#------------------------------------------------------------------------------ #$Date: 2020-10-06 11:32:58 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257502 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/53/7705344.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_7705344 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 '0.5(C68 H48 Cu4 N12 O20 S4)' _chemical_formula_sum 'C34 H24 Cu2 N6 O10 S2' _chemical_formula_weight 867.79 _space_group_crystal_system monoclinic _space_group_IT_number 11 _space_group_name_Hall '-P 2yb' _space_group_name_H-M_alt 'P 1 21/m 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _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 90 _cell_angle_beta 110.946(4) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.9361(4) _cell_length_b 24.6960(15) _cell_length_c 10.4597(4) _cell_measurement_reflns_used 13910 _cell_measurement_temperature 180 _cell_measurement_theta_max 28.9740 _cell_measurement_theta_min 2.2030 _cell_volume 2155.77(19) _computing_cell_refinement 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _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 'olex2.solve (Bourhis et al., 2015)' _diffrn_ambient_temperature 180 _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _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 -105.00 73.00 0.50 49.01 -- -15.60 45.00 179.33 356 2 \w -105.00 73.00 0.50 49.01 -- -15.60 45.00 162.84 356 3 \w -105.00 65.00 0.50 49.01 -- -15.60 45.00 169.46 340 4 \w -16.00 72.00 0.50 49.01 -- -15.60 45.00 58.13 176 5 \w -103.00 -32.00 0.50 49.01 -- -15.60 45.00 90.00 142 6 \w -20.00 68.00 0.50 49.01 -- -15.60 45.00 90.00 176 7 \w -49.00 35.00 0.50 49.01 -- -15.60 45.00 0.00 168 8 \w -105.00 -64.00 0.50 49.01 -- -15.60 45.00 150.00 82 9 \w -12.00 18.00 0.50 49.01 -- -15.60 45.00 150.00 60 10 \w 32.00 59.00 0.50 49.01 -- -15.60 45.00 150.00 54 11 \w -44.00 73.00 0.50 49.01 -- -15.60 45.00 -18.72 234 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB AFC10 (RCD3): fixed-chi single' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0264045000 _diffrn_orient_matrix_UB_12 0.0243941000 _diffrn_orient_matrix_UB_13 0.0209682000 _diffrn_orient_matrix_UB_21 -0.0541321000 _diffrn_orient_matrix_UB_22 -0.0149603000 _diffrn_orient_matrix_UB_23 0.0220395000 _diffrn_orient_matrix_UB_31 0.0598502000 _diffrn_orient_matrix_UB_32 -0.0027332000 _diffrn_orient_matrix_UB_33 0.0659093000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_unetI/netI 0.0277 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 3908 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.027 _diffrn_reflns_theta_max 25.027 _diffrn_reflns_theta_min 2.085 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.139 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.68654 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _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 1.337 _exptl_crystal_description block _exptl_crystal_F_000 880 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.01 _refine_diff_density_max 0.901 _refine_diff_density_min -0.540 _refine_diff_density_rms 0.121 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 281 _refine_ls_number_reflns 3908 _refine_ls_number_restraints 136 _refine_ls_restrained_S_all 1.055 _refine_ls_R_factor_all 0.1039 _refine_ls_R_factor_gt 0.0880 _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^)+(0.1664P)^2^+3.7496P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2652 _refine_ls_wR_factor_ref 0.2797 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2903 _reflns_number_total 3908 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02411b2.cif _cod_data_source_block najbc _cod_depositor_comments 'Adding full bibliography for 7705341--7705344.cif.' _cod_database_code 7705344 _shelx_shelxl_version_number 2018/1 _chemical_oxdiff_formula 'C38 N2 Cu2 O8 S4 ' _chemical_oxdiff_usercomment 'm 90 C' _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 0.983 _shelx_estimated_absorpt_t_min 0.847 _reflns_odcompleteness_completeness 99.95 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 24.97 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.689(8) 0.311(8) 2. Fixed Uiso At 1.2 times of: All C(H) groups 3. Restrained distances C3-O2 1.2 with sigma of 0.02 4. Rigid bond restraints O1, O102, C103 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 O101 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 O1, O2 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 O1, O2, C4 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 O101, O102, C103, C4A with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C4, C9, C5A with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 O1, O2, C4, C5, C6, C7, C8, C9 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C5, C6, C7 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 O101, O102, C103 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C17, C18, C19 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 5. Uiso/Uaniso restraints and constraints C5 \\sim C6 \\sim C7: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 Uanis(O2S) \\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C8A) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C9A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(O101) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C6) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(O1) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C5) = Uanis(C6) Uanis(C103) = Uanis(O102) = Uanis(O101) Uanis(O1) = Uanis(C3) = Uanis(O2) 6. Rigid body (RIGU) restrains O1, O2, C4 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 7. Others Fixed Sof: S8(0.5) S110(0.5) O1(0.5) O2(0.5) O101(0.5) O102(0.5) C3(0.5) C6(0.5) H6(0.5) C7(0.5) C8(0.5) H8(0.5) C9(0.5) H9(0.5) C4(0.5) C5(0.5) H5(0.5) C103(0.5) C4A(0.5) C5A(0.5) H5A(0.5) C6A(0.5) H6A(0.5) C7A(0.5) C8A(0.5) H8A(0.5) C9A(0.5) H9A(0.5) 8.a Aromatic/amide H refined with riding coordinates: C6(H6), C8(H8), C9(H9), C5(H5), C12(H12), C13(H13), C15(H15), C16(H16), C18(H18), C19(H19), C21(H21), C22(H22), C5A(H5A), C6A(H6A), C8A(H8A), C9A(H9A) 8.b Fitted hexagon refined as free rotating group: C6(C7,C8,C9,C4,C5), C4A(C5A,C6A,C7A,C8A,C9A) ; _shelx_res_file ; TITL najbc_a.res in P2(1)/m najbc.res created by SHELXL-2018/1 at 15:40:35 on 24-Aug-2020 REM Old TITL najbc_a.res in P2(1)/m REM SHELXT solution in P2(1)/m REM R1 0.376, Rweak 0.028, Alpha 0.151, Orientation as input REM Formula found by SHELXT: C14 N1S O101 