#------------------------------------------------------------------------------ #$Date: 2018-02-04 00:30:14 +0200 (Sun, 04 Feb 2018) $ #$Revision: 206132 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/43/4514361.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_4514361 loop_ _publ_author_name 'Pei, Lixia' 'Liu, Fengshou' 'Liao, Heng' 'Gao, Jie' 'Zhong, Liu' 'Gao, Haiyang' 'Wu, Qing' _publ_section_title ; Synthesis of Polyethylenes with Controlled Branching with \a-Diimine Nickel Catalysts and Revisiting Formation of Long-Chain Branching ; _journal_issue 2 _journal_name_full 'ACS Catalysis' _journal_page_first 1104 _journal_paper_doi 10.1021/acscatal.7b03282 _journal_volume 8 _journal_year 2018 _chemical_formula_moiety 'C38 H36 Br2 N2 Ni' _chemical_formula_sum 'C38 H36 Br2 N2 Ni' _chemical_formula_weight 739.22 _chemical_name_systematic ; ? ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_date 2016-10-17 _audit_creation_method ; Olex2 1.2-beta (compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227) ; _cell_angle_alpha 90 _cell_angle_beta 109.503(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.579(2) _cell_length_b 14.443(2) _cell_length_c 18.148(3) _cell_measurement_reflns_used 5662 _cell_measurement_temperature 100 _cell_measurement_theta_max 26.909 _cell_measurement_theta_min 2.162 _cell_volume 3355.0(9) _computing_cell_refinement 'SAINT v6.45A (Bruker, 2003)' _computing_data_reduction 'SAINT v6.45A (Bruker, 2003)' _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 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100.0 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0772 _diffrn_reflns_av_unetI/netI 0.1005 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 16888 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 27.05 _diffrn_reflns_theta_max 27.05 _diffrn_reflns_theta_min 1.845 _exptl_absorpt_coefficient_mu 2.989 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.543276 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS v.2.10 (Bruker,2003) was used for absorption correction. R(int) was 0.0999 before and 0.0636 after correction. The Ratio of minimum to maximum transmission is 0.5433. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1504 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.21 _refine_diff_density_max 1.152 _refine_diff_density_min -0.717 _refine_diff_density_rms 0.136 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 428 _refine_ls_number_reflns 7296 _refine_ls_number_restraints 98 _refine_ls_restrained_S_all 1.138 _refine_ls_R_factor_all 0.1393 _refine_ls_R_factor_gt 0.0966 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+45.3052P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2194 _refine_ls_wR_factor_ref 0.2339 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4662 _reflns_number_total 7296 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs7b03282_si_004.cif _cod_data_source_block 1 _cod_depositor_comments 'Adding full bibliography for 4514359--4514361.cif.' _cod_original_cell_volume 3355.2(9) _cod_database_code 4514361 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances H11A-H1C_$1 2.2 with sigma of 0.02 H11B-H7 2.2 with sigma of 0.02 C7-C8 \\sim C8-C7A with sigma of 0.02 C5-C4 \\sim C4-C5A with sigma of 0.02 C1-C3 \\sim C3-C1A with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(C1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 4. Rigid body (RIGU) restrains C1, C1A, C3, C4, C5, C5A, C6, C6A, C7, C7A, C8, C9 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7A)=1-FVAR(1) Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=FVAR(1) Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(H3B)=1-FVAR(2) Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(H3A)=FVAR(2) 6.a Ternary CH refined with riding coordinates: C3(H3A), C3(H3B), C10(H10) 6.b Me refined with riding coordinates: C2(H2A,H2B,H2C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C) 6.c Aromatic/amide H refined with riding coordinates: C5(H5), C5A(H5A), C6(H6), C6A(H6A), C7(H7), C7A(H7A), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38) 6.d Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C1A(H1AA,H1AB,H1AC) ; _shelx_res_file ; 1.res created by SHELXL-2014/7 TITL 1 in P2(1)/c CELL 0.71073 13.5792 14.4432 18.1483 90 109.503 90 ZERR 4 0.0022 0.0024 0.0029 0 0.003 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Br N Ni UNIT 152 144 8 8 4 L.S. 20 PLAN 25 TEMP -173.15 bond $h conf MORE -1 fmap 2 acta SHEL 999 0.82 OMIT 1 0 0 REM REM REM WGHT 0.000000 45.305199 FVAR 0.10024 0.58734 0.49987 Br1 5 -0.009586 0.394597 0.581114 11.000000 0.028490 0.041900 = 0.025690 0.005290 0.007310 -0.001010 Br2 5 0.230066 0.204127 0.641267 11.000000 0.069610 0.039460 = 0.049340 -0.009550 0.019200 0.018690 PART 1 N1 3 0.137061 0.359082 0.773086 21.000000 0.022140 0.021260 = 0.018230 0.001270 0.005710 0.002550 AFIX 66 C4 1 0.152864 0.224143 0.856148 21.000000 0.026680 0.023780 = 0.023560 0.002050 0.004500 -0.004930 C5 1 0.108653 0.153241 0.886454 21.000000 0.034720 0.031400 = 0.033070 0.003240 0.011070 0.000500 AFIX 43 H5A 2 0.150028 0.104639 0.913472 21.000000 -1.200000 AFIX 65 C6 1 0.002602 0.154979 0.876378 21.000000 0.041810 0.038880 = 0.036860 0.003440 0.015070 -0.004990 AFIX 43 H6A 2 -0.026978 0.107541 0.896655 21.000000 -1.200000 AFIX 65 C7 1 -0.059239 0.227620 0.835996 21.000000 0.035640 0.035000 = 0.029150 0.005100 0.009380 -0.003230 AFIX 43 H7A 2 -0.130194 0.228783 0.829255 21.000000 -1.200000 AFIX 65 C8 1 -0.015029 0.298523 0.805690 21.000000 0.035870 0.032280 = 0.026040 0.001150 0.008080 -0.005140 C9 1 0.091022 0.296785 0.815765 21.000000 0.022220 0.018110 = 0.012170 0.003070 0.000150 -0.008230 AFIX 0 C3 1 0.316569 0.129671 0.851481 21.000000 0.043980 0.043280 = 0.043990 -0.002860 0.012080 -0.004360 AFIX 33 H3A 2 0.279358 0.111093 0.798703 21.000000 -1.500000 H3B 2 0.309514 0.082765 0.886866 21.000000 -1.500000 H3C 2 0.389129 0.137906 0.857940 21.000000 -1.500000 AFIX 0 C2 1 0.333843 0.249490 0.954464 21.000000 0.054830 0.056080 = 0.054320 -0.003640 0.017330 -0.000160 AFIX 33 H2A 2 0.307656 0.306974 0.967004 21.000000 -1.500000 H2B 2 0.406240 