#------------------------------------------------------------------------------ #$Date: 2026-05-12 04:08:45 +0100 (Tue, 12 May 2026) $ #$Revision: 305932 $ #$URL: svn://www.crystallography.net/cod/cif/3/00/05/3000592.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_3000592 loop_ _publ_author_name 'Shin-ichiro Noro' _publ_section_title ; Structural Characterization of a Desolvated Flexible Porous Coordination Polymer using MicroED ; _journal_name_full 'Crystal Growth & Design' _journal_page_first 438 _journal_volume 26 _journal_year 2026 _chemical_formula_moiety 'C27 H28 Cu F3 N4 O3 S, C F3 O3 S' _chemical_formula_sum 'C28 H28 Cu F6 N4 O6 S2' _chemical_formula_weight 758.22 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2025-02-26 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _cell_angle_alpha 90 _cell_angle_beta 96.22(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.810(3) _cell_length_b 17.268(4) _cell_length_c 10.929(4) _cell_measurement_reflns_used 4154 _cell_measurement_temperature 79 _cell_measurement_theta_max 0.7472625083390779 _cell_measurement_theta_min 0.10645600954679486 _cell_volume 1652.9(9) _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 79 _diffrn_detector 'Falcon 3 direct electron camera (integration mode)' _diffrn_detector_type CMOS _diffrn_measured_fraction_theta_full 0.956 _diffrn_measured_fraction_theta_max 0.956 _diffrn_measurement_device_type 'Transmission electron microscope' _diffrn_measurement_method 'continuous rotation electron diffraction (MicroED)' _diffrn_radiation_probe electron _diffrn_radiation_type electron _diffrn_radiation_wavelength 0.02508 _diffrn_reflns_av_R_equivalents 0.2271 _diffrn_reflns_av_unetI/netI 0.2285 _diffrn_reflns_Laue_measured_fraction_full 0.956 _diffrn_reflns_Laue_measured_fraction_max 0.956 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 37133 _diffrn_reflns_point_group_measured_fraction_full 0.949 _diffrn_reflns_point_group_measured_fraction_max 0.949 _diffrn_reflns_theta_full 0.781 _diffrn_reflns_theta_max 0.781 _diffrn_reflns_theta_min 0.106 _diffrn_source 'Talos Arctica Field Emission Gun' _exptl_absorpt_coefficient_mu 0.000 _exptl_crystal_colour blue _exptl_crystal_colour_primary blue _exptl_crystal_density_diffrn 1.523 _exptl_crystal_description powder _exptl_crystal_F_000 265 _refine_diff_density_max 0.085 _refine_diff_density_min -0.096 _refine_diff_density_rms 0.025 _refine_ls_abs_structure_details ; All f" are zero, so absolute structure could not be determined ; _refine_ls_extinction_coef 597(24) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 0.920 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 498 _refine_ls_number_reflns 4224 _refine_ls_number_restraints 340 _refine_ls_restrained_S_all 0.904 _refine_ls_R_factor_all 0.1441 _refine_ls_R_factor_gt 0.0875 _refine_ls_shift/su_max 0.071 _refine_ls_shift/su_mean 0.015 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1051P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2002 _refine_ls_wR_factor_ref 0.2169 _reflns_Friedel_coverage 0.910 _reflns_Friedel_fraction_full 0.942 _reflns_Friedel_fraction_max 0.942 _reflns_number_gt 1971 _reflns_number_total 4224 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file CuCF3SO32bpp2_response_250227.cif _cod_data_source_block '[Cu(CF3SO3)2(bpp)2]' _cod_depositor_comments 'Releasing structure 3000592 into public domain as published material.' _cod_original_cell_volume 1652.9(6) _cod_database_code 3000592 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups 2. Restrained distances C6-C7 = C7-C8 1.52 with sigma of 0.002 C27-F1 \\sim C27-F2 \\sim C27-F3 \\sim C28-F4 \\sim C28-F5 \\sim C28-F6 with sigma of 0.02 F1-F2 \\sim F2-F3 \\sim F1-F3 \\sim F4-F5 \\sim F5-F6 \\sim F4-F6 with sigma of 0.02 N2-C11 \\sim N2A-C11A with sigma of 0.02 N2-C13 \\sim N2A-C13A with sigma of 0.02 C6-C7 \\sim C6-C7A with sigma of 0.02 C7-C8 \\sim C7A-C8A with sigma of 0.02 C9-C10 \\sim C9A-C10A with sigma of 0.02 C9-C12 \\sim C9A-C12A with sigma of 0.02 C9-C8 \\sim C9A-C8A with sigma of 0.02 C10-C11 \\sim C10A-C11A with sigma of 0.02 C12-C13 \\sim C12A-C13A with sigma of 0.02 N2-C10 \\sim N2A-C10A with sigma of 0.04 N2-C12 \\sim N2A-C12A with sigma of 0.04 C6-C8 \\sim C6-C8A with sigma of 0.04 C7-C9 \\sim C7A-C9A with sigma of 0.04 C9-C11 \\sim C9A-C11A with sigma of 0.04 C9-C13 \\sim C9A-C13A with sigma of 0.04 C10-C12 \\sim C10A-C12A with sigma of 0.04 C10-C8 \\sim C10A-C8A with sigma of 0.04 C11-C13 \\sim C11A-C13A with sigma of 0.04 C12-C8 \\sim C12A-C8A with sigma of 0.04 3. Restrained planarity C9, C10, C11, C12, C13, N2, C8 with sigma of 0.1 C8, C9, C10, C11, C12, C13, N2 with sigma of 0.1 C8A, C9A, C10A, C11A, C12A, C13A, N2A with sigma of 0.1 4. Uiso/Uaniso restraints and constraints F1 \\sim F2 \\sim F2 \\sim F3 \\sim F3 \\sim F1 \\sim F1 \\sim C27 \\sim F2 \\sim C27 \\sim F3 \\sim C27: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A O1 \\sim O2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A N4 \\sim C26 \\sim N4 \\sim C24: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A C7A \\sim C6 \\sim C7A \\sim C8A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A C9A \\sim C12A \\sim C9A \\sim C10A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A