#------------------------------------------------------------------------------ #$Date: 2020-06-03 01:48:12 +0300 (Wed, 03 Jun 2020) $ #$Revision: 252547 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/50/4135045.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_4135045 loop_ _publ_author_name 'McNeece, Andrew J.' 'Jesse, Kate' 'Xie, Jiaze' 'Filatov, Alexander S.' 'Anderson, John S.' _publ_section_title ; Generation and Oxidative Reactivity of a Ni(II) Superoxo Complex via Ligand-Based Redox Non-Innocence. ; _journal_name_full 'Journal of the American Chemical Society' _journal_paper_doi 10.1021/jacs.0c03244 _journal_year 2020 _chemical_formula_moiety 'C28 H34 N5 Ni' _chemical_formula_sum 'C28 H34 N5 Ni' _chemical_formula_weight 499.31 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_date 2019-07-02 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _cell_angle_alpha 90 _cell_angle_beta 93.198(4) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 51.354(6) _cell_length_b 5.7125(7) _cell_length_c 17.328(2) _cell_measurement_reflns_used 9963 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.07 _cell_measurement_theta_min 2.35 _cell_volume 5075.4(10) _computing_cell_refinement 'SAINT V.8.35A (Bruker AXS Inc., 2013)' _computing_data_collection 'APEX3 v.2015.9-0 (Bruker AXS Inc., 2015)' _computing_data_reduction 'SAINT V.8.35A (Bruker AXS Inc., 2013)' _computing_molecular_graphics ; OLEX2: a complete structure solution, refinement and analysis program Dolomanov et al., 2009 Mercury: visualization and analysis of crystal structures Macrae, et al., 2006 O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann. J. Appl. Cryst. (2009). 42, 339-341; C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor, M. Towler and J. van de Streek, J. Appl. Cryst. (2006). 39, 453-457. ; _computing_publication_material ; APEX3 v.2015.5-2 (Bruker AXS Inc., 2015) OLEX2 (Dolomanov et al., 2009) ; _computing_structure_refinement 'XL-2018/3 (Sheldrick, 2015b)' _computing_structure_solution 'XT 2014/5 (Sheldrick, 2015a)' _diffrn_ambient_temperature 100(2) _diffrn_detector 'Bruker PHOTON 100' _diffrn_detector_area_resol_mean 10.4167 _diffrn_detector_type CMOS _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method 'omega and phi scans' _diffrn_radiation_monochromator mirrors _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0850 _diffrn_reflns_av_unetI/netI 0.0449 _diffrn_reflns_Laue_measured_fraction_full 0.986 _diffrn_reflns_Laue_measured_fraction_max 0.986 _diffrn_reflns_limit_h_max 59 _diffrn_reflns_limit_h_min -60 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 40928 _diffrn_reflns_point_group_measured_fraction_full 0.986 _diffrn_reflns_point_group_measured_fraction_max 0.986 _diffrn_reflns_theta_full 25.164 _diffrn_reflns_theta_max 25.164 _diffrn_reflns_theta_min 2.354 _diffrn_source 'micro-focus X-ray tube' _diffrn_source_type 'INCOATEC ImuS' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.790 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_correction_T_min 0.5620 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1258 before and 0.0880 after correction. The Ratio of minimum to maximum transmission is 0.7542. ; _exptl_crystal_colour 'clear violet' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary violet _exptl_crystal_density_diffrn 1.307 _exptl_crystal_description plate _exptl_crystal_F_000 2120 _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _refine_diff_density_max 0.719 _refine_diff_density_min -0.761 _refine_diff_density_rms 0.090 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 407 _refine_ls_number_reflns 4486 _refine_ls_number_restraints 351 _refine_ls_restrained_S_all 1.059 _refine_ls_R_factor_all 0.0851 _refine_ls_R_factor_gt 0.0672 _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^)+(0.0624P)^2^+43.2597P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1602 _refine_ls_wR_factor_ref 0.1703 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3654 _reflns_number_total 4486 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja0c03244_si_002.cif _cod_data_source_block mo_0719_amtbu _cod_original_cell_volume 5075.5(10) _cod_database_code 4135045 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.877 _shelx_estimated_absorpt_t_min 0.764 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C22-C17 \\sim C22Y-C17 \\sim C22X-C17 with sigma of 0.01 C28Y-C25Y \\sim C28-C25 \\sim C28X-C25X with sigma of 0.01 C27-C22 \\sim C27X-C22X \\sim C27Y-C22Y with sigma of 0.01 C27-C26 \\sim C27X-C26X \\sim C27Y-C26Y with sigma of 0.01 C26-C25 \\sim C26X-C25X \\sim C26Y-C25Y with sigma of 0.01 C25X-C24X \\sim C25-C24 \\sim C25Y-C24Y with sigma of 0.01 C24X-C23X \\sim C24-C23 \\sim C24Y-C23Y with sigma of 0.01 C23X-C22X \\sim C23-C22 \\sim C23Y-C22Y with sigma of 0.01 C24-C28 \\sim C26-C28 with sigma of 0.01 C25X-C24X \\sim C26X-C25X with sigma of 0.01 C24X-C28X \\sim C26X-C28X with sigma of 0.01 C24Y-C28Y \\sim C26Y-C28Y with sigma of 0.01 3. Restrained planarity C22, C23, C24, C25, C26, C27 with sigma of 0.005 C22X, C23X, C24X, C25X, C26X, C27X with sigma of 0.005 C22Y, C23Y, C24Y, C25Y, C26Y, C27Y with sigma of 0.005 4. Uiso/Uaniso restraints and constraints C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C17: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 C25X \\sim C26X \\sim C27X \\sim C22X \\sim C23X \\sim C24X \\sim C28X \\sim C17: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 C27Y \\sim C22Y \\sim C23Y \\sim C24Y \\sim C25Y \\sim C26Y \\sim C28Y \\sim C17: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C25Y) = Uanis(C25X) = Uanis(C25) Uanis(C28X) = Uanis(C28Y) = Uanis(C28) Uanis(C22) = Uanis(C22X) = Uanis(C22Y) 5. Rigid body (RIGU) restrains C22, C23, C24, C25, C26, C27, C28, C17 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02 C25X, C26X, C27X, C22X, C23X, C24X, C28X, C17 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02 C27Y, C22Y, C23Y, C24Y, C25Y, C26Y, C28Y, C17 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02 6. Others Fixed Sof: C22(0.5) C23(0.5) H23(0.5) C24(0.5) H24(0.5) C25(0.5) C26(0.5) H26(0.5) C27(0.5) H27(0.5) C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5) C25X(0.25) C26X(0.25) H26X(0.25) C27X(0.25) H27X(0.25) C22X(0.25) C23X(0.25) H23X(0.25) C24X(0.25) H24X(0.25) C28X(0.25) H28D(0.25) H28E(0.25) H28F(0.25) C27Y(0.25) H27Y(0.25) C22Y(0.25) C23Y(0.25) H23Y(0.25) C24Y(0.25) H24Y(0.25) C25Y(0.25) C26Y(0.25) H26Y(0.25) C28Y(0.25) H28G(0.25) H28H(0.25) H28I(0.25) 7.a Aromatic/amide H refined with riding coordinates: C7(H7), C8(H8), C10(H10), C11(H11), C14(H14), C15(H15), C23(H23), C24(H24), C26(H26), C27(H27), C26X(H26X), C27X(H27X), C23X(H23X), C24X(H24X), C27Y(H27Y), C23Y(H23Y), C24Y(H24Y), C26Y(H26Y) 7.b Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C19(H19A, H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C28(H28A,H28B,H28C), C28X(H28D,H28E,H28F), C28Y(H28G,H28H,H28I) ; _shelx_res_file ; TITL mo_0719_amtbu_a.res in C2/c mo_0719_amtbu.res created by SHELXL-2018/3 at 17:18:50 on 02-Jul-2019 REM Old TITL mo_0719_AMtBu in C2/c REM SHELXT solution in C2/c: R1 0.170, Rweak 0.017, Alpha 0.090 REM 0.529 for 486 systematic absences, Orientation as input REM Formula found by SHELXT: C22 N6 Ni CELL 0.71073 51.354 5.7125 17.3283 90 93.198 90 ZERR 8 0.0061 0.0007 0.002 0 0.004 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H N Ni UNIT 224 272 40 8 EQIV $1 1.5-X,1.5-Y,1-Z SADI 0.01 C22 C17 C22Y C17 C22X C17 SADI 0.01 C28Y C25Y C28 C25 C28X C25X SADI 0.01 C27 C22 C27X C22X C27Y C22Y SADI 0.01 C27 C26 C27X C26X C27Y C26Y SADI 0.01 C26 C25 C26X C25X C26Y C25Y SADI 0.01 C25X C24X C25 C24 C25Y C24Y SADI 0.01 C24X C23X C24 C23 C24Y C23Y SADI 0.01 C23X C22X C23 C22 C23Y C22Y SADI 0.01 C24 C28 C26 C28 SADI 0.01 C25X C24X C26X C25X SADI 0.01 C24X C28X C26X C28X SADI 0.01 C24Y C28Y C26Y C28Y FLAT 0.005 C22 C23 C24 C25 C26 C27 FLAT 0.005 C22X C23X C24X C25X C26X C27X FLAT 0.005 C22Y C23Y C24Y C25Y C26Y C27Y SIMU 0.01 0.02 2 C22 C23 C24 C25 C26 