#------------------------------------------------------------------------------ #$Date: 2024-05-26 01:15:26 +0300 (Sun, 26 May 2024) $ #$Revision: 292039 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/17/1571712.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_1571712 loop_ _publ_author_name 'Song, Jianxin' 'Wang, Lina' 'Liao, Zian' 'Lin, Peng' 'Jia, Yingying' 'Liu, Le' 'Xu, Ling' 'Zhou, Mingbo' 'Yin, Bangshao' 'Rao, Yutao' 'Nakai, Akito' 'Tanaka, Takayuki' 'Shimizu, Daiki' 'Osuka, Atsuhiro' _publ_section_title ; Synthesis of NiII Porphyrin---NiII 5,15-Diazaporphyrin Hybrid Tapes ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC01450B _journal_year 2024 _chemical_formula_moiety 'C160 H168 N14 Ni3' _chemical_formula_sum 'C160 H168 N14 Ni3' _chemical_formula_weight 2463.20 _space_group_crystal_system monoclinic _space_group_IT_number 13 _space_group_name_Hall '-P 2yac' _space_group_name_H-M_alt 'P 1 2/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _audit_creation_date 2024-05-05 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2024-05-08 deposited with the CCDC. 2024-05-24 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 98.4471(18) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 16.4956(3) _cell_length_b 19.5137(8) _cell_length_c 27.9638(6) _cell_measurement_reflns_used 17711 _cell_measurement_temperature 100.2(5) _cell_measurement_theta_max 71.3570 _cell_measurement_theta_min 3.7020 _cell_volume 8903.6(4) _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve (Bourhis et al., 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.2(5) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 8.0697 _diffrn_detector_type EosS2 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -44.00 13.00 1.00 7.50 -- -34.73 57.00-150.00 57 2 \w -25.00 30.00 1.00 7.50 -- -34.73 57.00 0.00 55 3 \w -49.00 33.00 1.00 7.50 -- -34.73 57.00 90.00 82 4 \w -53.00 -23.00 1.00 7.50 -- -34.73 77.00 -90.00 30 5 \w -19.00 29.00 1.00 7.50 -- -34.73 77.00 -90.00 48 6 \w 9.00 99.00 1.00 7.50 -- 34.73 77.00 30.00 90 7 \w 23.00 87.00 1.00 7.50 -- 34.73-125.00-150.00 64 8 \w 8.00 48.00 1.00 7.50 -- 34.73 77.00-150.00 40 9 \w 17.00 102.00 1.00 7.50 -- 34.73 38.00 -30.00 85 10 \w 1.00 74.00 1.00 7.50 -- 34.73 -99.00 0.00 73 11 \w -33.00 47.00 1.00 7.50 -- 34.73 -57.00 90.00 80 12 \w 8.00 102.00 1.00 7.50 -- 34.73 77.00 -30.00 94 13 \w 60.00 94.00 1.00 7.50 -- 34.73 77.00 90.00 34 14 \w 19.00 102.00 1.00 7.50 -- 34.73 57.00-150.00 83 15 \w -3.00 24.00 1.00 7.50 -- 34.73 96.00 16.00 27 16 \w 62.00 101.00 1.00 7.50 -- 34.73 77.00-150.00 39 17 \w -1.00 26.00 1.00 7.50 -- 34.73 94.00 -94.84 27 18 \w 13.00 102.00 1.00 7.50 -- 34.73 29.00 163.00 89 19 \w 10.00 74.00 1.00 7.50 -- 34.73 77.00 120.00 64 20 \w 8.00 53.00 1.00 7.50 -- 34.73 77.00 90.00 45 21 \w -32.00 54.00 1.00 7.50 -- 34.73 -38.00-150.00 86 22 \w 79.00 105.00 1.00 27.50 -- 105.25 77.00 150.00 26 23 \w 114.00 173.00 1.00 27.50 -- 105.25 77.00 -30.00 59 24 \w 125.00 173.00 1.00 27.50 -- 105.25 77.00 30.00 48 25 \w 79.00 105.00 1.00 27.50 -- 105.25 77.00 -30.00 26 26 \w 116.00 172.00 1.00 27.50 -- 105.25 77.00 90.00 56 27 \w 84.00 113.00 1.00 27.50 -- 105.25 30.00-180.00 29 28 \w 79.00 105.00 1.00 27.50 -- 105.25 77.00-120.00 26 29 \w 144.00 170.00 1.00 27.50 -- 105.25 77.00-120.00 26 30 \w 79.00 105.00 1.00 27.50 -- 105.25 77.00-180.00 26 31 \w 79.00 105.00 1.00 27.50 -- 105.25 77.00 30.00 26 32 \w 79.00 104.00 1.00 27.50 -- 105.25 77.00 90.00 25 33 \w 87.00 113.00 1.00 27.50 -- 105.25 61.00 90.00 26 34 \w 133.00 169.00 1.00 27.50 -- 105.25 77.00 -90.00 36 35 \w 87.00 113.00 1.00 27.50 -- 105.25 61.00-150.00 26 36 \w 38.00 131.00 1.00 27.50 -- 105.25 -77.00 150.00 93 37 \w 79.00 105.00 1.00 27.50 -- 105.25 77.00 -90.00 26 38 \w 131.00 166.00 1.00 27.50 -- 105.25 61.00 120.00 35 39 \w 87.00 116.00 1.00 27.50 -- 105.25 61.00 120.00 29 40 \w 87.00 