#------------------------------------------------------------------------------ #$Date: 2021-10-07 02:46:29 +0300 (Thu, 07 Oct 2021) $ #$Revision: 269813 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/48/1564851.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_1564851 loop_ _publ_author_name 'Toikka, Yulia N.' 'Spiridonova, Dar’ya V.' 'Novikov, Alexander S.' 'Bokach, Nadezhda A.' _publ_section_title ; Copper(II) Prevents the Saccarine-Dialkylcyanamide Coupling by Forming Mononuclear (Saccharinate)(Dialkylcyanamide)copper(II) Complexes ; _journal_issue 9 _journal_name_full Inorganics _journal_page_first 69 _journal_paper_doi 10.3390/inorganics9090069 _journal_volume 9 _journal_year 2021 _chemical_formula_moiety 'C17 H18 Cu N4 O8 S2' _chemical_formula_sum 'C17 H18 Cu N4 O8 S2' _chemical_formula_weight 534.01 _space_group_crystal_system orthorhombic _space_group_IT_number 62 _space_group_name_Hall '-P 2ac 2n' _space_group_name_H-M_alt 'P n m a' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2021-02-02 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.14100(10) _cell_length_b 23.8599(4) _cell_length_c 12.48922(19) _cell_measurement_reflns_used 5013 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 70.2150 _cell_measurement_theta_min 1.8630 _cell_volume 2127.96(6) _computing_cell_refinement 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix3000 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _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 -62.00 -12.00 0.50 0.20 -- -38.82 97.00-113.00 100 2 \w -1.00 30.00 0.50 0.20 -- -38.82 27.00 111.00 62 3 \w -47.00 -6.00 0.50 0.20 -- -38.82 27.00 111.00 82 4 \w -72.00 -37.00 0.50 0.20 -- -38.82 122.00 -34.00 70 5 \w 77.00 102.00 0.50 0.20 -- 38.82 27.00 111.00 50 6 \w 18.00 58.00 0.50 0.20 -- 38.82-150.00 82.00 80 7 \w 24.00 49.00 0.50 0.20 -- 38.82 27.00 111.00 50 8 \w 33.00 59.00 0.50 0.20 -- 38.82 -97.00 139.00 52 9 \w 31.00 63.00 0.50 0.20 -- 38.82-122.00-115.00 64 10 \w -29.00 -3.00 0.50 0.20 -- 38.82 -27.00 -51.00 52 11 \w 85.00 147.00 0.50 0.20 -- 100.00 97.00-113.00 124 12 \w 31.00 72.00 0.50 0.20 -- 100.00 -27.00 -51.00 82 13 \w 110.00 136.00 0.50 0.20 -- 100.00 27.00 111.00 52 14 \w 69.00 94.00 0.50 0.20 -- 100.00-122.00-115.00 50 15 \w 60.00 93.00 0.50 0.20 -- 100.00 -97.00 139.00 66 16 \w 85.00 110.00 0.50 0.20 -- 100.00 150.00 127.00 50 17 \w -104.00 -51.00 0.50 0.20 -- -38.82 -21.00 120.00 106 18 \w -90.00 -65.00 0.50 0.20 -- -38.82 -27.00 -51.00 50 19 \w 56.00 81.00 0.50 0.20 -- 38.82 54.00-120.00 50 20 \w -18.00 8.00 0.50 0.20 -- 38.82 -43.00-150.00 52 21 \w 15.00 55.00 0.50 0.20 -- 38.82 -43.00-150.00 80 22 \w 89.00 115.00 0.50 0.20 -- 100.00 37.00-120.00 52 23 \w 55.00 83.00 0.50 0.20 -- 100.00-111.00 60.00 56 24 \w 84.00 156.00 0.50 0.20 -- 100.00 111.00 0.00 144 25 \w 70.00 155.00 0.50 0.20 -- 100.00 15.00 0.00 170 26 \w 34.00 125.00 0.50 0.20 -- 100.00 -69.00-180.00 182 27 \w 36.00 80.00 0.50 0.20 -- 100.00-133.00 150.00 88 28 \w 36.00 82.00 0.50 0.20 -- 100.00-133.00-150.00 92 29 \w 104.00 157.00 0.50 0.20 -- 100.00 93.00 30.00 106 30 \w 77.00 108.50 0.50 0.20 -- 100.00-150.00 82.00 63 