C27 C28 C17 SIMU 0.01 0.02 2 C25X C26X C27X C22X C23X C24X C28X C17 SIMU 0.01 0.02 2 C27Y C22Y C23Y C24Y C25Y C26Y C28Y C17 RIGU 0.01 0.02 C22 C23 C24 C25 C26 C27 C28 C17 RIGU 0.01 0.02 C25X C26X C27X C22X C23X C24X C28X C17 RIGU 0.01 0.02 C27Y C22Y C23Y C24Y C25Y C26Y C28Y C17 EADP C25Y C25X C25 EADP C28X C28Y C28 EADP C22 C22X C22Y L.S. 12 PLAN 10 SIZE 0.17 0.21 0.36 TEMP -173(2) FREE C26Y C26Y_$1 BOND $H list 4 fmap 2 53 acta REM REM REM WGHT 0.062400 43.259701 FVAR 0.19858 NI1 4 0.615171 0.782888 0.379531 11.00000 0.03059 0.02321 = 0.02628 0.00190 0.00092 -0.00555 N1 3 0.581762 0.661969 0.370685 11.00000 0.03322 0.01826 = 0.01561 0.00318 0.00207 -0.00006 N2 3 0.571001 0.502713 0.412878 11.00000 0.03214 0.01527 = 0.02034 -0.00312 0.00239 0.00034 N3 3 0.625005 0.600595 0.466479 11.00000 0.02677 0.02797 = 0.02086 -0.00139 0.00022 -0.00023 N4 3 0.668119 0.897049 0.422169 11.00000 0.03383 0.04703 = 0.03074 -0.00876 0.00457 -0.01449 N5 3 0.647503 0.921376 0.375570 11.00000 0.03440 0.03732 = 0.02887 -0.00524 0.00566 -0.01159 C1 1 0.560982 1.005057 0.310716 11.00000 0.04988 0.02083 = 0.02956 -0.00411 -0.00496 0.00607 AFIX 137 H1A 2 0.552337 1.047522 0.357744 11.00000 -1.50000 H1B 2 0.550780 1.064614 0.265420 11.00000 -1.50000 H1C 2 0.578488 1.073809 0.312406 11.00000 -1.50000 AFIX 0 C2 1 0.574820 0.662549 0.231153 11.00000 0.04050 0.02307 = 0.02287 -0.00349 -0.00043 0.00184 AFIX 137 H2A 2 0.592475 0.726506 0.229082 11.00000 -1.50000 H2B 2 0.563992 0.719312 0.186681 11.00000 -1.50000 H2C 2 0.575581 0.491189 0.229802 11.00000 -1.50000 AFIX 0 C3 1 0.535922 0.637054 0.308657 11.00000 0.03437 0.03566 = 0.03070 0.00787 -0.00325 0.00431 AFIX 137 H3A 2 0.537007 0.466026 0.305789 11.00000 -1.50000 H3B 2 0.524823 0.695595 0.265020 11.00000 -1.50000 H3C 2 0.528427 0.682414 0.357248 11.00000 -1.50000 AFIX 0 C4 1 0.563054 0.741075 0.305426 11.00000 0.03194 0.01869 = 0.01824 0.00161 -0.00167 0.00432 C5 1 0.515440 -0.226457 0.632229 11.00000 0.03982 0.02672 = 0.02549 0.00149 -0.00104 -0.00694 AFIX 137 H5A 2 0.524310 -0.373909 0.645810 11.00000 -1.50000 H5B 2 0.499797 -0.258929 0.598959 11.00000 -1.50000 H5C 2 0.510436 -0.147857 0.679442 11.00000 -1.50000 AFIX 0 C6 1 0.533520 -0.070889 0.589972 11.00000 0.03643 0.02012 = 0.01594 -0.00177 -0.00307 -0.00616 C7 1 0.524491 0.141875 0.559427 11.00000 0.02514 0.02534 = 0.02251 -0.00482 -0.00076 -0.00298 AFIX 43 H7 2 0.506782 0.184913 0.564139 11.00000 -1.20000 AFIX 0 C8 1 0.540850 0.290389 0.522568 11.00000 0.02894 0.01846 = 0.02036 -0.00183 -0.00344 0.00068 AFIX 43 H8 2 0.534225 0.434608 0.502474 11.00000 -1.20000 AFIX 0 C9 1 0.567003 0.233562 0.514067 11.00000 0.03035 0.02053 = 0.01219 -0.00198 -0.00304 -0.00099 C10 1 0.575847 0.017844 0.542477 11.00000 0.03046 0.02342 = 0.01905 -0.00542 0.00225 0.00235 AFIX 43 H10 2 0.593330 -0.028780 0.535706 11.00000 -1.20000 AFIX 0 C11 1 0.559345 -0.129245 0.580532 11.00000 0.03754 0.01866 = 0.01721 -0.00179 0.00011 0.00006 AFIX 43 H11 2 0.565902 -0.273677 0.600648 11.00000 -1.20000 AFIX 0 C12 1 0.583784 0.400711 0.474216 11.00000 0.02737 0.01805 = 0.01644 -0.00189 -0.00055 0.00137 C13 1 0.609223 0.448083 0.502060 11.00000 0.02948 0.02445 = 0.01853 -0.00060 0.00453 -0.00046 C14 1 0.623238 0.366336 0.571797 11.00000 0.03473 0.06687 = 0.01940 0.01117 -0.00286 -0.00773 AFIX 43 H14 2 0.616901 0.259732 0.608418 11.00000 -1.20000 AFIX 0 C15 1 0.646680 0.468086 0.575229 11.00000 0.03499 0.10154 = 0.02198 0.01906 -0.00660 -0.01973 AFIX 43 H15 2 0.660098 0.444995 0.614480 11.00000 -1.20000 AFIX 0 C16 1 0.648064 0.619278 0.508872 11.00000 0.02872 0.05345 = 0.02538 -0.00503 -0.00133 -0.00755 C17 1 0.668266 0.760002 0.485705 11.00000 0.02965 0.06641 = 0.03326 -0.00739 0.00292 -0.01427 C18 1 0.653926 1.069767 0.307065 11.00000 0.04468 0.03303 = 0.04013 -0.00266 0.00920 -0.01042 C19 1 0.628606 1.185468 0.274450 11.00000 0.05230 0.04528 = 0.05389 0.01065 0.00757 -0.00629 AFIX 137 H19A 2 0.616049 1.064010 0.257725 11.00000 -1.50000 H19B 2 0.632414 1.284281 0.230242 11.00000 -1.50000 H19C 2 0.621221 1.281845 0.314598 11.00000 -1.50000 AFIX 0 C20 1 0.673279 1.261663 0.329944 11.00000 0.05814 0.03975 = 0.06495 -0.00109 0.00976 -0.02062 AFIX 137 H20A 2 0.666616 1.354007 0.372236 11.00000 -1.50000 H20B 2 0.675687 1.363642 0.285425 11.00000 -1.50000 H20C 2 0.690032 1.191272 0.346945 11.00000 -1.50000 AFIX 0 C21 1 0.664239 0.906785 0.247186 11.00000 0.07549 0.04178 = 0.04454 -0.00420 0.02114 -0.00663 AFIX 137 H21A 2 0.667800 0.995998 0.200632 11.00000 -1.50000 H21B 2 0.651227 0.785569 0.234115 11.00000 -1.50000 H21C 2 0.680376 0.833130 0.267993 11.00000 -1.50000 AFIX 0 PART 1 C22 1 0.692804 0.816925 0.534341 10.50000 0.03285 0.06728 = 0.03404 -0.00312 -0.00161 -0.01932 C23 1 0.704307 0.639974 0.574612 10.50000 0.05335 0.09078 = 0.07695 0.01795 -0.01703 -0.02752 AFIX 43 H23 2 0.696994 0.487229 0.572079 10.50000 -1.20000 AFIX 0 C24 1 0.727605 0.684067 0.621166 10.50000 0.07072 0.10862 = 0.08999 0.02826 -0.02745 -0.02582 AFIX 43 H24 2 0.735953 0.561038 0.649943 10.50000 -1.20000 AFIX 0 C25 1 0.737756 0.904958 0.623878 10.50000 0.04227 0.09872 = 0.06632 0.00887 -0.01407 -0.02285 C26 1 0.726214 1.086244 0.583181 10.50000 0.05267 0.08553 = 0.06561 0.00395 -0.00861 -0.02638 AFIX 43 H26 2 0.733599 1.238695 0.585914 10.50000 -1.20000 AFIX 0 C27 1 0.703637 1.044062 0.538025 10.50000 0.04181 0.06844 = 0.04587 0.00291 -0.00142 -0.01885 AFIX 43 H27 2 0.695409 1.168110 0.509451 10.50000 -1.20000 AFIX 0 C28 1 0.763934 0.945997 0.668254 10.50000 0.05136 0.14963 = 0.10903 0.02276 -0.03100 -0.03101 AFIX 137 H28A 2 0.761221 1.040240 0.714375 10.50000 -1.50000 H28B 2 0.775716 1.028986 0.635066 10.50000 -1.50000 H28C 2 0.771642 0.795066 0.683760 10.50000 -1.50000 AFIX 0 PART 0 PART 2 C25X 1 0.744414 0.723612 0.611542 10.25000 0.04227 0.09872 = 0.06632 0.00887 -0.01407 -0.02285 C26X 1 0.731510 0.919437 0.586041 10.25000 0.04625 0.08822 = 0.04861 -0.00024 -0.01622 -0.02602 AFIX 43 H26X 2 0.739484 1.066356 0.597513 10.25000 -1.20000 AFIX 0 C27X 1 0.707723 0.920875 0.544785 10.25000 0.03798 0.07320 = 0.03877 -0.00348 -0.00838 -0.02095 AFIX 43 H27X 2 0.699995 1.065647 0.529190 10.25000 -1.20000 AFIX 0 C22X 1 0.694804 0.709150 0.525606 10.25000 0.03285 0.06728 = 0.03404 -0.00312 -0.00161 -0.01932 C23X 1 0.706616 0.507311 0.549207 10.25000 0.03163 0.07464 = 0.02761 -0.02024 -0.00506 -0.00593 AFIX 43 H23X 2 0.698768 0.359788 0.537849 10.25000 -1.20000 AFIX 0 C24X 1 0.731205 0.522867 0.591647 10.25000 0.03238 0.08926 = 0.04099 -0.01235 -0.00597 -0.00517 AFIX 43 H24X 2 0.739169 0.379460 0.607635 10.25000 -1.20000 AFIX 0 C28X 1 0.769827 0.728106 0.661289 10.25000 0.05136 0.14963 = 0.10903 0.02276 -0.03100 -0.03101 AFIX 137 H28D 2 0.779436 0.871796 0.650787 10.25000 -1.50000 H28E 2 0.780436 0.591852 0.649067 10.25000 -1.50000 H28F 2 0.765955 0.723560 0.716010 10.25000 -1.50000 AFIX 0 PART 0 PART 3 C27Y 1 0.717644 0.776067 0.500768 10.25000 0.02617 0.06136 = 0.03540 -0.00327 0.00182 -0.01173 AFIX 43 H27Y 2 0.717498 0.783810 0.445981 10.25000 -1.20000 AFIX 0 C22Y 1 0.693558 0.750888 0.535837 10.25000 0.03285 0.06728 = 0.03404 -0.00312 -0.00161 -0.01932 C23Y 1 0.695940 0.741557 0.614217 10.25000 0.03071 0.06185 = 0.03567 0.00106 -0.00929 -0.01427 AFIX 43 H23Y 2 0.680587 0.724745 0.641862 10.25000 -1.20000 AFIX 0 C24Y 1 0.720424 0.755838 0.656878 10.25000 0.03141 0.06701 = 0.03969 -0.00089 -0.01243 -0.01126 AFIX 43 H24Y 2 0.720856 0.748349 0.711702 10.25000 -1.20000 AFIX 0 C25Y 1 0.743286 0.780013 0.621002 10.25000 0.04227 0.09872 = 0.06632 0.00887 -0.01407 -0.02285 C26Y 1 0.741366 0.789944 0.542316 10.25000 0.02985 0.07572 = 0.04616 0.00162 -0.00221 -0.01368 AFIX 43 H26Y 2 0.756821 0.806942 0.515154 10.25000 -1.20000 AFIX 0 C28Y 1 0.769646 0.772044 0.665918 10.25000 0.05136 0.14963 = 0.10903 0.02276 -0.03100 -0.03101 AFIX 137 H28G 2 0.768275 0.849305 0.716023 10.25000 -1.50000 H28H 2 0.782684 0.853023 0.636491 10.25000 -1.50000 H28I 2 0.774929 0.608680 0.674122 10.25000 -1.50000 AFIX 0 HKLF 4 REM mo_0719_amtbu_a.res in C2/c REM wR2 = 0.1703, GooF = S = 