#------------------------------------------------------------------------------ #$Date: 2025-01-23 01:09:21 +0200 (Thu, 23 Jan 2025) $ #$Revision: 297424 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/37/1573739.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_1573739 loop_ _publ_author_name 'Das, Saikat' 'Sakai, Jin' 'Nakatani, Riki' 'Kondo, Ayumu' 'Tomioka, Rina' 'Das, Subhabrata' 'Takahashi, Shuntaro' 'Kawawaki, Tokuhisa' 'Biswas, Sourav' 'Negishi, Yuichi' _publ_section_title ; Tunable structural rearrangement in Cu cluster assemblies through linker and solvent alterations ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC07730J _journal_year 2025 _chemical_formula_moiety 'C40 H43 Cu6 F3 N4 O2 S8, 2.5[CH2Cl2]' _chemical_formula_sum 'C42.5 H48 Cl5 Cu6 F3 N4 O2 S8' _chemical_formula_weight 1518.82 _space_group_crystal_system orthorhombic _space_group_IT_number 74 _space_group_name_Hall '-I 2b 2' _space_group_name_H-M_alt 'I m m a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2024-09-27 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _audit_update_record ; 2024-11-05 deposited with the CCDC. 2025-01-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 24.6205(9) _cell_length_b 17.0084(7) _cell_length_c 22.4482(9) _cell_measurement_reflns_used 9851 _cell_measurement_temperature 273.15 _cell_measurement_theta_max 24.908 _cell_measurement_theta_min 2.325 _cell_volume 9400.3(6) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 273.15 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0681 _diffrn_reflns_av_unetI/netI 0.0331 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 48189 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.672 _diffrn_reflns_theta_min 2.326 _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_voltage 50.0 _exptl_absorpt_coefficient_mu 1.683 _exptl_absorpt_correction_T_max 0.7462 _exptl_absorpt_correction_T_min 0.6921 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0948 before and 0.0618 after correction. The Ratio of minimum to maximum transmission is 0.9275. The \l/2 correction factor is Not present. ; _exptl_crystal_colour Orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.073 _exptl_crystal_description block _exptl_crystal_F_000 3044 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _refine_diff_density_max 2.045 _refine_diff_density_min -0.858 _refine_diff_density_rms 0.128 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 282 _refine_ls_number_reflns 4702 _refine_ls_number_restraints 389 _refine_ls_restrained_S_all 1.091 _refine_ls_R_factor_all 0.0961 _refine_ls_R_factor_gt 0.0796 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+150.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1768 _refine_ls_wR_factor_ref 0.1862 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3525 _reflns_number_total 4702 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc07730j2.cif _cod_data_source_block Cu6-dpp _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_crystal_colour_primary' value 'Orange' was changed to 'orange' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas ; _cod_original_formula_sum 'C42.50 H48 Cl5 Cu6 F3 N4 O2 S8' _cod_database_code 1573739 _shelx_shelxl_version_number 2018/3 _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 0.786 _shelx_estimated_absorpt_t_min 0.786 _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. Restrained distances O3-C16 1.23 with sigma of 0.001 O3-O3_$1 2 with sigma of 0.001 O3-Cu3 2.05 with sigma of 0.001 C59-C16 1.53 with sigma of 0.001 F2-C32 = F2-C32 1.4 with sigma of 0.001 F3-C32 = F2-C32 = F1-C32 1.4 with sigma of 0.01 F2-C32 = F3-C32 = F1-C32 1.4 with sigma of 0.0001 F2-F3 = F3-F1 2.3 with sigma of 0.02 F1-F2 2.3 with sigma of 0.02 O1-C15 1.23 with sigma of 0.0001 O2-C15 1.23 with sigma of 0.0001 C32-C15 1.53 with sigma of 0.0001 Cu2-O1 2.05 with sigma of 0.0001 O2-O1 2 with sigma of 0.02 F6-C59 1.4 with sigma of 0.01 O2-C32 2.5 with sigma of 0.02 F4-C59 = F5-C59 1.4 with sigma of 0.001 C59-F6 1.4 with sigma of 0.001 O4-O3 2 with sigma of 0.02 O4-C59 2.4 with sigma of 0.02 C59-O3 2.4 with sigma of 0.02 O4-C16 1.23 with sigma of 0.001 F5-F6 = F5-F4 2.3 with sigma of 0.02 F6-F4 2.3 with sigma of 0.02 C4-C1 = C3-C1 = C2-C1 1.53 with sigma of 0.01 C2-C4 = C4-C3 2.5 with sigma of 0.02 C2-C3 2.5 with sigma of 