Cu CELL 0.71073 8.9361 24.696 10.4597 90 110.946 90 ZERR 2 0.0004 0.0015 0.0004 0 0.004 0 LATT 1 SYMM -X,0.5+Y,-Z SFAC C H Cu N O S DISP C 0.0052 0.0023 16.0976 DISP Cu 0.2556 1.6827 7813.756 DISP H -0 0 0.63 DISP N 0.0094 0.0046 28.7478 DISP O 0.0162 0.0086 48.7782 DISP S 0.1566 0.1676 825.3281 UNIT 68 48 4 12 20 4 DFIX 1.2 C3 O2 DELU O1 O102 C103 DELU O101 DELU O1 O2 DELU O1 O2 C4 DELU O101 O102 C103 C4A DELU C4 C9 C5A DELU O1 O2 C4 C5 C6 > C9 DELU C5 C6 C7 DELU O101 O102 C103 DELU C17 C18 C19 SIMU C5 C6 C7 RIGU O1 O2 C4 ISOR O2S C7A C8A C6A C5A C4A C9A ISOR C6 C7 C8 C9 C4 C5 ISOR O101 O2 ISOR C6 ISOR O1 C3 O2 EADP C5 C6 EADP C103 O102 O101 EADP O1 C3 O2 L.S. 40 0 0 PLAN 70 SIZE 0.01 0.1 0.1 TEMP -93.15 LIST 6 ABIN fmap 2 53 acta REM REM REM WGHT 0.166400 3.749600 BASF 0.31083 FVAR 11.50088 CU01 3 1.043007 0.440653 0.375599 11.00000 0.03485 0.12386 = 0.01912 0.00998 -0.00525 -0.01586 PART 1 S8 6 0.642850 0.277819 0.898826 10.50000 0.36013 0.06536 = 0.24683 -0.00529 0.26619 -0.00643 PART 0 PART 2 S110 6 0.485703 0.271604 0.762720 10.50000 0.22227 0.07034 = 0.30270 -0.00209 0.22981 -0.00242 PART 0 PART 1 O1 5 0.921247 0.480083 0.657169 10.50000 0.05857 0.28163 = 0.03086 0.02959 -0.00709 -0.07396 PART 0 O1S 5 1.199484 0.443753 0.270469 11.00000 0.05754 0.18004 = 0.04572 0.01541 0.00157 -0.03065 PART 1 O2 5 0.872617 0.435055 0.471002 10.50000 0.05857 0.28163 = 0.03086 0.02959 -0.00709 -0.07396 PART 0 O2S 5 1.179010 0.359168 0.289213 11.00000 0.27399 0.16501 = 0.25239 -0.02338 0.18242 -0.07980 O3S 5 1.319898 0.390953 0.185461 11.00000 0.48596 0.16318 = 0.50509 0.00594 0.42615 0.01252 PART 2 O101 5 0.966482 0.467784 0.635569 10.50000 0.03705 0.10962 = 0.02924 0.01943 0.00803 -0.00006 O102 5 0.906555 0.409879 0.461931 10.50000 0.03705 0.10962 = 0.02924 0.01943 0.00803 -0.00006 PART 0 N1S 4 1.239876 0.397536 0.251791 11.00000 0.15545 0.11876 = 0.17330 -0.01433 0.11421 -0.03150 N11 4 0.857407 0.441663 0.195457 11.00000 0.03753 0.12266 = 0.03350 0.01116 0.00179 -0.02158 N20 4 1.233231 0.435785 0.552449 11.00000 0.03307 0.09953 = 0.02413 0.00720 -0.00660 -0.00522 PART 1 C3 1 0.876985 0.439802 0.587136 10.50000 0.05857 0.28163 = 0.03086 0.02959 -0.00709 -0.07396 AFIX 66 C6 1 0.634618 0.328327 0.657369 10.50000 0.10953 0.08982 = 0.12278 0.01990 0.09687 0.00941 AFIX 43 H6 2 0.543989 0.306885 0.608302 10.50000 -1.20000 AFIX 65 C7 1 0.707296 0.322482 0.798338 10.50000 0.16669 0.05015 = 0.12431 0.01305 0.11581 0.02129 C8 1 0.839899 0.353854 0.870132 10.50000 0.13181 0.10179 = 0.11780 0.02672 0.10443 0.02316 AFIX 43 H8 2 0.889572 0.349860 0.966478 10.50000 -1.20000 AFIX 65 C9 1 0.899824 0.391072 0.800957 10.50000 0.11644 0.10237 = 0.09154 0.04266 0.07555 0.02481 AFIX 43 H9 2 0.990452 0.412513 0.850025 10.50000 -1.20000 AFIX 65 C4 1 0.827146 0.396917 0.659988 10.50000 0.07896 0.15567 = 0.09299 0.05692 0.04025 0.00385 C5 1 0.694544 0.365545 0.588193 10.50000 0.10953 0.08982 = 0.12278 0.01990 0.09687 0.00941 AFIX 43 H5 2 0.644872 0.369540 0.491847 10.50000 -1.20000 AFIX 0 PART 0 C12 1 0.858235 0.474163 0.095044 11.00000 0.05302 0.17506 = 0.02567 0.01758 0.00247 -0.05113 AFIX 43 H12 2 0.948577 0.496836 0.108934 11.00000 -1.20000 AFIX 0 C13 1 0.735703 0.476276 -0.026118 11.00000 0.05150 0.14193 = 