N21 C29 N22 C30 N22 C33 = N24 C33 N24 C34 N23 C34 N23 C32 N19 C29 N20 C30 N20 C28 N18 C27 N18 C25 N17 = C25 N17 C23 N17 C26 N16 C21 N14 C21 N14 C19 N13 C19 N13 C20 N15 C20 N15 C22 = N16 C22 N20 C27 N19 C26 N21 C32 SIMU 0.01 0.02 2 RIGU 0.001 0.001 ISOR 0.01 0.02 Au2 Br5 Br6 Br7 Br8 L.S. 5 0 68 PLAN 20 HTAB C1 O9_$1 HTAB C3 O7_$1 HTAB C14 O10_$2 HTAB C16 O8_$2 HTAB C30 O2_$3 HTAB C31 O4_$3 HTAB C36 O3 list 8 ABIN fmap 2 53 acta SHEL 99999 0.77 REM REM REM WGHT 0.200000 BASF 0.31481 FVAR 0.18351 K1 5 1.000000 1.000000 0.500000 10.50000 0.06912 0.07015 = 0.12882 -0.04578 -0.02015 -0.00520 O1 7 0.788752 0.696915 0.293569 11.00000 0.06765 0.06300 = 0.08701 -0.03592 0.00205 -0.00163 O2 7 1.040209 0.363661 0.285216 11.00000 0.04477 0.05065 = 0.12310 -0.02241 -0.01321 -0.00898 O3 7 0.971133 0.838361 0.289535 11.00000 0.04952 0.07278 = 0.09659 -0.03502 -0.00926 0.01056 O4 7 1.215256 0.496741 0.293557 11.00000 0.04330 0.04718 = 0.08484 -0.01822 -0.00691 -0.00164 O5 7 1.059823 0.814259 0.507241 11.00000 0.05126 0.05725 = 0.09594 -0.01817 0.00475 -0.00454 O6 7 1.315708 0.465828 0.499199 11.00000 0.08226 0.04854 = 0.09035 -0.03121 -0.01005 0.00247 O7 7 0.254037 0.870499 0.711586 11.00000 0.07335 0.05095 = 0.10827 -0.03420 -0.00762 -0.01127 O8 7 0.593689 1.117827 0.703348 11.00000 0.07133 0.04713 = 0.08463 -0.02409 -0.00337 -0.00244 O9 7 0.393602 0.693436 0.708758 11.00000 0.06016 0.09693 = 0.08994 -0.04718 -0.01054 -0.00230 O10 7 0.733742 0.937631 0.719095 11.00000 0.06174 0.05242 = 0.14070 -0.03223 0.00040 -0.00386 O11 7 0.469614 0.683614 0.503532 11.00000 0.05747 0.06868 = 0.08996 -0.03532 -0.01255 -0.00828 O12 7 0.812538 0.938529 0.498299 11.00000 0.05780 0.05418 = 0.11196 -0.03800 -0.00907 -0.00306 O13 7 1.014417 0.971647 0.682934 10.50000 0.08219 0.06444 = 0.12806 -0.04386 -0.02871 0.00567 N1 6 0.723222 0.432059 0.423046 11.00000 0.03945 0.04588 = 0.08923 -0.02682 -0.00513 -0.00833 N2 6 0.818844 0.294765 0.421543 11.00000 0.03928 0.05359 = 0.09636 -0.02858 -0.00161 -0.00270 N3 6 0.784730 0.544350 0.275900 11.00000 0.04863 0.05817 = 0.07986 -0.02914 -0.00605 0.00058 N4 6 0.885094 0.413479 0.276187 11.00000 0.04846 0.05427 = 0.09007 -0.02745 -0.00545 -0.00112 N5 6 0.890797 0.657581 0.200614 11.00000 0.04968 0.05870 = 0.07771 -0.02597 -0.00554 0.00228 N6 6 0.989494 0.520953 0.193177 11.00000 0.04966 0.05764 = 0.06742 -0.02853 -0.00730 -0.00070 N7 6 1.024107 0.763695 0.194817 11.00000 0.04948 0.05857 = 0.08713 -0.02583 -0.00742 0.00281 N8 6 1.121813 0.624781 0.198544 11.00000 0.04486 0.05168 = 0.06836 -0.01637 -0.00249 -0.00113 N9 6 1.126848 0.797711 0.281622 11.00000 0.04755 0.05218 = 0.09009 -0.02627 -0.00771 0.00346 N10 6 1.227570 0.665992 0.276832 11.00000 0.04635 0.04926 = 0.08411 -0.02292 -0.00797 0.00095 N11 6 1.184741 0.776085 0.428319 11.00000 0.04707 0.05097 = 0.09151 -0.02760 -0.00600 -0.00520 N12 6 1.287505 0.636426 0.427875 11.00000 0.04341 0.04895 = 0.08881 -0.02618 -0.01162 -0.00495 N13 6 0.301209 1.018721 0.722453 11.00000 0.07096 0.04295 = 0.09695 -0.02457 -0.01117 -0.00820 N14 6 0.431020 1.122127 0.721993 11.00000 0.06839 0.04165 = 0.08524 -0.02996 -0.01182 -0.00293 N15 6 0.367623 0.878058 0.808859 11.00000 0.07281 0.04510 = 0.09390 -0.02423 -0.00630 -0.00652 N16 6 0.509628 0.978984 0.801613 11.00000 0.06968 0.04456 = 0.07940 -0.02306 -0.01055 -0.00304 N17 6 0.476836 0.751373 0.805330 11.00000 0.05873 0.05012 = 0.07762 -0.02043 -0.00765 -0.00658 N18 6 0.609368 0.844987 0.814246 11.00000 0.05944 0.05281 = 0.08485 -0.02477 -0.01624 -0.00143 N19 6 0.556600 0.680219 0.726472 11.00000 0.06034 0.05345 = 0.08539 -0.02725 -0.01162 -0.00285 N20 6 0.690591 0.782093 0.720756 11.00000 0.05415 0.05643 = 0.09085 -0.02722 -0.01536 0.00055 N21 6 0.604686 0.686775 0.580132 11.00000 0.05797 0.04912 = 0.08843 -0.03284 -0.01445 -0.00175 N22 6 0.742212 0.782098 0.579817 11.00000 0.05828 0.05549 = 0.09491 -0.03299 -0.01387 -0.00470 N23 6 0.609624 0.752243 0.428466 11.00000 0.05144 0.05145 = 0.08845 -0.02920 -0.01403 0.00269 N24 6 0.741655 0.853673 0.426251 11.00000 0.05465 0.05001 = 0.09462 -0.02777 -0.01343 0.00065 C1 1 0.728103 0.321858 0.444230 11.00000 0.03516 0.04740 = 0.09551 -0.02919 -0.00293 -0.00760 AFIX 13 H1 2 0.676867 0.297112 0.419078 11.00000 -1.20000 AFIX 0 C2 1 0.695600 0.502524 0.334462 11.00000 0.04835 0.05638 = 0.08653 -0.02839 -0.00432 0.00111 AFIX 23 H2A 2 0.660111 0.557539 0.339828 11.00000 -1.20000 H2B 2 0.656810 0.468525 0.306421 11.00000 -1.20000 AFIX 0 C3 1 0.845818 0.307203 0.329006 11.00000 0.04475 0.05273 = 0.09685 -0.02906 -0.00161 0.00098 AFIX 23 H3A 2 0.791897 0.296639 0.298378 11.00000 -1.20000 H3B 2 0.892479 0.257207 0.331383 11.00000 -1.20000 AFIX 0 C4 1 0.829364 0.498873 0.225082 11.00000 0.04981 0.05810 = 0.08048 -0.02930 -0.00638 0.00155 AFIX 13 H4 2 0.786509 0.483790 0.185351 11.00000 -1.20000 AFIX 0 C5 1 0.817740 0.635971 0.261301 11.00000 0.05012 0.05873 = 0.07849 -0.02996 -0.00506 -0.00022 C6 1 0.976632 0.425792 0.253304 11.00000 0.04769 0.05820 = 0.08225 -0.02518 -0.00809 -0.00282 C7 1 0.908536 0.579348 0.167777 11.00000 0.05097 0.06087 = 0.07059 -0.02582 -0.00787 0.00129 AFIX 13 H7 2 0.899100 0.604157 0.101847 11.00000 -1.20000 AFIX 0 C8 1 0.934686 0.749052 0.159451 11.00000 0.04981 0.05806 = 0.08555 -0.02295 -0.00745 0.00189 AFIX 23 H8A 2 0.892258 0.800590 0.162091 11.00000 -1.20000 H8B 2 0.944679 0.762159 0.095408 11.00000 -1.20000 AFIX 0 C9 1 1.080178 0.564807 0.157441 11.00000 0.05059 0.05866 = 0.07170 -0.02084 -0.00684 -0.00022 AFIX 23 H9A 2 1.122457 0.509879 0.163052 11.00000 -1.20000 H9B 2 1.074674 0.606601 0.092702 11.00000 -1.20000 AFIX 0 C10 1 1.119998 0.734431 0.167242 11.00000 0.04912 0.05192 = 0.08067 -0.01894 -0.00590 0.00183 AFIX 13 H10 2 1.134449 0.769669 0.101630 11.00000 -1.20000 AFIX 0 C11 1 1.031771 0.800838 0.260583 11.00000 0.04754 0.05703 = 0.08798 -0.02576 -0.00688 0.00404 C12 1 1.189754 0.586721 0.259838 11.00000 0.04015 0.04823 = 0.06731 -0.01836 0.00044 -0.00131 C13 1 1.184562 0.760262 0.222968 11.00000 0.04871 0.05049 = 0.08765 -0.02368 -0.00677 0.00416 AFIX 13 H13 2 1.230607 0.811208 0.185399 11.00000 -1.20000 AFIX 0 C14 1 1.160531 0.843372 0.338573 11.00000 0.05455 0.05508 = 0.09158 -0.02829 -0.00697 -0.00033 AFIX 23 H14A 2 1.113244 0.889451 0.343580 11.00000 -1.20000 H14B 2 1.215194 0.883931 0.308665 11.00000 -1.20000 AFIX 0 C15 1 1.312852 0.646151 0.333792 11.00000 0.04824 0.04709 = 0.08714 -0.02269 -0.01017 -0.00128 AFIX 23 H15A 2 1.342269 0.584059 0.336765 11.00000 -1.20000 H15B 2 1.357208 0.701562 0.305598 11.00000 -1.20000 AFIX 0 C16 1 1.272003 0.723049 0.453453 11.00000 0.04677 0.04688 = 0.09082 -0.02526 -0.00502 -0.00678 AFIX 13 H16 2 1.323924 0.771568 0.429413 11.00000 -1.20000 AFIX 0 C17 1 1.136937 0.761563 0.509835 11.00000 0.04594 0.05756 = 0.09210 -0.02854 -0.00495 -0.00792 C18 1 1.294037 0.550927 0.502955 11.00000 0.02790 0.04598 = 0.08380 -0.03016 -0.01438 -0.00824 C19 1 0.361730 1.051086 0.774646 11.00000 0.06922 0.04372 = 0.09587 -0.02597 -0.01164 -0.00455 AFIX 13 H19 2 0.327346 1.073950 0.816639 11.00000 -1.20000 AFIX 0 C20 1 0.299025 0.913663 0.741972 11.00000 0.07314 0.04375 = 0.09895 -0.02600 -0.00961 -0.00861 C21 1 0.521215 1.080205 0.736256 11.00000 0.06863 0.04314 = 0.07842 -0.02380 -0.01006 -0.00252 C22 1 0.413420 0.958018 0.822881 11.00000 0.06990 0.04520 = 0.09110 -0.02471 -0.00808 -0.00331 AFIX 13 H22 2 0.405305 0.942882 0.888160 11.00000 -1.20000 AFIX 0 C23 1 0.399024 0.777015 0.847626 11.00000 0.06470 0.04474 = 0.08788 -0.02202 -0.00025 -0.00879 AFIX 23 H23A 2 0.347430 0.733069 0.848621 11.00000 -1.20000 H23B 2 0.414081 0.761216 0.910685 11.00000 -1.20000 AFIX 0 C24 1 0.586343 0.919878 0.846830 11.00000 0.06943 0.04609 = 0.08247 -0.01818 -0.00921 -0.00322 AFIX 23 H24A 2 0.639971 0.964051 0.838321 11.00000 -1.20000 H24B 2 0.571602 0.887341 0.911855 11.00000 -1.20000 AFIX 0 C25 1 0.568725 0.747254 0.837993 11.00000 0.06227 0.05432 = 0.08379 -0.02638 -0.01269 -0.00409 AFIX 13 H25 2 0.572714 0.703973 0.903335 11.00000 -1.20000 AFIX 0 C26 1 0.465005 0.705093 0.743671 11.00000 0.06024 0.05640 = 0.08145 -0.02549 -0.01238 -0.00146 C27 1 0.682765 0.862046 0.749545 11.00000 0.05639 0.05350 = 0.09261 -0.02570 -0.01334 -0.00176 C28 1 0.627487 0.704357 0.775557 11.00000 0.06006 0.05669 = 0.08667 -0.02848 -0.01317 -0.00225 AFIX 13 H28 2 0.661376 0.643093 0.813391 11.00000 -1.20000 AFIX 0 