#------------------------------------------------------------------------------ #$Date: 2020-10-06 11:32:58 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257502 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/53/7705341.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_7705341 loop_ _publ_author_name 'Jarrah, Najmeh' 'Troyano, Javier' 'Carn\'e-S\'anchez, Arnau' 'Imaz, Inhar' 'Tangestaninejad, Shahram' 'Moghadam, Majid' 'Maspoch, Daniel' _publ_section_title ; Dynamic porous coordination polymers built-up from flexible 4,4'-dithiodibenzoate and rigid N-based ligands. ; _journal_issue 37 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 13142 _journal_page_last 13151 _journal_paper_doi 10.1039/d0dt02411b _journal_volume 49 _journal_year 2020 _chemical_formula_moiety 'C17 H15 Cu N O5 S2, 0.5(C3 H7 N O)' _chemical_formula_sum 'C18.5 H18.5 Cu N1.5 O5.5 S2' _chemical_formula_weight 477.51 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2020-08-24 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-08-25 deposited with the CCDC. 2020-09-02 downloaded from the CCDC. ; _cell_angle_alpha 102.901(5) _cell_angle_beta 100.793(5) _cell_angle_gamma 113.618(5) _cell_formula_units_Z 2 _cell_length_a 9.960(5) _cell_length_b 10.210(5) _cell_length_c 12.060(5) _cell_measurement_reflns_used 2981 _cell_measurement_temperature 100 _cell_measurement_theta_max 30 _cell_measurement_theta_min 1 _cell_volume 1041.4(9) _computing_cell_refinement 'xds (Kabsch et al., 2010)' _computing_data_collection 'Mxcube (Gabadinho et al., 2010)' _computing_data_reduction 'xds (Kabsch et al., 2010)' _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_temperature 100 _diffrn_measured_fraction_theta_full 0.891 _diffrn_measured_fraction_theta_max 0.752 _diffrn_measurement_device_type 'Pilatus DECTRIS 6M' _diffrn_measurement_method 'w/ scan' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.82653 _diffrn_reflns_av_unetI/netI 0.0641 _diffrn_reflns_Laue_measured_fraction_full 0.891 _diffrn_reflns_Laue_measured_fraction_max 0.752 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 3976 _diffrn_reflns_point_group_measured_fraction_full 0.891 _diffrn_reflns_point_group_measured_fraction_max 0.752 _diffrn_reflns_theta_full 29.730 _diffrn_reflns_theta_max 33.846 _diffrn_reflns_theta_min 2.684 _exptl_absorpt_coefficient_mu 1.931 _exptl_absorpt_correction_type none _exptl_crystal_colour 'clear dark green' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 1.523 _exptl_crystal_description block _exptl_crystal_F_000 490 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.682 _refine_diff_density_min -0.738 _refine_diff_density_rms 0.162 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 276 _refine_ls_number_reflns 3976 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.060 _refine_ls_R_factor_all 0.0753 _refine_ls_R_factor_gt 0.0710 _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^)+(0.1597P)^2^+0.2243P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2098 _refine_ls_wR_factor_ref 0.2146 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3477 _reflns_number_total 3976 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02411b2.cif _cod_data_source_block import01_tw _cod_depositor_comments 'Adding full bibliography for 7705341--7705344.cif.' _cod_original_cell_volume 1041.4(8) _cod_original_formula_sum 'C18.50 H18.50 Cu N1.50 O5.50 S2' _cod_database_code 7705341 _shelx_shelxl_version_number 2018/1 _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 0.870 _shelx_estimated_absorpt_t_min 0.744 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.543(5) 0.457(5) 2. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 3. Restrained distances C12S-H12S 1.08 with sigma of 0.02 4. Others Fixed Sof: O11S(0.5) N13S(0.5) C12S(0.5) H12S(0.5) C14S(0.5) H14A(0.5) H14B(0.5) H14C(0.5) C15S(0.5) H15A(0.5) H15B(0.5) H15C(0.5) 5.a Free rotating group: O11S(N13S,C12S,C14S,C15S) 5.b Aromatic/amide H refined with riding coordinates: C2S(H2S), C5(H5), C6(H6), C8(H8), C9(H9), C13(H13), C14(H14), C16(H16), C17(H17), C12S(H12S) 5.c Idealised Me refined as rotating group: C4S(H4SA,H4SB,H4SC), C5S(H5SA,H5SB,H5SC), C14S(H14A,H14B,H14C), C15S(H15A, H15B,H15C) ; _shelx_res_file ; TITL import01 in P -1 import01_tw.res created by SHELXL-2018/1 at 16:20:00 on 24-Aug-2020 CELL 0.82653 9.96 10.21 12.06 102.901 100.793 113.618 ZERR 2 0.005 0.005 0.005 0.005 0.005 0.005 LATT 1 SFAC C H Cu N O S DISP C 0.005 0.002 16.098 DISP H -0 0 0.63 DISP N 0.009 0.005 28.748 DISP O 0.016 0.009 48.778 DISP S 0.157 0.168 825.328 UNIT 37 37 2 3 11 4 DFIX 1.08 C12S H12S L.S. 10 PLAN 6 SIZE 0.1 0.15 0.22 TEMP -173.15 LIST 6 MORE -1 BOND $H CONF fmap 2 acta MERG 0 REM REM REM WGHT 0.159700 0.224300 BASF 0.45724 FVAR 12.67179 CU1 3 0.130241 0.124704 0.058278 11.00000 0.03989 0.03037 = 0.03720 0.01059 0.00927 0.01290 S10 6 -0.469705 0.319153 0.433250 11.00000 0.04841 0.04966 = 0.05047 0.01818 0.01471 0.02847 S11 6 0.316602 -0.467487 0.405201 11.00000 0.05735 0.04246 = 0.04762 0.01667 0.01471 0.02993 O1 5 0.018950 0.185058 0.160803 11.00000 0.04313 0.03554 = 0.05016 0.00848 0.01169 0.01809 PART 1 O1S 5 0.350155 0.323334 0.128533 11.00000 0.05555 0.04009 = 0.04652 0.01260 0.01152 0.01130 PART 0 O2 5 -0.204197 -0.025026 0.056875 11.00000 0.04690 0.04293 = 0.04315 0.00123 0.01303 0.01050 O19 5 0.171581 0.012625 0.160269 11.00000 0.04571 0.03533 = 0.04959 0.01627 0.00983 0.01850 O20 5 -0.045055 -0.202689 0.057999 11.00000 0.05654 0.03992 = 0.05150 0.02001 0.00402 0.01504 PART 1 N3S 4 0.506166 0.566366 0.150355 11.00000 0.06586 0.05263 = 0.05603 0.01583 0.02350 0.01533 C2S 1 0.369956 0.442809 0.117267 11.00000 0.05957 0.05012 = 0.05549 0.01209 0.02187 0.02286 AFIX 43 H2S 2 0.281078 0.450513 0.081690 11.00000 -1.20000 AFIX 0 PART 0 C3 1 -0.123978 0.102502 0.137751 11.00000 0.04576 0.03721 = 0.03805 0.01283 0.00943 0.01681 C4 1 -0.204249 0.162085 0.211446 11.00000 0.04324 0.04029 = 0.03630 0.01158 0.00904 0.01694 PART 1 C4S 1 0.646478 0.559686 0.206628 11.00000 0.07499 0.07305 = 0.13306 0.04807 0.02629 0.01454 AFIX 137 H4SA 2 0.715289 0.654392 0.272733 11.00000 -1.50000 H4SB 2 0.698946 0.545693 0.147260 11.00000 -1.50000 H4SC 2 0.618759 0.474518 0.237415 11.00000 -1.50000 AFIX 0 PART 0 C5 1 -0.122154 0.278503 0.321890 11.00000 0.04327 0.04379 = 0.04635 0.00908 0.01090 0.01607 AFIX 43 H5 2 -0.012859 0.322991 0.349170 11.00000 -1.20000 AFIX 0 PART 1 C5S 1 0.517148 0.708041 0.140071 11.00000 0.09494 0.05095 = 0.08938 0.02152 0.04770 0.02342 AFIX 137 H5SA 2 0.413553 0.696044 0.107257 11.00000 -1.50000 H5SB 2 0.577884 0.738190 0.086684 11.00000 -1.50000 H5SC 2 0.567474 0.786203 0.219282 11.00000 -1.50000 AFIX 0 PART 0 C6 1 -0.197957 0.329394 0.391560 11.00000 0.04265 0.04528 = 0.03923 0.00649 0.00674 0.01485 AFIX 43 H6 2 -0.141436 0.405565 0.467756 11.00000 -1.20000 AFIX 0 C7 1 -0.358357 0.268375 0.349542 11.00000 0.04689 0.04283 = 0.04492 0.01795 0.01500 0.02391 C8 1 -0.441820 0.154671 0.238199 11.00000 0.03971 0.05269 = 0.04034 0.01606 0.00482 0.01968 AFIX 43 H8 2 -0.550613 0.114465 0.209201 11.00000 -1.20000 AFIX 0 C9 1 -0.366031 0.101134 0.170713 11.00000 0.04451 0.04609 = 0.04444 0.01352 0.00596 0.01996 AFIX 43 H9 2 -0.423286 0.022285 0.095896 11.00000 -1.20000 AFIX 0 C12 1 0.254984 -0.358302 0.332934 11.00000 0.05573 0.04027 = 0.04971 0.02064 0.02279 0.02870 C13 1 0.321906 -0.200930 0.375920 11.00000 0.05434 0.03973 = 0.04744 0.01359 0.00718 0.01866 AFIX 43 H13 2 0.405135 -0.144868 0.448304 11.00000 -1.20000 AFIX 0 C14 1 0.265269 -0.126617 0.311423 11.00000 0.05878 0.03684 = 0.04615 0.01331 0.00812 0.02064 AFIX 43 H14 2 0.312321 -0.019051 0.339153 11.00000 -1.20000 AFIX 0 C15 1 0.141995 -0.206880 0.207998 11.00000 0.05116 0.03607 = 0.04018 0.01363 0.01280 0.02000 C16 1 0.073769 -0.365600 0.166102 11.00000 0.05518 0.03824 = 0.04225 0.01287 0.01101 0.01962 AFIX 43 H16 2 -0.011610 -0.422023 