0.02290 0.01881 -0.00612 -0.03799 AFIX 43 H13 2 0.740376 0.502051 -0.092009 11.00000 -1.20000 AFIX 0 C14 1 0.603734 0.442751 -0.058973 11.00000 0.03813 0.08704 = 0.03090 0.00499 0.01119 -0.00113 C15 1 0.603804 0.409719 0.052316 11.00000 0.03668 0.14404 = 0.02573 0.02440 -0.00945 -0.03171 AFIX 43 H15 2 0.515863 0.386301 0.041852 11.00000 -1.20000 AFIX 0 C16 1 0.729312 0.411433 0.174014 11.00000 0.05679 0.13283 = 0.03223 0.02112 0.00263 -0.03057 AFIX 43 H16 2 0.724076 0.389673 0.247195 11.00000 -1.20000 AFIX 0 C17 1 0.476531 0.440593 -0.189348 11.00000 0.03145 0.08107 = 0.03205 0.00153 0.00648 0.00300 C18 1 0.470979 0.477334 -0.294999 11.00000 0.03988 0.16646 = 0.01662 0.02528 -0.01351 -0.03527 AFIX 43 H18 2 0.548483 0.505339 -0.278612 11.00000 -1.20000 AFIX 0 C19 1 0.351743 0.471991 -0.421974 11.00000 0.04673 0.18076 = 0.02757 0.02840 0.00148 -0.03673 AFIX 43 H19 2 0.353912 0.494956 -0.494155 11.00000 -1.20000 AFIX 0 C21 1 0.236776 0.403045 -0.351533 11.00000 0.06468 0.09457 = 0.04514 0.01170 -0.00897 -0.02805 AFIX 43 H21 2 0.153455 0.377002 -0.370002 11.00000 -1.20000 AFIX 0 C22 1 0.356035 0.403338 -0.221054 11.00000 0.05009 0.09851 = 0.01987 0.01573 -0.01577 -0.01785 AFIX 43 H22 2 0.353071 0.377581 -0.154541 11.00000 -1.20000 AFIX 0 PART 2 C103 1 0.899752 0.424700 0.569073 10.50000 0.03705 0.10962 = 0.02924 0.01943 0.00803 -0.00006 AFIX 66 C4A 1 0.786860 0.388392 0.619409 10.50000 0.06737 0.13642 = 0.09265 0.04066 0.05955 0.00174 C5A 1 0.647046 0.367300 0.524405 10.50000 0.08253 0.19377 = 0.14364 0.00707 0.02876 -0.06794 AFIX 43 H5A 2 0.615642 0.377171 0.430683 10.50000 -1.20000 AFIX 65 C6A 1 0.553181 0.331766 0.566532 10.50000 0.08410 0.12252 = 0.12679 -0.00894 0.05730 -0.01915 AFIX 43 H6A 2 0.457625 0.317351 0.501601 10.50000 -1.20000 AFIX 65 C7A 1 0.599129 0.317323 0.703663 10.50000 0.12926 0.08903 = 0.12675 -0.01657 0.10239 -0.01125 C8A 1 0.738942 0.338414 0.798668 10.50000 0.19858 0.09834 = 0.10947 0.01486 0.12437 -0.00173 AFIX 43 H8A 2 0.770345 0.328543 0.892390 10.50000 -1.20000 AFIX 65 C9A 1 0.832809 0.373949 0.756543 10.50000 0.16876 0.13858 = 0.07500 0.00415 0.07151 -0.04785 AFIX 43 H9A 2 0.928365 0.388364 0.821475 10.50000 -1.20000 AFIX 0 HKLF 5 REM najbc_a.res in P2(1)/m REM R1 = 0.0880 for 2903 Fo > 4sig(Fo) and 0.1039 for all 3908 data REM 281 parameters refined using 136 restraints END WGHT 0.1664 3.7495 REM Highest difference peak 0.901, deepest hole -0.540, 1-sigma level 0.121 Q1 1 0.9697 0.4361 0.4123 11.00000 0.05 0.90 Q2 1 1.0134 0.3631 0.3939 11.00000 0.05 0.86 Q3 1 1.1220 0.4387 0.3487 11.00000 0.05 0.83 Q4 1 1.1200 0.3449 0.1411 11.00000 0.05 0.68 Q5 1 1.3837 0.3996 0.2429 11.00000 0.05 0.67 Q6 1 1.2924 0.4393 0.6239 11.00000 0.05 0.60 Q7 1 1.2485 0.3812 0.0505 11.00000 0.05 0.56 Q8 1 0.5824 0.4403 -0.0121 11.00000 0.05 0.55 Q9 1 1.2333 0.3826 0.1674 11.00000 0.05 0.50 Q10 1 1.0347 0.4802 0.3760 11.00000 0.05 0.49 Q11 1 0.8093 0.4259 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-1 14 10 1.0353 -0.0886 0 14 10 0.7024 -0.1648 -6 15 10 0.3233 0.0551 -5 15 10 0.5818 -0.0088 -4 15 10 0.2434 -0.0557 -3 15 10 0.5533 -0.0486 -2 15 10 0.9293 -0.0775 -1 15 10 0.1754 -0.0483 0 15 10 0.5647 -0.0266 -5 16 10 -0.1325 -0.0002 -4 16 10 0.0358 0.0566 -3 16 10 -0.5604 