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, HyPix3000' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0649740000 _diffrn_orient_matrix_UB_12 -0.0593066000 _diffrn_orient_matrix_UB_13 -0.0314768000 _diffrn_orient_matrix_UB_21 0.0383342000 _diffrn_orient_matrix_UB_22 -0.0134764000 _diffrn_orient_matrix_UB_23 0.1186209000 _diffrn_orient_matrix_UB_31 -0.2021595000 _diffrn_orient_matrix_UB_32 -0.0216383000 _diffrn_orient_matrix_UB_33 0.0124252000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_unetI/netI 0.0247 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 7905 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 69.944 _diffrn_reflns_theta_min 3.705 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 3.773 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.77050 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear blue' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary blue _exptl_crystal_density_diffrn 1.667 _exptl_crystal_description prism _exptl_crystal_F_000 1092 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.561 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.082 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 163 _refine_ls_number_reflns 2068 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0338 _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^)+(0.0532P)^2^+1.6018P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0929 _refine_ls_wR_factor_ref 0.0951 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1919 _reflns_number_total 2068 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file YN44.cif _cod_data_source_block yn44 _cod_database_code 1564851 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'Cu1 C16 N4 O2' _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 0.704 _shelx_estimated_absorpt_t_min 0.550 _reflns_odcompleteness_completeness 98.88 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 70.93 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5), C6(H6) 2.b Idealised Me refined as rotating group: C9(H9A,H9B,H9C) ; _shelx_res_file ; TITL yn44_a.res in Pnma yn44.res created by SHELXL-2018/3 at 17:29:50 on 02-Feb-2021 REM Old TITL YN44 in Pnma #62 REM SHELXT solution in Pnma REM R1 0.386, Rweak 0.010, Alpha 0.029, Orientation as input REM Formula found by SHELXT: C19 Cu N11 CELL 1.54184 7.141003 23.859935 12.489225 90 90 90 ZERR 4 0.0001 0.000387 0.00019 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,-Z SYMM 0.5+X,0.5-Y,0.5-Z SFAC C H Cu N O S UNIT 68 72 4 16 32 8 L.S. 20 PLAN 20 SIZE 0.18 0.16 0.1 BOND $H HTAB conf list 4 fmap 2 acta OMIT -4 140 REM REM REM WGHT 0.053200 1.601800 FVAR 2.43641 CU1 3 0.751171 0.250000 0.588367 10.50000 0.01471 0.00898 = 0.01111 0.00000 -0.00006 0.00000 S1 6 0.763737 0.383053 0.523953 11.00000 0.02482 0.01082 = 0.01264 0.00158 0.00088 -0.00146 O1 5 0.477063 0.250000 0.600640 10.50000 0.01716 0.01307 = 0.02086 0.00000 0.00117 0.00000 H1 2 0.427262 0.278772 0.626017 11.00000 0.03658 O2 5 1.025881 0.250000 0.603762 10.50000 0.01762 0.01373 = 0.02638 0.00000 -0.00332 0.00000 H2 2 1.078451 0.279611 0.631968 11.00000 0.03994 O3 5 0.756318 0.325490 0.798856 