0.256414 0.959882 21.000000 -1.500000 H2C 2 0.326629 0.202055 0.989365 21.000000 -1.500000 AFIX 0 C1 1 0.270892 0.222092 0.869135 21.000000 0.030670 0.029650 = 0.031000 0.001280 0.008990 -0.000730 AFIX 13 H1A 2 0.284516 0.269353 0.835002 21.000000 -1.200000 AFIX 0 C10 1 -0.085815 0.379008 0.763189 21.000000 0.031160 0.036910 = 0.030300 -0.001510 0.014520 -0.002190 AFIX 13 H10 2 -0.044055 0.407799 0.734589 21.000000 -1.200000 AFIX 0 C11 1 -0.118013 0.463741 0.802504 21.000000 0.036000 0.045440 = 0.034020 -0.001540 0.016430 0.001120 AFIX 33 H11A 2 -0.058902 0.484861 0.845153 21.000000 -1.500000 H11B 2 -0.173108 0.446202 0.821806 21.000000 -1.500000 H11C 2 -0.141955 0.512599 0.764883 21.000000 -1.500000 AFIX 0 C12 1 -0.184182 0.346540 0.695989 21.000000 0.036790 0.040460 = 0.034910 0.001530 0.011600 -0.004620 AFIX 33 H12A 2 -0.167013 0.293452 0.670842 21.000000 -1.500000 H12B 2 -0.208267 0.395621 0.658606 21.000000 -1.500000 H12C 2 -0.238175 0.330444 0.716909 21.000000 -1.500000 PART 2 AFIX 0 N1' 3 0.137061 0.359082 0.773086 -21.000000 0.022140 0.021260 = 0.018230 0.001270 0.005710 0.002550 AFIX 66 C4' 1 0.118250 0.227927 0.849577 -21.000000 0.037160 0.036370 = 0.038710 -0.000740 0.010460 0.001600 C5' 1 0.064443 0.176437 0.888546 -21.000000 0.033570 0.027510 = 0.028270 0.002250 0.007410 0.004890 AFIX 43 H5'A 2 0.097021 0.126815 0.919889 -21.000000 -1.200000 AFIX 65 C6' 1 -0.038055 0.199113 0.880669 -21.000000 0.030900 0.028860 = 0.030290 0.005160 0.008620 -0.003650 AFIX 43 H6'A 2 -0.074055 0.164662 0.906742 -21.000000 -1.200000 AFIX 65 C7' 1 -0.086748 0.273279 0.833824 -21.000000 0.031860 0.032960 = 0.029700 0.003190 0.010080 -0.001270 AFIX 43 H7'A 2 -0.155326 0.288450 0.828554 -21.000000 -1.200000 AFIX 65 C8' 1 -0.032942 0.324769 0.794855 -21.000000 0.020710 0.014190 = 0.014210 0.005430 0.004760 -0.004930 C9' 1 0.069556 0.302094 0.802731 -21.000000 0.024720 0.018170 = 0.017110 0.001360 0.000290 -0.002300 AFIX 0 C3' 1 0.236778 0.099166 0.840422 -21.000000 0.061210 0.057470 = 0.059440 -0.000460 0.021610 0.003710 AFIX 33 H3'A 2 0.191623 0.090409 0.787486 -21.000000 -1.500000 H3'B 2 0.213954 0.060427 0.874577 -21.000000 -1.500000 H3'C 2 0.307027 0.083007 0.844632 -21.000000 -1.500000 AFIX 0 C2' 1 0.307736 0.212745 0.949279 -21.000000 0.050730 0.050600 = 0.053030 0.000200 0.017570 0.001630 AFIX 33 H2'A 2 0.305991 0.275632 0.965927 -21.000000 -1.500000 H2'B 2 0.377599 0.197158 0.952025 -21.000000 -1.500000 H2'C 2 0.285842 0.172151 0.982745 -21.000000 -1.500000 AFIX 0 C1' 1 0.233116 0.201921 0.863946 -21.000000 0.034490 0.031210 = 0.031950 0.000930 0.009950 0.001640 AFIX 13 H1'A 2 0.259421 0.240298 0.830033 -21.000000 -1.200000 AFIX 0 C10' 1 -0.090334 0.412676 0.754751 -21.000000 0.031190 0.036520 = 0.029200 -0.000590 0.014030 -0.000400 AFIX 13 H10A 2 -0.048198 0.458325 0.738577 -21.000000 -1.200000 AFIX 0 C11' 1 -0.128759 0.441671 0.822835 -21.000000 0.033820 0.043110 = 0.031300 0.000580 0.017740 -0.003640 AFIX 33 H11D 2 -0.070171 0.460895 0.866737 -21.000000 -1.500000 H11E 2 -0.162572 0.390053 0.837665 -21.000000 -1.500000 H11F 2 -0.177320 0.492014 0.806249 -21.000000 -1.500000 AFIX 0 C12' 1 -0.185331 0.372212 0.689021 -21.000000 0.035740 0.039460 = 0.032980 -0.001000 0.011700 -0.001680 AFIX 33 H12D 2 -0.166228 0.360722 0.643464 -21.000000 -1.500000 H12E 2 -0.242094 0.415612 0.676380 -21.000000 -1.500000 H12F 2 -0.206526 0.315234 0.706496 -21.000000 -1.500000 PART 0 AFIX 0 C13 1 0.174108 0.437823 0.800794 11.000000 0.021450 0.021450 = 0.017860 0.000650 0.006030 0.003460 AFIX 66 C14 1 0.149883 0.489555 0.863040 11.000000 0.017660 0.021460 = 0.023010 -0.001450 0.011310 0.000020 C15 1 0.154199 0.449615 0.933735 11.000000 0.028210 0.028160 = 0.021360 0.000860 0.005570 -0.002420 AFIX 43 H15 2 0.175595 0.388442 0.944381 11.000000 -1.200000 AFIX 65 C16 1 0.126534 0.501106 0.988520 11.000000 0.031690 0.052760 = 0.022170 -0.012430 0.015030 -0.009640 AFIX 43 H16 2 0.129421 0.474384 1.035819 11.000000 -1.200000 AFIX 65 C17 1 0.094553 0.592536 0.972608 11.000000 0.030640 0.046200 = 0.049780 -0.019250 0.022440 -0.001930 AFIX 43 H17 2 0.076044 0.626986 1.009262 11.000000 -1.200000 AFIX 65 C18 1 0.090238 0.632477 0.901914 11.000000 0.047270 0.026610 = 0.073800 -0.004360 0.033790 -0.001680 AFIX 43 H18 2 0.068841 0.693650 0.891269 11.000000 -1.200000 AFIX 65 C19 1 0.117902 0.580988 0.847129 11.000000 0.039070 0.025880 = 0.039680 -0.000080 0.023750 -0.001820 AFIX 43 H19 2 0.115015 0.607711 0.799829 11.000000 -1.200000 AFIX 0 C20 1 0.242587 0.482084 0.760946 11.000000 0.017640 0.022870 = 0.015270 -0.000620 0.003250 0.003380 AFIX 66 C21 1 0.313808 0.558322 0.798182 11.000000 0.019690 0.035130 = 0.025270 -0.004870 0.009840 -0.002800 C22 1 0.374023 0.550557 0.876661 11.000000 0.041630 0.043010 = 0.029570 -0.008810 0.019980 -0.003020 AFIX 43 H22 2 0.366479 0.499267 0.905297 11.000000 -1.200000 AFIX 65 C23 1 0.445513 0.619451 0.912341 11.000000 0.030430 0.078140 = 0.034920 -0.027030 0.008440 -0.021870 AFIX 43 H23 2 0.485801 0.614255 0.964848 11.000000 -1.200000 AFIX 65 C24 1 0.456789 0.696110 0.869541 11.000000 0.065240 0.062290 = 0.060500 -0.038660 0.036410 -0.042990 AFIX 43 H24 2 0.504621 0.742204 0.893414 11.000000 -1.200000 AFIX 65 C25 1 0.396574 0.703877 0.791062 11.000000 0.054820 0.064600 = 0.052960 -0.019490 0.032010 -0.032840 AFIX 43 H25 2 0.404119 0.755168 0.762427 11.000000 -1.200000 AFIX 65 C26 1 0.325084 0.634984 0.755382 11.000000 0.039900 0.033620 = 0.034860 -0.007200 0.024060 -0.013200 AFIX 43 H26 2 0.284796 0.640180 0.702874 11.000000 -1.200000 AFIX 0 N2 3 0.238614 0.442276 0.695665 11.000000 0.022610 0.029120 = 0.019940 0.000160 0.008490 0.000780 AFIX 66 C27 1 0.298474 0.471843 0.648703 11.000000 0.030210 0.034370 = 0.026030 -0.005840 0.014760 -0.000090 C28 1 0.241403 0.509162 0.576448 11.000000 0.033620 0.037450 = 0.028050 -0.001890 0.013870 -0.002670 AFIX 43 H28 2 0.168973 0.512562 0.561359 11.000000 -1.200000 AFIX 65 C29 1 0.292585 0.541397 0.526745 11.000000 0.036720 0.041550 = 0.030830 -0.002080 0.016670 -0.003370 AFIX 43 H29 2 0.254401 0.566366 0.478401 11.000000 -1.200000 AFIX 65 C30 1 0.400839 0.536315 0.549296 11.000000 