0.1063 -2 16 10 -1.0181 0.1001 -1 16 10 -0.4484 -0.0088 -4 17 10 -0.1995 -0.0346 -3 17 10 -0.7339 -0.0630 -2 17 10 -0.7789 -0.0947 -8 0 11 0.9705 -0.2739 -7 0 11 0.8124 -0.5072 -6 0 11 1.7881 -0.7739 -5 0 11 -1.0604 -0.9800 -4 0 11 -0.4281 -1.1805 -3 0 11 0.5066 -1.3533 -2 0 11 0.4571 -1.4199 -1 0 11 1.2312 -1.3465 0 0 11 1.2457 -0.9582 1 0 11 -3.2558 -0.5539 -8 1 11 0.8906 -0.0236 -7 1 11 0.0464 0.0111 -6 1 11 1.0517 0.0157 -5 1 11 2.7317 0.0979 -4 1 11 3.0803 0.0313 -3 1 11 0.7973 0.0168 -2 1 11 -0.5521 0.0473 -1 1 11 -2.5327 -0.1619 0 1 11 -2.9149 -0.0597 1 1 11 -0.4511 -0.2810 -7 2 11 -1.0223 0.1478 -6 2 11 -1.7213 0.1950 -5 2 11 0.9815 0.4796 -4 2 11 0.5283 0.5210 -3 2 11 -0.4374 0.6797 -2 2 11 -0.3332 0.7236 -1 2 11 -1.3112 0.5990 0 2 11 -1.3094 0.4050 1 2 11 3.0499 0.1395 -7 3 11 -0.5484 -0.0567 -6 3 11 -0.0723 -0.0601 -5 3 11 -1.5772 -0.1328 -4 3 11 -1.9867 0.0128 -3 3 11 -0.7350 0.0613 -2 3 11 0.2833 0.0177 -1 3 11 0.9033 0.2039 0 3 11 1.9314 0.2575 1 3 11 0.0025 0.7456 -7 4 11 1.2793 0.1742 -6 4 11 1.3722 0.2775 -5 4 11 -0.7557 0.0461 -4 4 11 -0.6344 0.1723 -3 4 11 0.2447 0.0723 -2 4 11 -0.0123 0.0502 -1 4 11 1.3782 0.1478 0 4 11 1.4119 0.1499 1 4 11 -2.3344 0.1643 -7 5 11 0.8989 0.0627 -6 5 11 -0.7812 0.0788 -5 5 11 0.3317 0.1403 -4 5 11 0.5064 0.0098 -3 5 11 0.3393 -0.0408 -2 5 11 -0.0903 -0.0371 -1 5 11 1.1622 -0.1698 0 5 11 -0.4280 -0.2998 -7 6 11 -1.0153 -0.2125 -6 6 11 -0.6263 -0.2868 -5 6 11 0.4782 -0.1925 -4 6 11 0.4853 -0.4059 -3 6 11 -0.0157 -0.3706 -2 6 11 0.4096 -0.3490 -1 6 11 -1.1440 -0.3916 0 6 11 -1.3490 -0.4036 -7 7 11 -0.6318 -0.0194 -6 7 11 0.6652 -0.0175 -5 7 11 0.1164 -0.0766 -4 7 11 0.4965 -0.0502 -3 7 11 0.3404 -0.0411 -2 7 11 0.2279 -0.0127 -1 7 11 -2.2246 0.0377 0 7 11 -0.8589 0.1813 -7 8 11 0.2962 0.0552 -6 8 11 -0.1795 -0.0313 -5 8 11 -0.3354 -0.0104 -4 8 11 -0.1741 0.1552 -3 8 11 -0.0827 0.1435 -2 8 11 -0.5400 0.1042 -1 8 11 0.6039 0.1534 0 8 11 0.9866 0.3808 -6 9 11 0.0772 -0.1287 -5 9 11 0.1037 -0.0828 -4 9 11 -0.6596 0.0101 -3 9 11 -0.7867 0.0564 -2 9 11 -0.5497 0.0597 -1 9 11 1.7380 0.1367 0 9 11 1.3260 -0.0187 -6 10 11 0.5244 0.2747 -5 10 11 0.3965 0.2186 -4 10 11 -0.0270 0.1805 -3 10 11 -0.0436 0.2121 -2 10 11 0.2599 0.2758 -1 10 11 -0.0928 0.1710 -6 11 11 -0.5299 0.2514 -5 11 11 -0.3270 0.2387 -4 11 11 0.3175 0.0893 -3 11 11 0.6434 0.0386 -2 11 11 0.6961 -0.0138 -1 11 11 -0.3959 -0.2261 -5 12 11 -0.4688 -0.1868 -4 12 11 0.0941 -0.2320 -3 12 11 0.2502 -0.2821 -2 12 11 0.1428 -0.3636 -4 13 11 -0.0609 -0.1223 -3 13 11 -0.1811 -0.1381 -2 13 11 -0.5020 -0.1042 -6 0 12 1.9324 0.1239 -5 0 12 3.4773 0.3853 -4 0 12 1.2633 0.6905 -3 0 12 -0.3471 0.9762 -2 0 12 -0.1434 1.0443 -6 1 12 0.2816 -0.1863 -5 1 12 -0.2246 -0.0282 -4 1 12 -0.2202 -0.0238 -3 1 12 0.0546 -0.0196 -2 1 12 -0.4868 -0.0684 -6 2 12 -1.7001 0.0520 -5 2 12 -3.0707 -0.0932 -4 2 12 -0.9417 -0.2870 -3 2 12 0.3551 -0.4590 -2 2 12 0.5055 -0.5487 -6 3 12 -0.1700 0.4409 -5 3 12 0.2943 0.0734 -4 3 12 0.1463 0.0874 -3 3 12 0.0689 0.0370 -2 3 12 0.2287 -0.0223 -5 4 12 2.0657 -0.1448 -4 4 12 0.3220 -0.0600 -3 4 12 -0.2985 0.0083 -2 4 12 -1.1669 0.0909 -5 5 12 -0.1483 0.0343 -4 5 12 0.0628 -0.0205 -3 5 12 -0.1174 0.0099 -2 5 12 0.1073 0.0663 -5 6 12 -0.9511 0.1141 -4 6 12 0.0100 0.0427 -3 