#------------------------------------------------------------------------------ #$Date: 2021-05-07 05:26:07 +0300 (Fri, 07 May 2021) $ #$Revision: 265025 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/73/7707359.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_7707359 loop_ _publ_author_name 'Wang, Kuiyuan' 'Prior, Timothy J.' 'Hughes, David L.' 'Arbaoui, Abdessamad' 'Redshaw, Carl' _publ_section_title ; Coordination chemistry of [2+2] Schiff-base macrocycles derived from the dianilines [(2-NH2C6H4)2X] (X = CH2CH2, O): Structural studies and ROP capability towards cyclic esters. ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT00711D _journal_year 2021 _chemical_formula_moiety 'C52 H52 Br Cu N4 O2, Br2 Cu, 2(C2 H3 N)' _chemical_formula_sum 'C56 H58 Br3 Cu2 N6 O2' _chemical_formula_weight 1213.89 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2021-04-29 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _audit_update_record ; 2021-04-29 deposited with the CCDC. 2021-05-04 downloaded from the CCDC. ; _cell_angle_alpha 71.443(2) _cell_angle_beta 82.738(2) _cell_angle_gamma 76.600(2) _cell_formula_units_Z 2 _cell_length_a 10.0808(2) _cell_length_b 15.0015(4) _cell_length_c 18.6604(4) _cell_measurement_reflns_used 28839 _cell_measurement_temperature 99.9(6) _cell_measurement_theta_max 70.1660 _cell_measurement_theta_min 4.5320 _cell_volume 2598.16(11) _computing_cell_refinement 'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 99.9(6) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.984 _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 -84.00 94.00 0.50 0.50 -- 5.00 37.00 82.00 356 2 \w -179.00 -1.00 0.50 0.50 -- -90.00 37.00 82.00 356 3 \w -89.00 89.00 0.50 0.50 -- 0.00 0.00-180.00 356 4 \w -89.00 89.00 0.50 0.50 -- 0.00 37.00 82.00 356 5 \w -179.00 -1.00 0.50 0.50 -- -90.00 56.00 -63.82 356 6 \w -179.00 -1.00 0.50 0.50 -- -90.00 58.00-161.78 356 7 \w -179.00 -1.00 0.50 0.50 -- -90.00 59.00 0.28 356 8 \w -179.00 -1.00 0.50 0.50 -- -90.00 59.00 0.28 356 9 \w -137.00 -58.00 0.50 0.50 -- -90.00 58.00 124.85 158 10 \w -169.00-127.00 0.50 0.50 -- -90.00 59.00-124.59 84 11 \w -107.00 -66.00 0.50 0.50 -- -90.00 59.00-124.59 82 12 \w -179.00 -2.00 0.50 0.50 -- -90.00 59.00 49.40 354 13 \w -179.00 -1.00 0.50 0.50 -- -90.00 59.00 -38.54 356 14 \w -58.00 -31.00 0.50 0.50 -- -90.00 58.00-161.78 54 15 \w -126.00 -93.00 0.50 0.50 -- -90.00 10.00 -60.00 66 16 \w -55.00 -16.00 0.50 0.50 -- -90.00 10.00 -60.00 78 17 \w -178.00 -49.00 0.50 0.50 -- -90.00 59.00-154.16 258 18 \w -179.00-149.00 0.50 0.50 -- -90.00 58.00 92.60 60 19 \w -139.00 -92.00 0.50 0.50 -- -90.00 58.00 92.60 94 20 \w -29.00 -2.00 0.50 0.50 -- -90.00 58.00 92.60 54 21 \w -135.00-109.00 0.50 0.50 -- -90.00 58.00 22.68 52 22 \w -55.00 -29.00 0.50 0.50 -- -90.00 58.00 22.68 52 23 \w -178.00-145.00 0.50 0.50 -- -90.00 20.00-180.00 66 24 \w -57.00 -30.00 0.50 0.50 -- -90.00 20.00-180.00 54 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB AFC11 (RCD3): quarter-chi single' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0461751000 _diffrn_orient_matrix_UB_12 -0.0655358000 _diffrn_orient_matrix_UB_13 -0.0512878000 _diffrn_orient_matrix_UB_21 0.1502457000 _diffrn_orient_matrix_UB_22 0.0009378000 _diffrn_orient_matrix_UB_23 0.0070840000 _diffrn_orient_matrix_UB_31 0.0074102000 _diffrn_orient_matrix_UB_32 -0.0891436000 _diffrn_orient_matrix_UB_33 0.0702008000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0834 _diffrn_reflns_av_unetI/netI 0.0348 _diffrn_reflns_Laue_measured_fraction_full 0.985 _diffrn_reflns_Laue_measured_fraction_max 0.984 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 44092 _diffrn_reflns_point_group_measured_fraction_full 0.985 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 68.250 _diffrn_reflns_theta_min 2.502 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 4.064 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.14868 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'dark red' _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.552 _exptl_crystal_description plate _exptl_crystal_F_000 1230 _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.15 _refine_diff_density_max 3.448 _refine_diff_density_min -1.244 _refine_diff_density_rms 0.133 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 622 _refine_ls_number_reflns 9332 _refine_ls_number_restraints 7 _refine_ls_restrained_S_all 1.064 _refine_ls_R_factor_all 0.0676 _refine_ls_R_factor_gt 0.0666 _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^)+(0.1141P)^2^+7.3661P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1824 _refine_ls_wR_factor_ref 0.1835 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8998 _reflns_number_total 9332 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt00711d2.cif _cod_data_source_block FeROP5 _cod_original_cell_volume 2598.13(11) _cod_database_code 7707359 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C56 H58 N6 O2 Br3 Cu2' _chemical_oxdiff_usercomment 'Cu tBu macro' _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. ; _cell_oxdiff_angle_alpha 71.443(2) _cell_oxdiff_angle_beta 82.738(2) _cell_oxdiff_angle_gamma 76.600(2) _cell_oxdiff_length_a 10.0808(2) _cell_oxdiff_length_b 15.0015(4) _cell_oxdiff_length_c 18.6604(4) _cell_oxdiff_measurement_reflns_used 28839 _cell_oxdiff_volume 2598.13(11) _shelx_estimated_absorpt_t_max 0.579 _shelx_estimated_absorpt_t_min 0.162 _reflns_odcompleteness_completeness 98.43 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 68.13 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C39-C40 \\sim C39-C40A with sigma of 0.02 C40-C41 \\sim C40A-C41A with sigma of 0.02 C41-C42 \\sim C41A-C42A with sigma of 0.02 C41-C43 \\sim C41A-C43 with sigma of 0.04 C42-C43 \\sim C42A-C43 with sigma of 0.02 C39-C41 \\sim C39-C41A with sigma of 0.04 C40-C42 \\sim C40A-C42A with sigma of 0.04 3. Others Sof(C42A)=Sof(H42A)=Sof(C41A)=Sof(H41A)=Sof(C40A)=Sof(H40A)=1-FVAR(1) Sof(C40)=Sof(H40)=Sof(C41)=Sof(H41)=Sof(C42)=Sof(H42)=FVAR(1) 4.a Secondary CH2 refined with riding coordinates: C18(H18A,H18B), C19(H19A,H19B), C44(H44A,H44B), C45(H45A,H45B) 4.b Me refined with riding coordinates: C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C) 4.c Aromatic/amide H refined with riding coordinates: N2(H2), N4(H4), C3(H3), C5(H5), C11(H11), C13(H13), C14(H14), C15(H15), C16(H16), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C29(H29), C31(H31), C37(H37), C39(H39), C40(H40), C41(H41), C42(H42), C47(H47), C48(H48), C49(H49), C50(H50), C52(H52), C42A(H42A), C41A(H41A), C40A(H40A) 4.d Idealised Me refined as rotating group: C54(H54A,H54B,H54C), C56(H56A,H56B,H56C) ; _shelx_res_file ; TITL shelxt_a.res in P-1 2019ncsx0240.res created by SHELXL-2018/3 at 12:22:02 on 29-Apr-2021 CELL 1.54184 10.0808 15.0015 18.6604 71.442 82.738 76.6 ZERR 2 0.0002 0.0004 0.0005 0.002 0.002 0.002 LATT 1 SFAC C H Br Cu N O UNIT 112 116 6 4 12 4 SADI C39 C40 C39 C40A SADI C40 C41 C40A C41A SADI C41 C42 C41A C42A SADI 0.04 C41 C43 C41A C43 SADI C42 C43 C42A C43 SADI 0.04 C39 C41 C39 C41A SADI 0.04 C40 C42 C40A C42A L.S. 10 PLAN 8 SIZE 0.15 0.6 0.7 TEMP -173.2(6) CONF BOND $H LIST 6 MORE -1 fmap 2 acta MERG 2 OMIT 3 1 6 OMIT -2 -2 5 OMIT 4 -1 1 OMIT 2 -1 2 OMIT -1 -2 7 REM REM REM WGHT 0.114100 7.366100 FVAR 4.09600 0.49339 O1 6 0.533361 0.708350 0.650840 11.00000 0.03180 0.02937 = 0.01554 -0.01083 -0.00100 -0.00563 O2 6 0.439230 0.614907 0.867351 11.00000 0.02899 0.02235 = 0.01792 -0.01071 0.00012 -0.00021 CU1 4 0.486620 0.661410 0.759334 11.00000 0.02837 0.02182 = 0.01420 -0.00917 -0.00031 -0.00238 BR1 3 0.692818 0.530728 0.777446 11.00000 0.03218 0.02337 = 0.02423 -0.00769 0.00121 0.00216 BR2 3 0.019784 0.971693 0.765529 11.00000 0.05825 0.05108 = 0.07954 -0.03930 0.01306 -0.01928 CU2 4 0.130066 1.091989 0.739170 11.00000 0.04578 0.04035 = 0.03402 -0.01664 0.00437 -0.00892 BR4 3 0.242825 1.211997 0.709110 11.00000 0.06065 0.05143 = 0.03858 -0.01266 0.01165 -0.02225 N1 5 0.302820 0.636964 0.734128 11.00000 0.02633 0.02617 = 0.01700 -0.01008 -0.00016 -0.00156 N2 5 0.365028 0.461174 0.962001 11.00000 0.02770 0.02214 = 0.01774 -0.00973 -0.00172 -0.00348 AFIX 43 H2 2 0.406646 0.487994 0.918784 11.00000 -1.20000 AFIX 0 N3 5 0.474200 0.797168 0.768728 11.00000 0.03494 0.02254 = 0.01786 -0.00634 -0.00043 -0.00284 N4 5 0.736789 0.767608 0.559966 11.00000 0.02809 0.02592 = 0.02119 -0.01052 -0.00018 -0.00309 AFIX 43 H4 2 0.691394 0.759531 0.604289 11.00000 -1.20000 AFIX 0 C1 1 0.487177 0.692894 0.594793 11.00000 0.03146 0.01811 = 0.01804 -0.00809 -0.00366 0.00007 C2 1 0.559370 0.712258 0.522400 11.00000 0.03115 0.02356 = 0.02186 -0.01053 -0.00136 -0.00376 C3 1 0.511507 0.695492 0.460580 11.00000 0.03549 0.02802 = 0.01794 -0.01184 0.00294 -0.00525 AFIX 43 H3 2 0.563051 0.708005 0.413478 11.00000 -1.20000 AFIX 0 C4 1 0.393440 0.661827 0.465834 11.00000 0.03444 0.02734 = 0.01961 -0.01099 0.00110 -0.00516 C5 1 0.320159 0.647239 0.536051 11.00000 0.03094 0.02557 = 0.02130 -0.01113 -0.00211 -0.00400 AFIX 43 H5 2 0.235749 0.627365 0.540806 11.00000 -1.20000 AFIX 0 C6 1 0.363832 0.660195 0.599857 11.00000 0.03184 0.02080 = 0.01645 -0.00890 -0.00120 -0.00187 C7 1 0.342602 0.639700 0.400825 11.00000 0.03601 0.03336 = 0.02203 -0.01585 0.00087 -0.00640 C8 1 0.451871 0.639228 0.336296 11.00000 0.04873 0.06710 = 0.02836 -0.02885 0.00658 -0.02398 AFIX 33 H8A 2 0.416235 0.624869 0.295621 11.00000 -1.50000 H8B 2 0.476731 0.702383 0.316758 11.00000 -1.50000 H8C 2 0.532803 0.590130 0.355077 11.00000 -1.50000 AFIX 0 C9 1 0.213854 0.714873 0.371797 11.00000 0.05607 0.03654 = 0.02346 -0.01116 -0.01015 -0.00357 AFIX 33 H9A 2 0.144334 0.714655 0.413582 11.00000 -1.50000 H9B 2 0.236720 0.778617 0.351607 11.00000 -1.50000 H9C 2 0.178378 0.699300 0.331686 11.00000 -1.50000 AFIX 0 C10 1 0.308478 0.539461 0.428927 11.00000 0.04159 0.03649 = 0.02918 -0.01719 -0.00348 -0.00725 AFIX 33 H10A 2 0.238328 0.536836 0.470587 11.00000 -1.50000 H10B 2 0.274352 0.525964 0.387370 11.00000 -1.50000 H10C 2 0.390924 0.491457 0.446804 11.00000 -1.50000 AFIX 0 C11 1 0.275114 0.640350 0.667866 11.00000 0.02796 0.02265 = 0.01969 -0.00902 -0.00236 -0.00175 AFIX 43 H11 2 0.188405 0.628761 0.663058 11.00000 -1.20000 AFIX 0 C12 1 0.197289 0.616625 0.792758 11.00000 0.02608 0.03371 = 0.01379 -0.00790 -0.00265 -0.00333 C13 1 0.129477 0.690845 0.821931 11.00000 0.02863 0.03248 = 0.02075 -0.01106 -0.00312 -0.00253 AFIX 43 H13 2 0.152200 0.752456 0.802191 11.00000 -1.20000 AFIX 0 C14 1 0.028508 0.674727 0.879957 11.00000 0.02444 0.04781 = 0.02487 -0.01473 -0.00232 0.00107 AFIX 43 H14 2 -0.017964 0.725217 0.899899 11.00000 -1.20000 AFIX 0 C15 1 -0.003699 0.585140 0.908332 11.00000 0.02632 0.05165 = 0.02168 -0.00919 -0.00061 -0.00663 AFIX 43 H15 2 -0.071848 0.573713 0.948355 11.00000 -1.20000 AFIX 0 C16 1 0.062792 0.511573 0.878802 11.00000 0.03161 0.04133 = 0.02279 -0.00561 -0.00148 -0.01130 AFIX 43 H16 2 0.037642 0.450730 0.898428 11.00000 -1.20000 AFIX 0 C17 1 0.166072 0.524276 0.820826 11.00000 0.03110 0.03684 = 0.01753 -0.00830 -0.00411 -0.00779 C18 1 0.242912 0.441769 0.793070 11.00000 0.04138 0.03375 = 0.02098 -0.01085 -0.00108 -0.01439 AFIX 