0.037100 0.046770 = 0.036910 -0.004190 0.019600 -0.003640 AFIX 43 H30 2 0.435084 0.557882 0.516041 11.000000 -1.200000 AFIX 65 C31 1 0.457912 0.498996 0.621551 11.000000 0.034350 0.047950 = 0.038250 -0.006600 0.018460 -0.000230 AFIX 43 H31 2 0.530341 0.495596 0.636639 11.000000 -1.200000 AFIX 65 C32 1 0.406730 0.466760 0.671255 11.000000 0.033270 0.046100 = 0.035700 -0.004680 0.016870 0.001220 AFIX 66 C33 1 0.473994 0.432455 0.751377 11.000000 0.038010 0.055540 = 0.039930 -0.003740 0.016070 0.005520 C34 1 0.560338 0.485210 0.792813 11.000000 0.041130 0.064640 = 0.046010 -0.004370 0.015570 0.002020 AFIX 43 H34 2 0.574416 0.540393 0.771861 11.000000 -1.200000 AFIX 65 C35 1 0.625641 0.455490 0.865564 11.000000 0.049380 0.070940 = 0.051080 -0.003200 0.012600 0.002980 AFIX 43 H35 2 0.683412 0.490787 0.893287 11.000000 -1.200000 AFIX 65 C36 1 0.604601 0.373013 0.896881 11.000000 0.051180 0.069550 = 0.051050 -0.000030 0.014490 0.008000 AFIX 43 H36 2 0.648293 0.353129 0.945556 11.000000 -1.200000 AFIX 65 C37 1 0.518256 0.320257 0.855446 11.000000 0.052320 0.063570 = 0.049080 0.001550 0.017170 0.008960 AFIX 43 H37 2 0.504178 0.265074 0.876399 11.000000 -1.200000 AFIX 65 C38 1 0.452952 0.349976 0.782694 11.000000 0.044340 0.057310 = 0.044210 -0.000190 0.017950 0.009430 AFIX 43 H38 2 0.395182 0.314678 0.754972 11.000000 -1.200000 AFIX 0 Ni1 4 0.145802 0.333244 0.666649 11.000000 0.032110 0.025100 = 0.018280 -0.003420 0.008500 -0.000280 HKLF 4 REM 1 in P2(1)/c REM R1 = 0.0891 for 4392 Fo > 4sig(Fo) and 0.1211 for all 6355 data REM 428 parameters refined using 98 restraints END WGHT 0.0000 45.3054 REM Highest difference peak 1.152, deepest hole -0.717, 1-sigma level 0.136 Q1 1 0.2190 0.2649 0.6507 11.00000 0.05 1.15 Q2 1 0.2040 0.1834 0.8585 11.00000 0.05 0.96 Q3 1 0.0865 0.2795 0.6653 11.00000 0.05 0.74 Q4 1 -0.0828 0.2986 0.8389 11.00000 0.05 0.73 Q5 1 0.1782 0.1639 0.6491 11.00000 0.05 0.72 Q6 1 -0.0187 0.4601 0.5814 11.00000 0.05 0.71 Q7 1 0.1412 0.3880 0.6624 11.00000 0.05 0.61 Q8 1 0.2799 0.1729 0.6482 11.00000 0.05 0.59 Q9 1 0.0401 0.1623 0.8959 11.00000 0.05 0.56 Q10 1 0.0582 0.3412 0.5653 11.00000 0.05 0.55 Q11 1 0.2795 0.2372 0.8653 11.00000 0.05 0.55 Q12 1 0.3973 0.7623 0.9163 11.00000 0.05 0.51 Q13 1 -0.0537 0.3431 0.7996 11.00000 0.05 0.48 Q14 1 -0.0230 0.4836 0.6301 11.00000 0.05 0.48 Q15 1 -0.0563 0.2828 0.8855 11.00000 0.05 0.48 Q16 1 0.0112 0.0791 0.8905 11.00000 0.05 0.47 Q17 1 -0.1160 0.4202 0.8251 11.00000 0.05 0.46 Q18 1 -0.1572 0.4115 0.6829 11.00000 0.05 0.45 Q19 1 0.0547 0.3324 0.6378 11.00000 0.05 0.45 Q20 1 0.0060 0.2715 0.8122 11.00000 0.05 0.44 Q21 1 -0.1590 0.3191 0.8664 11.00000 0.05 0.44 Q22 1 -0.1825 0.4968 0.8147 11.00000 0.05 0.42 Q23 1 0.2054 0.0331 0.8597 11.00000 0.05 0.42 Q24 1 0.3024 0.3679 0.6513 11.00000 0.05 0.42 Q25 1 -0.2581 0.2918 0.6954 11.00000 0.05 0.42 ; _shelx_res_checksum 81285 _shelx_hkl_file ; 1 0 0 0.14 0.08 2 0 0 -0.01 0.16 2 0 0 0.09 0.30 3 0 0 67.79 5.19 4 0 0 5.76 0.99 4 0 0 6.08 0.83 5 0 0 46.25 4.15 -5 0 0 47.99 3.30 5 0 0 48.92 3.84 6 0 0 13.11 1.68 6 0 0 13.69 1.50 -6 0 0 13.10 1.09 7 0 0 184.89 15.16 7 0 0 181.34 14.26 -7 0 0 195.32 12.61 8 0 0 166.70 13.36 -8 0 0 177.05 11.77 8 0 0 180.01 14.27 9 0 0 82.11 6.59 9 0 0 80.43 7.12 10 0 0 0.88 1.10 10 0 0 0.07 1.30 11 0 0 8.26 2.20 12 0 0 12.43 2.60 13 0 0 106.67 9.48 14 0 0 7.65 2.70 15 0 0 0.90 2.17 16 0 0 1.17 2.38 0 -1 0 -0.01 0.06 1 -1 0 410.61 32.57 -1 -1 0 419.22 32.58 2 1 0 216.72 16.00 2 -1 0 194.85 15.98 -2 1 0 196.19 13.58 3 1 0 356.83 28.88 -3 1 0 374.64 24.54 3 -1 0 369.77 28.90 -4 1 0 114.87 8.12 4 1 0 124.84 9.73 4 -1 0 111.00 9.73 4 1 0 133.17 9.20 -5 1 0 21.58 1.78 5 1 0 28.46 2.44 5 -1 0 22.27 2.43 5 1 0 30.16 2.27 6 1 0 23.90 2.53 -6 1 0 25.43 1.84 6 -1 0 24.83 2.56 6 1 0 27.02 2.36 7 1 0 21.83 2.10 7 -1 0 17.23 1.95 7 1 0 22.62 2.31 8 1 0 2.71 1.23 8 -1 0 1.32 0.95 8 -1 0 4.92 1.39 -8 1 0 3.15 0.54 9 -1 0 25.63 2.90 9 -1 0 23.62 2.50 9 1 0 25.94 2.83 10 1 0 9.24 2.03 10 -1 0 11.94 2.24 10 -1 0 10.61 1.65 11 -1 0 33.36 3.39 11 1 0 39.19 3.90 11 -1 0 32.86 3.84 12 1 0 59.74 5.52 12 -1 0 53.16 4.89 12 -1 0 51.05 5.37 13 -1 0 21.67 3.52 13 1 0 20.70 3.16 14 1 0 0.95 2.14 14 -1 0 1.20 2.22 15 1 0 0.68 2.11 15 -1 0 -0.78 2.13 16 -1 0 0.38 2.50 16 1 0 -1.06 2.37 0 -2 0 12.26 1.04 0 -2 0 11.31 0.99 1 -2 0 58.27 4.76 -1 -2 0 59.62 4.76 -2 -2 0 13.69 1.24 2 -2 0 11.93 1.09 3 -2 0 17.80 1.58 3 -2 0 13.38 1.34 -4 2 0 37.62 2.49 4 -2 0 33.47 2.85 5 -2 0 0.34 0.35 -5 2 0 0.30 0.28 5 -2 0 0.05 0.65 5 2 0 0.30 0.65 -6 2 0 26.55 1.87 6 -2 0 24.56 2.60 7 -2 0 54.69 4.71 -7 2 0 50.21 3.58 8 -2 0 0.67 1.14 8 2 0 0.25 1.02 8 -2 0 -0.50 0.50 9 -2 0 0.09 0.59 9 -2 0 0.19 1.18 9 2 0 -0.55 1.10 10 2 0 7.91 1.93 10 -2 0 10.85 2.15 11 -2 0 15.56 2.56 11 2 0 16.60 2.70 12 -2 0 -0.01 1.80 12 2 0 3.68 2.03 12 -2 0 0.87 0.95 13 2 0 -1.20 1.85 13 -2 0 0.64 1.09 13 -2 0 -0.34 2.07 14 -2 0 2.57 2.29 14 2 0 2.77 2.22 15 -2 0 3.57 2.50 15 2 0 0.89 2.29 16 -2 0 2.99 2.64 0 -3 0 -0.41 0.29 0 -3 0 -0.28 0.28 -1 -3 0 222.48 17.53 2 -3 0 6.84 0.96 -2 -3 0 10.03 1.02 3 -3 0 7.09 0.93 3 -3 0 5.40 0.74 -4 -3 0 61.57 5.05 4 -3 0 56.43 5.03 4 -3 0 61.99 4.70 5 -3 0 24.63 2.24 5 -3 0 27.00 2.53 6 3 0 11.19 1.73 6 -3 0 16.69 1.94 6 -3 0 17.30 1.63 7 -3 0 22.26 2.44 7 -3 0 20.89 2.09 8 -3 0 23.55 2.68 8 -3 0 23.21 2.30 9 -3 0 0.06 1.23 9 -3 0 1.69 0.87 9 3 0 1.48 1.32 10 3 0 22.89 3.04 10 -3 0 27.20 3.21 10 -3 0 28.89 2.73 11 3 0 16.89 2.80 11 -3 0 17.36 2.28 11 -3 0 17.41 2.68 12 3 0 11.02 2.50 12 -3 0 6.83 1.82 12 -3 0 9.56 2.59 13 -3 0 10.38 2.75 13 3 0 4.82 2.29 14 -3 0 17.17 3.54 15 -3 0 1.07 2.78 -15 -3 0 1.19 1.68 -16 -3 0 6.55 2.13 16 -3 0 3.16 2.70 0 -4 0 20.82 1.80 0 -4 0 18.45 1.72 -1 -4 0 288.46 23.90 1 -4 0 315.18 23.92 1 -4 0 307.31 22.67 -2 -4 0 280.22 23.06 2 -4 0 305.09 23.09 -3 -4 0 33.21 2.70 3 -4 0 26.62 2.65 4 -4 0 2.11 0.82 -4 -4 0 1.68 0.78 4 -4 0 1.66 0.53 5 -4 0 11.35 1.39 5 -4 0 11.68 1.60 -5 -4 0 16.66 1.75 6 -4 0 191.64 14.23 6 -4 0 183.93 13.34 -6 -4 0 150.84 14.14 -7 -4 0 55.73 5.28 7 -4 0 61.23 5.36 7 -4 0 63.73 4.94 8 -4 0 8.92 1.84 -8 -4 0 12.39 1.76 8 -4 0 8.44 1.49 9 -4 0 16.83 2.38 9 -4 0 15.45 1.93 10 