0.095115 11.00000 -1.20000 AFIX 0 C17 1 0.131871 -0.439661 0.229088 11.00000 0.05978 0.03772 = 0.04190 0.01020 0.01516 0.02310 AFIX 43 H17 2 0.086599 -0.547126 0.200537 11.00000 -1.20000 AFIX 0 C18 1 0.083748 -0.126650 0.135993 11.00000 0.05182 0.04069 = 0.04033 0.01497 0.01516 0.02470 PART -1 AFIX 6 O11S 5 0.738846 0.880341 0.431429 10.50000 0.20514 0.13403 = 0.15180 0.05335 0.09378 0.04858 N13S 4 1.000216 0.999502 0.500590 10.50000 0.11766 0.21133 = 0.06343 -0.03573 0.00138 0.06966 C12S 1 0.854397 0.961822 0.412870 10.50000 0.12421 0.07407 = 0.09100 0.03139 0.02995 0.00054 AFIX 43 H12S 2 0.850926 0.998296 0.347026 10.50000 -1.20000 AFIX 5 C14S 1 1.028605 1.023500 0.610220 10.50000 0.08948 0.09965 = 0.08863 0.04908 0.03798 0.04806 AFIX 137 H14A 2 1.081830 1.132956 0.652719 10.50000 -1.50000 H14B 2 1.094415 0.978721 0.635685 10.50000 -1.50000 H14C 2 0.931934 0.977726 0.628611 10.50000 -1.50000 AFIX 5 C15S 1 1.130557 1.131523 0.460691 10.50000 0.09172 0.11394 = 0.05074 0.03220 0.02334 0.03102 AFIX 137 H15A 2 1.088376 1.117242 0.376195 10.50000 -1.50000 H15B 2 1.225361 1.121070 0.472756 10.50000 -1.50000 H15C 2 1.153528 1.232826 0.509982 10.50000 -1.50000 AFIX 0 HKLF 5 REM import01 in P -1 REM R1 = 0.0710 for 3477 Fo > 4sig(Fo) and 0.0753 for all 3976 data REM 276 parameters refined using 1 restraints END WGHT 0.1597 0.2243 REM Highest difference peak 1.682, deepest hole -0.738, 1-sigma level 0.162 Q1 1 0.0780 0.1682 0.0457 11.00000 0.05 1.68 Q2 1 0.1807 0.0763 0.0706 11.00000 0.05 1.41 Q3 1 0.4503 0.3770 0.1156 11.00000 0.05 0.91 Q4 1 0.5608 0.4900 0.1454 11.00000 0.05 0.90 Q5 1 0.0602 0.0617 0.0531 11.00000 0.05 0.76 Q6 1 0.3660 -0.5011 0.4351 11.00000 0.05 0.75 ; _shelx_res_checksum 93161 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -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 0.13024(6) 0.12470(5) 0.05828(5) 0.0375(2) Uani 1 1 d . . . . . S10 S -0.46971(14) 0.31915(14) 0.43325(12) 0.0472(3) Uani 1 1 d . . . . . S11 S 0.31660(15) -0.46749(13) 0.40520(12) 0.0466(3) Uani 1 1 d . . . . . O1 O 0.0190(4) 0.1851(3) 0.1608(3) 0.0445(7) Uani 1 1 d . . . . . O1S O 0.3502(4) 0.3233(4) 0.1285(3) 0.0522(8) Uani 1 1 d . . . A 1 O2 O -0.2042(4) -0.0250(4) 0.0569(3) 0.0505(8) Uani 1 1 d . . . . . O19 O 0.1716(4) 0.0126(4) 0.1603(3) 0.0440(7) Uani 1 1 d . . . . . O20 O -0.0451(4) -0.2027(4) 0.0580(4) 0.0530(9) Uani 1 1 d . . . . . N3S N 0.5062(6) 0.5664(5) 0.1504(5) 0.0621(12) Uani 1 1 d . . . A 1 C2S C 0.3700(7) 0.4428(6) 0.1173(5) 0.0563(12) Uani 1 1 d . . . A 1 H2S H 0.281078 0.450513 0.081690 0.068 Uiso 1 1 calc R . . A 1 C3 C -0.1240(5) 0.1025(5) 0.1378(4) 0.0417(9) Uani 