23 H18A 2 0.262322 0.465830 0.737708 11.00000 -1.20000 H18B 2 0.184258 0.394186 0.802373 11.00000 -1.20000 AFIX 0 C19 1 0.378866 0.391183 0.831471 11.00000 0.03933 0.02857 = 0.02313 -0.01460 0.00423 -0.00903 AFIX 23 H19A 2 0.434270 0.349552 0.802142 11.00000 -1.20000 H19B 2 0.430491 0.440388 0.830204 11.00000 -1.20000 AFIX 0 C20 1 0.359461 0.331156 0.912289 11.00000 0.02810 0.02577 = 0.02525 -0.01405 0.00030 -0.00230 C21 1 0.343646 0.237135 0.925708 11.00000 0.03745 0.02738 = 0.03012 -0.01717 -0.00147 -0.00388 AFIX 43 H21 2 0.347005 0.213231 0.883949 11.00000 -1.20000 AFIX 0 C22 1 0.323310 0.178130 0.997844 11.00000 0.03867 0.02443 = 0.03700 -0.01322 -0.00331 -0.00601 AFIX 43 H22 2 0.313954 0.114114 1.005543 11.00000 -1.20000 AFIX 0 C23 1 0.316480 0.212693 1.059671 11.00000 0.03760 0.02539 = 0.02370 -0.00424 -0.00380 -0.00620 AFIX 43 H23 2 0.301254 0.172381 1.109487 11.00000 -1.20000 AFIX 0 C24 1 0.331851 0.305629 1.048553 11.00000 0.02801 0.02517 = 0.02481 -0.01039 -0.00266 -0.00242 AFIX 43 H24 2 0.328085 0.329003 1.090632 11.00000 -1.20000 AFIX 0 C25 1 0.352900 0.364693 0.975176 11.00000 0.02596 0.02530 = 0.02462 -0.01281 -0.00344 -0.00203 C26 1 0.320962 0.514885 1.007220 11.00000 0.02439 0.02530 = 0.01800 -0.00879 -0.00368 0.00013 AFIX 43 H26 2 0.286370 0.485612 1.056847 11.00000 -1.20000 AFIX 0 C27 1 0.376924 0.663555 0.913035 11.00000 0.02565 0.02540 = 0.01458 -0.00951 -0.00220 -0.00354 C28 1 0.358693 0.764567 0.895272 11.00000 0.02863 0.02548 = 0.01735 -0.01010 -0.00356 -0.00118 C29 1 0.291484 0.811312 0.948039 11.00000 0.03464 0.02313 = 0.02125 -0.01253 -0.00252 0.00087 AFIX 43 H29 2 0.279788 0.879192 0.934361 11.00000 -1.20000 AFIX 0 C30 1 0.241182 0.763331 1.019280 11.00000 0.03009 0.02608 = 0.02031 -0.01271 -0.00324 0.00203 C31 1 0.257759 0.664842 1.036862 11.00000 0.02542 0.02956 = 0.01835 -0.01281 -0.00149 -0.00094 AFIX 43 H31 2 0.224393 0.630053 1.085137 11.00000 -1.20000 AFIX 0 C32 1 0.322455 0.614035 0.985718 11.00000 0.02728 0.02484 = 0.01708 -0.00885 -0.00421 -0.00063 C33 1 0.164708 0.816658 1.075097 11.00000 0.04064 0.02687 = 0.02012 -0.01388 0.00332 0.00228 C34 1 0.184501 0.919865 1.051921 11.00000 0.09243 0.04000 = 0.05026 -0.02817 0.02647 -0.01629 AFIX 33 H34A 2 0.281916 0.920091 1.050608 11.00000 -1.50000 H34B 2 0.149983 0.954320 1.001597 11.00000 -1.50000 H34C 2 0.134341 0.951599 1.088645 11.00000 -1.50000 AFIX 0 C35 1 0.219300 0.766813 1.153636 11.00000 0.13206 0.04852 = 0.02763 -0.02265 -0.01436 0.02337 AFIX 33 H35A 2 0.316991 0.766725 1.151330 11.00000 -1.50000 H35B 2 0.170312 0.801185 1.188964 11.00000 -1.50000 H35C 2 0.205682 0.700496 1.171085 11.00000 -1.50000 AFIX 0 C36 1 0.014296 0.817973 1.076755 11.00000 0.04831 0.11040 = 0.09869 -0.08023 0.02141 -0.01127 AFIX 33 H36A 2 0.000042 0.751922 1.091607 11.00000 -1.50000 H36B 2 -0.035260 0.850066 1.113391 11.00000 -1.50000 H36C 2 -0.019618 0.852787 1.026343 11.00000 -1.50000 AFIX 0 C37 1 0.408277 0.825000 0.824381 11.00000 0.03455 0.02035 = 0.02050 -0.00995 -0.00120 -0.00226 AFIX 43 H37 2 0.390443 0.891954 0.818235 11.00000 -1.20000 AFIX 0 C38 1 0.510358 0.873233 0.704545 11.00000 0.04786 0.01763 = 0.02081 -0.00926 0.00503 -0.00160 C39 1 0.404948 0.933972 0.659495 11.00000 0.04791 0.03554 = 0.03108 -0.00513 0.00730 0.00614 PART 1 AFIX 43 H39 2 0.314333 0.923346 0.665572 11.00000 -1.20000 AFIX 0 C40 1 0.447997 1.014035 0.603124 21.00000 0.03334 AFIX 43 H40 2 0.379788 1.061782 0.573809 21.00000 -1.20000 AFIX 0 C41 1 0.583181 1.027082 0.588064 21.00000 0.03468 AFIX 43 H41 2 0.603992 1.080714 0.548200 21.00000 -1.20000 AFIX 0 C42 1 0.687497 0.961641 0.631358 21.00000 0.02970 AFIX 43 H42 2 0.780016 0.968522 0.622785 21.00000 -1.20000 AFIX 0 PART 0 C43 1 0.645437 0.885225 0.688280 11.00000 0.05051 0.02494 = 0.02414 -0.01535 0.00658 -0.00963 C44 1 0.762510 0.819413 0.734062 11.00000 0.04251 0.05229 = 0.02067 -0.01492 0.00294 -0.02189 AFIX 23 H44A 2 0.724785 0.782186 0.783142 11.00000 -1.20000 H44B 2 0.818649 0.859212 0.744904 11.00000 -1.20000 AFIX 0 C45 1 0.855645 0.748806 0.696023 11.00000 0.03787 0.03428 = 0.02465 -0.00685 -0.00911 -0.00911 AFIX 23 H45A 2 0.930920 0.710997 0.729375 11.00000 -1.20000 H45B 2 0.802373 0.703452 0.691190 11.00000 -1.20000 AFIX 0 C46 1 0.916171 0.795327 0.619168 11.00000 0.03179 0.02841 = 0.02751 -0.00908 -0.00661 -0.00113 C47 1 1.031985 0.833901 0.610998 11.00000 0.03599 0.03305 = 0.03547 -0.01112 -0.01138 -0.00349 AFIX 43 H47 2 1.072676 0.830948 0.655140 11.00000 -1.20000 AFIX 0 C48 1 1.089971 0.876447 0.540734 11.00000 0.03536 0.03138 = 0.04324 -0.01355 -0.00233 -0.00670 AFIX 43 H48 2 1.169313 0.901971 0.537072 11.00000 -1.20000 AFIX 0 C49 1 1.031807 0.881641 0.475797 11.00000 0.03701 0.02758 = 0.03892 -0.01248 0.00518 -0.00596 AFIX 43 H49 2 1.071518 0.910474 0.427425 11.00000 -1.20000 AFIX 0 C50 1 0.915821 0.844832 0.481348 11.00000 0.03672 0.02410 = 0.02896 -0.01090 0.00014 -0.00440 AFIX 43 H50 2 0.875530 0.848376 0.436909 11.00000 -1.20000 AFIX 0 C51 1 0.858639 0.802603 0.552455 11.00000 0.02753 0.02408 = 0.03161 -0.01204 -0.00240 -0.00113 C52 1 0.684111 0.745968 0.508699 11.00000 0.03104 0.02688 = 0.01880 -0.00745 0.00189 -0.00541 AFIX 43 H52 2 0.730837 0.752985 0.460335 11.00000 -1.20000 AFIX 0 N5 5 0.970957 0.601850 0.533284 11.00000 0.06237 0.04409 = 0.11172 -0.04070 0.02904 -0.01913 C53 1 0.988476 0.535567 0.585516 11.00000 0.03481 0.04707 = 0.08738 -0.04068 0.00680 -0.00938 C54 1 1.007502 0.450229 0.650561 11.00000 0.04479 0.11741 = 0.08375 -0.04296 -0.02171 -0.00627 AFIX 137 H54A 2 0.933788 0.457237 0.689229 11.00000 -1.50000 H54B 2 1.095583 0.441816 