1.078, Restrained GooF = 1.059 for all data REM R1 = 0.0672 for 3654 Fo > 4sig(Fo) and 0.0851 for all 4486 data REM 407 parameters refined using 351 restraints END WGHT 0.0623 43.2706 REM Highest difference peak 0.719, deepest hole -0.761, 1-sigma level 0.090 Q1 1 0.6423 0.7786 0.3809 11.00000 0.05 0.72 Q2 1 0.7407 0.8137 0.6005 11.00000 0.05 0.62 Q3 1 0.5967 0.7452 0.3779 11.00000 0.05 0.58 Q4 1 0.6184 0.6518 0.4197 11.00000 0.05 0.51 Q5 1 0.6220 0.8862 0.4260 11.00000 0.05 0.38 Q6 1 0.6216 0.8339 0.4341 11.00000 0.05 0.38 Q7 1 0.5601 0.6837 0.3812 11.00000 0.05 0.36 Q8 1 0.7646 1.0159 0.6988 11.00000 0.05 0.35 Q9 1 0.5785 0.5917 0.3961 11.00000 0.05 0.34 Q10 1 0.6761 0.7729 0.5024 11.00000 0.05 0.33 ; _shelx_res_checksum 58069 _shelx_hkl_file ; 6 0 0 732.83 49.60 -6 0 0 743.83 49.60 6 0 0 759.32 49.80 -8 0 0 2.40 1.10 -8 0 0 3.80 1.50 8 0 0 4.00 1.60 8 0 0 3.80 1.20 8 0 0 3.40 1.40 -8 0 0 4.50 1.60 -10 0 0 1368.86 97.69 10 0 0 1431.16 97.69 10 0 0 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97.59 19.60 -44 2 0 104.89 16.30 44 2 0 99.09 15.20 44 2 0 107.89 16.40 44 2 0 118.89 14.90 -44 2 0 110.69 13.20 44 2 0 117.89 17.90 46 -2 0 33.80 8.70 -46 -2 0 25.70 12.90 46 -2 0 32.60 9.10 -46 -2 0 35.10 9.00 46 2 0 40.10 12.00 46 2 0 7.20 12.40 46 2 0 26.60 9.80 -46 2 0 35.70 9.00 -46 2 0 27.40 9.00 46 2 0 44.90 12.80 -46 2 0 42.70 14.70 48 -2 0 87.69 16.70 48 -2 0 87.89 11.90 -48 -2 0 94.89 13.00 -48 -2 0 88.99 17.00 -48 2 0 57.99 12.50 48 2 0 58.79 11.90 48 2 0 90.89 14.30 -48 2 0 86.29 12.40 48 2 0 82.59 14.70 -50 -2 0 25.70 14.70 -50 -2 0 25.90 9.90 50 -2 0 17.50 9.60 50 2 0 20.80 9.10 50 2 0 6.60 12.10 -50 2 0 15.90 10.10 -52 -2 0 146.49 27.60 52 -2 0 113.49 19.70 -52 -2 0 154.98 20.00 -52 2 0 165.48 20.30 -52 2 0 116.99 19.60 -52 2 0 165.08 24.90 52 2 0 111.99 18.20 52 2 0 137.69 18.10 54 -2 0 6.60 11.10 -54 -2 0 20.40 10.40 -54 -2 0 31.90 16.40 -54 2 0 2.30 11.80 -54 2 0 1.30 11.00 54 2 0 11.40 10.70 54 2 0 8.80 14.80 -54 2 0 7.90 12.60 -56 -2 0 160.28 22.30 56 -2 0 111.29 17.60 -56 -2 0 132.29 22.00 -56 2 0 156.18 28.70 -56 2 0 147.89 22.60 -56 2 0 96.39 19.40 56 2 0 146.99 21.10 -58 -2 0 26.30 18.10 -58 -2 0 10.20 12.10 58 2 0 -5.90 14.00 -58 2 0 12.10 13.30 -58 2 0 13.20 14.50 1 -3 0 4.20 4.70 -1 -3 0 7.60 4.60 -1 3 0 5.20 4.60 1 3 0 8.70 4.90 1 3 0 1.30 4.00 -1 3 0 5.10 4.00 -1 3 0 9.30 4.20 -1 3 0 -2.50 5.30 -1 3 0 2.50 3.90 -1 3 0 9.00 5.00 1 3 0 6.50 5.20 1 3 0 8.00 5.20 -1 3 0 3.90 4.80 1 3 0 12.00 4.50 1 3 0 4.40 4.10 -3 -3 0 97.19 11.40 -3 -3 0 87.39 9.80 3 -3 0 108.19 10.80 3 3 0 83.79 9.30 -3 3 0 111.99 10.00 3 3 0 91.09 11.00 -3 3 0 106.49 10.50 -3 3 0 122.19 12.50 3 3 0 78.19 10.90 3 3 0 78.49 10.80 -3 3 0 114.49 10.70 -5 -3 0 16.30 5.40 -5 -3 0 21.60 4.70 5 3 0 20.40 5.80 5 3 0 14.30 4.80 5 3 0 29.10 4.70 5 3 0 21.00 5.10 5 3 0 29.00 5.90 -5 3 0 10.90 5.80 7 -3 0 272.97 21.60 -7 -3 0 296.67 21.50 -7 -3 0 261.07 20.70 7 3 0 287.07 20.60 7 3 0 319.17 21.10 -7 3 0 253.37 20.40 7 3 0 292.77 21.50 -7 3 0 250.57 21.40 -7 3 0 252.07 20.30 -7 3 0 271.87 20.70 -7 3 0 236.48 20.70 -7 3 0 260.27 21.80 -7 3 0 249.28 22.80 7 3 0 302.27 21.40 -9 -3 0 453.45 30.60 -9 -3 0 382.26 29.90 9 -3 0 439.46 31.00 -9 3 0 415.36 29.40 -9 3 0 377.36 30.70 -9 3 0 421.86 31.00 -9 3 0 401.56 29.70 -9 3 0 404.56 29.90 9 3 0 419.16 30.00 9 3 0 449.46 30.60 9 3 0 424.36 30.40 9 3 0 447.06 30.70 -9 3 0 384.46 29.90 -9 3 0 406.76 30.70 -11 -3 0 10.60 5.30 11 -3 0 0.20 3.30 11 -3 0 -0.50 5.10 -11 -3 0 8.30 4.20 11 3 0 9.30 5.10 -11 3 0 -1.40 4.90 -11 3 0 -1.70 3.90 -11 3 0 -4.20 3.30 -11 3 0 -3.90 4.50 11 3 0 -5.80 5.20 -11 3 0 -1.40 4.90 11 3 0 8.70 4.20 -11 3 0 -1.30 4.50 -11 3 0 0.20 3.10 11 3 0 4.00 5.60 13 -3 0 246.38 21.50 -13 -3 0 260.47 20.50 -13 -3 0 299.07 21.30 13 -3 0 265.37 20.20 -13 3 0 239.08 21.20 -13 3 0 257.77 20.20 -13 3 0 247.68 21.10 13 3 0 281.67 20.60 13 3 0 274.67 21.10 -13 3 0 262.57 21.30 13 3 0 271.57 21.20 -15 -3 0 7.40 3.80 -15 -3 0 3.10 5.40 15 -3 0 3.60 4.00 -15 -3 0 1.10 5.30 15 -3 0 1.20 5.40 -15 3 0 5.40 4.50 -15 3 0 1.90 3.80 15 3 0 5.90 5.40 15 3 0 1.90 5.20 -15 3 0 7.80 3.90 -15 3 0 12.50 4.70 15 3 0 10.40 4.50 -17 -3 0 460.15 35.10 -17 -3 0 529.35 35.00 17 -3 0 467.95 35.70 -17 -3 0 470.65 34.60 17 -3 0 471.95 34.40 -17 3 0 486.15 34.80 -17 3 0 466.25 35.30 17 3 0 479.95 34.60 -17 3 0 478.95 35.00 17 3 0 475.85 34.80 -17 3 0 489.05 34.00 -19 -3 0 110.59 11.30 -19 -3 0 88.39 12.40 -19 -3 0 114.09 12.60 19 -3 0 109.49 13.60 19 -3 0 100.39 12.30 19 -3 0 75.19 14.30 19 3 0 109.39 14.20 -19 3 0 105.69 12.30 -19 3 0 123.99 12.20 19 3 0 101.09 12.30 19 3 0 94.09 11.50 -19 3 0 119.99 10.70 -19 3 0 121.69 11.60 -21 -3 0 117.99 11.90 -21 -3 0 127.09 13.50 -21 -3 0 92.79 12.30 21 -3 0 100.69 14.10 21 -3 0 119.99 12.70 21 -3 0 104.09 12.40 21 3 0 107.09 13.00 -21 3 0 132.29 13.30 21 3 0 125.29 15.10 21 3 0 124.49 12.20 -21 3 0 127.29 11.20 -21 3 0 118.59 13.00 23 -3 0 343.57 24.40 23 -3 0 311.17 25.10 -23 -3 0 337.47 25.80 23 -3 0 321.27 26.20 -23 -3 0 348.37 25.00 -23 -3 0 269.47 24.50 -23 3 0 312.57 25.50 23 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0.00 8.80 33 -3 0 1.10 5.90 -33 -3 0 1.50 5.60 33 3 0 -2.30 8.80 -33 3 0 1.50 5.90 33 3 0 -4.80 7.50 -33 3 0 4.20 5.30 33 3 0 16.30 5.60 35 -3 0 32.30 8.80 35 -3 0 27.10 8.70 -35 -3 0 38.40 7.70 -35 -3 0 34.80 10.60 35 -3 0 40.50 8.10 -35 3 0 33.10 8.70 35 3 0 26.00 9.90 35 3 0 27.50 9.70 -35 3 0 32.00 6.90 35 3 0 27.50 7.50 35 3 0 34.50 9.00 37 -3 0 5.50 7.50 -37 -3 0 19.50 6.70 37 -3 0 23.40 7.30 -37 -3 0 32.30 10.60 37 3 0 8.40 9.30 -37 3 0 18.90 6.60 37 3 0 12.70 8.20 37 3 0 14.70 10.00 -37 3 0 20.00 7.80 37 3 0 13.80 7.00 -39 -3 0 115.19 15.20 -39 -3 0 158.88 20.70 39 -3 0 148.09 18.20 39 -3 0 152.68 16.60 39 3 0 145.49 19.40 39 3 0 111.89 16.70 39 3 0 130.29 18.70 -39 3 0 152.38 14.60 -39 3 0 125.99 16.90 41 -3 0 -5.10 7.40 -41 -3 0 -8.20 6.00 41 -3 0 4.80 7.60 41 3 0 -0.70 8.30 -41 3 0 -3.60 6.60 41 3 0 -11.80 7.80 -41 3 0 -4.30 7.00 41 3 0 -8.70 10.80 43 -3 0 158.48 19.30 -43 -3 0 133.59 16.90 -43 -3 0 176.98 22.90 43 -3 0 185.18 19.70 -43 3 0 137.09 18.30 43 3 0 106.39 19.10 43 3 0 163.38 19.00 -43 3 0 156.78 16.80 -45 -3 0 125.79 22.30 45 -3 0 117.59 17.60 -45 -3 0 105.19 15.80 45 -3 0 98.69 13.90 45 3 0 77.69 14.00 -45 3 0 95.99 16.60 45 3 0 105.49 18.10 -45 3 0 94.49 12.90 47 -3 0 1.00 10.00 -47 -3 0 26.10 14.00 -47 -3 0 15.00 8.50 47 3 0 -6.20 10.80 47 3 0 15.10 11.30 -47 3 0 0.80 9.20 -47 3 0 20.70 12.30 -49 -3 0 139.29 24.70 -49 -3 0 103.19 17.60 49 -3 0 123.19 16.30 -49 3 0 106.39 15.00 49 3 0 91.99 14.90 -49 3 0 90.49 15.10 -49 3 0 117.99 24.70 -51 -3 0 15.50 15.70 51 -3 0 5.10 12.50 -51 -3 0 7.10 9.50 -51 3 0 9.70 13.70 -51 3 0 -20.00 11.10 -51 3 0 -6.90 10.50 51 3 0 -12.80 11.00 -53 -3 0 41.00 17.50 -53 -3 0 32.60 11.70 53 -3 0 22.40 15.90 -53 3 0 14.00 11.50 -53 3 0 28.60 12.80 -53 3 0 19.10 16.10 53 3 0 17.70 12.30 0 -4 0 267.27 22.10 0 4 0 257.37 21.70 0 4 0 269.97 22.00 0 4 0 288.87 22.40 0 4 0 257.27 21.70 0 4 0 256.77 21.70 0 4 0 271.27 21.30 0 4 0 270.37 23.40 -2 -4 0 16.80 6.70 -2 4 0 7.70 4.80 2 4 0 15.50 9.40 -2 4 0 14.50 5.60 2 4 0 15.40 4.90 2 4 0 19.60 6.90 2 4 0 16.70 5.80 2 4 0 17.00 5.70 -2 4 0 10.40 6.60 2 4 0 16.30 6.20 -2 4 0 14.90 6.60 -2 4 0 14.70 6.40 -2 4 0 20.90 6.20 2 4 0 18.00 6.50 -4 -4 0 62.79 11.80 4 4 0 82.49 10.60 -4 4 0 43.70 8.10 -4 4 0 58.69 9.00 -4 4 0 58.89 9.40 4 4 0 78.89 9.70 -4 4 0 48.90 9.70 -4 4 0 80.49 11.50 4 4 0 74.69 11.10 -4 4 0 69.29 11.80 4 4 0 69.69 11.50 -4 4 0 57.09 9.10 4 4 0 78.09 11.80 -4 4 0 49.99 10.00 -6 -4 0 161.18 15.50 -6 -4 0 184.78 17.10 6 4 0 155.38 15.90 -6 4 0 172.68 16.30 6 4 0 151.68 15.90 6 4 0 155.98 17.10 -6 4 0 166.18 16.30 -6 4 0 197.88 16.60 6 4 0 181.58 15.80 6 4 0 170.58 17.00 -6 4 0 193.38 16.50 6 4 0 153.78 16.50 -6 4 0 147.49 15.90 -6 4 0 174.98 15.10 -6 4 0 155.88 17.60 -6 4 0 191.98 19.40 6 4 0 162.48 16.70 -8 -4 0 -0.40 4.80 -8 -4 0 8.40 6.20 -8 4 0 -5.20 4.20 -8 4 0 5.30 6.50 -8 4 0 3.90 6.40 -8 4 0 1.10 5.50 -8 4 0 4.80 5.40 -8 4 0 6.90 4.90 8 4 0 9.00 7.10 8 4 0 -0.50 7.00 8 4 0 6.20 