#------------------------------------------------------------------------------ #$Date: 2025-01-31 21:16:40 +0200 (Fri, 31 Jan 2025) $ #$Revision: 297545 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/38/1573818.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_1573818 loop_ _publ_author_name 'Michael B\"ohme' 'Adrian E. Ion' 'Benjamin Kintzel' 'Axel Buchholz' 'Helmar G\"orls' 'Winfried Plass' _publ_section_title ; Pentanuclear Nickel(II) Complex with two Vertex-Shared Triaminoguanidine Fragments and Symmetric Capping Ligand ; _journal_issue 13 _journal_name_full 'Zeitschrift fuer Anorganische und Allgemeine Chemie' _journal_page_first 999 _journal_page_last 1009 _journal_paper_doi 10.1002/zaac.202000054 _journal_volume 646 _journal_year 2020 _chemical_formula_moiety 'C76 H48 Br3 N24 Ni3 O3, N O3 [+ solvent]' _chemical_formula_sum 'C76 H48 Br3 N25 Ni3 O6' _chemical_formula_weight 1823.25 _space_group_crystal_system trigonal _space_group_IT_number 167 _space_group_name_Hall '-R 3 2"c' _space_group_name_H-M_alt 'R -3 c :H' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 12 _cell_length_a 22.1327(5) _cell_length_b 22.1327(5) _cell_length_c 65.0522(13) _cell_measurement_reflns_used 60181 _cell_measurement_temperature 183(2) _cell_measurement_theta_max 27.481 _cell_measurement_theta_min 2.215 _cell_volume 27597.0(10) _computing_cell_refinement DENZO _computing_data_collection COLLECT _computing_data_reduction DENZO _computing_molecular_graphics SHELXTL/PC _computing_publication_material 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 183(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'phi + omega - scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0832 _diffrn_reflns_av_unetI/netI 0.0438 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_l_max 84 _diffrn_reflns_limit_l_min -84 _diffrn_reflns_number 60181 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.481 _diffrn_reflns_theta_min 2.215 _exptl_absorpt_coefficient_mu 1.970 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6600 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 10992 _exptl_crystal_size_max 0.082 _exptl_crystal_size_mid 0.068 _exptl_crystal_size_min 0.054 _refine_diff_density_max 1.728 _refine_diff_density_min -0.505 _refine_diff_density_rms 0.083 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 347 _refine_ls_number_reflns 7038 _refine_ls_number_restraints 18 _refine_ls_restrained_S_all 0.991 _refine_ls_R_factor_all 0.0987 _refine_ls_R_factor_gt 0.0582 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1034P)^2^+65.6483P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1532 _refine_ls_wR_factor_ref 0.1794 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 4447 _reflns_number_total 7038 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file Ni5.cif _cod_data_source_block FO2972 _cod_original_cell_volume 27597.0(14) _cod_database_code 1573818 _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_min 0.855 _shelx_estimated_absorpt_t_max 0.901 _shelx_res_file ; TITL r3c in R-3c r3c.res created by SHELXL-2018/3 at 14:19:56 on 05-May-2020 CELL 0.71073 22.1327 22.1327 65.0522 90.000 90.000 120.000 ZERR 12.00 0.0005 0.0005 0.0013 0.000 0.000 0.000 LATT 3 SYMM -Y, X-Y, Z SYMM -X+Y, -X, Z SYMM Y, X, 0.5-Z SYMM X-Y, -Y, 0.5-Z SYMM -X, -X+Y, 0.5-Z SFAC C H N O NI BR UNIT 912 576 300 72 36 36 L.S. 8 0 61 BOND $H FMAP 2 PLAN 20 rem EADP O1N O2N ISOR 0.002 N1N > O2N ACTA TEMP -90 OMIT -2 4 0 OMIT 0 2 4 OMIT -1 2 3 SIZE 0.082 0.068 0.054 REM COLOR:brown ABIN WGHT 0.103400 65.648300 FVAR 0.04101 NI 5 -0.195684 0.449823 -0.046546 11.00000 0.03174 0.03306 = 0.05007 0.00020 -0.00176 0.01575 BR 6 -0.235754 0.764337 -0.057969 11.00000 0.08198 0.04234 = 0.13663 0.00439 0.00008 0.03879 O1 4 -0.146131 0.552833 -0.040551 11.00000 0.03775 0.03617 = 0.06861 -0.00263 -0.00719 0.01714 N1 3 -0.346132 0.386881 -0.052180 11.00000 0.03104 0.02906 = 0.05084 -0.00109 -0.00309 0.01436 N2 3 -0.284833 0.451085 -0.050621 11.00000 0.03035 0.03034 = 0.04790 -0.00279 0.00042 0.01402 N3 3 -0.191245 0.429040 -0.013895 