11.00000 0.02291 0.01568 = 0.01546 0.00538 0.00011 0.00032 O4 5 0.587016 0.387923 0.470234 11.00000 0.03600 0.02088 = 0.02341 0.00504 -0.00981 -0.00185 O5 5 0.926531 0.376115 0.458250 11.00000 0.03821 0.02225 = 0.02289 0.00080 0.01407 -0.00339 N1 4 0.752715 0.333393 0.616112 11.00000 0.01965 0.01126 = 0.01416 0.00144 0.00119 -0.00045 N2 4 0.750217 0.250000 0.416061 10.50000 0.02352 0.01965 = 0.01300 0.00000 0.00047 0.00000 N3 4 0.808134 0.250000 0.221516 10.50000 0.02964 0.02184 = 0.01287 0.00000 0.00265 0.00000 C1 1 0.766599 0.354116 0.715862 11.00000 0.01417 0.01262 = 0.01637 0.00108 0.00039 0.00080 C2 1 0.795914 0.416058 0.718085 11.00000 0.01330 0.01394 = 0.01939 0.00057 0.00109 0.00034 C3 1 0.824042 0.449756 0.806885 11.00000 0.01877 0.01990 = 0.01940 -0.00249 0.00220 0.00126 AFIX 43 H3 2 0.823941 0.434874 0.875708 11.00000 -1.20000 AFIX 0 C4 1 0.852538 0.506853 0.789301 11.00000 0.02069 0.02072 = 0.02756 -0.00789 0.00188 -0.00260 AFIX 43 H4 2 0.873260 0.530494 0.847306 11.00000 -1.20000 AFIX 0 C5 1 0.850393 0.528961 0.686079 11.00000 0.02286 0.01454 = 0.03408 -0.00260 0.00612 -0.00292 AFIX 43 H5 2 0.868790 0.567218 0.676463 11.00000 -1.20000 AFIX 0 C6 1 0.821309 0.495010 0.597108 11.00000 0.02334 0.01592 = 0.02392 0.00332 0.00369 -0.00110 AFIX 43 H6 2 0.818521 0.509727 0.528174 11.00000 -1.20000 AFIX 0 C7 1 0.796740 0.438396 0.615825 11.00000 0.01692 0.01439 = 0.01811 -0.00126 0.00215 -0.00011 C8 1 0.773447 0.250000 0.324665 10.50000 0.01469 0.01232 = 0.01724 0.00000 0.00026 0.00000 C9 1 0.785243 0.302575 0.161859 11.00000 0.04035 0.03550 = 0.02276 0.01366 0.00384 0.00395 AFIX 137 H9A 2 0.659544 0.305021 0.135005 11.00000 -1.50000 H9B 2 0.871771 0.303363 0.103050 11.00000 -1.50000 H9C 2 0.809446 0.333720 0.208513 11.00000 -1.50000 AFIX 0 HKLF 4 REM yn44_a.res in Pnma REM wR2 = 0.0951, GooF = S = 1.050, Restrained GooF = 1.050 for all data REM R1 = 0.0338 for 1919 Fo > 4sig(Fo) and 0.0357 for all 2068 data REM 163 parameters refined using 0 restraints END WGHT 0.0532 1.6018 REM Instructions for potential hydrogen bonds EQIV $2 x-1/2, y, -z+3/2 HTAB O1 O3_$2 EQIV $3 x+1/2, y, -z+3/2 HTAB O2 O3_$3 EQIV $4 x-1/2, y, -z+1/2 HTAB C9 O5_$4 REM Highest difference peak 0.561, deepest hole -0.462, 1-sigma level 0.082 Q1 1 0.6042 0.2500 0.5908 10.50000 0.05 0.56 Q2 1 0.9081 0.2500 0.5908 10.50000 0.05 0.55 Q3 1 0.6391 0.3833 0.5193 11.00000 0.05 0.54 Q4 1 0.7754 0.4144 0.5632 11.00000 0.05 0.37 Q5 1 0.6506 0.5287 0.6852 11.00000 0.05 0.34 Q6 1 0.7606 0.3499 0.5780 11.00000 0.05 0.34 Q7 1 0.6567 0.5070 0.7879 11.00000 0.05 0.32 Q8 1 0.6552 0.2500 0.2219 10.50000 0.05 0.31 Q9 1 0.6534 0.4509 0.8052 11.00000 0.05 0.29 Q10 1 0.6666 0.4403 0.6175 11.00000 0.05 0.28 Q11 1 0.6345 0.3311 0.6166 11.00000 0.05 0.26 Q12 1 0.9141 0.3897 0.4849 11.00000 0.05 0.26 Q13 1 0.6497 0.4932 0.5959 11.00000 0.05 0.26 Q14 1 0.6550 0.3094 0.1622 11.00000 0.05 0.25 Q15 1 0.7873 0.3825 0.7217 11.00000 0.05 0.24 Q16 1 0.7094 0.4180 0.7130 11.00000 0.05 0.23 Q17 1 0.6425 0.3784 0.4444 11.00000 0.05 0.22 Q18 1 0.6492 0.2500 0.4209 10.50000 0.05 0.22 Q19 1 1.0054 0.3015 0.5158 11.00000 0.05 0.20 Q20 1 0.8046 0.4294 0.6660 11.00000 0.05 0.20 ; _shelx_res_checksum 90594 _shelx_hkl_file ; 0 -1 0 19.1123 3.62534 10 0 -1 0 25.2211 4.05444 3 0 -2 0 65704.9 1767.25 10 0 -2 0 60563.7 1766.83 3 0 -3 0 87.1659 13.3007 3 0 -4 0 18272.9 541.474 3 0 -5 0 2.18428 10.4492 3 0 -6 0 68300.4 1946.30 3 0 -7 0 3.08744 10.6898 3 0 -8 0 406359. 