0.02 3. Rigid bond restraints All non-hydrogen atoms with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances 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 within 2A Uanis(F5) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 5. Others Fixed Sof: H5C(0.5) H5B(0.5) H5A(0.5) F1(0.125) F2(0.125) F3(0.125) F4(0.125) F5(0.125) F6(0.125) O1(0.125) O2(0.125) O3(0.125) O4(0.125) C1(0.25) C2(0.25) H2A(0.25) H2B(0.25) H2C(0.25) C3(0.25) H3A(0.25) H3B(0.25) H3C(0.25) C4(0.25) H4A(0.25) H4B(0.25) H4C(0.25) C15(0.125) C16(0.125) C32(0.125) C59(0.125) 6.a Me refined with riding coordinates: C5(H5C,H5B,H5A) 6.b Aromatic/amide H refined with riding coordinates: C8(H8), C9(H9), C10(H10), C12(H12) 6.c Fitted hexagon refined as free rotating group: N1(C8,C9,C10,C11,C12) 6.d Idealised Me refined as rotating group: C7(H7A,H7B,H7C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C) ; _smtbx_masks_special_details ; A solvent mask was calculated and 456 electrons were found in a volume of 4224\%A^3^ in 1 void per unit cell. This is consistent with the presence of 2.75[CH2Cl2] per formula unit which account for 462 electrons per unit cell. ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL 240509_rt_cutppa_90k_0ma_a_a.res in Imma 240509_rt_cutppa_90k_0ma_a.res created by SHELXL-2018/3 at 22:11:55 on 27-Sep-2024 REM Old TITL 240509_rt_cutppa_90k_0ma_a_a.res in Imma REM SHELXT solution in Imma: R1 0.238, Rweak 0.016, Alpha 0.040 REM 0.185 for 127 systematic absences, Orientation as input REM Formula found by SHELXT: C39 Cu6 N24 S4 Cl4 CELL 0.71073 24.6205 17.0084 22.4482 90 90 90 ZERR 4 0.0009 0.0007 0.0009 0 0 0 LATT 2 SYMM -X,0.5-Y,+Z SYMM -X,0.5+Y,-Z SYMM +X,-Y,-Z SFAC C H Cl Cu F N O S UNIT 170 192 20 24 12 16 8 32 EQIV $1 1-X,1.5-Y,+Z DFIX 1.23 0.001 O3 C16 DELU SIMU 0.01 0.02 2 DFIX 2 0.001 O3 O3_$1 DFIX 2.05 0.001 O3 Cu3 DFIX 1.53 0.001 C59 C16 DFIX 1.4 0.001 F2 C32 F2 C32 DFIX 1.4 0.01 F3 C32 F2 C32 F1 C32 DFIX 1.4 0.0001 F2 C32 F3 C32 F1 C32 DFIX 2.3 F2 F3 F3 F1 DFIX 2.3 F1 F2 DFIX 1.23 0.0001 O1 C15 DFIX 1.23 0.0001 O2 C15 DFIX 1.53 0.0001 C32 C15 DFIX 2.05 0.0001 Cu2 O1 DFIX 2 O2 O1 DFIX 1.4 0.01 F6 C59 DFIX 2.5 O2 C32 DFIX 1.4 0.001 F4 C59 F5 C59 DFIX 1.4 0.001 C59 F6 DFIX 2 O4 O3 DFIX 2.4 O4 C59 DFIX 2.4 C59 O3 DFIX 1.23 0.001 O4 C16 DFIX 2.3 F5 F6 F5 F4 DFIX 2.3 F6 F4 ISOR 0.005 0.01 F5 C59 F6 F4 O3 C16 O4 ISOR 0.005 0.01 F2 F3 C32 F1 O1 O2 C15 DFIX 1.53 0.01 C4 C1 C3 C1 C2 C1 DFIX 2.5 C2 C4 C4 C3 DFIX 2.5 C2 C3 L.S. 10 PLAN 90 SIZE 0.15 0.15 0.15 TEMP 0 CONF list 4 MORE -1 ABIN BOND $H fmap 2 ACTA SHEL 999 0.82 OMIT 0 0 4 OMIT 0 0 8 OMIT 0 1 3 OMIT 0 1 5 OMIT 0 1 7 OMIT 0 2 4 OMIT 0 2 8 OMIT 0 3 1 OMIT 0 3 3 OMIT 0 4 0 OMIT 0 4 2 OMIT 0 5 3 OMIT 0 7 7 OMIT 1 0 7 OMIT 1 3 2 OMIT 1 3 8 OMIT 1 6 1 OMIT 2 0 4 OMIT 2 2 4 OMIT 2 4 0 OMIT 2 5 3 OMIT 3 0 1 OMIT 3 4 3 OMIT 4 0 2 OMIT 5 0 1 OMIT 5 2 1 OMIT 8 0 0 REM REM REM WGHT 0.010000 150.000000 FVAR 0.16189 CU1 4 0.421266 0.659795 0.282463 11.00000 0.05329 0.04340 = 0.06315 0.00012 -0.00441 -0.01224 CU2 4 0.500000 0.750000 0.371863 10.25000 0.07696 0.06490 = 0.07257 0.00000 0.00000 0.00000 CU3 4 0.500000 0.750000 0.159440 10.25000 0.03767 0.07357 = 0.05740 0.00000 0.00000 0.00000 S1 8 0.423416 0.750000 0.211344 10.50000 0.03291 0.04734 = 0.05791 0.00000 -0.00161 0.00000 S2 8 0.500000 0.634856 0.327866 10.50000 0.05231 0.04820 = 0.06632 0.01824 0.00000 0.00000 S3 8 0.283612 0.345158 0.304488 11.00000 0.09286 0.03016 = 0.11981 0.00239 -0.06440 -0.00096 AFIX 66 N1 6 0.353531 0.607770 0.310960 11.00000 0.05079 0.03935 = 0.07074 0.00418 -0.01208 -0.01276 C8 1 0.327519 0.639234 0.360476 11.00000 0.05105 0.03761 = 0.06420 -0.00175 -0.01252 -0.00287 AFIX 43 H8 2 0.341629 0.683588 0.379116 11.00000 -1.20000 AFIX 65 C9 1 0.280417 0.604405 0.382132 11.00000 0.04853 0.04544 = 0.07663 -0.01007 -0.00574 0.00347 AFIX 43 H9 2 0.263013 0.625457 0.415261 11.00000 -1.20000 AFIX 65 C10 1 0.259327 0.538112 0.354272 11.00000 0.04399 0.04309 = 0.08014 -0.00071 -0.00518 -0.00505 AFIX 43 H10 2 0.227812 0.514810 0.368761 11.00000 -1.20000 AFIX 65 C11 1 0.285339 0.506648 0.304755 11.00000 0.03983 0.02954 = 0.07451 0.00139 -0.01608 -0.00014 C12 1 0.332441 0.541475 0.283099 11.00000 0.05096 0.03814 = 0.06762 -0.00381 -0.01016 -0.00908 AFIX 43 H12 2 0.349844 0.520423 0.249969 11.00000 -1.20000 AFIX 0 C5 1 0.310384 