C29 1 0.565980 0.627966 0.668340 11.00000 0.06141 0.05565 = 0.08816 -0.03015 -0.01380 -0.00099 AFIX 23 H29A 2 0.504886 0.603481 0.661493 11.00000 -1.20000 H29B 2 0.605108 0.569095 0.697626 11.00000 -1.20000 AFIX 0 C30 1 0.767137 0.769442 0.668836 11.00000 0.05658 0.05777 = 0.09529 -0.03375 -0.01206 -0.00645 AFIX 23 H30A 2 0.792644 0.702009 0.700401 11.00000 -1.20000 H30B 2 0.815484 0.818465 0.664171 11.00000 -1.20000 AFIX 0 C31 1 0.700400 0.706781 0.556375 11.00000 0.05740 0.05218 = 0.09075 -0.02928 -0.01588 -0.00237 AFIX 13 H31 2 0.736122 0.643627 0.580918 11.00000 -1.20000 AFIX 0 C32 1 0.548463 0.703541 0.504199 11.00000 0.05505 0.04778 = 0.08756 -0.03428 -0.01251 -0.00145 C33 1 0.771441 0.870004 0.502956 11.00000 0.05336 0.05086 = 0.09810 -0.03275 -0.01156 0.00071 C34 1 0.705964 0.755288 0.445887 11.00000 0.05194 0.04951 = 0.09052 -0.02842 -0.01576 0.00275 AFIX 13 H34 2 0.745002 0.716233 0.420584 11.00000 -1.20000 AFIX 0 C35 1 0.578013 0.769879 0.336795 11.00000 0.04869 0.04811 = 0.08668 -0.02611 -0.01374 0.00435 AFIX 23 H35A 2 0.622095 0.739447 0.308311 11.00000 -1.20000 H35B 2 0.518069 0.736518 0.342266 11.00000 -1.20000 AFIX 0 C36 1 0.776067 0.915710 0.340104 11.00000 0.05345 0.05688 = 0.09553 -0.02655 -0.01495 -0.00441 AFIX 23 H36A 2 0.804798 0.873954 0.311839 11.00000 -1.20000 H36B 2 0.823949 0.960130 0.345835 11.00000 -1.20000 AFIX 0 AU1 3 0.521905 0.677597 0.098715 10.66667 0.10227 0.06103 = 0.03746 -0.01207 -0.01574 -0.00048 BR1 4 0.368627 0.597888 0.107565 10.66667 0.10073 0.06385 = 0.07601 -0.01274 0.02950 -0.00854 BR2 4 0.594771 0.528012 0.092712 10.66667 0.08728 0.06460 = 0.08664 -0.00391 -0.01990 0.01522 BR3 4 0.672747 0.757942 0.083819 10.66667 0.10426 0.08864 = 0.08727 -0.00959 -0.05798 -0.00141 BR4 4 0.447936 0.829128 0.098257 10.66667 0.13698 0.08164 = 0.06317 -0.03834 -0.00221 0.00160 PART -1 AFIX 6 AU2 3 0.969240 1.006411 0.002658 10.33333 0.19932 0.05555 = 0.10997 0.01245 0.00851 -0.01384 BR5 4 0.848128 0.966110 -0.080462 10.33333 0.20254 0.09279 = 0.24331 0.06333 -0.08035 -0.04744 BR6 4 1.084205 0.947289 -0.077429 10.33333 0.22383 0.08076 = 0.07522 0.01910 -0.00462 0.00499 BR7 4 1.093831 1.043681 0.084138 10.33333 0.22306 0.08675 = 0.08309 0.00715 0.00568 -0.01329 BR8 4 0.852454 1.060602 0.087585 10.33333 0.23375 0.24224 = 0.24181 -0.00442 0.11839 0.02511 AFIX 0 HKLF 5 REM twin_twin1_hklf4 in P-1 REM R1 = 0.1496 for 7954 Fo > 4sig(Fo) and 0.2273 for all 15237 data REM 746 parameters refined using 1758 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 2.570, deepest hole -1.514, 1-sigma level 0.226 Q1 1 0.3903 0.7239 0.0883 11.00000 0.05 2.57 Q2 1 1.0256 0.9596 -0.0638 11.00000 0.05 2.56 Q3 1 0.8198 1.0060 -0.0050 11.00000 0.05 1.82 Q4 1 0.5159 0.6384 0.1718 11.00000 0.05 1.74 Q5 1 0.6357 0.6753 0.0791 11.00000 0.05 1.70 Q6 1 0.8704 1.0007 -0.0065 11.00000 0.05 1.53 Q7 1 0.5408 0.8210 0.0846 11.00000 0.05 1.51 Q8 1 0.5293 0.8024 0.0965 11.00000 0.05 1.38 Q9 1 0.8215 1.0431 0.0551 11.00000 0.05 1.28 Q10 1 0.4679 0.5513 0.0804 11.00000 0.05 1.12 Q11 1 0.5184 0.7153 0.0256 11.00000 0.05 1.12 Q12 1 0.5129 0.5621 0.0952 11.00000 0.05 1.11 Q13 1 0.6786 0.8367 0.0755 11.00000 0.05 1.04 Q14 1 0.7447 1.0206 -0.0200 11.00000 0.05 0.98 Q15 1 0.3315 0.5566 0.0605 11.00000 0.05 0.97 Q16 1 1.2523 0.8069 -0.0007 11.00000 0.05 0.89 Q17 1 0.6723 0.7135 0.0398 11.00000 0.05 0.88 Q18 1 0.6063 0.5849 0.1007 11.00000 0.05 0.87 Q19 1 1.0620 0.8982 0.6631 11.00000 0.05 0.81 Q20 1 0.5583 0.5032 0.0588 11.00000 0.05 0.80 ; _shelx_res_checksum 29912 _shelx_hkl_file ; 0 0 2 168.357 2.34269 -2 0 0 2 168.357 2.34269 1 0 0 3 314.091 2.37676 -2 0 0 3 314.091 2.37676 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12-0.06223 3.69273 2 11 2 -8-3.35376 3.32717 2 11 9 18-4.65525 4.86846 2 11 10 -6-1.71938 3.98391 2 11 10 -5 6.72265 3.91846 2 11 10 -4 5.72450 3.84934 2 11 10 -3-2.27419 2.79191 2 11 10 -2 2.67911 2.78933 2 11 10 -1 1.15821 2.50910 2 11 10 0 3.74774 2.50364 2 11 10 1 1.80057 2.02286 2 11 10 2 0.93421 1.97898 2 -11 -10 -3 4.50005 3.62235 2 -11 -10 -4-1.53158 3.65155 2 -11 -10 -5 0.59890 2.69823 2 -11 -10 -6-1.95595 2.74303 2 -11 -10 -7 0.79913 2.75295 2 -11 -10 -8 1.70773 