N2A \\sim C13A \\sim N2A \\sim C11A \\sim N2 \\sim C13 \\sim N2 \\sim C11: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A Uanis(F1) \\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(N2A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 5. Rigid body (RIGU) restrains C7, C7A, C8, C8A, C9, C9A, C10, C10A, C11, C11A, C12, C12A, C13, C13A, N2, N2A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 6. Others Sof(H6BC)=Sof(H6BD)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)= Sof(C9A)=Sof(C10A)=Sof(H10A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13A)=Sof(C11A)= Sof(H11A)=Sof(N2A)=1-FVAR(1) Sof(N2)=Sof(H6AA)=Sof(H6AB)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C9)=Sof(C10)= Sof(H10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=Sof(C8)= Sof(H8A)=Sof(H8B)=FVAR(1) 7.a Secondary CH2 refined with riding coordinates: C6(H6AA,H6AB), C6(H6BC,H6BD), C7(H7A,H7B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C8(H8A,H8B), C7A(H7AA,H7AB), C8A(H8AA,H8AB) 7.b Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18), C23(H23), C24(H24), C25(H25), C26(H26), C10A(H10A), C12A(H12A), C13A(H13A), C11A(H11A) ; _shelx_res_file ; TITL norocf3_a.res in P2(1) norocf3.res created by SHELXL-2018/3 at 17:37:51 on 26-Feb-2025 REM Old TITL norocf3_a.res in P2(1) REM SHELXT solution in P2(1): R1 0.250, Rweak 0.228, Alpha 0.033 REM 0.738 for 8 systematic absences, Orientation as input REM Flack x = -3.681 ( 2.200 ) from 677 Parsons' quotients REM Formula found by SHELXT: C30 C25 F C19 CELL 0.02508 8.8099 17.2683 10.9291 90 96.224 90 ZERR 2 0 0 0 0 0 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C 0.136 0.373 0.548 3.281 1.227 13.046 0.597 41.02 0 0 0 0 0.75 12.011 SFAC N 0.137 0.329 0.534 2.673 1.086 10.316 0.455 32.763 0 0 0 0 0.71 14.007 SFAC Cu 0.593 0.368 1.834 2.896 1.808 15.633 1.359 70.68 0 0 0 0 1.12 63.546 SFAC F 0.152 0.289 0.519 2.062 0.822 7.263 0.308 22.026 0 0 0 0 0.64 18.998 SFAC O 0.143 0.305 0.51 2.268 0.937 8.262 0.392 25.665 0 0 0 0 0.63 15.999 SFAC S 0.348 0.365 0.916 2.891 2.507 13.052 1.388 40.185 0 0 0 0 1.03 32.066 SFAC H 0.037 0.561 0.127 3.791 0.236 13.556 0.129 37.723 0 0 0 0 0.32 1.008 UNIT 56 8 2 12 12 4 56 SADI C27 F1 C27 F2 C27 F3 C28 F4 C28 F5 C28 F6 SADI F1 F2 F2 F3 F1 F3 F4 F5 F5 F6 F4 F6 FLAT C9 C10 C11 C12 C13 N2 C8 DFIX 1.52 0.002 C6 C7 C7 C8 FLAT C8 C9 C10 C11 C12 C13 N2 FLAT C8A C9A C10A C11A C12A C13A N2A SADI N2 C11 N2A C11A SADI N2 C13 N2A C13A SADI C6 C7 C6 C7A SADI C7 C8 C7A C8A SADI C9 C10 C9A C10A SADI C9 C12 C9A C12A SADI C9 C8 C9A C8A SADI C10 C11 C10A C11A SADI C12 C13 C12A C13A SADI 0.04 N2 C10 N2A C10A SADI 0.04 N2 C12 N2A C12A SADI 0.04 C6 C8 C6 C8A SADI 0.04 C7 C9 C7A C9A SADI 0.04 C9 C11 C9A C11A SADI 0.04 C9 C13 C9A C13A SADI 0.04 C10 C12 C10A C12A SADI 0.04 C10 C8 C10A C8A SADI 0.04 C11 C13 C11A C13A SADI 0.04 C12 C8 C12A C8A RIGU C7 C7A C8 C8A C9 C9A C10 C10A C11 C11A C12 C12A C13 C13A N2 N2A SIMU F1 F2 F2 F3 F3 F1 F1 C27 F2 C27 F3 C27 ISOR F1 C7A C27 N2 C7 C11 C12 N4 N2A SIMU O1 O2 SIMU N4 C26 N4 C24 SIMU C7A C6 C7A C8A SIMU C9A C12A C9A C10A SIMU N2A C13A N2A C11A N2 C13 N2 C11 L.S. 10 0 0 PLAN 20 TEMP -194.15 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.105100 EXTI 597.357910 FVAR 1.78957 0.54378 CU1 3 0.514526 0.155038 0.241263 11.00000 0.05829 0.08126 = 0.05151 -0.00970 -0.00571 -0.00437 S1 6 0.243098 0.077447 0.465227 11.00000 0.08743 0.09159 = 0.07728 -0.00123 -0.00484 -0.02703 S2 6 0.684884 0.242025 -0.032269 11.00000 0.06940 0.08509 = 0.04868 -0.00596 -0.00120 0.00505 PART 1 F1 4 0.288409 -0.066535 0.436619 11.00000 0.32520 0.04129 = 0.42454 -0.03369 0.09996 -0.03453 F2 4 0.209161 -0.040016 0.603531 11.00000 0.43112 0.09123 = 0.30820 0.04722 0.21779 -0.04832 F3 4 0.434425 -0.009627 0.572228 11.00000 0.20448 0.23016 = 0.16797 0.00078 -0.04554 0.09023 PART 0 F4 4 0.792012 0.377219 -0.087345 11.00000 0.09169 0.32905 = 0.40296 0.29296 -0.03704 -0.07695 F5 4 0.702026 0.372904 0.080387 11.00000 0.13043 0.14893 = 0.19825 -0.01639 -0.02632 -0.02216 F6 4 0.915394 0.318930 0.063321 11.00000 0.07924 0.15679 = 0.13481 0.02896 -0.01901 -0.03454 O1 5 0.095894 0.072854 0.423975 11.00000 0.15172 0.62555 = 0.20143 -0.21327 0.04562 -0.10574 O2 5 0.267505 0.122860 0.572787 11.00000 0.20278 0.13795 = 0.15212 0.02536 -0.01795 -0.05302 O3 5 0.359836 0.096282 0.380977 11.00000 0.13735 0.12553 = 0.07243 -0.01495 -0.00018 -0.02875 O4 5 0.777173 0.207735 -0.096636 11.00000 0.07683 0.21166 = 0.10592 -0.03930 -0.06064 0.02997 O5 5 0.680955 0.205126 0.078979 11.00000 0.09120 0.06221 = 0.07181 -0.00389 -0.04625 -0.00006 O6 5 0.538861 0.263556 -0.097673 11.00000 0.07318 0.09406 = 0.06460 -0.02067 0.00789 0.02295 N1 2 0.613207 0.053502 0.232577 11.00000 0.05838 0.07634 = 0.06769 -0.02311 -0.00694 -0.01574 PART 1 N2 2 1.308029 -0.311187 0.632934 21.00000 0.06446 0.09344 = 0.06388 -0.00687 -0.01057 0.02266 PART 0 N3 2 0.358014 0.124713 0.101651 11.00000 0.04581 0.09088 = 0.07343 -0.02343 -0.00194 -0.00386 N4 2 -0.407416 -0.242404 -0.254253 11.00000 0.10834 0.11015 = 0.00759 -0.00359 0.00130 0.01178 C1 1 0.762343 0.040886 0.217905 11.00000 0.10893 0.10275 = 0.05145 -0.01668 0.00321 -0.01064 AFIX 43 H1 7 0.822790 0.086561 0.222115 11.00000 -1.20000 AFIX 0 C2 1 0.843995 -0.026841 0.197709 11.00000 0.07821 0.09329 = 0.12038 0.01698 -0.02192 0.01142 AFIX 43 H2 7 0.947353 -0.027037 0.180368 11.00000 -1.20000 AFIX 0 C3 1 0.757738 -0.093483 0.205758 11.00000 0.04847 0.09220 = 0.09678 0.00635 -0.03466 -0.01193 C4 1 0.601791 -0.085097 0.220966 11.00000 0.10193 0.06628 = 0.09135 -0.00658 -0.02169 -0.02353 AFIX 43 H4 7 0.538598 -0.129690 0.220650 11.00000 -1.20000 AFIX 0 C5 1 0.540784 -0.013820 0.236094 11.00000 0.07620 0.07276 = 0.09073 -0.02626 -0.01445 -0.01684 AFIX 43 H5 7 0.436440 -0.012005 0.250554 11.00000 -1.20000 AFIX 0 C6 1 0.822459 -0.172307 0.187456 11.00000 0.12930 0.10054 = 0.11679 0.02966 -0.07043 0.03490 PART 1 AFIX 23 H6AA 7 0.897441 -0.166508 0.126844 21.00000 -1.20000 H6AB 7 0.738013 -0.204404 0.147608 21.00000 -1.20000 AFIX 23 PART 2 H6BC 7 0.873183 -0.175965 0.111143 -21.00000 -1.20000 H6BD 7 0.745257 -0.213842 0.189147 -21.00000 -1.20000 AFIX 0 PART 1 C7 1 0.899901 -0.219624 0.293706 21.00000 0.08315 0.06583 = 0.06906 0.02599 0.00600 -0.01680 AFIX 23 H7A 7 0.929566 -0.270921 0.263570 21.00000 -1.20000 H7B 7 0.828482 -0.227787 0.356484 21.00000 -1.20000 AFIX 0 C9 1 1.128627 -0.220194 0.445788 21.00000 0.13135 0.05213 = 0.06231 -0.02227 -0.04186 0.00920 C10 1 1.123731 -0.205875 0.571059 21.00000 0.11755 0.09909 = 0.06689 -0.02679 -0.03666 0.04108 AFIX 43 H10 7 1.059337 -0.166480 0.597345 21.00000 -1.20000 AFIX 0 C11 1 1.220115 -0.252839 0.662373 21.00000 0.07422 0.11938 = 0.07030 0.00375 -0.00382 0.04551 AFIX 43 H11 7 1.219192 -0.240617 0.747040 21.00000 -1.20000 AFIX 0 C12 1 1.232436 -0.275992 0.423367 21.00000 0.11605 0.05795 = 0.05987 -0.02565 -0.04740 0.00726 AFIX 43 H12 7 1.252230 -0.283969 0.340567 21.00000 -1.20000 AFIX 0 C13 1 1.310605 -0.321646 0.513774 21.00000 0.05829 0.08793 = 0.06400 -0.01506 -0.02607 0.01442 AFIX 43 H13 7 1.370037 -0.363286 0.488002 21.00000 -1.20000 AFIX 0 PART 0 C14 1 0.212841 0.128883 0.113435 11.00000 0.10541 0.09912 = 0.03403 -0.02893 -0.00542 0.01106 AFIX 43 H14 7 0.184793 0.145498 0.190742 11.00000 -1.20000 AFIX 0 C15 1 0.090151 0.110282 0.018397 11.00000 0.06290 0.15370 = 0.05374 -0.00754 0.00907 -0.05405 AFIX 43 H15 7 -0.014193 0.110585 0.033024 11.00000 -1.20000 AFIX 0 C16 1 0.137882 0.091557 -0.098344 11.00000 0.05692 0.05102 = 0.05492 -0.00376 -0.00588 -0.02351 C17 1 0.289279 0.079790 -0.102544 11.00000 0.07043 0.07553 = 0.05455 -0.01993 0.01202 -0.00415 AFIX 43 H17 7 0.324098 0.060242 -0.175812 11.00000 -1.20000 AFIX 0 C18 1 0.394047 0.095714 -0.002127 11.00000 0.04621 0.09536 = 0.05401 -0.02246 -0.01097 -0.01775 AFIX 43 H18 7 0.498580 0.084963 -0.008815 11.00000 -1.20000 AFIX 0 C19 1 0.016486 0.075548 -0.197048 11.00000 0.06212 0.14750 = 0.08457 -0.02879 -0.02241 -0.04787 AFIX 23 H19A 7 0.058171 0.078867 -0.277441 11.00000 -1.20000 H19B 7 -0.064685 0.115106 -0.195904 11.00000 -1.20000 AFIX 0 C20 1 -0.053745 -0.007005 -0.182293 11.00000 0.08995 0.10526 = 0.05725 -0.01515 0.01620 -0.03344 AFIX 23 H20A 7 0.023689 -0.047129 -0.193853 11.00000 -1.20000 H20B 7 -0.084928 -0.012723 -0.098419 11.00000 -1.20000 AFIX 0 C21 1 -0.193312 -0.017918 -0.278333 11.00000 0.08360 0.12957 = 0.06141 0.03935 -0.03248 -0.05461 AFIX 23 H21A 7 -0.268690 0.023217 -0.266687 11.00000 -1.20000 H21B 7 -0.160560 -0.011436 -0.361562 11.00000 -1.20000 AFIX 0 C22 1 -0.268429 -0.093993 -0.271808 11.00000 0.06382 0.10532 = 0.04572 0.00570 0.00000 -0.02384 C23 1 -0.311408 -0.123050 -0.158577 11.00000 0.09647 0.15670 = 0.05653 -0.00263 -0.01682 -0.04388 AFIX 43 H23 7 -0.292630 -0.093678 -0.084995 11.00000 -1.20000 AFIX 0 C24 1 -0.377647 -0.191370 -0.157744 11.00000 0.08905 0.08024 = 0.07521 -0.01138 -0.02666 -0.00108 AFIX 43 H24 7 -0.408741 -0.207454 -0.081158 11.00000 -1.20000 AFIX 0 C25 1 -0.289208 -0.142982 -0.372799 11.00000 0.15482 0.06119 = 0.07894 -0.02544 -0.05545 -0.00273 AFIX 43 H25 7 -0.256668 -0.128972 -0.449867 11.00000 -1.20000 AFIX 0 C26 1 -0.359821 -0.213464 -0.355912 11.00000 0.12655 0.10317 = 0.05261 -0.03864 -0.00513 0.04622 AFIX 43 H26 7 -0.376347 -0.245373 -0.426915 11.00000 -1.20000 AFIX 0 C27 1 0.296809 -0.013193 0.523552 11.00000 0.11979 0.11490 = 0.14922 0.06589 0.01662 -0.03911 C28 1 0.780210 0.336211 0.009117 11.00000 0.08176 0.11352 = 0.09184 0.03215 -0.01007 -0.03360 PART 1 C8 1 1.040810 -0.176580 0.350360 21.00000 0.08107 0.07255 = 0.05804 0.00014 -0.00324 0.00399 AFIX 23 H8A 7 1.106378 -0.164260 0.284915 21.00000 -1.20000 H8B 7 1.008824 -0.127038 0.385262 21.00000 -1.20000 AFIX 0 PART 2 C7A 1 0.938111 -0.171204 0.305259 -21.00000 0.08218 0.16851 = 0.11865 -0.02574 -0.08277 0.02341 AFIX 23 H7AA 7 1.018633 -0.132077 0.297468 -21.00000 -1.20000 H7AB 7 0.885553 -0.158428 0.378281 -21.00000 -1.20000 AFIX 0 C8A 1 1.006726 -0.251168 0.317780 -21.00000 0.10680 0.18232 = 0.09401 -0.03366 -0.06738 0.04912 AFIX 23 H8AA 7 0.921637 -0.288620 0.317727 -21.00000 -1.20000 H8AB 7 1.057593 -0.261444 0.242977 -21.00000 -1.20000 AFIX 0 C9A 1 1.115451 -0.268317 0.423422 -21.00000 0.06792 0.13088 = 0.05959 -0.06256 -0.04082 0.01424 C10A 1 1.096832 -0.247440 0.542458 -21.00000 0.11081 0.14578 = 0.06939 -0.05002 -0.01192 0.04354 AFIX 43 H10A 7 1.011331 -0.218005 0.561412 -21.00000 -1.20000 AFIX 0 C12A 1 1.246151 -0.309377 0.408055 -21.00000 