1 1 d . . . . . C4 C -0.2042(5) 0.1621(5) 0.2114(4) 0.0415(9) Uani 1 1 d . . . . . C4S C 0.6465(9) 0.5597(10) 0.2066(11) 0.099(3) Uani 1 1 d . . . A 1 H4SA H 0.715289 0.654392 0.272733 0.149 Uiso 1 1 calc GR . . A 1 H4SB H 0.698946 0.545693 0.147260 0.149 Uiso 1 1 calc GR . . A 1 H4SC H 0.618759 0.474518 0.237415 0.149 Uiso 1 1 calc GR . . A 1 C5 C -0.1222(6) 0.2785(5) 0.3219(5) 0.0475(10) Uani 1 1 d . . . . . H5 H -0.012859 0.322991 0.349170 0.057 Uiso 1 1 calc R . . . . C5S C 0.5171(10) 0.7080(7) 0.1401(8) 0.0794(19) Uani 1 1 d . . . A 1 H5SA H 0.413553 0.696044 0.107257 0.119 Uiso 1 1 calc GR . . A 1 H5SB H 0.577884 0.738190 0.086684 0.119 Uiso 1 1 calc GR . . A 1 H5SC H 0.567474 0.786203 0.219282 0.119 Uiso 1 1 calc GR . . A 1 C6 C -0.1980(6) 0.3294(5) 0.3916(5) 0.0466(10) Uani 1 1 d . . . . . H6 H -0.141436 0.405565 0.467756 0.056 Uiso 1 1 calc R . . . . C7 C -0.3584(6) 0.2684(5) 0.3495(5) 0.0430(9) Uani 1 1 d . . . . . C8 C -0.4418(6) 0.1547(6) 0.2382(5) 0.0459(10) Uani 1 1 d . . . . . H8 H -0.550613 0.114465 0.209201 0.055 Uiso 1 1 calc R . . . . C9 C -0.3660(6) 0.1011(6) 0.1707(5) 0.0468(10) Uani 1 1 d . . . . . H9 H -0.423286 0.022285 0.095896 0.056 Uiso 1 1 calc R . . . . C12 C 0.2550(6) -0.3583(5) 0.3329(5) 0.0442(10) Uani 1 1 d . . . . . C13 C 0.3219(6) -0.2009(5) 0.3759(5) 0.0497(11) Uani 1 1 d . . . . . H13 H 0.405135 -0.144868 0.448304 0.060 Uiso 1 1 calc R . . . . C14 C 0.2653(6) -0.1266(5) 0.3114(5) 0.0491(11) Uani 1 1 d . . . . . H14 H 0.312321 -0.019051 0.339153 0.059 Uiso 1 1 calc R . . . . C15 C 0.1420(6) -0.2069(5) 0.2080(4) 0.0425(9) Uani 1 1 d . . . . . C16 C 0.0738(6) -0.3656(5) 0.1661(5) 0.0466(10) Uani 1 1 d . . . . . H16 H -0.011610 -0.422023 0.095115 0.056 Uiso 1 1 calc R . . . . C17 C 0.1319(6) -0.4397(5) 0.2291(5) 0.0469(10) Uani 1 1 d . . . . . H17 H 0.086599 -0.547126 0.200537 0.056 Uiso 1 1 calc R . . . . C18 C 0.0837(6) -0.1266(5) 0.1360(4) 0.0427(10) Uani 1 1 d . . . . . O11S O 0.7388(13) 0.8803(17) 0.4314(15) 0.167(8) Uani 0.5 1 d . . P B -1 N13S N 1.0002(13) 0.9995(12) 0.5006(9) 0.152(7) Uani 0.5 1 d G . P B -1 C12S C 0.8544(13) 0.9618(13) 0.4129(10) 0.112(7) Uani 0.5 1 d DG . P B -1 H12S H 0.850926 0.998296 0.347026 0.135 Uiso 0.5 1 calc DR . P B -1 C14S C 1.0286(16) 1.0235(19) 0.6102(10) 0.086(4) Uani 0.5 1 d G . P B -1 H14A H 1.081830 1.132956 0.652719 0.129 Uiso 0.5 1 calc GR . P B -1 H14B H 1.094415 0.978721 0.635685 0.129 Uiso 0.5 1 calc GR . P B -1 H14C H 0.931934 0.977726 0.628611 0.129 Uiso 0.5 1 calc GR . P B -1 C15S C 1.1306(13) 1.1315(18) 0.4607(11) 0.090(5) Uani 0.5 1 d G . P B -1 H15A H 1.088376 1.117242 0.376195 0.135 Uiso 0.5 