2.55982 2 11 10 9-4.34849 3.86397 2 11 10 13 0.60152 3.83562 2 11 10 14 1.00977 5.45794 2 11 10 15-1.98906 5.40768 2 11 10 16 1.00118 3.48949 2 11 10 18 4.51458 4.86795 2 12 -10 -9 2.25400 2.84106 2 12 -9 -10 2.85605 2.35337 2 12 -9 -9 4.46744 2.76711 2 12 -9 -8-2.86651 2.92387 2 12 -9 -7 1.03155 3.18974 2 12 -9 -6 0.88068 3.55425 2 12 -9 -5-0.69134 3.36004 2 12 -9 -4 1.98747 3.37793 2 12 -9 -2-2.07837 3.06971 2 12 -9 -1 5.48232 2.91382 2 12 -9 0-0.77417 2.84148 2 12 -9 1 0.87241 2.61967 2 12 -9 2 2.80186 2.34699 2 12 -8 -10-0.76729 2.49596 2 12 -8 -9-1.38090 2.17944 2 12 -8 -8 3.02563 2.25388 2 12 -8 -7 0.76442 2.32583 2 12 -8 -6 2.79922 2.39623 2 12 -8 -5-0.74343 2.49373 2 12 -8 -4 3.67280 2.39566 2 12 -8 -3 3.86516 3.13466 2 12 -8 -2-2.14235 3.00468 2 12 -8 -1 1.48359 2.90634 2 12 -8 0 5.12884 2.80409 2 12 -8 1 0.54778 2.67524 2 12 -8 2 2.43917 2.46119 2 12 -8 3-1.42610 2.15409 2 12 -7 -15 6.48095 4.41480 2 12 -7 -14 8.93463 4.44164 2 12 -7 -11-2.05637 2.28252 2 12 -7 -10-2.57988 2.18487 2 12 -7 -9 0.96687 2.12066 2 12 -7 -8 1.21742 2.32226 2 12 -7 -7 4.07593 2.32660 2 12 -7 -6 7.28007 2.32907 2 12 -7 -5 3.87440 2.34333 2 12 -7 -4 3.69605 2.42052 2 12 -7 -3 2.91501 2.30084 2 12 -7 -2 1.42775 2.97311 2 12 -7 -1 4.32475 2.92474 2 12 -7 0 0.28435 2.77329 2 12 -7 1 0.08626 2.73807 2 12 -7 2 1.76689 2.50259 2 12 -7 3-1.44163 2.33595 2 12 -7 4 2.76226 1.98426 2 12 -6 5-0.46681 1.97192 2 12 -6 6 0.33193 1.34411 2 12 1 -10-0.95250 3.60368 2 12 1 -9 2.49449 3.55226 2 12 1 -8 2.18220 3.39614 2 12 1 -7 2.16629 3.33679 2 12 1 -6 1.69286 3.27072 2 12 1 -5 7.38339 3.30817 2 12 1 -4 15.0104 3.24692 2 -12 -1 3 3.67282 2.04920 2 12 1 -2-1.69153 3.09262 2 12 1 -1 8.00312 3.33310 2 12 1 0 26.1050 3.42041 2 12 1 1 3.69597 3.32257 2 12 1 2 21.8613 3.64345 2 12 1 3 1.51001 3.37002 2 12 1 4-2.05349 3.52780 2 12 1 5 6.22967 3.78216 2 12 1 6 15.5101 3.94312 2 12 1 10 0.17921 4.57313 2 12 1 11 2.44895 4.64972 2 12 1 12 0.02367 2.55676 2 12 1 13 1.66786 2.54968 2 12 1 14-4.25431 4.99780 2 -12 -2 13 0.80613 3.75702 2 -12 -2 12-1.11597 3.66279 2 12 2 -11-1.71509 2.79284 2 -12 -2 10-1.65102 3.52996 2 12 2 -9 2.86624 2.59133 2 12 2 -8 1.98706 2.44352 2 12 2 -7 1.55460 3.52579 2 12 2 -6 3.85321 3.47565 2 12 2 -5-1.29939 3.29520 2 12 2 -4 8.58029 3.38515 2 12 2 -3 4.03794 3.34703 2 12 2 -2 7.06438 3.04220 2 12 2 0 0.03006 3.21529 2 12 2 4 1.76305 3.46917 2 12 2 13 0.81662 3.26814 2 12 10 0-0.74443 4.47708 2 12 10 2 0.95461 4.24709 2 12 10 5 3.63858 4.14386 2 12 10 6-0.38873 4.01477 2 12 10 7 1.94845 4.16308 2 12 10 8-3.61734 4.07372 2 12 10 9 3.23373 4.04285 2 12 10 10-0.23264 4.11023 2 12 10 11 4.54585 4.01219 2 12 10 12 6.51928 3.82863 2 12 10 13 2.07009 4.02091 2 12 10 14 5.50921 4.22408 2 12 10 15-0.96243 4.46782 2 12 10 16 0.49869 4.63471 2 12 11 -1-0.52949 4.98021 2 12 11 0-2.87967 4.76679 2 12 11 1 0.09206 4.78338 2 12 11 6-1.17255 4.05242 2 13 -9 -9 4.79016 3.00208 2 13 -9 -8 4.57406 3.20202 2 13 -9 -7 1.30260 3.25324 2 13 -9 -6 8.33557 3.58862 2 13 -9 -5 4.02659 4.02004 2 13 -9 -4-0.70228 3.65597 2 13 -8 -15 0.22451 4.45595 2 13 -8 -9 0.09564 2.84631 2 13 -8 -8 3.76417 2.44721 2 13 -8 -7-0.92190 2.49734 2 13 -8 -6 0.29985 2.49625 2 13 -8 -5-4.54712 2.55445 2 13 -8 -4 5.29027 2.68698 2 13 -8 -3-2.31933 2.44280 2 13 -8 -2-2.43212 3.14772 2 13 -8 -1 3.97750 3.13542 2 13 -8 0 2.62071 2.94731 2 13 -8 1 4.96589 2.87762 2 13 -8 2-2.61933 2.64212 2 13 -7 -14-1.73901 4.43200 2 13 -7 -13-7.59032 4.29130 2 13 -7 -12-1.12637 4.10258 2 13 -7 -10-1.98311 2.78535 2 13 -7 -9 0.50871 2.68154 2 13 -7 -8 1.08196 2.42619 2 13 -7 -7-0.03861 2.39228 2 13 -7 -6-0.08868 2.44691 2 13 -7 -5 3.32693 2.45046 2 13 -7 -4-0.71501 2.45780 2 13 -7 -3 6.57385 2.56226 2 13 -7 -2 1.93202 2.36186 2 13 -7 -1-0.55590 2.06280 2 13 -7 0 3.91807 2.97725 2 13 -7 1-1.97268 2.88496 2 13 -7 2 0.93464 2.72845 2 13 -7 3 1.03838 2.51376 2 13 -6 3-0.07520 2.49889 2 13 -6 4 3.59061 2.48225 2 -13 -1 13 0.06491 4.02356 2 13 1 -4 4.07904 3.56600 2 13 1 -3 4.94808 3.30322 2 13 1 -2 4.48037 3.46741 2 13 1 -1 4.23756 3.49597 2 13 1 0 13.0092 3.71551 2 13 1 1 30.2732 3.69693 2 13 1 2 4.55209 3.92009 2 13 1 3 9.32573 3.84675 2 13 1 4 2.88359 3.84265 2 13 1 