#------------------------------------------------------------------------------ #$Date: 2024-07-25 01:14:29 +0300 (Thu, 25 Jul 2024) $ #$Revision: 293532 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572164.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1572164 loop_ _publ_author_name 'Madron du Vign\'e, Adrien' 'Cramer, Nicolai' _publ_section_title ; Streamlined Synthetic Assembly of \a-Chiral CAAC Ligands and Catalytic Performance of Their Copper and Ruthenium Complexes ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC04278F _journal_year 2024 _chemical_absolute_configuration rmad _chemical_formula_moiety 'C23 H35 Cl Cu N S' _chemical_formula_sum 'C23 H35 Cl Cu N S' _chemical_formula_weight 456.57 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_date 2023-11-27 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _audit_update_record ; 2024-06-27 deposited with the CCDC. 2024-07-24 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 103.104(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.5182(2) _cell_length_b 15.3074(5) _cell_length_c 9.1646(3) _cell_measurement_reflns_used 6828 _cell_measurement_temperature 140.0(3) _cell_measurement_theta_max 72.7060 _cell_measurement_theta_min 4.9370 _cell_volume 1163.87(6) _computing_cell_refinement 'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)' _computing_data_reduction 'CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2019/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 140.0(3) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2817 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.979 _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 -87.00 -54.00 1.00 6.50 -- -40.29 -26.00 -11.00 33 2 \w 10.00 117.00 1.00 6.50 -- 40.29 26.00 152.00 107 3 \w 14.00 40.00 1.00 6.50 -- 40.29 -26.00 -11.00 26 4 \w 62.00 108.00 1.00 26.00 -- 105.78 -26.00 -11.00 46 5 \w 102.00 127.00 1.00 26.00 -- 105.78 26.00 152.00 25 6 \w 33.00 60.00 1.00 26.00 -- 105.78 -26.00 -11.00 27 7 \w -110.00 -13.00 1.00 6.50 -- -40.29 -57.00 150.00 97 8 \w -51.00 -17.00 1.00 6.50 -- -40.29 -38.00-120.00 34 9 \w -42.00 -17.00 1.00 6.50 -- -40.29 26.00 152.00 25 10 \w -112.00 -12.00 1.00 6.50 -- -40.29 -57.00-120.00 100 11 \w 14.00 41.00 1.00 6.50 -- 40.29 57.00 -30.00 27 12 \w 29.00 89.00 1.00 6.50 -- 40.29-125.00-150.00 60 13 \w 21.00 46.00 1.00 6.50 -- 40.29 57.00 -90.00 25 14 \w 6.00 78.00 1.00 6.50 -- 40.29 -99.00 0.00 72 15 \w 78.00 105.00 1.00 26.00 -- 105.78 61.00-120.00 27 16 \w 61.00 91.00 1.00 26.00 -- 105.78 178.00 0.00 30 17 \w 77.00 103.00 1.00 26.00 -- 105.78 61.00 -60.00 26 18 \w 109.00 141.00 1.00 26.00 -- 105.78 178.00 0.00 32 19 \w 121.00 158.00 1.00 26.00 -- 105.78 61.00 -30.00 37 20 \w 85.00 147.00 1.00 26.00 -- 105.78 45.00-180.00 62 21 \w 72.00 105.00 1.00 26.00 -- 105.78 -94.00 -60.00 33 22 \w 78.00 109.00 1.00 26.00 -- 105.78 61.00-180.00 31 23 \w 82.00 107.00 1.00 26.00 -- 105.78 45.00 -60.00 25 24 \w 113.00 174.00 1.00 26.00 -- 105.78 61.00 -90.00 61 25 \w 77.00 112.00 1.00 26.00 -- 105.78 30.00-120.00 35 26 \w 81.00 108.00 1.00 26.00 -- 105.78 45.00 -30.00 27 27 \w 105.00 167.00 1.00 26.00 -- 105.78 111.00-180.00 62 28 \w 82.00 109.00 1.00 26.00 -- 105.78 45.00-120.00 27 29 \w 80.00 122.00 1.00 26.00 -- 105.78 45.00 -90.00 42 30 \w 83.00 110.00 1.00 26.00 -- 105.78 45.00-150.00 27 31 \w 81.00 108.00 1.00 26.00 -- 105.78 38.00 -69.63 27 32 \w 78.00 106.00 1.00 26.00 -- 105.78 61.00 -30.00 28 33 \w 77.00 104.00 1.00 26.00 -- 105.78 61.00 -90.00 27 34 \w 78.00 103.00 1.00 26.00 -- 105.78 61.00-150.00 25 35 \w 83.00 110.00 1.00 26.00 -- 105.78 30.00 -30.00 27 36 \w 86.00 126.00 1.00 26.00 -- 105.78 30.00 -90.00 40 37 \w 112.00 170.00 1.00 26.00 -- 105.78 111.00 90.00 58 38 \w 26.00 106.00 1.00 26.00 -- 105.78 -94.00 30.00 80 39 \w 31.00 71.00 1.00 26.00 -- 105.78 -94.00 -60.00 40 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0366484000 _diffrn_orient_matrix_UB_12 -0.0111847000 _diffrn_orient_matrix_UB_13 0.1714515000 _diffrn_orient_matrix_UB_21 0.1709877000 _diffrn_orient_matrix_UB_22 -0.0320690000 _diffrn_orient_matrix_UB_23 -0.0014574000 _diffrn_orient_matrix_UB_31 0.0621914000 _diffrn_orient_matrix_UB_32 0.0947931000 _diffrn_orient_matrix_UB_33 0.0196493000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_unetI/netI 0.0510 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.979 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 10462 _diffrn_reflns_point_group_measured_fraction_full 0.957 _diffrn_reflns_point_group_measured_fraction_max 0.921 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.322 _diffrn_reflns_theta_min 4.955 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 3.255 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.309 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.101a (Rigaku Oxford Diffraction, 2023) 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_crystal_colour 'clear pale colourless' _exptl_crystal_density_diffrn 1.303 _exptl_crystal_description plate _exptl_crystal_F_000 