121.00 1.00 27.50 -- 105.25 61.00 0.00 34 41 \w 87.00 113.00 1.00 27.50 -- 105.25 61.00 -90.00 26 42 \w 36.00 116.00 1.00 27.50 -- 105.25-111.00 150.00 80 43 \w 87.00 113.00 1.00 27.50 -- 105.25 61.00 30.00 26 44 \w 120.00 172.00 1.00 27.50 -- 105.25 61.00 150.00 52 45 \w 57.00 123.00 1.00 27.50 -- 105.25 -77.00 0.00 66 46 \w 87.00 113.00 1.00 27.50 -- 105.25 61.00-120.00 26 47 \w 121.00 173.00 1.00 27.50 -- 105.25 77.00 0.00 52 48 \w 79.00 105.00 1.00 27.50 -- 105.25 77.00 120.00 26 49 \w 87.00 113.00 1.00 27.50 -- 105.25 61.00 -30.00 26 50 \w 87.00 113.00 1.00 27.50 -- 105.25 61.00 150.00 26 51 \w 84.00 112.00 1.00 27.50 -- 105.25 30.00 60.00 28 52 \w 84.00 114.00 1.00 27.50 -- 105.25 30.00-120.00 30 53 \w 84.00 113.00 1.00 27.50 -- 105.25 30.00 90.00 29 54 \w 84.00 113.00 1.00 27.50 -- 105.25 30.00-150.00 29 55 \w 87.00 113.00 1.00 27.50 -- 105.25 61.00 60.00 26 56 \w 79.00 104.00 1.00 27.50 -- 105.25 77.00 0.00 25 57 \w 84.00 111.00 1.00 27.50 -- 105.25 30.00 -30.00 27 58 \w 84.00 111.00 1.00 27.50 -- 105.25 30.00 -60.00 27 59 \w 87.00 113.00 1.00 27.50 -- 105.25 61.00 -60.00 26 60 \w 84.00 119.00 1.00 27.50 -- 105.25 30.00 0.00 35 61 \w 85.00 123.00 1.00 27.50 -- 105.25 30.00 120.00 38 62 \w 82.00 108.00 1.00 27.50 -- 105.25 -94.00 0.00 26 63 \w 122.00 169.00 1.00 27.50 -- 105.25 77.00 -60.00 47 64 \w 123.00 173.00 1.00 27.50 -- 105.25 77.00 60.00 50 65 \w 52.00 111.00 1.00 27.50 -- 105.25-111.00 -30.00 59 66 \w 123.00 173.00 1.00 27.50 -- 105.25 77.00-150.00 50 67 \w 79.00 105.00 1.00 27.50 -- 105.25 77.00 -60.00 26 68 \w 79.00 105.00 1.00 27.50 -- 105.25 77.00-150.00 26 69 \w 129.00 172.00 1.00 27.50 -- 105.25 30.00 -90.00 43 70 \w 36.00 76.00 1.00 27.50 -- 105.25 -94.00 0.00 40 71 \w 84.00 111.00 1.00 27.50 -- 105.25 30.00 -90.00 27 72 \w 123.00 173.00 1.00 27.50 -- 105.25 77.00-180.00 50 73 \w 142.00 171.00 1.00 27.50 -- 105.25 77.00 150.00 29 74 \w 79.00 104.00 1.00 27.50 -- 105.25 77.00 60.00 25 75 \w 87.00 113.00 1.00 27.50 -- 105.25 61.00-180.00 26 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, EosS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0207035000 _diffrn_orient_matrix_UB_12 -0.0770000000 _diffrn_orient_matrix_UB_13 0.0023712000 _diffrn_orient_matrix_UB_21 -0.0793293000 _diffrn_orient_matrix_UB_22 -0.0145109000 _diffrn_orient_matrix_UB_23 0.0212889000 _diffrn_orient_matrix_UB_31 -0.0468696000 _diffrn_orient_matrix_UB_32 -0.0095389000 _diffrn_orient_matrix_UB_33 -0.0514033000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0733 _diffrn_reflns_av_unetI/netI 0.0468 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_number 126260 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 66.599 _diffrn_reflns_theta_max 66.599 _diffrn_reflns_theta_min 3.531 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.701 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.69735 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour green _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 0.919 _exptl_crystal_description block _exptl_crystal_F_000 2620 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _platon_squeeze_details ; ; _refine_diff_density_max 2.001 _refine_diff_density_min -0.926 _refine_diff_density_rms 0.086 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 818 _refine_ls_number_reflns 15742 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.126 _refine_ls_R_factor_all 0.1191 _refine_ls_R_factor_gt 0.0939 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2850 _refine_ls_wR_factor_ref 0.3089 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10217 _reflns_number_total 15742 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc01450b2.cif _cod_data_source_block 4b _cod_database_code 1571712 _shelx_shelxl_version_number 2016/6 _chemical_oxdiff_formula 'C100 H100 Ni3 N12' _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 0.986 _shelx_estimated_absorpt_t_min 0.873 _reflns_odcompleteness_completeness 99.91 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.49 _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.a Me refined with riding coordinates: C52(H52A,H52B,H52C) 2.b Aromatic/amide H refined with riding coordinates: C31(H31), C4(H4), C8(H8), C3(H3), C59(H59), C63(H63), C28(H28), C74(H74), C13(H13), C49(H49), C35(H35), C27(H27), C61(H61), C33(H33), C76(H76), C17(H17), C18(H18), C23(H23), C22(H22), C45(H45), C47(H47) 2.c Idealised Me refined as rotating group: C78(H78A,H78B,H78C), C38(H38A,H38B,H38C), C42(H42A,H42B,H42C), C37(H37A,H37B, H37C), C79(H79A,H79B,H79C), C39(H39A,H39B,H39C), C80(H80A,H80B,H80C), C69(H69A, H69B,H69C), C71(H71A,H71B,H71C), C57(H57A,H57B,H57C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C65(H65A,H65B,H65C), C70(H70A,H70B,H70C), C67(H67A,H67B, H67C), C55(H55A,H55B,H55C), C66(H66A,H66B,H66C), C56(H56A,H56B,H56C), C51(H51A, H51B,H51C), C53(H53A,H53B,H53C) ; _shelx_res_file ; TITL CF solution in P2/n exp_560-sr-sr.res created by SHELXL-2016/6 at 11:17:42 on 05-May-2024 CELL 1.54184 16.49558 19.51373 27.96377 90 98.4471 90 ZERR 2 0.00034 0.00076 0.00057 0 0.0018 0 LATT 1 SYMM 0.5-X,+Y,0.5-Z SFAC C H N Ni UNIT 320 336 28 6 L.S. 8 PLAN 9 SIZE 0.2 0.05 0.02 TEMP -172.9(5) fmap 2 acta SHEL 999 0.84 REM REM REM WGHT 0.200000 FVAR 1.00495 NI1 4 0.250000 0.856790 0.250000 10.50000 0.01510 0.06701 = 0.01543 0.00000 -0.00269 0.00000 NI2 4 0.109064 0.726436 0.512490 11.00000 0.02935 0.10116 = 0.02117 0.00813 0.00025 -0.01165 N1 3 0.332771 0.858032 0.305145 11.00000 0.01626 0.06508 = 0.02112 0.00041 -0.00434 -0.00305 N2 3 0.168077 0.856532 0.290920 11.00000 0.01848 0.07655 = 0.01808 -0.00013 -0.00312 0.00053 N3 3 0.251446 0.823455 0.364507 11.00000 0.01940 0.08234 = 0.02203 0.00394 -0.00125 -0.00283 N4 3 0.188966 0.748035 0.472025 11.00000 0.02706 0.10408 = 0.02392 0.00891 0.00163 -0.01086 N6 3 0.028574 0.701704 0.552544 11.00000 0.03328 0.09608 = 0.02821 0.00585 -0.00036 -0.00377 N7 3 0.034336 0.792402 0.477671 11.00000 0.02449 0.10358 = 0.02588 0.00778 -0.00336 -0.00727 C5 1 0.324023 0.846182 0.351328 11.00000 0.02051 0.07016 = 0.02175 0.00242 -0.00145 -0.00102 C2 1 0.414040 0.879879 0.306387 11.00000 0.01626 0.06710 = 0.02261 0.00166 -0.00239 0.00037 C6 1 0.178115 0.839153 0.337532 11.00000 0.02147 0.07723 = 0.02121 0.00830 -0.00034 -0.00017 N5 3 0.185723 0.663261 0.548550 11.00000 0.03889 0.09315 = 0.03031 0.00785 0.00100 -0.01213 C11 1 0.174740 0.783495 0.428548 11.00000 0.02330 0.09355 = 0.01775 0.00926 -0.00236 -0.00552 C10 1 0.102969 0.815763 0.407285 11.00000 0.02397 0.09145 = 0.02001 0.00524 -0.00573 -0.00961 C31 1 -0.148163 0.857972 0.588014 11.00000 0.02992 0.09475 = 0.03024 0.00381 0.00072 -0.00283 AFIX 43 H31 2 -0.101389 0.853342 0.612037 11.00000 -1.20000 AFIX 0 C30 1 -0.146006 0.829417 0.543029 11.00000 0.03237 0.11119 = 0.02201 0.00507 0.00130 -0.00456 C9 1 0.083061 0.871187 0.279919 11.00000 0.01376 0.07265 = 0.02352 0.00229 -0.00301 -0.00219 C29 1 0.040474 0.826208 0.434221 11.00000 0.02430 0.10455 = 0.01952 0.00196 0.00198 -0.00625 C1 1 0.454155 0.885411 0.266927 11.00000 0.01289 0.07100 = 0.02694 0.00435 -0.00424 0.00391 C14 1 0.271696 0.731356 0.477957 11.00000 0.02919 0.08327 = 0.02493 0.01373 -0.00595 -0.00879 C77 1 0.600511 0.845382 0.284531 11.00000 0.02260 0.10924 = 0.02129 -0.00173 -0.00549 0.01623 C4 1 0.395444 0.862072 0.383557 11.00000 0.01977 0.08125 = 0.01663 0.00131 -0.00350 0.00101 AFIX 43 H4 2 0.403076 0.858465 0.417803 11.00000 -1.20000 AFIX 0 C26 1 -0.033255 0.821251 0.493547 11.00000 0.02668 0.11781 = 0.02241 -0.00481 0.00185 -0.00891 C58 1 0.399886 0.676261 0.517897 11.00000 0.03836 0.06309 = 0.02247 0.00826 -0.00367 -0.00528 C34 1 -0.284868 0.871712 0.517607 11.00000 0.02652 0.09375 = 0.03207 0.00928 -0.00396 -0.01221 C8 1 0.044119 0.860619 0.320452 11.00000 