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6.64 1.03 1 -6 0 6.04 0.95 1 -6 0 6.71 0.99 -2 -6 0 41.38 3.52 2 -6 0 39.87 3.37 2 -6 0 40.81 3.55 -3 -6 0 232.22 17.08 3 -6 0 195.91 17.03 -4 -6 0 70.21 5.75 4 -6 0 65.25 5.74 5 -6 0 9.74 1.48 5 -6 0 7.77 1.22 6 -6 0 -0.09 1.04 -6 -6 0 0.51 1.04 6 -6 0 0.03 0.70 7 -6 0 11.88 1.92 7 -6 0 10.17 1.53 -7 -6 0 9.32 1.80 8 -6 0 13.91 2.08 -8 -6 0 9.17 1.95 8 -6 0 13.24 1.72 9 -6 0 33.13 3.20 9 -6 0 33.01 3.57 -10 -6 0 57.00 5.09 10 -6 0 50.51 4.63 10 -6 0 48.78 5.04 11 -6 0 33.58 4.21 -11 -6 0 42.81 4.15 -12 -6 0 7.13 2.36 12 -6 0 12.39 2.86 13 -6 0 1.79 2.30 -13 -6 0 1.80 1.83 14 -6 0 -1.99 2.45 -14 -6 0 2.46 1.95 -15 -6 0 -0.76 1.84 15 -6 0 -1.29 2.80 0 -7 0 0.08 0.67 0 -7 0 -0.61 0.63 1 -7 0 114.02 10.67 1 -7 0 121.64 10.16 -1 -7 0 152.46 10.75 -1 -7 0 144.38 10.23 -2 -7 0 222.26 15.89 2 -7 0 200.07 16.64 -2 -7 0 209.48 16.64 2 -7 0 203.32 15.79 3 -7 0 8.69 1.36 -4 -7 0 9.15 1.41 4 -7 0 9.04 1.55 -5 -7 0 2.43 1.23 5 -7 0 2.84 1.16 5 -7 0 1.72 0.69 -6 -7 0 6.79 1.54 6 -7 0 1.36 1.16 6 -7 0 2.20 0.91 7 -7 0 -0.59 1.20 7 -7 0 0.27 0.93 -7 -7 0 -0.11 1.24 8 -7 0 4.42 1.32 8 -7 0 6.84 1.76 9 -7 0 18.66 2.60 10 -7 0 22.67 2.53 10 -7 0 17.16 2.70 -11 -7 0 1.22 1.69 11 -7 0 4.29 2.15 -13 -7 0 0.86 1.81 13 -7 0 2.45 2.41 -14 -7 0 14.42 2.69 14 -7 0 10.22 3.19 15 -7 0 15.39 3.84 -15 -7 0 14.93 2.98 0 -8 0 21.39 2.12 0 -8 0 20.36 2.15 1 -8 0 4.19 1.03 -1 -8 0 2.80 0.93 1 -8 0 4.22 1.04 -1 -8 0 1.89 0.94 -2 -8 0 86.57 6.73 -2 -8 0 88.52 6.50 2 -8 0 73.28 6.71 2 -8 0 74.50 6.40 3 -8 0 51.58 5.11 -3 -8 0 64.33 5.15 3 -8 0 53.43 4.83 -3 -8 0 70.00 5.06 -4 -8 0 3.02 1.15 4 -8 0 -0.20 0.66 4 -8 0 0.33 1.04 5 -8 0 -0.09 0.57 -5 -8 0 2.82 1.31 5 -8 0 1.38 1.17 6 -8 0 8.44 1.77 6 -8 0 5.86 1.25 -6 -8 0 5.61 1.63 7 -8 0 14.30 1.99 7 -8 0 17.19 2.37 -7 -8 0 18.82 2.37 8 -8 0 4.10 1.76 8 -8 0 3.48 1.32 -8 -8 0 3.87 1.72 9 -8 0 11.53 1.83 9 -8 0 11.96 2.42 -9 -8 0 6.34 2.17 -10 -8 0 11.87 2.45 10 -8 0 6.43 2.21 -11 -8 0 27.47 3.47 -12 -8 0 7.83 2.54 12 -8 0 3.07 2.33 13 -8 0 0.60 2.26 -13 -8 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0 -20 20.12 2.78 4 0 -20 -1.10 1.73 3 0 -20 4.61 1.98 2 0 -20 0.74 1.86 1 0 -20 2.73 1.91 0 0 -20 -0.10 1.75 -1 0 -20 12.96 2.68 -2 0 -20 22.60 3.17 -3 0 -20 9.59 2.65 13 1 -20 -0.91 1.97 13 -1 -20 0.30 2.13 12 1 -20 2.72 2.07 12 -1 -20 4.48 2.28 11 -1 -20 6.60 2.26 10 -1 -20 3.06 2.05 8 1 -20 4.73 1.88 8 -1 -20 4.38 1.82 7 1 -20 -0.15 1.75 7 -1 -20 2.57 1.75 6 -1 -20 1.58 1.67 6 1 -20 0.20 1.75 5 1 -20 25.25 3.23 5 -1 -20 36.88 3.48 4 1 -20 34.97 3.79 4 -1 -20 39.34 3.81 3 1 -20 1.77 1.80 3 -1 -20 2.30 1.90 2 1 -20 -0.60 1.70 2 -1 -20 -1.10 1.71 1 1 -20 -1.62 1.62 1 -1 -20 -1.53 1.71 0 -1 -20 0.41 1.93 0 1 -20 0.94 1.98 -1 -1 -20 1.98 2.05 -1 1 -20 0.37 1.93 -2 -1 -20 0.98 2.01 -2 1 -20 1.80 2.10 -3 1 -20 10.51 2.63 -3 -1 -20 13.26 2.80 13 -2 -20 2.31 2.28 13 2 -20 4.33 2.36 12 2 -20 -0.06 1.96 12 -2 -20 0.85 1.99 11 -2 -20 1.02 2.04 10 -2 -20 2.63 1.98 8 2 -20 5.45 1.85 8 -2 -20 8.54 2.06 7 2 -20 -1.38 1.57 7 -2 -20 0.18 1.60 6 2 -20 7.67 2.11 6 -2 -20 11.05 2.34 5 -2 -20 3.86 1.97 5 2 -20 3.00 1.90 4 -2 -20 4.51 2.05 4 2 -20 10.50 2.31 3 2 -20 16.68 2.70 3 -2 -20 15.50 2.71 2 2 -20 14.37 2.62 2 -2 -20 8.58 2.34 1 2 -20 -0.79 1.75 1 -2 -20 1.16 1.94 0 2 -20 0.63 1.94 0 -2 -20 -1.13 1.93 -1 2 -20 -0.70 2.01 -1 -2 -20 0.50 2.01 -2 2 -20 -1.36 1.92 -2 -2 -20 2.56 2.22 -3 2 -20 0.07 2.08 -3 -2 -20 0.64 2.10 12 -3 -20 10.69 2.81 11 -3 -20 17.26 3.11 10 -3 -20 0.56 2.00 9 3 -20 11.64 2.38 9 -3 -20 11.14 2.60 8 3 -20 5.10 1.97 7 -3 -20 19.49 2.81 7 3 -20 18.98 2.86 6 3 -20 20.65 2.83 6 -3 -20 12.91 2.49 5 3 -20 9.03 2.24 5 -3 -20 8.38 2.12 4 -3 -20 3.79 2.00 4 3 -20 2.29 1.90 3 3 -20 1.56 1.82 3 -3 -20 3.33 1.92 2 -3 -20 6.16 2.25 2 3 -20 9.24 2.36 1 -3 -20 7.00 2.33 1 3 -20 4.90 2.12 0 -3 -20 2.22 2.08 0 3 -20 2.85 2.11 -1 3 -20 4.85 2.21 -1 -3 -20 1.10 2.16 -2 -3 -20 4.85 2.43 -2 3 -20 6.01 2.38 12 -4 -20 6.65 2.69 11 -4 -20 -0.14 2.18 10 -4 -20 3.43 2.29 9 -4 -20 -0.34 1.84 9 4 -20 -1.22 1.76 8 4 -20 0.72 1.74 8 -4 -20 1.13 1.87 7 -4 -20 6.68 2.15 7 4 -20 4.10 1.97 6 4 -20 9.45 2.28 6 -4 -20 7.19 2.17 5 -4 -20 10.88 2.42 5 4 -20 9.26 2.35 4 -4 -20 4.94 2.06 4 4 -20 1.82 1.80 3 -4 -20 0.68 2.11 3 4 -20 -1.21 1.77 2 4 -20 -0.67 1.82 2 -4 -20 -0.69 1.82 1 4 -20 0.25 1.90 1 -4 -20 1.72 2.21 0 4 -20 5.82 2.24 0 -4 -20 8.28 2.45 -1 -4 -20 14.80 3.14 -1 4 -20 20.04 3.12 -2 -4 -20 4.45 2.38 -2 4 -20 6.34 2.42 12 -5 -20 1.61 2.33 11 -5 -20 7.78 2.79 -10 -5 20 14.63 3.20 10 -5 -20 11.46 2.78 9 -5 -20 0.72 1.99 -9 -5 20 -0.22 2.32 -8 -5 20 5.61 2.48 8 -5 -20 0.56 1.86 8 5 -20 2.95 1.88 -7 -5 20 6.93 2.54 7 -5 -20 5.37 2.13 7 5 -20 5.84 2.05 6 5 -20 -1.91 1.79 6 -5 -20 -0.09 1.78 -6 -5 20 1.79 2.32 -5 -5 20 2.39 2.44 5 -5 -20 2.83 1.93 5 5 -20 2.61 1.91 -4 -5 20 1.12 2.39 4 -5 -20 2.72 2.05 4 5 -20 1.04 2.01 -3 -5 20 4.16 2.50 3 5 -20 3.48 2.19 3 -5 -20 10.46 2.33 2 5 -20 1.34 2.05 -2 -5 20 1.16 2.27 2 -5 -20 1.85 2.01 1 5 -20 16.61 3.03 1 -5 -20 22.83 3.25 0 -5 -20 0.70 2.03 0 5 -20 0.85 2.00 -1 5 -20 0.92 2.06 -1 -5 -20 0.41 2.24 11 -6 -20 5.45 2.43 -11 -6 20 1.61 2.61 -10 -6 20 7.14 2.86 10 -6 -20 8.38 2.68 -9 -6 20 6.26 2.93 9 -6 -20 9.43 2.41 8 -6 -20 3.81 2.19 -8 -6 20 9.14 2.71 -7 -6 20 1.92 2.49 7 -6 -20 3.76 2.06 7 6 -20 0.29 1.89 7 -6 -20 0.73 1.93 6 -6 -20 5.69 2.12 6 6 -20 2.78 2.07 -6 -6 20 6.22 2.54 5 6 -20 0.16 1.83 5 -6 -20 1.99 1.95 -5 -6 20 -0.16 2.27 -4 -6 20 0.21 2.37 4 -6 -20 0.02 2.02 4 6 -20 -0.49 1.90 3 6 -20 8.94 2.46 -3 -6 20 11.55 3.12 3 -6 -20 10.33 2.53 2 6 -20 16.65 2.88 -2 -6 20 13.34 3.30 2 -6 -20 10.64 2.78 1 6 -20 4.14 2.35 -1 -6 20 6.18 2.72 1 -6 -20 9.19 2.52 0 -6 -20 1.61 2.11 0 6 -20 -1.68 1.89 0 -6 20 0.78 2.51 -1 6 -20 1.01 2.16 -1 -6 -20 3.73 2.46 1 -6 20 1.56 2.77 10 -7 -20 -1.17 2.06 -10 -7 20 2.36 2.58 9 -7 -20 3.08 2.23 -9 -7 20 0.63 2.42 -8 -7 20 27.32 3.72 8 -7 -20 24.66 3.55 7 -7 -20 23.66 3.27 -7 -7 20 22.51 3.72 6 -7 -20 9.28 2.46 -6 -7 20 3.83 2.66 6 7 -20 4.94 2.19 5 -7 -20 0.49 1.98 -5 -7 20 3.58 2.56 5 7 -20 1.83 1.99 4 7 -20 0.28 2.07 -4 -7 20 1.75 2.49 4 -7 -20 2.12 2.09 3 7 -20 6.61 2.40 3 -7 -20 7.68 2.51 -3 -7 20 6.09 3.01 2 -7 -20 