5-0.15012 3.92625 2 13 1 7 2.04492 4.29529 2 13 1 10-2.20788 5.00815 2 13 1 11 4.43624 5.38283 2 13 1 12 3.16750 2.84589 2 13 1 13 5.10978 5.65931 2 -13 -2 12 0.10029 3.95854 2 -13 -2 11 4.54788 3.94760 2 -13 -2 10 0.10638 2.30301 2 -13 -2 9 2.37511 2.27568 2 -13 -2 8-0.18212 2.70211 2 -13 -2 7 4.16387 2.65801 2 -13 -2 6 1.49457 2.68240 2 -13 -2 5-0.72989 2.68452 2 -13 -2 4 0.21998 2.51433 2 -13 -2 3-0.58796 2.38056 2 13 2 -2 2.20060 3.35693 2 13 2 -1 8.50629 3.50309 2 13 2 0-1.71439 3.48647 2 13 2 1-1.36465 3.62505 2 13 2 2 5.89122 3.59103 2 13 2 3 2.43006 3.62315 2 13 2 4 10.7864 3.95735 2 13 2 6 1.22985 3.75307 2 13 2 10 4.20814 4.63597 2 13 2 11-5.68727 4.78304 2 13 2 12-1.79446 4.99189 2 13 2 13 1.73355 2.82704 2 13 3 14 6.04328 4.99608 2 13 11 -1 1.75228 3.77307 2 13 11 0 2.76202 3.56274 2 13 11 1 0.59109 3.43439 2 13 11 2 0.54379 2.72687 2 13 11 3 0.75956 3.30866 2 13 11 4 3.89725 3.33198 2 13 11 5-3.71960 4.46585 2 13 11 6 0.71161 4.35254 2 13 11 7 5.97353 4.62811 2 13 11 8 5.41521 4.53205 2 13 11 9 10.6054 4.70495 2 14 -8 -8 2.39396 3.37605 2 14 -8 -7 0.13248 3.51435 2 14 -8 -6 0.45104 3.53852 2 14 -8 -5 2.33505 3.78130 2 14 -8 -4-6.53114 4.06165 2 14 -8 -3 8.23332 4.58753 2 14 -8 -2 4.58453 4.08701 2 14 -8 -1-0.02224 2.33970 2 14 -8 0 2.54023 3.22023 2 14 -8 1-2.52165 2.98605 2 14 -7 -13 2.07143 4.48110 2 14 -7 -9 5.07461 2.95289 2 14 -7 -8 4.11685 3.24381 2 14 -7 -7 1.43391 2.61207 2 14 -7 -6 0.47619 2.64274 2 14 -7 -5 2.89406 2.52138 2 14 -7 -4 0.86911 2.55125 2 14 -7 -3-0.18750 2.51749 2 14 -7 -2-2.81354 2.58947 2 14 -7 -1 3.62309 2.49350 2 14 -7 0-0.13173 2.32041 2 14 -7 1 1.81845 3.09922 2 14 -7 2 0.48756 3.02748 2 14 -6 -9 1.75292 3.16432 2 14 -6 -8-1.74974 3.19097 2 14 -6 -7-1.06929 2.52972 2 14 -6 -6 0.28354 2.54236 2 14 -6 -5-0.76460 2.59999 2 14 -6 -4 5.53690 2.51768 2 14 -6 -3 1.22912 2.51840 2 14 -6 -2-1.64059 2.48502 2 14 -6 -1 4.16287 2.51799 2 14 -6 0 0.66741 2.47755 2 14 -6 1 0.12197 2.35063 2 14 -6 2 1.23309 2.91739 2 14 -6 3 3.20666 2.79671 2 14 -5 5 1.96246 2.58700 2 14 2 -10-3.37560 4.13620 2 14 2 -9-7.42098 4.10538 2 14 2 -8 0.21179 4.05333 2 14 2 -7 1.49476 3.89900 2 14 2 -6 0.80302 3.91333 2 -14 -2 5 4.81930 2.71848 2 -14 -2 4-2.23978 2.40789 2 14 2 -3 1.10554 3.77405 2 14 2 -2-2.89010 3.65647 2 14 2 -1 13.6848 3.72817 2 14 2 0 0.56586 3.77931 2 14 2 1-3.18902 3.91048 2 14 2 2 4.51181 3.94395 2 14 2 3-1.73680 3.80297 2 14 2 4 8.35820 4.03266 2 14 2 5 2.37516 4.12122 2 14 2 6-1.04649 4.14501 2 14 2 7-3.86890 4.13045 2 14 2 10 4.79624 4.77926 2 14 2 11-3.07435 4.94256 2 14 2 12 2.75117 5.21743 2 14 3 -9 4.18461 4.44946 2 14 3 -8-5.08687 4.04157 2 14 3 -5-0.64041 3.96371 2 14 3 0-4.39936 3.61961 2 15 -8 -7 2.88017 3.60201 2 15 -8 -6-3.35170 3.90047 2 15 -8 -5-0.13021 3.95371 2 15 -8 -4 4.78709 4.26746 2 15 -8 -3 0.27779 4.47549 2 15 -8 -2 1.06755 4.88657 2 15 -8 -1 6.20074 4.56475 2 15 -8 0 2.28335 4.15740 2 15 -7 -8-0.43712 3.43797 2 15 -7 -7-0.31654 3.73789 2 15 -7 -6 5.12409 3.78428 2 15 -7 -5-0.49005 2.75312 2 15 -7 -4-0.15726 2.67273 2 15 -7 -3 3.79134 2.72389 2 15 -7 -2-0.17976 2.73470 2 15 -7 -1 2.08985 2.80669 2 15 -7 0 2.00873 2.71874 2 15 -7 1-2.79354 2.67652 2 15 -7 2-3.99070 3.66417 2 15 -6 -8 5.44517 3.31778 2 15 -6 -7-1.33558 3.57224 2 15 -6 -6 8.06747 3.77850 2 15 -6 -5 1.95081 2.71450 2 15 -6 -4 7.48876 2.72826 2 15 -6 -3 3.92762 2.68147 2 15 -6 -2-0.15204 2.68921 2 15 -6 -1 1.15909 2.68388 2 15 -6 0 0.90547 2.75478 2 15 -6 1-1.15207 2.68155 2 15 -6 2 7.44617 2.67670 2 15 -6 3 2.68977 4.19837 2 15 2 -1-1.93411 3.81278 2 15 2 0 0.48890 3.98596 2 15 2 1 5.84911 4.09134 2 15 2 2 5.99409 4.20341 2 15 2 3 0.76116 4.15551 2 15 2 4 1.14044 4.14212 2 15 2 5 2.50585 4.58799 2 15 2 6-4.92223 4.44011 2 15 2 7 0.04415 4.51980 2 15 2 10-5.57531 4.88761 2 15 3 -10 0.34909 4.53459 2 15 3 -9 1.77952 4.56771 2 15 3 -8-1.80287 4.21277 2 15 3 -7 1.12110 4.36194 2 15 3 -6 0.61287 4.23082 2 -15 -3 5-0.55201 2.87041 2 -15 -3 4-2.82802 2.70274 2 -15 -3 3-1.36972 2.37918 2 15 3 -2-0.23125 4.12270 2 15 3 -1 6.07251 4.18054 2 15 3 0 3.24994 3.84295 2 15 3 1-0.84168 3.87196 2 15 3 2 5.21641 4.02247 2 15 3 3 2.53210 4.17552 2 15 3 4-0.32855 4.16179 2 15 3 5-7.76817 