0.01559 0.08458 = 0.02664 -0.00638 0.00025 -0.00305 AFIX 43 H8 2 -0.012636 0.866646 0.321842 11.00000 -1.20000 AFIX 0 C72 1 0.544466 0.901026 0.277129 11.00000 0.01681 0.09636 = 0.01937 0.00366 -0.00130 -0.00393 C25 1 -0.071047 0.795418 0.531710 11.00000 0.02887 0.10656 = 0.03833 -0.01431 0.00136 -0.00462 C3 1 0.451166 0.883622 0.355559 11.00000 0.01798 0.07291 = 0.02039 0.00338 -0.00670 0.00068 AFIX 43 H3 2 0.505416 0.898570 0.366843 11.00000 -1.20000 AFIX 0 C12 1 0.249203 0.788405 0.408367 11.00000 0.02443 0.08956 = 0.02091 0.00983 -0.00314 -0.00677 C7 1 0.103236 0.839672 0.358495 11.00000 0.01947 0.08403 = 0.02145 0.00357 -0.00068 -0.00657 C73 1 0.571037 0.967009 0.283767 11.00000 0.02828 0.09732 = 0.02990 0.00782 -0.00257 -0.01015 C59 1 0.454668 0.697190 0.557987 11.00000 0.04290 0.05718 = 0.02655 0.00584 -0.00154 -0.00290 AFIX 43 H59 2 0.434737 0.721218 0.583421 11.00000 -1.20000 AFIX 0 C15 1 0.311564 0.691141 0.515132 11.00000 0.04329 0.08031 = 0.02456 0.00395 0.00032 -0.01084 C63 1 0.430061 0.641028 0.480306 11.00000 0.06256 0.05718 = 0.02560 0.00100 -0.00209 -0.01030 AFIX 43 H63 2 0.392957 0.625795 0.453165 11.00000 -1.20000 AFIX 0 C28 1 -0.020454 0.877290 0.424320 11.00000 0.03406 0.10657 = 0.02251 0.00190 0.00418 -0.00595 AFIX 43 H28 2 -0.028448 0.907072 0.397161 11.00000 -1.20000 AFIX 0 C74 1 0.655154 0.978908 0.298811 11.00000 0.03386 0.11674 = 0.03616 -0.00178 0.00042 -0.02051 AFIX 43 H74 2 0.673934 1.024706 0.304002 11.00000 -1.20000 AFIX 0 C32 1 -0.216802 0.893680 0.599787 11.00000 0.03399 0.09210 = 0.02744 0.00606 0.00155 -0.01011 C13 1 0.309835 0.757220 0.439472 11.00000 0.02491 0.08577 = 0.02795 0.01256 0.00074 -0.00338 AFIX 43 H13 2 0.366099 0.753634 0.435977 11.00000 -1.20000 AFIX 0 C78 1 0.801315 0.941628 0.323956 11.00000 0.01868 0.21731 = 0.04107 -0.01043 -0.00244 -0.01980 AFIX 137 H78A 2 0.815403 0.986771 0.312205 11.00000 -1.50000 H78B 2 0.835416 0.906553 0.311641 11.00000 -1.50000 H78C 2 0.811039 0.941290 0.359381 11.00000 -1.50000 AFIX 0 C49 1 0.076012 0.547961 0.674159 11.00000 0.03888 0.07410 = 0.03640 0.00622 0.01163 0.00770 AFIX 43 H49 2 0.066275 0.592531 0.685746 11.00000 -1.20000 AFIX 0 C16 1 0.268986 0.658672 0.548093 11.00000 0.03956 0.08101 = 0.02939 0.00934 0.00124 -0.00366 C24 1 -0.044774 0.734619 0.555420 11.00000 0.03078 0.12426 = 0.02723 0.01118 -0.00137 -0.00520 C35 1 -0.215945 0.835758 0.507542 11.00000 0.03345 0.11247 = 0.02857 -0.00036 -0.00299 -0.00573 AFIX 43 H35 2 -0.216199 0.815481 0.476635 11.00000 -1.20000 AFIX 0 C27 1 -0.065376 0.875346 0.461399 11.00000 0.02930 0.10975 = 0.03261 -0.00726 0.00639 0.00477 AFIX 43 H27 2 -0.110007 0.904547 0.465324 11.00000 -1.20000 AFIX 0 C60 1 0.536614 0.683697 0.561293 11.00000 0.03973 0.05910 = 0.03324 0.00952 -0.00309 0.00288 C19 1 0.169656 0.614109 0.581504 11.00000 0.05390 0.09434 = 0.02576 0.00626 0.00716 -0.01758 C36 1 -0.356766 0.881491 0.476099 11.00000 0.03281 0.09230 = 0.03329 0.00666 -0.00982 -0.00806 C75 1 0.710625 0.926393 0.306169 11.00000 0.02037 0.17581 = 0.02398 0.00104 -0.00082 -0.00879 C61 1 0.565459 0.647889 0.523126 11.00000 0.04503 0.06808 = 0.03976 0.00911 0.00310 0.00429 AFIX 43 H61 2 0.622121 0.637187 0.525743 11.00000 -1.20000 AFIX 0 C33 1 -0.283929 0.899238 0.563197 11.00000 0.03335 0.08988 = 0.03474 0.01023 0.00100 -0.01267 AFIX 43 H33 2 -0.331149 0.923069 0.569989 11.00000 -1.20000 AFIX 0 C38 1 -0.392515 0.812489 0.461932 11.00000 0.04240 0.09361 = 0.04746 0.01493 -0.01687 -0.01160 AFIX 137 H38A 2 -0.350626 0.783606 0.450577 11.00000 -1.50000 H38B 2 -0.438935 0.817878 0.435992 11.00000 -1.50000 H38C 2 -0.411345 0.790891 0.489970 11.00000 -1.50000 AFIX 0 C21 1 0.028909 0.643195 0.581409 11.00000 0.05485 0.08496 = 0.03343 0.00356 0.01395 -0.02038 C76 1 0.683880 0.860148 0.298458 11.00000 0.02185 0.12893 = 0.04007 -0.00953 0.00025 0.00858 AFIX 43 H76 2 0.722453 0.823700 0.302620 11.00000 -1.20000 AFIX 0 C62 1 0.513626 0.628142 0.482302 11.00000 0.05499 0.05706 = 0.03586 0.00633 0.00832 0.00359 C40 1 -0.214399 0.926113 0.650828 11.00000 0.05064 0.08436 = 0.02825 -0.00124 -0.00556 -0.01204 C68 1 0.594588 0.705245 0.607089 11.00000 0.03967 0.09076 = 0.03545 0.01101 -0.00379 -0.00481 C20 1 0.093176 0.599364 0.594124 11.00000 0.04558 0.09475 = 0.02677 0.00736 0.00247 -0.00510 C17 1 0.304035 0.607936 0.581218 11.00000 0.04850 0.08411 = 0.03698 0.01528 0.00424 -0.00597 AFIX 43 H17 2 0.360279 0.595585 0.587767 11.00000 -1.20000 AFIX 0 C42 1 -0.194550 0.870963 0.688593 11.00000 0.05216 0.08905 = 0.02699 -0.00767 0.00800 0.00173 AFIX 137 H42A 2 -0.237412 0.835795 0.684208 11.00000 -1.50000 H42B 2 -0.191706 0.891191 0.720873 11.00000 -1.50000 H42C 2 -0.141648 0.850102 0.685213 11.00000 -1.50000 AFIX 0 C37 1 -0.324210 0.915218 0.432964 11.00000 0.04785 0.10496 = 0.03759 0.01038 -0.01317 -0.02214 AFIX 137 H37A 2 -0.292728 0.956304 0.443983 11.00000 -1.50000 H37B 2 -0.370392 0.928014 0.408411 11.00000 -1.50000 H37C 2 -0.288772 0.882822 0.419019 11.00000 -1.50000 AFIX 0 C79 1 0.512872 1.028047 0.278202 11.00000 0.05019 0.07465 = 0.07184 0.00806 -0.00595 -0.01487 AFIX 137 H79A 2 0.470383 1.020716 0.250284 11.00000 -1.50000 H79B 2 0.543608 1.069796 0.273263 11.00000 -1.50000 H79C 2 0.487199 1.032903 0.307478 11.00000 -1.50000 AFIX 0 C39 1 -0.424308 0.929101 0.490794 11.00000 0.04289 0.12686 = 0.04263 0.00836 -0.01219 -0.00301 AFIX 137 H39A 2 -0.446684 0.908892 0.518161 11.00000 -1.50000 H39B 2 -0.468240 0.934409 0.463380 11.00000 -1.50000 H39C 2 -0.400655 0.974070 0.500123 11.00000 -1.50000 AFIX 0 C80 1 0.573132 0.772661 0.279925 11.00000 0.04067 0.09359 = 0.06365 -0.00717 -0.00638 0.01799 AFIX 137 H80A 2 0.539303 0.762233 0.305023 11.00000 -1.50000 H80B 2 0.621135 0.742481 0.283736 11.00000 -1.50000 H80C 2 0.540938 0.765408 0.247986 11.00000 -1.50000 AFIX 0 C54 1 0.069884 0.497046 0.756924 11.00000 0.08038 0.08790 = 0.03179 0.01286 0.00265 0.00603 C48 1 0.077139 0.490784 0.704451 11.00000 0.07079 0.07701 = 0.04392 -0.00464 0.01928 -0.01098 C69 1 0.684720 0.701163 0.600173 11.00000 0.04272 0.13994 = 0.05124 -0.00701 -0.01327 -0.00474 AFIX 137 H69A 2 0.696548 0.655326 0.588650 11.00000 -1.50000 H69B 2 0.719498 0.710105 0.631069 11.00000 -1.50000 H69C 2 0.695871 0.735442 0.576368 11.00000 -1.50000 AFIX 0 C18 1 0.242647 0.580783 0.601491 11.00000 0.05543 0.09214 = 0.04067 0.02019 0.00807 -0.00163 AFIX 43 H18 2 0.247458 0.545427 0.625092 11.00000 -1.20000 AFIX 0 C23 1 -0.088716 0.693790 0.587219 11.00000 0.04310 0.07867 = 0.06127 -0.00312 0.02963 0.00003 AFIX 43 H23 2 -0.139276 0.706125 0.597319 11.00000 -1.20000 AFIX 0 C44 1 0.089621 0.537946 0.626173 11.00000 0.04371 0.08836 = 0.04209 0.00256 0.00533 -0.00151 C64 1 0.544628 0.592661 0.439725 11.00000 0.07611 0.06520 = 0.04315 0.00057 0.01346 0.00181 C71 1 0.578340 0.657488 0.648082 11.00000 0.06602 0.12029 = 0.03977 0.01710 -0.01017 -0.01435 AFIX 137 H71A 2 0.520717 0.661112 0.652645 11.00000 -1.50000 H71B 2 0.613490 0.670651 0.678019 11.00000 -1.50000 H71C 2 0.590412 0.610135 0.639818 11.00000 -1.50000 AFIX 0 C22 1 -0.048864 0.639428 0.599193 11.00000 0.03927 0.10811 = 0.04444 0.02015 0.00769 0.00790 AFIX 43 H22 2 -0.067092 0.602373 0.616911 11.00000 -1.20000 AFIX 0 C57 1 0.051757 0.564559 0.772271 11.00000 0.21119 0.14566 = 0.04706 -0.00448 0.05935 0.00147 AFIX 137 H57A 2 0.093364 0.596608 0.764103 11.00000 -1.50000 H57B 2 0.051810 0.564715 0.807320 11.00000 -1.50000 H57C 2 -0.002322 0.578599 0.755900 11.00000 -1.50000 AFIX 0 C46 1 0.109468 0.415885 0.638616 11.00000 0.05785 0.07963 = 0.05142 0.00458 0.00767 -0.00270 C45 1 0.105364 0.472782 0.609181 11.00000 0.05402 0.07708 = 0.04699 0.00152 0.01057 -0.00001 AFIX 43 H45 2 0.113470 0.467498 0.576444 11.00000 -1.20000 AFIX 0 C41 1 -0.146054 0.980571 0.656843 11.00000 0.07344 0.09952 = 0.06010 -0.00719 -0.00914 -0.02541 AFIX 137 H41A 2 -0.092924 0.958236 0.656526 11.00000 -1.50000 H41B 2 -0.145880 1.004576 0.687640 11.00000 -1.50000 H41C 2 -0.155878 1.013547 0.630188 11.00000 -1.50000 AFIX 0 C43 1 -0.295357 0.958623 0.657599 11.00000 0.07590 0.08265 = 0.04809 -0.00062 -0.00257 0.01520 AFIX 137 H43A 2 -0.308264 0.995669 0.634049 11.00000 -1.50000 H43B 2 -0.291382 0.977260 0.690403 11.00000 -1.50000 H43C 2 -0.338784 0.923967 0.652723 11.00000 -1.50000 AFIX 0 C47 1 0.096439 0.426914 0.687242 11.00000 0.07208 0.07323 = 0.05868 0.01655 0.00991 -0.00151 AFIX 43 H47 2 0.101135 0.389039 0.708818 11.00000 -1.20000 AFIX 0 C65 1 0.539907 0.645519 0.398710 11.00000 0.15127 0.08205 = 0.04613 -0.00143 0.04181 0.01285 AFIX 137 H65A 2 0.483698 0.647593 0.381577 11.00000 -1.50000 H65B 2 0.577141 0.632017 0.376102 11.00000 -1.50000 H65C 2 0.555872 0.690673 0.412282 11.00000 -1.50000 AFIX 0 C70 1 0.577333 0.780029 0.619665 11.00000 0.05136 0.10662 = 0.06503 -0.01183 -0.00390 -0.01634 AFIX 137 H70A 2 0.600601 0.810757 0.597514 11.00000 -1.50000 H70B 2 0.602393 0.789679 0.652965 11.00000 -1.50000 H70C 2 0.518008 0.787319 0.616532 11.00000 -1.50000 AFIX 0 C50 1 0.133230 0.343807 0.620387 11.00000 0.09098 0.06790 = 0.06702 -0.00404 0.00551 -0.01110 C67 1 0.497430 0.528962 0.424361 11.00000 0.11959 0.08247 = 0.07848 -0.00943 0.03207 -0.01307 AFIX 137 H67A 2 0.499862 0.497617 0.451916 11.00000 -1.50000 H67B 2 0.521320 0.506668 0.398291 11.00000 -1.50000 H67C 2 0.440185 0.540869 0.412808 11.00000 -1.50000 AFIX 0 C52 1 0.213541 0.327914 0.640119 11.00000 0.13017 0.09702 = 0.12915 -0.04085 0.01394 0.01095 AFIX 33 H52A 2 0.218682 0.328499 0.675479 11.00000 -1.50000 H52B 2 0.227526 0.282231 0.629277 11.00000 -1.50000 H52C 2 0.250908 0.361834 0.629482 11.00000 -1.50000 AFIX 0 C55 1 0.147390 0.473372 0.789039 11.00000 0.08960 0.14395 = 0.07182 0.01289 0.01477 -0.00371 AFIX 137 H55A 2 0.145354 0.423608 0.793427 11.00000 -1.50000 H55B 2 0.151363 0.496027 0.820574 11.00000 -1.50000 H55C 2 0.195349 0.485240 0.773792 11.00000 -1.50000 AFIX 0 C66 1 0.636077 0.573823 0.451555 11.00000 0.06957 0.15907 = 0.10357 -0.03853 0.01919 0.03498 AFIX 137 H66A 2 0.667549 0.614455 0.463608 11.00000 -1.50000 H66B 2 0.655712 0.557110 0.422258 11.00000 -1.50000 H66C 2 0.643140 0.537921 0.476323 11.00000 -1.50000 AFIX 0 C56 1 0.000388 0.448711 0.768311 11.00000 0.12407 0.14872 = 0.05498 0.00738 0.03102 -0.02745 AFIX 137 H56A 2 -0.047156 0.453274 0.743014 11.00000 -1.50000 H56B 2 -0.015370 0.461157 0.799628 11.00000 -1.50000 H56C 2 0.019841 0.401202 0.769474 11.00000 -1.50000 AFIX 0 C51 1 0.127102 0.342512 0.565492 11.00000 0.08873 0.13568 = 0.10068 -0.03859 -0.01281 0.00614 AFIX 137 H51A 2 0.069756 0.336175 0.551089 11.00000 -1.50000 H51B 2 0.160119 0.304600 0.555817 11.00000 -1.50000 H51C 2 0.147489 0.385926 0.554264 11.00000 -1.50000 AFIX 0 C53 1 0.072869 0.291085 0.638724 11.00000 0.22491 0.08265 = 0.18489 -0.04658 0.11185 -0.06393 AFIX 137 H53A 2 0.073652 0.296877 0.673601 11.00000 -1.50000 H53B 2 0.090019 0.244379 0.632102 11.00000 -1.50000 H53C 2 0.017243 0.299077 0.621921 11.00000 -1.50000 AFIX 0 HKLF 4 REM CF solution in P2/n REM R1 = 0.0939 for 10217 Fo > 4sig(Fo) and 0.1191 for all 15742 data REM 818 parameters refined using 0 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 2.001, deepest hole -0.926, 1-sigma level 0.086 Q1 1 0.2018 0.3284 0.6857 11.00000 0.05 2.00 Q2 1 0.0831 0.7665 0.5134 11.00000 0.05 1.98 Q3 1 -0.1034 0.7460 0.5909 11.00000 0.05 0.98 Q4 1 0.0385 0.5722 0.6216 11.00000 0.05 0.89 Q5 1 0.0038 0.7459 0.5534 11.00000 0.05 0.83 Q6 1 -0.1563 0.8795 0.5409 11.00000 0.05 0.76 Q7 1 0.1834 0.2890 0.5900 11.00000 0.05 0.70 Q8 1 -0.0580 0.7824 0.5598 11.00000 0.05 0.70 Q9 1 0.0027 0.5275 0.6018 11.00000 0.05 0.66 ; _shelx_res_checksum 87537 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.662 _oxdiff_exptl_absorpt_empirical_full_min 