1 calc GR . P B -1 H15B H 1.225361 1.121070 0.472756 0.135 Uiso 0.5 1 calc GR . P B -1 H15C H 1.153528 1.232826 0.509982 0.135 Uiso 0.5 1 calc GR . P B -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 0.0399(3) 0.0304(3) 0.0372(4) 0.0106(2) 0.0093(3) 0.0129(2) S10 0.0484(6) 0.0497(6) 0.0505(7) 0.0182(5) 0.0147(6) 0.0285(5) S11 0.0573(7) 0.0425(6) 0.0476(7) 0.0167(5) 0.0147(6) 0.0299(5) O1 0.0431(16) 0.0355(14) 0.0502(19) 0.0085(13) 0.0117(16) 0.0181(13) O1S 0.0556(19) 0.0401(16) 0.047(2) 0.0126(14) 0.0115(17) 0.0113(14) O2 0.0469(17) 0.0429(16) 0.0432(19) 0.0012(14) 0.0130(17) 0.0105(13) O19 0.0457(16) 0.0353(14) 0.0496(19) 0.0163(14) 0.0098(16) 0.0185(13) O20 0.057(2) 0.0399(16) 0.051(2) 0.0200(16) 0.004(2) 0.0150(16) N3S 0.066(3) 0.053(2) 0.056(3) 0.016(2) 0.024(3) 0.015(2) C2S 0.060(3) 0.050(3) 0.055(3) 0.012(2) 0.022(3) 0.023(2) C3 0.046(2) 0.0372(19) 0.038(2) 0.0128(18) 0.009(2) 0.0168(18) C4 0.043(2) 0.040(2) 0.036(2) 0.0116(18) 0.009(2) 0.0169(18) C4S 0.075(4) 0.073(4) 0.133(8) 0.048(5) 0.026(5) 0.015(4) C5 0.043(2) 0.044(2) 0.046(3) 0.009(2) 0.011(2) 0.0161(19) C5S 0.095(5) 0.051(3) 0.089(5) 0.022(3) 0.048(4) 0.023(3) C6 0.043(2) 0.045(2) 0.039(3) 0.0065(19) 0.007(2) 0.015(2) C7 0.047(2) 0.043(2) 0.045(3) 0.018(2) 0.015(2) 0.0239(19) C8 0.040(2) 0.053(2) 0.040(3) 0.016(2) 0.005(2) 0.020(2) C9 0.045(2) 0.046(2) 0.044(3) 0.014(2) 0.006(2) 0.020(2) C12 0.056(3) 0.040(2) 0.050(3) 0.021(2) 0.023(2) 0.029(2) C13 0.054(3) 0.040(2) 0.047(3) 0.014(2) 0.007(3) 0.019(2) C14 0.059(3) 0.037(2) 0.046(3) 0.0133(19) 0.008(3) 0.021(2) C15 0.051(2) 0.036(2) 0.040(2) 0.0136(18) 0.013(2) 0.0200(19) C16 0.055(3) 0.038(2) 0.042(3) 0.0129(19) 0.011(2) 0.020(2) C17 0.060(3) 0.0377(19) 0.042(3) 0.0102(19) 0.015(3) 0.023(2) C18 0.052(3) 0.041(2) 0.040(3) 0.015(2) 0.015(2) 0.025(2) O11S 0.21(2) 0.134(14) 0.152(17) 0.053(13) 0.094(16) 0.049(14) N13S 0.118(10) 0.211(17) 0.063(7) -0.036(9) 0.001(8) 0.070(11) C12S 0.124(16) 0.074(10) 0.091(13) 0.031(9) 0.030(13) 0.001(10) C14S 0.089(10) 0.100(11) 0.089(12) 0.049(10) 0.038(10) 0.048(9) C15S 0.092(10) 0.114(12) 0.051(8) 0.032(8) 0.023(8) 0.031(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0050 0.0020 '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 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0090 0.0050 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0160 0.0090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1570 0.1680 '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 Cu1 86.86(10) . 2 ? O1 Cu1 O1S 100.64(14) . . ? O1 Cu1 O2 168.52(14) . 2 ? O1 Cu1 O20 87.95(16) . 2 ? O1S Cu1 Cu1 171.46(11) . 