6.60 8 4 0 6.40 4.60 -8 4 0 8.70 6.40 -10 -4 0 67.99 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315.17 28.10 -18 4 0 318.77 25.30 -18 4 0 324.77 25.40 18 4 0 311.47 32.20 18 4 0 318.57 26.60 -18 4 0 325.27 27.00 18 4 0 331.77 25.30 -18 4 0 309.37 26.30 -20 -4 0 33.60 8.10 20 -4 0 27.40 8.30 20 -4 0 28.40 6.90 -20 -4 0 17.60 7.90 20 4 0 25.10 10.40 20 4 0 16.40 7.90 -20 4 0 10.80 6.30 20 4 0 22.70 8.70 -20 4 0 23.40 7.30 -20 4 0 26.20 6.80 20 4 0 23.70 6.10 22 -4 0 273.97 22.60 22 -4 0 270.67 25.10 -22 -4 0 275.67 23.90 -22 -4 0 279.37 22.70 22 4 0 251.17 24.20 22 4 0 218.48 23.00 -22 4 0 286.87 21.90 22 4 0 263.27 26.50 -22 4 0 261.57 25.30 -22 4 0 248.18 23.60 22 4 0 276.77 22.60 -22 4 0 296.97 23.70 24 -4 0 71.79 14.00 -24 -4 0 64.99 9.60 24 -4 0 61.09 9.20 -24 -4 0 56.99 11.20 -24 4 0 55.79 8.60 24 4 0 46.10 10.80 -24 4 0 56.59 10.00 24 4 0 53.39 11.10 -24 4 0 52.69 10.80 24 4 0 46.70 8.40 24 4 0 60.99 13.60 26 -4 0 52.09 10.30 -26 -4 0 48.20 10.10 -26 -4 0 59.59 9.30 26 -4 0 49.80 9.30 -26 4 0 34.40 8.90 26 4 0 44.50 10.20 -26 4 0 45.70 9.30 26 4 0 39.40 13.70 26 4 0 39.20 8.50 -26 4 0 57.59 8.60 26 4 0 59.39 11.40 28 -4 0 71.39 10.40 -28 -4 0 96.09 16.40 28 -4 0 74.09 15.00 -28 -4 0 75.29 12.20 28 4 0 79.29 12.60 -28 4 0 69.29 11.70 28 4 0 80.49 13.00 28 4 0 69.29 15.40 -28 4 0 97.49 14.90 -28 4 0 85.09 14.00 -30 -4 0 15.80 9.00 -30 -4 0 9.30 5.90 30 -4 0 14.10 8.30 30 -4 0 16.20 7.40 30 4 0 -6.60 8.50 -30 4 0 9.10 7.00 30 4 0 9.20 12.20 -30 4 0 10.30 7.80 -32 -4 0 46.40 9.20 32 -4 0 32.10 8.40 -32 -4 0 47.90 10.80 32 -4 0 34.10 9.50 -32 4 0 14.80 8.00 32 4 0 15.80 13.20 -32 4 0 36.20 8.50 32 4 0 19.90 10.00 -34 -4 0 3.10 8.80 34 -4 0 1.70 7.50 34 -4 0 2.50 8.00 -34 -4 0 13.10 6.80 -34 4 0 -8.60 7.10 -34 4 0 10.40 7.40 34 4 0 -6.50 12.10 34 4 0 -7.40 8.00 -36 -4 0 1.10 6.70 36 -4 0 5.80 8.30 -36 -4 0 16.50 20.00 -36 4 0 -1.60 7.90 36 4 0 -8.10 11.70 36 4 0 -6.10 8.40 -36 4 0 -1.50 7.10 -38 -4 0 205.18 19.40 -38 -4 0 190.38 22.80 38 -4 0 191.28 20.20 -38 4 0 160.28 19.60 38 4 0 154.28 19.80 -38 4 0 159.28 17.70 -38 4 0 199.18 25.20 38 4 0 120.29 19.50 -40 -4 0 111.29 15.80 -40 -4 0 86.29 15.50 40 -4 0 73.99 12.70 -40 4 0 84.29 15.80 40 4 0 46.90 15.30 -40 4 0 82.49 13.40 -40 4 0 67.49 11.30 40 4 0 60.09 13.40 42 -4 0 50.09 11.50 -42 -4 0 57.49 14.70 -42 -4 0 58.89 10.60 42 4 0 58.79 13.00 -42 4 0 39.30 12.30 -42 4 0 45.40 14.50 42 4 0 34.30 14.40 -44 -4 0 188.68 19.80 44 -4 0 155.28 22.60 -44 -4 0 157.18 21.40 44 4 0 139.19 21.10 -44 4 0 131.99 18.60 -44 4 0 146.69 28.70 -44 4 0 122.19 20.80 -46 -4 0 -4.50 15.00 46 -4 0 2.70 12.50 -46 -4 0 10.90 9.20 -46 4 0 9.00 8.90 -46 4 0 -3.10 10.50 -46 4 0 -8.30 14.90 46 4 0 3.50 12.60 -48 -4 0 116.69 19.90 -48 -4 0 138.19 23.10 48 4 0 135.49 24.50 -48 4 0 122.19 16.80 -48 4 0 131.89 22.10 -48 4 0 184.08 30.40 -1 5 0 106.79 16.70 1 5 0 94.79 16.00 1 5 0 78.99 14.20 -1 5 0 84.69 13.50 1 5 0 90.59 13.60 -1 5 0 109.69 18.30 -1 5 0 85.69 14.20 -1 5 0 69.19 12.80 -1 5 0 77.69 14.60 1 5 0 119.49 18.00 1 5 0 80.99 13.50 1 5 0 80.19 14.40 -1 5 0 108.59 18.00 -1 5 0 96.89 18.20 1 5 0 87.99 17.50 -3 -5 0 87.09 15.60 -3 5 0 44.70 9.60 3 5 0 62.39 12.60 3 5 0 78.39 15.60 -3 5 0 51.89 11.20 -3 5 0 61.99 13.10 -3 5 0 51.19 12.70 -3 5 0 86.19 16.50 -3 5 0 48.60 10.60 -3 5 0 45.60 11.20 -3 5 0 51.79 12.20 -5 -5 0 275.97 26.30 -5 5 0 251.57 26.30 5 5 0 277.17 27.90 5 5 0 267.97 26.70 -5 5 0 296.57 29.20 -5 5 0 316.07 25.40 5 5 0 340.57 26.00 -5 5 0 257.87 33.90 5 5 0 292.07 24.90 -5 5 0 309.37 29.10 -5 5 0 300.87 27.00 5 5 0 317.87 26.40 5 5 0 350.56 27.80 -5 5 0 288.57 26.00 5 5 0 273.57 26.50 -7 -5 0 100.79 16.80 -7 5 0 114.79 16.50 -7 5 0 88.29 19.20 7 5 0 77.39 17.20 -7 5 0 110.79 18.20 7 5 0 122.09 19.60 -7 5 0 86.19 17.00 -9 -5 0 470.85 37.20 -9 5 0 492.05 36.40 -9 5 0 435.16 38.50 9 5 0 460.45 36.90 -9 5 0 483.55 36.90 -9 5 0 499.15 38.00 9 5 0 483.25 37.30 -9 5 0 439.36 37.40 9 5 0 425.06 38.30 -9 5 0 512.25 40.40 -9 5 0 484.25 37.80 9 5 0 502.85 37.00 9 5 0 490.45 37.50 -11 -5 0 10.70 8.40 -11 5 0 -0.80 7.20 11 5 0 11.30 7.00 -11 5 0 33.70 10.20 11 5 0 16.70 10.50 11 5 0 16.30 8.40 -11 5 0 28.30 10.40 -11 5 0 26.10 8.80 11 5 0 3.40 6.90 -11 5 0 21.30 8.20 -13 -5 0 258.37 23.90 -13 -5 0 224.18 21.00 -13 5 0 253.57 24.80 13 5 0 186.08 22.60 -13 5 0 225.78 24.10 -13 5 0 213.98 22.20 13 5 0 228.18 21.70 -13 5 0 229.38 21.30 13 5 0 251.47 21.70 13 5 0 212.78 23.90 -13 5 0 211.98 26.50 -13 5 0 168.98 23.10 13 5 0 222.48 25.30 -13 5 0 231.78 23.10 -13 5 0 240.88 23.00 -15 -5 0 28.50 10.30 -15 -5 0 26.80 7.90 -15 5 0 34.00 11.70 -15 5 0 23.70 9.00 -15 5 0 18.50 9.90 -15 5 0 19.40 9.10 15 5 0 17.70 9.40 15 5 0 35.90 12.70 -15 5 0 24.40 9.40 -15 5 0 7.40 7.80 -15 5 0 19.50 10.90 -17 -5 0 193.78 22.00 -17 -5 0 226.18 19.80 17 5 0 143.59 21.30 -17 5 0 197.88 22.00 -17 5 0 210.78 20.40 -17 5 0 178.78 20.30 -17 5 0 192.78 22.00 17 5 0 183.78 24.30 -17 5 0 188.28 21.80 -17 5 0 175.18 22.70 -17 5 0 209.28 26.40 -19 -5 0 4.60 9.40 -19 -5 0 9.80 6.40 -19 5 0 3.40 10.30 -19 5 0 -5.50 6.60 -19 5 0 -2.50 7.70 19 5 0 17.50 12.00 19 5 0 -7.10 8.80 -21 -5 0 128.19 15.30 -21 -5 0 121.69 19.10 -21 5 0 95.49 16.70 -21 5 0 107.29 13.90 -21 5 0 105.99 16.60 21 5 0 96.49 17.30 21 5 0 100.69 15.40 -23 -5 0 26.80 7.90 -23 -5 0 24.20 11.00 23 5 0 14.70 9.60 -23 5 0 24.70 9.40 -23 5 0 16.60 15.50 -23 5 0 27.70 9.50 -23 5 0 41.00 12.60 23 5 0 29.00 14.80 -25 -5 0 43.50 9.00 -25 5 0 40.80 10.20 25 5 0 35.60 16.00 25 5 0 26.60 11.00 -25 5 0 54.59 11.20 -25 5 0 48.30 11.20 -25 5 0 52.19 13.50 -27 -5 0 16.40 7.00 -27 -5 0 39.00 12.00 27 5 0 10.10 16.50 -27 5 0 14.50 9.70 -27 5 0 22.60 8.80 -27 5 0 18.50 10.00 27 5 0 6.00 10.00 -27 5 0 36.30 12.40 -29 -5 0 111.19 16.30 -29 -5 0 160.68 22.20 -29 5 0 148.19 19.70 29 5 0 102.49 15.70 -29 5 0 105.49 14.90 -29 5 0 125.09 25.20 -29 5 0 99.79 16.80 29 5 0 86.09 20.90 -31 -5 0 115.99 16.90 -31 -5 0 89.79 14.10 -31 5 0 140.99 26.20 31 5 0 97.39 15.40 -31 5 0 88.89 13.90 -31 5 0 116.59 20.00 31 5 0 71.49 20.90 -31 5 0 92.39 13.30 -33 -5 0 22.60 13.30 -33 -5 0 35.40 9.60 33 -5 0 22.50 11.50 -33 5 0 51.49 12.40 33 5 0 18.00 22.20 -33 5 0 40.50 10.60 33 5 0 22.50 11.50 -33 5 0 40.60 11.90 -33 5 0 52.19 14.40 35 -5 0 52.59 13.10 -35 -5 0 47.00 14.00 -35 -5 0 46.70 10.40 -35 5 0 46.50 11.90 35 5 0 28.50 20.70 -35 5 0 65.39 15.70 35 5 0 26.50 13.00 -35 5 0 30.10 11.40 -37 -5 0 16.70 9.10 37 -5 0 -3.20 12.60 -37 -5 0 -13.00 13.10 -37 5 0 19.40 13.50 -37 5 0 0.60 10.30 -37 5 0 1.70 11.50 -39 -5 0 45.00 16.90 39 -5 0 54.59 15.20 -39 -5 0 32.40 11.00 -39 5 0 56.59 13.50 39 5 0 33.40 13.50 -39 5 0 66.49 16.30 -39 5 0 40.80 12.60 -41 -5 0 12.30 16.30 -41 -5 0 33.00 13.50 41 5 0 22.90 13.20 -41 5 0 31.00 22.20 -41 5 0 17.10 12.40 -41 5 0 14.90 11.50 0 6 0 50.49 14.80 0 6 0 60.89 14.40 0 6 0 57.39 14.90 0 6 0 55.69 11.70 0 6 0 67.99 17.20 -2 6 0 18.70 12.10 -2 6 0 31.80 15.10 2 6 0 20.10 11.90 2 6 0 3.50 12.00 2 6 0 33.00 12.80 -2 6 0 20.30 10.00 -2 6 0 18.50 12.60 -2 6 0 21.80 12.10 2 6 0 34.30 10.30 2 6 0 43.60 16.60 -4 6 0 30.40 9.90 4 6 0 42.00 10.70 -4 6 0 22.50 13.50 4 6 0 49.80 14.50 4 6 0 35.60 15.00 -4 6 0 43.20 13.90 4 6 0 60.19 17.30 4 6 0 48.80 13.20 -4 6 0 19.80 12.90 -4 6 0 62.89 16.70 6 6 0 61.69 15.00 6 6 0 75.89 17.30 6 6 0 65.49 12.80 -6 6 0 51.09 14.00 -6 6 0 85.59 17.80 -6 6 0 47.10 12.70 6 6 0 73.19 15.60 -6 6 0 56.89 13.80 -6 6 0 78.99 15.20 -6 6 0 42.90 18.70 6 6 0 61.39 14.90 -8 -6 0 44.20 13.20 -8 6 0 47.00 13.20 8 6 0 53.09 14.20 -8 6 0 37.20 15.60 -8 6 0 43.10 10.70 8 6 0 52.39 11.50 8 6 0 48.70 25.30 -8 6 0 68.79 18.00 8 6 0 69.39 17.30 -8 6 0 41.40 13.70 -8 6 0 48.90 13.70 -10 -6 0 8.30 10.80 -10 6 0 11.20 11.70 10 6 0 15.40 12.30 10 6 0 19.20 9.90 -10 6 0 -11.80 15.40 -10 6 0 -4.30 11.80 -10 6 0 -5.10 8.90 -10 6 0 -0.80 10.30 10 6 0 19.50 18.30 -12 -6 0 25.40 11.80 -12 6 0 10.50 16.90 -12 6 0 26.80 11.50 12 6 0 13.50 12.30 12 6 0 24.50 25.20 -12 6 0 5.40 12.60 -12 6 0 18.90 12.60 -12 6 0 12.00 9.80 12 6 0 21.20 10.20 -14 -6 0 36.80 12.20 -14 6 0 39.20 13.50 -14 6 0 6.80 10.60 14 6 0 31.40 12.80 -14 