11.00000 0.03841 0.04065 = 0.05090 -0.00066 -0.00123 0.01893 N4 3 -0.105182 0.450179 -0.043392 11.00000 0.03344 0.03619 = 0.04855 -0.00435 -0.00602 0.01520 N5 3 -0.028676 0.430982 -0.022809 11.00000 0.04159 0.05388 = 0.05559 -0.00740 -0.00954 0.02630 N6 3 -0.001697 0.465174 -0.058079 11.00000 0.03567 0.04488 = 0.05830 -0.00571 -0.00040 0.01722 N7 3 -0.152163 0.469637 -0.077486 11.00000 0.04199 0.03906 = 0.04831 -0.00091 -0.00099 0.02097 N8 3 0.086169 0.418319 -0.019975 11.00000 0.04445 0.06177 = 0.06879 -0.00546 -0.00675 0.02787 C1 1 -0.333333 0.333333 -0.051996 10.33333 0.03127 0.03127 = 0.04360 0.00000 0.00000 0.01563 C2 1 -0.289711 0.505215 -0.054761 11.00000 0.03344 0.03691 = 0.05857 0.00181 -0.00056 0.01748 AFIX 43 H2A 2 -0.333060 0.497493 -0.060014 11.00000 -1.20000 AFIX 0 C3 1 -0.234803 0.577178 -0.052119 11.00000 0.04464 0.03218 = 0.05818 0.00299 0.00208 0.01936 C4 1 -0.254341 0.628076 -0.056177 11.00000 0.04478 0.04041 = 0.08412 0.00589 0.00139 0.02215 AFIX 43 H4A 2 -0.299448 0.614239 -0.061453 11.00000 -1.20000 AFIX 0 C5 1 -0.208457 0.696790 -0.052513 11.00000 0.06162 0.03317 = 0.10348 -0.00110 -0.00106 0.02637 C6 1 -0.143321 0.717740 -0.044427 11.00000 0.05218 0.03274 = 0.12394 -0.00788 -0.00297 0.01435 AFIX 43 H6A 2 -0.112254 0.765666 -0.041595 11.00000 -1.20000 AFIX 0 C7 1 -0.123585 0.669598 -0.040505 11.00000 0.04256 0.03783 = 0.10656 -0.01466 -0.01115 0.01594 AFIX 43 H7A 2 -0.078572 0.684713 -0.034935 11.00000 -1.20000 AFIX 0 C8 1 -0.168709 0.596965 -0.044537 11.00000 0.04313 0.03438 = 0.06539 0.00057 0.00261 0.01738 C9 1 -0.236185 0.421416 0.000669 11.00000 0.04176 0.04801 = 0.06080 -0.00464 0.00036 0.01987 AFIX 43 H9A 2 -0.274415 0.427683 -0.002767 11.00000 -1.20000 AFIX 0 C10 1 -0.229579 0.404452 0.020970 11.00000 0.04741 0.05336 = 0.05104 -0.00255 0.00218 0.01661 AFIX 43 H10A 2 -0.262440 0.399936 0.031123 11.00000 -1.20000 AFIX 0 C11 1 -0.175029 0.394447 0.025994 11.00000 0.05724 0.05410 = 0.05057 0.00171 -0.00487 0.02621 AFIX 43 H11A 2 -0.170478 0.381681 0.039606 11.00000 -1.20000 AFIX 0 C12 1 -0.126564 0.403074 0.011090 11.00000 0.04754 0.05236 = 0.05509 -0.00304 -0.00339 0.02592 AFIX 43 H12A 2 -0.088211 0.396676 0.014228 11.00000 -1.20000 AFIX 0 C13 1 -0.135909 0.421292 -0.008486 11.00000 0.04108 0.04320 = 0.05277 -0.00420 -0.00557 0.02044 C14 1 -0.086183 0.435476 -0.025566 11.00000 0.03763 0.04010 = 0.05851 -0.00864 -0.00255 0.01803 C15 1 -0.061181 0.465488 -0.059024 11.00000 0.03477 0.03351 = 0.06060 -0.00151 0.00366 0.01466 C16 1 0.011159 0.445876 -0.039568 11.00000 0.03975 0.04612 = 0.05603 -0.01377 -0.00348 0.02092 C17 1 0.075339 0.440385 -0.038210 11.00000 0.04266 0.05286 = 0.06372 -0.01415 -0.01046 0.02702 C18 1 0.120049 0.456612 -0.054562 11.00000 0.04596 0.06814 = 0.07027 -0.01873 -0.00602 0.02956 AFIX 43 H18A 2 0.110600 0.471443 -0.067261 11.00000 -1.20000 AFIX 0 C19 1 0.179467 0.450914 -0.052177 11.00000 0.05079 0.07935 = 0.07846 -0.02311 -0.00252 0.03566 AFIX 43 H19A 2 0.211872 0.463121 -0.063143 11.00000 -1.20000 AFIX 0 C20 1 0.190835 0.427659 -0.033966 11.00000 0.04761 0.06990 = 0.09640 -0.02285 -0.01150 0.03449 AFIX 43 H20A 2 0.230350 0.422064 -0.032150 11.00000 -1.20000 AFIX 0 C21 1 0.143252 0.412394 -0.018174 11.00000 0.05823 0.07353 = 0.08732 -0.00948 -0.01588 0.04374 AFIX 43 H21A 2 0.151584 0.396936 -0.005420 11.00000 -1.20000 AFIX 0 C22 1 -0.087244 0.478101 -0.078508 11.00000 0.04252 0.03182 = 0.05565 0.00038 0.00107 0.01501 C23 1 -0.049475 0.494111 -0.096843 11.00000 0.05039 0.04794 = 0.05696 0.00279 0.00939 0.02513 AFIX 43 H23A 2 -0.003376 0.501399 -0.096960 11.00000 -1.20000 AFIX 0 C24 1 -0.079277 0.499122 -0.114430 11.00000 0.08491 0.06623 = 0.05429 0.00875 0.01259 0.04826 AFIX 43 H24A 2 -0.054074 0.510689 -0.127000 11.00000 -1.20000 AFIX 0 C25 1 -0.147469 0.487111 -0.113910 11.00000 0.08681 0.08067 = 0.05347 0.00525 0.00247 0.05580 AFIX 43 H25A 2 -0.170312 0.488211 -0.126150 11.00000 -1.20000 AFIX 0 C26 1 -0.181499 0.473319 -0.094753 11.00000 0.06431 0.06061 = 0.06191 0.00335 -0.00037 0.03966 AFIX 43 H26A 2 -0.227441 0.466381 -0.094236 11.00000 -1.20000 AFIX 0 