484 _exptl_crystal_size_max 0.398 _exptl_crystal_size_mid 0.122 _exptl_crystal_size_min 0.087 _refine_diff_density_max 1.344 _refine_diff_density_min -0.555 _refine_diff_density_rms 0.073 _refine_ls_abs_structure_details ; Flack x determined using 1729 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.01(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 248 _refine_ls_number_reflns 4323 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.040 _refine_ls_R_factor_all 0.0493 _refine_ls_R_factor_gt 0.0472 _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^)+(0.0892P)^2^+0.0102P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1217 _refine_ls_wR_factor_ref 0.1234 _reflns_Friedel_coverage 0.810 _reflns_Friedel_fraction_full 0.910 _reflns_Friedel_fraction_max 0.859 _reflns_number_gt 4127 _reflns_number_total 4323 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc04278f2.cif _cod_data_source_block amd-r1398-dia2 _cod_database_code 1572164 _shelx_shelxl_version_number 2019/3 _chemical_oxdiff_formula 'C23 H35 N1 S1 Cl1 Cu1' _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. ; _shelx_estimated_absorpt_t_max 0.765 _shelx_estimated_absorpt_t_min 0.357 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C16(H16), C18(H18) 2.b Secondary CH2 refined with riding coordinates: C3(H3A,H3B), C6(H6A,H6B), C7(H7A,H7B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B) 2.c Aromatic/amide H refined with riding coordinates: C9(H9), C10(H10), C11(H11), C12(H12), C13(H13) 2.d Idealised Me refined as rotating group: C5(H5A,H5B,H5C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C) ; _shelx_res_file ; TITL AMD-R1398-dia2 in P2(1) amd-r1398-dia2.res created by SHELXL-2019/3 at 12:23:27 on 27-Nov-2023 CELL 1.54184 8.518225 15.30743 9.16459 90 103.1043 90 ZERR 2 0.000223 0.000477 0.000278 0 0.0028 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H Cl Cu N S UNIT 46 70 2 2 2 2 L.S. 10 PLAN 20 SIZE 0.398 0.122 0.087 TEMP -133 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.089200 0.010200 FVAR 6.90093 CU1 4 0.515112 0.337961 0.448662 11.00000 0.01620 0.01648 = 0.03523 0.00064 0.00482 0.00232 CL1 3 0.716527 0.256657 0.455324 11.00000 0.02196 0.02057 = 0.04444 0.00406 0.01105 0.00534 S1 6 0.435701 0.588599 0.063238 11.00000 0.08553 0.02821 = 0.05580 0.00885 0.04536 0.01634 N1 5 0.189856 0.386786 0.440652 11.00000 0.02133 0.01258 = 0.03145 0.00014 0.00918 0.00108 C1 1 0.338218 0.411320 0.451129 11.00000 0.02242 0.01855 = 0.02388 0.00035 0.00438 -0.00247 C2 1 0.353145 0.508626 0.480271 11.00000 0.01924 0.01563 = 0.03423 -0.00029 0.00505 0.00175 C3 1 0.179831 0.539970 0.476329 11.00000 0.02333 0.01711 = 0.04270 -0.00181 0.01315 -0.00028 AFIX 23 H3A 2 0.176938 0.573531 0.568024 11.00000 -1.20000 H3B 2 0.140117 0.577857 0.388135 11.00000 -1.20000 AFIX 0 C4 1 0.074790 0.457105 0.466797 11.00000 0.02276 0.01358 = 0.04215 0.00057 0.01417 0.00437 C5 1 0.463546 0.523000 0.635870 11.00000 0.03991 0.02520 = 0.03923 -0.00350 -0.00655 -0.00049 AFIX 137 H5A 2 0.423270 0.489018 0.710350 11.00000 -1.50000 H5B 2 0.464656 0.585166 0.661640 11.00000 -1.50000 H5C 2 0.573168 0.503989 0.634918 11.00000 -1.50000 AFIX 0 C6 1 0.433067 0.552688 0.364011 11.00000 0.02132 0.02054 = 0.04423 0.00328 0.01074 -0.00022 AFIX 23 H6A 2 0.447148 0.615630 0.388289 11.00000 -1.20000 H6B 2 0.541614 0.527149 0.372965 11.00000 -1.20000 AFIX 0 C7 1 0.338984 0.543380 0.202659 11.00000 0.04228 0.01756 = 0.04050 0.00352 0.01465 0.00120 AFIX 23 H7A 2 0.233015 0.572178 0.192699 11.00000 -1.20000 H7B 2 0.318701 0.480513 0.180893 11.00000 -1.20000 AFIX 0 C8 1 0.395532 0.702224 0.060814 11.00000 0.03293 0.02352 = 0.03624 0.00225 0.01139 0.00289 C9 1 0.333438 0.746983 0.168920 11.00000 0.03388 0.02711 = 0.02988 0.00180 0.00987 0.00142 AFIX 43 H9 2 0.307519 0.715865 0.250023 11.00000 -1.20000 AFIX 0 C10 1 0.310017 0.835944 0.157620 11.00000 0.03220 0.02596 = 0.03094 -0.00379 0.00377 0.00091 AFIX 43 H10 2 0.267315 0.865626 0.231041 11.00000 -1.20000 AFIX 0 C11 1 0.347843 0.883013 0.040530 11.00000 0.03125 0.02311 = 0.04263 -0.00182 0.00345 -0.00016 AFIX 43 H11 2 0.333045 0.944528 0.034451 11.00000 -1.20000 AFIX 0 C12 1 0.407863 0.838466 -0.067860 11.00000 0.03502 0.03005 = 0.04019 0.00746 0.01159 -0.00379 AFIX 43 H12 2 0.434006 0.869794 -0.148648 11.00000 -1.20000 AFIX 0 C13 1 0.429544 0.749049 -0.058479 11.00000 0.03382 0.03459 = 0.03606 0.00035 0.01208 0.00252 AFIX 43 H13 2 0.468084 0.719195 -0.134272 11.00000 -1.20000 AFIX 0 C14 1 0.026170 0.437597 0.614503 11.00000 0.04085 0.02239 = 0.05091 -0.00264 0.02605 0.00279 AFIX 137 H14A 2 -0.029571 0.381209 0.606992 11.00000 -1.50000 H14B 2 -0.045848 0.483694 0.634769 11.00000 -1.50000 H14C 2 0.122831 0.435410 0.696229 11.00000 -1.50000 AFIX 0 C15 1 -0.073894 0.462111 0.337629 11.00000 0.02223 0.02252 = 0.05521 0.00077 0.00529 0.00177 AFIX 137 H15A 2 -0.040201 0.471162 0.243359 11.00000 -1.50000 H15B 2 -0.142081 0.510939 0.354451 11.00000 -1.50000 H15C 2 -0.134827 0.407444 0.332173 11.00000 -1.50000 AFIX 0 C16 1 