#------------------------------------------------------------------------------ #$Date: 2021-12-07 05:40:43 +0200 (Tue, 07 Dec 2021) $ #$Revision: 271196 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/10/7061030.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_7061030 loop_ _publ_author_name 'Korchagin, D. V.' 'Ivakhnenko, E. P.' 'Demidov, O. P.' 'Akimov, A. V.' 'Morgunov, R. B.' 'Starikov, A. G.' 'Palii, A. V.' 'Minkin, V. I.' 'Aldoshin, S. M.' _publ_section_title ; Field supported slow magnetic relaxation in a quasi-one-dimensional copper(ii) complex with a pentaheterocyclic triphenodioxazine ; _journal_issue 46 _journal_name_full 'New Journal of Chemistry' _journal_page_first 21912 _journal_page_last 21918 _journal_paper_doi 10.1039/D1NJ03217H _journal_volume 45 _journal_year 2021 _chemical_compound_source 'Rostov-on-Don, Russia' _chemical_formula_moiety '2(C5 H Cu0.5 F6 O2), C26 H25 Cl N2 O2' _chemical_formula_sum 'C36 H27 Cl Cu F12 N2 O6' _chemical_formula_weight 910.58 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_cell_setting triclinic _symmetry_Int_Tables_number 2 _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2021-03-30 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-03-30 deposited with the CCDC. 2021-10-12 downloaded from the CCDC. ; _cell_angle_alpha 91.745(2) _cell_angle_beta 97.906(2) _cell_angle_gamma 105.700(2) _cell_formula_units_Z 2 _cell_length_a 9.4631(2) _cell_length_b 13.7164(3) _cell_length_c 15.5325(3) _cell_measurement_reflns_used 11750 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 75.8930 _cell_measurement_theta_min 4.2330 _cell_volume 1917.60(7) _computing_cell_refinement 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _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 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2529 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.994 _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 -114.00 -14.00 1.00 4.00 -- -41.72 -57.00-120.00 100 2 \w -116.00 -17.00 1.00 4.00 -- -41.72 -38.00 120.00 99 3 \w -70.00 31.00 1.00 4.00 -- -41.72 57.00 30.00 101 4 \w 7.00 34.00 1.00 4.00 -- 41.72 83.00 60.20 27 5 \w 8.00 42.00 1.00 4.00 -- 41.72 81.00-130.07 34 6 \w -21.00 74.00 1.00 4.00 -- 41.72 -77.00 90.00 95 7 \w 36.00 109.00 1.00 16.00 -- 112.00-111.00 120.00 73 8 \w 36.00 145.00 1.00 16.00 -- 112.00 -77.00 30.00 109 9 \w 28.00 178.00 1.00 16.00 -- 112.00 -9.00 -18.39 150 10 \w 36.00 109.00 1.00 16.00 -- 112.00-111.00 90.00 73 11 \w 36.00 140.00 1.00 16.00 -- 112.00 -30.00 60.00 104 12 \w 30.00 106.00 1.00 16.00 -- 112.00 -95.00 -30.00 76 13 \w 30.00 106.00 1.00 16.00 -- 112.00 -95.00 30.00 76 14 \w 40.00 141.00 1.00 16.00 -- 112.00 -61.00 30.00 101 15 \w 39.00 138.00 1.00 16.00 -- 112.00 -45.00 150.00 99 16 \w 36.00 109.00 1.00 16.00 -- 112.00-111.00-120.00 73 17 \w 36.00 109.00 1.00 16.00 -- 112.00-111.00 -60.00 73 18 \w 36.00 109.00 1.00 16.00 -- 112.00-111.00 0.00 73 19 \w 36.00 140.00 1.00 16.00 -- 112.00 -30.00-120.00 104 20 \w 36.00 109.00 1.00 16.00 -- 112.00-111.00-150.00 73 21 \w 36.00 109.00 1.00 16.00 -- 112.00-111.00 30.00 73 22 \w 86.00 178.00 1.00 16.00 -- 112.00 45.00 -90.00 92 23 \w 30.00 106.00 1.00 16.00 -- 112.00 -95.00 120.00 76 24 \w 104.00 178.00 1.00 16.00 -- 112.00 111.00 0.00 74 25 \w 36.00 140.00 1.00 16.00 -- 112.00 -30.00-180.00 104 26 \w 86.00 178.00 1.00 16.00 -- 112.00 45.00 -30.00 92 27 \w 61.00 146.00 1.00 16.00 -- 112.00 178.00 -60.00 85 28 \w 36.00 109.00 1.00 16.00 -- 112.00-111.00 -30.00 73 29 \w 40.00 141.00 1.00 16.00 -- 112.00 -61.00 90.00 101 30 \w 36.00 145.00 1.00 16.00 -- 112.00 -77.00 -90.00 109 31 \w 36.00 109.00 1.00 16.00 -- 112.00-111.00-180.00 73 32 \w 104.00 178.00 1.00 16.00 -- 112.00 111.00 -60.00 74 33 \w 30.00 106.00 1.00 16.00 -- 112.00 -95.00 150.00 76 34 \w 83.00 178.00 1.00 16.00 -- 112.00 61.00-180.00 95 35 \w 40.00 141.00 1.00 16.00 -- 112.00 -61.00 -30.00 101 36 \w 40.00 141.00 1.00 16.00 -- 112.00 -61.00 150.00 101 37 \w 36.00 145.00 1.00 16.00 -- 112.00 -77.00-150.00 109 38 \w 84.00 137.00 1.00 16.00 -- 112.00 -34.00 -67.69 53 39 \w 73.00 98.00 1.00 4.00 -- 41.60-125.00-120.00 25 40 \w 63.00 89.00 1.00 16.00 -- 112.00 -36.00 161.35 26 41 \w 142.00 167.00 1.00 16.00 -- 112.00 6.00 59.62 25 42 \w 107.00 133.00 1.00 16.00 -- 112.00 111.00-150.00 26 43 \w 149.00 175.00 1.00 16.00 -- 112.00 111.00-150.00 26 44 \w 30.00 76.00 1.00 16.00 -- 112.00 6.00 59.62 46 45 \w 129.00 154.00 1.00 16.00 -- 112.00 77.00 -60.00 25 46 \w 79.00 105.00 1.00 16.00 -- 112.00 178.00 0.00 26 47 \w 121.00 146.00 1.00 16.00 -- 112.00 178.00 0.00 25 48 \w 104.00 146.00 1.00 16.00 -- 112.00 45.00-150.00 42 49 \w 67.00 92.00 1.00 16.00 -- 112.00 -61.00 -60.00 25 50 \w 97.00 123.00 1.00 16.00 -- 112.00 45.00 90.00 26 51 \w 120.00 146.00 1.00 16.00 -- 112.00 45.00 120.00 26 52 \w 79.00 105.00 1.00 16.00 -- 112.00 -79.00 12.18 26 53 \w 123.00 149.00 1.00 16.00 -- 112.00 77.00 30.00 