2 ? O2 Cu1 Cu1 81.81(11) 2 2 ? O2 Cu1 O1S 90.79(15) 2 . ? O2 Cu1 O20 92.47(17) 2 2 ? O19 Cu1 Cu1 85.61(11) . 2 ? O19 Cu1 O1 89.16(14) . . ? O19 Cu1 O1S 98.48(14) . . ? O19 Cu1 O2 88.10(15) . 2 ? O19 Cu1 O20 168.17(14) . 2 ? O20 Cu1 Cu1 82.78(11) 2 2 ? O20 Cu1 O1S 93.33(15) 2 . ? C7 S10 S11 105.50(18) . 2_556 ? C12 S11 S10 105.59(19) . 2_556 ? C3 O1 Cu1 119.8(3) . . ? C2S O1S Cu1 123.4(4) . . ? C3 O2 Cu1 125.8(3) . 2 ? C18 O19 Cu1 121.3(3) . . ? C18 O20 Cu1 123.8(3) . 2 ? C2S N3S C4S 118.9(5) . . ? C2S N3S C5S 121.6(6) . . ? C5S N3S C4S 119.4(6) . . ? O1S C2S N3S 125.8(6) . . ? O1S C2S H2S 117.1 . . ? N3S C2S H2S 117.1 . . ? O1 C3 C4 117.0(4) . . ? O2 C3 O1 125.5(4) . . ? O2 C3 C4 117.4(4) . . ? C5 C4 C3 121.3(4) . . ? C5 C4 C9 118.7(4) . . ? C9 C4 C3 120.1(4) . . ? N3S C4S H4SA 109.5 . . ? N3S C4S H4SB 109.5 . . ? N3S C4S H4SC 109.5 . . ? H4SA C4S H4SB 109.5 . . ? H4SA C4S H4SC 109.5 . . ? H4SB C4S H4SC 109.5 . . ? C4 C5 H5 119.6 . . ? C6 C5 C4 120.9(5) . . ? C6 C5 H5 119.6 . . ? N3S C5S H5SA 109.5 . . ? N3S C5S H5SB 109.5 . . ? N3S C5S H5SC 109.5 . . ? H5SA C5S H5SB 109.5 . . ? H5SA C5S H5SC 109.5 . . ? H5SB C5S H5SC 109.5 . . ? C5 C6 H6 120.1 . . ? C5 C6 C7 119.7(5) . . ? C7 C6 H6 120.1 . . ? C6 C7 S10 123.9(4) . . ? C8 C7 S10 115.8(3) . . ? C8 C7 C6 120.2(4) . . ? C7 C8 H8 120.1 . . ? C9 C8 C7 119.8(4) . . ? C9 C8 H8 120.1 . . ? C4 C9 H9 119.7 . . ? C8 C9 C4 120.7(5) . . ? C8 C9 H9 119.7 . . ? C13 C12 S11 123.9(4) . . ? C17 C12 S11 115.8(3) . . ? C17 C12 C13 120.3(4) . . ? C12 C13 H13 120.4 . . ? C12 C13 C14 119.1(5) . . ? C14 C13 H13 120.4 . . ? C13 C14 H14 119.5 . . ? C15 C14 C13 121.0(4) . . ? C15 C14 H14 119.5 . . ? C14 C15 C16 119.6(4) . . ? C14 C15 C18 121.0(4) . . ? C16 C15 C18 119.3(4) . . ? C15 C16 H16 120.2 . . ? C17 C16 C15 119.5(5) . . ? C17 C16 H16 120.2 . . ? C12 C17 C16 120.5(4) . . ? C12 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? O19 C18 C15 116.3(4) . . ? O20 C18 O19 125.9(4) . . ? O20 C18 C15 117.8(4) . . ? C12S N13S C15S 101.8 . . ? C14S N13S C12S 128.1 . . ? C14S N13S C15S 114.9 . . ? O11S C12S N13S 114.7 . . ? O11S C12S H12S 122.7 . . ? N13S C12S H12S 122.7 . . ? N13S C14S H14A 109.5 . . ? N13S C14S H14B 109.5 . . ? N13S C14S H14C 109.5 . . ? H14A C14S H14B 109.5 . . ? H14A C14S H14C 109.5 . . ? H14B C14S H14C 109.5 . . ? N13S C15S H15A 109.5 . . ? N13S C15S H15B 109.5 . . ? N13S C15S H15C 109.5 . . ? H15A C15S H15B 109.5 . . ? H15A C15S H15C 109.5 . . ? H15B C15S H15C 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 Cu1 2.6332(13) 2 ? Cu1 O1 1.964(3) . ? Cu1 O1S 2.146(4) . ? Cu1 O2 1.965(3) 2 ? Cu1 O19 1.951(3) . ? Cu1 O20 1.979(3) 2 ? S10 S11 2.033(2) 