0.136310 0.293675 0.423765 11.00000 0.02342 0.01294 = 0.03961 -0.00188 0.01243 -0.00194 AFIX 13 H16 2 0.016904 0.293246 0.413478 11.00000 -1.20000 AFIX 0 C17 1 0.211142 0.243758 0.566480 11.00000 0.04554 0.01752 = 0.04592 0.00723 0.01947 0.00028 AFIX 137 H17A 2 0.325784 0.233771 0.570996 11.00000 -1.50000 H17B 2 0.156277 0.187478 0.566377 11.00000 -1.50000 H17C 2 0.199482 0.277928 0.653834 11.00000 -1.50000 AFIX 0 C18 1 0.169325 0.253685 0.279285 11.00000 0.01598 0.01522 = 0.03777 -0.00412 0.00487 -0.00088 AFIX 13 H18 2 0.287973 0.257054 0.285899 11.00000 -1.20000 AFIX 0 C19 1 0.084065 0.302823 0.138463 11.00000 0.02375 0.02535 = 0.03429 -0.00319 0.00083 0.00016 AFIX 23 H19A 2 -0.033450 0.303045 0.132460 11.00000 -1.20000 H19B 2 0.121539 0.364222 0.145237 11.00000 -1.20000 AFIX 0 C20 1 0.116430 0.261416 -0.003382 11.00000 0.03439 0.04332 = 0.03214 -0.00419 0.00169 0.00330 AFIX 23 H20A 2 0.054424 0.293159 -0.091997 11.00000 -1.20000 H20B 2 0.232364 0.267243 -0.002615 11.00000 -1.20000 AFIX 0 C21 1 0.070135 0.165672 -0.016442 11.00000 0.03549 0.04550 = 0.04874 -0.02013 -0.00307 0.00381 AFIX 23 H21A 2 0.101380 0.140071 -0.104941 11.00000 -1.20000 H21B 2 -0.048169 0.160006 -0.030888 11.00000 -1.20000 AFIX 0 C22 1 0.153102 0.116194 0.123426 11.00000 0.03806 0.02310 = 0.05401 -0.01493 0.00623 0.00038 AFIX 23 H22A 2 0.270765 0.115624 0.130257 11.00000 -1.20000 H22B 2 0.114944 0.054916 0.115518 11.00000 -1.20000 AFIX 0 C23 1 0.120327 0.156800 0.265269 11.00000 0.02940 0.01543 = 0.05415 -0.00430 0.01254 -0.00338 AFIX 23 H23A 2 0.181334 0.124502 0.353682 11.00000 -1.20000 H23B 2 0.004129 0.151545 0.263745 11.00000 -1.20000 AFIX 0 HKLF 4 REM AMD-R1398-dia2 in P2(1) REM wR2 = 0.1234, GooF = S = 1.041, Restrained GooF = 1.040 for all data REM R1 = 0.0472 for 4127 Fo > 4sig(Fo) and 0.0493 for all 4323 data REM 248 parameters refined using 1 restraints END WGHT 0.0892 0.0102 REM Highest difference peak 1.344, deepest hole -0.555, 1-sigma level 0.073 Q1 1 0.4991 0.3390 0.3452 11.00000 0.05 1.34 Q2 1 0.5333 0.3385 0.5564 11.00000 0.05 0.99 Q3 1 0.7011 0.2598 0.3527 11.00000 0.05 0.82 Q4 1 0.7334 0.2605 0.5623 11.00000 0.05 0.80 Q5 1 0.4179 0.5934 -0.0410 11.00000 0.05 0.51 Q6 1 0.4672 0.5875 0.1663 11.00000 0.05 0.34 Q7 1 0.3765 0.5404 0.2983 11.00000 0.05 0.29 Q8 1 0.1754 0.2970 0.5271 11.00000 0.05 0.27 Q9 1 0.6206 0.2010 0.3518 11.00000 0.05 0.27 Q10 1 0.6467 0.3798 0.3971 11.00000 0.05 0.27 Q11 1 0.5484 0.8602 0.0590 11.00000 0.05 0.27 Q12 1 0.3805 0.2958 0.4951 11.00000 0.05 0.27 Q13 1 0.1549 0.2781 0.3553 11.00000 0.05 0.26 Q14 1 0.2066 0.3836 0.5267 11.00000 0.05 0.26 Q15 1 0.5357 0.2572 0.4153 11.00000 0.05 0.26 Q16 1 0.1748 0.3945 0.3405 11.00000 0.05 0.26 Q17 1 0.3557 0.4672 0.4820 11.00000 0.05 0.25 Q18 1 0.6251 0.2958 0.3611 11.00000 0.05 0.25 Q19 1 0.0862 0.4502 0.5533 11.00000 0.05 0.24 Q20 1 0.3015 0.5416 0.0781 11.00000 0.05 0.24 ; _shelx_res_checksum 73349 _shelx_hkl_file ; 0 -15 5 20396.1 877.130 34 0 -15 6 7775.88 531.449 34 0 -15 6 6928.46 521.734 28 0 -14 6 599.148 267.737 34 0 -14 7 4319.19 415.171 34 0 -13 6 5772.21 530.802 30 0 -13 7 5760.69 524.800 34 0 -13 7 5651.51 483.840 30 0 -13 7 5917.91 516.527 25 0 -13 8 4311.56 379.562 34 0 -12 0 81103.2 4399.63 11 0 -12 1 8975.91 1487.15 7 0 -12 -1 10611.9 1726.93 11 0 -12 1 13055.6 2030.54 13 0 -12 2 46525.4 3496.43 7 0 -12 -2 56422.1 4296.90 10 0 -12 2 55807.8 4532.89 13 0 -12 -3 5032.54 1443.63 10 0 -12 5 1221.54 304.650 30 0 -12 6 3907.34 518.736 30 0 -12 6 3306.89 509.516 25 0 -12 7 6109.21 555.084 30 0 -12 7 5610.08 553.838 34 0 -12 7 6199.06 467.086 22 0 -12 7 6057.31 616.347 25 0 -12 8 11844.9 656.334 30 0 -12 8 10676.9 651.146 34 0 -12 8 11257.0 692.288 25 0 -11 0-336.496 437.619 11 0 -11 0 368.003 442.910 13 0 -11 -1 177.404 500.816 10 0 -11 -1 336.706 470.446 11 0 -11 1 612.774 813.119 13 0 -11 2 14620.6 1877.00 7 0 -11 2 16975.2 2397.21 13 0 -11 -2 17902.4 2347.05 10 0 -11 3 15313.6 2058.51 7 0 -11 -3 17750.5 2417.52 10 0 -11 3 14941.5 2276.25 13 0 -11 4 6566.94 1399.80 7 0 -11 -4 8864.09 1736.73 10 0 -11 6 14150.4 783.263 22 0 -11 6 15024.6 955.077 30 0 -11 7 10139.1 775.094 30 0 -11 7 10935.6 658.368 22 0 -11 8 7757.44 620.400 34 0 -11 8 6800.56 582.978 30 0 -11 8 7933.07 657.553 25 0 -10 0 98858.8 4175.44 10 0 -10 0 91867.5 3901.64 13 0 -10 -1 98859.6 4675.28 11 0 -10 -1 100015. 4684.33 10 0 -10 1 97341.9 4554.28 13 0 -10 1 112581. 