5.71 2.36 2 7 -20 5.08 2.36 -2 -7 20 7.21 2.99 1 7 -20 6.19 2.47 1 -7 -20 5.14 2.36 -1 -7 20 3.79 2.91 0 7 -20 11.28 2.92 0 -7 -20 11.98 2.84 0 -7 20 13.86 3.50 -9 -8 20 7.79 2.86 9 -8 -20 3.08 2.40 8 -8 -20 2.62 2.34 -8 -8 20 5.27 2.68 -7 -8 20 -0.04 2.69 7 -8 -20 0.17 2.13 -6 -8 20 2.37 2.91 6 -8 -20 1.51 2.06 6 -8 -20 2.07 2.12 5 -8 -20 -0.81 1.94 -5 -8 20 -0.91 2.54 4 -8 -20 16.51 2.96 -4 -8 20 14.12 3.55 3 -8 -20 3.03 2.23 -3 -8 20 1.19 2.84 3 8 -20 6.10 2.44 2 -8 -20 3.61 2.37 2 8 -20 0.02 2.24 -2 -8 20 2.11 2.69 1 -8 -20 1.24 2.08 -1 -8 20 0.45 2.65 1 8 -20 2.48 2.37 7 -9 -20 -0.36 2.13 6 -9 -20 1.99 2.17 6 -9 -20 1.99 2.28 -6 -9 20 0.61 2.61 -5 -9 20 6.32 3.09 4 -9 -20 0.13 2.23 -4 -9 20 -0.17 2.66 3 -9 -20 -1.50 2.10 8 0 -21 5.85 2.07 7 0 -21 1.78 1.78 6 0 -21 1.24 1.79 5 0 -21 0.57 1.82 4 0 -21 -0.20 1.74 3 0 -21 2.41 2.01 2 0 -21 -0.67 1.88 1 0 -21 0.52 2.02 0 0 -21 2.39 2.17 -1 0 -21 0.60 2.07 12 -1 -21 1.38 2.08 8 -1 -21 0.79 1.81 8 1 -21 0.94 1.79 7 -1 -21 -1.17 1.65 7 1 -21 2.01 1.80 6 -1 -21 0.66 1.80 6 1 -21 1.28 1.84 5 1 -21 -1.22 1.62 5 -1 -21 -0.65 1.74 4 -1 -21 -0.79 1.78 4 1 -21 -0.23 1.77 3 1 -21 -0.51 1.94 3 -1 -21 -1.30 1.77 2 1 -21 -0.18 1.78 2 -1 -21 -1.80 1.95 1 1 -21 1.58 2.04 1 -1 -21 1.24 2.07 0 1 -21 13.28 2.78 0 -1 -21 11.05 2.68 -1 1 -21 7.17 2.42 -1 -1 -21 4.27 2.32 12 -2 -21 9.86 2.68 11 -2 -21 6.49 2.44 8 2 -21 3.23 2.06 7 -2 -21 17.65 2.74 7 2 -21 14.01 2.71 6 2 -21 11.75 2.39 6 -2 -21 9.59 2.31 5 2 -21 18.83 3.00 5 -2 -21 22.22 3.02 4 -2 -21 14.19 2.72 4 2 -21 13.93 2.59 3 -2 -21 10.06 2.54 3 2 -21 12.74 2.62 2 2 -21 0.31 1.83 2 -2 -21 -0.53 2.09 1 2 -21 -1.19 1.86 1 -2 -21 2.00 2.20 0 2 -21 0.51 1.97 0 -2 -21 6.14 2.34 -1 2 -21 23.10 3.56 -1 -2 -21 23.30 3.45 11 -3 -21 3.47 2.43 8 3 -21 1.63 1.96 7 3 -21 3.15 2.04 7 -3 -21 3.10 2.03 6 3 -21 -0.96 1.90 6 -3 -21 2.43 2.07 5 3 -21 -0.85 1.77 5 -3 -21 -0.93 1.70 4 3 -21 0.93 1.91 4 -3 -21 0.88 1.88 3 3 -21 -1.29 1.89 3 -3 -21 1.14 1.95 2 3 -21 -1.87 1.85 2 -3 -21 -0.42 1.94 1 3 -21 10.41 2.65 1 -3 -21 13.21 2.78 0 -3 -21 18.31 3.11 0 3 -21 17.09 3.08 -1 -3 -21 4.14 2.41 -1 3 -21 2.92 2.27 11 -4 -21 1.93 2.22 10 -4 -21 7.20 2.60 9 4 -21 16.30 2.84 8 4 -21 7.58 2.36 7 -4 -21 -0.23 1.87 7 4 -21 -0.36 1.73 6 -4 -21 0.95 1.84 6 4 -21 1.77 1.96 5 -4 -21 0.19 1.85 5 4 -21 0.65 1.92 4 4 -21 4.32 2.15 4 -4 -21 -0.42 1.98 3 4 -21 3.61 2.15 3 -4 -21 2.98 2.16 2 4 -21 26.02 3.27 2 -4 -21 24.72 3.27 1 4 -21 23.70 3.19 1 -4 -21 24.59 3.53 0 4 -21 1.50 2.22 0 -4 -21 3.23 2.28 10 -5 -21 6.65 2.57 9 -5 -21 4.50 2.25 8 5 -21 6.77 2.37 7 -5 -21 4.47 2.11 7 5 -21 3.50 2.08 6 5 -21 1.47 2.04 6 -5 -21 1.22 2.11 5 5 -21 0.57 1.94 5 -5 -21 -1.27 1.99 4 -5 -21 0.34 1.97 4 5 -21 -1.16 2.01 3 5 -21 4.65 2.28 3 -5 -21 1.62 2.22 2 -5 -21 2.82 2.13 2 5 -21 0.66 2.04 1 -5 -21 1.39 2.18 1 5 -21 1.01 2.25 0 -5 -21 7.79 2.59 0 5 -21 7.79 2.55 9 -6 -21 5.11 2.38 -9 -6 21 9.18 2.96 -8 -6 21 0.64 2.53 -7 -6 21 3.02 2.48 7 6 -21 -0.78 1.99 7 -6 -21 -3.42 1.93 6 6 -21 11.69 2.80 6 -6 -21 21.24 3.15 -6 -6 21 13.91 3.17 -5 -6 21 6.43 2.89 5 6 -21 5.68 2.40 5 -6 -21 14.21 2.76 -4 -6 21 5.45 2.83 4 -6 -21 5.17 2.32 4 6 -21 7.88 2.57 3 -6 -21 5.09 2.29 3 6 -21 5.51 2.39 2 6 -21 -2.60 2.02 2 -6 -21 -0.94 2.17 1 -6 -21 11.88 2.85 1 6 -21 12.35 2.96 8 -7 -21 4.00 2.24 -7 -7 21 2.09 2.80 6 -7 -21 5.89 2.35 6 7 -21 -0.66 2.07 -6 -7 21 1.90 2.68 5 -7 -21 -0.33 1.97 5 7 -21 -2.68 2.00 -5 -7 21 0.60 2.74 4 7 -21 8.09 2.52 4 -7 -21 13.64 2.84 -3 -7 21 5.46 3.17 3 7 -21 1.31 2.23 3 -7 -21 0.50 2.22 2 7 -21 -2.46 2.17 8 0 -22 -1.42 1.70 7 0 -22 0.25 2.01 6 0 -22 4.50 2.22 5 0 -22 45.30 4.49 4 0 -22 7.09 2.33 3 0 -22 1.98 2.11 2 0 -22 8.94 2.52 1 0 -22 5.44 2.36 8 -1 -22 -1.63 1.84 8 1 -22 -0.23 1.78 7 1 -22 5.28 2.17 7 -1 -22 9.88 2.50 6 -1 -22 21.77 3.05 6 1 -22 22.57 3.25 5 1 -22 6.01 2.26 5 -1 -22 6.35 2.31 4 1 -22 1.88 2.04 4 -1 -22 0.19 1.97 3 -1 -22 -0.89 1.96 3 1 -22 0.70 2.03 2 1 -22 3.04 2.15 2 -1 -22 7.87 2.51 1 1 -22 16.78 3.10 1 -1 -22 16.41 3.12 8 2 -22 4.55 2.19 7 -2 -22 2.13 2.01 7 2 -22 1.56 2.04 6 2 -22 0.12 1.94 6 -2 -22 -0.25 1.94 5 -2 -22 1.50 2.14 5 2 -22 0.37 1.98 4 -2 -22 -2.75 1.91 4 2 -22 -1.72 1.96 3 -2 -22 4.24 2.30 3 2 -22 0.69 1.99 2 2 -22 9.94 2.65 2 -2 -22 6.87 2.39 1 -2 -22 0.84 2.21 1 2 -22 3.15 2.29 8 3 -22 4.08 2.24 7 3 -22 0.60 1.97 7 -3 -22 1.49 1.98 6 3 -22 -2.15 1.78 6 -3 -22 -0.55 1.98 5 -3 -22 2.31 2.07 5 3 -22 1.66 2.13 4 3 -22 10.93 2.63 4 -3 -22 10.49 2.61 3 3 -22 8.06 2.41 3 -3 -22 6.47 2.36 2 3 -22 4.99 2.38 2 -3 -22 6.72 2.27 8 4 -22 -0.68 2.02 7 4 -22 -2.33 1.98 7 -4 -22 1.68 2.19 6 -4 -22 -0.98 1.93 6 4 -22 -0.06 1.95 5 -4 -22 7.48 2.51 5 4 -22 10.52 2.70 4 -4 -22 2.66 2.18 4 4 -22 1.75 2.15 3 -4 -22 4.47 2.38 3 4 -22 1.83 2.17 2 -4 -22 -0.55 2.20 2 4 -22 1.10 2.21 8 5 -22 1.71 2.18 7 5 -22 4.83 2.37 7 -5 -22 12.14 2.66 6 5 -22 2.32 2.09 6 -5 -22 3.98 2.53 5 -5 -22 1.87 2.29 5 5 -22 0.62 2.06 4 -5 -22 0.13 2.12 4 5 -22 3.34 2.27 3 -5 -22 -1.21 2.19 3 5 -22 0.41 2.13 7 0 -23 -2.11 2.00 6 0 -23 -3.66 1.97 5 0 -23 4.58 2.28 4 0 -23 -1.20 2.11 7 1 -23 0.32 2.13 7 -1 -23 2.01 2.22 6 -1 -23 2.91 2.13 6 1 -23 4.20 2.29 5 1 -23 3.20 2.27 5 -1 -23 3.82 2.16 4 1 -23 2.93 2.22 4 -1 -23 0.04 2.00 6 -2 -23 1.77 2.10 6 2 -23 0.69 2.02 5 2 -23 -0.59 1.96 5 -2 -23 0.36 2.10 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 33416 _shelx_shelxl_version_number 2014/7 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br -0.00959(4) 0.39460(4) 0.58111(3) 0.03246(14) Uani 1 1 d . . . Br2 Br 0.23007(5) 0.20413(5) 0.64127(4) 0.05297(19) Uani 1 1 d . . . N1 N 0.13706(9) 0.35908(11) 0.77309(9) 0.0208(6) Uani 0.525(4) 1 d PDU A 1 C4 C 0.15287(7) 0.22416(11) 0.85615(12) 0.0257(17) Uani 0.525(4) 1 d PGDU A 1 C5 C 0.10867(15) 0.15324(17) 0.8865(2) 0.0331(18) Uani 0.525(4) 1 d PGU A 1 H5A H 0.1501 0.1046 0.9135 0.040 Uiso 0.525(4) 1 calc PR A 1 C6 C 0.00262(16) 0.15497(18) 0.8764(3) 0.0387(19) Uani 0.525(4) 1 d PGU A 1 H6A H -0.0269 0.1075 0.8967 0.046 Uiso 0.525(4) 1 calc PR A 1 C7 C -0.05923(9) 0.2276(2) 0.8360(2) 0.0336(18) Uani 0.525(4) 1 d PGU A 1 H7A H -0.1302 0.2288 0.8293 0.040 Uiso 0.525(4) 1 calc PR A 1 C8 C -0.01503(14) 0.2985(2) 0.8057(3) 0.0320(18) Uani 