4.06541 2 16 -7 -7-2.10083 3.98286 2 16 -7 -6-6.37074 3.99109 2 16 -7 -5-0.35641 4.34703 2 16 -7 -4 2.61396 4.29546 2 16 -7 -3-1.33686 2.86520 2 16 -7 -2-0.08336 4.62341 2 16 -7 -1 1.36199 4.96341 2 16 -7 0 6.23769 5.33742 2 16 -7 1-13.4779 5.20785 2 16 -7 2 0.63967 5.20575 2 16 -6 -10 5.75761 4.27914 2 16 -6 -9-1.01826 4.08705 2 16 -6 -8-4.15147 3.83749 2 16 -6 -7 1.69072 2.71095 2 16 -6 -6 2.02327 2.77266 2 16 -6 -5 0.13296 2.63517 2 16 -6 -4 3.65596 2.72000 2 16 -6 -3 3.40972 2.89460 2 16 -6 -2 4.42919 2.89902 2 16 -6 -1 3.42173 2.84607 2 16 -6 0-0.30233 2.86177 2 16 -6 1-1.26344 2.92019 2 16 -6 2 6.31683 5.63209 2 16 -6 3 4.75196 5.37281 2 16 -5 -8 1.92124 3.86974 2 16 -5 -7-1.28963 3.68989 2 16 -5 -6 0.50917 3.93306 2 16 -5 -4-2.90340 4.07069 2 16 -5 -3 3.98155 2.92605 2 16 -5 -2 3.30080 2.85109 2 16 -5 -1-0.35897 3.64544 2 16 -5 0 3.63838 3.54811 2 16 -5 2 1.39177 3.40357 2 16 -5 4-2.85500 5.65681 2 16 3 -9-1.87758 4.73125 2 16 3 -8 4.03717 4.45381 2 16 3 -7 1.86981 4.61164 2 16 3 -6 1.08906 4.49590 2 16 3 -5-0.31823 4.36402 2 16 3 -4-0.20431 4.49601 2 16 3 -3 1.38300 4.45450 2 16 3 -2 3.86599 4.53403 2 16 3 -1 3.12516 4.48106 2 16 3 0-3.30569 3.94781 2 16 3 1 9.08852 4.29446 2 16 3 2 3.75960 4.38694 2 16 3 3-3.13359 4.49304 2 16 3 4 6.18862 4.64311 2 16 3 5 2.37934 4.54163 2 16 3 6-0.52092 4.49688 2 16 3 7-1.74296 4.67117 2 16 4 -7-0.76263 4.77794 2 17 -7 -5 4.98463 4.32107 2 17 -7 -4-1.43823 4.71414 2 17 -7 -3 0.72040 4.65089 2 17 -7 -2 2.85655 4.83309 2 17 -7 -1-7.11309 5.10128 2 17 -7 0-1.47839 5.37360 2 17 -6 -6 2.81675 4.29029 2 17 -6 -5 0.69358 4.40876 2 17 -6 -4 3.08988 4.47054 2 17 -6 -3 8.04031 4.77686 2 17 -6 -2-6.00184 4.66078 2 17 -6 -1 4.11567 3.00821 2 17 -6 0-5.09178 5.14697 2 17 -5 -7-0.42194 3.79309 2 17 -5 -6 7.80950 4.19841 2 17 -5 -5-3.65062 4.39014 2 17 -5 -4 7.09781 4.49096 2 17 -5 -3 0.80106 4.61837 2 17 -5 -2 5.00787 4.78879 2 17 -5 -1 2.89021 2.97748 2 17 -5 0-2.26985 2.96569 2 17 -5 1-2.74627 5.14620 2 17 3 -2 6.11176 4.83825 2 17 3 0 5.52514 4.46896 2 17 3 1-1.69574 4.54624 2 17 3 2-1.27524 4.64420 2 17 3 3-6.05396 4.71090 2 17 3 4-0.65435 4.88602 2 17 4 -2 0.43479 4.69433 2 17 4 -1 2.60315 4.83743 2 17 4 0 0.65829 4.75104 2 17 4 1-0.96708 4.73823 2 17 4 2-2.09528 4.53892 2 18 -6 -5 2.97598 4.69181 2 18 -6 -4 5.61959 4.67448 2 18 -6 -3 3.24930 4.89524 2 18 -6 -2-0.62821 5.05928 2 18 -5 -5-2.52611 4.48050 2 18 -5 -4 1.54750 3.00362 2 18 -5 -3 2.37016 2.89812 2 18 -5 -2-1.16443 2.91017 2 18 -5 -1-3.31785 3.05076 2 18 -4 -4-0.68329 4.66225 2 0 0 0 0.00000 0.00000 0 TITL twin_twin1_hklf4 in P-1 REM P-1 (#2 in standard setting) CELL 0.71073 14.329904 14.377221 15.985301 66.2279 88.4679 89.7814 ZERR 2.00 0.001394 0.001052 0.001151 0.0069 0.0069 0.0069 LATT 1 SFAC C H N O K Br Au UNIT 72.00 72.00 48.00 24.00 2.00 8.00 2.00 TREF HKLF 5 BASF 0.34201 END ; _shelx_hkl_checksum 62071 _shelx_fab_file ; 5 8 20 1.33 0.00 5 7 20 -0.08 0.00 4 7 20 -1.00 0.00 5 6 20 0.96 0.00 4 6 20 -1.05 0.00 4 5 20 -1.44 0.00 4 4 20 1.04 0.00 5 12 19 -0.48 0.00 6 11 19 -0.94 0.00 5 11 19 1.21 0.00 6 10 19 0.51 0.00 5 10 19 0.08 0.00 1 10 19 -0.53 0.00 0 10 19 1.40 0.00 7 9 19 0.01 0.00 6 9 19 -0.21 0.00 5 9 19 -0.02 0.00 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-6 6 18 0.65 0.00 -5 6 18 -1.78 0.00 -4 6 18 -1.15 0.00 8 6 18 -1.78 0.00 9 6 18 1.39 0.00 -9 7 18 1.46 0.00 -8 7 18 -0.55 0.00 -7 7 18 -1.02 0.00 -6 7 18 -1.34 0.00 9 7 18 1.01 0.00 -8 8 18 -2.08 0.00 -8 9 18 0.26 0.00 -8 10 18 0.74 0.00 -7 10 18 -0.31 0.00 9 10 18 1.23 0.00 -7 11 18 -1.51 0.00 -7 12 18 -2.25 0.00 -6 12 18 -1.27 0.00 2 12 18 -0.58 0.00 3 12 18 0.33 0.00 -6 13 18 3.35 0.00 -5 13 18 -0.39 0.00 -4 13 18 1.39 0.00 1 13 18 -0.63 0.00 2 13 18 0.30 0.00 3 13 18 -3.39 0.00 4 13 18 -0.15 0.00 -4 14 18 0.55 0.00 -3 14 18 0.83 0.00 2 14 18 1.56 0.00 3 14 18 0.57 0.00 4 14 18 0.06 0.00 5 14 18 1.56 0.00 -2 15 18 1.64 0.00 -1 15 18 0.38 0.00 2 15 18 -0.90 0.00 -1 0 19 1.54 0.00 0 0 19 -2.67 0.00 1 0 19 2.04 0.00 2 0 19 -1.05 0.00 -4 1 19 2.15 0.00 -3 1 19 -1.93 0.00 -2 1 19 1.28 0.00 5 1 19 -0.70 0.00 -5 2 19 -2.76 0.00 -4 2 19 -1.41 0.00 -3 2 19 -0.43 0.00 -1 2 19 0.79 0.00 6 2 19 0.36 0.00 -6 3 19 2.64 0.00 -5 