0.750000 0.200540 10.50000 0.03727 0.07300 = 0.06620 0.00000 -0.00416 0.00000 PART -1 AFIX 33 H5C 2 0.308932 0.702605 0.223709 10.50000 -1.50000 H5B 2 0.310763 0.794653 0.226694 10.50000 -1.50000 H5A 2 0.279107 0.752742 0.175089 10.50000 -1.50000 AFIX 0 PART 0 C6 1 0.362461 0.750000 0.162112 10.50000 0.03758 0.07572 = 0.06531 0.00000 -0.00646 0.00000 C7 1 0.365565 0.674473 0.124604 11.00000 0.04878 0.11727 = 0.07040 -0.02552 -0.00839 -0.00366 AFIX 137 H7A 2 0.401293 0.669476 0.107901 11.00000 -1.50000 H7B 2 0.339289 0.676973 0.093063 11.00000 -1.50000 H7C 2 0.358049 0.629824 0.149432 11.00000 -1.50000 AFIX 0 C13 1 0.265210 0.435927 0.274051 11.00000 0.04543 0.02650 = 0.09097 -0.00056 -0.02393 -0.00062 C14 1 0.250000 0.289450 0.250000 10.50000 0.07993 0.03363 = 0.11254 0.00000 -0.05688 0.00000 PART -1 F1 5 0.619406 0.779689 0.571312 10.12500 0.05008 0.06488 = 0.02994 -0.01539 -0.02086 -0.00924 F2 5 0.531640 0.815776 0.571432 10.12500 0.04982 0.05026 = 0.04291 -0.01870 0.00503 -0.00459 F3 5 0.555722 0.682895 0.574239 10.12500 0.04271 0.04837 = 0.03055 0.00963 0.00735 -0.00320 F4 5 0.442157 0.823321 -0.028892 10.12500 0.05979 0.07050 = 0.05611 0.00374 -0.01064 0.00629 F5 5 0.534437 0.833482 -0.042539 10.12500 0.06240 0.06100 = 0.05205 0.01204 0.00507 0.00233 F6 5 0.489428 0.726560 -0.075212 10.12500 0.05746 0.07165 = 0.04813 -0.00903 -0.00870 0.00247 O1 7 0.521199 0.747321 0.460152 10.12500 0.03767 0.03491 = 0.03975 0.00624 0.00440 -0.00059 O2 7 0.607503 0.743961 0.453636 10.12500 0.02820 0.00815 = 0.02225 0.00886 -0.00010 0.00481 O3 7 0.505936 0.808157 0.079707 10.12500 0.05556 0.07437 = 0.05794 0.00267 0.00131 0.00613 O4 7 0.492708 0.699628 0.057702 10.12500 0.04340 0.07566 = 0.07179 0.03409 0.00234 0.01357 C1 1 0.497000 0.551667 0.381270 10.25000 0.03094 0.04279 = 0.04286 0.02113 -0.00061 -0.01123 C2 1 0.551306 0.542086 0.412912 10.25000 0.03034 0.02549 = 0.03810 0.01970 -0.00011 -0.00404 AFIX 137 H2A 2 0.548769 0.500180 0.441425 10.25000 -1.50000 H2B 2 0.560407 0.590118 0.433032 10.25000 -1.50000 H2C 2 0.578978 0.529920 0.384228 10.25000 -1.50000 AFIX 0 C3 1 0.453155 0.570444 0.427389 10.25000 0.02156 0.04735 = 0.05100 0.02977 -0.00400 -0.01245 AFIX 137 H3A 2 0.447814 0.525707 0.452797 10.25000 -1.50000 H3B 2 0.419757 0.582740 0.407381 10.25000 -1.50000 H3C 2 0.464372 0.614673 0.450938 10.25000 -1.50000 AFIX 0 C4 1 0.481975 0.477615 0.346573 10.25000 0.04122 0.03619 = 0.05238 0.03051 -0.01514 -0.01429 AFIX 137 H4A 2 0.507553 0.469843 0.314836 10.25000 -1.50000 H4B 2 0.446156 0.483367 0.330247 10.25000 -1.50000 H4C 2 0.482766 0.433060 0.372812 10.25000 -1.50000 AFIX 0 C15 1 0.566168 0.753278 0.483589 10.12500 0.03526 0.03057 = 0.03148 0.00157 0.00487 -0.00112 C16 1 0.502906 0.764458 0.036175 10.12500 0.04365 0.05238 = 0.05211 0.00291 0.00069 0.00273 C32 1 0.567636 0.757653 0.551647 10.12500 0.03920 0.04159 = 0.03531 0.00035 0.00277 -0.00296 C59 1 0.491489 0.782382 -0.029426 10.12500 0.05287 0.05587 = 0.05121 0.00046 -0.00080 0.00064 HKLF 4 REM 240509_rt_cutppa_90k_0ma_a_a.res in Imma REM wR2 = 0.1862, GooF = S = 1.089, Restrained GooF = 1.091 for all data REM R1 = 0.0796 for 3525 Fo > 4sig(Fo) and 0.0961 for all 4702 data REM 282 parameters refined using 389 restraints END WGHT 0.1536 50.3820 REM Highest difference peak 2.045, deepest hole -0.858, 1-sigma level 0.128 Q1 1 0.5000 0.7500 0.0769 10.25000 0.05 2.05 Q2 1 0.5000 0.7500 0.0239 10.25000 0.05 1.59 Q3 1 0.5000 0.7500 0.4633 10.25000 0.05 1.24 Q4 1 0.6416 0.8161 0.5452 11.00000 0.05 1.20 Q5 1 0.5956 0.8046 0.5774 11.00000 0.05 1.14 Q6 1 0.6513 0.7500 0.5194 10.50000 0.05 1.13 Q7 1 0.5000 0.6629 0.0334 10.50000 0.05 1.05 Q8 1 0.6163 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1.1632 -0.0070 26 8 8 0.1992 -0.3099 26 8 10 2.6080 0.4458 26 8 12 5.0262 -0.4221 26 8 14 9.0478 0.5003 26 8 16 0.5393 -0.1170 26 9 1 3.1484 0.4812 26 9 3 0.7160 0.4572 26 9 5 0.1151 -0.4664 26 9 7 -3.7448 0.3870 26 9 9 3.2794 0.2026 26 9 11 0.5111 -0.2423 26 9 13 -2.3908 -0.2620 26 9 15 -5.1808 -0.4125 26 10 0 1.4271 1.8106 26 10 2 -3.1996 -1.1476 26 10 4 0.5363 0.0169 26 10 6 0.4863 -0.1534 26 10 8 1.2392 -0.1620 26 10 10 3.3262 0.2235 26 10 12 3.5497 0.0392 26 10 14 8.2442 0.8788 26 11 1 -0.5090 -1.4390 26 11 3 -0.4607 0.3456 26 11 5 -3.2938 0.2549 26 11 7 -0.0015 0.2255 26 11 9 7.8706 -0.4601 26 11 11 4.1024 