0.08718 0.08812 = 0.02914 -0.01089 -0.01111 0.01991 AFIX 43 H12A 7 1.261817 -0.326011 0.327525 -21.00000 -1.20000 AFIX 0 C13A 1 1.355635 -0.327546 0.504183 -21.00000 0.06861 0.08844 = 0.05009 -0.02162 -0.02800 -0.01171 AFIX 43 H13A 7 1.445999 -0.352766 0.485168 -21.00000 -1.20000 AFIX 0 C11A 1 1.216837 -0.273170 0.639636 -21.00000 0.08049 0.11257 = 0.07219 -0.02296 -0.01451 -0.00560 AFIX 43 H11A 7 1.202771 -0.260830 0.722363 -21.00000 -1.20000 AFIX 0 N2A 2 1.342156 -0.311962 0.620760 -21.00000 0.06041 0.07376 = 0.04535 -0.00686 -0.01600 -0.03248 HKLF 4 REM norocf3_a.res in P2(1) REM wR2 = 0.2169, GooF = S = 0.920, Restrained GooF = 0.904 for all data REM R1 = 0.0875 for 1971 Fo > 4sig(Fo) and 0.1441 for all 4224 data REM 498 parameters refined using 340 restraints END WGHT 0.1082 0.0000 REM Highest difference peak 0.085, deepest hole -0.096, 1-sigma level 0.025 Q1 1 0.2259 0.0469 0.0418 11.00000 0.05 0.08 Q2 1 0.7647 0.2404 -0.0003 11.00000 0.05 0.08 Q3 1 0.3629 0.0655 0.4818 11.00000 0.05 0.08 Q4 1 1.1940 -0.2055 0.8586 11.00000 0.05 0.08 Q5 1 0.7776 0.2605 0.0646 11.00000 0.05 0.08 Q6 1 0.7814 0.2851 0.0901 11.00000 0.05 0.08 Q7 1 0.1855 0.0046 0.4568 11.00000 0.05 0.08 Q8 1 -0.1208 0.0388 -0.2813 11.00000 0.05 0.08 Q9 1 -0.1590 0.0618 -0.2535 11.00000 0.05 0.08 Q10 1 -0.5409 -0.2037 -0.5728 11.00000 0.05 0.08 Q11 1 0.2139 0.0384 0.4005 11.00000 0.05 0.07 Q12 1 0.6152 0.2850 0.0110 11.00000 0.05 0.07 Q13 1 0.1085 -0.0168 0.5283 11.00000 0.05 0.07 Q14 1 0.1414 0.0237 0.0822 11.00000 0.05 0.07 Q15 1 0.8770 0.2985 -0.0393 11.00000 0.05 0.07 Q16 1 0.2759 0.0437 0.5988 11.00000 0.05 0.07 Q17 1 1.0287 -0.0246 0.1116 11.00000 0.05 0.07 Q18 1 0.8192 0.3051 -0.0598 11.00000 0.05 0.06 Q19 1 0.8696 -0.1833 0.2182 11.00000 0.05 0.06 Q20 1 -0.2202 -0.1972 -0.2666 11.00000 0.05 0.06 ; _shelx_res_checksum 45930 _shelx_hkl_file ; -9 0 1 2.99 14.57 -9 0 1 16.07 49.32 -9 0 1 1.12 20.92 -9 0 1 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7.10 61.28 -8 8 0 -3.36 32.13 8 -8 0 5.23 16.07 8 -8 0 0.75 17.56 8 8 1 8.22 19.43 8 8 1 4.11 16.81 8 8 1 10.09 8.97 -8 -8 -1 4.11 5.60 -8 -8 -1 6.35 21.67 -8 -8 -1 3.74 9.34 -8 -8 -1 8.22 6.73 -8 8 -1 10.46 19.80 -8 8 -1 -0.37 7.47 -8 8 -1 1.87 15.32 8 -8 1 7.85 23.91 8 -8 1 2.62 18.68 8 -8 1 4.11 14.57 8 8 2 8.97 17.19 8 8 2 5.60 75.10 8 8 2 7.85 19.43 8 8 2 42.97 39.61 8 8 2 16.07 13.08 8 8 2 6.73 4.48 -8 -8 -2 5.60 36.62 -8 -8 -2 11.58 17.94 -8 -8 -2 29.89 39.61 -8 -8 -2 17.56 11.21 -8 -8 -2 10.46 4.11 -8 8 -2 20.55 40.73 -8 8 -2 10.84 7.47 -8 8 -2 17.19 24.66 -8 8 -2 4.48 19.06 8 -8 2 34.75 57.17 8 -8 2 9.34 8.97 8 -8 2 11.58 20.55 8 -8 2 6.35 17.56 8 8 3 8.59 9.72 8 8 3 4.86 17.94 8 8 3 5.98 42.60 8 8 3 8.59 23.54 8 8 3 9.72 15.69 8 8 3 6.73 5.23 -8 -8 -3 2.24 7.85 -8 -8 -3 7.10 11.96 -8 -8 -3 10.46 26.16 -8 -8 -3 11.21 27.65 -8 -8 -3 7.10 13.83 -8 -8 -3 4.11 4.86 -8 8 -3 29.15 77.35 -8 8 -3 3.74 9.34 -8 8 -3 3.74 22.05 -8 8 -3 8.22 25.41 -8 8 -3 5.98 4.11 8 -8 3 7.85 2.62 8 -8 3 8.59 67.63 8 -8 3 7.47 14.57 8 -8 3 7.47 48.20 8 -8 3 7.47 20.18 8 -8 3 6.35 3.36 8 9 0 0.37 7.10 8 9 0 -1.49 6.73 8 9 0 2.99 11.96 8 9 0 4.11 7.47 -8 -9 0 1.87 8.59 -8 -9 0 0.00 24.66 -8 -9 0 0.37 4.48 -8 9 0 0.75 20.55 -8 9 0 4.86 93.79 -8 9 0 -0.37 93.41 -8 9 0 -6.35 68.75 -8 9 0 6.35 29.89 8 -9 0 0.37 16.44 8 -9 0 -7.47 96.40 8 -9 0 0.00 14.20 8 9 1 2.99 20.92 8 9 1 4.86 16.07 8 9 1 4.11 11.58 8 9 1 4.48 6.73 -8 -9 -1 3.74 5.60 -8 -9 -1 -4.86 107.24 -8 -9 -1 1.12 19.06 -8 -9 -1 0.75 8.59 -8 -9 -1 3.36 9.34 -8 9 -1 1.49 16.07 -8 9 -1 0.00 90.05 -8 9 -1 4.86 6.35 -8 9 -1 0.37 7.47 -8 9 -1 0.37 12.33 8 -9 1 3.36 19.06 8 -9 1 0.37 8.22 8 -9 1 3.36 17.19 8 -9 1 -2.62 11.58 8 9 2 3.36 35.50 8 9 2 1.87 17.19 8 9 2 3.36 36.62 8 9 2 5.23 14.20 8 9 2 1.12 4.48 -8 -9 -2 1.87 18.31 -8 -9 -2 5.23 16.81 -8 -9 -2 12.33 36.99 -8 -9 -2 10.46 13.08 -8 -9 -2 1.87 3.74 -8 9 -2 0.00 27.65 -8 9 -2 7.47 87.81 -8 9 -2 0.37 8.59 -8 9 -2 6.35 26.53 -8 9 -2 1.12 16.07 -8 9 -2 1.12 2.24 8 -9 2 9.34 41.48 8 -9 2 2.99 11.96 8 -9 2 2.99 18.31 8 -9 2 4.11 14.57 8 10 0 0.75 5.98 8 10 0 2.99 10.09 8 10 0 2.62 10.09 -8 -10 0 0.37 7.47 -8 -10 0 -1.49 22.05 -8 -10 0 1.87 7.85 -8 10 0 -0.75 36.62 -8 10 0 5.98 79.96 -8 10 0 0.75 97.90 -8 10 0 6.73 28.40 8 -10 0 0.37 22.05 8 -10 0 15.32 91.92 8 -10 0 -3.36 99.02 8 -10 0 0.37 7.47 8 -10 0 -1.87 12.70 9 0 0 -0.37 8.59 9 0 0 0.00 17.19 -9 0 0 4.11 10.46 -9 0 0 -1.12 69.13 -9 0 0 2.62 18.31 -9 0 0 7.85 30.27 9 0 1 4.11 12.33 -9 0 -1 1.49 13.08 -9 0 -1 6.35 28.40 -9 0 -1 -0.37 7.85 9 0 2 19.06 3.74 9 0 2 41.85 34.75 -9 0 -2 13.83 11.21 -9 0 -2 11.96 68.75 -9 0 -2 50.07 35.87 9 1 0 -1.49 14.95 -9 -1 0 0.37 8.97 -9 -1 0 -8.59 56.42 -9 -1 0 -1.87 17.56 -9 -1 0 2.24 30.64 -9 1 0 3.74 11.96 -9 1 0 -7.10 66.51 -9 1 0 1.49 19.43 -9 1 0 5.98 34.00 9 -1 0 1.12 16.81 9 -1 0 1.87 29.15 9 1 1 4.11 21.67 9 1 1 -0.75 13.45 -9 -1 -1 0.00 11.96 -9 -1 -1 0.00 23.54 -9 -1 -1 -0.75 7.47 -9 1 -1 -5.98 39.98 -9 1 -1 0.75 8.22 9 -1 1 0.00 14.57 9 1 2 1.12 2.62 9 1 2 6.73 32.51 -9 -1 -2 0.75 5.60 -9 -1 -2 -2.24 64.27 -9 -1 -2 2.24 32.88 -9 1 -2 -6.73 71.37 -9 1 -2 6.35 35.12 9 -1 2 3.74 6.35 9 -1 2 19.06 35.12 -9 -2 0 3.36 10.09 -9 -2 0 3.36 18.68 -9 -2 0 4.86 30.27 -9 2 0 0.37 13.08 -9 2 0 16.07 55.67 -9 2 0 1.12 20.18 -9 2 0 -2.62 