0.525(4) 1 d PGDU A 1 C9 C 0.09102(14) 0.29679(19) 0.8158(2) 0.0189(16) Uani 0.525(4) 1 d PGDU A 1 C3 C 0.31658(18) 0.12968(9) 0.85148(10) 0.044(2) Uani 0.525(4) 1 d PDU A 1 H3A H 0.2794 0.1111 0.7987 0.067 Uiso 0.525(4) 1 calc PR A 1 H3B H 0.3095 0.0828 0.8869 0.067 Uiso 0.525(4) 1 calc PR A 1 H3C H 0.3891 0.1379 0.8579 0.067 Uiso 0.525(4) 1 calc PR A 1 C2 C 0.3338(3) 0.24949(13) 0.95447(7) 0.055(2) Uani 0.525(4) 1 d PDU A 1 H2A H 0.3076 0.3070 0.9670 0.083 Uiso 0.525(4) 1 calc PR A 1 H2B H 0.4062 0.2564 0.9599 0.083 Uiso 0.525(4) 1 calc PR A 1 H2C H 0.3266 0.2021 0.9894 0.083 Uiso 0.525(4) 1 calc PR A 1 C1 C 0.27090(8) 0.22210(11) 0.86913(9) 0.0308(11) Uani 0.525(4) 1 d PDU A 1 H1A H 0.2845 0.2694 0.8350 0.037 Uiso 0.525(4) 1 calc PR A 1 C10 C -0.08584(10) 0.37898(8) 0.76318(9) 0.0317(10) Uani 0.525(4) 1 d PDU A 1 H10 H -0.0441 0.4078 0.7346 0.038 Uiso 0.525(4) 1 calc PR A 1 C11 C -0.1180(2) 0.46371(9) 0.80251(10) 0.0373(13) Uani 0.525(4) 1 d PDU A 1 H11A H -0.0589 0.4848 0.8452 0.056 Uiso 0.525(4) 1 calc PR A 1 H11B H -0.1731 0.4462 0.8218 0.056 Uiso 0.525(4) 1 calc PR A 1 H11C H -0.1420 0.5126 0.7649 0.056 Uiso 0.525(4) 1 calc PR A 1 C12 C -0.18422(16) 0.34653(14) 0.69598(11) 0.0375(13) Uani 0.525(4) 1 d PDU A 1 H12A H -0.1671 0.2934 0.6708 0.056 Uiso 0.525(4) 1 calc PR A 1 H12B H -0.2083 0.3956 0.6586 0.056 Uiso 0.525(4) 1 calc PR A 1 H12C H -0.2382 0.3304 0.7169 0.056 Uiso 0.525(4) 1 calc PR A 1 N1' N 0.13706(9) 0.35908(11) 0.77309(9) 0.0208(6) Uani 0.475(4) 1 d PDU A 2 C4' C 0.11826(7) 0.22792(10) 0.84959(13) 0.038(2) Uani 0.475(4) 1 d PGDU A 2 C5' C 0.06445(14) 0.17643(19) 0.88855(19) 0.0305(19) Uani 0.475(4) 1 d PGU A 2 H5'A H 0.0970 0.1268 0.9199 0.037 Uiso 0.475(4) 1 calc PR A 2 C6' C -0.03805(16) 0.1991(2) 0.8807(2) 0.0304(19) Uani 0.475(4) 1 d PGU A 2 H6'A H -0.0740 0.1646 0.9067 0.037 Uiso 0.475(4) 1 calc PR A 2 C7' C -0.08674(12) 0.27327(19) 0.8338(2) 0.0316(19) Uani 0.475(4) 1 d PGU A 2 H7'A H -0.1553 0.2884 0.8286 0.038 Uiso 0.475(4) 1 calc PR A 2 C8' C -0.03293(16) 0.3248(2) 0.7949(3) 0.0166(17) Uani 0.475(4) 1 d PGDU A 2 C9' C 0.06957(14) 0.30209(18) 0.8027(2) 0.0217(18) Uani 0.475(4) 1 d PGDU A 2 C3' C 0.2368(5) 0.09918(7) 0.84043(10) 0.059(2) Uani 0.475(4) 1 d PDU A 2 H3'A H 0.1916 0.0904 0.7875 0.089 Uiso 0.475(4) 1 calc PR A 2 H3'B H 0.2139 0.0604 0.8746 0.089 Uiso 0.475(4) 1 calc PR A 2 H3'C H 0.3070 0.0830 0.8446 0.089 Uiso 0.475(4) 1 calc PR A 2 C2' C 0.3078(3) 0.21276(16) 0.94928(8) 0.051(2) Uani 0.475(4) 1 d PDU A 2 H2'A H 0.3060 0.2756 0.9659 0.077 Uiso 0.475(4) 1 calc PR A 2 H2'B H 0.3776 0.1972 0.9520 0.077 Uiso 0.475(4) 1 calc PR A 2 H2'C H 0.2859 0.1722 0.9827 0.077 Uiso 0.475(4) 1 calc PR A 2 C1' C 0.23314(9) 0.20194(10) 0.86395(9) 0.0328(12) Uani 0.475(4) 1 d PDU A 2 H1'A H 0.2594 0.2403 0.8300 0.039 Uiso 0.475(4) 1 calc PR A 2 C10' C -0.09031(10) 0.41268(10) 0.75476(6) 0.0313(10) Uani 0.475(4) 1 d PDU A 2 H10A H -0.0482 0.4583 0.7386 0.038 Uiso 0.475(4) 1 calc PR A 2 C11' C -0.12874(17) 0.44168(18) 0.82284(7) 0.0344(12) Uani 0.475(4) 1 d PDU A 2 H11D H -0.0702 0.4609 0.8667 0.052 Uiso 0.475(4) 1 calc PR A 2 H11E H -0.1626 0.3901 0.8377 0.052 Uiso 0.475(4) 1 calc PR A 2 H11F H -0.1773 0.4920 0.8062 0.052 Uiso 0.475(4) 1 calc PR A 2 C12' C -0.18531(16) 0.37223(18) 0.68902(9) 0.0360(13) Uani 0.475(4) 1 d PDU A 2 H12D H -0.1662 0.3607 0.6435 0.054 Uiso 0.475(4) 1 calc PR A 2 H12E H -0.2421 0.4156 0.6764 0.054 Uiso 0.475(4) 1 calc PR A 2 H12F H -0.2065 0.3153 0.7065 0.054 Uiso 0.475(4) 1 calc PR A 2 C13 C 0.1741(3) 0.4378(3) 0.8008(2) 0.0204(8) Uani 1 1 d U . . C14 C 0.14988(17) 0.48955(17) 0.86304(12) 0.0196(11) Uani 1 1 d G A . C15 C 0.1542(2) 0.4496(2) 0.93374(14) 0.0266(13) Uani 1 1 d G . . H15 H 0.1756 0.3884 0.9444 0.032 Uiso 1 1 calc R A . C16 C 0.1265(3) 0.5011(3) 0.98852(15) 0.0340(15) Uani 1 1 d G A . H16 H 0.1294 0.4744 1.0358 0.041 Uiso 1 1 calc R . . C17 C 0.0946(3) 0.5925(3) 0.9726(2) 0.0399(16) Uani 1 1 d G . . H17 H 0.0760 0.6270 1.0093 0.048 Uiso 1 1 calc R A . C18 C 0.0902(3) 0.6325(2) 0.9019(2) 0.0458(17) Uani 1 1 d G A . H18 H 0.0688 0.6937 0.8913 0.055 Uiso 1 1 calc R . . C19 C 0.1179(2) 0.58099(18) 0.84713(16) 0.0322(14) Uani 1 1 d G . . H19 H 0.1150 0.6077 0.7998 0.039 Uiso 1 1 calc R A . C20 C 0.2426(3) 0.4821(3) 0.7609(2) 0.0192(11) Uani 1 1 d . A . C21 C 0.31381(18) 0.55832(18) 0.79818(14) 0.0261(13) Uani 1 1 d G . . C22 C 0.3740(2) 0.5506(2) 0.87666(14) 0.0360(15) Uani 1 1 d G A . H22 H 0.3665 0.4993 0.9053 0.043 Uiso 1 1 calc R . . C23 C 0.4455(3) 0.6195(3) 0.91234(17) 0.0484(18) Uani 1 1 d G A . H23 H 0.4858 0.6143 0.9648 0.058 Uiso 1 1 calc R . . C24 C 0.4568(3) 0.6961(3) 0.8695(2) 0.0588(19) Uani 1 1 d G A . H24 H 0.5046 0.7422 0.8934 0.071 Uiso 1 1 calc R . . C25 C 0.3966(3) 0.7039(2) 0.7911(2) 0.0539(19) Uani 1 1 d G A . H25 H 0.4041 0.7552 0.7624 0.065 Uiso 1 1 calc R . . C26 C 0.3251(3) 0.6350(2) 0.75538(16) 0.0332(14) Uani 1 1 d G A . H26 H 0.2848 0.6402 0.7029 0.040 Uiso 1 1 calc R . . N2 N 0.2386(3) 0.4423(3) 0.6957(2) 0.0235(9) Uani 1 1 d U . . C27 C 0.29847(17) 0.47184(18) 0.64870(12) 0.0289(8) Uani 1 1 d GU A . C28 C 0.2414(2) 0.5092(2) 0.57645(14) 0.0321(8) Uani 1 1 d GU . . H28 H 0.1690 0.5126 0.5614 0.039 Uiso 1 1 calc R A . C29 C 0.2926(3) 0.5414(3) 0.52674(15) 0.0350(8) Uani 1 1 d GU A . H29 H 0.2544 0.5664 0.4784 0.042 Uiso 1 1 calc R . . C30 C 0.4008(3) 0.5363(3) 0.5493(2) 0.0384(8) Uani 1 1 d GU . . H30 H 0.4351 0.5579 0.5160 0.046 Uiso 1 1 calc R A . C31 C 0.4579(2) 0.4990(3) 0.6216(2) 0.0386(8) Uani 1 1 d GU A . H31 H 0.5303 0.4956 0.6366 0.046 Uiso 1 1 calc R . . C32 C 0.40673(17) 0.4668(2) 0.67125(15) 0.0370(7) Uani 1 1 d GU . . C33 C 0.4740(2) 0.4325(2) 0.75138(16) 0.0437(8) Uani 1 1 d GU A . C34 C 0.5603(3) 0.4852(3) 0.79281(19) 0.0503(9) Uani 1 1 d GU . . H34 H 0.5744 0.5404 0.7719 0.060 Uiso 1 1 calc R A . C35 C 0.6256(3) 0.4555(4) 0.8656(2) 0.0582(9) Uani 1 1 d GU A . H35 H 0.6834 0.4908 0.8933 0.070 Uiso 1 1 calc R . . C36 C 0.6046(3) 0.3730(4) 0.89688(18) 0.0579(9) Uani 1 1 d GU . . H36 H 0.6483 0.3531 0.9456 0.069 Uiso 1 1 calc R A . C37 C 0.5183(4) 0.3203(3) 0.8554(2) 0.0549(9) Uani 1 1 d GU A . H37 H 0.5042 0.2651 0.8764 0.066 Uiso 1 1 calc R . . C38 C 0.4530(3) 0.3500(2) 0.7827(2) 0.0478(9) Uani 1 1 d GU . . H38 H 0.3952 0.3147 0.7550 0.057 Uiso 1 1 calc R A . Ni1 Ni 0.14580(5) 0.33324(5) 0.66665(3) 0.02514(16) Uani 1 1 d U A . 