0.671442 11.00000 -1.50000 H54C 2 1.005985 0.393991 0.634950 11.00000 -1.50000 AFIX 0 N6 5 0.437416 1.012716 0.893015 11.00000 0.08816 0.03510 = 0.06757 -0.01754 -0.00631 -0.01330 C55 1 0.510461 1.040025 0.842057 11.00000 0.07425 0.02725 = 0.05074 -0.01926 -0.00877 -0.00880 C56 1 0.600306 1.074472 0.778568 11.00000 0.07559 0.05071 = 0.06424 -0.03008 -0.00001 -0.01138 AFIX 137 H56A 2 0.566591 1.071735 0.732459 11.00000 -1.50000 H56B 2 0.692085 1.034278 0.786381 11.00000 -1.50000 H56C 2 0.603785 1.140997 0.773376 11.00000 -1.50000 AFIX 0 PART 2 C42A 1 0.654766 0.965594 0.622447 -21.00000 0.02788 AFIX 43 H42A 2 0.742160 0.981852 0.609398 -21.00000 -1.20000 AFIX 0 C41A 1 0.551678 1.022400 0.575572 -21.00000 0.03268 AFIX 43 H41A 2 0.570448 1.073273 0.532489 -21.00000 -1.20000 AFIX 0 C40A 1 0.419312 1.004044 0.592367 -21.00000 0.03084 AFIX 43 H40A 2 0.346204 1.037114 0.560195 -21.00000 -1.20000 AFIX 0 HKLF 4 REM shelxt_a.res in P-1 REM wR2 = 0.1835, GooF = S = 1.061, Restrained GooF = 1.064 for all data REM R1 = 0.0666 for 8998 Fo > 4sig(Fo) and 0.0676 for all 9332 data REM 622 parameters refined using 7 restraints END WGHT 0.1141 7.3661 REM Highest difference peak 3.448, deepest hole -1.244, 1-sigma level 0.133 Q1 1 1.2330 0.9091 0.5538 11.00000 0.05 3.45 Q2 1 -0.0723 1.0011 0.7606 11.00000 0.05 1.81 Q3 1 0.6112 1.1094 0.5164 11.00000 0.05 1.71 Q4 1 0.7835 0.5180 0.7724 11.00000 0.05 1.34 Q5 1 0.6870 0.4739 0.8026 11.00000 0.05 1.23 Q6 1 0.2595 0.9248 0.6719 11.00000 0.05 1.16 Q7 1 0.0301 1.1054 0.7390 11.00000 0.05 1.12 Q8 1 0.5999 0.5482 0.7803 11.00000 0.05 1.09 ; _shelx_res_checksum 62699 _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 2.423 _oxdiff_exptl_absorpt_empirical_full_min 0.374 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 O1 O 0.5334(3) 0.7083(2) 0.65084(15) 0.0247(6) Uani 1 1 d . . . . . O2 O 0.4392(3) 0.61491(19) 0.86735(15) 0.0230(6) Uani 1 1 d . . . . . Cu1 Cu 0.48662(6) 0.66141(4) 0.75933(3) 0.02110(17) Uani 1 1 d . . . . . Br1 Br 0.69282(4) 0.53073(3) 0.77745(2) 0.02806(15) Uani 1 1 d . . . . . Br2 Br 0.01978(7) 0.97169(5) 0.76553(4) 0.0584(2) Uani 1 1 d . . . . . Cu2 Cu 0.13007(8) 1.09199(5) 0.73917(4) 0.0393(2) Uani 1 1 d . . . . . Br4 Br 0.24283(6) 1.21200(4) 0.70911(3) 0.04989(19) Uani 1 1 d . . . . . N1 N 0.3028(3) 0.6370(2) 0.73413(18) 0.0230(7) Uani 1 1 d . . . . . N2 N 0.3650(3) 0.4612(2) 0.96200(18) 0.0219(7) Uani 1 1 d . . . . . H2 H 0.406646 0.487994 0.918784 0.026 Uiso 1 1 calc R U . . . N3 N 0.4742(4) 0.7972(2) 0.76873(19) 0.0257(7) Uani 1 1 d . . . . . N4 N 0.7368(4) 0.7676(2) 0.55997(19) 0.0248(7) Uani 1 1 d . . . . . H4 H 0.691394 0.759531 0.604289 0.030 Uiso 1 1 calc R U . . . C1 C 0.4872(4) 0.6929(3) 0.5948(2) 0.0226(8) Uani 1 1 d . . . . . C2 C 0.5594(4) 0.7123(3) 0.5224(2) 0.0249(8) Uani 1 1 d . . . . . C3 C 0.5115(4) 0.6955(3) 0.4606(2) 0.0266(8) Uani 1 1 d . . . . . H3 H 0.563051 0.708005 0.413478 0.032 Uiso 1 1 calc R U . . . C4 C 0.3934(4) 0.6618(3) 0.4658(2) 0.0266(8) Uani 1 1 d . . . . . C5 C 0.3202(4) 0.6472(3) 0.5361(2) 0.0252(8) Uani 1 1 d . . . . . H5 H 0.235749 0.627365 0.540806 0.030 Uiso 1 1 calc R U . . . C6 C 0.3638(4) 0.6602(3) 0.5999(2) 0.0228(8) Uani 1 1 d . . . . . C7 C 0.3426(5) 0.6397(3) 0.4008(2) 0.0290(9) Uani 1 1 d . . . . . C8 C 0.4519(6) 0.6392(4) 0.3363(3) 0.0433(12) Uani 1 1 d . . . . . H8A H 0.416235 0.624869 0.295621 0.065 Uiso 1 1 calc R U . . . H8B H 0.476731 0.702383 0.316758 0.065 Uiso 1 1 calc R U . . . H8C H 0.532803 0.590130 0.355077 0.065 Uiso 1 1 calc R U . . . C9 C 0.2139(6) 0.7149(4) 0.3718(3) 0.0384(11) Uani 1 1 d . . . . . H9A H 0.144334 0.714655 0.413582 0.058 Uiso 1 1 calc R U . . . H9B H 0.236720 0.778617 0.351607 0.058 Uiso 1 1 calc R U . . . H9C H 0.178378 0.699300 0.331686 0.058 Uiso 1 1 calc R U . . . C10 C 0.3085(5) 0.5395(3) 0.4289(3) 0.0340(10) Uani 1 1 d . . . . . H10A H 0.238328 0.536836 0.470587 0.051 Uiso 1 1 calc R U . . . H10B H 0.274352 0.525964 0.387370 0.051 Uiso 1 1 calc R U . . . H10C H 0.390924 0.491457 0.446804 0.051 Uiso 1 1 calc R U . . . C11 C 0.2751(4) 0.6403(3) 0.6679(2) 0.0233(8) Uani 1 1 d . . . . . H11 H 0.188405 0.628761 0.663058 0.028 Uiso 1 1 calc R U . . . C12 C 0.1973(4) 0.6166(3) 0.7928(2) 0.0247(8) Uani 1 1 d . . . . . C13 C 0.1295(4) 0.6908(3) 0.8219(2) 0.0270(8) Uani 1 1 d . . . . . H13 H 0.152200 0.752456 0.802191 0.032 Uiso 1 1 calc R U . . . C14 C 0.0285(4) 0.6747(4) 0.8800(2) 0.0328(10) Uani 1 1 d . . . . . H14 H -0.017964 0.725217 0.899899 0.039 Uiso 1 1 calc R U . . . C15 C -0.0037(4) 0.5851(4) 0.9083(2) 0.0339(10) Uani 1 1 d . . . . . H15 H -0.071848 0.573713 0.948355 0.041 Uiso 1 1 calc R U . . . C16 C 0.0628(5) 0.5116(4) 0.8788(2) 0.0322(9) Uani 1 1 d . . . . . H16 H 0.037642 0.450730 0.898428 0.039 Uiso 1 1 calc R U . . . C17 C 0.1661(4) 0.5243(3) 0.8208(2) 0.0281(9) Uani 1 1 d . . . . . C18 C 0.2429(5) 0.4418(3) 0.7931(2) 0.0303(9) Uani 1 1 d . . . . . H18A H 0.262322 0.465830 0.737708 0.036 Uiso 1 1 calc R U . . . H18B H 0.184258 0.394186 0.802373 0.036 Uiso 1 1 calc R U . . . C19 C 0.3789(5) 0.3912(3) 0.8315(2) 0.0289(9) Uani 1 1 d . . . . . H19A H 0.434270 0.349552 0.802142 0.035 Uiso 1 1 calc R U . . . H19B H 0.430491 0.440388 0.830204 0.035 Uiso 1 1 calc R U . . . C20 C 0.3595(4) 0.3312(3) 0.9123(2) 0.0255(8) Uani 1 1 d . . . . . C21 C 0.3436(5) 0.2371(3) 0.9257(3) 0.0301(9) Uani 1 1 d . . . . . H21 H 0.347005 0.213231 0.883949 0.036 Uiso 1 1 calc R U . . . C22 C 0.3233(5) 0.1781(3) 0.9978(3) 0.0324(9) Uani 1 1 d . . . . . H22 H 0.313954 0.114114 1.005543 0.039 Uiso 1 1 calc R U . . . C23 C 0.3165(5) 0.2127(3) 