26 54 \w 53.00 79.00 1.00 16.00 -- 112.00 -95.00 0.00 26 55 \w 99.00 146.00 1.00 16.00 -- 112.00 45.00 0.00 47 56 \w 89.00 115.00 1.00 16.00 -- 112.00 61.00 90.00 26 57 \w 47.00 73.00 1.00 16.00 -- 112.00 -61.00 120.00 26 58 \w 74.00 100.00 1.00 16.00 -- 112.00 -66.00 -94.04 26 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0400800000 _diffrn_orient_matrix_UB_12 0.0881911000 _diffrn_orient_matrix_UB_13 -0.0473287000 _diffrn_orient_matrix_UB_21 0.0972188000 _diffrn_orient_matrix_UB_22 0.0757600000 _diffrn_orient_matrix_UB_23 0.0742282000 _diffrn_orient_matrix_UB_31 0.1349472000 _diffrn_orient_matrix_UB_32 0.0127714000 _diffrn_orient_matrix_UB_33 -0.0482494000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_unetI/netI 0.0272 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 47151 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.524 _diffrn_reflns_theta_min 2.880 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 2.410 _exptl_absorpt_correction_T_max 0.971 _exptl_absorpt_correction_T_min 0.899 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'reddish brown' _exptl_crystal_colour_modifier reddish _exptl_crystal_colour_primary brown _exptl_crystal_density_diffrn 1.577 _exptl_crystal_description block _exptl_crystal_F_000 918 _exptl_crystal_size_max 0.268 _exptl_crystal_size_mid 0.167 _exptl_crystal_size_min 0.062 _refine_diff_density_max 0.354 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.044 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 652 _refine_ls_number_reflns 8016 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.026 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0467 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0693P)^2^+0.4813P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1263 _refine_ls_wR_factor_ref 0.1404 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5990 _reflns_number_total 8016 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1nj03217h2.cif _cod_data_source_block ka_185_2 _cod_depositor_comments 'Adding full bibliography for 7061030.cif.' _cod_database_code 7061030 _shelx_shelxl_version_number 2014/7 _chemical_oxdiff_formula 'C36 H27 Cl Cu F12 N2 O6' _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 0.865 _shelx_estimated_absorpt_t_min 0.564 _reflns_odcompleteness_completeness 100.00 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(F22) = Uanis(F24) = Uanis(F23) Uanis(F5) = Uanis(F6) = Uanis(F2) 3. Others Sof(F16)=Sof(F17)=Sof(F18)=1-FVAR(1) Sof(F13)=Sof(F14)=Sof(F15)=FVAR(1) Sof(F5)=Sof(F6)=Sof(F2)=1-FVAR(2) Sof(F1)=Sof(F3)=Sof(F4)=FVAR(2) Sof(F9)=Sof(F12)=1-FVAR(3) Sof(F8)=Sof(F11)=FVAR(3) Sof(F10)=1-FVAR(4) Sof(F7)=FVAR(4) Sof(F24)=Sof(F22)=Sof(F23)=1-FVAR(5) Sof(F21)=Sof(F19)=Sof(F20)=FVAR(5) Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)= Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=1-FVAR(6) Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)= Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(6) 4.a Aromatic/amide H refined with riding coordinates: C7(H7), C16(H16), C13(H13), C4(H4), C2(H2), C10(H10), C30(H30), C11(H11), C35(H35) 4.b Idealised Me refined as rotating group: C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C28(H28A,H28B, H28C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C29(H29A, H29B,H29C), C27(H27A,H27B,H27C) ; _shelx_res_file ; ka_185_2.res created by SHELXL-2014/7 TITL ka_185_2_a.res in P-1 REM Old TITL REM SHELXT solution in P-1 REM R1 0.315, Rweak 0.014, Alpha 0.080, Orientation as input REM Formula found by SHELXT: C47 N2 O6 Cl2 CELL 1.54184 9.4631 13.7164 15.5325 91.745 97.906 105.7 ZERR 2 0.0002 0.0003 0.0003 0.002 0.002 0.002 LATT 1 SFAC C H Cl Cu F N O UNIT 72 54 2 2 24 4 12 EADP F22 F24 F23 EADP F5 F6 F2 L.S. 10 PLAN 20 SIZE 0.062 0.167 0.268 BOND $H list 4 fmap 2 ACTA REM REM REM WGHT 0.069300 0.481300 FVAR 0.30108 0.48804 0.76531 0.52836 0.81991 0.86219 0.51725 CU2 4 0.500000 0.500000 1.000000 10.50000 0.03973 0.06904 = 0.08172 0.03787 0.00796 0.01231 CU1 4 1.000000 0.500000 0.500000 10.50000 0.04419 0.06051 = 0.08942 0.03483 0.00047 0.00738 CL1 3 1.167555 0.936207 0.514266 11.00000 0.10356 0.06095 = 0.08804 0.02471 0.05014 0.00701 O2 7 0.681528 0.291818 0.744042 11.00000 0.05660 0.03833 = 0.05310 0.00667 0.02606 0.01168 O6 7 0.294441 0.416610 0.983334 11.00000 0.04464 0.06068 = 0.05785 0.01240 0.01340 0.01596 O5 7 0.450387 0.596435 0.920867 11.00000 0.05185 0.06096 = 0.05633 0.01838 0.01490 0.02018 O4 7 0.800613 0.409731 0.483027 11.00000 0.04915 0.05275 = 0.06182 0.01194 0.00965 0.01225 O3 7 0.941681 0.594619 0.422160 11.00000 0.05038 0.05712 = 0.06020 0.01672 0.01006 0.01601 O1 7 0.818267 0.706609 0.760371 11.00000 0.07623 0.03872 = 0.05715 0.00634 0.03374 0.01443 N2 6 0.574561 0.398141 0.867162 11.00000 0.04649 0.04333 = 0.04785 0.00757 0.01867 0.01220 N1 6 0.922231 0.599793 0.634478 11.00000 0.04793 0.04219 = 0.04615 0.00674 0.01715 0.01044 PART 1 F7 5 0.026665 