0.1135 26 11 13 2.4358 -0.8285 26 12 0 1.0420 -1.1804 26 12 2 -1.0920 0.2823 26 12 4 -2.9804 0.4178 26 12 6 3.4622 -0.4844 26 12 8 -0.3090 0.1771 26 12 10 2.4510 0.0132 26 13 1 -0.9274 0.5795 26 13 3 -1.0052 -0.3154 26 13 5 -2.0190 -0.0697 26 13 7 2.4444 0.1071 26 13 9 10.5786 -0.1449 26 14 0 -0.1037 -0.0312 26 14 2 0.1926 0.3799 26 14 4 -1.1920 -0.5931 26 14 6 6.0200 0.4879 27 0 1 2.0825 -0.6687 27 0 3 5.8968 -0.2916 27 0 5 -7.0439 -0.8285 27 0 7 4.6542 2.3553 27 0 9 -5.9037 -2.5837 27 0 11 -1.5786 1.1962 27 0 13 -5.4225 -0.0038 27 0 15 -12.8966 -0.3867 27 0 17 -8.6875 -0.5095 27 1 2 4.0897 -0.4440 27 1 4 -1.2866 -0.5215 27 1 6 5.8161 -0.3559 27 1 8 -4.4047 0.8302 27 1 10 0.5775 -0.3115 27 1 12 -0.4931 -0.1724 27 1 14 2.0939 0.3796 27 1 16 -3.8753 0.0250 27 1 18 2.8515 -0.8521 27 2 1 4.1521 0.2114 27 2 3 1.2416 -0.1967 27 2 5 0.4016 0.0050 27 2 7 -3.8027 0.4125 27 2 9 -1.7511 -0.1902 27 2 11 -5.1580 0.1098 27 2 13 5.0538 -0.3421 27 2 15 -6.1883 0.6769 27 2 17 5.1917 -0.2804 27 3 2 -1.8594 -0.3640 27 3 4 -1.6147 0.3936 27 3 6 -0.0257 -0.2353 27 3 8 3.2179 0.3617 27 3 10 1.0939 -0.2712 27 3 12 4.0198 0.2945 27 3 14 1.4787 0.0704 27 3 16 -2.0161 0.1259 27 4 1 2.8092 0.7544 27 4 3 -1.0392 -0.2786 27 4 5 -4.8587 0.2148 27 4 7 0.7377 -0.3755 27 4 9 -1.0133 0.2000 27 4 11 -8.4090 0.2452 27 4 13 -2.5594 -0.3708 27 4 15 -5.1158 0.2029 27 4 17 1.7480 -0.5851 27 5 2 -0.2079 -0.0402 27 5 4 -5.5614 0.6250 27 5 6 1.6873 -0.2989 27 5 8 -0.3517 -0.1355 27 5 10 -0.6064 0.2785 27 5 12 4.3966 -0.1068 27 5 14 9.5243 -0.3593 27 5 16 3.6462 -0.0938 27 6 1 4.2786 0.2612 27 6 3 -3.2377 -0.4686 27 6 5 3.3746 0.3256 27 6 7 -2.0472 -0.5854 27 6 9 -3.9628 0.3991 27 6 11 -1.8664 -0.1414 27 6 13 -5.7571 0.2063 27 6 15 1.8008 0.0475 27 7 2 -1.8981 -0.0036 27 7 4 -0.5227 0.0953 27 7 6 -2.4052 0.2531 27 7 8 -1.3140 -0.2548 27 7 10 0.4048 -0.1028 27 7 12 -4.9461 -0.2942 27 7 14 12.3232 0.1715 27 8 1 1.4788 -0.2387 27 8 3 -4.1879 -0.1134 27 8 5 -1.7290 0.2786 27 8 7 -0.2035 -0.2820 27 8 9 -3.9869 -0.0427 27 8 11 -1.9672 -0.1993 27 8 13 -0.8768 0.2671 27 8 15 -6.9203 -0.1788 27 9 2 -2.2199 -0.1231 27 9 4 3.3046 -0.2703 27 9 6 2.8913 0.2785 27 9 8 -0.7414 -0.1829 27 9 10 4.4444 0.3081 27 9 12 3.4890 -0.2402 27 9 14 0.9060 0.3952 27 10 1 1.4304 0.3760 27 10 3 2.2029 0.1560 27 10 5 -2.2592 -0.1003 27 10 7 -3.4709 0.4133 27 10 9 1.9938 -0.4635 27 10 11 3.2475 -0.0919 27 11 2 2.3657 0.1406 27 11 4 2.2508 -0.1056 27 11 6 0.8914 -0.2515 27 11 8 -2.2146 0.2908 27 11 10 -2.8003 0.4137 27 12 1 2.7372 0.0558 27 12 3 -0.0104 0.2030 27 12 5 -2.6318 -0.0660 27 12 7 -1.6200 0.2224 27 12 9 3.8773 -0.5910 27 13 2 -3.5850 0.4219 27 13 4 -2.4962 -0.1497 27 13 6 2.2899 -0.0552 28 0 0 1.9153 -2.1488 28 0 2 -0.9251 1.4707 28 0 4 2.5094 0.2881 28 0 6 2.3223 -1.3951 28 0 8 1.7852 0.0905 28 0 10 -1.0370 1.1495 28 0 12 0.9395 -0.9120 28 0 14 5.7966 -0.3968 28 0 16 1.8336 1.1864 28 1 1 -2.5380 0.3921 28 1 3 1.4884 0.1782 28 1 5 -0.4980 0.7559 28 1 7 0.9637 -0.5636 28 1 9 -2.6973 0.4684 28 1 11 2.0380 0.1474 28 1 13 -4.6190 0.1241 28 1 15 -0.3123 -0.4300 28 1 17 4.6319 1.3596 28 2 0 -5.3466 0.8918 28 2 2 -0.1158 -0.6481 28 2 4 1.3107 -0.3694 28 2 6 3.7454 0.1099 28 2 8 -5.9599 -0.3141 28 2 10 3.3697 -0.0226 28 2 12 -3.2454 -0.0577 28 2 14 7.3857 0.1304 28 2 16 14.2551 -0.4198 28 3 1 1.2858 -0.6551 28 3 3 4.0949 0.0213 28 3 5 -0.2162 0.4765 28 3 7 -6.1171 -0.2592 28 3 9 1.3154 0.1924 28 3 11 -0.6525 0.0581 28 3 13 -1.8217 0.2889 28 3 15 4.8651 -0.4440 28 4 0 -1.9854 -0.0685 28 4 2 0.1480 -0.0135 28 4 4 -0.7794 -0.0644 28 4 6 -1.1275 0.3892 28 4 8 -1.7277 -0.3499 28 4 10 3.0107 -0.2404 28 4 12 5.5486 -0.1722 28 4 14 1.5152 0.1216 28 4 16 2.0882 -0.1668 28 5 1 0.3205 0.4517 28 5 3 2.8880 -0.5343 28 5 5 2.5945 -0.0337 28 5 7 -0.0434 0.0567 28 5 9 1.5916 0.0672 28 5 11 -0.1777 -0.1868 28 5 13 -12.1443 0.0758 28 5 15 -4.7636 0.1072 28 6 0 -2.9619 0.1458 28 6 2 -2.1790 0.1022 28 6 4 -0.1220 -0.3062 28 6 6 -3.0751 0.2227 28 6 8 1.1518 -0.0083 28 6 10 -5.0200 0.1887 28 6 12 -1.5431 -0.2286 28 6 14 4.9544 0.3312 28 7 1 -0.3466 -0.5318 28 7 3 1.6794 0.1518 28 7 5 0.1778 -0.2163 28 7 7 -0.6208 -0.0677 28 7 9 -4.6871 0.1296 28 7 11 -0.1807 -0.0739 28 7 13 -1.6894 -0.0743 28 8 0 -3.0736 -1.0473 28 8 2 -2.6892 0.7274 28 8 4 -0.9216 -0.1348 28 8 6 -0.9060 -0.0447 28 8 8 2.3665 -0.0576 28 8 10 -3.7050 0.2938 28 8 12 -4.7059 -0.0933 28 9 1 -0.2313 0.4045 28 9 3 -1.1731 0.4555 28 9 5 3.5080 -0.3880 28 9 7 0.3374 0.2130 28 9 9 -2.8064 0.0409 28 9 11 -4.5576 0.0701 28 10 0 -1.3721 0.8801 28 10 2 -0.3524 -0.4919 28 10 4 2.7206 0.2961 28 10 6 -0.2572 0.1030 28 10 8 3.0276 -0.1086 28 10 10 -4.5107 0.1648 28 11 1 1.6734 -0.3254 28 11 3 0.1304 -0.0858 28 11 5 0.6619 0.3546 28 11 7 3.3809 -0.0186 28 11 9 -2.8899 -0.2592 28 12 0 -3.2031 -0.2526 28 12 2 -1.8275 0.2444 28 12 4 0.2801 0.1690 28 12 6 4.3020 -0.4260 29 0 1 2.0234 0.5274 29 0 3 6.9198 -1.4502 29 0 5 6.3169 0.9354 29 0 7 -4.7176 0.3253 29 0 9 -3.1466 -0.8072 29 0 11 2.4786 0.2643 29 0 13 6.9750 0.7516 29 0 15 -2.5280 -0.4191 29 1 2 -0.0497 0.4325 29 1 4 -3.8601 -0.3009 29 1 6 -2.4204 -0.4753 29 1 8 0.7027 0.8976 29 1 10 2.7001 -0.2877 29 1 12 3.2283 -0.2689 29 1 14 0.2226 0.7388 29 2 1 -1.8457 -0.1135 29 2 3 -1.8293 -0.1843 29 2 5 0.4485 -0.1390 29 2 7 -0.2433 -0.0922 29 2 9 7.2938 -0.0240 29 2 11 2.6425 -0.4628 29 2 13 5.5682 -0.1367 29 2 15 -7.8267 0.1162 29 3 2 3.1020 0.3555 29 3 4 0.9883 0.2217 29 3 6 -0.4030 -0.1788 29 3 8 4.8393 0.4623 29 3 10 -1.2160 -0.0817 29 3 12 8.9726 0.0508 29 3 14 3.9439 0.1565 29 4 1 2.6714 0.0297 29 4 3 3.0742 0.0906 29 4 5 0.2016 -0.2433 29 4 7 8.7628 -0.3292 29 4 9 3.9728 0.5173 29 4 11 5.9554 -0.0186 29 4 13 9.9064 -0.0233 29 5 2 1.5300 0.0996 29 5 4 -5.4134 0.2017 29 5 6 3.6551 0.0086 29 5 8 -3.3715 0.3204 29 5 10 1.1942 0.1857 29 5 12 8.8383 0.3408 29 5 14 -1.7081 0.1231 29 6 1 2.6730 -0.0997 29 6 3 -5.3303 -0.2500 29 6 5 1.1498 0.4145 29 6 7 0.3423 -0.2063 29 6 9 9.2010 -0.0402 29 6 11 13.0802 -0.3498 29 6 13 -8.0885 -0.2978 29 7 2 -3.6363 -0.0060 29 7 4 0.4084 -0.1142 29 7 6 1.0448 -0.0195 29 7 8 5.4834 -0.2713 29 7 10 9.3380 -0.3930 29 7 12 -4.2402 0.2677 29 8 1 5.2721 -0.0377 29 8 3 7.0882 -0.1060 29 8 5 4.0365 0.0612 29 8 7 2.4892 0.0242 29 8 9 3.9885 0.0077 29 8 11 1.3520 0.1401 29 9 2 -1.6432 -0.1704 29 9 4 -2.6014 -0.3191 29 9 6 -4.9639 0.1866 29 9 8 -0.0356 0.0927 29 9 10 1.3989 -0.3133 29 10 1 -0.8126 0.2823 29 10 3 2.5044 -0.0195 29 10 5 -1.8015 -0.4395 29 10 7 1.4077 0.2650 29 11 2 -0.0334 0.0241 29 11 4 -2.6213 0.2917 30 0 0 3.5156 -0.2363 30 0 2 3.7728 -0.8665 30 0 4 -4.3378 1.6806 30 0 6 0.9320 -1.8122 30 0 8 10.1270 0.3772 30 0 10 2.8383 1.2123 30 0 12 1.7825 -0.9816 30 0 14 4.5654 0.5357 30 1 1 -1.4833 -0.3952 30 1 3 -1.8805 0.1003 30 1 5 -1.9389 0.8342 30 1 7 -0.1390 -0.4146 30 1 9 -2.9157 0.2059 30 1 11 -0.0316 0.1113 30 1 13 -2.0762 0.0390 30 2 0 0.4044 -0.2878 30 2 2 -1.4001 -0.2171 30 2 4 -6.0284 -0.1159 30 2 6 -1.2107 0.0332 30 2 8 -3.7033 -0.3627 30 2 10 2.3492 0.0458 30 2 12 -2.1212 -0.1715 30 3 1 -3.9952 -0.8447 30 3 3 -0.8435 0.3020 30 3 5 1.0307 0.4090 30 3 7 -3.1489 -0.0080 30 3 9 6.8292 -0.0295 30 3 11 -1.7870 0.0776 30 3 13 -8.5949 0.0580 30 4 0 2.7766 -0.7321 30 4 2 3.7910 0.4020 30 4 4 3.2279 -0.2560 30 4 6 -2.3218 0.0798 30 4 8 1.9824 -0.1915 30 4 10 -4.7144 0.0047 30 4 12 -7.1726 0.2079 30 5 1 -1.6407 0.7223 30 5 3 -3.7147 0.0658 30 5 5 -5.8063 -0.6675 30 5 7 1.9853 0.3632 30 5 9 -0.2398 -0.1312 30 5 11 -3.3559 0.0908 30 6 0 -1.2752 1.1771 30 6 2 -4.5873 -0.1893 30 6 4 3.7959 -0.4171 30 6 6 1.2712 0.2416 30 6 8 -4.7963 0.1083 30 6 10 -10.1484 -0.3765 30 7 1 0.0547 -1.2602 30 7 3 4.3522 0.0912 30 7 5 0.5662 -0.0542 30 7 7 2.0129 -0.1073 30 7 9 -0.2723 -0.0786 30 8 0 6.2472 -0.7739 30 8 2 -0.3423 0.3552 30 8 4 4.4670 -0.1242 30 8 6 3.3812 -0.1498 30 8 8 -1.7921 0.2003 30 9 1 -2.2583 0.0775 30 9 3 3.6265 0.1621 30 9 5 1.9563 0.0619 30 9 7 -2.2869 -0.2256 30 10 0 -2.6460 -0.2733 30 10 2 -1.0728 -0.2173 30 10 4 -0.5191 -0.1995 31 0 1 -4.7836 1.1423 31 0 3 -4.9929 -1.8871 31 0 5 6.6686 1.4818 31 0 7 -8.2756 -0.6568 31 0 9 4.4328 0.2045 31 0 11 -6.8382 -0.7827 31 1 2 2.6835 1.1908 31 1 4 4.1033 -0.4830 31 1 6 -0.3800 -0.2347 31 1 8 2.7106 0.7185 31 1 10 -5.8794 -0.2577 31 1 12 0.6877 -0.7456 31 2 1 0.5169 -0.4135 31 2 3 0.5119 -0.0186 31 2 5 3.0306 -0.0689 31 2 7 -2.7896 -0.2549 31 2 9 -5.1797 0.3035 31 2 11 -10.1931 -0.3966 31 3 2 -4.4211 0.5269 31 3 4 -1.6802 -0.2745 31 3 6 1.3621 -0.0077 31 3 8 -1.7183 0.1759 31 3 10 -12.6618 0.2414 31 4 1 -4.5735 -0.3066 31 4 3 -0.6217 0.3400 31 4 5 -3.9063 -0.4704 31 4 7 -1.8697 -0.3517 31 4 9 -8.6060 0.2246 31 5 2 0.4591 -0.0342 31 5 4 0.5062 0.1776 31 5 6 4.8360 0.0969 31 5 8 -6.7442 0.1084 31 5 10 -1.8463 -0.3501 31 6 1 1.7333 -0.0991 31 6 3 2.6987 0.2699 31 6 5 1.5427 -0.0289 31 6 7 -3.0821 0.0906 31 6 9 -0.3655 0.4165 31 7 2 -3.2194 0.0418 31 7 4 -1.6259 -0.0934 31 7 6 -4.1310 0.3529 31 8 1 -5.0620 0.0555 31 8 3 -1.9723 0.1240 31 8 5 -7.2714 0.0928 31 9 2 -0.8246 0.2990 32 0 0 -0.5401 0.3432 32 0 2 -1.3965 -0.9922 32 0 4 -10.3825 1.8381 32 0 6 -0.3877 -1.7079 32 0 8 0.2547 0.2552 32 1 1 -1.6454 -0.4481 32 1 3 1.5837 -0.1007 32 1 5 3.4958 0.4133 32 1 7 -0.0421 -0.7181 32 1 9 2.3198 -0.6228 32 2 0 3.5501 -0.2533 32 2 2 5.0313 0.4184 32 2 4 -0.6542 0.0252 32 2 6 4.4997 0.1311 32 2 8 5.0659 -0.0644 32 3 1 0.8460 -0.5383 32 3 3 2.6270 0.5069 32 3 5 1.5728 -0.0622 32 3 7 -3.6526 -0.0979 32 4 0 -0.3905 -0.8888 32 4 2 -3.6982 0.2646 32 4 4 -0.9829 -0.0995 32 4 6 -1.6836 0.0319 32 4 8 2.1779 -0.2750 32 5 1 2.9918 0.3545 32 5 3 8.1540 0.1716 32 5 5 1.4519 -0.6496 32 5 7 1.9752 0.3162 32 6 0 8.3846 1.3860 32 6 2 1.2464 -0.5801 32 6 4 -0.4364 0.0974 32 7 1 -0.9430 0.2175 33 0 1 -7.3149 0.7576 33 0 3 3.4303 -1.2390 33 0 5 1.1511 1.1919 33 1 2 1.7025 0.9941 33 1 4 -7.4436 -0.5998 33 1 6 0.5854 0.2040 33 2 1 -1.3926 -0.5631 33 2 3 -3.7527 0.2969 33 2 5 4.8166 0.0608 33 3 2 -1.3257 0.1027 33 3 4 3.5892 -0.4880 33 4 1 -1.2057 -0.3011 33 4 3 5.9620 0.7461 0 0 0 0.0 0.0 ; _shelx_fab_checksum 80097 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y+1/2, z' '-x, y+1/2, -z' 'x, -y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y-1/2, -z' 'x, -y-1/2, z' '-x, y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'x+1/2, -y, z+1/2' '-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 0.42127(3) 0.65979(5) 0.28246(4) 0.0533(3) Uani 1 1 d . U . . . Cu2 Cu 0.500000 0.750000 0.37186(8) 0.0715(6) Uani 1 4 d DS TU P . . Cu3 Cu 0.500000 0.750000 0.15944(8) 0.0562(5) Uani 1 4 d DS TU P . . S1 S 0.42342(9) 0.750000 0.21134(11) 0.0461(5) Uani 1 2 d S TU P . . S2 S 0.500000 0.63486(15) 0.32787(12) 0.0556(6) Uani 1 2 d S TU P B . S3 S 0.28361(10) 0.34516(10) 0.30449(11) 0.0809(8) Uani 1 1 d . U . . . N1 N 0.35353(13) 0.6078(2) 0.31096(18) 0.0536(12) Uani 1 1 d G U . . . C8 C 0.32752(16) 0.63923(19) 0.36048(18) 0.0510(14) Uani 1 1 d G U . . . H8 H 0.341629 0.683588 0.379116 0.061 Uiso 1 1 calc R U . . . C9 C 0.28042(16) 0.6044(2) 0.38213(17) 0.0569(16) Uani 1 1 d G U . . . H9 H 0.263013 0.625457 0.415261 0.068 Uiso 1 1 calc R U . . . C10 C 0.25933(13) 0.5381(2) 0.3543(2) 0.0557(15) Uani 1 1 d G U . . . H10 H 0.227812 0.514810 0.368761 0.067 Uiso 1 1 calc R U . . . C11 C 0.28534(15) 0.50665(19) 0.30476(19) 0.0480(13) Uani 1 1 d G U . . . C12 C 0.33244(15) 0.5415(2) 0.28310(16) 0.0522(15) Uani 1 1 d G U . . . H12 H 0.349844 0.520423 0.249969 0.063 Uiso 1 1 calc R U . . . C5 C 0.3104(4) 0.750000 0.2005(5) 0.059(2) Uani 1 2 d S TU P . . H5C H 0.308932 0.702605 0.223709 0.088 Uiso 0.5 1 calc R U P A -1 H5B H 0.310763 0.794653 0.226694 0.088 Uiso 0.5 1 calc R U P A -1 H5A H 0.279107 0.752742 0.175089 0.088 Uiso 0.5 1 calc R U P A -1 C6 C 0.3625(4) 0.750000 0.1621(5) 0.060(2) Uani 1 2 d S TU P . . C7 C 0.3656(3) 0.6745(6) 0.1246(4) 0.079(2) Uani 1 1 d . U . . . H7A H 0.401293 0.669476 0.107901 0.118 Uiso 1 1 calc R U . . . H7B H 0.339289 0.676973 0.093063 0.118 Uiso 1 1 calc R U . . . H7C H 0.358049 0.629824 0.149432 0.118 Uiso 1 1 calc R U . . . C13 C 0.2652(3) 0.4359(3) 0.2741(3) 0.0543(16) Uani 1 1 d . U . . . C14 C 0.250000 0.2894(5) 0.250000 0.075(3) Uani 1 2 d S TU P . . F1 F 0.61941(14) 0.7797(6) 0.5713(4) 0.048(5) Uani 0.125 1 d D U P B -1 F2 F 0.5316(2) 0.8158(3) 0.5714(4) 0.048(5) Uani 0.125 1 d D U P B -1 F3 F 0.5557(5) 0.6829(2) 0.5742(4) 0.041(5) Uani 0.125 1 d D U P B -1 F4 F 0.4422(7) 0.8233(15) -0.0289(13) 0.062(6) Uani 0.125 1 d D U P C -1 F5 F 0.5344(8) 0.8335(13) -0.0425(13) 0.058(6) Uani 0.125 1 d D U P C -1 F6 F 0.4894(10) 0.7266(10) -0.0752(8) 0.059(6) Uani 0.125 1 d D U P C -1 O1 O 0.52120(13) 0.7473(19) 0.46015(9) 0.037(3) Uani 0.125 1 d D U P B -1 O2 O 0.60750(16) 0.7440(14) 0.4536(3) 0.020(4) Uani 0.125 1 d D U P B -1 O3 O 0.506(2) 0.8082(5) 0.07971(10) 0.063(4) Uani 0.125 1 d D U P C -1 O4 O 0.493(2) 0.6996(9) 0.0577(9) 0.064(6) Uani 0.125 1 d D U P C -1 C1 C 0.4970(9) 0.5517(8) 0.3813(6) 0.039(3) Uani 0.25 1 d D U P B -1 C2 C 0.5513(9) 0.5421(13) 0.4129(12) 0.031(5) Uani 0.25 1 d D U P B -1 H2A H 0.548769 0.500180 0.441425 0.047 Uiso 0.25 1 calc