6 0 32.60 17.60 -14 6 0 41.80 13.70 14 6 0 41.80 10.80 -14 6 0 20.90 13.10 -16 -6 0 11.30 11.50 16 6 0 2.50 9.20 16 6 0 -8.90 11.90 -16 6 0 -1.20 11.70 -16 6 0 -12.10 17.40 -16 6 0 0.80 11.10 -16 6 0 8.10 9.70 -18 -6 0 55.59 14.50 -18 6 0 49.10 15.10 -18 6 0 71.19 12.70 18 6 0 32.40 14.50 -18 6 0 54.89 16.60 18 6 0 58.89 12.60 -18 6 0 39.40 13.80 -18 6 0 57.29 18.10 -20 -6 0 12.40 12.40 -20 6 0 3.60 10.40 20 6 0 -11.00 9.00 -20 6 0 -4.40 13.30 -20 6 0 -2.90 11.10 -22 -6 0 31.50 13.70 -22 -6 0 -2.50 10.00 -22 6 0 2.00 11.30 -22 6 0 -2.10 11.20 22 6 0 8.70 9.70 -22 6 0 6.80 14.40 22 6 0 -15.40 11.90 -24 -6 0 -7.30 13.30 -24 -6 0 -4.40 9.90 -24 6 0 7.40 11.40 -24 6 0 0.40 13.30 -24 6 0 -12.50 14.00 24 6 0 -3.40 12.20 -26 -6 0 29.80 11.60 -26 -6 0 -2.40 13.60 -26 6 0 -11.60 14.50 -26 6 0 -14.80 11.10 26 6 0 -10.10 12.20 -26 6 0 3.50 13.90 -28 -6 0 16.00 15.00 -28 -6 0 29.30 11.60 -28 6 0 3.00 11.90 -28 6 0 -2.90 15.70 -28 6 0 3.20 12.60 -60 0 1 -2.90 12.30 -60 0 1 -14.90 11.80 -58 0 1 -5.90 10.30 -58 0 1 27.10 16.00 -58 0 1 12.00 11.00 -56 0 1 6.80 9.60 -56 0 1 9.60 14.40 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140.39 14.70 -4 4 -2 157.98 15.80 6 -4 2 148.29 15.00 -6 -4 -2 131.19 13.10 -6 -4 -2 126.89 14.20 6 4 2 110.09 14.10 -6 4 -2 144.89 14.90 -6 4 -2 116.79 14.30 -6 4 -2 154.58 15.30 6 4 2 122.49 15.00 -6 4 -2 117.59 15.80 -6 4 -2 109.59 14.50 6 4 2 120.39 15.30 -6 4 -2 117.89 13.60 6 4 2 153.68 15.10 6 4 2 153.58 17.20 -6 4 -2 144.79 16.80 6 4 2 145.09 13.40 -8 -4 -2 140.49 14.90 8 -4 2 147.99 15.60 -8 -4 -2 134.39 13.60 -8 4 -2 106.69 14.70 8 4 2 173.58 15.50 -8 4 -2 145.99 13.90 8 4 2 114.49 14.50 8 4 2 150.38 13.90 -8 4 -2 136.79 16.90 8 4 2 135.39 15.50 8 4 2 113.79 16.10 -8 4 -2 130.89 14.50 -8 4 -2 136.69 15.30 -8 4 -2 138.59 16.80 8 4 2 150.08 17.30 -8 4 -2 170.38 15.50 -10 -4 -2 95.59 13.10 -10 -4 -2 80.59 11.50 10 -4 2 119.29 13.80 -10 4 -2 127.09 15.10 -10 4 -2 76.89 13.00 -10 4 -2 91.39 15.20 10 4 2 110.79 12.40 10 4 2 115.39 12.10 -10 4 -2 89.49 11.80 10 4 2 86.99 13.30 10 4 2 75.09 14.10 -10 4 -2 92.89 11.80 -12 -4 -2 56.09 8.90 -12 -4 -2 49.60 8.40 12 -4 2 73.29 12.40 -12 4 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4 62.19 12.90 -44 4 4 56.59 14.10 44 4 -4 64.49 13.80 -44 4 4 50.29 15.60 -44 4 4 58.29 11.50 -42 -4 4 17.40 10.20 -42 -4 4 35.70 14.40 -42 4 4 3.80 12.20 -42 4 4 3.90 10.10 42 4 -4 19.70 10.90 -42 4 4 21.40 8.80 -40 -4 4 3.50 8.60 -40 -4 4 10.20 12.80 -40 4 4 -0.30 7.60 40 4 -4 11.80 9.90 -40 4 4 -2.10 10.70 -40 4 4 -11.20 9.90 -38 -4 4 36.20 13.00 -38 -4 4 44.20 9.60 -38 4 4 39.90 8.10 -38 4 4 29.40 10.80 38 4 -4 19.60 9.30 -38 4 4 36.40 8.50 -38 4 4 23.90 12.00 -36 -4 4 15.20 10.80 -36 -4 4 3.60 7.20 -36 4 4 1.60 8.60 -36 4 4 -8.50 6.20 36 4 -4 1.30 9.60 -36 4 4 -12.10 9.30 -36 4 4 -4.20 6.70 -34 -4 4 52.19 10.00 -34 -4 4 60.89 12.80 -34 4 4 49.70 8.80 -34 4 4 36.40 10.10 34 4 -4 57.69 12.00 -34 4 4 38.70 7.60 -34 4 4 46.20 12.60 -32 -4 4 36.20 9.10 -32 -4 4 26.30 10.30 -32 4 4 22.80 7.20 -32 4 4 24.40 6.80 32 4 -4 19.50 9.50 -32 4 4 20.00 9.80 -32 4 4 13.80 9.10 32 4 -4 4.00 14.60 -30 -4 4 211.48 20.30 30 -4 -4 219.88 22.80 -30 -4 4 223.58 22.70 30 4 -4 211.08 20.80 -30 4 4 190.48 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202.48 17.40 -4 4 4 171.18 15.80 4 4 -4 145.29 15.20 -4 4 4 160.28 15.50 -4 4 4 161.08 19.60 4 4 -4 157.68 16.00 4 4 -4 163.58 17.80 -4 4 4 161.78 15.40 -4 4 4 177.58 16.10 -4 4 4 148.99 16.70 -2 -4 4 12.40 6.70 -2 -4 4 9.00 7.20 2 -4 -4 14.30 5.40 -2 -4 4 21.00 6.50 -2 4 4 18.10 6.00 -2 4 4 28.70 7.10 -2 4 4 30.30 8.20 -2 4 4 25.60 7.10 -2 4 4 21.20 6.30 -2 4 4 11.00 6.90 2 4 -4 25.60 9.00 2 4 -4 25.20 8.00 2 4 -4 9.80 5.80 -2 4 4 7.50 5.50 -2 4 4 22.70 8.20 0 -4 -4 195.58 16.70 0 -4 4 179.68 18.00 0 -4 4 158.78 19.40 0 -4 4 168.88 18.20 0 4 4 170.78 20.10 0 4 4 201.08 17.90 0 4 4 197.18 17.10 0 4 -4 208.78 18.70 0 4 4 192.38 17.40 0 4 4 204.98 18.20 0 4 -4 173.38 17.20 0 4 -4 194.68 20.30 0 4 4 208.38 18.90 0 4 -4 191.08 16.60 0 4 4 215.58 21.10 0 4 -4 183.58 20.00 2 -4 4 25.40 8.10 -2 -4 -4 17.60 5.30 2 4 4 24.20 9.50 2 4 4 30.60 6.30 2 4 4 31.10 6.60 2 4 4 27.00 8.10 -2 4 -4 17.00 5.30 -2 4 -4 23.80 6.90 -2 4 -4 20.90 7.70 4 -4 4 247.48 21.70 -4 -4 -4 246.08 20.00 4 -4 4 250.67 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141.69 26.50 2 -2 -18 91.69 15.60 2 -2 -18 85.69 12.60 -2 -2 18 140.49 23.30 2 2 -18 70.99 13.30 -2 2 18 75.59 12.90 -2 2 18 44.50 15.90 0 -2 -18 116.29 17.50 0 -2 18 98.49 17.50 0 -2 -18 81.39 14.40 0 2 -18 84.99 18.20 0 2 18 97.69 13.70 0 2 18 49.60 17.50 0 2 -18 70.59 13.30 2 -2 18 49.80 13.70 -2 -2 -18 36.70 13.20 -2 -2 -18 35.20 11.20 -2 2 -18 59.69 16.60 -2 2 -18 36.50 11.30 2 2 18 34.60 11.50 2 2 18 5.90 14.10 4 -2 18 102.79 16.40 -4 -2 -18 105.59 17.20 4 2 18 99.49 14.90 -4 2 -18 78.39 20.00 -4 2 -18 90.39 14.60 4 2 18 76.69 19.00 6 -2 18 163.08 25.70 -6 -2 -18 225.28 24.70 -6 -2 -18 177.08 23.00 6 2 18 208.58 23.30 -6 2 -18 179.18 29.60 6 2 18 150.68 28.30 -6 2 -18 182.08 21.50 -8 -2 -18 26.80 13.70 8 -2 18 27.00 12.40 -8 -2 -18 15.20 11.90 -8 2 -18 31.60 17.20 8 2 18 -4.90 13.90 -8 2 -18 16.40 11.00 8 2 18 7.80 10.70 10 -2 18 21.60 13.40 -10 -2 -18 50.89 14.80 -10 2 -18 43.30 19.00 -12 -2 -18 21.00 13.50 12 -2 18 40.80 13.70 -12 2 -18 67.99 20.10 -12 2 -18 46.90 11.30 12 2 18 38.30 16.00 -14 -2 -18 50.79 16.50 -14 -2 -18 13.40 13.30 -14 2 -18 29.10 21.30 -14 2 -18 37.80 13.60 14 2 18 29.60 16.40 -14 2 -18 12.90 10.40 -16 -2 -18 73.49 17.90 -16 -2 -18 42.70 14.90 -16 2 -18 75.19 23.20 16 2 18 29.70 17.00 -16 2 -18 58.09 14.60 -16 2 -18 40.10 11.90 -18 -2 -18 2.00 13.10 -18 -2 -18 44.30 16.90 -18 2 -18 10.80 12.60 -18 2 -18 10.00 10.40 -18 2 -18 28.70 21.00 -20 -2 -18 26.00 15.80 -20 2 -18 -2.60 10.40 -20 2 -18 -4.70 11.30 -20 2 -18 15.40 21.00 20 2 18 -3.50 16.10 -15 -3 18 56.99 21.90 -15 -3 18 69.39 18.70 15 3 -18 7.60 12.10 15 3 -18 28.80 15.20 13 -3 -18 48.50 14.90 -13 -3 18 103.39 20.10 13 3 -18 59.49 17.40 13 3 -18 68.29 13.60 -11 -3 18 165.58 34.80 11 -3 -18 102.29 17.40 -11 -3 18 92.79 19.30 11 3 -18 87.09 18.50 11 3 -18 65.79 14.10 9 -3 -18 16.60 13.30 -9 -3 18 13.20 15.90 9 3 -18 -7.90 16.10 9 3 -18 -9.80 10.50 -7 -3 18 70.69 16.80 7 -3 -18 57.59 14.40 7 3 -18 60.59 18.10 7 3 -18 35.90 13.30 -5 -3 18 43.50 15.40 5 -3 -18 42.00 13.40 5 3 -18 37.80 12.20 5 3 -18 42.80 18.60 3 -3 -18 13.30 12.70 -3 -3 18 -2.60 13.40 3 3 -18 17.70 19.20 3 3 -18 3.80 11.10 -1 -3 18 2.60 14.70 1 -3 -18 17.80 12.90 1 3 -18 7.70 11.50 1 3 -18 10.90 18.20 -1 -3 -18 85.99 16.20 -1 -3 -18 59.39 12.60 1 -3 18 87.79 16.70 -1 3 -18 70.19 21.00 -1 3 -18 36.00 13.60 -3 -3 -18 47.10 14.80 3 -3 18 8.80 14.80 -3 3 -18 -0.50 20.30 -3 3 -18 13.00 11.70 -5 -3 -18 63.19 16.70 5 -3 18 58.09 16.10 -5 -3 -18 90.09 14.40 -5 3 -18 45.10 21.00 -5 3 -18 69.29 14.50 -7 -3 -18 54.29 13.90 7 -3 18 30.00 15.80 -7 -3 -18 49.50 15.70 -7 3 -18 35.20 12.50 -7 3 -18 45.80 21.20 7 3 18 3.90 18.50 -9 -3 -18 157.78 27.70 -9 -3 -18 116.29 16.90 -9 3 -18 104.89 22.80 9 3 18 71.99 22.70 -9 3 -18 83.99 15.30 -11 -3 -18 57.09 26.90 -26 0 19 -26.10 18.10 26 0 -19 3.60 14.70 -26 0 19 13.00 19.60 -24 0 19 -2.30 17.40 24 0 -19 20.30 14.80 -22 0 19 9.70 16.90 22 0 -19 36.10 14.70 -20 0 19 6.70 14.70 20 0 -19 48.20 14.30 -18 0 19 1.20 14.40 18 0 -19 -5.90 9.20 -18 0 19 -19.00 16.00 -16 0 19 11.80 13.90 16 0 -19 -16.70 20.70 16 0 -19 -10.10 9.60 14 0 -19 -19.20 20.70 -14 0 19 -17.40 14.40 14 0 -19 11.00 9.90 -14 0 19 19.00 14.30 12 0 -19 -2.80 9.80 -12 0 19 0.30 13.40 -12 0 19 -22.40 13.50 12 0 -19 16.00 13.40 12 0 -19 -18.00 21.00 -10 0 19 -19.40 13.70 -10 0 19 -6.20 12.10 -10 0 19 5.60 10.90 10 0 -19 0.20 10.30 10 0 -19 5.30 22.20 10 0 -19 14.00 13.70 8 0 -19 -13.10 10.40 -8 0 19 1.10 11.50 8 0 -19 -10.10 13.50 8 0 -19 -14.80 21.70 -8 0 19 -23.50 14.40 -6 0 19 -18.50 13.60 -6 0 19 15.70 12.10 -6 0 19 14.10 13.20 6 0 -19 -13.70 10.90 6 0 -19 -12.70 21.80 -4 0 19 -8.50 12.70 4 0 -19 -16.70 12.90 4 0 -19 -9.20 13.30 4 0 -19 6.20 22.00 -4 0 19 -0.20 11.90 -4 0 19 -6.50 11.20 2 0 -19 -15.90 10.80 -2 0 