N1N 3 -0.333333 0.626723 0.083333 10.33333 0.03719 0.04063 = 0.03713 -0.00016 -0.00032 0.01860 O1N 4 -0.333333 0.691760 0.083333 10.33333 0.11383 0.11379 = 0.12389 0.00263 0.00526 0.05691 O2N 4 -0.343581 0.589215 0.064330 10.66666 0.10045 0.13912 = 0.11534 -0.00668 -0.01182 0.04696 HKLF 4 REM r3c in R-3c REM wR2 = 0.1794, GooF = S = 0.986, Restrained GooF = 0.991 for all data REM R1 = 0.0582 for 4447 Fo > 4sig(Fo) and 0.0987 for all 7038 data REM 347 parameters refined using 18 restraints END WGHT 0.1000 61.1838 REM Highest difference peak 1.728, deepest hole -0.505, 1-sigma level 0.083 Q1 1 -0.3387 0.5413 0.0647 11.00000 0.05 1.73 Q2 1 -0.3491 0.5910 0.0457 11.00000 0.05 0.70 Q3 1 -0.1943 0.7773 -0.0617 11.00000 0.05 0.61 Q4 1 -0.2413 0.7598 -0.0432 11.00000 0.05 0.54 Q5 1 -0.3333 0.6043 0.0833 10.50000 0.05 0.47 Q6 1 -0.3439 0.6905 0.0742 11.00000 0.05 0.40 Q7 1 -0.2719 0.7337 -0.0659 11.00000 0.05 0.40 Q8 1 -0.3443 0.3598 -0.0510 11.00000 0.05 0.37 Q9 1 -0.3187 0.4193 -0.0528 11.00000 0.05 0.33 Q10 1 -0.2102 0.4682 -0.0387 11.00000 0.05 0.28 Q11 1 -0.0433 0.5413 -0.0144 11.00000 0.05 0.28 Q12 1 0.0533 0.4478 0.0061 11.00000 0.05 0.28 Q13 1 -0.0654 0.5335 -0.0225 11.00000 0.05 0.27 Q14 1 -0.2484 0.6002 -0.0495 11.00000 0.05 0.27 Q15 1 -0.3601 0.3907 -0.0609 11.00000 0.05 0.26 Q16 1 0.0311 0.4710 -0.0639 11.00000 0.05 0.25 Q17 1 -0.1595 0.5772 -0.0403 11.00000 0.05 0.25 Q18 1 -0.3968 0.6642 0.0833 11.00000 0.05 0.25 Q19 1 -0.0800 0.5671 -0.0164 11.00000 0.05 0.25 Q20 1 -0.2876 0.7503 0.0782 11.00000 0.05 0.24 ; _shelx_res_checksum 8016 _shelx_hkl_file ; 0 0 15 2.50 1.70 0 0 -21 -3.00 1.80 0 0 24 13.20 2.00 0 0 -24 16.80 2.20 0 0 27 -2.60 1.90 0 0 -27 -2.60 1.30 0 0 -30 3213.80 73.10 0 0 -33 -2.10 1.60 0 0 -36 184.40 5.80 0 0 -39 -1.90 1.50 0 0 -42 207.30 6.80 0 0 -45 -1.80 1.60 0 0 -48 24.60 2.20 0 0 -51 -0.40 2.00 0 0 -54 10.80 2.10 0 0 -57 -0.60 1.90 0 0 -60 3.60 2.30 0 0 -63 -1.50 2.00 0 0 -66 2.90 2.80 0 0 -69 1.10 2.30 0 0 -72 0.80 2.90 0 0 75 6.80 4.60 0 0 -75 2.20 2.70 0 0 78 -10.90 5.30 0 0 -78 -1.80 3.20 0 0 81 -0.40 5.50 0 0 -81 -3.00 4.10 0 0 84 8.20 6.10 0 0 -84 3.30 5.00 2 -1 84 -1.40 6.40 -2 1 -81 1.20 3.20 2 -1 81 0.30 6.00 -2 1 -78 -3.90 4.00 2 -1 78 -3.70 6.60 -2 1 -75 -1.90 2.50 2 -1 75 5.20 5.10 -2 1 -72 2.00 2.30 -2 1 -69 1.50 2.20 -2 1 -66 2.90 1.90 -2 1 -63 1.80 2.30 -2 1 -60 22.70 2.20 -2 1 -57 41.10 2.80 -2 1 -54 46.20 3.00 -2 1 -51 18.30 1.90 -2 1 -48 52.50 2.80 -2 1 -45 11.60 1.60 -2 1 -42 206.70 6.20 -2 1 -39 214.30 6.30 -2 1 -36 8.70 1.70 -2 1 -33 86.40 2.90 -2 1 -30 103.30 3.30 2 -1 30 100.60 4.30 -2 1 -27 236.90 8.80 2 -1 27 238.00 8.50 -2 1 -24 399.40 14.30 2 -1 24 400.20 13.50 -2 1 -21 806.80 27.30 2 -1 21 769.10 25.40 -2 1 -18 10.10 1.40 2 -1 18 8.90 1.30 2 -1 15 811.60 26.70 2 -1 12 36.30 1.70 2 -1 9 97.30 3.40 2 -1 6 18.40 0.80 2 -1 3 115.40 4.10 2 -1 -3 132.50 5.20 -2 1 9 100.40 4.30 2 -1 -9 97.50 4.10 -2 1 12 30.70 2.40 2 -1 -12 37.10 2.40 -2 1 15 779.40 26.60 2 -1 -15 780.10 19.50 -2 1 18 6.20 2.10 2 -1 -18 9.90 1.50 -2 1 21 798.60 26.80 2 -1 -21 807.50 20.10 2 -1 -24 406.90 10.80 2 -1 -27 243.70 6.80 2 -1 -30 99.60 3.50 2 -1 -33 94.40 3.50 2 -1 -36 7.60 2.10 2 -1 -39 220.50 6.70 2 -1 -42 207.70 6.50 2 -1 -45 17.10 2.10 2 -1 -48 55.10 3.20 2 -1 -51 15.60 2.80 2 -1 -54 38.70 2.90 2 -1 -57 39.00 3.20 2 -1 -60 19.80 2.70 2 -1 -63 0.90 2.50 2 -1 -66 3.20 2.50 2 -1 -69 7.20 2.60 2 -1 -72 -6.30 3.40 -2 1 75 -4.60 5.40 2 -1 -75 -0.80 3.10 -2 1 78 5.40 5.10 2 -1 -78 -2.10 3.40 -2 1 81 8.00 5.20 2 -1 -81 -3.40 4.20 -2 1 84 -0.40 5.30 2 -1 -84 -1.30 4.30 4 -2 81 -6.90 6.30 -4 2 -78 4.20 3.40 4 -2 78 5.50 5.60 -4 2 -75 1.00 2.10 4 -2 75 1.40 5.50 -4 2 -72 1.00 2.30 4 -2 72 8.10 5.20 -4 2 -69 10.70 2.30 -4 2 -66 3.40 1.80 -4 2 -63 21.00 2.30 -4 2 -60 0.70 1.60 -4 2 -57 37.50 2.50 -4 2 -54 8.40 1.80 -4 2 -51 20.40 1.70 -4 2 -48 0.20 1.50 -4 2 -45 65.40 2.80 -4 2 -42 3.50 1.90 -4 2 -39 343.20 9.10 -4 2 -36 2.00 1.10 -4 2 -33 120.20 3.40 -4 2 -30 92.10 4.00 4 -2 30 88.20 3.50 -4 2 -27 497.30 16.90 4 -2 27 507.90 16.20 -4 2 -24 1.50 1.00 4 -2 24 1.70 1.10 4 -2 21 400.30 13.20 4 -2 18 84.60 3.10 4 -2 15 99.00 3.50 4 -2 12 183.80 6.00 4 -2 9 11.30 0.90 4 -2 6 8.90 1.10 4 -2 3 198.10 7.00 4 -2 0 42.00 2.30 -4 2 3 195.30 6.80 4 -2 -3 196.90 5.30 -4 2 6 4.90 0.60 4 -2 -6 8.30 1.30 4 -2 -9 11.80 1.20 4 -2 -12 189.70 5.50 4 -2 -15 102.40 3.30 4 -2 -18 89.00 3.20 4 -2 -21 402.60 10.80 4 -2 -24 -0.90 1.70 4 -2 -27 522.40 13.20 4 -2 -30 93.00 3.70 4 -2 -33 125.00 4.40 4 -2 -36 -1.20 1.90 4 -2 -39 353.30 10.30 4 -2 -42 -2.00 2.10 4 -2 -45 68.70 3.40 4 -2 -48 1.90 2.20 4 -2 -51 23.20 2.80 4 -2 -54 7.20 2.50 4 -2 -57 39.10 3.40 4 -2 -60 -1.90 2.40 4 -2 -63 22.60 3.10 4 -2 -66 13.60 3.10 4 -2 -69 11.50 3.30 -4 2 72 -8.40 4.10 4 -2 -72 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-27 160.20 5.10 6 -3 -30 4.50 2.10 6 -3 -33 30.90 2.40 6 -3 -36 -0.70 2.10 6 -3 -39 51.40 3.10 6 -3 -42 19.50 2.60 6 -3 -45 8.90 2.60 6 -3 -48 17.50 2.90 6 -3 -51 7.80 2.50 6 -3 -54 17.70 2.80 6 -3 -57 19.70 3.10 6 -3 -60 1.90 2.60 6 -3 -63 21.00 3.30 6 -3 -66 12.50 3.20 -6 3 69 19.40 3.80 6 -3 -69 28.10 3.70 -6 3 72 4.70 3.70 6 -3 -72 -1.00 3.40 -6 3 75 1.40 5.00 6 -3 -75 14.20 5.60 -6 3 78 2.10 5.20 6 -3 -78 2.50 6.20 -6 3 81 3.90 4.70 6 -3 -81 2.30 5.10 8 -4 81 -0.10 6.90 8 -4 78 3.50 6.70 8 -4 75 -9.10 6.00 8 -4 72 -1.70 5.40 -8 4 -69 0.70 1.30 8 -4 69 1.10 5.30 -8 4 -66 -1.10 1.30 8 -4 66 0.30 5.10 -8 4 -63 7.50 1.20 -8 4 -60 10.80 1.30 -8 4 -57 0.70 1.00 -8 4 -54 2.20 0.90 -8 4 -51 1.20 0.90 -8 4 -48 1.90 0.90 -8 4 -45 14.00 1.00 -8 4 -42 180.60 4.60 -8 4 -39 13.50 1.10 -8 4 -36 40.00 1.60 8 -4 21 12.10 0.80 8 -4 18 321.00 10.20 8 -4 15 28.20 1.50 -8 4 -12 8.80 1.40 8 -4 12 9.70 1.30 -8 4 -9 278.60 9.90 8 -4 9 285.70 10.00 -8 4 -6 243.10 9.20 8 -4 6 241.60 6.30 -8 4 -3 21.40 2.40 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80 -9.75 0.00 -2 5 80 -9.18 0.00 -4 6 80 -1.29 0.00 -1 6 80 8.36 0.00 -6 7 80 -5.70 0.00 -3 7 80 -7.57 0.00 0 7 80 -9.22 0.00 -5 8 80 -8.26 0.00 -2 8 80 -4.62 0.00 -4 9 80 2.82 0.00 -1 2 81 -8.56 0.00 -2 4 81 -1.66 0.00 -4 5 81 -2.70 0.00 -1 5 81 6.11 0.00 -3 6 81 -3.25 0.00 -5 7 81 -2.54 0.00 -2 7 81 -8.54 0.00 -4 8 81 4.07 0.00 -1 1 82 2.34 0.00 0 2 82 1.06 0.00 -2 3 82 -6.36 0.00 -4 4 82 1.73 0.00 -1 4 82 0.98 0.00 -3 5 82 -3.27 0.00 0 5 82 -0.09 0.00 -5 6 82 -5.21 0.00 -2 6 82 2.42 0.00 -1 3 83 2.79 0.00 -3 4 83 -2.60 0.00 -2 5 83 -1.24 0.00 0 0 84 -4.73 0.00 -1 2 84 -3.04 0.00 -1 2 0 325.67 0.00 -8 28 0 -5.00 0.00 -24 26 1 2.58 0.00 0 1 2 377.02 0.00 0 25 2 -9.37 0.00 -2 26 2 -4.34 0.00 -20 28 3 -4.05 0.00 -8 28 3 -4.19 0.00 -1 1 4 798.19 0.00 -25 25 4 -1.71 0.00 -5 27 4 -2.45 0.00 -22 27 5 4.71 0.00 0 0 6 868.72 0.00 -20 28 6 -0.25 0.00 -8 28 6 -3.98 0.00 -5 27 7 -1.98 0.00 0 1 8 416.11 0.00 -22 27 8 -2.55 0.00 -5 27 10 -3.73 0.00 -19 28 10 4.96 0.00 -9 28 11 -0.37 0.00 0 0 12 608.58 0.00 -3 26 13 3.48 0.00 -19 28 13 -1.55 0.00 -23 26 14 5.10 0.00 -18 28 14 2.97 0.00 -21 27 15 -4.68 0.00 -6 27 15 3.74 0.00 -1 25 16 0.67 0.00 -10 28 16 -7.97 0.00 -24 25 17 4.98 0.00 0 0 18 -4.22 0.00 -17 28 18 -3.81 0.00 -11 28 18 -6.31 0.00 -20 27 19 3.13 0.00 -16 28 19 -2.06 0.00 -13 28 19 4.08 0.00 -7 27 20 0.37 0.00 -15 28 20 4.35 0.00 -12 28 20 -0.39 0.00 -22 26 21 -2.19 0.00 -4 26 21 4.18 0.00 -14 28 21 5.17 0.00 -19 27 23 3.71 0.00 -24 24 24 12.03 0.00 0 24 24 6.35 0.00 -23 25 24 0.86 0.00 -2 25 24 1.62 0.00 -21 26 25 -4.18 0.00 -23 24 28 1.76 0.00 -22 25 28 -3.40 0.00 -6 26 28 -0.98 0.00 -17 27 28 -1.43 0.00 -11 27 28 -0.26 0.00 -1 24 29 2.79 0.00 -20 26 29 -6.32 0.00 -16 27 29 7.96 0.00 -13 27 29 -1.76 0.00 -19 26 30 -2.95 0.00 -7 26 30 -0.84 0.00 -15 27 30 -8.54 0.00 -12 27 30 0.35 0.00 -4 25 31 1.62 0.00 -22 24 32 -4.74 0.00 -8 26 32 0.34 0.00 -20 25 33 -7.55 0.00 -5 25 33 1.21 0.00 -9 26 34 -7.61 0.00 -22 23 36 3.72 0.00 -21 24 36 -12.46 0.00 -3 24 36 -1.72 0.00 -16 26 36 -3.24 0.00 -10 26 36 -1.83 0.00 -12 26 37 11.39 0.00 -4 24 38 -2.63 0.00 -18 25 38 -10.02 0.00 -17 25 39 -3.41 0.00 -8 25 39 -7.67 0.00 -22 22 40 1.51 0.00 -21 23 40 0.65 0.00 -5 24 40 -8.30 0.00 -16 25 40 4.78 0.00 -19 24 41 4.15 0.00 -15 25 41 1.62 0.00 -9 25 41 -0.75 0.00 -18 24 42 -14.41 0.00 -6 24 42 -0.71 0.00 -14 25 42 8.53 0.00 -11 25 42 10.98 0.00 -1 22 43 5.32 0.00 -7 24 44 -7.02 0.00 -20 22 45 -2.23 0.00 -2 22 45 1.58 0.00 -19 23 45 -1.89 0.00 -4 23 45 7.99 0.00 -18 23 46 -8.45 0.00 -14 24 46 4.15 0.00 -13 24 47 -0.27 0.00 -10 24 47 0.16 0.00 -4 22 49 -2.26 0.00 -19 21 50 -2.45 0.00 -18 22 50 1.19 0.00 -14 23 50 3.56 0.00 -8 23 50 -2.89 0.00 -17 22 51 -3.91 0.00 -5 22 51 -0.46 0.00 -13 23 51 -3.35 0.00 -10 23 51 -7.98 0.00 -16 22 52 7.83 0.00 -15 22 53 0.62 0.00 -14 22 54 1.54 0.00 -8 22 54 -6.19 0.00 -18 20 55 -5.49 0.00 -5 21 55 7.27 0.00 -10 22 55 -13.15 0.00 -17 20 56 -1.50 0.00 -11 21 58 -1.11 0.00 -8 21 58 -5.06 0.00 -5 20 59 11.25 0.00 -13 20 60 0.21 0.00 -7 20 60 1.90 0.00 -4 19 61 16.90 0.00 -12 20 61 4.64 0.00 -9 20 61 -9.15 0.00 -17 17 62 3.03 0.00 -16 18 62 -7.36 0.00 -15 18 63 -0.41 0.00 -3 18 63 5.37 0.00 -14 18 64 3.49 0.00 -10 19 64 8.69 0.00 -2 17 65 3.39 0.00 -13 18 65 9.16 0.00 -9 18 66 -5.14 0.00 -11 17 68 1.99 0.00 0 14 70 -2.87 0.00 -2 15 70 3.95 0.00 -10 16 70 8.37 0.00 -9 15 72 9.10 0.00 -6 15 72 14.19 0.00 -1 13 73 -5.16 0.00 -3 14 73 -4.01 0.00 -8 14 74 11.20 0.00 -5 14 74 8.56 0.00 0 11 76 0.04 0.00 -2 12 76 0.21 0.00 -7 13 76 -4.54 0.00 -7 12 77 0.49 0.00 -4 12 77 3.36 0.00 -7 11 78 -1.93 0.00 -4 11 78 -6.00 0.00 -7 10 79 -0.20 0.00 -8 8 80 -27.06 0.00 -7 9 80 -10.15 0.00 -1 9 80 -1.30 0.00 -7 8 81 2.59 0.00 -1 8 81 5.07 0.00 -4 7 82 3.32 0.00 -1 7 82 3.18 0.00 -4 6 83 0.34 0.00 -3 3 84 -10.32 0.00 0 3 84 -9.08 0.00 -2 4 84 -7.00 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 250420) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 874 274 ' ' 2 0.333 0.667 0.167 885 274 ' ' 3 0.000 0.000 0.250 157 50 ' ' 4 -0.333 0.333 0.333 882 274 ' ' 5 0.000 0.000 0.500 874 274 ' ' 6 0.333 0.667 0.667 885 274 ' ' 7 0.000 0.000 0.750 157 50 ' ' 8 -0.333 0.333 0.833 882 274 ' ' 9 0.333 0.667 0.417 157 50 ' ' 10 0.333 0.667 0.917 157 50 ' ' 11 0.667 0.333 0.083 157 50 ' ' 12 0.667 0.333 0.583 157 50 ' ' # Missing Reflections Below sin(th)/lambda = 0.25 loop_ _platon_missing_refln_index_h _platon_missing_refln_index_k _platon_missing_refln_index_l _platon_missing_refln_theta -1 2 0 1.840 0 1 2 1.233 -1 1 4 1.642 0 0 6 1.878 0 1 8 2.721 0 0 12 3.759 0 0 18 5.643 _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL r3c R -3 c :H R = 0.14 CELL 22.1327 22.1327 65.0522 90.00 90.00 120.00 SPGR R-3c # Solvent Accessible Volume = 6215 # Electrons Found in S.A.V. = 1934 # Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others C101 0.976 0.381 0.480 ! 9.55 eA-3 C102 1.000 1.001 0.035 ! 6.42 eA-3 C103 0.953 1.000 0.250 ! 4.94 eA-3 C104 0.258 0.319 0.183 ! 4.39 eA-3 C105 0.336 0.671 0.433 ! 3.57 eA-3 C106 0.592 0.587 0.333 ! 3.16 eA-3 C107 0.283 0.687 0.132 ! 2.21 eA-3 C108 1.000 1.001 0.555 ! 2.16 eA-3 Q109 0.337 0.463 0.934 ! 2.12 eA-3 C110 0.627 0.110 0.832 ! 1.93 eA-3 C111 1.000 1.000 0.250 ! 1.53 eA-3 C112 0.562 0.194 0.075 ! 1.38 eA-3 C113 0.227 0.534 0.406 ! 1.36 eA-3 C114 0.102 0.974 0.758 ! 1.32 eA-3 C115 0.148 0.639 0.165 ! 1.30 eA-3 C116 0.251 0.707 0.910 ! 1.22 eA-3 C117 0.370 0.555 0.172 ! 1.16 eA-3 C118 0.705 0.480 0.339 ! 1.15 eA-3 C119 0.921 0.126 0.001 ! 1.09 eA-3 C120 0.413 0.534 0.668 ! 1.08 eA-3 C121 0.915 0.867 0.491 ! 1.03 eA-3 C122 0.468 0.555 0.661 ! 1.02 eA-3 C123 0.444 0.914 0.660 ! 1.02 eA-3 C124 0.365 0.476 0.161 ! 1.00 eA-3 Q125 0.814 1.000 0.250 ! 0.99 eA-3 C126 0.883 0.438 0.836 ! 0.99 eA-3 C127 0.720 0.191 0.336 ! 0.98 eA-3 Q128 0.391 0.072 0.120 ! 0.95 eA-3 C129 0.727 0.296 0.347 ! 0.91 eA-3 Q130 0.640 0.111 0.770 ! 0.90 eA-3 Q131 0.908 0.589 0.550 ! 0.89 eA-3 C132 0.048 0.901 0.492 ! 0.84 eA-3 C133 0.225 0.062 0.504 ! 0.83 eA-3 C134 0.618 0.435 0.838 ! 0.82 eA-3 C135 0.931 0.838 1.001 ! 0.81 eA-3 C136 1.001 0.131 0.997 ! 0.80 eA-3 Q137 0.266 0.266 0.250 ! 0.79 eA-3 Q138 0.757 0.999 0.043 ! 0.77 eA-3 Q139 0.010 0.077 0.890 ! 0.75 eA-3 C140 0.218 0.603 0.667 ! 0.75 eA-3 Q141 0.091 0.069 0.040 ! 0.74 eA-3 C142 0.604 0.257 0.573 ! 0.73 eA-3 Q143 0.656 0.639 0.082 ! 0.72 eA-3 C144 0.695 0.800 0.499 ! 0.70 eA-3 Q145 0.590 0.682 0.809 ! 