6 12 0.0778 -0.0035 -2 6 12 1.3137 -0.0452 -4 7 12 -0.3218 -0.0846 -3 7 12 -0.0523 -0.0571 0 0 0 0.0 0.0 ; _shelx_fab_checksum 34799 _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 1.278 _oxdiff_exptl_absorpt_empirical_full_min 0.756 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu01 Cu 1.04301(9) 0.44065(4) 0.37560(7) 0.0633(4) Uani 1 1 d . . . . . S8 S 0.6428(16) 0.2778(3) 0.8988(11) 0.181(5) Uani 0.5 1 d . . P A 1 S110 S 0.4857(13) 0.2716(2) 0.7627(13) 0.161(4) Uani 0.5 1 d . . P A 2 O1 O 0.9212(18) 0.4801(11) 0.6572(15) 0.130(7) Uani 0.5 1 d . U P A 1 O1S O 1.1995(8) 0.4438(4) 0.2705(7) 0.099(2) Uani 1 1 d . . . . . O2 O 0.873(2) 0.4351(9) 0.4710(16) 0.130(7) Uani 0.5 1 d D U P A 1 O2S O 1.1790(17) 0.3592(5) 0.2892(15) 0.206(6) Uani 1 1 d . U . . . O3S O 1.320(3) 0.3910(6) 0.185(2) 0.317(12) Uani 1 1 d . . . . . O101 O 0.9665(13) 0.4678(6) 0.6356(12) 0.060(2) Uani 0.5 1 d . U P A 2 O102 O 0.9066(16) 0.4099(5) 0.4619(14) 0.060(2) Uani 0.5 1 d . U P A 2 N1S N 1.2399(16) 0.3975(5) 0.2518(14) 0.134(4) Uani 1 1 d . . . . . N11 N 0.8574(7) 0.4417(3) 0.1955(6) 0.0675(18) Uani 1 1 d . . . . . N20 N 1.2332(6) 0.4358(2) 0.5524(5) 0.0568(15) Uani 1 1 d . . . . . C3 C 0.877(3) 0.4398(16) 0.587(2) 0.130(7) Uani 0.5 1 d D U P A 1 C6 C 0.6346(18) 0.3283(6) 0.6574(16) 0.092(4) Uani 0.5 1 d . U P A 1 H6 H 0.543989 0.306885 0.608302 0.111 Uiso 0.5 1 calc R . P A 1 C7 C 0.707(2) 0.3225(6) 0.7983(17) 0.096(6) Uani 0.5 1 d G U P A 1 C8 C 0.840(2) 0.3539(7) 0.8701(14) 0.101(5) Uani 0.5 1 d G U P A 1 H8 H 0.889572 0.349860 0.966478 0.121 Uiso 0.5 1 calc R . P A 1 C9 C 0.900(2) 0.3911(7) 0.8010(17) 0.093(6) Uani 0.5 1 d G U P A 1 H9 H 0.990452 0.412513 0.850025 0.112 Uiso 0.5 1 calc R . P A 1 C4 C 0.827(2) 0.3969(7) 0.6600(17) 0.107(9) Uani 0.5 1 d G U P A 1 C5 C 0.695(2) 0.3655(7) 0.5882(14) 0.092(4) Uani 0.5 1 d G U P A 1 H5 H 0.644872 0.369540 0.491847 0.111 Uiso 0.5 1 calc R . P A 1 C12 C 0.8582(9) 0.4742(4) 0.0950(7) 0.088(3) Uani 1 1 d . . . . . H12 H 0.948577 0.496836 0.108934 0.105 Uiso 1 1 calc R . . . . C13 C 0.7357(9) 0.4763(4) -0.0261(6) 0.077(3) Uani 1 1 d . . . . . H13 H 0.740376 0.502051 -0.092009 0.093 Uiso 1 1 calc R . . . . C14 C 0.6037(8) 0.4428(3) -0.0590(7) 0.0523(16) Uani 1 1 d . . . . . C15 C 0.6038(8) 0.4097(4) 0.0523(6) 0.074(2) Uani 1 1 d . . . . . H15 H 0.515863 0.386301 0.041852 0.089 Uiso 1 1 calc R . . . . C16 C 0.7293(9) 0.4114(4) 0.1740(7) 0.078(2) Uani 1 1 d . . . . . H16 H 0.724076 0.389673 0.247195 0.093 Uiso 1 1 calc R . . . . C17 C 0.4765(7) 0.4406(3) -0.1893(6) 0.0495(15) Uani 1 1 d . U . . . C18 C 0.4710(8) 0.4773(4) -0.2950(6) 0.081(3) Uani 1 1 d . U . . . H18 H 0.548483 0.505339 -0.278612 0.097 Uiso 1 1 calc R . . . . C19 C 0.3517(9) 0.4720(4) -0.4220(7) 0.088(3) Uani 1 1 d . U . . . H19 H 0.353912 0.494956 -0.494155 0.106 Uiso 1 1 calc R . . . . C21 C 0.2368(10) 0.4030(3) -0.3515(8) 0.076(2) Uani 1 1 d . . . . . H21 H 0.153455 0.377002 -0.370002 0.091 Uiso 1 1 calc R . . . . C22 C 0.3560(8) 0.4033(3) -0.2211(6) 0.064(2) Uani 1 1 d . . . . . H22 H 0.353071 0.377581 -0.154541 0.077 Uiso 1 1 calc R . . . . C103 C 0.900(2) 0.4247(9) 0.569(2) 0.060(2) Uani 0.5 1 d . U P A 2 C4A C 0.787(2) 0.3884(9) 0.6194(17) 0.090(7) Uani 0.5 1 d . U P A 2 C5A C 