11337.6 3 0 -9 0 4.11925 11.3776 3 0 -10 0 64842.0 1887.41 3 0 -11 0 10.4653 12.2177 3 0 -12 0 82333.7 2399.28 6 0 -13 0-6.44508 15.0454 6 0 -14 0 225600. 6399.73 6 0 -15 0-7.80164 18.2122 6 0 -16 0 266204. 7552.45 6 0 -17 0 9.39591 19.6185 6 0 -18 0 81.3306 36.8324 6 0 -19 0-11.0018 19.8946 6 0 -20 0 14334.7 595.131 12 0 -21 0-12.3716 34.1710 12 0 -22 0 105303. 3215.61 16 0 -22 0 110815. 3245.91 12 0 -23 0 45.2986 31.2942 16 0 -23 0 24.9462 36.8423 12 0 -24 0 76739.6 2375.57 16 0 -24 0 79853.5 2409.27 12 0 -25 0 11.3768 33.5914 12 0 -25 0-10.0107 25.5977 16 0 -26 0 1252.99 131.388 12 0 -26 0 1217.75 120.572 16 0 -27 0-17.9066 28.0410 12 0 -27 0-7.74864 19.8161 16 0 -28 0 14699.6 523.444 16 0 -28 0 14902.3 542.546 12 0 -29 0 5.82775 31.6117 12 0 0 -1 4.25677 3.55590 17 0 0 -1 1.98251 3.23675 21 0 -1 -1 109341. 3099.18 21 0 -1 -1 108747. 3100.03 5 0 -1 -1 115920. 3101.87 17 0 1 -1 110430. 3100.86 7 0 1 1 111915. 3100.47 18 0 -2 1-2.43022 5.22999 19 0 -2 1-1.03861 4.47030 2 0 -2 -1 5.68687 5.17536 17 0 -3 1 21409.4 622.779 2 0 -3 1 21553.5 625.403 19 0 -4 1 5.06788 7.05658 3 0 -4 1 6.93143 7.46102 19 0 -4 -1 10.0688 8.21909 10 0 -5 -1 960.838 53.5648 10 0 -5 1 878.212 52.0773 3 0 -5 1 817.157 50.2483 19 0 -6 -1 2.56416 11.0377 10 0 -6 1 2.29614 10.1707 19 0 -6 1 15.9058 12.3771 3 0 -7 -1 46.7848 15.0017 10 0 -7 1 70.6270 17.1241 19 0 -7 1 54.0026 17.3013 3 0 -8 -1 10.8792 11.9863 10 0 -8 1 44.5205 17.3307 3 0 -9 1 94.2749 24.6406 3 0 -10 1-4.82897 13.3378 3 0 -11 -1 163258. 4375.73 6 0 -11 1 160500. 4375.66 6 0 -12 1 11.7640 16.2456 6 0 -12 1-5.88193 13.7299 3 0 -12 -1-5.83242 12.1770 6 0 -13 -1 5602.58 255.586 6 0 -13 1 5527.24 256.360 6 0 -13 1 5653.95 257.916 3 0 -14 -1-7.09568 18.1438 6 0 -14 1 7.20613 13.0293 3 0 -14 1 14.3485 21.1827 6 0 -15 1 10310.6 413.599 3 0 -15 -1 9843.73 409.119 6 0 -15 1 10540.6 417.872 6 0 -16 1-17.2669 22.0785 6 0 -16 -1-8.51857 19.8872 6 0 -17 1 560.021 83.3485 6 0 -17 1 514.037 82.6791 12 0 -17 -1 739.082 93.5917 6 0 -18 1 10.2654 21.4324 6 0 -18 -1 10.1080 23.5947 6 0 -18 1-11.0443 36.4585 12 0 -19 1 23.4513 27.3706 12 0 -19 1-11.1007 23.1762 6 0 -19 -1 21.8423 25.4927 6 0 -20 1 12.2810 28.6688 12 0 -21 1 445.020 85.8801 12 0 -22 1 11.5921 32.0169 16 0 -22 1 12.8053 40.1031 12 0 -22 -1 24.7960 40.9276 12 0 -22 -1-11.4191 31.5391 16 0 -23 -1 122.710 51.1487 16 0 -23 -1 355.194 78.0270 12 0 -23 1 268.365 73.3383 12 0 -23 1 283.111 70.2199 16 0 -24 1-10.7893 27.5886 16 0 -24 -1 11.7967 30.1645 12 0 -24 1 24.5981 31.4491 12 0 -24 -1-10.6322 33.2969 16 0 -25 1 10130.2 435.932 16 0 -25 -1 9659.63 443.687 12 0 -25 1 10230.8 458.191 12 0 -25 -1 9725.82 430.388 16 0 -26 1 8.86608 22.6735 16 0 -26 -1 8.75607 24.1860 16 0 -26 1-31.0584 43.2307 12 0 -27 1 1367.43 125.007 12 0 -27 -1 1361.86 116.738 16 0 -27 -1 1376.73 123.148 12 0 -27 1 1200.18 111.158 16 0 -28 