0.68 eA-3 Q146 0.914 0.527 0.844 ! 0.66 eA-3 Q147 0.355 0.994 0.757 ! 0.66 eA-3 Q148 0.047 0.967 0.555 ! 0.66 eA-3 Q149 0.265 0.273 0.271 ! 0.65 eA-3 Q150 0.984 0.660 0.180 ! 0.64 eA-3 Q151 0.601 0.665 0.602 ! 0.63 eA-3 Q152 0.147 0.668 0.652 ! 0.62 eA-3 Q153 0.047 0.720 0.015 ! 0.62 eA-3 C154 0.696 0.251 0.348 ! 0.62 eA-3 Q155 0.024 0.351 0.387 ! 0.61 eA-3 Q156 0.360 0.586 0.493 ! 0.61 eA-3 C157 0.023 0.894 0.242 ! 0.60 eA-3 Q158 0.664 0.391 0.894 ! 0.60 eA-3 Q159 0.200 0.188 0.871 ! 0.60 eA-3 Q160 0.422 0.471 0.024 ! 0.60 eA-3 Q161 0.124 0.382 0.481 ! 0.59 eA-3 Q162 0.662 0.466 0.707 ! 0.59 eA-3 Q163 1.000 1.003 0.390 ! 0.57 eA-3 C164 0.248 0.691 0.672 ! 0.57 eA-3 Q165 0.220 0.771 0.187 ! 0.56 eA-3 Q166 0.741 0.961 0.207 ! 0.56 eA-3 Q167 0.765 0.648 0.376 ! 0.55 eA-3 Q168 0.423 0.775 0.547 ! 0.55 eA-3 Q169 0.865 0.742 0.298 ! 0.55 eA-3 Q170 0.095 0.445 0.605 ! 0.55 eA-3 Q171 0.725 0.999 0.918 ! 0.55 eA-3 Q172 0.059 0.040 0.552 ! 0.55 eA-3 C173 0.983 0.039 0.496 ! 0.54 eA-3 C174 0.554 0.227 0.313 ! 0.54 eA-3 Q175 0.229 0.540 0.144 ! 0.54 eA-3 Q176 0.757 0.004 0.684 ! 0.54 eA-3 Q177 0.774 0.281 0.687 ! 0.53 eA-3 Q178 0.117 0.619 0.305 ! 0.53 eA-3 Q179 0.181 0.065 0.679 ! 0.53 eA-3 Q180 0.578 0.330 0.882 ! 0.53 eA-3 Q181 0.038 0.546 0.295 ! 0.53 eA-3 Q182 0.335 0.976 0.723 ! 0.53 eA-3 C183 0.570 0.705 0.160 ! 0.52 eA-3 Q184 0.663 0.229 0.297 ! 0.52 eA-3 Q185 0.704 0.265 0.444 ! 0.52 eA-3 C186 0.548 0.816 0.684 ! 0.51 eA-3 Q187 0.079 0.671 0.497 ! 0.51 eA-3 Q188 0.046 0.095 0.886 ! 0.51 eA-3 Q189 0.765 0.228 0.648 ! 0.50 eA-3 ) ; _shelx_fab_checksum 50440 loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' 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 Ni Ni -0.19568(2) 0.44982(2) -0.04655(2) 0.03849(16) Uani 1 1 d . . . . . Br Br -0.23575(3) 0.76434(3) -0.05797(2) 0.0836(2) Uani 1 1 d . . . . . O1 O -0.14613(14) 0.55283(14) -0.04055(5) 0.0481(7) Uani 1 1 d . . . . . N1 N -0.34613(15) 0.38688(15) -0.05218(5) 0.0373(7) Uani 1 1 d . . . . . N2 N -0.28483(15) 0.45108(15) -0.05062(5) 0.0367(7) Uani 1 1 d . . . . . N3 N -0.19125(17) 0.42904(17) -0.01390(5) 0.0437(8) Uani 1 1 d . . . . . N4 N -0.10518(16) 0.45018(16) -0.04339(5) 0.0404(7) Uani 1 1 d . . . . . N5 N -0.02868(18) 0.43098(19) -0.02281(6) 0.0493(8) Uani 1 1 d . . . . . N6 N -0.00170(17) 0.46517(18) -0.05808(6) 0.0476(8) Uani 1 1 d . . . . . N7 N -0.15216(17) 0.46964(17) -0.07749(5) 0.0428(7) Uani 1 1 d . . . . . N8 N 0.0862(2) 0.4183(2) -0.01997(6) 0.0578(10) Uani 1 1 d . . . . . C1 C -0.333333 0.333333 -0.05200(10) 0.0354(13) Uani 1 3 d S T P . . C2 C -0.2897(2) 0.5052(2) -0.05476(6) 0.0430(9) Uani 1 1 d . . . . . H2A H -0.333060 0.497493 -0.060014 0.052 Uiso 1 1 calc R U . . . C3 C -0.2348(2) 0.5772(2) -0.05212(6) 0.0449(9) Uani 1 1 d . . . . . C4 C -0.2543(2) 0.6281(2) -0.05618(8) 0.0561(11) Uani 1 1 d . . . . . H4A H -0.299448 0.614239 -0.061453 0.067 Uiso 1 1 calc R U . . . C5 C -0.2085(3) 0.6968(2) -0.05251(9) 0.0649(13) Uani 1 1 d . . . . . C6 C -0.1433(3) 0.7177(2) -0.04443(9) 0.0727(15) Uani 1 1 d . . . . . H6A H -0.112254 0.765666 -0.041595 0.087 Uiso 1 1 calc R U . . . C7 C -0.1236(2) 0.6696(2) -0.04051(9) 0.0642(13) Uani 1 1 d . . . . . H7A H -0.078572 0.684713 -0.034935 0.077 Uiso 1 1 calc R U . . . C8 C -0.1687(2) 0.5970(2) -0.04454(7) 0.0485(10) Uani 1 1 d . . . . . C9 C -0.2362(2) 0.4214(2) 0.00067(7) 0.0513(10) Uani 1 1 d . . . . . H9A H -0.274415 0.427683 -0.002767 0.062 Uiso 1 1 calc R U . . . C10 C -0.2296(2) 0.4045(2) 0.02097(7) 0.0544(11) Uani 1 1 d . . . . . H10A H -0.262440 0.399936 0.031123 0.065 Uiso 1 1 calc R U . . . C11 C -0.1750(2) 0.3944(2) 0.02599(7) 0.0547(11) Uani 1 1 d . . . . . H11A H -0.170478 0.381681 0.039606 0.066 Uiso 1 1 calc R U . . . C12 C -0.1266(2) 0.4031(2) 0.01109(6) 0.0512(10) Uani 1 1 d . . . . . H12A H -0.088211 0.396676 0.014228 0.061 Uiso 1 1 calc R U . . . C13 C -0.1359(2) 0.4213(2) -0.00849(6) 0.0460(9) Uani 1 1 d . . . . . C14 C -0.0862(2) 0.4355(2) -0.02557(6) 0.0460(9) Uani 1 1 d . . . . . C15 C -0.0612(2) 0.4655(2) -0.05902(6) 0.0440(9) Uani 1 1 d . . . . . C16 C 0.0112(2) 0.4459(2) -0.03957(7) 