0.647(2) 0.3673(10) 0.5244(15) 0.143(12) Uani 0.5 1 d G U P A 2 H5A H 0.615642 0.377171 0.430683 0.172 Uiso 0.5 1 calc R . P A 2 C6A C 0.5532(18) 0.3318(8) 0.5665(19) 0.106(7) Uani 0.5 1 d G U P A 2 H6A H 0.457625 0.317351 0.501601 0.127 Uiso 0.5 1 calc R . P A 2 C7A C 0.599(2) 0.3173(6) 0.704(2) 0.100(7) Uani 0.5 1 d G U P A 2 C8A C 0.739(3) 0.3384(8) 0.7987(15) 0.117(11) Uani 0.5 1 d G U P A 2 H8A H 0.770345 0.328543 0.892390 0.140 Uiso 0.5 1 calc R . P A 2 C9A C 0.833(2) 0.3739(9) 0.7565(16) 0.120(10) Uani 0.5 1 d G U P A 2 H9A H 0.928365 0.388364 0.821475 0.144 Uiso 0.5 1 calc R . P A 2 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 Cu01 0.0349(5) 0.1239(9) 0.0191(5) 0.0100(4) -0.0053(3) -0.0159(4) S8 0.360(14) 0.065(3) 0.247(10) -0.005(5) 0.266(11) -0.006(6) S110 0.222(9) 0.070(3) 0.303(12) -0.002(5) 0.230(9) -0.002(4) O1 0.059(7) 0.282(19) 0.031(5) 0.030(8) -0.007(5) -0.074(9) O1S 0.058(4) 0.180(8) 0.046(3) 0.015(4) 0.002(3) -0.031(4) O2 0.059(7) 0.282(19) 0.031(5) 0.030(8) -0.007(5) -0.074(9) O2S 0.274(15) 0.165(9) 0.252(14) -0.023(10) 0.182(13) -0.080(10) O3S 0.49(3) 0.163(11) 0.51(3) 0.006(14) 0.43(3) 0.013(14) O101 0.037(4) 0.110(5) 0.029(4) 0.019(3) 0.008(3) 0.000(3) O102 0.037(4) 0.110(5) 0.029(4) 0.019(3) 0.008(3) 0.000(3) N1S 0.155(10) 0.119(8) 0.173(12) -0.014(8) 0.114(9) -0.031(7) N11 0.038(3) 0.123(5) 0.033(3) 0.011(3) 0.002(2) -0.022(3) N20 0.033(3) 0.100(4) 0.024(2) 0.007(3) -0.007(2) -0.005(3) C3 0.059(7) 0.282(19) 0.031(5) 0.030(8) -0.007(5) -0.074(9) C6 0.110(11) 0.090(9) 0.123(10) 0.020(8) 0.097(9) 0.009(8) C7 0.167(17) 0.050(10) 0.124(12) 0.013(9) 0.116(12) 0.021(10) C8 0.132(16) 0.102(15) 0.118(13) 0.027(11) 0.104(11) 0.023(11) C9 0.116(14) 0.102(15) 0.092(11) 0.043(11) 0.076(10) 0.025(10) C4 0.079(15) 0.16(2) 0.093(13) 0.057(14) 0.040(11) 0.004(12) C5 0.110(11) 0.090(9) 0.123(10) 0.020(8) 0.097(9) 0.009(8) C12 0.053(4) 0.175(9) 0.026(3) 0.018(4) 0.002(3) -0.051(5) C13 0.051(4) 0.142(7) 0.023(3) 0.019(4) -0.006(3) -0.038(4) C14 0.038(3) 0.087(5) 0.031(3) 0.005(3) 0.011(3) -0.001(3) C15 0.037(3) 0.144(7) 0.026(3) 0.024(4) -0.009(3) -0.032(4) C16 0.057(4) 0.133(7) 0.032(3) 0.021(4) 0.003(3) -0.031(5) C17 0.031(3) 0.081(5) 0.032(3) 0.002(3) 0.006(3) 0.003(3) C18 0.040(4) 0.166(8) 0.017(3) 0.025(4) -0.014(2) -0.035(4) C19 0.047(4) 0.181(9) 0.028(3) 0.028(5) 0.001(3) -0.037(5) C21 0.065(5) 0.095(6) 0.045(4) 0.012(4) -0.009(3) -0.028(4) C22 0.050(4) 0.099(5) 0.020(3) 0.016(3) -0.016(3) -0.018(4) C103 0.037(4) 0.110(5) 0.029(4) 0.019(3) 0.008(3) 0.000(3) C4A 0.067(13) 0.136(17) 0.093(14) 0.041(12) 0.060(12) 0.002(11) C5A 0.083(16) 0.19(3) 0.14(2) 0.01(2) 0.029(16) -0.068(18) C6A 0.084(14) 0.123(17) 0.127(19) -0.009(15) 0.057(14) -0.019(13) C7A 0.13(2) 0.089(14) 0.13(2) -0.017(14) 0.102(18) -0.011(13) C8A 0.20(3) 0.098(18) 0.109(19) 0.015(16) 0.12(2) 0.00(2) C9A 0.17(3) 0.14(2) 0.075(15) 0.004(14) 0.072(17) -0.048(18) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0052 0.0023 '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 0.2556 1.6827 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0094 0.0046 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0162 0.0086 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1566 0.1676 '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 Cu01 O1S 72.4(6) 3_766 . ? O1 Cu01 O2 109.1(8) 3_766 . ? O1 Cu01 O101 15.1(5) 3_766 3_766 ? O1S Cu01 O2 176.2(5) . . ? O1S Cu01 O101 87.5(4) . 