2_556 ? S10 C7 1.779(5) . ? S11 C12 1.778(4) . ? O1 C3 1.265(6) . ? O1S C2S 1.199(6) . ? O2 C3 1.262(6) . ? O19 C18 1.263(6) . ? O20 C18 1.248(6) . ? N3S C2S 1.339(8) . ? N3S C4S 1.470(10) . ? N3S C5S 1.442(8) . ? C2S H2S 0.9500 . ? C3 C4 1.488(6) . ? C4 C5 1.401(7) . ? C4 C9 1.410(7) . ? C4S H4SA 0.9800 . ? C4S H4SB 0.9800 . ? C4S H4SC 0.9800 . ? C5 H5 0.9500 . ? C5 C6 1.379(7) . ? C5S H5SA 0.9800 . ? C5S H5SB 0.9800 . ? C5S H5SC 0.9800 . ? C6 H6 0.9500 . ? C6 C7 1.398(7) . ? C7 C8 1.398(7) . ? C8 H8 0.9500 . ? C8 C9 1.376(7) . ? C9 H9 0.9500 . ? C12 C13 1.391(7) . ? C12 C17 1.381(8) . ? C13 H13 0.9500 . ? C13 C14 1.393(7) . ? C14 H14 0.9500 . ? C14 C15 1.378(8) . ? C15 C16 1.402(6) . ? C15 C18 1.507(6) . ? C16 H16 0.9500 . ? C16 C17 1.388(7) . ? C17 H17 0.9500 . ? O11S C12S 1.2162 . ? N13S C12S 1.4737 . ? N13S C14S 1.2441 . ? N13S C15S 1.6897 . ? C12S H12S 0.9500 . ? C14S H14A 0.9800 . ? C14S H14B 0.9800 . ? C14S H14C 0.9800 . ? C15S H15A 0.9800 . ? C15S H15B 0.9800 . ? C15S H15C 0.9800 . ? 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 O1 C3 O2 5.1(6) . . . . ? Cu1 O1 C3 C4 -174.1(3) . . . . ? Cu1 O1S C2S N3S -174.1(4) . . . . ? Cu1 O2 C3 O1 -2.7(7) 2 . . . ? Cu1 O2 C3 C4 176.5(3) 2 . . . ? Cu1 O19 C18 O20 -10.1(7) . . . . ? Cu1 O19 C18 C15 169.4(3) . . . . ? Cu1 O20 C18 O19 7.2(7) 2 . . . ? Cu1 O20 C18 C15 -172.4(3) 2 . . . ? S10 S11 C12 C13 9.1(5) 2_556 . . . ? S10 S11 C12 C17 -170.1(3) 2_556 . . . ? S10 C7 C8 C9 -175.7(4) . . . . ? S11 S10 C7 C6 -2.7(4) 2_556 . . . ? S11 S10 C7 C8 173.9(3) 2_556 . . . ? S11 C12 C13 C14 179.4(4) . . . . ? S11 C12 C17 C16 179.5(4) . . . . ? O1 C3 C4 C5 -18.7(6) . . . . ? O1 C3 C4 C9 161.5(4) . . . . ? O2 C3 C4 C5 162.1(4) . . . . ? O2 C3 C4 C9 -17.8(6) . . . . ? C3 C4 C5 C6 -177.7(4) . . . . ? C3 C4 C9 C8 179.7(4) . . . . ? C4 C5 C6 C7 -2.5(7) . . . . ? C4S N3S C2S O1S -0.5(10) . . . . ? C5 C4 C9 C8 -0.1(7) . . . . ? C5 C6 C7 S10 177.4(4) . . . . ? C5 C6 C7 C8 1.0(7) . . . . ? C5S N3S C2S O1S -175.9(6) . . . . ? C6 C7 C8 C9 1.0(7) . . . . ? C7 C8 C9 C4 -1.4(7) . . . . ? C9 C4 C5 C6 2.1(7) . . . . ? C12 C13 C14 C15 1.7(8) . . . . ? C13 C12 C17 C16 0.2(7) . . . . ? C13 C14 C15 C16 -0.9(8) . . . . ? C13 C14 C15 C18 -178.0(5) . . . . ? C14 C15 C16 C17 -0.3(7) . . . . ? C14 C15 C18 O19 14.5(7) . . . . ? C14 C15 C18 O20 -165.9(5) . . . . ? C15 C16 C17 C12 0.6(8) . . . . ? C16 C15 C18 O19 -162.6(4) . . . . ? C16 C15 C18 O20 16.9(7) . . . . ? C17 C12 C13 C14 -1.4(8) . . . . ? C18 C15 C16 C17 176.9(4) . . . . ? C14S N13S C12S O11S -36.5 . . . . ? C15S N13S C12S O11S -171.7 . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.543(5) 2 0.457(5)