3 19 -0.47 0.00 -4 3 19 1.91 0.00 -3 3 19 -3.06 0.00 7 3 19 -1.79 0.00 -6 4 19 0.70 0.00 -5 4 19 1.32 0.00 -4 4 19 2.20 0.00 -3 4 19 0.95 0.00 7 4 19 -0.26 0.00 -7 5 19 -0.77 0.00 -6 5 19 0.12 0.00 -5 5 19 -3.08 0.00 -4 5 19 0.66 0.00 -3 5 19 -3.38 0.00 8 5 19 -0.50 0.00 -7 6 19 -0.14 0.00 -6 6 19 -0.35 0.00 -5 6 19 -0.29 0.00 -4 6 19 1.32 0.00 -3 6 19 1.15 0.00 -2 6 19 0.14 0.00 -1 6 19 0.56 0.00 8 6 19 1.30 0.00 -7 7 19 -0.54 0.00 -6 7 19 1.08 0.00 -5 7 19 0.18 0.00 -4 7 19 1.66 0.00 -3 7 19 -1.49 0.00 -2 7 19 -0.01 0.00 -1 7 19 -0.12 0.00 8 7 19 -0.36 0.00 -7 8 19 -0.57 0.00 -6 8 19 0.66 0.00 -5 8 19 -0.61 0.00 -4 8 19 -1.76 0.00 8 8 19 2.28 0.00 -7 9 19 0.10 0.00 -6 9 19 -0.85 0.00 4 9 19 -2.06 0.00 -6 10 19 -0.45 0.00 -5 10 19 0.55 0.00 3 10 19 0.20 0.00 4 10 19 -1.20 0.00 7 10 19 -1.88 0.00 -6 11 19 -0.89 0.00 -5 11 19 1.55 0.00 -4 11 19 -1.94 0.00 -3 11 19 0.60 0.00 4 11 19 -1.30 0.00 -5 12 19 -0.67 0.00 -4 12 19 -0.53 0.00 -1 12 19 -0.26 0.00 0 12 19 0.57 0.00 1 12 19 -2.87 0.00 3 12 19 -0.69 0.00 4 12 19 -0.87 0.00 1 13 19 1.66 0.00 2 13 19 -0.25 0.00 3 13 19 1.92 0.00 4 13 19 -0.80 0.00 0 14 19 0.32 0.00 1 14 19 -0.96 0.00 -2 3 20 -1.82 0.00 -1 3 20 -0.35 0.00 0 3 20 -1.09 0.00 1 3 20 0.05 0.00 2 3 20 -1.56 0.00 3 3 20 -0.01 0.00 -3 4 20 -0.41 0.00 -2 4 20 1.21 0.00 -1 4 20 -0.39 0.00 0 4 20 3.82 0.00 1 4 20 1.36 0.00 2 4 20 1.52 0.00 3 4 20 -0.95 0.00 -4 5 20 -0.46 0.00 -3 5 20 3.03 0.00 -2 5 20 -1.00 0.00 -1 5 20 -2.02 0.00 0 5 20 -5.19 0.00 5 5 20 0.83 0.00 -4 6 20 -1.41 0.00 -3 6 20 -1.34 0.00 -2 6 20 -0.04 0.00 -1 6 20 -0.71 0.00 0 6 20 2.28 0.00 1 6 20 1.69 0.00 -5 7 20 1.17 0.00 -4 7 20 -1.12 0.00 -3 7 20 2.20 0.00 -2 7 20 0.04 0.00 -1 7 20 3.66 0.00 0 7 20 1.00 0.00 1 7 20 2.64 0.00 2 7 20 -1.11 0.00 -4 8 20 -1.87 0.00 -3 8 20 -1.15 0.00 -2 8 20 -0.65 0.00 -1 8 20 -1.38 0.00 0 8 20 -2.65 0.00 1 8 20 -3.11 0.00 2 8 20 -0.30 0.00 3 8 20 0.02 0.00 -4 9 20 1.02 0.00 -3 9 20 3.01 0.00 -2 9 20 0.50 0.00 -1 9 20 1.83 0.00 0 9 20 0.53 0.00 1 9 20 2.59 0.00 2 9 20 0.14 0.00 3 9 20 -1.06 0.00 4 9 20 -1.98 0.00 5 9 20 -2.43 0.00 -4 10 20 -0.22 0.00 -3 10 20 -1.47 0.00 -2 10 20 -1.55 0.00 -1 10 20 -2.10 0.00 0 10 20 -1.16 0.00 1 10 20 -0.11 0.00 2 10 20 0.71 0.00 3 10 20 0.62 0.00 4 10 20 2.09 0.00 5 10 20 0.59 0.00 -3 11 20 -0.22 0.00 -2 11 20 2.17 0.00 -1 11 20 1.92 0.00 0 11 20 0.56 0.00 1 11 20 0.28 0.00 2 11 20 -1.62 0.00 3 11 20 -2.07 0.00 4 11 20 0.11 0.00 -1 12 20 -1.81 0.00 0 12 20 -2.01 0.00 1 12 20 -0.33 0.00 2 12 20 -0.29 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 230917) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.000 285 68 ' ' 2 -0.001 0.500 0.500 137 19 ' ' 3 0.500 1.000 0.500 137 26 ' ' 4 0.500 0.464 0.584 12 4 ' ' 5 0.500 0.539 0.410 12 4 ' ' # Missing Reflections Below sin(th)/lambda = 0.25 loop_ _platon_missing_refln_index_h _platon_missing_refln_index_k _platon_missing_refln_index_l _platon_missing_refln_theta 1 0 0 1.422 -3 1 0 4.530 -2 1 0 3.228 0 1 0 1.548 -4 2 0 6.467 -3 2 0 5.257 -6 -3 1 10.187 -4 -2 1 6.947 -1 -1 1 2.871 -3 0 1 4.527 -2 0 1 3.201 -1 0 1 2.017 0 0 1 1.392 1 0 1 1.963 -2 1 1 3.293 -1 1 1 2.167 0 1 1 1.611 -5 2 1 7.689 -4 2 1 6.380 -3 2 1 5.140 -6 3 1 9.588 -5 3 1 8.326 -5 -3 2 9.628 -4 -3 2 8.596 -6 -2 2 9.987 -5 -2 2 8.764 -4 -2 2 7.622 -3 -2 2 6.596 -2 -2 2 5.748 -4 -1 2 6.869 -3 -1 2 5.716 -2 -1 2 4.718 -5 0 2 7.728 -4 0 2 6.413 -3 0 2 5.164 -2 0 2 4.037 -1 1 2 2.981 -1 2 2 3.546 -6 3 2 9.654 -5 3 2 8.396 -5 -2 3 9.527 -4 -2 3 8.478 -3 -2 3 7.560 -6 -1 3 10.049 -5 -1 3 8.831 -4 -1 3 7.693 -3 -1 3 6.672 -2 -1 3 5.829 -5 0 3 8.372 -4 0 3 7.166 -3 0 3 6.062 -2 0 3 5.124 -1 1 3 4.120 -1 2 3 4.350 -4 -2 4 9.468 -5 -1 4 9.701 -4 -1 4 8.668 -3 -1 4 7.767 -5 0 4 9.189 -4 0 4 8.095 -3 0 4 7.125 -4 -1 5 9.752 -5 0 5 10.137 -4 0 5 9.148 -3 5 6 9.908 _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL twin_twin1P -1f5 R = 0.17 CELL 14.3299 14.3772 15.9853 66.23 88.47 89.78 SPGR P-1 # Solvent Accessible Volume = 580 # Electrons Found in S.A.V. = 120 # Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others Q101 0.392 0.713 0.093 ! 3.15 eA-3 Q102 0.981 0.045 0.078 ! 2.94 eA-3 C103 0.062 0.231 0.187 ! 2.89 eA-3 C104 0.849 0.345 0.093 ! 