19 7.00 12.80 2 0 -19 -25.90 21.20 -2 0 19 3.70 11.00 -2 0 19 -6.90 13.70 2 0 -19 -2.30 12.70 0 0 -19 -7.20 11.20 0 0 -19 20.30 13.70 0 0 19 -9.60 12.10 0 0 19 -6.10 13.50 0 0 -19 -5.80 21.20 0 0 19 -2.90 11.50 2 0 19 -18.90 12.60 -2 0 -19 2.70 23.00 -2 0 -19 -3.00 11.30 2 0 19 3.10 10.30 2 0 19 -3.50 12.50 -2 0 -19 -11.00 14.30 -4 0 -19 5.20 11.60 -4 0 -19 -11.60 15.30 4 0 19 -4.40 10.90 4 0 19 14.60 12.70 6 0 19 2.40 10.80 -6 0 -19 10.40 12.00 -6 0 -19 0.70 16.90 6 0 19 18.00 13.40 -8 0 -19 -16.20 12.00 8 0 19 -4.90 12.20 8 0 19 -13.80 10.80 -8 0 -19 -15.70 16.00 -10 0 -19 -4.10 17.20 -10 0 -19 -24.10 12.30 -10 0 -19 12.60 10.10 10 0 19 -8.70 11.70 -12 0 -19 21.60 17.30 -12 0 -19 -17.60 12.40 -12 0 -19 -3.20 10.00 12 0 19 8.80 12.00 -14 0 -19 -2.20 12.40 -14 0 -19 -5.50 18.60 -16 0 -19 -2.70 19.50 16 0 19 38.80 13.60 -16 0 -19 30.00 13.80 -18 0 -19 17.20 13.50 18 0 19 24.40 13.50 -18 0 -19 -8.20 18.10 -20 0 -19 7.70 17.20 -20 0 -19 3.20 14.10 25 -1 -19 88.19 18.10 -25 -1 19 43.10 24.70 -23 -1 19 52.49 18.20 23 -1 -19 60.49 15.30 -23 -1 19 10.00 22.10 -23 1 19 84.59 21.60 23 1 -19 42.70 13.20 23 1 -19 48.40 13.90 -21 -1 19 79.79 26.00 -21 -1 19 158.88 28.50 21 -1 -19 181.78 22.50 21 -1 -19 107.49 22.50 -21 1 19 176.18 24.80 21 1 -19 131.19 21.00 21 1 -19 130.09 19.50 -19 -1 19 -30.40 19.70 -19 -1 19 29.70 16.20 19 -1 -19 -0.20 18.70 19 -1 -19 16.70 13.10 -19 1 19 12.30 16.80 19 1 -19 10.30 11.00 19 1 -19 38.80 13.20 -17 -1 19 57.59 16.30 -17 -1 19 -2.50 19.20 17 -1 -19 47.10 12.60 17 -1 -19 16.20 17.90 17 1 -19 29.10 17.30 -17 1 19 32.00 15.80 17 1 -19 72.79 14.50 15 -1 -19 -13.60 22.00 15 -1 -19 14.40 12.70 -15 -1 19 -9.90 14.80 -15 -1 19 -1.70 18.10 15 1 -19 -3.80 12.80 -15 1 19 23.00 27.40 15 1 -19 -0.30 12.20 13 -1 -19 140.09 20.20 -13 -1 19 106.89 18.10 13 -1 -19 130.09 21.20 -13 -1 19 102.39 23.70 -13 -1 19 120.49 19.50 13 1 -19 155.48 21.70 -13 1 19 139.39 19.60 13 1 -19 111.79 15.40 -11 -1 19 19.70 12.90 -11 -1 19 30.80 18.60 11 -1 -19 22.80 9.80 -11 -1 19 30.00 14.80 11 -1 -19 22.60 12.70 -11 1 19 28.90 13.80 -11 1 19 -2.80 13.60 11 1 -19 20.40 10.90 -9 -1 19 57.69 17.40 -9 -1 19 39.50 14.00 9 -1 -19 41.30 14.10 -9 -1 19 64.29 15.60 9 -1 -19 57.99 11.50 -9 1 19 13.10 14.50 9 1 -19 34.10 10.80 -9 1 19 46.50 14.40 7 -1 -19 23.90 10.80 -7 -1 19 34.60 14.00 -7 -1 19 25.90 14.60 -7 -1 19 7.90 12.20 7 -1 -19 -17.20 12.00 -7 1 19 -6.30 13.00 7 1 -19 -7.80 9.80 -7 1 19 7.90 11.90 7 1 -19 -5.00 29.10 5 -1 -19 55.19 15.50 -5 -1 19 77.99 17.60 5 -1 -19 82.59 12.90 -5 -1 19 61.09 16.40 -5 -1 19 44.20 14.50 5 1 -19 35.50 27.20 -5 1 19 69.89 19.10 5 1 -19 85.69 17.30 5 1 -19 54.79 11.90 3 -1 -19 72.09 15.10 -3 -1 19 78.59 15.20 -3 -1 19 76.19 17.10 3 -1 -19 118.99 18.60 3 1 -19 65.89 12.30 -3 1 19 72.69 13.70 -3 1 19 67.49 13.50 3 1 -19 73.99 18.00 -3 1 19 44.20 16.20 3 1 -19 53.39 26.50 1 -1 -19 97.89 15.90 -1 -1 19 66.19 15.90 1 -1 -19 69.79 15.70 -1 -1 19 83.39 15.70 -1 1 19 41.90 16.60 1 1 -19 68.99 12.60 1 1 -19 51.89 26.10 1 1 -19 89.89 18.90 -1 1 19 75.09 12.90 -1 1 19 72.69 14.40 1 -1 19 159.38 24.40 1 -1 19 157.18 25.80 -1 -1 -19 193.08 23.90 -1 1 -19 156.58 29.40 -1 1 -19 168.68 20.10 -1 1 -19 186.38 27.90 1 1 19 159.98 25.90 3 -1 19 14.20 12.30 3 -1 19 41.90 13.10 -3 1 -19 21.10 10.80 3 1 19 1.20 12.60 3 1 19 26.80 15.30 -3 1 -19 35.00 17.30 -3 1 -19 19.00 23.50 5 -1 19 47.30 14.40 -5 1 -19 59.89 13.30 -5 1 -19 65.69 25.10 -5 1 -19 74.09 20.00 5 1 19 63.99 15.80 5 1 19 51.79 14.80 -7 -1 -19 14.80 16.20 -7 -1 -19 37.10 13.10 7 -1 19 15.90 12.50 7 -1 19 46.60 13.60 -7 1 -19 -9.10 10.80 -7 1 -19 2.30 23.50 7 1 19 20.20 14.50 -7 1 -19 34.20 19.50 -9 -1 -19 97.49 15.80 -9 -1 -19 78.29 19.50 9 -1 19 68.59 15.50 -9 1 -19 67.79 14.20 -9 1 -19 71.09 25.40 -9 1 -19 105.99 22.10 9 1 19 63.79 18.10 -11 -1 -19 30.00 16.30 -11 -1 -19 23.30 13.70 -11 1 -19 16.00 12.00 -11 1 -19 22.80 19.20 11 1 19 22.70 13.70 -13 -1 -19 51.39 15.30 -13 -1 -19 47.50 18.90 -13 1 -19 37.80 21.10 -13 1 -19 33.20 13.40 13 1 19 53.29 15.60 -13 1 -19 30.30 13.00 -15 -1 -19 34.20 14.50 -15 -1 -19 47.60 18.00 -15 1 -19 27.60 12.30 -15 1 -19 -2.80 12.20 15 1 19 17.80 12.80 -15 1 -19 21.40 19.50 -17 -1 -19 103.79 21.20 -17 -1 -19 88.29 16.70 -17 1 -19 70.59 13.60 -17 1 -19 97.09 23.80 -17 1 -19 78.19 15.60 17 1 19 46.30 16.70 -19 -1 -19 70.69 20.40 -19 1 -19 90.49 21.60 -18 -2 19 11.70 15.40 -18 -2 19 12.00 19.70 18 -2 -19 -15.70 13.80 18 2 -19 13.70 15.30 18 2 -19 14.10 11.10 -16 -2 19 4.70 18.90 -16 -2 19 18.50 15.70 16 -2 -19 -22.20 12.60 16 2 -19 5.10 11.40 16 2 -19 9.10 15.10 -14 -2 19 32.30 15.50 -14 -2 19 35.90 19.50 14 -2 -19 5.20 12.80 14 2 -19 26.10 12.30 14 2 -19 -0.20 14.40 12 -2 -19 18.80 12.50 -12 -2 19 5.20 18.30 -12 -2 19 42.10 16.60 12 2 -19 27.70 15.00 12 2 -19 -0.20 11.00 -10 -2 19 14.00 14.70 10 -2 -19 19.80 12.60 -10 -2 19 24.40 17.30 10 2 -19 4.10 11.20 10 2 -19 -5.40 15.80 -8 -2 19 27.80 17.80 8 -2 -19 -6.20 13.20 -8 -2 19 19.90 15.60 8 2 -19 -4.30 10.90 8 2 -19 -2.20 15.70 -6 -2 19 12.60 13.60 -6 -2 19 43.00 17.60 6 2 -19 -1.00 11.00 6 2 -19 26.90 16.10 -4 -2 19 36.20 16.70 4 -2 -19 12.00 12.90 4 -2 -19 5.30 11.00 -4 -2 19 35.60 14.40 4 2 -19 43.00 16.40 4 2 -19 5.70 11.50 -4 2 19 -21.60 13.20 2 -2 -19 26.90 14.10 -2 -2 19 3.30 13.40 -2 -2 19 48.60 17.80 2 -2 -19 -1.80 10.80 2 2 -19 14.60 12.20 2 2 -19 12.70 16.80 0 -2 -19 70.49 13.20 0 -2 -19 47.70 13.50 0 -2 19 48.40 15.60 0 2 19 15.50 14.90 0 2 -19 49.30 13.10 0 2 -19 35.40 19.20 2 -2 19 48.90 15.80 -2 -2 -19 58.39 15.70 -2 -2 -19 64.69 15.80 -2 2 -19 32.80 12.10 -2 2 -19 24.40 18.50 -4 -2 -19 17.40 14.60 4 -2 19 7.70 13.90 -4 -2 -19 6.50 11.20 -4 2 -19 -17.60 19.40 -4 2 -19 -2.50 11.40 4 2 19 -15.90 14.70 -6 -2 -19 0.70 11.90 6 -2 19 4.10 13.90 -6 -2 -19 12.60 14.30 6 2 19 6.90 18.90 -6 2 -19 7.80 18.70 -6 2 -19 -4.20 11.50 6 2 19 -20.30 14.10 -8 -2 -19 76.19 17.00 -8 -2 -19 46.50 14.60 8 -2 19 66.79 16.80 -8 2 -19 75.39 22.20 10 -2 19 3.90 13.60 -10 -2 -19 40.00 16.20 -10 -2 -19 -2.00 13.50 10 2 19 12.60 15.20 -10 2 -19 33.50 21.00 -12 -2 -19 95.29 19.80 -18 0 20 -5.80 18.70 -16 0 20 -17.90 17.10 -16 0 20 17.90 16.70 14 0 -20 39.80 15.70 -14 0 20 -5.70 15.40 14 0 -20 -3.70 18.20 12 0 -20 48.30 15.40 -12 0 20 -5.90 14.50 12 0 -20 -1.00 11.90 10 0 -20 38.50 13.70 10 0 -20 51.49 15.10 -10 0 20 47.40 15.90 -8 0 20 14.70 15.00 -8 0 20 -9.10 15.50 8 0 -20 7.40 14.30 8 0 -20 6.40 17.50 -6 0 20 18.40 14.90 6 0 -20 41.10 13.00 6 0 -20 20.90 15.10 -6 0 20 32.20 15.40 -4 0 20 213.08 31.90 4 0 -20 262.57 26.30 -4 0 20 240.48 38.60 4 0 -20 272.57 28.10 -2 0 20 11.60 14.70 -2 0 20 51.69 17.10 2 0 -20 56.09 14.00 -2 0 20 17.70 13.70 0 0 -20 282.47 26.50 0 0 20 217.38 28.00 0 0 -20 285.07 30.80 0 0 20 186.68 31.00 2 0 20 36.20 14.80 -2 0 -20 52.79 13.70 2 0 20 14.30 12.60 -2 0 -20 36.60 17.60 4 0 20 73.99 16.50 4 0 20 55.89 16.30 -4 0 -20 92.19 20.50 -4 0 -20 79.19 16.60 -6 0 -20 -7.40 14.40 6 0 20 23.50 14.10 -6 0 -20 31.30 18.60 -8 0 -20 104.19 17.90 8 0 20 76.69 16.50 -8 0 -20 89.19 21.60 10 0 20 9.60 16.50 -10 0 -20 23.70 19.50 -10 0 -20 11.60 14.50 -12 0 -20 209.18 34.00 -15 -1 20 0.00 20.90 15 1 -20 43.40 21.50 -15 1 20 -22.60 15.40 15 1 -20 -14.10 10.90 -13 -1 20 48.20 17.30 13 -1 -20 39.60 16.30 -13 -1 20 22.50 20.60 13 1 -20 18.10 11.70 13 1 -20 70.39 16.90 -13 1 20 34.50 19.80 -11 -1 20 19.90 15.30 -11 -1 20 -11.30 17.60 11 -1 -20 -10.80 13.40 11 1 -20 1.50 10.70 -11 1 20 -10.90 14.80 -9 -1 20 39.10 17.20 -9 -1 20 11.30 17.10 9 1 -20 -3.30 11.00 9 1 -20 50.09 16.80 -7 -1 20 10.40 16.60 7 -1 -20 0.60 12.70 -7 -1 20 19.50 17.00 7 -1 -20 -2.40 14.90 7 1 -20 -3.40 11.10 7 1 -20 19.40 15.70 5 -1 -20 3.60 12.30 -5 -1 20 11.50 16.00 -5 -1 20 24.50 14.70 5 1 -20 16.10 17.90 5 1 -20 -4.40 11.20 -3 -1 20 17.60 13.90 3 -1 -20 47.20 27.70 3 -1 -20 -0.10 13.40 -3 -1 20 16.50 14.90 3 1 -20 -7.90 18.40 -3 1 20 -13.80 14.20 3 1 -20 15.70 11.80 1 -1 -20 6.50 14.40 -1 -1 20 13.60 14.40 -1 -1 20 -1.80 13.70 1 -1 -20 16.70 13.30 1 1 -20 -15.40 19.10 1 1 -20 -9.60 33.20 1 1 -20 10.90 11.30 -1 -1 -20 64.99 15.80 -1 -1 -20 44.80 14.70 1 -1 20 