1-14.9452 25.8722 12 0 -28 -1-6.22220 15.9110 16 0 -28 -1-7.27179 22.7736 12 0 -28 1 6.26552 16.0218 16 0 -29 -1 4875.38 224.595 12 0 -29 1 4907.61 226.242 12 0 0 -2 7421.53 243.076 17 0 0 -2 7713.57 236.013 21 0 -1 -2 1.74796 2.47622 6 0 -1 -2 5.34295 7.20091 17 0 -1 -2 12.6745 8.10259 5 0 -1 -2-2.92613 5.71508 21 0 -1 2 2.90909 2.24693 6 0 1 -2 5.47118 5.71184 20 0 2 2 18061.0 523.828 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180.723 66.5991 11 2 -4 11 82.0816 45.3019 11 -2 4 11 159.865 55.7429 11 -2 -4 11 119.628 52.0410 11 -2 -5 11 18285.3 769.057 27 2 -5 11 19316.8 761.922 11 2 5 11 19387.4 766.295 11 -2 -5 11 21119.1 773.365 11 -2 5 11 18958.3 753.994 11 2 -6 11-25.5733 29.8523 11 -2 -6 11 14.2031 33.1579 27 -2 -7 11 27.9738 32.6580 27 -2 8 -11 451.316 88.4253 29 -2 -8 11 622.738 105.798 27 -2 9 -11 508.299 93.4667 29 -2 -9 11 505.357 91.9500 27 2 9 11 588.112 87.2687 25 2 10 11 1157.70 122.131 25 -2 -10 11 1404.65 149.982 27 -2 10 -11 1155.72 142.349 29 -2 -11 11 8102.01 399.419 27 2 11 11 8342.44 377.563 25 -2 11 -11 8516.16 420.062 29 -2 -12 11 203.129 54.8624 27 -2 12 -11 124.573 48.8683 29 2 12 11 171.435 49.1526 25 2 13 11 669.017 84.8979 25 -2 13 -11 834.101 111.006 29 2 14 11-7.89322 21.8018 25 -2 14 -11-11.2044 33.0831 29 2 15 11 10383.1 415.144 25 -2 15 -11 11147.6 466.402 29 -2 16 -11 1125.09 119.010 29 -2 17 11 1366.15 124.714 28 -2 17 -11 2003.63 145.349 29 -2 18 11 1331.17 113.971 28 -2 18 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707.433 74.5816 28 -7 0 -9 2560.43 155.711 26 -7 0 9 2919.63 159.106 15 -7 -1 -9 2181.63 143.480 26 -7 -1 9 2461.53 142.663 15 -7 1 9 2338.84 140.920 15 -7 -2 -9 1040.29 92.0704 26 -7 -2 9 927.596 82.6341 15 -7 2 9 906.531 82.3517 15 -8 0 0 16777.1 623.121 14 -8 -1 0 8873.96 396.385 14 -8 1 0 9745.66 408.308 14 -8 2 0 19951.8 712.721 14 -8 3 0 2020.46 157.717 14 -8 4 0 357.517 68.8362 14 -8 5 0 136.126 44.5671 14 -8 6 0 461.152 70.9982 14 -8 7 0 436.633 67.8850 26 -8 7 0 584.010 78.9415 14 -8 8 0 13676.8 514.282 26 -8 8 0 13663.8 510.771 14 -8 9 0 1042.82 101.337 26 -8 9 0 1118.86 101.896 14 -8 10 0 4561.85 230.522 26 -8 10 0 4840.00 230.146 14 -8 11 0 291.636 49.3511 26 -8 11 0 313.323 49.9162 14 -8 0 1 88.4249 39.2230 14 -8 0 -1 69.9878 36.5951 14 -8 -1 1 6899.29 320.692 14 -8 -1 -1 5967.78 303.488 14 -8 1 1 6913.38 321.757 14 -8 1 -1 6535.11 315.556 14 -8 2 1 361.352 67.3274 14 -8 2 -1 481.254 76.7350 14 -8 3 1 5668.68 284.927 14 -8 3 -1 5396.09 279.206 14 -8 4 1 5653.99 286.394 14 -8 4 -1 6106.52 292.404 14 -8 5 -1 1868.15 148.977 26 -8 5 1 1976.92 151.553 14 -8 5 -1 1958.92 149.451 14 -8 6 -1 496.686 75.8399 26 -8 6 1 563.832 77.2289 14 -8 6 -1 613.305 79.6277 14 -8 7 -1 1003.71 103.890 26 -8 7 1 939.792 98.5808 14 -8 7 -1 982.713 99.3203 14 -8 8 -1 378.431 63.7605 26 -8 8 1 385.664 60.2405 14 -8 8 -1 366.464 60.1786 14 -8 9 -1 2466.71 161.064 26 -8 9 1 2330.14 151.680 26 -8 9 1 2373.81 151.443 14 -8 9 -1 2096.24 145.316 14 -8 10 -1 247.156 48.2018 26 -8 10 1 240.184 46.4052 26 -8 10 1 242.334 44.4582 14 -8 10 -1 201.183 42.5098 14 -8 11 -1 1912.04 130.444 26 -8 11 1 1766.63 122.363 26 -8 11 1 1881.91 122.825 14 -8 11 -1 2028.64 127.502 14 -8 0 2 3628.48 212.541 14 -8 0 -2 3179.63 200.811 14 -8 -1 -2 40.7510 34.0653 14 -8 1 2 41.9054 33.9182 14 -8 1 -2 82.6467 35.6039 14 -8 2 2 899.078 100.549 14 -8 2 -2 758.211 91.4584 14 -8 3 -2 303.047 62.0659 26 -8 3 2 377.931 66.5886 14 -8 3 -2 375.493 65.6173 14 -8 4 -2 17.4467 25.7688 26 -8 4 2 24.1411 26.5759 14 -8 4 -2 56.2108 34.5717 14 -8 5 -2 260.967 58.0605 26 -8 5 2 296.867 58.8600 14 -8 5 -2 375.957 63.9038 14 -8 6 -2 10505.6 446.984 26 -8 6 2 11910.4 447.576 14 -8 6 -2 11484.3 444.380 14 -8 7 -2 1585.46 131.964 26 -8 7 2 1369.43 115.908 14 -8 7 -2 1372.65 116.499 14 -8 8 -2 2385.97 161.802 26 -8 8 2 2206.86 147.823 14 -8 8 -2 2322.59 150.724 14 -8 9 -2 74.3242 32.0248 26 -8 9 2 61.7211 27.3764 14 -8 9 -2 37.9353 22.9122 14 -8 10 -2 354.459 56.1222 26 -8 10 -2 396.860 55.7111 14 -8 10 2 390.585 53.7932 14 -8 11 -2 777.897 78.8712 26 -8 0 3 735.589 92.3143 15 -8 1 -3 6356.84 298.310 26 -8 -1 3 6367.72 304.468 15 -8 1 3 5744.63 295.433 15 -8 2 -3 244.429 54.5813 26 -8 -2 3 261.577 54.6415 15 -8 2 3 170.901 47.5951 15 -8 3 -3 595.796 82.6151 26 -8 4 -3 127.583 41.7958 26 -8 5 -3 2260.55 162.243 26 -8 6 -3 303.302 57.3817 26 -8 7 -3 7653.27 336.950 26 -8 8 -3 252.819 54.7865 26 -8 9 -3 3071.91 178.482 26 -8 10 -3 6.18095 17.0720 26 -8 0 -4 184.048 44.8824 26 -8 0 4 197.501 49.7609 15 -8 -1 -4 243.304 49.1008 26 -8 1 -4 196.591 49.6719 26 -8 -1 4 218.751 48.6761 15 -8 1 4 282.941 57.2057 15 -8 2 -4 6362.74 294.709 26 -8 -2 4 6057.52 288.514 15 -8 2 4 6124.80 290.498 15 -8 3 -4 1235.76 113.893 26 -8 -3 4 1199.13 107.914 15 -8 3 4 1178.12 108.177 15 -8 4 -4 4459.60 233.422 26 -8 -4 4 4247.81 216.772 15 -8 4 4 4009.62 215.579 15 -8 5 -4 1473.91 122.709 26 -8 6 -4 2772.92 173.304 26 -8 7 -4 917.806 93.5759 26 -8 8 -4 197.818 42.2280 26 -8 0 -5 3708.24 205.342 26 -8 0 5 4411.37 216.945 15 -8 -1 -5 2814.37 167.137 26 -8 1 -5 2842.47 171.358 26 -8 -1 5 2490.89 159.856 15 -8 1 5 2811.23 167.933 15 -8 -2 -5 32.2887 21.3639 26 -8 2 -5 108.318 35.3854 26 -8 -2 5 39.3769 25.6723 15 -8 2 5 59.7594 27.7613 15 -8 3 -5 380.859 60.6888 26 -8 -3 5 330.805 52.9028 15 -8 3 5 285.700 49.5344 15 -8 4 -5 1055.49 98.3205 26 -8 -4 5 1017.60 88.7006 15 -8 4 5 932.745 87.0181 15 -8 5 -5 81.4200 32.5362 26 -8 6 -5 365.882 56.1797 26 -8 0 -6 992.949 89.5863 26 -8 0 6 1012.93 88.6683 15 -8 1 -6 388.424 55.2192 26 -8 -1 6 362.937 52.1064 15 -8 1 6 243.262 45.2115 15 -8 2 -6 6930.64 290.454 26 0 0 0 0.00 0.00 0 TITL YN44 in Pnma REM Pnma (#62, found as Pnam in a-cb setting) CELL 1.54184 7.141003 23.859935 12.489225 90.0000 90.0000 90.0000 ZERR 5.00 0.000100 0.000387 0.000190 0.0000 0.0000 0.0000 LATT 1 SYMM -x+1/2,-y, z+1/2 SYMM -x, y+1/2,-z SYMM x+1/2,-y+1/2,-z+1/2 SFAC C N O Cu UNIT 80.00 20.00 10.00 5.00 TREF HKLF 4 END ; _shelx_hkl_checksum 48439 _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 1.206 _oxdiff_exptl_absorpt_empirical_full_min 0.797 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' 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 0.75117(4) 0.250000 0.58837(3) 0.01160(15) Uani 1 2 d S T P . . S1 S 0.76374(6) 0.38305(2) 0.52395(4) 0.01609(16) Uani 1 1 d . . . . . O1 O 0.4771(3) 0.250000 0.60064(15) 0.0170(4) Uani 1 2 d S T P . . H1 H 0.427(4) 0.2788(10) 0.626(2) 0.037(7) Uiso 1 1 d . . . . . O2 O 1.0259(3) 0.250000 0.60376(16) 0.0192(4) Uani 1 2 d S T P . . H2 H 1.078(4) 0.2796(10) 0.632(2) 0.040(7) Uiso 1 1 d . . . . . O3 O 0.75632(16) 0.32549(6) 0.79886(11) 0.0180(3) Uani 1 1 d . . . . . O4 O 0.5870(2) 0.38792(6) 0.47023(11) 0.0268(3) Uani 1 1 d . . . . . O5 O 0.9265(2) 0.37612(6) 0.45825(11) 0.0278(4) Uani 1 1 d . . . . . N1 N 0.75272(19) 0.33339(7) 0.61611(14) 0.0150(4) Uani 1 1 d . . . . . N2 N 0.7502(3) 0.250000 0.41606(19) 0.0187(6) Uani 1 2 d S T P . . N3 N 0.8081(4) 0.250000 0.22152(18) 0.0215(5) Uani 1 2 d S T P . . C1 C 0.7666(2) 0.35412(8) 0.71586(16) 0.0144(4) Uani 1 1 d . . . . . C2 C 0.7959(3) 0.41606(8) 0.71808(15) 0.0155(4) Uani 1 1 d . . . . . C3 C 0.8240(3) 0.44976(8) 0.80689(15) 0.0194(4) Uani 1 1 d . . . . . H3 H 0.823941 0.434874 0.875708 0.023 Uiso 1 1 calc R . . . . C4 C 0.8525(3) 0.50685(8) 0.78930(16) 0.0230(4) Uani 1 1 d . . . . . H4 H 0.873260 0.530494 0.847306 0.028 Uiso 1 1 calc R . . . . C5 C 0.8504(3) 0.52896(8) 0.68608(17) 0.0238(4) Uani 1 1 d . . . . . H5 H 0.868790 0.567218 0.676463 0.029 Uiso 1 1 calc R . . . . C6 C 0.8213(3) 0.49501(8) 0.59711(16) 0.0211(4) Uani 1 1 d . . . . . H6 H 0.818521 0.509727 0.528174 0.025 Uiso 1 1 calc R . . . . C7 C 0.7967(3) 0.43840(8) 0.61582(15) 0.0165(4) Uani 1 1 d . . . . . C8 C 0.7734(3) 0.250000 0.3247(2) 0.0147(5) Uani 1 2 d S T P . . C9 C 0.7852(3) 0.30258(10) 0.16186(19) 0.0329(5) Uani 1 1 d . . . . . H9A H 0.659544 0.305021 0.135005 0.049 Uiso 1 1 calc GR . . . . H9B H 0.871771 0.303363 0.103050 0.049 Uiso 1 1 calc GR . . . . H9C H 0.809446 0.333720 0.208513 0.049 Uiso 1 1 calc GR . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0147(2) 0.0090(2) 0.0111(2) 0.000 -0.00006(12) 0.000 S1 0.0248(3) 0.0108(3) 0.0126(3) 0.00158(17) 0.00088(15) -0.00146(16) O1 0.0172(9) 0.0131(9) 0.0209(9) 0.000 0.0012(7) 0.000 O2 0.0176(10) 0.0137(9) 0.0264(10) 0.000 -0.0033(8) 0.000 O3 0.0229(7) 0.0157(7) 0.0155(7) 0.0054(6) 0.0001(5) 0.0003(5) O4 0.0360(9) 0.0209(7) 0.0234(7) 0.0050(6) -0.0098(6) -0.0018(6) O5 0.0382(9) 0.0222(7) 0.0229(7) 0.0008(6) 0.0141(6) -0.0034(6) N1 0.0197(8) 0.0113(8) 0.0142(8) 0.0014(7) 0.0012(5) -0.0004(5) N2 0.0235(14) 0.0197(13) 0.0130(13) 0.000 0.0005(8) 0.000 N3 0.0296(12) 0.0218(12) 0.0129(11) 0.000 0.0026(10) 0.000 C1 0.0142(8) 0.0126(9) 0.0164(9) 0.0011(8) 0.0004(6) 0.0008(6) C2 0.0133(8) 0.0139(9) 0.0194(9) 0.0006(7) 0.0011(7) 0.0003(7) C3 0.0188(9) 0.0199(9) 0.0194(9) -0.0025(7) 0.0022(7) 0.0013(8) C4 0.0207(9) 0.0207(10) 0.0276(10) -0.0079(8) 0.0019(8) -0.0026(8) C5 0.0229(10) 0.0145(9) 0.0341(11) -0.0026(8) 0.0061(8) -0.0029(8) C6 0.0233(10) 0.0159(9) 0.0239(10) 0.0033(7) 0.0037(8) -0.0011(8) C7 0.0169(8) 0.0144(9) 0.0181(9) -0.0013(7) 0.0022(7) -0.0001(7) C8 0.0147(12) 0.0123(12) 0.0172(13) 0.000 0.0003(9) 0.000 C9 0.0404(12) 0.0355(13) 0.0228(11) 0.0137(10) 0.0038(9) 0.0039(10) 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' 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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O1 Cu1 O2 169.92(9) . . ? O1 Cu1 N1 89.54(4) . . ? O1 Cu1 N1 89.54(4) . 