2.68 eA-3 C105 0.202 0.328 0.078 ! 2.60 eA-3 Q106 0.911 0.735 0.470 ! 2.51 eA-3 C107 1.000 0.500 0.000 ! 2.49 eA-3 C108 0.086 0.319 0.488 ! 2.46 eA-3 C109 0.021 0.324 0.095 ! 2.45 eA-3 C110 0.885 0.280 0.115 ! 2.39 eA-3 Q111 0.186 1.006-0.002 ! 2.38 eA-3 C112 0.505 0.547 0.390 ! 2.27 eA-3 C113 0.575 0.111 0.452 ! 2.20 eA-3 Q114 0.691 0.090 0.485 ! 2.15 eA-3 Q115 0.519 0.635 0.174 ! 2.12 eA-3 C116 0.904 0.491 0.013 ! 2.11 eA-3 C117 0.126 0.487 0.002 ! 2.03 eA-3 C118 0.095 0.443 0.458 ! 2.01 eA-3 C119 0.316 0.921 0.474 ! 1.93 eA-3 Q120 0.278 0.950 0.445 ! 1.92 eA-3 Q121 0.638 0.671 0.079 ! 1.83 eA-3 Q122 0.125 1.003-0.006 ! 1.79 eA-3 Q123 0.483 0.960 0.425 ! 1.75 eA-3 Q124 0.154 0.230 0.088 ! 1.68 eA-3 Q125 0.263 0.360 0.079 ! 1.64 eA-3 Q126 0.810 0.044 0.058 ! 1.63 eA-3 C127 0.840 0.449 0.057 ! 1.62 eA-3 Q128 0.654 0.704 0.058 ! 1.62 eA-3 Q129 0.070 0.288 0.169 ! 1.61 eA-3 Q130 0.534 0.823 0.082 ! 1.60 eA-3 Q131 0.521 0.863 0.081 ! 1.55 eA-3 C132 0.927 0.515 0.457 ! 1.55 eA-3 C133 0.825 0.518 0.026 ! 1.52 eA-3 Q134 0.969 0.470 0.073 ! 1.51 eA-3 C135 0.815 0.413 0.036 ! 1.51 eA-3 Q136 0.687 0.845 0.073 ! 1.50 eA-3 Q137 0.818 0.260 0.160 ! 1.49 eA-3 C138 0.512 0.097 0.438 ! 1.49 eA-3 Q139 0.527 0.564 0.099 ! 1.48 eA-3 Q140 0.564 0.550 0.435 ! 1.45 eA-3 C141 0.433 0.914 0.468 ! 1.42 eA-3 Q142 0.750 0.190 0.008 ! 1.41 eA-3 C143 0.044 0.460 0.008 ! 1.39 eA-3 Q144 0.609 0.585 0.099 ! 1.38 eA-3 Q145 0.585 0.719 0.093 ! 1.38 eA-3 Q146 0.534 0.074 0.294 ! 1.37 eA-3 Q147 0.560 0.467 0.456 ! 1.34 eA-3 Q148 0.470 0.552 0.083 ! 1.31 eA-3 Q149 0.172 0.513 0.018 ! 1.31 eA-3 Q150 0.186 0.216 0.185 ! 1.31 eA-3 Q151 0.531 0.479 0.410 ! 1.30 eA-3 Q152 0.318 0.557 0.074 ! 1.30 eA-3 Q153 0.090 0.265 0.460 ! 1.29 eA-3 Q154 0.748 0.387 0.140 ! 1.29 eA-3 Q155 0.169 0.076 0.137 ! 1.28 eA-3 Q156 0.567 0.037 0.327 ! 1.27 eA-3 C157 0.144 0.341 0.096 ! 1.26 eA-3 C158 0.919 0.573 0.467 ! 1.25 eA-3 Q159 0.351 1.002 0.441 ! 1.24 eA-3 Q160 0.061 0.047 0.318 ! 1.22 eA-3 Q161 0.095 0.259 0.234 ! 1.21 eA-3 Q162 0.519 0.714 0.030 ! 1.21 eA-3 C163 0.185 0.455 0.019 ! 1.20 eA-3 Q164 0.607 0.827 0.099 ! 1.19 eA-3 Q165 0.103 0.479 0.391 ! 1.19 eA-3 Q166 0.079 0.529 0.422 ! 1.18 eA-3 Q167 0.530 0.733 0.110 ! 1.18 eA-3 Q168 0.463 0.729 0.096 ! 1.17 eA-3 Q169 0.144 0.173 0.096 ! 1.17 eA-3 Q170 0.518 0.552 0.328 ! 1.17 eA-3 Q171 0.155 0.039 0.116 ! 1.17 eA-3 Q172 0.194 0.582 0.422 ! 1.17 eA-3 Q173 0.255 0.297 0.014 ! 1.16 eA-3 Q174 0.670 0.294 0.414 ! 1.16 eA-3 Q175 0.361 0.931 0.105 ! 1.15 eA-3 Q176 0.354 0.034 0.450 ! 1.15 eA-3 Q177 0.730 0.334 0.158 ! 1.14 eA-3 Q178 0.764 0.401 0.323 ! 1.13 eA-3 Q179 0.247 0.959 0.024 ! 1.13 eA-3 C180 0.127 0.285 0.109 ! 1.12 eA-3 Q181 0.414 0.936 0.429 ! 1.12 eA-3 Q182 0.149 0.300 0.506 ! 1.12 eA-3 Q183 0.814 0.385 0.134 ! 1.11 eA-3 Q184 0.236 0.249 0.022 ! 1.11 eA-3 Q185 0.922 0.787 0.172 ! 1.11 eA-3 Q186 0.960 0.707 0.455 ! 1.09 eA-3 Q187 0.227 0.731 0.020 ! 1.08 eA-3 Q188 0.907 0.611 0.423 ! 1.08 eA-3 Q189 0.754 0.273 0.189 ! 1.07 eA-3 Q190 0.153 0.103 0.078 ! 1.07 eA-3 Q191 0.403 0.174 0.450 ! 1.07 eA-3 Q192 0.471 0.888 0.074 ! 1.07 eA-3 Q193 0.050 0.083 0.281 ! 1.07 eA-3 C194 0.095 0.366 0.102 ! 1.07 eA-3 Q195 0.114 0.286 0.006 ! 1.06 eA-3 Q196 0.434 0.499 0.482 ! 1.06 eA-3 Q197 0.675 0.590 0.109 ! 1.06 eA-3 Q198 0.422 1.005 0.349 ! 1.06 eA-3 Q199 0.376 0.589 0.408 ! 1.05 eA-3 ) ; _shelx_fab_checksum 22126 _platon_squeeze_details ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.000 285 68 ' ' 2 -0.001 0.500 0.500 137 19 ' ' 3 0.500 1.000 0.500 137 26 ' ' 4 0.500 0.464 0.584 12 4 ' ' 5 0.500 0.539 0.410 12 4 ' ' _platon_squeeze_void_probe_radius 1.20 _olex2_date_sample_data_collection 2020-01-02 _olex2_date_sample_submission 2019-12-22 _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 cx1754 _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 1.367 _oxdiff_exptl_absorpt_empirical_full_min 0.674 _oxdiff_twin_integration_method simultaneous _oxdiff_twin_items 2 loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.685(3) 2 0.315(3) _twin_special_details ; Component 2 rotated by -179.9229\% around [0.00 0.00 1.00] (reciprocal) or [-0.02 -0.41 0.91] (direct) ;