0.639 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, 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 0.250000 0.85679(5) 0.250000 0.0330(3) Uani 1 2 d S T P . . Ni2 Ni 0.10906(4) 0.72644(5) 0.51249(2) 0.0509(3) Uani 1 1 d . . . . . N1 N 0.33277(17) 0.85803(18) 0.30515(11) 0.0349(7) Uani 1 1 d . . . . . N2 N 0.16808(17) 0.85653(19) 0.29092(11) 0.0383(8) Uani 1 1 d . . . . . N3 N 0.25145(18) 0.8235(2) 0.36451(12) 0.0417(8) Uani 1 1 d . . . . . N4 N 0.1890(2) 0.7480(2) 0.47203(13) 0.0519(10) Uani 1 1 d . . . . . N6 N 0.0286(2) 0.7017(2) 0.55254(13) 0.0530(10) Uani 1 1 d . . . . . N7 N 0.03434(19) 0.7924(2) 0.47767(13) 0.0520(10) Uani 1 1 d . . . . . C5 C 0.3240(2) 0.8462(2) 0.35133(14) 0.0379(9) Uani 1 1 d . . . . . C2 C 0.4140(2) 0.8799(2) 0.30639(13) 0.0358(8) Uani 1 1 d . . . . . C6 C 0.1781(2) 0.8392(2) 0.33753(14) 0.0403(9) Uani 1 1 d . . . . . N5 N 0.1857(2) 0.6633(2) 0.54855(14) 0.0545(10) Uani 1 1 d . . . . . C11 C 0.1747(2) 0.7835(3) 0.42855(14) 0.0454(10) Uani 1 1 d . . . . . C10 C 0.1030(2) 0.8158(3) 0.40728(14) 0.0460(11) Uani 1 1 d . . . . . C31 C -0.1482(2) 0.8580(3) 0.58801(16) 0.0520(11) Uani 1 1 d . . . . . H31 H -0.101389 0.853342 0.612037 0.062 Uiso 1 1 calc R . . . . C30 C -0.1460(3) 0.8294(3) 0.54303(16) 0.0555(13) Uani 1 1 d . . . . . C9 C 0.08306(19) 0.8712(2) 0.27992(14) 0.0372(9) Uani 1 1 d . . . . . C29 C 0.0405(2) 0.8262(3) 0.43422(15) 0.0496(11) Uani 1 1 d . . . . . C1 C 0.45416(19) 0.8854(2) 0.26693(14) 0.0377(9) Uani 1 1 d . . . . . C14 C 0.2717(2) 0.7314(3) 0.47796(15) 0.0468(10) Uani 1 1 d . . . . . C77 C 0.6005(2) 0.8454(3) 0.28453(15) 0.0519(12) Uani 1 1 d . . . . . C4 C 0.3954(2) 0.8621(2) 0.38356(14) 0.0398(9) Uani 1 1 d . . . . . H4 H 0.403076 0.858465 0.417803 0.048 Uiso 1 1 calc R . . . . C26 C -0.0333(2) 0.8213(3) 0.49355(15) 0.0558(13) Uani 1 1 d . . . . . C58 C 0.3999(2) 0.6763(2) 0.51790(14) 0.0421(9) Uani 1 1 d . . . . . C34 C -0.2849(2) 0.8717(3) 0.51761(16) 0.0516(12) Uani 1 1 d . . . . . C8 C 0.0441(2) 0.8606(2) 0.32045(15) 0.0426(10) Uani 1 1 d . . . . . H8 H -0.012636 0.866646 0.321842 0.051 Uiso 1 1 calc R . . . . C72 C 0.5445(2) 0.9010(3) 0.27713(14) 0.0446(11) Uani 1 1 d . . . . . C25 C -0.0710(3) 0.7954(3) 0.53171(17) 0.0583(13) Uani 1 1 d . . . . . C3 C 0.4512(2) 0.8836(2) 0.35556(13) 0.0380(9) Uani 1 1 d . . . . . H3 H 0.505416 0.898570 0.366843 0.046 Uiso 1 1 calc R . . . . C12 C 0.2492(2) 0.7884(3) 0.40837(14) 0.0456(10) Uani 1 1 d . . . . . C7 C 0.1032(2) 0.8397(3) 0.35849(14) 0.0420(10) Uani 1 1 d . . . . . C73 C 0.5710(2) 0.9670(3) 0.28377(16) 0.0525(12) Uani 1 1 d . . . . . C59 C 0.4547(3) 0.6972(2) 0.55799(15) 0.0429(9) Uani 1 1 d . . . . . H59 H 0.434737 0.721218 0.583421 0.051 Uiso 1 1 calc R . . . . C15 C 0.3116(3) 0.6911(3) 0.51513(15) 0.0499(11) Uani 1 1 d . . . . . C63 C 0.4301(3) 0.6410(2) 0.48031(16) 0.0493(10) Uani 1 1 d . . . . . H63 H 0.392957 0.625795 0.453165 0.059 Uiso 1 1 calc R . . . . C28 C -0.0205(3) 0.8773(3) 0.42432(16) 0.0544(12) Uani 1 1 d . . . . . H28 H -0.028448 0.907072 0.397161 0.065 Uiso 1 1 calc R . . . . C74 C 0.6552(3) 0.9789(3) 0.29881(17) 0.0627(14) Uani 1 1 d . . . . . H74 H 0.673934 1.024706 0.304002 0.075 Uiso 1 1 calc R . . . . C32 C -0.2168(3) 0.8937(3) 0.59979(16) 0.0515(11) Uani 1 1 d . . . . . C13 C 0.3098(2) 0.7572(3) 0.43947(15) 0.0465(10) Uani 1 1 d . . . . . H13 H 0.366099 0.753634 0.435977 0.056 Uiso 1 1 calc R . . . . C78 C 0.8013(3) 0.9416(5) 0.32396(19) 0.093(3) Uani 1 1 d . . . . . H78A H 0.815403 0.986771 0.312205 0.140 Uiso 1 1 calc GR . . . . H78B H 0.835416 0.906553 0.311641 0.140 Uiso 1 1 calc GR . . . . H78C H 0.811039 0.941290 0.359381 0.140 Uiso 1 1 calc GR . . . . C49 C 0.0760(3) 0.5480(3) 0.67416(16) 0.0492(10) Uani 1 1 d . . . . . H49 H 0.066275 0.592531 0.685746 0.059 Uiso 1 1 calc R . . . . C16 C 0.2690(3) 0.6587(3) 0.54809(16) 0.0504(11) Uani 