1.0597(2) 0.0295(9) Uani 1 1 d . . . . . H23 H 0.301254 0.172381 1.109487 0.035 Uiso 1 1 calc R U . . . C24 C 0.3319(4) 0.3056(3) 1.0486(2) 0.0257(8) Uani 1 1 d . . . . . H24 H 0.328085 0.329003 1.090632 0.031 Uiso 1 1 calc R U . . . C25 C 0.3529(4) 0.3647(3) 0.9752(2) 0.0244(8) Uani 1 1 d . . . . . C26 C 0.3210(4) 0.5149(3) 1.0072(2) 0.0227(8) Uani 1 1 d . . . . . H26 H 0.286370 0.485612 1.056847 0.027 Uiso 1 1 calc R U . . . C27 C 0.3769(4) 0.6636(3) 0.9130(2) 0.0212(8) Uani 1 1 d . . . . . C28 C 0.3587(4) 0.7646(3) 0.8953(2) 0.0235(8) Uani 1 1 d . . . . . C29 C 0.2915(4) 0.8113(3) 0.9480(2) 0.0260(8) Uani 1 1 d . . . . . H29 H 0.279788 0.879192 0.934361 0.031 Uiso 1 1 calc R U . . . C30 C 0.2412(4) 0.7633(3) 1.0193(2) 0.0253(8) Uani 1 1 d . . . . . C31 C 0.2578(4) 0.6648(3) 1.0369(2) 0.0239(8) Uani 1 1 d . . . . . H31 H 0.224393 0.630053 1.085137 0.029 Uiso 1 1 calc R U . . . C32 C 0.3225(4) 0.6140(3) 0.9857(2) 0.0230(8) Uani 1 1 d . . . . . C33 C 0.1647(5) 0.8167(3) 1.0751(2) 0.0296(9) Uani 1 1 d . . . . . C34 C 0.1845(8) 0.9199(4) 1.0519(4) 0.0597(17) Uani 1 1 d . . . . . H34A H 0.281916 0.920091 1.050608 0.090 Uiso 1 1 calc R U . . . H34B H 0.149983 0.954320 1.001597 0.090 Uiso 1 1 calc R U . . . H34C H 0.134341 0.951599 1.088645 0.090 Uiso 1 1 calc R U . . . C35 C 0.2193(9) 0.7668(5) 1.1536(3) 0.073(2) Uani 1 1 d . . . . . H35A H 0.316991 0.766725 1.151330 0.109 Uiso 1 1 calc R U . . . H35B H 0.170312 0.801185 1.188964 0.109 Uiso 1 1 calc R U . . . H35C H 0.205682 0.700496 1.171085 0.109 Uiso 1 1 calc R U . . . C36 C 0.0143(7) 0.8180(7) 1.0768(5) 0.077(2) Uani 1 1 d . . . . . H36A H 0.000042 0.751922 1.091607 0.116 Uiso 1 1 calc R U . . . H36B H -0.035260 0.850066 1.113391 0.116 Uiso 1 1 calc R U . . . H36C H -0.019618 0.852787 1.026343 0.116 Uiso 1 1 calc R U . . . C37 C 0.4083(4) 0.8250(3) 0.8244(2) 0.0248(8) Uani 1 1 d . . . . . H37 H 0.390443 0.891954 0.818235 0.030 Uiso 1 1 calc R U . . . C38 C 0.5104(5) 0.8732(3) 0.7045(2) 0.0294(9) Uani 1 1 d . . . . . C39 C 0.4049(6) 0.9340(4) 0.6595(3) 0.0427(12) Uani 1 1 d D . . . . H39 H 0.314333 0.923346 0.665572 0.051 Uiso 1 1 calc R U . A 1 C40 C 0.4480(15) 1.0140(8) 0.6031(8) 0.033(3) Uiso 0.49(4) 1 d D . P B 1 H40 H 0.379788 1.061782 0.573809 0.040 Uiso 0.49(4) 1 calc R U P B 1 C41 C 0.5832(16) 1.0271(7) 0.5881(8) 0.035(4) Uiso 0.49(4) 1 d D . P B 1 H41 H 0.603992 1.080714 0.548200 0.042 Uiso 0.49(4) 1 calc R U P B 1 C42 C 0.6875(18) 0.9616(7) 0.6314(7) 0.030(3) Uiso 0.49(4) 1 d D . P B 1 H42 H 0.780016 0.968522 0.622785 0.036 Uiso 0.49(4) 1 calc R U P B 1 C43 C 0.6454(5) 0.8852(3) 0.6883(2) 0.0317(10) Uani 1 1 d D . . . . C44 C 0.7625(5) 0.8194(4) 0.7341(2) 0.0359(10) Uani 1 1 d . . . . . H44A H 0.724785 0.782186 0.783142 0.043 Uiso 1 1 calc R U . . . H44B H 0.818649 0.859212 0.744904 0.043 Uiso 1 1 calc R U . . . C45 C 0.8556(5) 0.7488(3) 0.6960(2) 0.0318(9) Uani 1 1 d . . . . . H45A H 0.930920 0.710997 0.729375 0.038 Uiso 1 1 calc R U . . . H45B H 0.802373 0.703452 0.691190 0.038 Uiso 1 1 calc R U . . . C46 C 0.9162(4) 0.7953(3) 0.6192(2) 0.0295(9) Uani 1 1 d . . . . . C47 C 1.0320(5) 0.8339(3) 0.6110(3) 0.0344(10) Uani 1 1 d . . . . . H47 H 1.072676 0.830948 0.655140 0.041 Uiso 1 1 calc R U . . . C48 C 1.0900(5) 0.8764(3) 0.5407(3) 0.0361(10) Uani 1 1 d . . . . . H48 H 1.169313 0.901971 0.537072 0.043 Uiso 1 1 calc R U . . . C49 C 1.0318(5) 0.8816(3) 0.4758(3) 0.0347(10) Uani 1 1 d . . . . . H49 H 1.071518 0.910474 0.427425 0.042 Uiso 1 1 calc R U . . . C50 C 0.9158(5) 0.8448(3) 0.4813(3) 0.0297(9) Uani 1 1 d . . . . . H50 H 0.875530 0.848376 0.436909 0.036 Uiso 1 1 calc R U . . . C51 C 0.8586(4) 0.8026(3) 0.5525(2) 0.0275(9) Uani 1 1 d . . . . . C52 C 0.6841(4) 0.7460(3) 0.5087(2) 0.0258(8) Uani 1 1 d . . . . . H52 H 0.730837 0.752985 0.460335 0.031 Uiso 1 1 calc R U . . . N5 N 0.9710(6) 0.6019(4) 0.5333(4) 0.0702(18) Uani 1 1 d . . . . . C53 C 0.9885(6) 0.5356(5) 0.5855(4) 0.0522(15) Uani 1 1 d . . . . . C54 C 1.0075(7) 0.4502(7) 0.6506(5) 0.079(2) Uani 1 1 d . . . . . H54A H 0.933788 0.457237 0.689229 0.118 Uiso 1 1 calc R U . . . H54B H 1.095583 0.441816 0.671442 0.118 Uiso 1 1 calc R U . . . H54C H 1.005985 0.393991 0.634950 0.118 Uiso 1 1 calc R U . . . N6 N 0.4374(7) 1.0127(4) 0.8930(4) 0.0628(14) Uani 1 1 d . . . . . C55 C 0.5105(7) 1.0400(4) 0.8421(4) 0.0487(13) Uani 1 1 d . . . . . C56 C 0.6003(8) 1.0745(5) 0.7786(4) 0.0610(16) Uani 1 1 d . . . . . H56A H 0.566591 1.071735 0.732459 0.092 Uiso 1 1 calc R U . . . H56B H 0.692085 1.034278 0.786381 0.092 Uiso 1 1 calc R U . . . H56C H 0.603785 1.140997 0.773376 0.092 Uiso 1 1 calc R U . . . C42A C 0.6548(17) 0.9656(7) 0.6224(6) 0.028(3) Uiso 0.51(4) 1 d D . P B 2 H42A H 0.742160 0.981852 0.609398 0.033 Uiso 0.51(4) 1 calc R U P B 2 C41A C 0.5517(15) 1.0224(7) 0.5756(7) 0.033(3) Uiso 0.51(4) 1 d D . P B 2 H41A H 0.570448 1.073273 0.532489 0.039 Uiso 0.51(4) 1 calc R U P B 2 C40A C 0.4193(14) 1.0040(8) 0.5924(6) 0.031(3) Uiso 0.51(4) 1 d D . P B 2 H40A H 0.346204 1.037114 0.560195 0.037 Uiso 0.51(4) 1 calc R U P B 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 O1 0.0318(15) 0.0294(15) 0.0155(13) -0.0108(11) -0.0010(11) -0.0056(11) O2 0.0290(14) 0.0223(13) 0.0179(13) -0.0107(11) 0.0001(10) -0.0002(11) Cu1 0.0284(3) 0.0218(3) 0.0142(3) -0.0092(2) -0.0003(2) -0.0024(2) Br1 0.0322(3) 0.0234(2) 0.0242(2) -0.00769(18) 0.00121(17) 0.00216(17) Br2 0.0583(4) 0.0511(4) 0.0795(5) -0.0393(3) 0.0131(3) -0.0193(3) Cu2 0.0458(4) 0.0403(4) 0.0340(4) -0.0166(3) 0.0044(3) -0.0089(3) Br4 0.0607(4) 0.0514(4) 0.0386(3) -0.0127(3) 0.0116(2) -0.0223(3) N1 0.0263(16) 