R U P B -1 H2B H 0.560407 0.590118 0.433032 0.047 Uiso 0.25 1 calc R U P B -1 H2C H 0.578978 0.529920 0.384228 0.047 Uiso 0.25 1 calc R U P B -1 C3 C 0.4532(9) 0.5704(15) 0.4274(12) 0.040(5) Uani 0.25 1 d D U P B -1 H3A H 0.447814 0.525707 0.452797 0.060 Uiso 0.25 1 calc R U P B -1 H3B H 0.419757 0.582740 0.407381 0.060 Uiso 0.25 1 calc R U P B -1 H3C H 0.464372 0.614673 0.450938 0.060 Uiso 0.25 1 calc R U P B -1 C4 C 0.4820(8) 0.4776(9) 0.3466(8) 0.043(5) Uani 0.25 1 d D U P B -1 H4A H 0.507553 0.469843 0.314836 0.065 Uiso 0.25 1 calc R U P B -1 H4B H 0.446156 0.483367 0.330247 0.065 Uiso 0.25 1 calc R U P B -1 H4C H 0.482766 0.433060 0.372812 0.065 Uiso 0.25 1 calc R U P B -1 C15 C 0.56617(11) 0.7533(12) 0.48359(10) 0.032(3) Uani 0.125 1 d D U P B -1 C16 C 0.503(2) 0.7645(6) 0.0362(4) 0.049(4) Uani 0.125 1 d D U P C -1 C32 C 0.56764(12) 0.75765(16) 0.55165(10) 0.039(4) Uani 0.125 1 d D U P B -1 C59 C 0.4915(7) 0.7824(9) -0.0294(5) 0.053(4) Uani 0.125 1 d D U P C -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 Cu1 0.0533(5) 0.0434(5) 0.0632(5) 0.0001(4) -0.0044(4) -0.0122(4) Cu2 0.0770(14) 0.0649(12) 0.0726(13) 0.000 0.000 0.000 Cu3 0.0377(9) 0.0736(12) 0.0574(11) 0.000 0.000 0.000 S1 0.0329(10) 0.0473(12) 0.0579(14) 0.000 -0.0016(10) 0.000 S2 0.0523(14) 0.0482(13) 0.0663(16) 0.0182(12) 0.000 0.000 S3 0.0929(15) 0.0302(8) 0.1198(18) 0.0024(10) -0.0644(14) -0.0010(9) N1 0.051(3) 0.039(3) 0.071(3) 0.004(2) -0.012(2) -0.013(2) C8 0.051(3) 0.038(3) 0.064(4) -0.002(3) -0.013(3) -0.003(3) C9 0.049(3) 0.045(3) 0.077(4) -0.010(3) -0.006(3) 0.003(3) C10 0.044(3) 0.043(3) 0.080(4) -0.001(3) -0.005(3) -0.005(3) C11 0.040(3) 0.030(2) 0.075(4) 0.001(3) -0.016(3) 0.000(2) C12 0.051(3) 0.038(3) 0.068(4) -0.004(3) -0.010(3) -0.009(3) C5 0.037(4) 0.073(6) 0.066(6) 0.000 -0.004(4) 0.000 C6 0.038(4) 0.076(5) 0.065(5) 0.000 -0.006(4) 0.000 C7 0.049(4) 0.117(7) 0.070(5) -0.026(5) -0.008(4) -0.004(4) C13 0.045(3) 0.027(2) 0.091(4) -0.001(3) -0.024(3) -0.001(2) C14 0.080(6) 0.034(4) 0.113(7) 0.000 -0.057(5) 0.000 F1 0.050(7) 0.065(9) 0.030(8) -0.015(7) -0.021(6) -0.009(6) F2 0.050(8) 0.050(7) 0.043(8) -0.019(7) 0.005(7) -0.005(7) F3 0.043(8) 0.048(7) 0.031(8) 0.010(7) 0.007(7) -0.003(6) F4 0.060(8) 0.070(9) 0.056(9) 0.004(7) -0.011(7) 0.006(7) F5 0.062(9) 0.061(9) 0.052(9) 0.012(7) 0.005(8) 0.002(7) F6 0.057(11) 0.072(9) 0.048(7) -0.009(6) -0.009(7) 0.002(7) O1 0.038(5) 0.035(5) 0.040(4) 0.006(4) 0.004(4) -0.001(5) O2 0.028(6) 0.008(7) 0.022(6) 0.009(8) 0.000(5) 0.005(8) O3 0.056(6) 0.074(6) 0.058(5) 0.003(4) 0.001(4) 0.006(4) O4 0.043(10) 0.076(7) 0.072(9) 0.034(6) 0.002(8) 0.014(8) C1 0.031(6) 0.043(5) 0.043(6) 0.021(5) -0.001(6) -0.011(7) C2 0.030(7) 0.025(12) 0.038(12) 0.020(8) 0.000(7) -0.004(8) C3 0.022(8) 0.047(14) 0.051(12) 0.030(9) -0.004(8) -0.012(9) C4 0.041(11) 0.036(7) 0.052(10) 0.031(7) -0.015(8) -0.014(7) C15 0.035(5) 0.031(5) 0.031(4) 0.002(4) 0.005(3) -0.001(4) C16 0.044(6) 0.052(6) 0.052(5) 0.003(4) 0.001(4) 0.003(4) C32 0.039(5) 0.042(5) 0.035(5) 0.000(4) 0.003(4) -0.003(4) C59 0.053(6) 0.056(6) 0.051(5) 0.000(4) -0.001(4) 0.001(4) 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 '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 S1 Cu1 S2 116.12(9) . . ? N1 Cu1 S1 123.97(14) . . ? N1 Cu1 S2 119.73(14) . . ? S2 Cu2 S2 126.48(15) . 2_665 ? O1 Cu2 S2 114.6(9) . . ? O1 Cu2 S2 117.1(9) . 2_665 ? S1 Cu3 S1 116.57(15) . 2_665 ? O3 Cu3 S1 113.5(14) . 2_665 ? O3 Cu3 S1 121.3(15) . . ? O3 Cu3 S1 121.3(15) 2_665 2_665 ? O3 Cu3 S1 113.5(14) 2_665 . ? O3 Cu3 O3 58.38(5) 2_665 . ? Cu1 S1 Cu1 87.69(10) . 11_575 ? Cu1 S1 Cu3 113.53(8) 11_575 . ? Cu1 S1 Cu3 113.53(8) . . ? C6 S1 Cu1 114.1(2) . . ? C6 S1 Cu1 114.1(2) . 11_575 ? C6 S1 Cu3 111.9(4) . . ? Cu1 S2 Cu1 120.68(12) 12_655 . ? Cu2 S2 Cu1 92.06(8) . . ? Cu2 S2 Cu1 92.06(8) . 12_655 ? C1 S2 Cu1 118.3(7) . 12_655 ? C1 S2 Cu1 113.9(7) . . ? C1 S2 Cu2 112.9(5) . . ? C13 S3 C14 94.7(3) . . ? C8 N1 Cu1 118.1(2) . . ? C8 N1 C12 120.0 . . ? C12 N1 Cu1 121.9(2) . . ? N1 C8 H8 120.0 . . ? N1 C8 C9 120.0 . . ? C9 C8 H8 120.0 . . ? C8 C9 H9 120.0 . . ? C10 C9 C8 120.0 . . ? C10 C9 H9 120.0 . . ? C9 C10 H10 120.0 . . ? C9 C10 C11 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C12 120.0 . . ? C10 C11 C13 122.3(4) . . ? C12 C11 C13 117.7(4) . . ? N1 C12 H12 120.0 . . ? C11 C12 N1 120.0 . . ? C11 C12 H12 120.0 . . ? H5C C5 H5B 109.5 . . ? H5C C5 H5A 109.5 . . ? H5B C5 H5A 109.5 . . ? C6 C5 H5C 109.5 . . ? C6 C5 H5B 109.5 . . ? C6 C5 H5A 109.5 . . ? C5 C6 S1 109.7(7) . . ? C7 C6 S1 106.5(5) 11_575 . ? C7 C6 S1 106.5(5) . . ? C7 C6 C5 110.3(5) . . ? C7 C6 C5 110.3(5) 11_575 . ? C7 C6 C7 113.3(10) 11_575 . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C11 C13 S3 116.8(4) . . ? C13 C13 S3 118.0(2) 7_545 . ? C13 C13 C11 125.2(3) 7_545 . ? S3 C14 S3 114.6(5) 7_545 . ? C14 C14 S3 122.7(3) 13 . ? C14 C14 S3 122.7(3) 13 7_545 ? C15 O1 Cu2 129.9(2) . . ? C16 O3 Cu3 113.4(6) . . ? C2 C1 S2 110.4(15) . . ? C2 C1 C3 109.0(10) . . ? C2 C1 C4 111.3(12) . . ? C3 C1 S2 107.8(15) . . ? C4 C1 S2 108.0(10) . . ? C4 C1 C3 110.3(12) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O1 C15 C32 116.9(3) . . ? O2 C15 O1 120.0(5) . . ? O2 C15 C32 122.2(4) . . ? O3 C16 C59 131.0(12) . . ? O4 C16 O3 104.0(12) . . ? O4 C16 C59 121.3(14) . . ? F1 C32 F2 106.7(4) . . ? F1 C32 F3 108.6(7) . . ? F1 C32 C15 110.4(5) . . ? F2 C32 F3 113.2(5) . . ? F2 C32 C15 109.6(7) . . ? F3 C32 C15 108.2(9) . . ? F4 C59 F5 110.4(12) . . ? F4 C59 F6 108.2(12) . . ? F4 C59 C16 104(2) . . ? F5 C59 C16 100.8(19) . . ? F6 C59 F5 107.1(11) . . ? F6 C59 C16 125.3(13) . . ? 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 S1 2.215(2) . ? Cu1 S2 2.2308(15) . ? Cu1 N1 1.993(3) . ? Cu2 S2 2.193(3) 2_665 ? Cu2 S2 2.193(3) . ? Cu2 O1 2.05000(15) . ? Cu3 S1 2.216(2) . ? Cu3 S1 2.217(2) 2_665 ? Cu3 O3 2.0502(10) . ? Cu3 O3 2.0502(10) 2_665 ? S1 C6 1.864(10) . ? S2 C1 1.856(14) . ? S3 C13 1.748(6) . ? S3 C14 1.755(5) . ? N1 C8 1.3900 . ? N1 C12 1.3900 . ? C8 H8 0.9300 . ? C8 C9 1.3900 . ? C9 H9 0.9300 . ? C9 C10 1.3900 . ? C10 H10 0.9300 . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C11 C13 1.472(6) . ? C12 H12 0.9300 . ? C5 H5C 0.9600 . ? C5 H5B 0.9600 . ? C5 H5A 0.9600 . ? C5 C6 1.545(13) . ? C6 C7 1.538(10) . ? C6 C7 1.538(10) 11_575 ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C13 C13 1.314(13) 7_545 ? C14 C14 1.342(18) 13 ? F1 C32 1.40000(11) . ? F2 C32 1.40000(11) . ? F3 C32 1.40000(11) . ? F4 C59 1.4001(10) . ? F5 C59 1.4000(10) . ? F6 C59 1.4001(10) . ? O1 C15 1.23000(16) . ? O2 C15 1.23000(12) . ? O3 C16 1.2300(10) . ? O4 C16 1.2298(10) . ? C1 C2 1.523(10) . ? C1 C3 1.529(9) . ? C1 C4 1.526(9) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C15 C32 1.53000(12) . ? C16 C59 1.5299(10) . ? 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 S1 C6 C5 -49.36(14) 11_575 . . . ? Cu1 S1 C6 C5 49.36(14) . . . . ? Cu1 S1 C6 C7 168.7(5) . . . 11_575 ? Cu1 S1 C6 C7 70.0(7) 11_575 . . 11_575 ? Cu1 S1 C6 C7 -168.7(5) 11_575 . . . ? Cu1 S1 C6 C7 -70.0(7) . . . . ? Cu1 S2 C1 C2 32.7(12) 12_655 . . . ? Cu1 S2 C1 C2 -176.5(10) . . . . ? Cu1 S2 C1 C3 -57.5(11) . . . . ? Cu1 S2 C1 C3 151.7(10) 12_655 . . . ? Cu1 S2 C1 C4 61.7(12) . . . . ? Cu1 S2 C1 C4 -89.2(12) 12_655 . . . ? Cu1 N1 C8 C9 -179.5(3) . . . . ? Cu1 N1 C12 C11 179.5(3) . . . . ? Cu2 S2 C1 C2 -73.2(12) . . . . ? Cu2 S2 C1 C3 45.9(12) . . . . ? Cu2 S2 C1 C4 165.0(9) . . . . ? Cu2 O1 C15 O2 -17(3) . . . . ? Cu2 O1 C15 C32 173.6(19) . . . . ? Cu3 S1 C6 C5 180.000(0) . . . . ? Cu3 S1 C6 C7 60.6(6) . . . . ? Cu3 S1 C6 C7 -60.6(6) . . . 11_575 ? Cu3 O3 C16 O4 5(5) . . . . ? Cu3 O3 C16 C59 163(4) . . . . ? N1 C8 C9 C10 0.0 . . . . ? C8 N1 C12 C11 0.0 . . . . ? C8 C9 C10 C11 0.0 . . . . ? C9 C10 C11 C12 0.0 . . . . ? C9 C10 C11 C13 179.1(5) . . . . ? C10 C11 C12 N1 0.0 . . . . ? C10 C11 C13 S3 -82.8(5) . . . . ? C10 C11 C13 C13 97.2(11) . . . 7_545 ? C12 N1 C8 C9 0.0 . . . . ? C12 C11 C13 S3 96.3(5) . . . . ? C12 C11 C13 C13 -83.6(10) . . . 7_545 ? C13 S3 C14 S3 -0.2(3) . . . 7_545 ? C13 S3 C14 C14 179.7(3) . . . 13 ? C13 C11 C12 N1 -179.2(4) . . . . ? C14 S3 C13 C11 -179.0(5) . . . . ? C14 S3 C13 C13 0.9(9) . . . 7_545 ? O1 C15 C32 F1 -168.3(18) . . . . ? O1 C15 C32 F2 -51(2) . . . . ? O1 C15 C32 F3 73(2) . . . . ? O2 C15 C32 F1 23(2) . . . . ? O2 C15 C32 F2 139.8(17) . . . . ? O2 C15 C32 F3 -96.3(19) . . . . ? O3 C16 C59 F4 -55(5) . . . . ? O3 C16 C59 F5 59(5) . . . . ? O3 C16 C59 F6 180(4) . . . . ? O4 C16 C59 F4 99(4) . . . . ? O4 C16 C59 F5 -146(4) . . . . ? O4 C16 C59 F6 -26(5) . . . . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.000 -0.009 0.500 2111.5 227.9 '5 CH2Cl2' 2 0.500 -0.347 0.000 2111.5 227.9 '5 CH2Cl2'