0.329810 1.021419 51.00000 0.05517 0.14598 = 0.10500 0.04902 0.02120 0.00809 PART 0 C6 1 0.659051 0.446732 0.812441 11.00000 0.04393 0.04327 = 0.03998 0.00595 0.01275 0.01214 C15 1 0.841053 0.551327 0.691082 11.00000 0.04226 0.04172 = 0.03926 0.00518 0.01130 0.01061 C17 1 0.715354 0.394054 0.747818 11.00000 0.04343 0.03742 = 0.04349 0.00616 0.01347 0.01118 PART 1 F8 5 -0.075555 0.397350 0.918320 41.00000 0.05057 0.17118 = 0.15490 0.07104 -0.02378 0.00992 PART 0 C8 1 0.785403 0.603730 0.756160 11.00000 0.04834 0.03918 = 0.04200 0.00484 0.01324 0.01178 C14 1 0.952774 0.705019 0.639839 11.00000 0.04527 0.04140 = 0.04285 0.00646 0.01059 0.00942 PART 1 F21 5 0.520761 0.337298 0.526505 61.00000 0.07674 0.13533 = 0.09811 0.02739 0.04059 0.00023 PART 0 C7 1 0.699863 0.554540 0.813103 11.00000 0.05644 0.04236 = 0.04520 0.00350 0.02185 0.01423 AFIX 43 H7 2 0.667230 0.591765 0.853303 11.00000 -1.20000 AFIX 0 C9 1 0.900788 0.757856 0.701256 11.00000 0.05587 0.04251 = 0.04670 0.00746 0.01676 0.01082 C5 1 0.534436 0.292435 0.858134 11.00000 0.04435 0.04286 = 0.04699 0.00856 0.01424 0.01097 C16 1 0.802390 0.443553 0.691264 11.00000 0.05133 0.04141 = 0.04460 0.00481 0.01995 0.01348 AFIX 43 H16 2 0.837263 0.406509 0.652068 11.00000 -1.20000 AFIX 0 C18 1 0.585433 0.238544 0.796600 11.00000 0.04432 0.04271 = 0.04675 0.00950 0.01548 0.01048 C1 1 0.540732 0.133065 0.784300 11.00000 0.05420 0.04146 = 0.05315 0.00738 0.01549 0.01094 C36 1 0.322664 0.592688 0.884566 11.00000 0.06224 0.05949 = 0.05146 0.00706 0.00278 0.02594 PART 1 F11 5 0.026703 0.282365 0.897440 41.00000 0.11087 0.11166 = 0.16193 -0.03575 0.02045 -0.02995 PART 0 C3 1 0.384553 0.133116 0.899135 11.00000 0.05124 0.05034 = 0.05991 0.01514 0.02147 0.01070 C13 1 1.038253 0.762804 0.582552 11.00000 0.05680 0.04670 = 0.05201 0.00747 0.01979 0.00924 AFIX 43 H13 2 1.076785 0.731012 0.541398 11.00000 -1.20000 AFIX 0 C31 1 0.689488 0.428442 0.440974 11.00000 0.04510 0.06361 = 0.05248 0.00576 0.00686 0.01193 C32 1 0.811494 0.588619 0.388961 11.00000 0.05667 0.06076 = 0.04818 0.00977 0.00737 0.02139 C37 1 0.187405 0.439021 0.940033 11.00000 0.04518 0.06371 = 0.05471 0.00037 0.00724 0.01714 C4 1 0.433511 0.237074 0.909349 11.00000 0.05000 0.05163 = 0.05571 0.01075 0.02313 0.01439 AFIX 43 H4 2 0.399338 0.271501 0.950867 11.00000 -1.20000 AFIX 0 PART 1 F19 5 0.556880 0.256047 0.420904 61.00000 0.12296 0.07459 = 0.18564 -0.03793 0.05018 -0.02219 PART 0 C2 1 0.439410 0.082994 0.836651 11.00000 0.05931 0.04245 = 0.06445 0.01018 0.02184 0.00708 AFIX 43 H2 2 0.406289 0.012504 0.829841 11.00000 -1.20000 AFIX 0 C19 1 0.595710 0.075295 0.715378 11.00000 0.07338 0.04457 = 0.06163 0.00303 0.02488 0.01260 C12 1 1.064849 0.866579 0.587467 11.00000 0.06276 0.04966 = 0.05688 0.01357 0.01907 0.00902 C10 1 0.928222 0.861666 0.705846 11.00000 0.08625 0.04382 = 0.06709 0.00628 0.03426 0.01711 AFIX 43 H10 2 0.891171 0.894145 0.747288 11.00000 -1.20000 AFIX 0 PART 1 F20 5 0.428418 0.362446 0.400498 61.00000 0.05655 0.20106 = 0.20541 0.12154 -0.04300 -0.02045 PART 0 C39 1 0.036169 0.363373 0.944401 11.00000 0.05189 0.07684 = 0.08745 0.00643 0.00457 0.01111 C30 1 0.683836 0.511870 0.395002 11.00000 0.05213 0.07499 = 0.07408 0.01968 0.00165 0.01832 AFIX 43 H30 2 0.592654 0.516897 0.367446 11.00000 -1.20000 AFIX 0 PART 1 F1 5 0.337748 0.764054 0.875088 31.00000 0.26387 0.07424 = 0.15425 0.01117 0.02531 0.08820 PART 0 C11 1 1.011515 0.917491 0.648228 11.00000 0.08649 0.04166 = 0.07427 0.01285 0.02973 0.01266 AFIX 43 H11 2 1.031214 0.987797 0.650328 11.00000 -1.20000 AFIX 0 C34 1 0.545180 0.346033 0.445432 11.00000 0.05627 0.08169 = 0.08176 0.02357 0.00327 0.00416 C35 1 0.191514 0.521227 0.890820 11.00000 0.05409 0.07255 = 0.08562 0.01462 -0.00528 0.02177 AFIX 43 H35 2 0.103253 0.528646 0.861002 11.00000 -1.20000 AFIX 0 C38 1 0.316403 0.680603 0.828159 11.00000 0.08776 0.06652 = 0.09964 0.02502 -0.01629 0.01593 PART 1 F3 5 0.436992 0.705904 0.785582 31.00000 0.16717 0.14775 = 0.13217 0.09449 0.05510 0.05873 PART 0 C23 1 0.264475 0.073226 0.949899 11.00000 0.06607 0.05497 = 0.08575 0.01346 0.04093 0.00358 PART 1 F13 5 0.666447 0.696259 0.334665 21.00000 0.11657 0.14535 = 0.13675 0.07898 0.04913 0.09222 PART 0 C33 1 0.795622 0.678640 0.336097 11.00000 0.07174 0.08245 = 0.08167 0.03208 0.00666 0.02524 C21 1 0.764472 0.096820 0.735050 11.00000 0.07733 0.06570 = 0.09441 0.00155 0.03358 0.02974 AFIX 137 H21A 2 0.810030 0.167875 0.731408 11.00000 -1.50000 H21B 2 0.797516 0.058144 0.693431 11.00000 -1.50000 H21C 2 0.791871 0.077963 0.792667 11.00000 -1.50000 AFIX 0 PART 1 F4 5 0.203465 0.665163 0.769970 31.00000 0.13445 0.17389 = 0.23593 0.12698 -0.11000 -0.01548 PART 0 C20 1 0.528310 -0.039211 0.714986 11.00000 0.12047 0.04760 = 0.09299 -0.00227 0.04751 0.01218 AFIX 137 H20A 2 0.557368 -0.061869 0.770829 11.00000 -1.50000 H20B 2 0.563155 -0.072975 0.670719 11.00000 -1.50000 H20C 2 0.422016 -0.054806 0.703164 11.00000 -1.50000 AFIX 