0.0262(17) 0.0170(16) -0.0101(13) -0.0002(13) -0.0016(13) N2 0.0277(16) 0.0221(16) 0.0177(15) -0.0097(13) -0.0017(12) -0.0035(13) N3 0.0349(18) 0.0225(17) 0.0179(16) -0.0063(13) -0.0004(13) -0.0028(14) N4 0.0281(17) 0.0259(17) 0.0212(17) -0.0105(14) -0.0002(13) -0.0031(13) C1 0.031(2) 0.0181(18) 0.0180(18) -0.0081(15) -0.0037(15) 0.0001(15) C2 0.031(2) 0.024(2) 0.022(2) -0.0105(16) -0.0014(16) -0.0038(16) C3 0.035(2) 0.028(2) 0.0179(19) -0.0118(16) 0.0029(16) -0.0052(17) C4 0.034(2) 0.027(2) 0.0196(19) -0.0110(16) 0.0011(16) -0.0052(16) C5 0.031(2) 0.026(2) 0.021(2) -0.0111(16) -0.0021(16) -0.0040(16) C6 0.032(2) 0.0208(18) 0.0165(18) -0.0089(15) -0.0012(15) -0.0019(15) C7 0.036(2) 0.033(2) 0.022(2) -0.0158(17) 0.0009(17) -0.0064(18) C8 0.049(3) 0.067(3) 0.028(2) -0.029(2) 0.007(2) -0.024(3) C9 0.056(3) 0.037(3) 0.023(2) -0.0112(19) -0.010(2) -0.004(2) C10 0.042(2) 0.036(2) 0.029(2) -0.0172(19) -0.0035(18) -0.0072(19) C11 0.028(2) 0.0226(19) 0.0197(19) -0.0090(15) -0.0024(15) -0.0018(15) C12 0.0261(19) 0.034(2) 0.0138(17) -0.0079(16) -0.0026(14) -0.0033(16) C13 0.029(2) 0.032(2) 0.0208(19) -0.0111(17) -0.0031(16) -0.0025(16) C14 0.024(2) 0.048(3) 0.025(2) -0.015(2) -0.0023(16) 0.0011(18) C15 0.026(2) 0.052(3) 0.022(2) -0.009(2) -0.0006(16) -0.0066(19) C16 0.032(2) 0.041(3) 0.023(2) -0.0056(18) -0.0015(17) -0.0113(18) C17 0.031(2) 0.037(2) 0.0175(19) -0.0083(17) -0.0041(16) -0.0078(17) C18 0.041(2) 0.034(2) 0.021(2) -0.0109(17) -0.0011(17) -0.0144(19) C19 0.039(2) 0.029(2) 0.023(2) -0.0146(17) 0.0042(17) -0.0090(18) C20 0.028(2) 0.026(2) 0.025(2) -0.0141(17) 0.0003(15) -0.0023(15) C21 0.037(2) 0.027(2) 0.030(2) -0.0172(18) -0.0015(17) -0.0039(17) C22 0.039(2) 0.024(2) 0.037(2) -0.0132(18) -0.0033(19) -0.0060(17) C23 0.038(2) 0.025(2) 0.024(2) -0.0042(17) -0.0038(17) -0.0062(17) C24 0.028(2) 0.025(2) 0.025(2) -0.0104(16) -0.0027(16) -0.0024(15) C25 0.0260(19) 0.025(2) 0.025(2) -0.0128(16) -0.0034(15) -0.0020(15) C26 0.0244(19) 0.025(2) 0.0180(18) -0.0088(15) -0.0037(14) 0.0001(15) C27 0.0257(19) 0.025(2) 0.0146(17) -0.0095(15) -0.0022(14) -0.0035(15) C28 0.029(2) 0.025(2) 0.0174(18) -0.0101(16) -0.0036(15) -0.0012(15) C29 0.035(2) 0.023(2) 0.0212(19) -0.0125(16) -0.0025(16) 0.0009(16) C30 0.030(2) 0.026(2) 0.0203(19) -0.0127(16) -0.0032(15) 0.0020(16) C31 0.0254(19) 0.030(2) 0.0183(18) -0.0128(16) -0.0015(14) -0.0009(15) C32 0.0273(19) 0.025(2) 0.0171(18) -0.0089(15) -0.0042(15) -0.0006(15) C33 0.041(2) 0.027(2) 0.020(2) -0.0139(17) 0.0033(17) 0.0023(17) C34 0.092(5) 0.040(3) 0.050(3) -0.028(3) 0.026(3) -0.016(3) C35 0.132(7) 0.049(3) 0.028(3) -0.023(3) -0.014(3) 0.023(4) C36 0.048(4) 0.110(6) 0.099(6) -0.080(5) 0.021(4) -0.011(4) C37 0.035(2) 0.0204(19) 0.0205(19) -0.0099(16) -0.0012(16) -0.0023(15) C38 0.048(3) 0.0176(19) 0.021(2) -0.0093(16) 0.0050(17) -0.0016(17) C39 0.048(3) 0.036(3) 0.031(2) -0.005(2) 0.007(2) 0.006(2) C43 0.051(3) 0.025(2) 0.024(2) -0.0154(17) 0.0066(18) -0.0096(19) C44 0.043(3) 0.052(3) 0.021(2) -0.015(2) 0.0029(18) -0.022(2) C45 0.038(2) 0.034(2) 0.025(2) -0.0068(18) -0.0091(18) -0.0091(18) C46 0.032(2) 0.028(2) 0.028(2) -0.0091(17) -0.0066(17) -0.0011(17) C47 0.036(2) 0.033(2) 0.035(2) -0.0111(19) -0.0114(19) -0.0035(18) C48 0.035(2) 0.031(2) 0.043(3) -0.014(2) -0.002(2) -0.0067(18) C49 0.037(2) 0.028(2) 0.039(3) -0.0125(19) 0.0052(19) -0.0060(18) C50 0.037(2) 0.024(2) 0.029(2) -0.0109(17) 0.0001(17) -0.0044(17) C51 0.028(2) 0.024(2) 0.032(2) -0.0120(17) -0.0024(17) -0.0011(16) C52 0.031(2) 0.027(2) 0.0188(19) -0.0074(16) 0.0019(15) -0.0054(16) N5 0.062(3) 0.044(3) 0.112(5) -0.041(3) 0.029(3) -0.019(3) C53 0.035(3) 0.047(3) 0.087(5) -0.041(4) 0.007(3) -0.009(2) C54 0.045(4) 0.117(7) 0.084(5) -0.043(5) -0.022(3) -0.006(4) N6 0.088(4) 0.035(3) 0.068(4) -0.018(2) -0.006(3) -0.013(3) C55 0.074(4) 0.027(2) 0.051(3) -0.019(2) -0.009(3) -0.009(2) C56 0.076(4) 0.051(3) 0.064(4) -0.030(3) 0.000(3) -0.011(3) 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' Br Br -0.6763 1.2805 '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' 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_ _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 C1 O1 Cu1 129.1(3) . . ? C27 O2 Cu1 128.9(2) . . ? O1 Cu1 Br1 91.57(9) . . ? O1 Cu1 N1 89.23(12) . . ? O1 Cu1 N3 90.12(13) . . ? O2 Cu1 O1 179.75(13) . . ? O2 Cu1 Br1 88.65(8) . . ? O2 Cu1 N1 90.58(12) . . ? O2 Cu1 N3 89.83(12) . . ? N1 Cu1 Br1 119.56(9) . . ? N3 Cu1 Br1 125.79(10) . . ? N3 Cu1 N1 114.64(14) . . ? Br2 Cu2 Br4 178.17(4) . . ? C11 N1 Cu1 124.3(3) . . ? C11 N1 C12 115.6(3) . . ? C12 N1 Cu1 120.0(2) . . ? C25 N2 H2 116.4 . . ? C26 N2 H2 116.4 . . ? C26 N2 C25 127.2(4) . . ? C37 N3 Cu1 122.9(3) . . ? C37 N3 C38 114.9(3) . . ? C38 N3 Cu1 120.6(3) . . ? C51 N4 H4 116.2 . . ? C52 N4 H4 116.2 . . ? C52 N4 C51 127.6(4) . . ? O1 C1 C2 119.8(4) . . ? O1 C1 C6 123.8(4) . . ? C6 C1 C2 116.4(3) . . ? C3 C2 C1 120.8(4) . . ? C3 C2 C52 116.5(4) . . ? C52 C2 C1 122.6(4) . . ? C2 C3 H3 118.6 . . ? C4 C3 C2 122.8(4) . . ? C4 C3 H3 118.6 . . ? C3 C4 C5 115.9(4) . . ? C3 C4 C7 123.8(4) . . ? C5 C4 C7 120.4(4) . . ? C4 C5 H5 118.0 . . ? C4 C5 C6 124.0(4) . . ? C6 C5 H5 118.0 . . ? C1 C6 C11 123.9(3) . . ? C5 C6 C1 120.0(4) . . ? C5 C6 C11 116.0(4) . . ? C4 C7 C9 109.1(3) . . ? C4 C7 C10 109.7(4) . . ? C8 C7 C4 111.5(4) . . ? C8 C7 C9 110.1(4) . . ? C8 C7 C10 107.0(4) . . ? C10 C7 C9 109.5(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C6 126.0(4) . . ? N1 C11 H11 117.0 . . ? C6 C11 H11 117.0 . . ? C13 C12 N1 117.5(4) . . ? C13 C12 C17 121.4(4) . . ? C17 C12 N1 121.1(4) . . ? C12 C13 H13 120.0 . . ? C14 