4753.82 10 0 -10 2 4929.47 1153.04 7 0 -10 -2 5724.90 1268.64 10 0 -10 2 4616.30 1219.83 13 0 -10 -2 5286.53 1313.94 11 0 -10 3 26454.9 2574.14 7 0 -10 -4 14355.5 1954.37 8 0 -10 4 14337.2 1885.97 7 0 -10 5 1766.13 364.105 22 0 -10 -6 852.319 237.451 32 0 -10 6 1124.40 313.681 22 0 -10 7 5463.86 599.412 30 0 -10 7 4907.41 495.881 22 0 -10 8 1488.76 308.182 20 0 -10 8 801.509 289.192 34 0 -10 8 1604.16 385.171 30 0 -10 8 1317.96 278.374 22 0 -10 8 1206.05 353.871 25 0 -10 9 3840.32 397.085 34 0 -10 9 4302.59 425.295 30 0 -10 9 4795.78 482.816 25 0 -9 0 60.8120 336.392 10 0 -9 0-237.744 423.294 13 0 -9 -1 13527.4 1355.93 8 0 -9 1 11383.0 1500.01 13 0 -9 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12904.9 1274.64 21 1 13 7 10756.7 884.627 21 -1 14 7 10039.3 753.516 37 -1 14 7 12598.0 885.787 21 -1 14 6 3787.39 552.881 37 -1 14 6 4063.96 799.783 21 -1 14 5 20327.8 1308.90 37 1 14 -4 1566.96 837.429 18 -1 14 4 3766.53 1172.58 39 -1 14 4 2084.07 470.443 37 1 14 -3 4787.01 1306.49 18 -1 14 3 4045.75 1274.23 18 -1 14 3 5116.12 996.393 39 -1 14 3 4504.87 648.727 37 1 14 -2 9962.52 1929.14 18 -1 14 2 6583.06 1521.13 18 -1 14 2 6497.82 795.878 37 -1 14 2 9894.96 1402.90 39 1 14 -1 39425.3 3339.88 18 -1 14 1 41530.7 3464.79 18 -1 14 1 43226.6 2512.67 39 1 14 0 27067.4 2857.42 18 -1 14 0 30376.8 3003.00 18 -1 14 0 30992.1 2080.04 39 1 14 0 28825.5 2073.86 21 -1 14 -1 41332.0 3440.73 18 1 14 1 44424.2 3589.17 18 1 14 2 12302.2 1945.99 18 -1 14 -2 11118.9 1883.92 18 1 14 2 8953.37 1299.66 21 -1 14 -3 20178.7 2319.93 18 1 14 3 27490.9 2215.11 21 1 14 4 2038.53 827.102 21 1 14 5 2681.72 739.618 21 1 14 6 443.290 392.851 21 -1 15 6 4740.07 674.152 21 -1 15 5 7339.75 765.164 37 -1 15 5 10628.6 1126.47 21 -1 15 4 5543.80 729.919 37 -1 15 4 7981.79 1192.69 39 -1 15 3 13434.5 1829.09 18 1 15 -3 15986.2 2047.91 18 -1 15 3 16039.3 1603.07 39 -1 15 2 5241.98 1508.35 18 1 15 -2 5624.40 1412.60 18 -1 15 2 5248.67 1082.39 39 1 15 -1 7380.43 1702.09 18 -1 15 1 9024.14 1729.05 18 -1 15 1 7925.25 1144.65 39 1 15 0 7500.78 1691.74 18 -1 15 0 5722.04 1628.68 18 1 15 1 6055.62 1538.74 18 -1 15 -1 6571.10 1555.78 18 1 15 1 5054.27 991.335 21 -1 15 -2 5886.19 1574.98 18 1 15 2 4020.14 1122.95 18 1 15 2 6655.31 1087.19 21 -1 15 -3 2743.23 1130.68 18 1 15 3 3302.69 773.192 21 1 15 4 16756.3 1509.41 21 1 15 5 9291.51 1001.09 21 1 15 6 8720.51 815.575 21 -1 16 5 4602.05 681.895 21 -1 16 4 3292.67 717.141 21 -1 16 3 5458.72 1105.12 18 1 16 -3 6327.53 1334.48 18 1 16 -2 18103.2 2052.97 18 -1 16 2 15488.6 1850.25 18 -1 16 2 17360.9 1563.44 39 1 16 -1 2972.12 1205.58 18 -1 16 1 2921.72 1153.37 18 -1 16 1 2412.55 754.457 39 -1 16 0 26584.4 2595.57 18 1 16 0 25577.5 2658.50 18 1 16 1 2961.00 1118.53 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32 2 -14 4 745.406 330.691 34 2 -14 4 385.960 258.090 28 2 -14 5 5132.21 518.728 34 2 -14 5 4478.82 528.245 28 2 -14 6 3090.91 375.994 28 -2 -13 8 1192.11 249.164 34 -2 -13 7 2454.52 353.523 22 -2 -13 7 3105.64 412.692 30 -2 -13 6 1196.38 269.675 22 2 -13 4 10270.3 843.718 34 2 -13 5 9585.03 742.041 34 2 -13 6 556.967 232.881 34 2 -13 6 109.448 231.308 28 2 -13 6 619.944 253.724 25 2 -13 7 218.838 178.722 15 2 -13 7 289.376 204.555 28 -2 -12 8 7548.94 494.582 22 -2 -12 8 7815.75 607.430 25 2 -12 -7 920.867 229.952 32 -2 -12 7 1504.62 322.852 22 -2 -12 6 2964.36 396.145 22 2 -12 -2 5407.72 1494.35 11 2 -12 -2 4423.85 1229.83 10 2 -12 -1 1750.63 845.580 11 2 -12 -1 2389.02 920.794 10 2 -12 0 11531.3 2224.61 11 2 -12 0 10686.8 2039.92 10 2 -12 1 2777.86 1256.35 10 2 -12 3 3354.12 531.673 34 2 -12 4 619.104 406.634 34 2 -12 4 310.047 265.619 25 2 -12 5 1684.96 423.967 34 2 -12 5 1479.95 390.590 30 2 -12 5 1410.73 361.520 25 2 -12 6 7895.64 648.024 30 2 -12 6 8385.76 701.201 34 2 -12 6 7540.11 678.995 25 2 -12 7 334.350 216.227 34 2 -12 7 410.049 225.856 25 2 -12 7 242.652 265.159 28 -2 -11 9 1001.81 240.748 34 -2 -11 9 952.377 221.773 22 -2 -11 9 964.790 262.218 30 -2 -11 9 719.456 223.442 25 2 -11 -8 782.244 215.669 32 -2 -11 8 1289.15 299.373 22 2 -11 -7 1162.50 283.780 32 -2 -11 7 1160.05 312.944 22 2 -11 -7 1220.02 256.631 26 2 -11 -6 6944.09 570.490 26 2 -11 -5 9478.25 720.373 17 2 -11 -4 32892.3 3164.99 8 -2 -11 4 28952.0 2952.84 7 2 -11 -3 10734.0 1853.10 10 -2 -11 3 9572.88 1724.77 7 2 -11 -3 11205.5 1845.45 8 2 -11 -2 37771.1 3293.16 10 2 -11 -2 37693.7 3765.98 11 2 -11 -1 1899.19 843.555 11 2 -11 -1 2055.50 780.928 10 2 -11 0 20973.8 2510.80 10 2 -11 1 2779.20 1302.89 10 2 -11 2 8733.19 1912.29 13 2 -11 2 10926.2 2612.20 10 2 -11 3 15561.4 1073.72 34 2 -11 4 11405.0 933.620 34 2 -11 4 14063.6 1098.16 25 2 -11 5 16108.0 1047.89 34 2 -11 5 17910.1 1098.22 30 2 -11 5 15744.8 1162.70 25 2 -11 6 2973.02 489.117 34 2 -11 6 3002.27 466.705 30 2 -11 6 3531.34 549.423 25 2 -11 7 3411.10 465.585 34 2 -11 7 3276.26 438.128 30 2 -11 7 3604.55 488.073 25 2 -11 8-85.3575 178.654 28 2 -11 8 503.354 216.122 25 -2 -10 9 7387.40 505.218 20 2 -10 -9 5640.56 406.378 32 -2 -10 9 5862.98 492.253 34 -2 -10 9 7368.61 476.456 22 -2 -10 9 6555.13 539.540 30 -2 -10 8 1947.88 342.172 20 2 -10 -8 1997.14 343.684 32 -2 -10 8 1955.72 351.425 22 -2 -10 7 10500.6 719.376 20 -2 -10 7 8917.03 636.786 22 2 -10 -7 9597.76 673.724 26 -2 -10 6 2466.47 367.729 20 2 -10 -6 2563.53 381.607 26 2 -10 -5 57839.7 1764.69 17 2 -10 -4 23352.6 2618.23 8 -2 -10 4 20636.4 2458.61 7 2 -10 -4 22982.6 2862.91 10 2 -10 -3 11355.4 1773.67 8 -2 -10 3 9336.86 1562.08 7 2 -10 -3 10417.4 1755.03 10 -2 -10 2 29750.5 2734.74 7 2 -10 -2 29129.4 2634.39 8 2 -10 -2 29816.0 3161.60 11 2 -10 -2 28980.5 2740.78 10 2 -10 -1 51942.0 3492.08 10 2 -10 -1 55006.8 3987.10 11 2 -10 0 14207.2 