3_766 ? O2 Cu01 O101 94.0(6) . 3_766 ? O102 Cu01 O1S 158.7(5) . . ? O102 Cu01 N11 89.8(4) . . ? O102 Cu01 N20 90.8(4) . . ? N11 Cu01 O1 87.5(4) . 3_766 ? N11 Cu01 O1S 89.4(2) . . ? N11 Cu01 O2 87.2(5) . . ? N11 Cu01 O101 86.4(4) . 3_766 ? N11 Cu01 N20 176.8(3) . . ? N20 Cu01 O1 94.6(4) . 3_766 ? N20 Cu01 O1S 88.9(2) . . ? N20 Cu01 O2 94.4(5) . . ? N20 Cu01 O101 96.3(4) . 3_766 ? S8 S8 C7 128.9(6) 4_565 . ? S110 S110 C7A 129.6(6) 4_565 . ? C3 O1 Cu01 136.4(15) . 3_766 ? N1S O1S Cu01 110.0(7) . . ? C3 O2 Cu01 134.7(15) . . ? C103 O102 Cu01 124.9(13) . . ? O2S N1S O1S 118.5(12) . . ? O3S N1S O1S 119.8(12) . . ? O3S N1S O2S 121.1(14) . . ? C12 N11 Cu01 120.8(5) . . ? C16 N11 Cu01 121.8(5) . . ? C16 N11 C12 117.4(6) . . ? C19 N20 Cu01 119.4(5) 1_656 . ? C21 N20 Cu01 122.2(5) 1_656 . ? C21 N20 C19 118.0(6) 1_656 1_656 ? O1 C3 C4 111.9(16) . . ? O2 C3 O1 125(3) . . ? O2 C3 C4 123(3) . . ? C7 C6 C5 120.0 . . ? C6 C7 S8 124.8(10) . . ? C8 C7 S8 115.2(10) . . ? C8 C7 C6 120.0 . . ? C7 C8 C9 120.0 . . ? C4 C9 C8 120.0 . . ? C9 C4 C3 120.9(14) . . ? C9 C4 C5 120.0 . . ? C5 C4 C3 118.8(14) . . ? C4 C5 C6 120.0 . . ? N11 C12 C13 122.4(7) . . ? C12 C13 C14 123.1(7) . . ? C13 C14 C15 113.0(6) . . ? C13 C14 C17 125.2(6) . . ? C15 C14 C17 121.8(6) . . ? C16 C15 C14 120.4(6) . . ? N11 C16 C15 123.5(6) . . ? C18 C17 C14 120.9(6) . . ? C22 C17 C14 123.1(6) . . ? C22 C17 C18 116.0(6) . . ? C19 C18 C17 119.3(7) . . ? N20 C19 C18 122.7(6) 1_454 . ? N20 C21 C22 123.9(7) 1_454 . ? C17 C22 C21 120.0(6) . . ? O101 C103 C4A 121.0(14) . . ? O102 C103 O101 125.8(17) . . ? O102 C103 C4A 113.0(18) . . ? C5A C4A C103 119.6(13) . . ? C5A C4A C9A 120.0 . . ? C9A C4A C103 120.2(13) . . ? C4A C5A C6A 120.0 . . ? C7A C6A C5A 120.0 . . ? C6A C7A S110 122.0(12) . . ? C6A C7A C8A 120.0 . . ? C8A C7A S110 118.0(12) . . ? C7A C8A C9A 120.0 . . ? C8A C9A C4A 120.0 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu01 O1 2.03(2) 3_766 ? Cu01 O1S 2.066(7) . ? Cu01 O2 2.102(16) . ? Cu01 O101 2.264(14) 3_766 ? Cu01 O102 1.915(13) . ? Cu01 N11 2.017(6) . ? Cu01 N20 2.019(5) . ? S8 S8 1.374(13) 4_565 ? S8 C7 1.757(11) . ? S110 S110 1.067(12) 4_565 ? S110 C7A 1.770(12) . ? O1 C3 1.21(4) . ? O1S N1S 1.234(12) . ? O2 C3 1.207(16) . ? O2S N1S 1.224(13) . ? O3S N1S 1.172(15) . ? O101 C103 1.29(2) . ? O102 C103 1.201(18) . ? N11 C12 1.324(9) . ? N11 C16 1.317(9) . ? N20 C19 1.338(10) 1_656 ? N20 C21 1.281(9) 1_656 ? C3 C4 1.46(3) . ? C6 C7 1.3900 . ? C6 C5 1.3900 . ? C7 C8 1.3900 . ? C8 C9 1.3900 . ? C9 C4 1.3900 . ? C4 C5 1.3900 . ? C12 C13 1.347(10) . ? C13 C14 1.380(10) . ? C14 C15 1.421(9) . ? C14 C17 1.430(10) . ? C15 C16 1.364(9) . ? C17 C18 1.417(9) . ? C17 C22 1.364(9) . ? C18 C19 1.380(9) . ? C21 C22 1.399(9) . ? C103 C4A 1.57(2) . ? C4A C5A 1.3900 . ? C4A C9A 1.3900 . ? C5A C6A 1.3900 . ? C6A C7A 1.3900 . ? C7A C8A 1.3900 . ? C8A C9A 1.3900 . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.689(8) 2 0.311(8) 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 -0.853 0.250 -0.111 270.8 61.1 '2 DMF' 2 -0.657 0.750 -0.087 270.8 61.6 '2 DMF'