C13 C12 120.0(4) . . ? C14 C13 H13 120.0 . . ? C13 C14 H14 120.2 . . ? C15 C14 C13 119.6(4) . . ? C15 C14 H14 120.2 . . ? C14 C15 H15 119.8 . . ? C14 C15 C16 120.4(4) . . ? C16 C15 H15 119.8 . . ? C15 C16 H16 119.0 . . ? C15 C16 C17 122.0(4) . . ? C17 C16 H16 119.0 . . ? C12 C17 C18 122.3(4) . . ? C16 C17 C12 116.6(4) . . ? C16 C17 C18 121.0(4) . . ? C17 C18 H18A 108.9 . . ? C17 C18 H18B 108.9 . . ? C17 C18 C19 113.4(3) . . ? H18A C18 H18B 107.7 . . ? C19 C18 H18A 108.9 . . ? C19 C18 H18B 108.9 . . ? C18 C19 H19A 108.9 . . ? C18 C19 H19B 108.9 . . ? H19A C19 H19B 107.7 . . ? C20 C19 C18 113.3(4) . . ? C20 C19 H19A 108.9 . . ? C20 C19 H19B 108.9 . . ? C21 C20 C19 118.1(4) . . ? C21 C20 C25 117.8(4) . . ? C25 C20 C19 124.0(4) . . ? C20 C21 H21 119.1 . . ? C22 C21 C20 121.7(4) . . ? C22 C21 H21 119.1 . . ? C21 C22 H22 120.1 . . ? C21 C22 C23 119.7(4) . . ? C23 C22 H22 120.1 . . ? C22 C23 H23 119.9 . . ? C24 C23 C22 120.2(4) . . ? C24 C23 H23 119.9 . . ? C23 C24 H24 120.2 . . ? C23 C24 C25 119.6(4) . . ? C25 C24 H24 120.2 . . ? C20 C25 N2 118.3(4) . . ? C24 C25 N2 120.8(4) . . ? C24 C25 C20 121.0(4) . . ? N2 C26 H26 118.3 . . ? N2 C26 C32 123.4(4) . . ? C32 C26 H26 118.3 . . ? O2 C27 C28 123.8(4) . . ? O2 C27 C32 119.5(3) . . ? C28 C27 C32 116.7(3) . . ? C27 C28 C37 123.5(3) . . ? C29 C28 C27 120.2(4) . . ? C29 C28 C37 116.3(4) . . ? C28 C29 H29 118.3 . . ? C30 C29 C28 123.3(4) . . ? C30 C29 H29 118.3 . . ? C29 C30 C33 122.2(4) . . ? C31 C30 C29 116.8(4) . . ? C31 C30 C33 120.9(4) . . ? C30 C31 H31 118.8 . . ? C30 C31 C32 122.4(4) . . ? C32 C31 H31 118.8 . . ? C26 C32 C27 122.3(4) . . ? C31 C32 C26 117.0(4) . . ? C31 C32 C27 120.5(4) . . ? C34 C33 C30 111.7(4) . . ? C34 C33 C35 107.2(5) . . ? C35 C33 C30 109.8(4) . . ? C36 C33 C30 108.7(4) . . ? C36 C33 C34 108.6(5) . . ? C36 C33 C35 110.8(6) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N3 C37 C28 126.7(4) . . ? N3 C37 H37 116.7 . . ? C28 C37 H37 116.7 . . ? C39 C38 N3 117.3(4) . . ? C43 C38 N3 121.1(4) . . ? C43 C38 C39 121.6(4) . . ? C38 C39 H39 123.5 . . ? C38 C39 C40 112.9(8) . . ? C40 C39 H39 123.5 . . ? C40A C39 C38 126.4(8) . . ? C39 C40 H40 117.5 . . ? C41 C40 C39 124.9(10) . . ? C41 C40 H40 117.5 . . ? C40 C41 H41 119.8 . . ? C42 C41 C40 120.4(9) . . ? C42 C41 H41 119.8 . . ? C41 C42 H42 122.5 . . ? C41 C42 C43 115.0(11) . . ? C43 C42 H42 122.5 . . ? C38 C43 C42 124.7(9) . . ? C38 C43 C44 123.2(4) . . ? C38 C43 C42A 110.5(8) . . ? C42 C43 C44 112.0(9) . . ? C42A C43 C44 126.3(8) . . ? C43 C44 H44A 108.6 . . ? C43 C44 H44B 108.6 . . ? C43 C44 C45 114.9(4) . . ? H44A C44 H44B 107.5 . . ? C45 C44 H44A 108.6 . . ? C45 C44 H44B 108.6 . . ? C44 C45 H45A 108.6 . . ? C44 C45 H45B 108.6 . . ? H45A C45 H45B 107.6 . . ? C46 C45 C44 114.5(4) . . ? C46 C45 H45A 108.6 . . ? C46 C45 H45B 108.6 . . ? C47 C46 C45 121.3(4) . . ? C47 C46 C51 116.8(4) . . ? C51 C46 C45 121.9(4) . . ? C46 C47 H47 118.9 . . ? C48 C47 C46 122.2(4) . . ? C48 C47 H47 118.9 . . ? C47 C48 H48 120.2 . . ? C47 C48 C49 119.7(4) . . ? C49 C48 H48 120.2 . . ? C48 C49 H49 120.0 . . ? C50 C49 C48 120.0(4) . . ? C50 C49 H49 120.0 . . ? C49 C50 H50 120.2 . . ? C49 C50 C51 119.5(4) . . ? C51 C50 H50 120.2 . . ? C46 C51 N4 117.4(4) . . ? C50 C51 N4 120.8(4) . . ? C50 C51 C46 121.7(4) . . ? N4 C52 C2 122.7(4) . . ? N4 C52 H52 118.7 . . ? C2 C52 H52 118.7 . . ? N5 C53 C54 178.0(7) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54B 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N6 C55 C56 179.6(8) . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56B 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C43 C42A H42A 116.1 . . ? C41A C42A C43 127.8(11) . . ? C41A C42A H42A 116.1 . . ? C42A C41A H41A 120.4 . . ? C42A C41A C40A 119.3(9) . . ? C40A C41A H41A 120.4 . . ? C39 C40A C41A 113.9(10) . . ? C39 C40A H40A 123.1 . . ? C41A C40A H40A 123.1 . . ? 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 O1 Cu1 1.955(3) . ? O1 C1 1.301(5) . ? O2 Cu1 1.948(3) . ? O2 C27 1.305(5) . ? Cu1 Br1 2.4790(7) . ? Cu1 N1 2.106(3) . ? Cu1 N3 2.073(4) . ? Br2 Cu2 2.2274(9) . ? Cu2 Br4 2.2344(9) . ? N1 C11 1.285(5) . ? N1 C12 1.437(5) . ? N2 H2 0.8800 . ? N2 C25 1.421(5) . ? N2 C26 1.316(5) . ? N3 C37 1.291(5) . ? N3 C38 1.443(5) . ? N4 H4 0.8800 . ? N4 C51 1.419(6) . ? N4 C52 1.307(5) . ? C1 C2 1.428(6) . ? C1 C6 1.421(6) . ? C2 C3 1.417(6) . ? C2 C52 1.426(6) . ? C3 H3 0.9500 . ? C3 C4 1.378(6) . ? C4 C5 1.399(6) . ? C4 C7 1.529(6) . ? C5 H5 0.9500 . ? C5 C6 1.403(6) . ? C6 C11 1.447(6) . ? C7 C8 1.526(6) . ? C7 C9 1.536(7) . ? C7 C10 1.532(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11 0.9500 . ? C12 C13 1.394(6) . ? C12 C17 1.411(6) . ? C13 H13 0.9500 . ? C13 C14 1.391(6) . ? C14 H14 0.9500 . ? C14 C15 1.378(7) . ? C15 H15 0.9500 . ? C15 C16 1.386(7) . ? C16 H16 0.9500 . ? C16 C17 1.402(6) . ? C17 C18 1.504(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C18 C19 1.545(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C19 C20 1.505(6) . ? C20 C21 1.395(6) . ? C20 C25 1.405(6) . ? C21 H21 0.9500 . ? C21 C22 1.376(7) . ? C22 H22 0.9500 . ? C22 C23 1.396(6) . ? C23 H23 0.9500 . ? C23 C24 1.385(6) . ? C24 H24 0.9500 . ? C24 C25 1.395(6) . ? C26 H26 0.9500 . ? C26 C32 1.415(6) . ? C27 C28 1.416(6) . ? C27 C32 1.433(6) . ? C28 C29 1.404(5) . ? C28 C37 1.450(6) . ? C29 H29 0.9500 . ? C29 C30 1.390(6) . ? C30 C31 1.382(6) . ? C30 C33 1.536(5) . ? C31 H31 0.9500 . ? C31 C32 1.411(5) . ? C33 C34 1.523(7) . ? C33 C35 1.525(7) . ? C33 C36 1.508(8) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37 0.9500 . ? C38 C39 1.398(7) . ? C38 C43 1.398(7) . ? C39 H39 0.9500 . ? C39 C40 1.435(11) . ? C39 C40A 1.372(10) . ? C40 H40 0.9500 . ? C40 C41 1.402(15) . ? C41 H41 0.9500 . ? C41 C42 1.398(15) . ? C42 H42 0.9500 . ? C42 C43 1.399(10) . ? C43 C44 1.508(7) . ? C43 C42A 1.433(10) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C44 C45 1.535(7) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C45 C46 1.502(6) . ? C46 C47 1.390(7) . ? C46 C51 1.402(6) . ? C47 H47 0.9500 . ? C47 C48 1.384(7) . ? C48 H48 0.9500 . ? C48 C49 1.384(7) . ? C49 H49 0.9500 . ? C49 C50 1.384(7) . ? C50 H50 0.9500 . ? C50 C51 1.391(6) . ? C52 H52 0.9500 . ? N5 C53 1.147(9) . ? C53 C54 1.451(12) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? N6 C55 1.153(8) . ? C55 C56 1.431(10) . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C42A H42A 0.9500 . ? C42A C41A 1.384(15) . ? C41A H41A 0.9500 . ? C41A C40A 1.402(14) . ? C40A H40A 0.9500 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 179.6(4) . . . . ? O1 C1 C2 C52 1.8(6) . . . . ? O1 C1 C6 C5 178.7(4) . . . . ? O1 C1 C6 C11 0.1(6) . . . . ? O2 C27 C28 C29 -179.4(4) . . . . ? O2 C27 C28 C37 -0.4(6) . . . . ? O2 C27 C32 C26 -6.7(6) . . . . ? O2 C27 C32 C31 178.4(4) . . . . ? Cu1 O1 C1 C2 -163.5(3) . . . . ? Cu1 O1 C1 C6 18.8(5) . . . . ? Cu1 O2 C27 C28 -15.2(5) . . . . ? Cu1 O2 C27 C32 164.7(3) . . . . ? Cu1 N1 C11 C6 0.7(6) . . . . ? Cu1 N1 C12 C13 68.9(4) . . . . ? Cu1 N1 C12 C17 -109.6(4) . . . . ? Cu1 N3 C37 C28 14.0(6) . . . . ? Cu1 N3 C38 C39 93.4(4) . . . . ? Cu1 N3 C38 C43 -86.4(4) . . . . ? N1 C12 C13 C14 -178.6(4) . . . . ? N1 C12 C17 C16 179.1(4) . . . . ? N1 C12 C17 C18 1.7(6) . . . . ? N2 C26 C32 C27 -2.2(6) . . . . ? N2 C26 C32 C31 172.9(4) . . . . ? N3 C38 C39 C40 172.7(8) . . . . ? N3 C38 C39 C40A -173.2(9) . . . . ? N3 C38 C43 C42 -174.2(7) . . . . ? N3 C38 C43 C44 1.8(6) . . . . ? N3 C38 C43 C42A -179.6(6) . . . . ? C1 C2 C3 C4 1.2(6) . . . . ? C1 C2 C52 N4 -4.6(6) . . . . ? C1 C6 C11 N1 -9.8(6) . . . . ? C2 C1 C6 C5 0.9(6) . . . . ? C2 C1 C6 C11 -177.7(4) . . . . ? C2 C3 C4 C5 1.7(6) . . . . ? C2 C3 C4 C7 -177.7(4) . . . . ? C3 C2 C52 N4 177.4(4) . . . . ? C3 C4 C5 C6 -3.3(6) . . . . ? C3 C4 C7 C8 11.9(6) . . . . ? C3 C4 C7 C9 -109.9(5) . . . . ? C3 C4 C7 C10 130.2(4) . . . . ? C4 C5 C6 C1 2.1(6) . . . . ? C4 C5 C6 C11 -179.2(4) . . . . ? C5 C4 C7 C8 -167.4(4) . . . . ? C5 C4 C7 C9 70.9(5) . . . . ? C5 C4 C7 C10 -49.1(5) . . . . ? C5 C6 C11 N1 171.5(4) . . . . ? C6 C1 C2 C3 -2.5(6) . . . . ? C6 C1 C2 C52 179.6(4) . . . . ? C7 C4 C5 C6 176.0(4) . . . . ? C11 N1 C12 C13 -110.0(4) . . . . ? C11 N1 C12 C17 71.5(5) . . . . ? C12 N1 C11 C6 179.5(4) . . . . ? C12 C13 C14 C15 0.1(6) . . . . ? C12 C17 C18 C19 82.1(5) . . . . ? C13 C12 C17 C16 0.6(6) . . . . ? C13 C12 C17 C18 -176.7(4) . . . . ? C13 C14 C15 C16 -0.7(6) . . . . ? C14 C15 C16 C17 1.4(7) . . . . ? C15 C16 C17 C12 -1.3(6) . . . . ? C15 C16 C17 C18 176.1(4) . . . . ? C16 C17 C18 C19 -95.1(5) . . . . ? C17 C12 C13 C14 0.0(6) . . . . ? C17 C18 C19 C20 72.8(5) . . . . ? C18 C19 C20 C21 85.3(5) . . . . ? C18 C19 C20 C25 -93.1(5) . . . . ? C19 C20 C21 C22 -179.0(4) . . . . ? C19 C20 C25 N2 0.1(6) . . . . ? C19 C20 C25 C24 178.6(4) . . . . ? C20 C21 C22 C23 0.8(7) . . . . ? C21 C20 C25 N2 -178.3(4) . . . . ? C21 C20 C25 C24 0.3(6) . . . . ? C21 C22 C23 C24 -0.8(7) . . . . ? C22 C23 C24 C25 0.6(6) . . . . ? C23 C24 C25 N2 178.2(4) . . . . ? C23 C24 C25 C20 -0.3(6) . . . . ? C25 N2 C26 C32 -172.0(4) . . . . ? C25 C20 C21 C22 -0.5(6) . . . . ? C26 N2 C25 C20 157.1(4) . . . . ? C26 N2 C25 C24 -21.5(6) . . . . ? C27 C28 C29 C30 0.7(6) . . . . ? C27 C28 C37 N3 -0.1(7) . . . . ? C28 C27 C32 C26 173.2(4) . . . . ? C28 C27 C32 C31 -1.8(6) . . . . ? C28 C29 C30 C31 -1.1(6) . . . . ? C28 C29 C30 C33 -178.4(4) . . . . ? C29 C28 C37 N3 178.9(4) . . . . ? C29 C30 C31 C32 0.0(6) . . . . ? C29 C30 C33 C34 -14.9(6) . . . . ? C29 C30 C33 C35 -133.8(5) . . . . ? C29 C30 C33 C36 104.9(6) . . . . ? C30 C31 C32 C26 -173.8(4) . . . . ? C30 C31 C32 C27 1.4(6) . . . . ? C31 C30 C33 C34 167.9(5) . . . . ? C31 C30 C33 C35 49.1(6) . . . . ? C31 C30 C33 C36 -72.2(6) . . . . ? C32 C27 C28 C29 0.7(6) . . . . ? C32 C27 C28 C37 179.7(4) . . . . ? C33 C30 C31 C32 177.3(4) . . . . ? C37 N3 C38 C39 -72.5(5) . . . . ? C37 N3 C38 C43 107.7(5) . . . . ? C37 C28 C29 C30 -178.3(4) . . . . ? C38 N3 C37 C28 179.6(4) . . . . ? C38 C39 C40 C41 6.2(15) . . . . ? C38 C39 C40A C41A -9.4(14) . . . . ? C38 C43 C44 C45 104.9(5) . . . . ? C38 C43 C42A C41A -4.4(13) . . . . ? C39 C38 C43 C42 5.9(9) . . . . ? C39 C38 C43 C44 -178.1(4) . . . . ? C39 C38 C43 C42A 0.5(7) . . . . ? C39 C40 C41 C42 -2.8(19) . . . . ? C40 C41 C42 C43 0.3(16) . . . . ? C41 C42 C43 C38 -1.8(13) . . . . ? C41 C42 C43 C44 -178.3(8) . . . . ? C42 C43 C44 C45 -78.6(7) . . . . ? C43 C38 C39 C40 -7.5(9) . . . . ? C43 C38 C39 C40A 6.7(11) . . . . ? C43 C44 C45 C46 56.1(5) . . . . ? C43 C42A C41A C40A 1.5(17) . . . . ? C44 C43 C42A C41A 174.1(9) . . . . ? C44 C45 C46 C47 82.0(5) . . . . ? C44 C45 C46 C51 -97.5(5) . . . . ? C45 C46 C47 C48 179.5(4) . . . . ? C45 C46 C51 N4 2.5(6) . . . . ? C45 C46 C51 C50 -179.3(4) . . . . ? C46 C47 C48 C49 0.2(7) . . . . ? C47 C46 C51 N4 -177.1(4) . . . . ? C47 C46 C51 C50 1.1(6) . . . . ? C47 C48 C49 C50 0.3(7) . . . . ? C48 C49 C50 C51 -0.1(7) . . . . ? C49 C50 C51 N4 177.5(4) . . . . ? C49 C50 C51 C46 -0.6(6) . . . . ? C51 N4 C52 C2 -179.2(4) . . . . ? C51 C46 C47 C48 -0.9(7) . . . . ? C52 N4 C51 C46 -162.3(4) . . . . ? C52 N4 C51 C50 19.4(6) . . . . ? C52 C2 C3 C4 179.2(4) . . . . ? C42A C43 C44 C45 -73.5(8) . . . . ? C42A C41A C40A C39 5.2(15) . . . . ?