1889.87 10 2 -10 1 47200.3 4107.08 10 2 -10 1 52327.6 3799.32 13 2 -10 2 5004.86 1776.27 10 2 -10 2 4565.10 1249.14 13 2 -10 3 13272.7 2858.07 10 2 -10 3 11728.8 1739.16 7 2 -10 3 12380.5 2372.98 13 2 -10 3 14563.4 1080.15 25 2 -10 4 11025.8 914.966 30 2 -10 4 10310.5 1019.66 25 2 -10 5 18373.9 1133.58 34 2 -10 5 20947.4 1235.25 30 2 -10 5 22232.1 1417.22 25 2 -10 6 8963.75 816.961 34 2 -10 6 8903.52 901.661 25 2 -10 7 2538.50 438.510 34 2 -10 7 2018.89 409.991 25 2 -10 7 2511.69 440.652 30 2 -10 8 2137.72 313.825 34 2 -10 8 2086.18 358.579 28 2 -10 8 2162.12 354.924 25 -2 -9 10 556.545 182.631 30 -2 -9 10 583.212 188.960 25 -2 -9 9 5761.27 510.110 20 2 -9 -9 5389.48 452.890 32 -2 -9 9 5888.41 482.948 22 -2 -9 9 6918.24 601.979 30 -2 -9 8 1967.49 432.568 20 2 -9 -8 1574.35 324.917 32 -2 -9 8 1987.40 376.077 22 -2 -9 7 20966.3 1040.79 20 2 -9 -7 21462.8 1036.55 26 -2 -9 6 23608.8 1110.36 20 2 -9 -6 21608.3 1054.00 26 2 -9 -5 57552.1 4216.61 8 2 -9 -5 57291.0 4570.48 10 2 -9 -5 52626.7 1673.40 17 2 -9 -4 31135.2 2895.42 8 -2 -9 4 27381.3 2684.87 7 2 -9 -4 27251.9 2940.98 10 -2 -9 3 99773.1 4910.23 7 2 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9580.85 786.872 24 9 -2 -3 5756.63 513.507 4 9 -2 -3 5140.71 614.538 24 9 -2 -2 8649.78 620.094 4 9 -2 -1 10477.1 706.578 4 9 -2 0 13442.0 883.519 4 9 -2 1 14219.0 988.335 4 9 -2 2 1472.88 379.142 4 9 -2 3 2225.81 351.250 4 -9 -1 7 1039.17 260.403 5 9 -1 -7 1077.69 222.316 24 9 -1 -6 9413.94 655.938 24 9 -1 -5 8438.21 642.043 4 9 -1 -5 9777.57 747.711 24 9 -1 -4 22504.5 1024.52 4 9 -1 -4 20629.7 1158.79 24 9 -1 -3 22375.9 996.267 4 9 -1 -3 19205.5 1111.08 24 9 -1 -2 20840.1 987.149 4 9 -1 -1 17934.7 970.586 4 9 -1 0 1992.55 397.945 4 9 -1 1 657.242 336.736 4 9 -1 2 685.345 328.062 4 9 -1 2 992.344 237.496 27 9 -1 3 1053.43 272.910 4 9 -1 3 1412.06 204.604 27 -9 0 7 7824.47 516.662 5 9 0 -7 8231.32 528.775 24 9 0 -6 3774.41 423.550 24 9 0 -5 1228.52 301.332 4 9 0 -5 1376.09 333.605 24 9 0 -4 993.675 256.557 4 9 0 -4 1155.15 333.881 24 9 0 -3 720.906 249.124 4 9 0 -3 661.343 271.535 24 9 0 -2 2842.08 363.309 4 9 0 -1 14605.6 895.016 4 9 0 0 8492.40 790.883 4 9 0 1 17936.7 1272.01 4 9 0 2 7265.91 854.107 4 9 0 2 13660.9 748.108 27 9 0 3 7432.44 459.535 27 -9 1 7 1540.50 277.504 5 9 1 -7 1211.94 222.827 24 9 1 -6 9256.08 643.504 24 9 1 -5 10170.5 688.115 4 9 1 -5 10384.7 742.698 24 9 1 -4 21551.9 1006.35 4 9 1 -4 18539.3 1034.10 24 9 1 -3 23635.9 1026.08 4 9 1 -2 20112.7 973.788 4 9 1 -1 18500.5 998.188 4 9 1 0 2438.80 458.029 4 9 1 1 833.825 366.641 4 9 1 2 715.101 369.298 4 9 1 2 652.718 201.563 27 9 1 3 1513.48 336.375 4 9 1 3 1216.24 204.058 27 -9 2 7 455.771 224.962 5 9 2 -7 450.671 154.507 24 9 2 -6 20779.1 920.245 24 9 2 -5 3550.70 422.311 4 9 2 -5 4055.71 469.435 24 9 2 -4 9700.38 676.972 4 9 2 -4 8781.20 673.202 24 9 2 -3 5494.95 504.255 4 9 2 -2 8764.92 637.173 4 9 2 -1 11118.9 752.127 4 9 2 0 15271.1 977.436 4 9 2 1 16866.1 1176.76 4 9 2 1 17958.5 881.706 27 9 2 2 1486.30 419.355 4 9 2 2 1658.05 276.196 27 9 2 3 2015.09 347.474 4 9 2 3 3675.38 321.495 27 -9 3 7 3742.60 348.240 5 9 3 -7 3529.14 331.268 24 9 3 -6 15364.7 733.890 24 9 3 -5 11750.2 734.481 24 9 3 -4 7999.73 598.187 4 9 3 -3 10315.7 666.558 4 9 3 -2 6728.79 522.434 4 9 3 -1 18020.1 910.400 4 9 3 0 8755.87 716.678 4 9 3 1 2664.62 451.429 4 9 3 1 3082.61 377.288 27 9 3 2 5147.70 600.174 4 9 3 2 6774.49 505.477 27 9 3 3 411.921 168.350 4 9 3 3 449.192 150.849 27 9 4 -7 14479.6 583.573 24 9 4 -6 4182.13 379.735 24 -9 4 5 10168.1 2141.90 16 9 4 -5 15306.9 732.108 24 9 4 -4 17437.4 848.485 4 9 4 -3 6173.34 503.403 4 9 4 -2 6120.97 506.627 4 9 4 -1 6069.71 505.974 4 9 4 0 2055.23 331.898 4 9 4 1 12050.4 790.523 4 -9 4 -1 10295.4 1678.51 16 9 4 1 12251.8 700.650 27 9 4 2 5415.88 484.896 4 9 4 2 6411.52 478.071 27 -9 5 6 1763.21 265.238 5 9 5 -6 1171.81 219.573 24 -9 5 5 4044.10 1619.69 16 9 5 -4 340.982 180.562 4 -9 5 4 410.520 1121.28 16 9 5 -3 9288.20 587.960 4 9 5 -2 7526.06 522.314 4 9 5 -1 3477.62 361.435 4 9 5 0 12280.3 686.938 4 -9 5 0 10163.7 1908.54 16 9 5 0 10889.0 627.605 27 9 5 1 12492.4 663.152 4 -9 5 -1 14292.7 1898.69 16 9 5 1 13778.4 715.259 27 9 5 2 8124.32 515.253 27 -9 6 5 6454.25 1547.43 16 -9 6 4 12673.9 2207.97 16 9 6 -3 9795.18 572.811 4 -9 6 3 8504.59 1911.76 16 9 6 -2 2865.83 304.264 4 -9 6 2 5019.58 1837.94 16 9 6 -1 5339.57 409.841 4 -9 6 1 4382.00 1656.29 16 -9 6 0 5855.89 1458.01 16 -9 6 -1 1494.98 829.728 16 9 6 1 270.423 156.169 27 9 6 2 7687.70 472.331 27 -9 7 4 3321.84 1103.29 16 -9 7 3 2127.11 1304.24 16 -9 7 2 9938.02 1981.40 16 -9 7 1 12302.4 2050.22 16 -9 7 0 3596.60 1190.31 16 -9 8 4 6846.49 1459.60 16 -9 8 3 8832.34 1748.29 16 -9 8 2 1972.35 881.253 16 -9 8 1 7644.03 1560.99 16 -9 8 0 3887.89 954.963 16 -9 9 4 13284.7 888.517 39 -9 9 3 12816.5 1683.98 16 -9 9 2 13181.4 1641.90 16 -9 9 1 25808.1 2283.00 16 10 -4 -4 2566.08 332.871 24 10 -4 -3 2030.61 218.944 4 10 -4 -2 527.676 130.311 4 10 -4 -1 477.458 121.706 4 10 -3 -5 3147.75 320.899 24 10 -3 -4 8248.90 585.501 24 10 -3 -3 14441.6 598.196 4 10 -3 -2 17149.1 654.456 4 10 -3 -1 10253.7 507.575 4 10 -3 0 2948.67 263.356 4 10 -2 -5 5107.16 415.979 24 10 -2 -4 16895.6 674.919 4 10 -2 -4 15197.2 749.829 24 10 -2 -3 814.698 170.412 4 10 -2 -2 522.804 140.680 4 10 -2 -1 2702.45 281.316 4 10 -2 0 8040.62 473.763 4 10 -1 -5 2164.35 286.443 24 10 -1 -4 10225.4 551.469 4 10 -1 -3 12999.9 611.312 4 10 -1 -2 17992.9 734.885 4 10 -1 -1 22811.2 834.653 4 10 -1 0 5855.45 433.639 4 10 -1 1 7981.56 457.965 4 -10 0 6 4090.77 311.400 5 10 0 -4 5498.88 418.991 4 10 0 -3 852.847 187.293 4 10 0 -2 164.894 107.083 4 10 0 -1 137.151 111.040 4 10 0 0 1892.23 273.006 4 10 0 1 6725.79 440.552 4 10 1 -4 8495.13 503.449 4 10 1 -3 12119.0 595.540 4 10 1 -2 17349.7 731.926 4 10 1 -1 25037.9 899.407 4 10 1 0 7475.70 521.908 4 10 1 1 8181.90 486.893 4 10 2 -4 16156.4 683.680 4 10 2 -3 783.272 174.280 4 10 2 -2 341.331 136.082 4 10 2 -1 3209.94 329.248 4 10 2 0 10966.1 624.693 4 -10 2 0 6273.60 1180.88 16 -10 3 4 10345.1 2026.42 16 10 3 -3 16555.6 653.917 4 10 3 -2 20619.8 740.947 4 10 3 -1 13933.5 632.334 4 -10 3 1 10424.7 1800.93 16 10 3 0 4257.45 349.986 4 -10 4 4 1532.37 945.401 16 10 4 -3 2077.58 232.295 4 -10 4 3 963.902 964.411 16 10 4 -2 590.114 135.753 4 -10 4 2 239.557 758.650 16 10 4 -1 697.010 143.593 4 -10 4 1 425.085 794.596 16 -10 5 3 4828.32 1296.95 16 -10 5 2-206.887 734.996 16 -10 5 1 1218.88 796.652 16 -10 6 2 2693.01 986.194 16 0 0 0 0.00 0.00 0 TITL amd-r1398-dia2 in P2(1) REM P2(1) (#4 in standard setting) CELL 1.54184 8.518225 15.307430 9.164590 90.0000 103.1043 90.0000 ZERR 2.00 0.000223 0.000477 0.000278 0.0000 0.0028 0.0000 LATT -1 SYMM -x, y+1/2,-z SFAC C H N S Cl Cu UNIT 46.00 70.00 2.00 2.00 2.00 2.00 REM CrysAlisPro recorded range (K): Min=139.8; max=140.2; aver:140.0 TEMP -133 SIZE 0.09 0.12 0.40 TREF HKLF 4 END ; _shelx_hkl_checksum 21911 _olex2_date_sample_data_collection 2023-09-19 _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 - Detector area scaling - B-factor correction ; _oxdiff_exptl_absorpt_empirical_full_max 6.570 _oxdiff_exptl_absorpt_empirical_full_min 0.400 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' 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 Cu1 Cu 0.51511(7) 0.33796(4) 0.44866(7) 0.02280(19) Uani 1 1 d . . . . . Cl1 Cl 0.71653(13) 0.25666(8) 0.45532(13) 0.0284(3) Uani 1 1 d . . . . . S1 S 0.4357(3) 0.58860(11) 0.06324(19) 0.0518(5) Uani 1 1 d . . . . . N1 N 0.1899(5) 0.3868(3) 0.4407(4) 0.0213(8) Uani 1 1 d . . . . . C1 C 0.3382(6) 0.4113(3) 0.4511(5) 0.0218(9) Uani 1 1 d . . . . . C2 C 0.3531(5) 0.5086(3) 0.4803(5) 0.0232(9) Uani 1 1 d . . . . . C3 C 0.1798(6) 0.5400(3) 0.4763(6) 0.0268(10) Uani 1 1 d . . . . . H3A H 0.176938 0.573531 0.568024 0.032 Uiso 1 1 calc R U . . . H3B H 0.140117 0.577857 0.388135 0.032 Uiso 1 1 calc R U . . . C4 C 0.0748(5) 0.4571(3) 0.4668(6) 0.0251(9) Uani 1 1 d . . . . . C5 C 0.4635(7) 0.5230(4) 0.6359(6) 0.0373(12) Uani 1 1 d . . . . . H5A H 0.423270 0.489018 0.710350 0.056 Uiso 1 1 calc R U . . . H5B H 0.464656 0.585166 0.661640 0.056 Uiso 1 1 calc R U . . . H5C H 0.573168 0.503989 0.634918 0.056 Uiso 1 1 calc R U . . . C6 C 0.4331(5) 0.5527(4) 0.3640(6) 0.0282(10) Uani 1 1 d . . . . . H6A H 0.447148 0.615630 0.388289 0.034 Uiso 1 1 calc R U . . . H6B H 0.541614 0.527149 0.372965 0.034 Uiso 1 1 calc R U . . . C7 C 0.3390(7) 0.5434(4) 0.2027(6) 0.0326(11) Uani 1 1 d . . . . . H7A H 0.233015 0.572178 0.192699 0.039 Uiso 1 1 calc R U . . . H7B H 0.318701 0.480513 0.180893 0.039 Uiso 1 1 calc R U . . . C8 C 0.3955(6) 0.7022(4) 0.0608(6) 0.0303(10) Uani 1 1 d . . . . . C9 C 0.3334(6) 0.7470(4) 0.1689(5) 0.0299(10) Uani 1 1 d . . . . . H9 H 0.307519 0.715865 0.250023 0.036 Uiso 1 1 calc R U . . . C10 C 0.3100(6) 0.8359(4) 0.1576(5) 0.0302(9) Uani 1 1 d . . . . . H10 H 0.267315 0.865626 0.231041 0.036 Uiso 1 1 calc R U . . . C11 C 0.3478(7) 0.8830(4) 0.0405(6) 0.0331(11) Uani 1 1 d . . . . . H11 H 0.333045 0.944528 0.034451 0.040 Uiso 1 1 calc R U . . . C12 C 0.4079(6) 0.8385(5) -0.0679(6) 0.0346(10) Uani 1 1 d . . . . . H12 H 0.434006 0.869794 -0.148648 0.042 Uiso 1 1 calc R U . . . C13 C 0.4295(6) 0.7490(4) -0.0585(6) 0.0342(11) Uani 1 1 d . . . . . H13 H 0.468084 0.719195 -0.134272 0.041 Uiso 1 1 calc R U . . . C14 C 0.0262(7) 0.4376(4) 0.6145(7) 0.0356(12) Uani 1 1 d . . . . . H14A H -0.029571 0.381209 0.606992 0.053 Uiso 1 1 calc R U . . . H14B H -0.045848 0.483694 0.634769 0.053 Uiso 1 1 calc R U . . . H14C H 0.122831 0.435410 0.696229 0.053 Uiso 1 1 calc R U . . . C15 C -0.0739(6) 0.4621(4) 0.3376(7) 0.0339(11) Uani 1 1 d . . . . . H15A H -0.040201 0.471162 0.243359 0.051 Uiso 1 1 calc R U . . . H15B H -0.142081 0.510939 0.354451 0.051 Uiso 1 1 calc R U . . . H15C H -0.134827 0.407444 0.332173 0.051 Uiso 1 1 calc R U . . . C16 C 0.1363(6) 0.2937(3) 0.4238(5) 0.0245(9) Uani 1 1 d . . . . . H16 H 0.016904 0.293246 0.413478 0.029 Uiso 1 1 calc R U . . . C17 C 0.2111(7) 0.2438(4) 0.5665(6) 0.0349(11) Uani 1 1 d . . . . . H17A H 0.325784 0.233771 0.570996 0.052 Uiso 