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 Br1 0.0285(2) 0.0419(3) 0.0257(2) 0.0053(2) 0.00731(17) -0.0010(2) Br2 0.0696(4) 0.0395(3) 0.0493(3) -0.0096(3) 0.0192(3) 0.0187(3) N1 0.0221(10) 0.0213(10) 0.0182(9) 0.0013(9) 0.0057(8) 0.0025(9) C4 0.027(3) 0.024(3) 0.024(3) 0.002(2) 0.005(2) -0.005(2) C5 0.035(3) 0.031(3) 0.033(3) 0.003(2) 0.011(2) 0.000(2) C6 0.042(3) 0.039(3) 0.037(3) 0.003(2) 0.015(2) -0.005(2) C7 0.036(3) 0.035(3) 0.029(3) 0.005(2) 0.009(2) -0.003(2) C8 0.036(3) 0.032(3) 0.026(3) 0.001(2) 0.008(2) -0.005(2) C9 0.022(3) 0.018(3) 0.012(2) 0.003(2) 0.0002(19) -0.008(2) C3 0.044(3) 0.043(3) 0.044(3) -0.003(2) 0.012(2) -0.004(2) C2 0.055(3) 0.056(3) 0.054(3) -0.004(3) 0.017(2) 0.000(3) C1 0.0307(17) 0.0297(17) 0.0310(17) 0.0013(15) 0.0090(13) -0.0007(15) C10 0.0312(15) 0.0369(15) 0.0303(15) -0.0015(13) 0.0145(13) -0.0022(14) C11 0.036(2) 0.0454(19) 0.0340(19) -0.0016(15) 0.0164(16) 0.0011(18) C12 0.037(2) 0.040(2) 0.0349(19) 0.0015(16) 0.0116(16) -0.0046(19) N1' 0.0221(10) 0.0213(10) 0.0182(9) 0.0013(9) 0.0057(8) 0.0025(9) C4' 0.037(3) 0.036(3) 0.039(3) -0.001(2) 0.010(2) 0.002(2) C5' 0.034(3) 0.028(3) 0.028(3) 0.002(2) 0.007(2) 0.005(2) C6' 0.031(3) 0.029(3) 0.030(3) 0.005(2) 0.009(2) -0.004(2) C7' 0.032(3) 0.033(3) 0.030(3) 0.003(2) 0.010(2) -0.001(2) C8' 0.021(3) 0.014(3) 0.014(2) 0.005(2) 0.0048(19) -0.005(2) C9' 0.025(3) 0.018(3) 0.017(3) 0.001(2) 0.000(2) -0.002(2) C3' 0.061(3) 0.058(3) 0.059(3) 0.000(3) 0.022(2) 0.004(3) C2' 0.051(3) 0.051(3) 0.053(3) 0.000(3) 0.018(2) 0.002(3) C1' 0.0345(17) 0.0312(18) 0.0320(17) 0.0009(15) 0.0100(14) 0.0016(15) C10' 0.0312(15) 0.0365(17) 0.0292(14) -0.0006(14) 0.0140(12) -0.0004(15) C11' 0.034(2) 0.043(2) 0.0313(16) 0.0006(17) 0.0177(14) -0.0036(19) C12' 0.036(2) 0.039(2) 0.0330(18) -0.0010(17) 0.0117(16) -0.0017(19) C13 0.0214(13) 0.0215(12) 0.0179(11) 0.0007(10) 0.0060(11) 0.0035(12) C14 0.0177(18) 0.021(2) 0.0230(19) -0.0014(18) 0.0113(15) 0.0000(19) C15 0.028(2) 0.028(3) 0.021(2) 0.001(2) 0.0056(18) -0.002(2) C16 0.032(2) 0.053(3) 0.022(2) -0.012(2) 0.0150(17) -0.010(3) C17 0.031(2) 0.046(3) 0.050(3) -0.019(3) 0.022(2) -0.002(3) C18 0.047(3) 0.027(3) 0.074(3) -0.004(3) 0.034(2) -0.002(3) C19 0.039(2) 0.026(3) 0.040(2) 0.000(2) 0.0237(19) -0.002(2) C20 0.0176(19) 0.023(2) 0.0153(18) -0.0006(18) 0.0032(15) 0.0034(19) C21 0.020(2) 0.035(3) 0.025(2) -0.005(2) 0.0098(16) -0.003(2) C22 0.042(3) 0.043(3) 0.030(2) -0.009(2) 0.0200(19) -0.003(3) C23 0.030(3) 0.078(4) 0.035(3) -0.027(3) 0.008(2) -0.022(3) C24 0.065(3) 0.062(4) 0.060(3) -0.039(3) 0.036(3) -0.043(3) C25 0.055(3) 0.065(4) 0.053(3) -0.019(3) 0.032(2) -0.033(3) C26 0.040(2) 0.034(3) 0.035(2) -0.007(2) 0.0241(18) -0.013(2) N2 0.0226(14) 0.0291(17) 0.0199(13) 0.0002(13) 0.0085(10) 0.0008(12) C27 0.0302(11) 0.0344(14) 0.0260(11) -0.0058(12) 0.0148(10) -0.0001(13) C28 0.0336(12) 0.0374(15) 0.0281(12) -0.0019(12) 0.0139(9) -0.0027(13) C29 0.0367(12) 0.0416(15) 0.0308(12) -0.0021(12) 0.0167(10) -0.0034(13) C30 0.0371(11) 0.0468(15) 0.0369(12) -0.0042(12) 0.0196(11) -0.0036(13) C31 0.0343(12) 0.0479(15) 0.0382(11) -0.0066(12) 0.0185(9) -0.0002(13) C32 0.0333(11) 0.0461(13) 0.0357(10) -0.0047(10) 0.0169(9) 0.0012(12) C33 0.0380(12) 0.0555(12) 0.0399(11) -0.0037(10) 0.0161(10) 0.0055(11) C34 0.0411(14) 0.0646(14) 0.0460(13) -0.0044(12) 0.0156(11) 0.0020(12) C35 0.0494(15) 0.0709(14) 0.0511(14) -0.0032(13) 0.0126(12) 0.0030(13) C36 0.0512(14) 0.0695(15) 0.0510(14) 0.0000(12) 0.0145(12) 0.0080(13) C37 0.0523(14) 0.0636(15) 0.0491(14) 0.0015(13) 0.0172(12) 0.0090(12) C38 0.0443(14) 0.0573(14) 0.0442(13) -0.0002(12) 0.0179(12) 0.0094(12) Ni1 0.0321(3) 0.0251(3) 0.0183(2) -0.0034(2) 0.0085(2) -0.0003(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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 C13 N1 C9 121.5(3) C13 N1 Ni1 113.7(2) C9 N1 Ni1 124.7(2) C5 C4 C9 120.0 C5 C4 C1 119.34(12) C9 C4 C1 120.65(12) C6 C5 C4 120.0 C6 C5 H5A 120.0 C4 C5 H5A 120.0 C5 C6 C7 120.0 C5 C6 H6A 120.0 C7 C6 H6A 120.0 C8 C7 C6 120.0 C8 C7 H7A 120.0 C6 C7 H7A 120.0 C9 C8 C7 120.0 C9 C8 C10 121.68(15) C7 C8 C10 118.30(14) C8 C9 C4 120.0 C8 C9 N1 121.91(12) C4 C9 N1 117.08(12) C1 C3 H3A 109.5 C1 C3 H3B 109.5 H3A C3 H3B 109.5 C1 C3 H3C 109.5 H3A C3 H3C 109.5 H3B C3 H3C 109.5 C1 C2 H2A 109.5 C1 C2 H2B 109.5 H2A C2 H2B 109.5 C1 C2 H2C 109.5 H2A C2 H2C 109.5 H2B C2 H2C 109.5 C4 C1 C2 110.3(2) C4 C1 C3 116.92(15) C2 C1 C3 107.53(12) C4 C1 H1A 107.2 C2 C1 H1A 107.2 C3 C1 H1A 107.2 C8 C10 C12 113.3(2) C8 C10 C11 126.1(2) C12 C10 C11 107.42(12) C8 C10 H10 102.2 C12 C10 H10 102.2 C11 C10 H10 102.2 C10 C11 H11A 109.5 C10 C11 H11B 109.5 H11A C11 H11B 109.5 C10 C11 H11C 109.5 H11A C11 H11C 109.5 H11B C11 H11C 109.5 C10 C12 H12A 109.5 C10 C12 H12B 109.5 H12A C12 H12B 109.5 C10 C12 H12C 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 C5' C4' C9' 120.0 C5' C4' C1' 117.28(13) C9' C4' C1' 122.65(12) C6' C5' C4' 120.0 C6' C5' H5'A 120.0 C4' C5' H5'A 120.0 C5' C6' C7' 120.0 C5' C6' H6'A 120.0 C7' C6' H6'A 120.0 C6' C7' C8' 120.0 C6' C7' H7'A 120.0 C8' C7' H7'A 120.0 C9' C8' C7' 120.0 C9' C8' C10' 125.05(14) C7' C8' C10' 114.38(16) C8' C9' C4' 120.0 C1' C3' H3'A 109.5 C1' C3' H3'B 109.5 H3'A C3' H3'B 109.5 C1' C3' H3'C 109.5 H3'A C3' H3'C 109.5 H3'B C3' H3'C 109.5 C1' C2' H2'A 109.5 C1' C2' H2'B 109.5 H2'A C2' H2'B 109.5 C1' C2' H2'C 109.5 H2'A C2' H2'C 109.5 H2'B C2' H2'C 109.5 C4' C1' C3' 108.1(3) C4' C1' C2' 115.60(19) C3' C1' C2' 107.55(13) C4' C1' H1'A 108.5 C3' C1' H1'A 108.5 C2' C1' H1'A 108.5 C8' C10' C12' 102.3(2) C8' C10' C11' 95.6(2) C12' C10' C11' 107.47(12) C8' C10' H10A 116.3 C12' C10' H10A 116.3 C11' C10' H10A 116.3 C10' C11' H11D 109.5 C10' C11' H11E 109.5 H11D C11' H11E 109.5 C10' C11' H11F 109.5 H11D C11' H11F 109.5 H11E C11' H11F 109.5 C10' C12' H12D 109.5 C10' C12' H12E 109.5 H12D C12' H12E 109.5 C10' C12' H12F 109.5 H12D C12' H12F 109.5 H12E C12' H12F 109.5 N1 C13 C14 126.3(4) N1 C13 C20 114.6(4) C14 C13 C20 119.0(4) C15 C14 