31.39 -9 2 0 1.87 30.27 9 -2 0 6.35 23.91 9 -2 0 -0.37 18.31 9 -2 0 -5.60 32.13 9 2 1 0.00 11.96 9 2 1 -1.12 14.95 9 2 1 0.37 1.87 -9 -2 -1 4.11 10.84 -9 -2 -1 5.23 24.29 -9 -2 -1 -1.49 20.55 -9 -2 -1 0.75 7.85 -9 2 -1 -4.48 63.52 -9 2 -1 5.23 51.94 -9 2 -1 -0.37 7.47 9 -2 1 1.12 63.52 9 -2 1 -1.49 14.20 9 2 2 0.00 58.29 -9 -2 -2 0.75 12.33 -9 -2 -2 4.86 3.74 -9 -2 -2 -4.86 50.07 -9 -2 -2 8.59 36.62 -9 2 -2 7.85 71.74 -9 2 -2 7.47 34.38 9 -2 2 4.48 7.47 9 -2 2 -0.75 34.00 -9 -3 0 1.87 33.26 -9 -3 0 2.62 20.18 -9 -3 0 -1.49 29.52 -9 3 0 7.10 41.85 -9 3 0 -3.74 22.79 -9 3 0 2.24 29.15 -9 3 0 2.24 35.12 9 -3 0 0.37 31.39 9 -3 0 5.98 15.32 9 -3 0 0.75 34.75 9 3 1 1.49 10.46 9 3 1 4.48 8.59 9 3 1 0.37 21.30 9 3 1 8.97 6.73 -9 -3 -1 1.87 9.34 -9 -3 -1 1.49 19.43 -9 -3 -1 2.24 18.68 -9 -3 -1 4.48 5.23 -9 -3 -1 2.62 7.85 -9 3 -1 28.02 74.73 -9 3 -1 12.70 62.40 -9 3 -1 -0.37 7.47 9 -3 1 32.13 74.36 9 -3 1 -7.10 68.38 9 -3 1 0.37 13.45 9 -3 1 0.37 31.01 9 3 2 1.12 11.58 9 3 2 3.36 56.05 9 3 2 0.37 3.36 -9 -3 -2 3.74 12.70 -9 -3 -2 0.37 3.36 -9 -3 -2 -1.87 36.24 -9 -3 -2 0.75 37.37 -9 3 -2 -2.99 74.73 -9 3 -2 8.22 34.38 9 -3 2 3.36 31.76 9 4 0 11.96 54.18 9 4 0 1.12 27.65 9 4 0 2.24 18.31 -9 -4 0 6.35 21.67 -9 -4 0 1.12 27.28 -9 4 0 6.73 30.27 -9 4 0 3.36 28.40 -9 4 0 -8.22 33.26 9 -4 0 -5.23 45.59 9 -4 0 -6.35 49.32 9 -4 0 0.75 13.83 9 -4 0 0.37 26.16 9 4 1 0.37 9.34 9 4 1 2.62 6.35 9 4 1 0.75 19.06 -9 -4 -1 1.49 8.97 -9 -4 -1 3.74 11.58 -9 -4 -1 -0.37 17.94 -9 -4 -1 0.37 7.47 -9 4 -1 8.22 67.63 -9 4 -1 -23.17 68.75 -9 4 -1 0.37 7.10 9 -4 1 -5.98 79.59 9 -4 1 2.24 71.37 9 -4 1 -1.87 13.08 9 -4 1 -3.74 36.24 9 5 0 -2.24 22.42 9 5 0 2.24 20.92 -9 -5 0 2.99 30.64 -9 -5 0 -0.75 22.05 -9 -5 0 -3.36 27.28 -9 5 0 5.60 23.17 -9 5 0 -7.10 45.59 -9 5 0 7.85 26.53 9 -5 0 2.99 32.13 9 -5 0 11.96 60.91 9 -5 0 2.99 14.95 9 -5 0 3.74 19.80 9 5 1 0.37 8.22 9 5 1 0.00 5.23 9 5 1 0.37 17.94 -9 -5 -1 1.12 16.81 -9 -5 -1 1.12 8.22 -9 -5 -1 1.87 17.19 -9 -5 -1 -1.87 7.47 -9 5 -1 24.29 54.18 -9 5 -1 -2.62 70.99 -9 5 -1 -0.37 6.73 9 -5 1 -0.37 70.62 9 -5 1 0.75 75.10 9 -5 1 -0.37 15.69 9 -5 1 -2.24 26.90 9 6 0 2.62 14.20 9 6 0 8.59 22.05 9 6 0 1.87 12.33 -9 -6 0 -1.87 25.41 -9 -6 0 5.98 16.07 -9 -6 0 1.12 25.78 -9 6 0 10.09 20.18 -9 6 0 1.49 57.54 -9 6 0 0.00 23.91 9 -6 0 0.75 24.29 9 -6 0 7.47 66.51 9 -6 0 0.00 14.20 9 -6 0 3.36 16.81 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 53246 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.5145(5) 0.1550(4) 0.2413(5) 0.0645(17) Uani 1 1 d . . . . . S1 S 0.2431(11) 0.0774(5) 0.4652(10) 0.086(3) Uani 1 1 d . . . . . S2 S 0.6849(10) 0.2420(5) -0.0323(9) 0.068(3) Uani 1 1 d . . . . . F1 F 0.288(4) -0.0665(11) 0.437(3) 0.26(2) Uani 1 1 d D U . A 1 F2 F 0.209(4) -0.0400(14) 0.604(3) 0.26(2) Uani 1 1 d D U . B 1 F3 F 0.434(3) -0.0096(16) 0.572(3) 0.206(15) Uani 1 1 d D U . C 1 F4 F 0.792(2) 0.3772(18) -0.087(3) 0.28(3) Uani 1 1 d D . . . . F5 F 0.702(3) 0.3729(15) 0.080(2) 0.162(12) Uani 1 1 d D . . . . F6 F 0.9154(18) 0.3189(11) 0.0633(18) 0.126(8) Uani 1 1 d D . . . . O1 O 0.096(4) 0.073(3) 0.424(4) 0.32(3) Uani 1 1 d . . . . . O2 O 0.268(3) 0.1229(13) 0.573(3) 0.167(11) Uani 1 1 d . . . . . O3 O 0.360(3) 0.0963(10) 0.3810(19) 0.113(7) Uani 1 1 d . . . . . O4 O 0.777(2) 0.2077(14) -0.097(2) 0.137(8) Uani 1 1 d . . . . . O5 O 0.6810(15) 0.2051(7) 0.0790(13) 0.079(5) Uani 1 1 d . . . . . O6 O 0.5389(15) 0.2636(8) -0.0977(13) 0.077(5) Uani 1 1 d . . . . . N1 N 0.6132(18) 0.0535(8) 0.2326(14) 0.068(5) Uani 1 1 d . . . . . N2 N 1.308(5) -0.311(3) 0.633(4) 0.075(11) Uani 0.54(2) 1 d D U P D 1 N3 N 0.3580(17) 0.1247(8) 0.1017(17) 0.071(5) Uani 1 1 d . . . . . N4 N -0.4074(19) -0.2424(9) -0.2543(15) 0.076(5) Uani 1 1 d . U . . . C1 C 0.762(2) 0.0409(11) 0.2179(15) 0.088(6) Uani 1 1 d . . . . . H1 H 0.822790 0.086561 0.222115 0.106 Uiso 1 1 calc R U . . . C2 C 0.844(2) -0.0268(11) 0.1977(17) 0.100(6) Uani 1 1 d . . . . . H2 H 0.947353 -0.027037 0.180368 0.120 Uiso 1 1 calc R U . . . C3 C 0.7577(18) -0.0935(10) 0.2058(15) 0.082(6) Uani 1 1 d . . . . . C4 C 0.602(2) -0.0851(10) 0.2210(15) 0.089(6) Uani 1 1 d . . . . . H4 H 0.538598 -0.129690 0.220650 0.107 Uiso 1 1 calc R U . . . C5 C 0.5408(18) -0.0138(9) 0.2361(14) 0.082(6) Uani 1 1 d . . . . . H5 H 0.436440 -0.012005 0.250554 0.098 Uiso 1 1 calc R U . . . C6 C 0.822(2) -0.1723(9) 0.1875(17) 0.122(9) Uani 1 1 d D U . . . H6AA H 0.897441 -0.166508 0.126844 0.146 Uiso 0.54(2) 1 calc R U P D 1 H6AB H 0.738013 -0.204404 0.147608 0.146 Uiso 0.54(2) 1 calc R U P D 1 H6BC H 0.873183 -0.175965 0.111143 0.146 Uiso 0.46(2) 1 calc R U P D 2 H6BD H 0.745257 -0.213842 0.189147 0.146 Uiso 0.46(2) 1 calc R U P D 2 C7 C 0.900(3) -0.2196(12) 0.294(2) 0.073(11) Uani 0.54(2) 1 d D U P D 1 H7A H 0.929566 -0.270921 0.263570 0.087 Uiso 0.54(2) 1 calc R U P D 1 H7B H 0.828482 -0.227787 0.356484 0.087 Uiso 0.54(2) 1 calc R U P D 1 C9 C 1.129(3) -0.2202(13) 0.446(3) 0.086(11) Uani 0.54(2) 1 d D . P D 1 C10 C 1.124(4) -0.2059(17) 0.571(3) 0.098(13) Uani 0.54(2) 1 d D . P D 1 H10 H 1.059337 -0.166480 0.597345 0.118 Uiso 0.54(2) 1 calc R U P D 1 C11 C 1.220(4) -0.253(2) 0.662(3) 0.089(11) Uani 0.54(2) 1 d D U P D 1 H11 H 1.219192 -0.240617 0.747040 0.107 Uiso 0.54(2) 1 calc R U P D 1 C12 C 