36.70 14.80 1 -1 20 29.90 13.90 -1 1 -20 23.60 12.70 1 1 20 7.60 15.50 -1 1 -20 27.80 19.10 3 -1 20 38.60 14.10 -3 -1 -20 48.70 14.90 3 1 20 29.50 14.90 -3 1 -20 23.70 19.90 -3 1 -20 26.50 12.90 5 -1 20 1.50 13.50 -5 -1 -20 6.50 14.20 -5 -1 -20 15.90 16.60 -5 1 -20 20.80 21.20 -5 1 -20 9.20 12.50 5 1 20 3.00 15.30 -7 -1 -20 0.00 18.80 -7 -1 -20 32.90 15.30 7 -1 20 30.40 14.10 7 -1 20 38.80 15.30 -7 1 -20 54.09 22.00 -7 1 -20 34.00 13.20 -9 -1 -20 19.50 18.40 -9 1 -20 17.80 20.80 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 54230 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -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_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 Ni1 Ni 0.61517(2) 0.78289(10) 0.37953(3) 0.0267(2) Uani 1 1 d . . . . . N1 N 0.58176(7) 0.6620(6) 0.37068(19) 0.0223(8) Uani 1 1 d . . . . . N2 N 0.57100(7) 0.5027(6) 0.4129(2) 0.0225(8) Uani 1 1 d . . . . . N3 N 0.62501(7) 0.6006(7) 0.4665(2) 0.0252(8) Uani 1 1 d . . . . . N4 N 0.66812(8) 0.8970(8) 0.4222(2) 0.0371(10) Uani 1 1 d . . . . . N5 N 0.64750(8) 0.9214(7) 0.3756(2) 0.0334(10) Uani 1 1 d . . . . . C1 C 0.56098(10) 1.0051(8) 0.3107(3) 0.0337(11) Uani 1 1 d . . . . . H1A H 0.552337 1.047522 0.357744 0.051 Uiso 1 1 calc GR . . . . H1B H 0.550780 1.064614 0.265420 0.051 Uiso 1 1 calc GR . . . . H1C H 0.578488 1.073809 0.312406 0.051 Uiso 1 1 calc GR . . . . C2 C 0.57482(9) 0.6625(8) 0.2312(3) 0.0289(10) Uani 1 1 d . . . . . H2A H 0.592475 0.726506 0.229082 0.043 Uiso 1 1 calc GR . . . . H2B H 0.563992 0.719312 0.186681 0.043 Uiso 1 1 calc GR . . . . H2C H 0.575581 0.491189 0.229802 0.043 Uiso 1 1 calc GR . . . . C3 C 0.53592(9) 0.6371(9) 0.3087(3) 0.0338(11) Uani 1 1 d . . . . . H3A H 0.537007 0.466026 0.305789 0.051 Uiso 1 1 calc GR . . . . H3B H 0.524823 0.695595 0.265020 0.051 Uiso 1 1 calc GR . . . . H3C H 0.528427 0.682414 0.357248 0.051 Uiso 1 1 calc GR . . . . C4 C 0.56305(9) 0.7411(7) 0.3054(2) 0.0231(9) Uani 1 1 d . . . . . C5 C 0.51544(9) -0.2265(8) 0.6322(3) 0.0308(11) Uani 1 1 d . . . . . H5A H 0.524310 -0.373909 0.645810 0.046 Uiso 1 1 calc GR . . . . H5B H 0.499797 -0.258929 0.598959 0.046 Uiso 1 1 calc GR . . . . H5C H 0.510436 -0.147857 0.679442 0.046 Uiso 1 1 calc GR . . . . C6 C 0.53352(9) -0.0709(7) 0.5900(2) 0.0243(10) Uani 1 1 d . . . . . C7 C 0.52449(8) 0.1419(8) 0.5594(2) 0.0244(10) Uani 1 1 d . . . . . H7 H 0.506782 0.184913 0.564139 0.029 Uiso 1 1 calc R . . . . C8 C 0.54085(8) 0.2904(8) 0.5226(2) 0.0228(9) Uani 1 1 d . . . . . H8 H 0.534225 0.434608 0.502474 0.027 Uiso 1 1 calc R . . . . C9 C 0.56700(8) 0.2336(7) 0.5141(2) 0.0212(9) Uani 1 1 d . . . . . C10 C 0.57585(9) 0.0178(8) 0.5425(2) 0.0243(10) Uani 1 1 d . . . . . H10 H 0.593330 -0.028780 0.535706 0.029 Uiso 1 1 calc R . . . . C11 C 0.55935(9) -0.1292(8) 0.5805(2) 0.0245(10) Uani 1 1 d . . . . . H11 H 0.565902 -0.273677 0.600648 0.029 Uiso 1 1 calc R . . . . C12 C 0.58378(8) 0.4007(7) 0.4742(2) 0.0207(9) Uani 1 1 d . . . . . C13 C 0.60922(8) 0.4481(8) 0.5021(2) 0.0240(9) Uani 1 1 d . . . . . C14 C 0.62324(10) 0.3663(11) 0.5718(3) 0.0405(13) Uani 1 1 d . . . . . H14 H 0.616901 0.259732 0.608418 0.049 Uiso 1 1 calc R . . . . C15 C 0.64668(10) 0.4681(13) 0.5752(3) 0.0531(17) Uani 1 1 d . . . . . H15 H 0.660098 0.444995 0.614480 0.064 Uiso 1 1 calc R . . . . C16 C 0.64806(9) 0.6193(10) 0.5089(3) 0.0360(12) Uani 1 1 d . . . . . C17 C 0.66827(10) 0.7600(11) 0.4857(3) 0.0431(13) Uani 1 1 d D U . . . C18 C 0.65393(10) 1.0698(9) 0.3071(3) 0.0390(12) Uani 1 1 d . . . . . C19 C 0.62861(11) 1.1855(11) 0.2744(4) 0.0503(15) Uani 1 1 d . . . . . H19A H 0.616049 1.064010 0.257725 0.075 Uiso 1 1 calc GR . . . . H19B H 0.632414 1.284281 0.230242 0.075 Uiso 1 1 calc GR . . . . H19C H 0.621221 1.281845 0.314598 0.075 Uiso 1 1 calc GR . . . . C20 C 0.67328(12) 1.2617(10) 0.3299(4) 0.0540(16) Uani 1 1 d . . . . . H20A H 0.666616 1.354007 0.372236 0.081 Uiso 1 1 calc GR . . . . H20B H 0.675687 1.363642 0.285425 0.081 Uiso 1 1 calc GR . . . . H20C H 0.690032 1.191272 0.346945 0.081 Uiso 1 1 calc GR . . . . C21 C 0.66424(13) 0.9068(11) 0.2472(3) 0.0533(16) Uani 1 1 d . . . . . H21A H 0.667800 0.995998 0.200632 0.080 Uiso 1 1 calc GR . . . . H21B H 0.651227 0.785569 0.234115 0.080 Uiso 1 1 calc GR . . . . H21C H 0.680376 0.833130 0.267993 0.080 Uiso 1 1 calc GR . . . . C22 C 0.69280(17) 0.817(2) 0.5343(5) 0.0449(17) Uani 0.5 1 d D U P A 1 C23 C 0.7043(2) 0.640(3) 0.5746(7) 0.074(3) Uani 0.5 1 d D U P A 1 H23 H 0.696994 0.487229 0.572079 0.089 Uiso 0.5 1 calc R . P A 1 C24 C 0.7276(2) 0.684(3) 0.6212(7) 0.091(4) Uani 0.5 1 d D U P A 1 H24 H 0.735953 0.561038 0.649943 0.109 Uiso 0.5 1 calc R . P A 1 C25 C 0.7378(2) 0.905(2) 0.6239(7) 0.070(2) Uani 0.5 1 d D U P A 1 C26 C 0.7262(2) 1.086(3) 0.5832(6) 0.068(3) Uani 0.5 1 d D U P A 1 H26 H 0.733599 1.238695 0.585914 0.082 Uiso 0.5 1 calc R . P A 1 C27 C 0.7036(2) 1.044(2) 0.5380(7) 0.052(3) Uani 0.5 1 d D U P A 1 H27 H 0.695409 1.168110 0.509451 0.063 Uiso 0.5 1 calc R . P A 1 C28 C 0.7639(3) 0.946(3) 0.6683(12) 0.105(4) Uani 0.5 1 d D U P A 1 H28A H 0.761221 1.040240 0.714375 0.157 Uiso 0.5 1 calc GR . P A 1 H28B H 0.775716 1.028986 0.635066 0.157 Uiso 0.5 1 calc GR . P A 1 H28C H 0.771642 0.795066 0.683760 0.157 Uiso 0.5 1 calc GR . P A 1 C25X C 0.7444(5) 0.724(4) 0.6115(12) 0.070(2) Uani 0.25 1 d D U P A 2 C26X C 0.7315(4) 0.919(5) 0.5860(12) 0.062(4) Uani 0.25 1 d D U P A 2 H26X H 0.739484 1.066356 0.597513 0.074 Uiso 0.25 1 calc R . P A 2 C27X C 0.7077(4) 0.921(4) 0.5448(11) 0.050(4) Uani 0.25 1 d D U P A 2 H27X H 0.699995 1.065647 0.529190 0.060 Uiso 0.25 1 calc R . P A 2 C22X C 0.6948(2) 0.709(4) 0.5256(10) 0.0449(17) Uani 0.25 1 d D U P A 2 C23X C 0.7066(3) 0.507(4) 0.5492(8) 0.045(4) Uani 0.25 1 d D U P A 2 H23X H 0.698768 0.359788 0.537849 0.054 Uiso 0.25 1 calc R . P A 2 C24X C 0.7312(3) 0.523(5) 0.5916(9) 0.055(4) Uani 0.25 1 d D U P A 2 H24X H 0.739169 0.379460 0.607635 0.065 Uiso 0.25 1 calc R . P A 2 C28X C 0.7698(7) 0.728(5) 0.661(3) 0.105(4) Uani 0.25 1 d D U P A 2 H28D H 0.779436 0.871796 0.650787 0.157 Uiso 0.25 1 calc GR . P A 2 H28E H 0.780436 0.591852 0.649067 0.157 Uiso 0.25 1 calc GR . P A 2 H28F H 0.765955 0.723560 0.716010 0.157 Uiso 0.25 1 calc GR . P A 2 C27Y C 0.7176(3) 0.776(3) 0.5008(11) 0.041(3) Uani 0.25 1 d D U P A 3 H27Y H 0.717498 0.783810 0.445981 0.049 Uiso 0.25 1 calc R . P A 3 C22Y C 0.6936(2) 0.751(3) 0.5358(9) 0.0449(17) Uani 0.25 1 d D U P A 3 C23Y C 0.6959(3) 0.742(3) 0.6142(9) 0.043(4) Uani 0.25 1 d D U P A 3 H23Y H 0.680587 0.724745 0.641862 0.052 Uiso 0.25 1 calc R . P A 3 C24Y C 0.7204(3) 0.756(3) 0.6569(12) 0.047(4) Uani 0.25 1 d D U P A 3 H24Y H 0.720856 0.748349 0.711702 0.056 Uiso 0.25 1 calc R . P A 3 C25Y C 0.7433(4) 0.780(3) 0.6210(11) 0.070(2) Uani 0.25 1 d D U P A 3 C26Y C 0.7414(3) 0.790(3) 0.5423(11) 0.051(4) Uani 0.25 1 d D U P A 3 H26Y H 0.756821 0.806942 0.515154 0.061 Uiso 0.25 1 calc R . P A 3 C28Y C 0.7696(5) 0.772(9) 0.6659(15) 0.105(4) Uani 0.25 1 d D U P A 3 H28G H 0.768275 0.849305 0.716023 0.157 Uiso 0.25 1 calc GR . P A 3 H28H H 0.782684 0.853023 0.636491 0.157 Uiso 0.25 1 calc GR . P A 3 H28I H 0.774929 0.608680 0.674122 0.157 Uiso 0.25 1 calc GR . P A 3 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 Ni1 0.0306(3) 0.0232(3) 0.0263(3) 0.0019(3) 0.0009(2) -0.0055(3) N1 0.033(2) 0.0183(19) 0.0156(17) 0.0032(15) 0.0021(15) -0.0001(15) N2 0.032(2) 0.0153(18) 0.0203(18) -0.0031(15) 0.0024(15) 0.0003(15) N3 0.0268(19) 0.028(2) 0.0209(19) -0.0014(16) 0.0002(15) -0.0002(16) N4 0.034(2) 0.047(3) 0.031(2) -0.009(2) 0.0046(18) -0.014(2) N5 0.034(2) 0.037(2) 0.029(2) -0.0052(18) 0.0057(18) -0.0116(19) C1 0.050(3) 0.021(2) 0.030(3) -0.004(2) -0.005(2) 0.006(2) C2 0.041(3) 0.023(2) 0.023(2) -0.0035(19) 0.000(2) 0.002(2) C3 0.034(3) 0.036(3) 0.031(3) 0.008(2) -0.003(2) 0.004(2) C4 0.032(2) 0.019(2) 0.018(2) 0.0016(17) -0.0017(18) 0.0043(18) C5 0.040(3) 0.027(2) 0.025(2) 0.001(2) -0.001(2) -0.007(2) C6 0.036(2) 0.020(2) 0.016(2) -0.0018(17) -0.0031(18) -0.0062(19) C7 0.025(2) 0.025(2) 