7_565 ? O1 Cu1 N2 94.30(8) . . ? O2 Cu1 N1 88.73(4) . 7_565 ? O2 Cu1 N1 88.73(4) . . ? O2 Cu1 N2 95.78(8) . . ? N1 Cu1 N1 160.23(10) 7_565 . ? N1 Cu1 N2 99.88(5) . . ? N1 Cu1 N2 99.88(5) 7_565 . ? O4 S1 N1 109.99(8) . . ? O4 S1 C7 111.16(9) . . ? O5 S1 O4 117.10(10) . . ? O5 S1 N1 110.76(8) . . ? O5 S1 C7 110.51(9) . . ? N1 S1 C7 95.16(9) . . ? Cu1 O1 H1 117.0(19) . 7_565 ? Cu1 O1 H1 117.0(19) . . ? H1 O1 H1 110(4) . 7_565 ? Cu1 O2 H2 117.8(18) . 7_565 ? Cu1 O2 H2 117.8(18) . . ? H2 O2 H2 108(3) . 7_565 ? S1 N1 Cu1 125.92(10) . . ? C1 N1 Cu1 121.46(13) . . ? C1 N1 S1 112.21(13) . . ? C8 N2 Cu1 171.5(2) . . ? C8 N3 C9 118.51(13) . . ? C8 N3 C9 118.51(13) . 7_565 ? C9 N3 C9 117.4(3) 7_565 . ? O3 C1 N1 124.49(18) . . ? O3 C1 C2 122.45(18) . . ? N1 C1 C2 113.07(16) . . ? C3 C2 C1 127.60(17) . . ? C7 C2 C1 111.39(16) . . ? C7 C2 C3 121.00(18) . . ? C2 C3 H3 121.2 . . ? C2 C3 C4 117.53(18) . . ? C4 C3 H3 121.2 . . ? C3 C4 H4 119.5 . . ? C5 C4 C3 120.93(18) . . ? C5 C4 H4 119.5 . . ? C4 C5 H5 119.3 . . ? C6 C5 C4 121.37(18) . . ? C6 C5 H5 119.3 . . ? C5 C6 H6 121.5 . . ? C7 C6 C5 116.94(18) . . ? C7 C6 H6 121.5 . . ? C2 C7 S1 108.13(14) . . ? C6 C7 S1 129.66(15) . . ? C6 C7 C2 122.21(18) . . ? N2 C8 N3 177.4(3) . . ? N3 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? N3 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? 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 O1 1.963(2) . ? Cu1 O2 1.971(2) . ? Cu1 N1 2.0197(17) 7_565 ? Cu1 N1 2.0197(17) . ? Cu1 N2 2.152(2) . ? S1 O4 1.4339(15) . ? S1 O5 1.4325(15) . ? S1 N1 1.6538(17) . ? S1 C7 1.7652(19) . ? O1 H1 0.84(2) . ? O1 H1 0.84(2) 7_565 ? O2 H2 0.87(3) . ? O2 H2 0.87(3) 7_565 ? O3 C1 1.244(2) . ? N1 C1 1.344(3) . ? N2 C8 1.153(4) . ? N3 C8 1.312(4) . ? N3 C9 1.468(2) 7_565 ? N3 C9 1.468(2) . ? C1 C2 1.493(3) . ? C2 C3 1.384(3) . ? C2 C7 1.384(3) . ? C3 H3 0.9300 . ? C3 C4 1.395(3) . ? C4 H4 0.9300 . ? C4 C5 1.393(3) . ? C5 H5 0.9300 . ? C5 C6 1.391(3) . ? C6 H6 0.9300 . ? C6 C7 1.382(3) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? 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 N1 C1 O3 -9.3(2) . . . . ? Cu1 N1 C1 C2 170.81(11) . . . . ? S1 N1 C1 O3 177.65(13) . . . . ? S1 N1 C1 C2 -2.28(18) . . . . ? O3 C1 C2 C3 3.2(3) . . . . ? O3 C1 C2 C7 -178.20(16) . . . . ? O4 S1 N1 Cu1 74.31(11) . . . . ? O4 S1 N1 C1 -112.97(13) . . . . ? O4 S1 C7 C2 113.04(14) . . . . ? O4 S1 C7 C6 -67.3(2) . . . . ? O5 S1 N1 Cu1 -56.71(12) . . . . ? O5 S1 N1 C1 116.01(13) . . . . ? O5 S1 C7 C2 -115.17(14) . . . . ? O5 S1 C7 C6 64.5(2) . . . . ? N1 S1 C7 C2 -0.72(14) . . . . ? N1 S1 C7 C6 178.93(19) . . . . ? N1 C1 C2 C3 -176.83(17) . . . . ? N1 C1 C2 C7 1.7(2) . . . . ? C1 C2 C3 C4 178.63(17) . . . . ? C1 C2 C7 S1 -0.41(19) . . . . ? C1 C2 C7 C6 179.91(18) . . . . ? C2 C3 C4 C5 0.7(3) . . . . ? C3 C2 C7 S1 178.26(15) . . . . ? C3 C2 C7 C6 -1.4(3) . . . . ? C3 C4 C5 C6 -0.5(3) . . . . ? C4 C5 C6 C7 -0.7(3) . . . . ? C5 C6 C7 S1 -177.98(15) . . . . ? C5 C6 C7 C2 1.6(3) . . . . ? C7 S1 N1 Cu1 -170.94(10) . . . . ? C7 S1 N1 C1 1.77(13) . . . . ? C7 C2 C3 C4 0.2(3) . . . . ?