1 1 calc R U . . . H17B H 0.156277 0.187478 0.566377 0.052 Uiso 1 1 calc R U . . . H17C H 0.199482 0.277928 0.653834 0.052 Uiso 1 1 calc R U . . . C18 C 0.1693(5) 0.2537(3) 0.2793(5) 0.0232(9) Uani 1 1 d . . . . . H18 H 0.287973 0.257054 0.285899 0.028 Uiso 1 1 calc R U . . . C19 C 0.0841(6) 0.3028(4) 0.1385(5) 0.0287(10) Uani 1 1 d . . . . . H19A H -0.033450 0.303045 0.132460 0.034 Uiso 1 1 calc R U . . . H19B H 0.121539 0.364222 0.145237 0.034 Uiso 1 1 calc R U . . . C20 C 0.1164(7) 0.2614(4) -0.0034(6) 0.0375(12) Uani 1 1 d . . . . . H20A H 0.054424 0.293159 -0.091997 0.045 Uiso 1 1 calc R U . . . H20B H 0.232364 0.267243 -0.002615 0.045 Uiso 1 1 calc R U . . . C21 C 0.0701(7) 0.1657(5) -0.0164(7) 0.0453(14) Uani 1 1 d . . . . . H21A H 0.101380 0.140071 -0.104941 0.054 Uiso 1 1 calc R U . . . H21B H -0.048169 0.160006 -0.030888 0.054 Uiso 1 1 calc R U . . . C22 C 0.1531(7) 0.1162(4) 0.1234(7) 0.0391(13) Uani 1 1 d . . . . . H22A H 0.270765 0.115624 0.130257 0.047 Uiso 1 1 calc R U . . . H22B H 0.114944 0.054916 0.115518 0.047 Uiso 1 1 calc R U . . . C23 C 0.1203(6) 0.1568(4) 0.2653(7) 0.0325(11) Uani 1 1 d . . . . . H23A H 0.181334 0.124502 0.353682 0.039 Uiso 1 1 calc R U . . . H23B H 0.004129 0.151545 0.263745 0.039 Uiso 1 1 calc R U . . . 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 Cu1 0.0162(3) 0.0165(4) 0.0352(3) 0.0006(3) 0.0048(2) 0.0023(2) Cl1 0.0220(5) 0.0206(6) 0.0444(6) 0.0041(4) 0.0110(4) 0.0053(4) S1 0.0855(12) 0.0282(9) 0.0558(8) 0.0088(6) 0.0454(8) 0.0163(7) N1 0.0213(19) 0.013(2) 0.0314(18) 0.0001(14) 0.0092(14) 0.0011(14) C1 0.022(2) 0.019(3) 0.024(2) 0.0003(16) 0.0044(15) -0.0025(17) C2 0.019(2) 0.016(2) 0.034(2) -0.0003(17) 0.0051(17) 0.0017(16) C3 0.023(2) 0.017(3) 0.043(3) -0.0018(18) 0.0132(18) -0.0003(17) C4 0.023(2) 0.014(2) 0.042(2) 0.0006(18) 0.0142(18) 0.0044(17) C5 0.040(3) 0.025(3) 0.039(3) -0.003(2) -0.007(2) 0.000(2) C6 0.021(2) 0.021(3) 0.044(3) 0.003(2) 0.0107(18) -0.0002(17) C7 0.042(3) 0.018(3) 0.040(3) 0.004(2) 0.015(2) 0.001(2) C8 0.033(2) 0.024(3) 0.036(2) 0.002(2) 0.0114(19) 0.0029(19) C9 0.034(2) 0.027(3) 0.030(2) 0.0018(19) 0.0099(18) 0.0014(19) C10 0.032(2) 0.026(3) 0.031(2) -0.004(2) 0.0038(16) 0.001(2) C11 0.031(3) 0.023(3) 0.043(3) -0.002(2) 0.003(2) -0.0002(19) C12 0.035(2) 0.030(3) 0.040(2) 0.007(2) 0.0116(18) -0.004(2) C13 0.034(2) 0.035(3) 0.036(2) 0.000(2) 0.012(2) 0.003(2) C14 0.041(3) 0.022(3) 0.051(3) -0.003(2) 0.026(2) 0.003(2) C15 0.022(2) 0.023(3) 0.055(3) 0.001(2) 0.005(2) 0.002(2) C16 0.023(2) 0.013(2) 0.040(3) -0.0019(18) 0.0124(18) -0.0019(17) C17 0.046(3) 0.018(3) 0.046(3) 0.007(2) 0.019(2) 0.000(2) C18 0.0160(18) 0.015(2) 0.038(2) -0.0041(18) 0.0049(16) -0.0009(16) C19 0.024(2) 0.025(3) 0.034(2) -0.0032(19) 0.0008(18) 0.0002(18) C20 0.034(3) 0.043(4) 0.032(2) -0.004(2) 0.0017(19) 0.003(2) C21 0.035(3) 0.045(4) 0.049(3) -0.020(3) -0.003(2) 0.004(3) C22 0.038(3) 0.023(3) 0.054(3) -0.015(2) 0.006(2) 0.000(2) C23 0.029(2) 0.015(3) 0.054(3) -0.004(2) 0.013(2) -0.0034(18) 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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 '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' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 2 1 -1 0.2262 -2 -1 1 0.1587 -2 1 1 0.1578 2 -1 -1 0.2262 2 0 -1 0.2326 1 0 -1 0.2079 0 -1 -1 0.0411 1 -10 0 0.0649 -1 10 0 0.0639 5 5 0 0.2125 0 4 5 0.0443 1 -1 5 0.0554 1 -9 2 0.0551 4 1 3 0.1589 -1 2 -5 0.0305 1 9 -3 0.1122 2 -4 5 0.0637 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 C1 Cu1 Cl1 177.68(14) . . ? C8 S1 C7 105.5(2) . . ? C1 N1 C4 115.9(4) . . ? C1 N1 C16 123.5(4) . . ? C16 N1 C4 120.2(4) . . ? N1 C1 Cu1 126.4(4) . . ? N1 C1 C2 109.8(4) . . ? C2 C1 Cu1 123.6(3) . . ? C1 C2 C3 105.1(4) . . ? C1 C2 C5 108.3(4) . . ? C1 C2 C6 109.9(4) . . ? C5 C2 C3 111.0(4) . . ? C5 C2 C6 107.8(4) . . ? C6 C2 C3 114.6(4) . . ? C2 C3 H3A 110.4 . . ? C2 C3 H3B 110.4 . . ? H3A C3 H3B 108.6 . . ? C4 C3 C2 106.5(4) . . ? C4 C3 H3A 110.4 . . ? C4 C3 H3B 110.4 . . ? N1 C4 C3 101.9(4) . . ? N1 C4 C14 108.4(4) . . ? N1 C4 C15 111.5(4) . . ? C14 C4 C3 112.3(4) . . ? C15 C4 C3 111.8(4) . . ? C15 C4 C14 110.6(4) . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C2 C6 H6A 108.7 . . ? C2 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? C7 C6 C2 114.4(4) . . ? C7 C6 H6A 108.7 . . ? C7 C6 H6B 108.7 . . ? S1 C7 H7A 108.4 . . ? S1 C7 H7B 108.4 . . ? C6 C7 S1 115.3(4) . . ? C6 C7 H7A 108.4 . . ? C6 C7 H7B 108.4 . . ? H7A C7 H7B 107.5 . . ? C9 C8 S1 125.0(4) . . ? C13 C8 S1 116.2(4) . . ? C13 C8 C9 118.8(5) . . ? C8 C9 H9 120.0 . . ? C10 C9 C8 120.1(5) . . ? C10 C9 H9 120.0 . . ? C9 C10 H10 119.5 . . ? C9 C10 C11 121.1(5) . . ? C11 C10 H10 119.5 . . ? C10 C11 H11 120.5 . . ? C10 C11 C12 118.9(5) . . ? C12 C11 H11 120.5 . . ? C11 C12 H12 119.8 . . ? C13 C12 C11 120.4(5) . . ? C13 C12 H12 119.8 . . ? C8 C13 H13 119.6 . . ? C12 C13 C8 120.7(5) . . ? C12 C13 H13 119.6 . . ? C4 C14 H14A 109.5 . . ? C4 C14 H14B 109.5 . . ? C4 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C4 