0 C22 1 0.549688 0.107914 0.624542 11.00000 0.10257 0.07133 = 0.05978 -0.00542 0.02061 0.01543 AFIX 137 H22A 2 0.445256 0.102167 0.616012 11.00000 -1.50000 H22B 2 0.570807 0.064901 0.581024 11.00000 -1.50000 H22C 2 0.604214 0.177077 0.619770 11.00000 -1.50000 AFIX 0 PART 1 F14 5 0.897045 0.760949 0.361079 21.00000 0.14892 0.07409 = 0.17970 0.06006 -0.06786 -0.00751 C28 1 0.287678 0.110618 1.036934 71.00000 0.12380 0.09850 = 0.08245 0.01958 0.05166 -0.01641 AFIX 137 H28A 2 0.295224 0.181896 1.039484 71.00000 -1.50000 H28B 2 0.377919 0.100137 1.066333 71.00000 -1.50000 H28C 2 0.205826 0.075502 1.064759 71.00000 -1.50000 AFIX 0 C24 1 0.113233 0.084182 0.897287 71.00000 0.05522 0.10387 = 0.11696 0.02642 0.03605 0.00758 AFIX 137 H24A 2 0.101808 0.056981 0.838258 71.00000 -1.50000 H24B 2 0.115556 0.154600 0.897625 71.00000 -1.50000 H24C 2 0.031248 0.047563 0.924292 71.00000 -1.50000 AFIX 0 C26 1 0.242102 -0.041169 0.941087 71.00000 0.09970 0.06486 = 0.17144 0.04767 0.08696 0.01898 AFIX 137 H26A 2 0.167095 -0.074224 0.974569 71.00000 -1.50000 H26B 2 0.333693 -0.056003 0.962218 71.00000 -1.50000 H26C 2 0.211433 -0.065305 0.880925 71.00000 -1.50000 AFIX 0 F15 5 0.800416 0.659740 0.254409 21.00000 0.26960 0.19375 = 0.07249 0.06985 0.07149 0.15330 PART 0 PART 2 F16 5 0.799703 0.753586 0.391615 -21.00000 0.25372 0.08317 = 0.16553 0.02913 0.01972 0.08678 F17 5 0.682491 0.663346 0.284368 -21.00000 0.13396 0.16447 = 0.20792 0.11639 -0.09751 -0.01569 F18 5 0.907164 0.711817 0.298450 -21.00000 0.11273 0.22152 = 0.17366 0.15682 0.03880 0.04102 F5 5 0.280264 0.652427 0.750075 -31.00000 0.13837 0.10679 = 0.07680 0.03696 0.00068 0.06341 F6 5 0.408518 0.750009 0.840921 -31.00000 0.13837 0.10679 = 0.07680 0.03696 0.00068 0.06341 F2 5 0.187711 0.708466 0.838553 -31.00000 0.13837 0.10679 = 0.07680 0.03696 0.00068 0.06341 F9 5 -0.071301 0.410630 0.940182 -41.00000 0.05045 0.09833 = 0.16992 -0.01243 0.02980 0.03051 F12 5 -0.009174 0.296829 0.875137 -41.00000 0.07837 0.10865 = 0.11923 -0.05058 0.00589 -0.00894 F10 5 0.045085 0.297055 1.000730 -51.00000 0.05440 0.12672 = 0.17465 0.04652 0.04779 -0.00043 F24 5 0.438946 0.382333 0.449960 -61.00000 0.04462 0.11657 = 0.14308 0.00403 0.01546 0.00198 F22 5 0.550697 0.279140 0.483637 -61.00000 0.04462 0.11657 = 0.14308 0.00403 0.01546 0.00198 F23 5 0.488229 0.303830 0.366702 -61.00000 0.04462 0.11657 = 0.14308 0.00403 0.01546 0.00198 C25 1 0.129306 0.034744 0.892578 -71.00000 0.06999 0.19335 = 0.10173 -0.00682 0.02135 -0.03291 AFIX 137 H25A 2 0.054713 -0.003060 0.924221 -71.00000 -1.50000 H25B 2 0.143354 -0.008929 0.846966 -71.00000 -1.50000 H25C 2 0.098097 0.090100 0.867636 -71.00000 -1.50000 AFIX 0 C29 1 0.245306 0.140198 1.030248 -71.00000 0.08336 0.07576 = 0.08112 0.01429 0.05355 0.00668 AFIX 137 H29A 2 0.200584 0.191712 1.009365 -71.00000 -1.50000 H29B 2 0.340832 0.171629 1.063899 -71.00000 -1.50000 H29C 2 0.182903 0.097781 1.066100 -71.00000 -1.50000 AFIX 0 C27 1 0.320411 -0.012569 0.996962 -71.00000 0.15589 0.09222 = 0.13907 0.06461 0.09451 0.04490 AFIX 137 H27A 2 0.254042 -0.042261 1.036555 -71.00000 -1.50000 H27B 2 0.418294 0.016226 1.028707 -71.00000 -1.50000 H27C 2 0.322980 -0.063947 0.954299 -71.00000 -1.50000 AFIX 0 HKLF 4 REM ka_185_2_a.res in P-1 REM R1 = 0.0467 for 5990 Fo > 4sig(Fo) and 0.0621 for all 8016 data REM 652 parameters refined using 0 restraints END WGHT 0.0693 0.4809 REM Highest difference peak 0.354, deepest hole -0.362, 1-sigma level 0.044 Q1 1 0.2114 0.7235 0.8833 11.00000 0.05 0.35 Q2 1 0.4741 0.3858 0.5001 11.00000 0.05 0.33 Q3 1 -0.0231 0.4003 1.0106 11.00000 0.05 0.28 Q4 1 0.3451 0.6405 0.7517 11.00000 0.05 0.26 Q5 1 0.3788 0.7735 0.8749 11.00000 0.05 0.25 Q6 1 0.2291 0.6186 0.7491 11.00000 0.05 0.25 Q7 1 0.4647 0.5631 0.9380 11.00000 0.05 0.24 Q8 1 0.1490 0.6703 0.8224 11.00000 0.05 0.22 Q9 1 0.9370 0.7347 0.6818 11.00000 0.05 0.21 Q10 1 0.9417 0.5550 0.4330 11.00000 0.05 0.20 Q11 1 0.7220 0.5002 0.3702 11.00000 0.05 0.20 Q12 1 0.5361 0.2984 0.3611 11.00000 0.05 0.20 Q13 1 0.7995 0.6221 0.3647 11.00000 0.05 0.20 Q14 1 0.4127 0.5967 0.9288 11.00000 0.05 0.19 Q15 1 0.8814 0.5177 0.4606 11.00000 0.05 0.19 Q16 1 0.8846 0.6026 0.4294 11.00000 0.05 0.19 Q17 1 0.7822 0.3998 0.4617 11.00000 0.05 0.19 Q18 1 0.4441 0.7287 0.8184 11.00000 0.05 0.19 Q19 1 0.2809 0.4043 0.9613 11.00000 0.05 0.19 Q20 1 0.2736 0.5486 0.8685 11.00000 0.05 0.19 ; _shelx_res_checksum 91103 _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 1.596 _oxdiff_exptl_absorpt_empirical_full_min 0.769 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 Cu2 Cu 0.5000 0.5000 1.0000 0.06347(16) Uani 1 2 d S T P . . Cu1 Cu 1.0000 0.5000 0.5000 0.06643(17) Uani 1 2 d S T P . . Cl1 Cl 1.16756(9) 0.93621(5) 0.51427(5) 0.0834(2) Uani 1 1 d . . . . . O2 O 0.68153(16) 0.29182(10) 0.74404(9) 0.0478(3) Uani 1 1 d . . . . . O6 O 0.29444(16) 0.41661(12) 0.98333(10) 0.0534(3) Uani 1 1 d . . . . . O5 O 0.45039(17) 0.59644(12) 