0.0475(10) Uani 1 1 d . . . . . C17 C 0.0753(2) 0.4404(2) -0.03821(7) 0.0517(10) Uani 1 1 d . . . . . C18 C 0.1200(2) 0.4566(3) -0.05456(8) 0.0610(12) Uani 1 1 d . . . . . H18A H 0.110600 0.471443 -0.067261 0.073 Uiso 1 1 calc R U . . . C19 C 0.1795(3) 0.4509(3) -0.05218(9) 0.0681(14) Uani 1 1 d . . . . . H19A H 0.211872 0.463121 -0.063143 0.082 Uiso 1 1 calc R U . . . C20 C 0.1908(3) 0.4277(3) -0.03397(9) 0.0690(14) Uani 1 1 d . . . . . H20A H 0.230350 0.422064 -0.032150 0.083 Uiso 1 1 calc R U . . . C21 C 0.1433(3) 0.4124(3) -0.01817(9) 0.0682(14) Uani 1 1 d . . . . . H21A H 0.151584 0.396936 -0.005420 0.082 Uiso 1 1 calc R U . . . C22 C -0.0872(2) 0.4781(2) -0.07851(6) 0.0449(9) Uani 1 1 d . . . . . C23 C -0.0495(2) 0.4941(2) -0.09684(7) 0.0515(10) Uani 1 1 d . . . . . H23A H -0.003376 0.501399 -0.096960 0.062 Uiso 1 1 calc R U . . . C24 C -0.0793(3) 0.4991(3) -0.11443(7) 0.0638(13) Uani 1 1 d . . . . . H24A H -0.054074 0.510689 -0.127000 0.077 Uiso 1 1 calc R U . . . C25 C -0.1475(3) 0.4871(3) -0.11391(8) 0.0675(14) Uani 1 1 d . . . . . H25A H -0.170312 0.488211 -0.126150 0.081 Uiso 1 1 calc R U . . . C26 C -0.1815(3) 0.4733(3) -0.09475(7) 0.0585(12) Uani 1 1 d . . . . . H26A H -0.227441 0.466381 -0.094236 0.070 Uiso 1 1 calc R U . . . N1N N -0.333333 0.6267(3) 0.083333 0.0387(14) Uani 0.6667 2 d S TU P . . O1N O -0.333333 0.6918(5) 0.083333 0.117(3) Uani 0.6667 2 d S TU P . . O2N O -0.3436(4) 0.5892(5) 0.06433(13) 0.124(3) Uani 0.6667 1 d . U P . . 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 Ni 0.0317(3) 0.0331(3) 0.0501(3) 0.0002(2) -0.0018(2) 0.0157(2) Br 0.0820(4) 0.0423(3) 0.1366(6) 0.0044(3) 0.0001(3) 0.0388(3) O1 0.0378(15) 0.0362(14) 0.0686(18) -0.0026(13) -0.0072(13) 0.0171(12) N1 0.0310(15) 0.0291(15) 0.0508(18) -0.0011(13) -0.0031(13) 0.0144(13) N2 0.0303(15) 0.0303(15) 0.0479(17) -0.0028(13) 0.0004(13) 0.0140(13) N3 0.0384(17) 0.0407(18) 0.0509(19) -0.0007(15) -0.0012(15) 0.0189(15) N4 0.0334(16) 0.0362(16) 0.0486(18) -0.0043(14) -0.0060(14) 0.0152(14) N5 0.0416(19) 0.054(2) 0.056(2) -0.0074(17) -0.0095(16) 0.0263(17) N6 0.0357(17) 0.0449(19) 0.058(2) -0.0057(16) -0.0004(15) 0.0172(15) N7 0.0420(18) 0.0391(17) 0.0483(19) -0.0009(15) -0.0010(15) 0.0210(15) N8 0.044(2) 0.062(2) 0.069(3) -0.0055(19) -0.0067(18) 0.0279(18) C1 0.0313(19) 0.0313(19) 0.044(3) 0.000 0.000 0.0156(9) C2 0.0334(19) 0.037(2) 0.059(2) 0.0018(18) -0.0006(17) 0.0175(16) C3 0.045(2) 0.0322(19) 0.058(2) 0.0030(17) 0.0021(18) 0.0194(17) C4 0.045(2) 0.040(2) 0.084(3) 0.006(2) 0.001(2) 0.0222(19) C5 0.062(3) 0.033(2) 0.103(4) -0.001(2) -0.001(3) 0.026(2) C6 0.052(3) 0.033(2) 0.124(5) -0.008(3) -0.003(3) 0.014(2) C7 0.043(2) 0.038(2) 0.107(4) -0.015(2) -0.011(2) 0.0159(19) C8 0.043(2) 0.034(2) 0.065(3) 0.0006(19) 0.003(2) 0.0174(18) C9 0.042(2) 0.048(2) 0.061(3) -0.005(2) 0.000(2) 0.020(2) C10 0.047(2) 0.053(3) 0.051(2) -0.003(2) 0.0022(19) 0.017(2) C11 0.057(3) 0.054(3) 0.051(2) 0.002(2) -0.005(2) 0.026(2) C12 0.048(2) 0.052(2) 0.055(3) -0.003(2) -0.003(2) 0.026(2) C13 0.041(2) 0.043(2) 0.053(2) -0.0042(18) -0.0056(18) 0.0204(18) C14 0.038(2) 0.040(2) 0.059(2) -0.0086(18) -0.0026(18) 0.0180(17) C15 0.035(2) 0.0335(19) 0.061(2) -0.0015(18) 0.0037(18) 0.0147(16) C16 0.040(2) 0.046(2) 0.056(2) -0.0138(19) -0.0035(19) 0.0209(18) C17 0.043(2) 0.053(3) 0.064(3) -0.014(2) -0.010(2) 0.027(2) C18 0.046(2) 0.068(3) 0.070(3) -0.019(2) -0.006(2) 0.030(2) C19 0.051(3) 0.079(4) 0.078(3) -0.023(3) -0.003(2) 0.036(3) C20 0.048(3) 0.070(3) 0.096(4) -0.023(3) -0.012(3) 0.034(3) C21 0.058(3) 0.074(3) 0.087(4) -0.009(3) -0.016(3) 0.044(3) C22 0.043(2) 0.0318(19) 0.056(2) 0.0004(17) 0.0011(18) 0.0150(17) C23 0.050(2) 0.048(2) 0.057(3) 0.003(2) 0.009(2) 0.025(2) C24 0.085(4) 0.066(3) 0.054(3) 0.009(2) 0.013(3) 0.048(3) C25 0.087(4) 0.081(4) 0.053(3) 0.005(2) 0.002(3) 0.056(3) C26 0.064(3) 0.061(3) 0.062(3) 0.003(2) 0.000(2) 0.040(2) N1N 0.0372(19) 0.0406(19) 0.037(2) -0.0002(8) -0.0003(15) 0.0186(9) O1N 0.114(4) 0.114(4) 0.124(4) 0.0026(16) 0.005(3) 0.057(2) O2N 0.100(4) 0.139(4) 0.115(4) -0.007(3) -0.012(3) 0.047(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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' Br Br -0.2901 2.4595 '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 N2 Ni N4 178.05(13) . . N2 Ni O1 89.57(12) . . N4 Ni O1 89.90(12) . . N2 Ni N1 77.38(12) . 