0.023(2) -0.0048(19) -0.0008(18) -0.0030(18) C8 0.029(2) 0.018(2) 0.020(2) -0.0018(18) -0.0034(17) 0.0007(18) C9 0.030(2) 0.021(2) 0.0122(19) -0.0020(17) -0.0030(17) -0.0010(18) C10 0.030(2) 0.023(2) 0.019(2) -0.0054(18) 0.0023(18) 0.0024(19) C11 0.038(3) 0.019(2) 0.017(2) -0.0018(18) 0.0001(18) 0.0001(19) C12 0.027(2) 0.018(2) 0.016(2) -0.0019(17) -0.0005(17) 0.0014(18) C13 0.029(2) 0.024(2) 0.019(2) -0.0006(18) 0.0045(18) -0.0005(19) C14 0.035(3) 0.067(4) 0.019(2) 0.011(2) -0.003(2) -0.008(3) C15 0.035(3) 0.102(5) 0.022(3) 0.019(3) -0.007(2) -0.020(3) C16 0.029(2) 0.053(3) 0.025(2) -0.005(2) -0.001(2) -0.008(2) C17 0.030(2) 0.066(4) 0.033(3) -0.007(3) 0.003(2) -0.014(2) C18 0.045(3) 0.033(3) 0.040(3) -0.003(2) 0.009(2) -0.010(2) C19 0.052(3) 0.045(3) 0.054(4) 0.011(3) 0.008(3) -0.006(3) C20 0.058(4) 0.040(3) 0.065(4) -0.001(3) 0.010(3) -0.021(3) C21 0.075(4) 0.042(3) 0.045(3) -0.004(3) 0.021(3) -0.007(3) C22 0.033(3) 0.067(4) 0.034(3) -0.003(3) -0.002(2) -0.019(3) C23 0.053(6) 0.091(7) 0.077(7) 0.018(6) -0.017(6) -0.028(6) C24 0.071(7) 0.109(8) 0.090(7) 0.028(7) -0.027(6) -0.026(7) C25 0.042(4) 0.099(5) 0.066(4) 0.009(5) -0.014(3) -0.023(4) C26 0.053(6) 0.086(7) 0.066(6) 0.004(6) -0.009(5) -0.026(6) C27 0.042(5) 0.068(6) 0.046(5) 0.003(5) -0.001(4) -0.019(5) C28 0.051(6) 0.150(11) 0.109(7) 0.023(10) -0.031(5) -0.031(8) C25X 0.042(4) 0.099(5) 0.066(4) 0.009(5) -0.014(3) -0.023(4) C26X 0.046(7) 0.088(8) 0.049(8) 0.000(8) -0.016(7) -0.026(7) C27X 0.038(7) 0.073(8) 0.039(7) -0.003(8) -0.008(6) -0.021(7) C22X 0.033(3) 0.067(4) 0.034(3) -0.003(3) -0.002(2) -0.019(3) C23X 0.032(6) 0.075(8) 0.028(7) -0.020(7) -0.005(6) -0.006(7) C24X 0.032(7) 0.089(8) 0.041(7) -0.012(7) -0.006(6) -0.005(7) C28X 0.051(6) 0.150(11) 0.109(7) 0.023(10) -0.031(5) -0.031(8) C27Y 0.026(6) 0.061(8) 0.035(7) -0.003(7) 0.002(6) -0.012(6) C22Y 0.033(3) 0.067(4) 0.034(3) -0.003(3) -0.002(2) -0.019(3) C23Y 0.031(6) 0.062(8) 0.036(6) 0.001(7) -0.009(6) -0.014(7) C24Y 0.031(7) 0.067(8) 0.040(7) -0.001(7) -0.012(6) -0.011(7) C25Y 0.042(4) 0.099(5) 0.066(4) 0.009(5) -0.014(3) -0.023(4) C26Y 0.030(6) 0.076(8) 0.046(7) 0.002(7) -0.002(6) -0.014(7) C28Y 0.051(6) 0.150(11) 0.109(7) 0.023(10) -0.031(5) -0.031(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N3 93.79(15) . . ? N5 Ni1 N1 172.33(17) . . ? N5 Ni1 N3 93.75(17) . . ? N2 N1 Ni1 129.2(3) . . ? N2 N1 C4 110.8(3) . . ? C4 N1 Ni1 119.9(3) . . ? N1 N2 C12 122.5(4) . . ? C13 N3 Ni1 125.3(3) . . ? C13 N3 C16 109.1(4) . . ? C16 N3 Ni1 125.2(3) . . ? N5 N4 C17 122.3(4) . . ? N4 N5 Ni1 129.3(3) . . ? N4 N5 C18 110.0(4) . . ? C18 N5 Ni1 120.4(3) . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C1 H1A 109.5 . . ? C4 C1 H1B 109.5 . . ? C4 C1 H1C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? N1 C4 C1 107.2(4) . . ? N1 C4 C2 106.2(3) . . ? N1 C4 C3 113.7(3) . . ? C1 C4 C2 112.2(4) . . ? C1 C4 C3 108.6(4) . . ? C3 C4 C2 108.9(4) . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C6 C5 H5A 109.5 . . ? C6 C5 H5B 109.5 . . ? C6 C5 H5C 109.5 . . ? C7 C6 C5 119.9(4) . . ? C11 C6 C5 122.4(4) . . ? C11 C6 C7 117.7(4) . . ? C6 C7 H7 119.5 . . ? C8 C7 C6 121.0(4) . . ? C8 C7 H7 119.5 . . ? C7 C8 H8 119.3 . . ? C7 C8 C9 121.4(4) . . ? C9 C8 H8 119.3 . . ? C8 C9 C12 119.1(4) . . ? C10 C9 C8 117.7(4) . . ? C10 C9 C12 123.2(4) . . ? C9 C10 H10 119.7 . . ? C11 C10 C9 120.5(4) . . ? C11 C10 H10 119.7 . . ? C6 C11 C10 121.7(4) . . ? C6 C11 H11 119.2 . . ? C10 C11 H11 119.2 . . ? N2 C12 C9 112.0(4) . . ? N2 C12 C13 126.4(4) . . ? C13 C12 C9 121.5(4) . . ? N3 C13 C12 122.5(4) . . ? N3 C13 C14 107.7(4) . . ? C12 C13 C14 129.7(4) . . ? C13 C14 H14 126.2 . . ? C15 C14 C13 107.6(5) . . ? C15 C14 H14 126.2 . . ? C14 C15 H15 126.0 . . ? C14 C15 C16 108.0(4) . . ? C16 C15 H15 126.0 . . ? N3 C16 C15 107.6(4) . . ? N3 C16 C17 122.0(5) . . ? C17 C16 C15 130.3(5) . . ? N4 C17 C16 126.9(5) . . ? N4 C17 C22 107.2(6) . . ? N4 C17 C22X 116.4(8) . . ? N4 C17 C22Y 116.8(7) . . ? C16 C17 C22 125.2(6) . . ? C16 C17 C22X 115.0(9) . . ? C16 C17 C22Y 116.3(8) . . ? N5 C18 C19 108.2(4) . . ? N5 C18 C20 111.6(4) . . ? N5 C18 C21 107.1(4) . . ? C20 C18 C19 108.3(5) . . ? C21 C18 C19 109.5(5) . . ? C21 C18 C20 112.0(5) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C17 117.1(9) . . ? C23 C22 C27 120.4(9) . . ? C27 C22 C17 122.5(10) . . ? C22 C23 H23 120.3 . . ? C22 C23 C24 119.4(13) . . ? C24 C23 H23 120.3 . . ? C23 C24 H24 120.4 . . ? C25 C24 C23 119.3(14) . . ? C25 C24 H24 120.4 . . ? C24 C25 C26 121.9(12) . . ? C24 C25 C28 118.8(8) . . ? C26 C25 C28 119.1(8) . . ? C25 C26 H26 120.5 . . ? C25 C26 C27 119.0(13) . . ? C27 C26 H26 120.5 . . ? C22 C27 H27 120.0 . . ? C26 C27 C22 120.1(13) . . ? C26 C27 H27 120.0 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26X C25X C24X 112(2) . . ? C26X C25X C28X 123.8(14) . . ? C24X C25X C28X 123.7(14) . . ? C25X C26X H26X 117.5 . . ? C25X C26X C27X 125(3) . . ? C27X C26X H26X 117.5 . . ? C26X C27X H27X 119.7 . . ? C26X C27X C22X 121(2) . . ? C22X C27X H27X 119.7 . . ? C27X C22X C17 109.9(14) . . ? C23X C22X C17 132.4(15) . . ? C23X C22X C27X 117.5(14) . . ? C22X C23X H23X 121.0 . . ? C22X C23X C24X 118.1(19) . . ? C24X C23X H23X 121.0 . . ? C25X C24X C23X 126(2) . . ? C25X C24X H24X 116.8 . . ? C23X C24X H24X 116.8 . . ? C25X C28X H28D 109.5 . . ? C25X C28X H28E 109.5 . . ? C25X C28X H28F 109.5 . . ? H28D C28X H28E 109.5 . . ? H28D C28X H28F 109.5 . . ? H28E C28X H28F 109.5 . . ? C22Y C27Y H27Y 118.4 . . ? C26Y C27Y H27Y 118.4 . . ? C26Y C27Y C22Y 123.2(17) . . ? C27Y C22Y C17 119.3(13) . . ? C23Y C22Y C17 126.8(13) . . ? C23Y C22Y C27Y 113.7(13) . . ? C22Y C23Y H23Y 118.5 . . ? C22Y C23Y C24Y 123.0(17) . . ? C24Y C23Y H23Y 118.5 . . ? C23Y C24Y H24Y 119.1 . . ? C25Y C24Y C23Y 122(2) . . ? C25Y C24Y H24Y 119.1 . . ? C24Y C25Y C28Y 121.7(13) . . ? C26Y C25Y C24Y 116(2) . . ? C26Y C25Y C28Y 121.7(13) . . ? C27Y C26Y H26Y 119.0 . . ? C25Y C26Y C27Y 122(2) . . ? C25Y C26Y H26Y 119.0 . . ? C25Y C28Y H28G 109.5 . . ? C25Y C28Y H28H 109.5 . . ? C25Y C28Y H28I 109.5 . . ? H28G C28Y H28H 109.5 . . ? H28G C28Y H28I 109.5 . . ? H28H C28Y H28I 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.848(4) . ? Ni1 N3 1.877(4) . ? Ni1 N5 1.844(4) . ? N1 N2 1.309(5) . ? N1 C4 1.512(5) . ? N2 C12 1.350(5) . ? N3 C13 1.361(6) . ? N3 C16 1.362(6) . ? N4 N5 1.303(6) . ? N4 C17 1.351(7) . ? N5 C18 1.510(7) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1 C4 1.515(6) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C2 C4 1.520(6) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C3 C4 1.519(6) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C5 C6 1.505(6) . ? C6 C7 1.395(6) . ? C6 C11 1.386(6) . ? C7 H7 0.9500 . ? C7 C8 1.376(6) . ? C8 H8 0.9500 . ? C8 C9 1.398(6) . ? C9 C10 1.394(6) . ? C9 C12 1.482(6) . ? C10 H10 0.9500 . ? C10 C11 1.386(6) . ? C11 H11 0.9500 . ? C12 C13 1.394(6) . ? C13 C14 1.449(6) . ? C14 H14 0.9500 . ? C14 C15 1.335(7) . ? C15 H15 0.9500 . ? C15 C16 1.443(7) . ? C16 C17 1.389(7) . ? C17 C22 1.512(9) . ? C17 C22X 1.521(10) . ? C17 C22Y 1.523(10) . ? C18 C19 1.538(8) . ? C18 C20 1.517(7) . ? C18 C21 1.512(8) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.346(14) . ? C22 C27 1.412(14) . ? C23 H23 0.9500 . ? C23 C24 1.428(12) . ? C24 H24 0.9500 . ? C24 C25 1.365(11) . ? C25 C26 1.369(11) . ? C25 C28 1.529(13) . ? C26 H26 0.9500 . ? C26 C27 1.383(12) . ? C27 H27 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C25X C26X 1.361(12) . ? C25X C24X 1.367(12) . ? C25X C28X 1.524(14) . ? C26X H26X 0.9500 . ? C26X C27X 1.381(14) . ? C27X H27X 0.9500 . ? C27X C22X 1.410(16) . ? C22X C23X 1.355(16) . ? C23X H23X 0.9500 . ? C23X C24X 1.428(13) . ? C24X H24X 0.9500 . ? C28X H28D 0.9800 . ? C28X H28E 0.9800 . ? C28X H28F 0.9800 . ? C27Y H27Y 0.9500 . ? C27Y C22Y 1.416(15) . ? C27Y C26Y 1.382(14) . ? C22Y C23Y 1.358(15) . ? C23Y H23Y 0.9500 . ? C23Y C24Y 1.425(13) . ? C24Y H24Y 0.9500 . ? C24Y C25Y 1.366(12) . ? C25Y C26Y 1.363(12) . ? C25Y C28Y 1.524(14) . ? C26Y H26Y 0.9500 . ? C28Y H28G 0.9800 . ? C28Y H28H 0.9800 . ? C28Y H28I 0.9800 . ?