0.92087(10) 0.0545(4) Uani 1 1 d . . . . . O4 O 0.80061(17) 0.40973(12) 0.48303(11) 0.0547(3) Uani 1 1 d . . . . . O3 O 0.94168(17) 0.59462(12) 0.42216(11) 0.0553(4) Uani 1 1 d . . . . . O1 O 0.81827(19) 0.70661(11) 0.76037(10) 0.0553(4) Uani 1 1 d . . . . . N2 N 0.57456(18) 0.39814(12) 0.86716(11) 0.0447(3) Uani 1 1 d . . . . . N1 N 0.92223(18) 0.59979(12) 0.63448(11) 0.0448(3) Uani 1 1 d . . . . . F7 F 0.0267(11) 0.3298(15) 1.0214(8) 0.104(3) Uani 0.82(7) 1 d . . . A 1 C6 C 0.6591(2) 0.44673(14) 0.81244(12) 0.0417(4) Uani 1 1 d . . . . . C15 C 0.8411(2) 0.55133(14) 0.69108(12) 0.0407(4) Uani 1 1 d . . . . . C17 C 0.7154(2) 0.39405(14) 0.74782(12) 0.0407(4) Uani 1 1 d . . . . . F8 F -0.0756(11) 0.3973(14) 0.9183(13) 0.132(4) Uani 0.53(4) 1 d . . . A 1 C8 C 0.7854(2) 0.60373(14) 0.75616(12) 0.0426(4) Uani 1 1 d . . . . . C14 C 0.9528(2) 0.70502(15) 0.63984(13) 0.0432(4) Uani 1 1 d . . . . . F21 F 0.5208(3) 0.3373(3) 0.52651(18) 0.1061(12) Uani 0.862(7) 1 d . . . B 1 C7 C 0.6999(2) 0.55454(15) 0.81310(13) 0.0465(4) Uani 1 1 d . . . . . H7 H 0.6672 0.5918 0.8533 0.056 Uiso 1 1 calc R . . . . C9 C 0.9008(2) 0.75786(15) 0.70126(14) 0.0479(4) Uani 1 1 d . . . . . C5 C 0.5344(2) 0.29244(15) 0.85813(13) 0.0441(4) Uani 1 1 d . . . . . C16 C 0.8024(2) 0.44355(15) 0.69126(13) 0.0444(4) Uani 1 1 d . . . . . H16 H 0.8373 0.4065 0.6521 0.053 Uiso 1 1 calc R . . . . C18 C 0.5854(2) 0.23854(15) 0.79660(13) 0.0439(4) Uani 1 1 d . . . . . C1 C 0.5407(2) 0.13307(16) 0.78430(14) 0.0493(4) Uani 1 1 d . . . . . C36 C 0.3227(3) 0.59269(19) 0.88457(15) 0.0564(5) Uani 1 1 d . . . . . F11 F 0.027(3) 0.2824(18) 0.8974(17) 0.141(6) Uani 0.53(4) 1 d . . . A 1 C3 C 0.3846(2) 0.13312(17) 0.89914(15) 0.0530(5) Uani 1 1 d . . . . . C13 C 1.0383(2) 0.76280(16) 0.58255(14) 0.0516(5) Uani 1 1 d . . . . . H13 H 1.0768 0.7310 0.5414 0.062 Uiso 1 1 calc R . . . . C31 C 0.6895(2) 0.42844(19) 0.44097(15) 0.0544(5) Uani 1 1 d . . . . . C32 C 0.8115(3) 0.58862(18) 0.38896(15) 0.0541(5) Uani 1 1 d . . . . . C37 C 0.1874(2) 0.43902(19) 0.94003(15) 0.0542(5) Uani 1 1 d . . . . . C4 C 0.4335(2) 0.23707(17) 0.90935(15) 0.0508(5) Uani 1 1 d . . . . . H4 H 0.3993 0.2715 0.9509 0.061 Uiso 1 1 calc R . . . . F19 F 0.5569(4) 0.2560(2) 0.4209(3) 0.1359(17) Uani 0.862(7) 1 d . . . B 1 C2 C 0.4394(3) 0.08299(17) 0.83665(16) 0.0554(5) Uani 1 1 d . . . . . H2 H 0.4063 0.0125 0.8298 0.067 Uiso 1 1 calc R . . . . C19 C 0.5957(3) 0.07529(17) 0.71538(16) 0.0592(5) Uani 1 1 d . . . . . C12 C 1.0648(3) 0.86658(17) 0.58747(16) 0.0565(5) Uani 1 1 d . . . . . C10 C 0.9282(3) 0.86167(18) 0.70585(17) 0.0636(6) Uani 1 1 d . . . . . H10 H 0.8912 0.8941 0.7473 0.076 Uiso 1 1 calc R . . . . F20 F 0.4284(4) 0.3624(5) 0.4005(3) 0.169(3) Uani 0.862(7) 1 d . . . B 1 C39 C 0.0362(3) 0.3634(3) 0.9444(2) 0.0740(7) Uani 1 1 d . . . . . C30 C 0.6838(3) 0.5119(2) 0.39500(19) 0.0674(6) Uani 1 1 d . . . . . H30 H 0.5927 0.5169 0.3674 0.081 Uiso 1 1 calc R . . . . F1 F 0.3377(8) 0.7641(3) 0.8751(3) 0.157(2) Uani 0.765(8) 1 d . . . C 1 C11 C 1.0115(3) 0.91749(18) 0.64823(18) 0.0666(6) Uani 1 1 d . . . . . H11 H 1.0312 0.9878 0.6503 0.080 Uiso 1 1 calc R . . . . C34 C 0.5452(3) 0.3460(3) 0.4454(2) 0.0765(8) Uani 1 1 d . . . . . C35 C 0.1915(3) 0.5212(2) 0.8908(2) 0.0713(7) Uani 1 1 d . . . . . H35 H 0.1033 0.5286 0.8610 0.086 Uiso 1 1 calc R . . . . C38 C 0.3164(4) 0.6806(3) 0.8282(3) 0.0883(10) Uani 1 1 d . . . . . F3 F 0.4370(5) 0.7059(4) 0.7856(3) 0.141(2) Uani 0.765(8) 1 d . . . C 1 C23 C 0.2645(3) 0.0732(2) 0.9499(2) 0.0685(7) Uani 1 1 d . . . . . F13 F 0.6664(10) 0.6963(8) 0.3347(7) 0.117(4) Uani 0.488(15) 1 d . . . D 1 C33 C 0.7956(3) 0.6786(3) 0.3361(2) 0.0778(8) Uani 1 1 d . . . . . C21 C 0.7645(3) 0.0968(2) 0.7351(2) 0.0753(7) Uani 1 1 d . . . . . H21A H 0.8100 0.1679 0.7314 0.113 Uiso 1 1 calc GR . . . . H21B H 0.7975 0.0581 0.6934 0.113 Uiso 1 1 calc GR . . . . H21C H 0.7919 0.0780 0.7927 0.113 Uiso 1 1 calc GR . . . . F4 F 0.2035(6) 0.6652(5) 0.7700(5) 0.204(5) Uani 0.765(8) 1 d . . . C 1 C20 C 0.5283(4) -0.0392(2) 0.7150(2) 0.0863(9) Uani 1 1 d . . . . . H20A H 0.5574 -0.0619 0.7708 0.129 Uiso 1 1 calc GR . . . . H20B H 0.5632 -0.0730 0.6707 0.129 Uiso 1 1 calc GR . . . . H20C H 0.4220 -0.0548 0.7032 0.129 Uiso 1 1 calc GR . . . . C22 C 0.5497(4) 0.1079(2) 0.62454(18) 0.0790(8) Uani 1 1 d . . . . . H22A H 0.4453 0.1022 0.6160 0.119 Uiso 1 1 calc GR . . . . H22B H 0.5708 0.0649 0.5810 0.119 Uiso 1 1 calc GR . . . . H22C H 0.6042 0.1771 0.6198 0.119 Uiso 1 1 calc GR . . . . F14 F 0.8970(14) 0.7609(6) 0.3611(10) 0.150(7) Uani 0.488(15) 1 d . . . D 1 C28 C 0.288(2) 0.1106(15) 1.0369(11) 0.107(5) Uani 0.52(3) 1 d . . . E 1 H28A H 0.2952 0.1819 1.0395 0.161 Uiso 0.52(3) 1 calc GR . . E 1 H28B H 0.3779 0.1001 1.0663 0.161 Uiso 0.52(3) 1 calc GR . . E 1 H28C H 0.2058 0.0755 1.0648 0.161 Uiso 0.52(3) 1 calc GR . . E 1 C24 C 0.1132(14) 0.0842(10) 0.8973(11) 0.092(3) Uani 0.52(3) 1 d . . . E 1 H24A H 0.1018 0.0570 