1.232(4) -0.2760(19) 0.423(3) 0.082(12) Uani 0.54(2) 1 d D U P D 1 H12 H 1.252230 -0.283969 0.340567 0.099 Uiso 0.54(2) 1 calc R U P D 1 C13 C 1.311(4) -0.322(3) 0.514(4) 0.072(11) Uani 0.54(2) 1 d D U P D 1 H13 H 1.370037 -0.363286 0.488002 0.087 Uiso 0.54(2) 1 calc R U P D 1 C14 C 0.213(2) 0.1289(8) 0.1134(15) 0.080(6) Uani 1 1 d . . . . . H14 H 0.184793 0.145498 0.190742 0.097 Uiso 1 1 calc R U . . . C15 C 0.0902(19) 0.1103(10) 0.0184(18) 0.090(6) Uani 1 1 d . . . . . H15 H -0.014193 0.110585 0.033024 0.108 Uiso 1 1 calc R U . . . C16 C 0.1379(17) 0.0916(7) -0.0983(16) 0.055(5) Uani 1 1 d . . . . . C17 C 0.2893(18) 0.0798(8) -0.1025(14) 0.066(5) Uani 1 1 d . . . . . H17 H 0.324098 0.060242 -0.175812 0.080 Uiso 1 1 calc R U . . . C18 C 0.3940(16) 0.0957(8) -0.0021(15) 0.066(5) Uani 1 1 d . . . . . H18 H 0.498580 0.084963 -0.008815 0.080 Uiso 1 1 calc R U . . . C19 C 0.0165(18) 0.0755(11) -0.1970(16) 0.100(6) Uani 1 1 d . . . . . H19A H 0.058171 0.078867 -0.277441 0.120 Uiso 1 1 calc R U . . . H19B H -0.064685 0.115106 -0.195904 0.120 Uiso 1 1 calc R U . . . C20 C -0.0537(18) -0.0070(9) -0.1823(16) 0.084(5) Uani 1 1 d . . . . . H20A H 0.023689 -0.047129 -0.193853 0.100 Uiso 1 1 calc R U . . . H20B H -0.084928 -0.012723 -0.098419 0.100 Uiso 1 1 calc R U . . . C21 C -0.1933(17) -0.0179(9) -0.2783(15) 0.094(7) Uani 1 1 d . . . . . H21A H -0.268690 0.023217 -0.266687 0.113 Uiso 1 1 calc R U . . . H21B H -0.160560 -0.011436 -0.361562 0.113 Uiso 1 1 calc R U . . . C22 C -0.2684(16) -0.0940(10) -0.2718(17) 0.072(5) Uani 1 1 d . . . . . C23 C -0.311(2) -0.1230(12) -0.159(2) 0.105(8) Uani 1 1 d . . . . . H23 H -0.292630 -0.093678 -0.084995 0.126 Uiso 1 1 calc R U . . . C24 C -0.3776(18) -0.1914(9) -0.1577(16) 0.084(6) Uani 1 1 d . U . . . H24 H -0.408741 -0.207454 -0.081158 0.101 Uiso 1 1 calc R U . . . C25 C -0.289(2) -0.1430(9) -0.3728(17) 0.103(8) Uani 1 1 d . . . . . H25 H -0.256668 -0.128972 -0.449867 0.124 Uiso 1 1 calc R U . . . C26 C -0.360(2) -0.2135(11) -0.356(2) 0.095(7) Uani 1 1 d . U . . . H26 H -0.376347 -0.245373 -0.426915 0.114 Uiso 1 1 calc R U . . . C27 C 0.297(2) -0.0132(12) 0.524(2) 0.128(9) Uani 1 1 d D U . . . C28 C 0.780(2) 0.3362(11) 0.0091(19) 0.097(8) Uani 1 1 d D . . . . C8 C 1.041(3) -0.1766(12) 0.350(3) 0.071(10) Uani 0.54(2) 1 d D . P D 1 H8A H 1.106378 -0.164260 0.284915 0.086 Uiso 0.54(2) 1 calc R U P D 1 H8B H 1.008824 -0.127038 0.385262 0.086 Uiso 0.54(2) 1 calc R U P D 1 C7A C 0.938(5) -0.171(2) 0.305(4) 0.130(17) Uani 0.46(2) 1 d D U P D 2 H7AA H 1.018633 -0.132077 0.297468 0.156 Uiso 0.46(2) 1 calc R U P D 2 H7AB H 0.885553 -0.158428 0.378281 0.156 Uiso 0.46(2) 1 calc R U P D 2 C8A C 1.007(4) -0.251(2) 0.318(3) 0.133(18) Uani 0.46(2) 1 d D U P D 2 H8AA H 0.921637 -0.288620 0.317727 0.160 Uiso 0.46(2) 1 calc R U P D 2 H8AB H 1.057593 -0.261444 0.242977 0.160 Uiso 0.46(2) 1 calc R U P D 2 C9A C 1.115(3) -0.2683(17) 0.423(3) 0.090(13) Uani 0.46(2) 1 d D U P D 2 C10A C 1.097(5) -0.247(3) 0.542(3) 0.110(17) Uani 0.46(2) 1 d D U P D 2 H10A H 1.011331 -0.218005 0.561412 0.132 Uiso 0.46(2) 1 calc R U P D 2 C12A C 1.246(4) -0.309(2) 0.408(3) 0.069(13) Uani 0.46(2) 1 d D U P D 2 H12A H 1.261817 -0.326011 0.327525 0.083 Uiso 0.46(2) 1 calc R U P D 2 C13A C 1.356(6) -0.328(3) 0.504(4) 0.072(11) Uani 0.46(2) 1 d D U P D 2 H13A H 1.445999 -0.352766 0.485168 0.086 Uiso 0.46(2) 1 calc R U P D 2 C11A C 1.217(6) -0.273(3) 0.640(4) 0.090(12) Uani 0.46(2) 1 d D U P D 2 H11A H 1.202771 -0.260830 0.722363 0.108 Uiso 0.46(2) 1 calc R U P D 2 N2A N 1.342(5) -0.312(3) 0.621(4) 0.061(9) Uani 0.46(2) 1 d D U P D 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 Cu1 0.058(3) 0.081(3) 0.052(4) -0.010(3) -0.006(3) -0.004(2) S1 0.087(7) 0.092(6) 0.077(8) -0.001(5) -0.005(6) -0.027(5) S2 0.069(6) 0.085(5) 0.049(7) -0.006(5) -0.001(5) 0.005(4) F1 0.33(4) 0.041(10) 0.42(6) -0.034(17) 0.10(4) -0.035(15) F2 0.43(5) 0.091(15) 0.31(5) 0.047(19) 0.22(4) -0.05(2) F3 0.20(3) 0.23(3) 0.17(3) 0.00(2) -0.05(2) 0.09(2) F4 0.092(14) 0.33(4) 0.40(5) 0.29(4) -0.04(2) -0.077(18) F5 0.13(2) 0.149(19) 0.20(3) -0.016(17) -0.03(2) -0.022(14) F6 0.079(12) 0.157(15) 0.135(19) 0.029(12) -0.019(12) -0.035(10) O1 0.15(3) 0.63(9) 0.20(4) -0.21(5) 0.05(3) -0.11(4) O2 0.20(2) 0.138(16) 0.15(2) 0.025(15) -0.02(2) -0.053(16) O3 0.137(16) 0.126(14) 0.072(15) -0.015(10) 0.000(13) -0.029(11) O4 0.077(11) 0.212(19) 0.106(17) -0.039(15) -0.061(12) 0.030(13) O5 0.091(10) 0.062(7) 0.072(11) -0.004(7) -0.046(9) 0.000(6) O6 0.073(9) 0.094(9) 0.065(12) -0.021(7) 0.008(8) 0.023(7) N1 0.058(9) 0.076(10) 0.068(12) -0.023(7) -0.007(8) -0.016(8) N2 0.06(2) 0.093(17) 0.064(14) -0.007(14) -0.011(15) 0.023(15) N3 0.046(9) 0.091(10) 0.073(15) -0.023(8) -0.002(8) -0.004(7) N4 0.108(11) 0.110(11) 0.008(9) -0.004(8) 0.001(9) 0.012(9) C1 0.109(16) 0.103(14) 0.051(14) -0.017(9) 0.003(11) -0.011(12) C2 0.078(11) 0.093(13) 0.120(18) 0.017(11) -0.022(11) 0.011(12) C3 0.048(10) 0.092(12) 0.097(16) 0.006(10) -0.035(9) -0.012(10) C4 0.102(15) 0.066(11) 0.091(16) -0.007(9) -0.022(11) -0.024(10) C5 0.076(11) 0.073(12) 0.091(15) -0.026(9) -0.014(10) -0.017(10) C6 0.129(15) 0.101(13) 0.117(17) 0.030(11) -0.070(14) 0.035(11) C7 0.08(2) 0.066(18) 0.07(3) 0.026(16) 0.006(17) -0.017(14) C9 0.13(2) 