3_455 N4 Ni N1 103.22(12) . 3_455 O1 Ni N1 166.72(12) . 3_455 N2 Ni N7 102.37(12) . . N4 Ni N7 75.76(12) . . O1 Ni N7 90.88(12) . . N1 Ni N7 94.30(13) 3_455 . N2 Ni N3 106.23(12) . . N4 Ni N3 75.64(12) . . O1 Ni N3 89.64(12) . . N1 Ni N3 91.62(12) 3_455 . N7 Ni N3 151.40(12) . . C8 O1 Ni 127.1(3) . . C1 N1 N2 111.7(2) . . C1 N1 Ni 112.22(18) . 2_565 N2 N1 Ni 133.4(2) . 2_565 C2 N2 N1 116.3(3) . . C2 N2 Ni 125.7(3) . . N1 N2 Ni 117.3(2) . . C9 N3 C13 117.7(4) . . C9 N3 Ni 127.8(3) . . C13 N3 Ni 114.5(3) . . C14 N4 C15 116.7(3) . . C14 N4 Ni 121.7(3) . . C15 N4 Ni 121.6(3) . . C16 N5 C14 114.0(4) . . C15 N6 C16 114.2(4) . . C26 N7 C22 118.0(4) . . C26 N7 Ni 128.1(3) . . C22 N7 Ni 113.9(3) . . C21 N8 C17 117.4(4) . . N1 C1 N1 119.999(14) 3_455 2_565 N1 C1 N1 119.989(15) 3_455 . N1 C1 N1 119.989(15) 2_565 . N2 C2 C3 125.7(4) . . N2 C2 H2A 117.1 . . C3 C2 H2A 117.1 . . C8 C3 C4 120.4(4) . . C8 C3 C2 124.0(4) . . C4 C3 C2 115.4(4) . . C5 C4 C3 120.0(4) . . C5 C4 H4A 120.0 . . C3 C4 H4A 120.0 . . C4 C5 C6 120.8(4) . . C4 C5 Br 119.4(4) . . C6 C5 Br 119.7(3) . . C7 C6 C5 119.9(4) . . C7 C6 H6A 120.1 . . C5 C6 H6A 120.1 . . C6 C7 C8 121.9(4) . . C6 C7 H7A 119.1 . . C8 C7 H7A 119.1 . . O1 C8 C3 124.2(4) . . O1 C8 C7 118.9(4) . . C3 C8 C7 116.9(4) . . N3 C9 C10 122.5(4) . . N3 C9 H9A 118.8 . . C10 C9 H9A 118.8 . . C11 C10 C9 119.1(4) . . C11 C10 H10A 120.4 . . C9 C10 H10A 120.4 . . C10 C11 C12 119.6(4) . . C10 C11 H11A 120.2 . . C12 C11 H11A 120.2 . . C13 C12 C11 117.8(4) . . C13 C12 H12A 121.1 . . C11 C12 H12A 121.1 . . N3 C13 C12 123.3(4) . . N3 C13 C14 113.4(3) . . C12 C13 C14 123.3(4) . . N4 C14 N5 124.4(4) . . N4 C14 C13 114.4(3) . . N5 C14 C13 121.1(4) . . N6 C15 N4 124.6(4) . . N6 C15 C22 121.7(4) . . N4 C15 C22 113.5(3) . . N5 C16 N6 125.9(4) . . N5 C16 C17 118.1(4) . . N6 C16 C17 116.0(4) . . N8 C17 C18 122.7(4) . . N8 C17 C16 115.6(4) . . C18 C17 C16 121.7(4) . . C17 C18 C19 118.7(5) . . C17 C18 H18A 120.6 . . C19 C18 H18A 120.6 . . C20 C19 C18 119.5(5) . . C20 C19 H19A 120.3 . . C18 C19 H19A 120.3 . . C19 C20 C21 118.3(5) . . C19 C20 H20A 120.8 . . C21 C20 H20A 120.8 . . N8 C21 C20 123.4(5) . . N8 C21 H21A 118.3 . . C20 C21 H21A 118.3 . . N7 C22 C23 122.4(4) . . N7 C22 C15 114.8(3) . . C23 C22 C15 122.7(4) . . C24 C23 C22 119.2(4) . . C24 C23 H23A 120.4 . . C22 C23 H23A 120.4 . . C23 C24 C25 119.3(5) . . C23 C24 H24A 120.4 . . C25 C24 H24A 120.4 . . C24 C25 C26 118.2(5) . . C24 C25 H25A 120.9 . . C26 C25 H25A 120.9 . . N7 C26 C25 122.7(5) . . N7 C26 H26A 118.7 . . C25 C26 H26A 118.7 . . O1N N1N O2N 119.8(5) . . O1N N1N O2N 119.8(5) . 18_444 O2N N1N O2N 120.4(9) . 18_444 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ni N2 2.005(3) . Ni N4 2.010(3) . Ni O1 2.013(3) . Ni N1 2.066(3) 3_455 Ni N7 2.179(3) . Ni N3 2.186(3) . Br C5 1.905(5) . O1 C8 1.326(5) . N1 C1 1.349(3) . N1 N2 1.394(4) . N2 C2 1.284(5) . N3 C9 1.322(5) . N3 C13 1.365(5) . N4 C14 1.328(5) . N4 C15 1.329(5) . N5 C16 1.336(6) . N5 C14 1.337(5) . N6 C15 1.321(5) . N6 C16 1.355(6) . N7 C26 1.320(6) . N7 C22 1.355(5) . N8 C21 1.339(6) . N8 C17 1.349(6) . C2 C3 1.452(5) . C2 H2A 0.9500 . C3 C8 1.391(6) . C3 C4 1.419(6) . C4 C5 1.363(6) . C4 H4A 0.9500 . C5 C6 1.379(7) . C6 C7 1.363(7) . C6 H6A 0.9500 . C7 C8 1.430(6) . C7 H7A 0.9500 . C9 C10 1.400(6) . C9 H9A 0.9500 . C10 C11 1.371(6) . C10 H10A 0.9500 . C11 C12 1.386(6) . C11 H11A 0.9500 . C12 C13 1.382(6) . C12 H12A 0.9500 . C13 C14 1.483(6) . C15 C22 1.476(6) . C16 C17 1.488(6) . C17 C18 1.373(7) . C18 C19 1.391(7) . C18 H18A 0.9500 . C19 C20 1.364(8) . C19 H19A 0.9500 . C20 C21 1.387(7) . C20 H20A 0.9500 . C21 H21A 0.9500 . C22 C23 1.397(6) . C23 C24 1.353(7) . C23 H23A 0.9500 . C24 C25 1.396(8) . C24 H24A 0.9500 . C25 C26 1.408(7) . C25 H25A 0.9500 . C26 H26A 0.9500 . N1N O1N 1.439(13) . N1N O2N 1.442(9) . N1N O2N 1.442(9) 18_444