0.8383 0.138 Uiso 0.52(3) 1 calc GR . . E 1 H24B H 0.1156 0.1546 0.8976 0.138 Uiso 0.52(3) 1 calc GR . . E 1 H24C H 0.0312 0.0476 0.9243 0.138 Uiso 0.52(3) 1 calc GR . . E 1 C26 C 0.2421(17) -0.0412(7) 0.9411(16) 0.105(5) Uani 0.52(3) 1 d . . . E 1 H26A H 0.1671 -0.0742 0.9746 0.158 Uiso 0.52(3) 1 calc GR . . E 1 H26B H 0.3337 -0.0560 0.9622 0.158 Uiso 0.52(3) 1 calc GR . . E 1 H26C H 0.2114 -0.0653 0.8809 0.158 Uiso 0.52(3) 1 calc GR . . E 1 F15 F 0.800(2) 0.6597(10) 0.2544(5) 0.155(6) Uani 0.488(15) 1 d . . . D 1 F16 F 0.800(2) 0.7536(8) 0.3916(6) 0.160(5) Uani 0.512(15) 1 d . . . D 2 F17 F 0.6825(13) 0.6633(10) 0.2844(11) 0.190(8) Uani 0.512(15) 1 d . . . D 2 F18 F 0.9072(10) 0.7118(12) 0.2984(10) 0.166(5) Uani 0.512(15) 1 d . . . D 2 F5 F 0.2803(17) 0.6524(10) 0.7501(8) 0.102(3) Uani 0.235(8) 1 d . . . C 2 F6 F 0.4085(15) 0.7500(11) 0.8409(8) 0.102(3) Uani 0.235(8) 1 d . . . C 2 F2 F 0.1877(16) 0.7085(9) 0.8386(7) 0.102(3) Uani 0.235(8) 1 d . . . C 2 F9 F -0.0713(11) 0.4106(9) 0.9402(11) 0.103(3) Uani 0.47(4) 1 d . . . A 2 F12 F -0.0092(19) 0.2968(16) 0.8751(13) 0.111(4) Uani 0.47(4) 1 d . . . A 2 F10 F 0.045(4) 0.297(7) 1.001(5) 0.120(11) Uani 0.18(7) 1 d . . . A 2 F24 F 0.439(2) 0.3823(18) 0.4500(16) 0.105(5) Uani 0.138(7) 1 d . . . B 2 F22 F 0.5507(14) 0.2791(17) 0.4836(17) 0.105(5) Uani 0.138(7) 1 d . . . B 2 F23 F 0.4882(17) 0.3038(17) 0.3667(15) 0.105(5) Uani 0.138(7) 1 d . . . B 2 C25 C 0.1293(18) 0.035(2) 0.8926(11) 0.135(9) Uani 0.48(3) 1 d . . . E 2 H25A H 0.0547 -0.0031 0.9242 0.202 Uiso 0.48(3) 1 calc GR . . E 2 H25B H 0.1434 -0.0089 0.8470 0.202 Uiso 0.48(3) 1 calc GR . . E 2 H25C H 0.0981 0.0901 0.8676 0.202 Uiso 0.48(3) 1 calc GR . . E 2 C29 C 0.2453(17) 0.1402(11) 1.0302(11) 0.079(3) Uani 0.48(3) 1 d . . . E 2 H29A H 0.2006 0.1917 1.0094 0.118 Uiso 0.48(3) 1 calc GR . . E 2 H29B H 0.3408 0.1716 1.0639 0.118 Uiso 0.48(3) 1 calc GR . . E 2 H29C H 0.1829 0.0978 1.0661 0.118 Uiso 0.48(3) 1 calc GR . . E 2 C27 C 0.320(3) -0.0126(14) 0.9970(15) 0.119(6) Uani 0.48(3) 1 d . . . E 2 H27A H 0.2540 -0.0423 1.0366 0.178 Uiso 0.48(3) 1 calc GR . . E 2 H27B H 0.4183 0.0162 1.0287 0.178 Uiso 0.48(3) 1 calc GR . . E 2 H27C H 0.3230 -0.0639 0.9543 0.178 Uiso 0.48(3) 1 calc GR . . E 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 Cu2 0.0397(2) 0.0690(3) 0.0817(3) 0.0379(3) 0.0080(2) 0.01231(19) Cu1 0.0442(2) 0.0605(3) 0.0894(4) 0.0348(3) 0.0005(2) 0.00738(19) Cl1 0.1036(5) 0.0609(4) 0.0880(5) 0.0247(3) 0.0501(4) 0.0070(3) O2 0.0566(8) 0.0383(7) 0.0531(8) 0.0067(6) 0.0261(6) 0.0117(6) O6 0.0446(7) 0.0607(9) 0.0578(8) 0.0124(7) 0.0134(6) 0.0160(6) O5 0.0518(8) 0.0610(9) 0.0563(8) 0.0184(7) 0.0149(7) 0.0202(7) O4 0.0491(8) 0.0527(8) 0.0618(9) 0.0119(7) 0.0096(7) 0.0122(6) O3 0.0504(8) 0.0571(9) 0.0602(9) 0.0167(7) 0.0101(7) 0.0160(6) O1 0.0762(10) 0.0387(7) 0.0572(8) 0.0063(6) 0.0337(8) 0.0144(6) N2 0.0465(8) 0.0433(8) 0.0479(9) 0.0076(7) 0.0187(7) 0.0122(6) N1 0.0479(8) 0.0422(8) 0.0461(8) 0.0067(7) 0.0171(7) 0.0104(6) F7 0.055(2) 0.146(5) 0.105(4) 0.049(3) 0.0212(17) 0.008(3) C6 0.0439(9) 0.0433(9) 0.0400(9) 0.0060(7) 0.0127(7) 0.0121(7) C15 0.0423(9) 0.0417(9) 0.0393(9) 0.0052(7) 0.0113(7) 0.0106(7) C17 0.0434(9) 0.0374(9) 0.0435(9) 0.0062(7) 0.0135(7) 0.0112(7) F8 0.051(3) 0.171(9) 0.155(7) 0.071(6) -0.024(4) 0.010(4) C8 0.0483(9) 0.0392(9) 0.0420(9) 0.0048(7) 0.0132(8) 0.0118(7) C14 0.0453(9) 0.0414(9) 0.0428(9) 0.0065(7) 0.0106(8) 0.0094(7) F21 0.0767(14) 0.135(3) 0.0981(18) 0.0274(16) 0.0406(13) 0.0002(14) C7 0.0564(11) 0.0424(10) 0.0452(10) 0.0035(8) 0.0218(9) 0.0142(8) C9 0.0559(11) 0.0425(10) 0.0467(10) 0.0075(8) 0.0168(9) 0.0108(8) C5 0.0443(9) 0.0429(9) 0.0470(10) 0.0086(8) 0.0142(8) 0.0110(7) C16 0.0513(10) 0.0414(9) 0.0446(10) 0.0048(7) 0.0199(8) 0.0135(8) C18 0.0443(9) 0.0427(10) 0.0467(10) 0.0095(8) 0.0155(8) 0.0105(7) C1 0.0542(11) 0.0415(10) 0.0531(11) 0.0074(8) 0.0155(9) 0.0109(8) C36 0.0622(13) 0.0595(13) 0.0515(11) 0.0071(10) 0.0028(10) 0.0259(10) F11 0.111(10) 0.112(7) 0.162(12) -0.036(8) 0.020(8) -0.030(7) C3 0.0512(11) 0.0503(11) 0.0599(12) 0.0151(9) 0.0215(9) 0.0107(9) C13 0.0568(11) 0.0467(11) 0.0520(11) 0.0075(9) 0.0198(9) 0.0092(8) C31 0.0451(10) 0.0636(13) 0.0525(11) 0.0058(10) 0.0069(9) 0.0119(9) C32 0.0567(12) 0.0608(13) 0.0482(11) 0.0098(9) 0.0074(9) 0.0214(10) C37 0.0452(10) 0.0637(13) 0.0547(12) 0.0004(10) 0.0072(9) 0.0171(9) C4 0.0500(10) 0.0516(11) 0.0557(11) 0.0108(9) 0.0231(9) 0.0144(8) F19 0.123(3) 0.0746(17) 0.186(4) -0.038(2) 0.050(3) -0.0222(16) C2 0.0593(12) 0.0425(10) 0.0645(13) 0.0102(9) 0.0218(10) 0.0071(9) C19 0.0734(14) 0.0446(11) 0.0616(13) 0.0030(9) 0.0249(11) 0.0126(10) C12 0.0628(13) 0.0497(11) 0.0569(12) 0.0136(9) 0.0191(10) 0.0090(9) C10 0.0862(17) 0.0438(11) 0.0671(14) 0.0063(10) 0.0343(13) 0.0171(11) F20 0.0565(14) 0.201(5) 0.205(5) 0.122(4) -0.043(2) -0.020(2) C39 0.0519(13) 0.0768(19) 0.087(2) 0.0064(17) 0.0046(13) 0.0111(12) C30 0.0521(12) 0.0750(16) 0.0741(16) 