C19 120.0 C15 C14 C13 122.9(2) C19 C14 C13 117.0(2) C14 C15 C16 120.0 C14 C15 H15 120.0 C16 C15 H15 120.0 C17 C16 C15 120.0 C17 C16 H16 120.0 C15 C16 H16 120.0 C16 C17 C18 120.0 C16 C17 H17 120.0 C18 C17 H17 120.0 C17 C18 C19 120.0 C17 C18 H18 120.0 C19 C18 H18 120.0 C18 C19 C14 120.0 C18 C19 H19 120.0 C14 C19 H19 120.0 N2 C20 C21 124.7(4) N2 C20 C13 114.0(4) C21 C20 C13 121.1(4) C22 C21 C26 120.0 C22 C21 C20 118.8(2) C26 C21 C20 121.1(2) C23 C22 C21 120.0 C23 C22 H22 120.0 C21 C22 H22 120.0 C22 C23 C24 120.0 C22 C23 H23 120.0 C24 C23 H23 120.0 C25 C24 C23 120.0 C25 C24 H24 120.0 C23 C24 H24 120.0 C24 C25 C26 120.0 C24 C25 H25 120.0 C26 C25 H25 120.0 C25 C26 C21 120.0 C25 C26 H26 120.0 C21 C26 H26 120.0 C20 N2 C27 123.6(4) C20 N2 Ni1 115.1(3) C27 N2 Ni1 121.3(3) C28 C27 C32 120.0 C28 C27 N2 115.51(19) C32 C27 N2 124.49(18) C29 C28 C27 120.0 C29 C28 H28 120.0 C27 C28 H28 120.0 C30 C29 C28 120.0 C30 C29 H29 120.0 C28 C29 H29 120.0 C31 C30 C29 120.0 C31 C30 H30 120.0 C29 C30 H30 120.0 C30 C31 C32 120.0 C30 C31 H31 120.0 C32 C31 H31 120.0 C31 C32 C27 120.0 C31 C32 C33 117.3(2) C27 C32 C33 122.54(19) C34 C33 C38 120.0 C34 C33 C32 117.9(2) C38 C33 C32 122.1(2) C33 C34 C35 120.0 C33 C34 H34 120.0 C35 C34 H34 120.0 C34 C35 C36 120.0 C34 C35 H35 120.0 C36 C35 H35 120.0 C37 C36 C35 120.0 C37 C36 H36 120.0 C35 C36 H36 120.0 C36 C37 C38 120.0 C36 C37 H37 120.0 C38 C37 H37 120.0 C37 C38 C33 120.0 C37 C38 H38 120.0 C33 C38 H38 120.0 N2 Ni1 N1 80.38(12) N2 Ni1 Br2 112.44(12) N1 Ni1 Br2 122.21(5) N2 Ni1 Br1 103.24(11) N1 Ni1 Br1 103.78(5) Br2 Ni1 Br1 124.78(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Br1 Ni1 2.3367(8) Br2 Ni1 2.3132(10) N1 C13 1.277(5) N1 C9 1.4573(16) N1 Ni1 2.0094(18) C4 C5 1.3900 C4 C9 1.3900 C4 C1 1.5404(13) C5 C6 1.3900 C5 H5A 0.9300 C6 C7 1.3900 C6 H6A 0.9300 C7 C8 1.3900 C7 H7A 0.9300 C8 C9 1.3900 C8 C10 1.5412(15) C3 C1 1.5498(15) C3 H3A 0.9600 C3 H3B 0.9600 C3 H3C 0.9600 C2 C1 1.5497(15) C2 H2A 0.9600 C2 H2B 0.9600 C2 H2C 0.9600 C1 H1A 0.9800 C10 C12 1.5504(15) C10 C11 1.5512(16) C10 H10 0.9800 C11 H11A 0.9600 C11 H11B 0.9600 C11 H11C 0.9600 C12 H12A 0.9600 C12 H12B 0.9600 C12 H12C 0.9600 C4' C5' 1.3900 C4' C9' 1.3900 C4' C1' 1.5396(14) C5' C6' 1.3900 C5' H5'A 0.9300 C6' C7' 1.3900 C6' H6'A 0.9300 C7' C8' 1.3900 C7' H7'A 0.9300 C8' C9' 1.3900 C8' C10' 1.5396(15) C3' C1' 1.5497(15) C3' H3'A 0.9600 C3' H3'B 0.9600 C3' H3'C 0.9600 C2' C1' 1.5497(15) C2' H2'A 0.9600 C2' H2'B 0.9600 C2' H2'C 0.9600 C1' H1'A 0.9800 C10' C12' 1.5496(15) C10' C11' 1.5507(16) C10' H10A 0.9800 C11' H11D 0.9600 C11' H11E 0.9600 C11' H11F 0.9600 C12' H12D 0.9600 C12' H12E 0.9600 C12' H12F 0.9600 C13 C14 1.480(5) C13 C20 1.498(7) C14 C15 1.3900 C14 C19 1.3900 C15 C16 1.3900 C15 H15 0.9300 C16 C17 1.3900 C16 H16 0.9300 C17 C18 1.3900 C17 H17 0.9300 C18 C19 1.3900 C18 H18 0.9300 C19 H19 0.9300 C20 N2 1.302(6) C20 C21 1.472(5) C21 C22 1.3900 C21 C26 1.3900 C22 C23 1.3900 C22 H22 0.9300 C23 C24 1.3900 C23 H23 0.9300 C24 C25 1.3900 C24 H24 0.9300 C25 C26 1.3900 C25 H25 0.9300 C26 H26 0.9300 N2 C27 1.426(5) N2 Ni1 1.975(4) C27 C28 1.3900 C27 C32 1.3900 C28 C29 1.3900 C28 H28 0.9300 C29 C30 1.3900 C29 H29 0.9300 C30 C31 1.3900 C30 H30 0.9300 C31 C32 1.3900 C31 H31 0.9300 C32 C33 1.519(4) C33 C34 1.3900 C33 C38 1.3900 C34 C35 1.3900 C34 H34 0.9300 C35 C36 1.3900 C35 H35 0.9300 C36 C37 1.3900 C36 H36 0.9300 C37 C38 1.3900 C37 H37 0.9300 C38 H38 0.9300 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 C9 C4 C5 C6 0.0 C1 C4 C5 C6 178.89(14) C4 C5 C6 C7 0.0 C5 C6 C7 C8 0.0 C6 C7 C8 C9 0.0 C6 C7 C8 C10 -178.4(4) C7 C8 C9 C4 0.0 C10 C8 C9 C4 178.4(4) C7 C8 C9 N1 168.1(4) C10 C8 C9 N1 -13.47(19) C5 C4 C9 C8 0.0 C1 C4 C9 C8 -178.88(14) C5 C4 C9 N1 -168.7(4) C1 C4 C9 N1 12.4(4) C13 N1 C9 C8 91.1(3) Ni1 N1 C9 C8 -87.27(15) C13 N1 C9 C4 -100.4(4) Ni1 N1 C9 C4 81.2(3) C5 C4 C1 C2 -75.1(2) C9 C4 C1 C2 103.8(2) C5 C4 C1 C3 48.1(2) C9 C4 C1 C3 -133.0(2) C9 C8 C10 C12 127.3(2) C7 C8 C10 C12 -54.3(4) C9 C8 C10 C11 -96.9(2) C7 C8 C10 C11 81.5(4) C9' C4' C5' C6' 0.0 C1' C4' C5' C6' 177.19(15) C4' C5' C6' C7' 0.0 C5' C6' C7' C8' 0.0 C6' C7' C8' C9' 0.0 C6' C7' C8' C10' -171.7(4) C7' C8' C9' C4' 0.0 C10' C8' C9' C4' 170.8(4) C5' C4' C9' C8' 0.0 C1' C4' C9' C8' -177.04(16) C5' C4' C1' C3' 58.3(2) C9' C4' C1' C3' -124.6(2) C5' C4' C1' C2' -62.3(2) C9' C4' C1' C2' 114.9(2) C9' C8' C10' C12' 121.3(2) C7' C8' C10' C12' -67.4(3) C9' C8' C10' C11' -129.4(2) C7' C8' C10' C11' 41.9(3) C9 N1 C13 C14 -19.6(5) Ni1 N1 C13 C14 159.0(3) C9 N1 C13 C20 164.8(2) Ni1 N1 C13 C20 -16.7(4) N1 C13 C14 C15 49.7(4) C20 C13 C14 C15 -134.8(3) N1 C13 C14 C19 -127.9(3) C20 C13 C14 C19 47.6(4) C19 C14 C15 C16 0.0 C13 C14 C15 C16 -177.5(3) C14 C15 C16 C17 0.0 C15 C16 C17 C18 0.0 C16 C17 C18 C19 0.0 C17 C18 C19 C14 0.0 C15 C14 C19 C18 0.0 C13 C14 C19 C18 177.6(2) N1 C13 C20 N2 12.0(5) C14 C13 C20 N2 -164.0(3) N1 C13 C20 C21 -162.8(3) C14 C13 C20 C21 21.2(5) N2 C20 C21 C22 -129.1(4) C13 C20 C21 C22 45.1(5) N2 C20 C21 C26 47.8(5) C13 C20 C21 C26 -138.0(3) C26 C21 C22 C23 0.0 C20 C21 C22 C23 176.9(3) C21 C22 C23 C24 0.0 C22 C23 C24 C25 0.0 C23 C24 C25 C26 0.0 C24 C25 C26 C21 0.0 C22 C21 C26 C25 0.0 C20 C21 C26 C25 -176.9(3) C21 C20 N2 C27 -4.4(6) C13 C20 N2 C27 -179.0(3) C21 C20 N2 Ni1 173.6(3) C13 C20 N2 Ni1 -0.9(5) C20 N2 C27 C28 -112.7(4) Ni1 N2 C27 C28 69.4(3) C20 N2 C27 C32 66.3(5) Ni1 N2 C27 C32 -111.7(2) C32 C27 C28 C29 0.0 N2 C27 C28 C29 179.0(3) C27 C28 C29 C30 0.0 C28 C29 C30 C31 0.0 C29 C30 C31 C32 0.0 C30 C31 C32 C27 0.0 C30 C31 C32 C33 -176.2(3) C28 C27 C32 C31 0.0 N2 C27 C32 C31 -178.9(3) C28 C27 C32 C33 176.0(3) N2 C27 C32 C33 -2.9(3) C31 C32 C33 C34 44.3(2) C27 C32 C33 C34 -131.8(2) C31 C32 C33 C38 -134.1(2) C27 C32 C33 C38 49.8(3) C38 C33 C34 C35 0.0 C32 C33 C34 C35 -178.5(2) C33 C34 C35 C36 0.0 C34 C35 C36 C37 0.0 C35 C36 C37 C38 0.0 C36 C37 C38 C33 0.0 C34 C33 C38 C37 0.0 C32 C33 C38 C37 178.4(2) C20 N2 Ni1 N1 -5.9(3) C27 N2 Ni1 N1 172.2(3) C20 N2 Ni1 Br2 -126.9(3) C27 N2 Ni1 Br2 51.2(3) C20 N2 Ni1 Br1 96.1(3) C27 N2 Ni1 Br1 -85.8(3) C13 N1 Ni1 N2 12.8(3) C9 N1 Ni1 N2 -168.67(16) C13 N1 Ni1 Br2 123.4(2) C9 N1 Ni1 Br2 -58.13(13) C13 N1 Ni1 Br1 -88.6(2) C9 N1 Ni1 Br1 89.93(12)