C15 H15A 109.5 . . ? C4 C15 H15B 109.5 . . ? C4 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N1 C16 H16 107.2 . . ? N1 C16 C17 109.3(4) . . ? N1 C16 C18 110.9(4) . . ? C17 C16 H16 107.2 . . ? C17 C16 C18 114.6(4) . . ? C18 C16 H16 107.2 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18 107.8 . . ? C19 C18 C16 112.7(4) . . ? C19 C18 H18 107.8 . . ? C19 C18 C23 109.6(4) . . ? C23 C18 C16 110.8(4) . . ? C23 C18 H18 107.8 . . ? C18 C19 H19A 109.2 . . ? C18 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? C20 C19 C18 111.8(4) . . ? C20 C19 H19A 109.2 . . ? C20 C19 H19B 109.2 . . ? C19 C20 H20A 109.2 . . ? C19 C20 H20B 109.2 . . ? H20A C20 H20B 107.9 . . ? C21 C20 C19 112.0(5) . . ? C21 C20 H20A 109.2 . . ? C21 C20 H20B 109.2 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? C20 C21 C22 110.7(5) . . ? H21A C21 H21B 108.1 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? C21 C22 H22A 109.2 . . ? C21 C22 H22B 109.2 . . ? C21 C22 C23 112.1(5) . . ? H22A C22 H22B 107.9 . . ? C23 C22 H22A 109.2 . . ? C23 C22 H22B 109.2 . . ? C18 C23 H23A 109.3 . . ? C18 C23 H23B 109.3 . . ? C22 C23 C18 111.5(5) . . ? C22 C23 H23A 109.3 . . ? C22 C23 H23B 109.3 . . ? H23A C23 H23B 108.0 . . ? 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 Cu1 Cl1 2.1092(12) . ? Cu1 C1 1.883(5) . ? S1 C7 1.808(5) . ? S1 C8 1.772(6) . ? N1 C1 1.301(6) . ? N1 C4 1.511(6) . ? N1 C16 1.494(6) . ? C1 C2 1.514(7) . ? C2 C3 1.545(6) . ? C2 C5 1.536(7) . ? C2 C6 1.544(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.543(7) . ? C4 C14 1.532(7) . ? C4 C15 1.527(7) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C6 C7 1.520(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.403(7) . ? C8 C13 1.392(7) . ? C9 H9 0.9500 . ? C9 C10 1.377(9) . ? C10 H10 0.9500 . ? C10 C11 1.390(8) . ? C11 H11 0.9500 . ? C11 C12 1.394(8) . ? C12 H12 0.9500 . ? C12 C13 1.381(10) . ? C13 H13 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16 1.0000 . ? C16 C17 1.524(7) . ? C16 C18 1.541(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18 1.0000 . ? C18 C19 1.528(7) . ? C18 C23 1.538(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C19 C20 1.526(7) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C20 C21 1.515(10) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C21 C22 1.518(10) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C22 C23 1.523(8) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? 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 Cu1 C1 C2 C3 -178.2(3) . . . . ? Cu1 C1 C2 C5 -59.6(5) . . . . ? Cu1 C1 C2 C6 57.9(5) . . . . ? S1 C8 C9 C10 178.6(4) . . . . ? S1 C8 C13 C12 -177.7(4) . . . . ? N1 C1 C2 C3 -3.2(5) . . . . ? N1 C1 C2 C5 115.4(5) . . . . ? N1 C1 C2 C6 -127.0(4) . . . . ? N1 C16 C18 C19 -59.0(5) . . . . ? N1 C16 C18 C23 177.7(4) . . . . ? C1 N1 C4 C3 7.6(5) . . . . ? C1 N1 C4 C14 -111.0(5) . . . . ? C1 N1 C4 C15 127.0(5) . . . . ? C1 N1 C16 C17 66.7(6) . . . . ? C1 N1 C16 C18 -60.6(6) . . . . ? C1 C2 C3 C4 7.7(5) . . . . ? C1 C2 C6 C7 61.5(5) . . . . ? C2 C3 C4 N1 -8.8(5) . . . . ? C2 C3 C4 C14 107.0(5) . . . . ? C2 C3 C4 C15 -128.0(4) . . . . ? C2 C6 C7 S1 -176.4(3) . . . . ? C3 C2 C6 C7 -56.6(6) . . . . ? C4 N1 C1 Cu1 171.9(3) . . . . ? C4 N1 C1 C2 -2.9(6) . . . . ? C4 N1 C16 C17 -105.3(5) . . . . ? C4 N1 C16 C18 127.4(4) . . . . ? C5 C2 C3 C4 -109.1(5) . . . . ? C5 C2 C6 C7 179.3(5) . . . . ? C6 C2 C3 C4 128.5(5) . . . . ? C7 S1 C8 C9 12.7(6) . . . . ? C7 S1 C8 C13 -167.5(4) . . . . ? C8 S1 C7 C6 -81.0(5) . . . . ? C8 C9 C10 C11 -0.4(8) . . . . ? C9 C8 C13 C12 2.2(8) . . . . ? C9 C10 C11 C12 1.1(8) . . . . ? C10 C11 C12 C13 -0.1(8) . . . . ? C11 C12 C13 C8 -1.5(8) . . . . ? C13 C8 C9 C10 -1.3(8) . . . . ? C16 N1 C1 Cu1 -0.3(7) . . . . ? C16 N1 C1 C2 -175.2(4) . . . . ? C16 N1 C4 C3 -179.8(4) . . . . ? C16 N1 C4 C14 61.6(6) . . . . ? C16 N1 C4 C15 -60.5(6) . . . . ? C16 C18 C19 C20 -179.2(4) . . . . ? C16 C18 C23 C22 -179.7(4) . . . . ? C17 C16 C18 C19 176.7(4) . . . . ? C17 C16 C18 C23 53.4(5) . . . . ? C18 C19 C20 C21 55.8(6) . . . . ? C19 C18 C23 C22 55.3(5) . . . . ? C19 C20 C21 C22 -54.4(6) . . . . ? C20 C21 C22 C23 54.7(7) . . . . ? C21 C22 C23 C18 -55.9(6) . . . . ? C23 C18 C19 C20 -55.2(5) . . . . ? 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 1.9983 1.0012 -1.0005 -0.1095 0.3110 0.1995 -1.9983 -1.0012 1.0005 0.1095 -0.3110 -0.1995 -1.9993 0.9990 1.0012 0.0872 -0.3753 -0.0100 1.9993 -0.9990 -1.0012 -0.0872 0.3753 0.0100 1.9988 0.0011 -1.0009 -0.0984 0.3432 0.1047 0.9997 0.0010 -1.0009 -0.1350 0.1724 0.0426 0.0011 -0.9993 -1.0013 -0.1604 0.0337 -0.1143 1.2269 -9.6817 -0.1719 0.1238 0.5205 -0.8448 -1.0947 9.7338 0.1764 -0.1187 -0.4996 0.8581 4.6722 4.7801 0.2190 0.1553 0.6453 0.7480 0.1710 4.1518 5.2202 0.8548 -0.1115 0.5068 0.9663 -0.7730 5.4518 0.9788 0.1821 0.0939 1.2410 -8.9119 1.8977 0.4705 0.4952 -0.7303 4.0950 1.3102 2.8224 0.6193 0.6541 0.4343 -0.7100 2.1545 -5.4338 -0.9817 -0.1826 0.0533 0.9871 8.6479 -2.8922 -0.5564 -0.1043 0.8243 1.5401 -3.7842 4.7325 0.9102 0.3778 -0.1699