0.0197(13) 0.0017(11) 0.0183(11) F1 0.264(7) 0.074(2) 0.154(4) 0.011(2) 0.025(4) 0.088(3) C11 0.0865(17) 0.0417(11) 0.0743(16) 0.0128(10) 0.0297(13) 0.0127(11) C34 0.0563(15) 0.082(2) 0.0818(19) 0.0236(16) 0.0033(13) 0.0042(13) C35 0.0541(13) 0.0725(16) 0.0856(18) 0.0146(14) -0.0053(12) 0.0218(11) C38 0.088(2) 0.0665(18) 0.100(3) 0.0250(17) -0.0163(18) 0.0159(16) F3 0.167(4) 0.148(4) 0.132(3) 0.094(3) 0.055(3) 0.059(3) C23 0.0661(14) 0.0550(13) 0.0858(18) 0.0135(12) 0.0409(13) 0.0036(10) F13 0.117(6) 0.145(7) 0.137(7) 0.079(6) 0.049(6) 0.092(6) C33 0.0717(17) 0.082(2) 0.0817(19) 0.0321(16) 0.0067(15) 0.0252(15) C21 0.0773(17) 0.0657(15) 0.094(2) 0.0015(14) 0.0336(15) 0.0297(13) F4 0.134(4) 0.174(5) 0.236(7) 0.127(5) -0.110(5) -0.015(3) C20 0.120(3) 0.0476(14) 0.093(2) -0.0023(13) 0.0475(19) 0.0122(14) C22 0.103(2) 0.0713(17) 0.0598(15) -0.0054(13) 0.0206(14) 0.0154(15) F14 0.149(8) 0.074(4) 0.180(12) 0.060(5) -0.068(8) -0.008(4) C28 0.124(12) 0.099(10) 0.082(5) 0.020(6) 0.052(7) -0.016(7) C24 0.055(3) 0.104(7) 0.117(8) 0.026(6) 0.036(4) 0.008(5) C26 0.100(7) 0.065(4) 0.171(13) 0.048(6) 0.087(8) 0.019(4) F15 0.270(15) 0.194(9) 0.072(4) 0.070(5) 0.071(7) 0.153(11) F16 0.254(15) 0.083(5) 0.166(7) 0.029(5) 0.020(9) 0.087(8) F17 0.134(8) 0.164(9) 0.208(13) 0.116(9) -0.098(8) -0.016(6) F18 0.113(6) 0.222(11) 0.174(9) 0.157(8) 0.039(6) 0.041(7) F5 0.138(7) 0.107(5) 0.077(5) 0.037(3) 0.001(4) 0.063(5) F6 0.138(7) 0.107(5) 0.077(5) 0.037(3) 0.001(4) 0.063(5) F2 0.138(7) 0.107(5) 0.077(5) 0.037(3) 0.001(4) 0.063(5) F9 0.050(4) 0.098(5) 0.170(8) -0.012(5) 0.030(5) 0.031(3) F12 0.078(5) 0.109(6) 0.119(7) -0.051(6) 0.006(4) -0.009(4) F10 0.054(8) 0.13(3) 0.17(3) 0.05(2) 0.048(15) 0.000(9) F24 0.045(4) 0.117(8) 0.143(12) 0.004(9) 0.015(5) 0.002(4) F22 0.045(4) 0.117(8) 0.143(12) 0.004(9) 0.015(5) 0.002(4) F23 0.045(4) 0.117(8) 0.143(12) 0.004(9) 0.015(5) 0.002(4) C25 0.070(7) 0.19(2) 0.102(7) -0.007(12) 0.021(6) -0.033(10) C29 0.083(6) 0.076(6) 0.081(6) 0.014(4) 0.054(5) 0.007(4) C27 0.156(13) 0.092(8) 0.139(12) 0.065(8) 0.095(11) 0.045(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -3 0 -8 0.0836 2 -1 -10 0.0962 -4 7 -4 0.0425 5 -7 -2 0.0484 3 -8 2 0.0369 -3 8 -2 0.0277 5 -6 -4 0.0484 4 -7 -3 0.0404 1 -9 1 0.0589 -5 1 6 0.1064 6 0 -5 0.1111 6 0 2 0.1090 2 -5 8 0.0656 3 -7 5 0.0495 4 -8 1 0.0307 -3 8 -2 0.0277 2 -9 0 0.0470 -3 9 1 0.0307 4 -7 -5 0.0511 -3 8 4 0.0408 -2 -5 -6 0.0893 -3 4 8 0.0618 0 -3 -9 0.0749 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 O6 Cu2 O6 180.00(9) 2_667 . ? O5 Cu2 O6 88.35(7) . 2_667 ? O5 Cu2 O6 88.35(7) 2_667 . ? O5 Cu2 O6 91.65(7) 2_667 2_667 ? O5 Cu2 O6 91.65(7) . . ? O5 Cu2 O5 180.00(9) . 2_667 ? O4 Cu1 O4 180.0 2_766 . ? O4 Cu1 O3 87.89(7) 2_766 . ? O4 Cu1 O3 87.89(7) . 2_766 ? O4 Cu1 O3 92.11(7) . . ? O4 Cu1 O3 92.11(7) 2_766 2_766 ? O3 Cu1 O3 180.00(8) . 2_766 ? C17 O2 C18 119.65(15) . . ? C37 O6 Cu2 125.14(15) . . ? C36 O5 Cu2 125.31(15) . . ? C31 O4 Cu1 124.97(15) . . ? C32 O3 Cu1 125.11(15) . . ? C8 O1 C9 118.42(15) . . ? C6 N2 C5 116.94(16) . . ? C15 N1 C14 116.45(16) . . ? N2 C6 C17 122.48(17) . . ? N2 C6 C7 121.42(17) . . ? C7 C6 C17 116.11(16) . . ? N1 C15 C8 122.72(17) . . ? N1 C15 C16 121.26(17) . . ? C16 C15 C8 116.02(16) . . ? O2 C17 C6 119.13(16) . . ? O2 C17 C16 118.05(16) . . ? C16 C17 C6 122.82(17) . . ? O1 C8 C15 119.49(16) . . ? C7 C8 O1 117.47(17) . . ? C7 C8 C15 123.04(18) . . ? N1 C14 C9 122.41(17) . . ? N1 C14 C13 120.46(18) . . ? C9 C14 C13 117.14(19) . . ? C6 C7 H7 119.5 . . ? C8 C7 C6 121.02(17) . . ? C8 C7 H7 119.5 . . ? O1 C9 C14 120.49(18) . . ? O1 C9 C10 116.81(19) . . ? C10 C9 C14 122.70(19) . . ? N2 C5 C18 122.48(17) . . ? N2 C5 C4 119.17(18) . . ? C18 C5 C4 118.28(19) . . ? C15 C16 H16 119.5 . . ? C17 C16 C15 120.97(17) . . ? C17 C16 H16 119.5 . . ? O2 C18 C5 119.07(17) . . ? O2 C18 C1 117.95(18) . . ? C1 C18 C5 122.95(17) . . ? C18 C1 C2 115.8(2) . . ? C18 C1 C19 122.25(18) . . ? C2 C1 C19 122.0(2) . . ? O5 C36 C35 128.2(2) . . ? O5 C36 C38 113.8(2) . . ? C35 C36 C38 118.0(2) . . ? C4 C3 C2 118.23(18) . . ? C4 C3 C23 121.0(2) . . ? C2 C3 C23 120.6(2) . . ? C14 C13 H13 120.1 . . ? C12 C13 C14 119.8(2) . . ? C12 C13 H13 120.1 . . ? O4 C31 C30 128.2(2) . . ? O4 C31 C34 112.7(2) . . ? C30 C31 C34 119.1(2) . . ? O3 C32 C30 127.8(2) . . ? O3 C32 C33 114.1(2) . . ? C30 C32 C33 118.0(2) . . ? O6 C37 C39 113.8(2) . . ? O6 C37 C35 127.7(2) . . ? C35 C37 C39 118.5(2) . . ? C5 C4 H4 119.4 . . ? C3 C4 C5 121.1(2) . . ? C3 C4 H4 119.4 . . ? C1 C2 C3 123.7(2) . . ? C1 C2 H2 118.2 . . ? C3 C2 H2 118.2 . . ? C21 C19 C1 109.9(2) . . ? C21 C19 C22 110.4(2) . . ? C20 C19 C1 111.4(2) . . ? C20 C19 C21 107.8(2) . . ? C20 C19 C22 107.8(2) . . ? C22 C19 C1 109.5(2) . . ? C13 C12 Cl1 118.90(18) . . ? C13 C12 C11 122.3(2) . . ? C11 C12 Cl1 118.81(18) . . ? C9 C10 H10 120.3 . . ? C9 C10 C11 119.4(2) . . ? C11 C10 H10 120.3 . . ? F7 C39 C37 112.3(4) . . ? F8 C39 F7 110.2(12) . . ? F8 C39 C37 