0.052(17) 0.062(16) -0.022(13) -0.042(17) 0.009(14) C10 0.12(3) 0.10(2) 0.067(16) -0.027(15) -0.037(18) 0.041(19) C11 0.074(19) 0.12(2) 0.070(17) 0.004(16) -0.004(15) 0.046(17) C12 0.12(3) 0.06(2) 0.060(18) -0.026(13) -0.047(15) 0.007(14) C13 0.06(2) 0.088(18) 0.064(15) -0.015(13) -0.026(16) 0.014(15) C14 0.105(15) 0.099(12) 0.034(12) -0.029(8) -0.005(11) 0.011(9) C15 0.063(10) 0.154(15) 0.054(14) -0.008(11) 0.009(10) -0.054(9) C16 0.057(10) 0.051(8) 0.055(13) -0.004(7) -0.006(9) -0.024(6) C17 0.070(11) 0.076(9) 0.055(12) -0.020(8) 0.012(9) -0.004(8) C18 0.046(9) 0.095(11) 0.054(12) -0.022(9) -0.011(9) -0.018(7) C19 0.062(10) 0.148(14) 0.085(15) -0.029(12) -0.022(10) -0.048(10) C20 0.090(11) 0.105(12) 0.057(13) -0.015(9) 0.016(10) -0.033(9) C21 0.084(12) 0.130(14) 0.061(13) 0.039(10) -0.032(10) -0.055(10) C22 0.064(10) 0.105(12) 0.046(13) 0.006(10) 0.000(9) -0.024(9) C23 0.096(14) 0.157(19) 0.057(17) -0.003(12) -0.017(12) -0.044(12) C24 0.089(12) 0.080(11) 0.075(14) -0.011(9) -0.027(11) -0.001(9) C25 0.155(17) 0.061(10) 0.079(15) -0.025(9) -0.055(13) -0.003(10) C26 0.127(15) 0.103(14) 0.053(16) -0.039(11) -0.005(13) 0.046(12) C27 0.120(16) 0.115(17) 0.15(2) 0.066(16) 0.017(15) -0.039(14) C28 0.082(16) 0.114(16) 0.09(2) 0.032(13) -0.010(14) -0.034(11) C8 0.081(19) 0.073(17) 0.058(19) 0.000(13) -0.003(16) 0.004(12) C7A 0.08(3) 0.17(3) 0.12(3) -0.03(2) -0.08(2) 0.02(2) C8A 0.11(3) 0.18(3) 0.09(2) -0.03(3) -0.07(2) 0.05(2) C9A 0.068(18) 0.13(3) 0.060(17) -0.063(18) -0.041(15) 0.014(18) C10A 0.11(3) 0.15(4) 0.069(19) -0.05(2) -0.01(2) 0.04(3) C12A 0.09(2) 0.09(3) 0.029(18) -0.011(19) -0.011(15) 0.020(19) C13A 0.07(2) 0.09(2) 0.050(15) -0.022(15) -0.028(16) -0.012(17) C11A 0.080(19) 0.11(3) 0.072(18) -0.023(19) -0.015(15) -0.006(17) N2A 0.060(17) 0.074(17) 0.045(15) -0.007(14) -0.016(15) -0.032(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.0000 0.0000 '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' 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 N1 Cu1 N2 88.7(15) . 2_756 N1 Cu1 N3 90.1(6) . . N1 Cu1 N4 177.8(9) . 2 N1 Cu1 N2A 92.6(15) . 2_756 N3 Cu1 N2 172.8(15) . 2_756 N3 Cu1 N4 89.7(6) . 2 N4 Cu1 N2 91.8(15) 2 2_756 N2A Cu1 N3 177.0(17) 2_756 . O1 S1 O2 112(2) . . O1 S1 O3 121(2) . . O1 S1 C27 107(3) . . O2 S1 O3 109.9(14) . . O2 S1 C27 100.6(13) . . O3 S1 C27 104.2(12) . . O4 S2 O5 110.5(14) . . O4 S2 O6 115.5(10) . . O4 S2 C28 104.0(14) . . O5 S2 O6 116.6(11) . . O5 S2 C28 104.1(8) . . O6 S2 C28 104.4(9) . . C1 N1 Cu1 126.0(12) . . C5 N1 Cu1 124.3(13) . . C5 N1 C1 109.7(15) . . C11 N2 Cu1 118(3) . 2_746 C13 N2 Cu1 122(2) . 2_746 C13 N2 C11 115(2) . . C14 N3 Cu1 120.7(15) . . C14 N3 C18 116.1(13) . . C18 N3 Cu1 123.1(11) . . C24 N4 Cu1 124.0(16) . 2_545 C26 N4 Cu1 125.6(13) . 2_545 C26 N4 C24 110.4(17) . . N1 C1 H1 113.9 . . N1 C1 C2 132.2(18) . . C2 C1 H1 113.9 . . C1 C2 H2 123.6 . . C3 C2 C1 112.8(18) . . C3 C2 H2 123.6 . . C2 C3 C4 118.0(15) . . C2 C3 C6 121.8(17) . . C4 C3 C6 120.0(15) . . C3 C4 H4 119.6 . . C5 C4 C3 120.7(15) . . C5 C4 H4 119.7 . . N1 C5 C4 126.2(17) . . N1 C5 H5 116.9 . . C4 C5 H5 116.9 . . C3 C6 H6AA 106.8 . . C3 C6 H6AB 106.8 . . C3 C6 H6BC 112.6 . . C3 C6 H6BD 112.6 . . C3 C6 C7 122.2(19) . . C3 C6 C7A 95.9(16) . . H6AA C6 H6AB 106.6 . . H6BC C6 H6BD 110.1 . . C7 C6 H6AA 106.8 . . C7 C6 H6AB 106.8 . . C7A C6 H6BC 112.6 . . C7A C6 H6BD 112.5 . . C6 C7 H7A 109.8 . . C6 C7 H7B 109.9 . . C6 C7 C8 109.1(13) . . H7A C7 H7B 108.3 . . C8 C7 H7A 109.9 . . C8 C7 H7B 109.9 . . C10 C9 C8 123(3) . . C12 C9 C10 113(2) . . C12 C9 C8 124(3) . . C9 C10 H10 120.4 . . C9 C10 C11 119(3) . . C11 C10 H10 120.4 . . N2 C11 C10 124(3) . . N2 C11 H11 118.0 . . C10 C11 H11 118.1 . . C9 C12 H12 117.9 . . C9 C12 C13 124(3) . . C13 C12 H12 117.9 . . N2 C13 C12 124(3) . . N2 C13 H13 117.8 . . C12 C13 H13 117.8 . . N3 C14 H14 117.3 . . N3 C14 C15 125.5(19) . . C15 C14 H14 117.3 . . C14 C15 H15 122.5 . . C16 C15 C14 115.0(16) . . C16 C15 H15 122.5 . . C15 C16 C19 116.2(15) . . C17 C16 C15 116.9(13) . . C17 C16 C19 126.2(18) . . C16 C17 H17 119.4 . . C16 C17 C18 121.2(17) . . C18 C17 H17 119.4 . . N3 C18 C17 124.0(15) . . N3 C18 H18 118.0 . . C17 C18 H18 118.0 . . C16 C19 H19A 109.4 . . C16 C19 H19B 109.4 . . C16 C19 C20 111.2(14) . . H19A C19 H19B 108.0 . . C20 C19 H19A 109.4 . . C20 C19 H19B 109.4 . . C19 C20 H20A 109.7 . . C19 C20 H20B 109.8 . . H20A C20 H20B 108.2 . . C21 C20 C19 109.6(13) . . C21 C20 H20A 109.7 . . C21 C20 H20B 109.7 . . C20 C21 H21A 108.8 . . C20 C21 H21B 108.8 . . H21A C21 H21B 107.7 . . C22 C21 C20 113.9(12) . . C22 C21 H21A 108.8 . . C22 C21 H21B 108.8 . . C23 C22 C21 121.2(16) . . C25 C22 C21 121.7(19) . . C25 C22 C23 116.9(16) . . C22 C23 H23 120.6 . . C24 C23 C22 118.8(17) . . C24 C23 H23 120.6 . . N4 C24 H24 116.0 . . C23 C24 N4 128(2) . . C23 C24 H24 116.0 . . C22 C25 H25 121.6 . . C26 C25 C22 117(2) . . C26 C25 H25 121.6 . . N4 C26 C25 128.9(17) . . N4 C26 H26 115.6 . . C25 C26 H26 115.5 . . F1 C27 S1 111.9(17) . . F2 C27 S1 114.0(19) . . F2 C27 F1 104.0(16) . . F3 C27 S1 108.6(16) . . F3 C27 F1 108.2(19) . . F3 C27 F2 110.0(18) . . F4 C28 S2 110.9(19) . . F4 C28 F6 110.3(15) . . F5 C28 S2 109.0(17) . . F5 C28 F4 109.1(19) . . F5 C28 F6 111.5(17) . . F6 C28 S2 106.0(14) . . C7 C8 H8A 109.0 . . C7 C8 H8B 109.0 . . C9 C8 C7 112.9(13) . . C9 C8 H8A 109.0 . . C9 C8 H8B 109.0 . . H8A C8 H8B 107.8 . . C6 C7A H7AA 110.4 . . C6 C7A H7AB 110.4 . . H7AA C7A H7AB 108.6 . . C8A C7A C6 107(2) . . C8A C7A H7AA 110.4 . . C8A C7A H7AB 110.4 . . C7A C8A H8AA 107.6 . . C7A C8A H8AB 107.6 . . H8AA C8A H8AB 107.0 . . C9A C8A C7A 119(2) . . C9A C8A H8AA 107.6 . . C9A C8A H8AB 107.6 . . C10A C9A C8A 124(3) . . C12A C9A C8A 120(3) . . C12A C9A C10A 116(2) . . C9A C10A H10A 121.6 . . C9A C10A C11A 117(3) . . C11A C10A H10A 121.7 . . C9A C12A H12A 118.5 . . C9A C12A C13A 123(3) . . C13A C12A H12A 118.3 . . C12A C13A H13A 118.1 . . N2A C13A C12A 124(3) . . N2A C13A H13A 117.9 . . C10A C11A H11A 117.2 . . N2A C11A C10A 125(3) . . N2A C11A H11A 117.3 . . C13A N2A C11A 115(3) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cu1 N1 1.964(15) . Cu1 N2 2.05(3) 2_756 Cu1 N3 2.012(13) . Cu1 N4 2.019(18) 2 Cu1 N2A 1.94(3) 2_756 S1 O1 1.33(3) . S1 O2 1.41(3) . S1 O3 1.49(2) . S1 C27 1.74(2) . S2 O4 1.28(2) . S2 O5 1.376(16) . S2 O6 1.451(13) . S2 C28 1.86(2) . F1 C27 1.32(2) . F2 C27 1.312(19) . F3 C27 1.272(19) . F4 C28 1.284(19) . F5 C28 1.264(19) . F6 C28 1.306(17) . N1 C1 1.36(2) . N1 C5 1.329(18) . N2 C11 1.33(3) . N2 C13 1.32(3) . N3 C14 1.30(2) . N3 C18 1.31(2) . N4 C24 1.38(2) . N4 C26 1.33(2) . C1 H1 0.9500 . C1 C2 1.40(2) . C2 H2 0.9500 . C2 C3 1.39(2) . C3 C4 1.41(2) . C3 C6 1.50(2) . C4 H4 0.9500 . C4 C5 1.36(2) . C5 H5 0.9500 . C6 H6AA 0.9900 . C6 H6AB 0.9900 . C6 H6BC 0.9900 . C6 H6BD 0.9900 . C6 C7 1.520(3) . C6 C7A 1.55(2) . C7 H7A 0.9900 . C7 H7B 0.9900 . C7 C8 1.520(3) . C9 C10 1.40(4) . C9 C12 1.37(3) . C9 C8 1.44(3) . C10 H10 0.9500 . C10 C11 1.48(3) . C11 H11 0.9500 . C12 H12 0.9500 . C12 C13 1.39(3) . C13 H13 0.9500 . C14 H14 0.9500 . C14 C15 1.45(2) . C15 H15 0.9500 . C15 C16 1.42(2) . C16 C17 1.355(19) . C16 C19 1.461(16) . C17 H17 0.9500 . C17 C18 1.383(17) . C18 H18 0.9500 . C19 H19A 0.9900 . C19 H19B 0.9900 . C19 C20 1.57(2) . C20 H20A 0.9900 . C20 H20B 0.9900 . C20 C21 1.539(17) . C21 H21A 0.9900 . C21 H21B 0.9900 . C21 C22 1.476(19) . C22 C23 1.42(2) . C22 C25 1.39(2) . C23 H23 0.9500 . C23 C24 1.32(2) . C24 H24 0.9500 . C25 H25 0.9500 . C25 C26 1.39(3) . C26 H26 0.9500 . C8 H8A 0.9900 . C8 H8B 0.9900 . C7A H7AA 0.9900 . C7A H7AB 0.9900 . C7A C8A 1.51(3) . C8A H8AA 0.9900 . C8A H8AB 0.9900 . C8A C9A 1.45(3) . C9A C10A 1.38(4) . C9A C12A 1.38(4) . C10A H10A 0.9500 . C10A C11A 1.48(3) . C12A H12A 0.9500 . C12A C13A 1.38(3) . C13A H13A 0.9500 . C13A N2A 1.32(3) . C11A H11A 0.9500 . C11A N2A 1.33(3) . 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 Cu1 N1 C1 C2 -172.5(15) . . . . Cu1 N1 C5 C4 174.6(12) . . . . Cu1 N2 C11 C10 159(2) 2_746 . . . Cu1 N2 C13 C12 -153(4) 2_746 . . . Cu1 N3 C14 C15 178.5(11) . . . . Cu1 N3 C18 C17 -175.0(11) . . . . Cu1 N4 C24 C23 -178.6(14) 2_545 . . . Cu1 N4 C26 C25 178.2(13) 2_545 . . . O1 S1 C27 F1 65(2) . . . . O1 S1 C27 F2 -52(3) . . . . O1 S1 C27 F3 -175(2) . . . . O2 S1 C27 F1 -178(2) . . . . O2 S1 C27 F2 65(2) . . . . O2 S1 C27 F3 -58(2) . . . . O3 S1 C27 F1 -63.9(19) . . . . O3 S1 C27 F2 178(2) . . . . O3 S1 C27 F3 55(2) . . . . O4 S2 C28 F4 64.1(18) . . . . O4 S2 C28 F5 -175.7(17) . . . . O4 S2 C28 F6 -55.7(16) . . . . O5 S2 C28 F4 179.9(16) . . . . O5 S2 C28 F5 -60.0(18) . . . . O5 S2 C28 F6 60.1(16) . . . . O6 S2 C28 F4 -57.4(18) . . . . O6 S2 C28 F5 62.8(18) . . . . O6 S2 C28 F6 -177.1(14) . . . . N1 C1 C2 C3 -7(3) . . . . N3 C14 C15 C16 -5(2) . . . . C1 N1 C5 C4 -3(2) . . . . C1 C2 C3 C4 6(2) . . . . C1 C2 C3 C6 -179.9(14) . . . . C2 C3 C4 C5 -5(2) . . . . C2 C3 C6 C7 91(2) . . . . C2 C3 C6 C7A 67(3) . . . . C3 C4 C5 N1 3(2) . . . . C3 C6 C7 C8 -63(3) . . . . C3 C6 C7A C8A 173(4) . . . . C4 C3 C6 C7 -95(2) . . . . C4 C3 C6 C7A -118(3) . . . . C5 N1 C1 C2 5(3) . . . . C6 C3 C4 C5 -179.1(14) . . . . C6 C7 C8 C9 -175(3) . . . . C6 C7A C8A C9A -178(3) . . . . C9 C10 C11 N2 -3(3) . . . . C9 C12 C13 N2 -8(6) . . . . C10 C9 C12 C13 8(4) . . . . C10 C9 C8 C7 -102(3) . . . . C11 N2 C13 C12 1(6) . . . . C12 C9 C10 C11 -3(2) . . . . C12 C9 C8 C7 82(3) . . . . C13 N2 C11 C10 4(5) . . . . C14 N3 C18 C17 9(2) . . . . C14 C15 C16 C17 11.3(19) . . . . C14 C15 C16 C19 -177.7(13) . . . . C15 C16 C17 C18 -9(2) . . . . C15 C16 C19 C20 -75.9(19) . . . . C16 C17 C18 N3 -2(2) . . . . C16 C19 C20 C21 173.2(16) . . . . C17 C16 C19 C20 94(2) . . . . C18 N3 C14 C15 -5(2) . . . . C19 C16 C17 C18 -178.7(14) . . . . C19 C20 C21 C22 -179.8(17) . . . . C20 C21 C22 C23 51(2) . . . . C20 C21 C22 C25 -123.7(17) . . . . C21 C22 C23 C24 -179.8(15) . . . . C21 C22 C25 C26 179.4(14) . . . . C22 C23 C24 N4 3(3) . . . . C22 C25 C26 N4 -2(3) . . . . C23 C22 C25 C26 4(2) . . . . C24 N4 C26 C25 0(2) . . . . C25 C22 C23 C24 -5(2) . . . . C26 N4 C24 C23 0(2) . . . . C8 C9 C10 C11 -178.9(15) . . . . C8 C9 C12 C13 -176(3) . . . . C7A C8A C9A C10A 45(5) . . . . C7A C8A C9A C12A -137(5) . . . . C8A C9A C10A C11A 177(3) . . . . C8A C9A C12A C13A 180(4) . . . . C9A C10A C11A N2A 2(6) . . . . C9A C12A C13A N2A 4(7) . . . . C10A C9A C12A C13A -2(5) . . . . C10A C11A N2A Cu1 -178(3) . . . 2_746 C10A C11A N2A C13A 0(7) . . . . C12A C9A C10A C11A -1(4) . . . . C12A C13A N2A Cu1 174(4) . . . 2_746 C12A C13A N2A C11A -3(7) . . . .