113.9(6) . . ? F11 C39 F7 102.3(16) . . ? F11 C39 F8 109.3(10) . . ? F11 C39 C37 108.1(9) . . ? F9 C39 C37 111.0(6) . . ? F12 C39 C37 112.2(9) . . ? F12 C39 F9 102.8(9) . . ? F10 C39 C37 112.4(13) . . ? F10 C39 F9 121(4) . . ? F10 C39 F12 96(5) . . ? C31 C30 C32 121.3(2) . . ? C31 C30 H30 119.3 . . ? C32 C30 H30 119.3 . . ? C12 C11 C10 118.7(2) . . ? C12 C11 H11 120.7 . . ? C10 C11 H11 120.7 . . ? F21 C34 C31 110.5(3) . . ? F21 C34 F19 103.9(4) . . ? F19 C34 C31 110.7(3) . . ? F20 C34 F21 107.5(4) . . ? F20 C34 C31 113.9(3) . . ? F20 C34 F19 109.8(4) . . ? F24 C34 C31 112.0(10) . . ? F24 C34 F23 92.1(13) . . ? F22 C34 C31 118.6(7) . . ? F22 C34 F24 117.8(14) . . ? F22 C34 F23 102.6(16) . . ? F23 C34 C31 109.2(8) . . ? C36 C35 C37 121.7(2) . . ? C36 C35 H35 119.1 . . ? C37 C35 H35 119.1 . . ? F1 C38 C36 111.4(4) . . ? F1 C38 F3 100.0(5) . . ? F3 C38 C36 110.5(3) . . ? F4 C38 C36 115.7(4) . . ? F4 C38 F1 111.8(5) . . ? F4 C38 F3 106.1(5) . . ? F5 C38 C36 112.1(6) . . ? F5 C38 F2 96.6(8) . . ? F6 C38 C36 117.9(5) . . ? F6 C38 F5 113.3(10) . . ? F6 C38 F2 106.5(9) . . ? F2 C38 C36 107.9(5) . . ? C3 C23 C24 103.9(5) . . ? C3 C23 C29 111.7(6) . . ? C3 C23 C27 109.3(6) . . ? C28 C23 C3 112.1(7) . . ? C28 C23 C24 112.6(10) . . ? C28 C23 C26 112.1(7) . . ? C26 C23 C3 113.3(4) . . ? C26 C23 C24 102.1(7) . . ? C25 C23 C3 109.6(7) . . ? C25 C23 C29 111.7(11) . . ? C25 C23 C27 112.8(9) . . ? C27 C23 C29 101.6(7) . . ? F13 C33 C32 113.1(4) . . ? F14 C33 C32 113.7(4) . . ? F14 C33 F13 108.6(8) . . ? F14 C33 F15 106.7(7) . . ? F15 C33 C32 110.9(4) . . ? F15 C33 F13 103.1(6) . . ? F16 C33 C32 107.4(4) . . ? F17 C33 C32 115.5(5) . . ? F17 C33 F16 107.9(8) . . ? F17 C33 F18 110.1(7) . . ? F18 C33 C32 110.9(5) . . ? F18 C33 F16 104.4(8) . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C29 H29A 109.5 . . ? C23 C29 H29B 109.5 . . ? C23 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 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 Cu2 O6 1.9490(15) 2_667 ? Cu2 O6 1.9490(15) . ? Cu2 O5 1.9383(15) . ? Cu2 O5 1.9384(15) 2_667 ? Cu1 O4 1.9343(15) . ? Cu1 O4 1.9343(15) 2_766 ? Cu1 O3 1.9366(15) 2_766 ? Cu1 O3 1.9366(15) . ? Cl1 C12 1.737(2) . ? O2 C17 1.349(2) . ? O2 C18 1.381(2) . ? O6 C37 1.252(3) . ? O5 C36 1.248(3) . ? O4 C31 1.251(3) . ? O3 C32 1.248(3) . ? O1 C8 1.358(2) . ? O1 C9 1.373(2) . ? N2 C6 1.319(2) . ? N2 C5 1.393(3) . ? N1 C15 1.323(2) . ? N1 C14 1.391(3) . ? F7 C39 1.301(9) . ? C6 C17 1.458(3) . ? C6 C7 1.423(3) . ? C15 C8 1.457(3) . ? C15 C16 1.424(3) . ? C17 C16 1.358(3) . ? F8 C39 1.288(11) . ? C8 C7 1.353(3) . ? C14 C9 1.399(3) . ? C14 C13 1.403(3) . ? F21 C34 1.314(4) . ? C7 H7 0.9300 . ? C9 C10 1.374(3) . ? C5 C18 1.403(3) . ? C5 C4 1.405(3) . ? C16 H16 0.9300 . ? C18 C1 1.392(3) . ? C1 C2 1.394(3) . ? C1 C19 1.539(3) . ? C36 C35 1.375(4) . ? C36 C38 1.521(4) . ? F11 C39 1.29(2) . ? C3 C4 1.372(3) . ? C3 C2 1.405(3) . ? C3 C23 1.539(3) . ? C13 H13 0.9300 . ? C13 C12 1.375(3) . ? C31 C30 1.376(4) . ? C31 C34 1.531(3) . ? C32 C30 1.388(4) . ? C32 C33 1.533(3) . ? C37 C39 1.535(4) . ? C37 C35 1.376(4) . ? C4 H4 0.9300 . ? F19 C34 1.318(6) . ? C2 H2 0.9300 . ? C19 C21 1.528(4) . ? C19 C20 1.526(3) . ? C19 C22 1.535(4) . ? C12 C11 1.384(4) . ? C10 H10 0.9300 . ? C10 C11 1.385(3) . ? F20 C34 1.300(5) . ? C39 F9 1.342(8) . ? C39 F12 1.333(17) . ? C39 F10 1.29(4) . ? C30 H30 0.9300 . ? F1 C38 1.291(6) . ? C11 H11 0.9300 . ? C34 F24 1.25(2) . ? C34 F22 1.12(2) . ? C34 F23 1.31(2) . ? C35 H35 0.9300 . ? C38 F3 1.366(6) . ? C38 F4 1.267(6) . ? C38 F5 1.234(13) . ? C38 F6 1.094(14) . ? C38 F2 1.399(12) . ? C23 C28 1.398(17) . ? C23 C24 1.594(14) . ? C23 C26 1.525(10) . ? C23 C25 1.414(16) . ? C23 C29 1.586(15) . ? C23 C27 1.576(13) . ? F13 C33 1.306(7) . ? C33 F14 1.277(8) . ? C33 F15 1.297(7) . ? C33 F16 1.310(9) . ? C33 F17 1.211(7) . ? C33 F18 1.261(7) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -2.8843 -0.1384 -7.9140 0.4780 -0.8783 -0.0092 2.4104 -0.7440 -9.7202 0.2978 -0.5435 0.7848 -3.5943 7.1151 -4.2745 0.9738 -0.1277 -0.1879 5.0779 -6.7656 -1.5498 -0.7268 -0.1339 0.6736 3.1190 -8.3685 2.0523 -0.9602 -0.1784 0.2150 -3.4479 8.2786 -1.5753 0.9428 0.1750 -0.2836 4.7926 -6.4883 -3.8852 -0.5804 -0.3140 0.7513 4.4397 -7.1823 -3.2745 -0.6564 -0.3556 0.6654 1.2543 -8.8688 0.9700 -0.8783 -0.4780 0.0092 -5.3087 0.7711 6.0812 -0.0070 -0.0063 -1.0000 5.5419 0.3875 -4.5613 0.0279 0.2296 0.9729 5.6261 -0.4610 2.0305 -0.3623 0.6628 0.6554 1.9818 -4.8462 8.0461 -0.8876 0.4228 -0.1827 2.9955 -7.1255 5.0889 -0.9893 0.1291 0.0677 3.8118 -8.1227 0.9878 -0.9159 -0.1715 0.3630 -3.3622 8.3091 -1.6904 0.9475 0.1772 -0.2660 2.4127 -8.8153 -0.4302 -0.8538 -0.4652 0.2338 -3.0498 8.5667 1.2609 0.8181 0.4461 -0.3630 3.9112 -6.6386 -5.3402 -0.4895 -0.5191 0.7007 -2.6692 7.9208 4.1176 0.6106 0.6462 -0.4577 -1.6339 -5.3189 -5.7892 -0.1296 -0.9915 -0.0091 -2.5875 4.3869 8.4456 0.0909 0.7077 -0.7006 -0.0208 -2.9714 -9.0889 0.1690 -0.9018 0.3978