1 1 d . . . . . C24 C -0.0448(3) 0.7346(3) 0.55542(17) 0.0613(14) Uani 1 1 d . . . . . C35 C -0.2159(3) 0.8358(3) 0.50754(17) 0.0589(13) Uani 1 1 d . . . . . H35 H -0.216199 0.815481 0.476635 0.071 Uiso 1 1 calc R . . . . C27 C -0.0654(3) 0.8753(3) 0.46140(16) 0.0570(13) Uani 1 1 d . . . . . H27 H -0.110007 0.904547 0.465324 0.068 Uiso 1 1 calc R . . . . C60 C 0.5366(3) 0.6837(2) 0.56129(16) 0.0449(10) Uani 1 1 d . . . . . C19 C 0.1697(3) 0.6141(3) 0.58150(16) 0.0579(13) Uani 1 1 d . . . . . C36 C -0.3568(3) 0.8815(3) 0.47610(17) 0.0543(12) Uani 1 1 d . . . . . C75 C 0.7106(3) 0.9264(4) 0.30617(17) 0.074(2) Uani 1 1 d . . . . . C61 C 0.5655(3) 0.6479(3) 0.52313(17) 0.0513(11) Uani 1 1 d . . . . . H61 H 0.622121 0.637187 0.525743 0.062 Uiso 1 1 calc R . . . . C33 C -0.2839(3) 0.8992(3) 0.56320(16) 0.0531(12) Uani 1 1 d . . . . . H33 H -0.331149 0.923069 0.569989 0.064 Uiso 1 1 calc R . . . . C38 C -0.3925(3) 0.8125(3) 0.46193(19) 0.0635(14) Uani 1 1 d . . . . . H38A H -0.350626 0.783606 0.450577 0.095 Uiso 1 1 calc GR . . . . H38B H -0.438935 0.817878 0.435992 0.095 Uiso 1 1 calc GR . . . . H38C H -0.411345 0.790891 0.489970 0.095 Uiso 1 1 calc GR . . . . C21 C 0.0289(3) 0.6432(3) 0.58141(17) 0.0570(12) Uani 1 1 d . . . . . C76 C 0.6839(3) 0.8601(4) 0.29846(18) 0.0640(15) Uani 1 1 d . . . . . H76 H 0.722453 0.823700 0.302620 0.077 Uiso 1 1 calc R . . . . C62 C 0.5136(3) 0.6281(2) 0.48230(17) 0.0491(10) Uani 1 1 d . . . . . C40 C -0.2144(3) 0.9261(3) 0.65083(16) 0.0556(12) Uani 1 1 d . . . . . C68 C 0.5946(3) 0.7052(3) 0.60709(17) 0.0562(12) Uani 1 1 d . . . . . C20 C 0.0932(3) 0.5994(3) 0.59412(16) 0.0560(12) Uani 1 1 d . . . . . C17 C 0.3040(3) 0.6079(3) 0.58122(17) 0.0567(12) Uani 1 1 d . . . . . H17 H 0.360279 0.595585 0.587767 0.068 Uiso 1 1 calc R . . . . C42 C -0.1946(3) 0.8710(3) 0.68859(16) 0.0558(12) Uani 1 1 d . . . . . H42A H -0.237412 0.835795 0.684208 0.084 Uiso 1 1 calc GR . . . . H42B H -0.191706 0.891191 0.720873 0.084 Uiso 1 1 calc GR . . . . H42C H -0.141648 0.850102 0.685213 0.084 Uiso 1 1 calc GR . . . . C37 C -0.3242(3) 0.9152(3) 0.43296(18) 0.0654(15) Uani 1 1 d . . . . . H37A H -0.292728 0.956304 0.443983 0.098 Uiso 1 1 calc GR . . . . H37B H -0.370392 0.928014 0.408411 0.098 Uiso 1 1 calc GR . . . . H37C H -0.288772 0.882822 0.419019 0.098 Uiso 1 1 calc GR . . . . C79 C 0.5129(3) 1.0280(3) 0.2782(2) 0.0671(14) Uani 1 1 d . . . . . H79A H 0.470383 1.020716 0.250284 0.101 Uiso 1 1 calc GR . . . . H79B H 0.543608 1.069796 0.273263 0.101 Uiso 1 1 calc GR . . . . H79C H 0.487199 1.032903 0.307478 0.101 Uiso 1 1 calc GR . . . . C39 C -0.4243(3) 0.9291(4) 0.4908(2) 0.0726(16) Uani 1 1 d . . . . . H39A H -0.446684 0.908892 0.518161 0.109 Uiso 1 1 calc GR . . . . H39B H -0.468240 0.934409 0.463380 0.109 Uiso 1 1 calc GR . . . . H39C H -0.400655 0.974070 0.500123 0.109 Uiso 1 1 calc GR . . . . C80 C 0.5731(3) 0.7727(3) 0.2799(2) 0.0674(15) Uani 1 1 d . . . . . H80A H 0.539303 0.762233 0.305023 0.101 Uiso 1 1 calc GR . . . . H80B H 0.621135 0.742481 0.283736 0.101 Uiso 1 1 calc GR . . . . H80C H 0.540938 0.765408 0.247986 0.101 Uiso 1 1 calc GR . . . . C54 C 0.0699(4) 0.4970(3) 0.75692(18) 0.0673(14) Uani 1 1 d . . . . . C48 C 0.0771(3) 0.4908(3) 0.70445(19) 0.0628(13) Uani 1 1 d . . . . . C69 C 0.6847(3) 0.7012(4) 0.6002(2) 0.0800(19) Uani 1 1 d . . . . . H69A H 0.696548 0.655326 0.588650 0.120 Uiso 1 1 calc GR . . . . H69B H 0.719498 0.710105 0.631069 0.120 Uiso 1 1 calc GR . . . . H69C H 0.695871 0.735442 0.576368 0.120 Uiso 1 1 calc GR . . . . C18 C 0.2426(3) 0.5808(3) 0.60149(19) 0.0626(13) Uani 1 1 d . . . . . H18 H 0.247458 0.545427 0.625092 0.075 Uiso 1 1 calc R . . . . C23 C -0.0887(3) 0.6938(3) 0.5872(2) 0.0588(13) Uani 1 1 d . . . . . H23 H -0.139276 0.706125 0.597319 0.071 Uiso 1 1 calc R . . . . C44 C 0.0896(3) 0.5379(3) 0.62617(18) 0.0581(12) Uani 1 1 d . . . . . C64 C 0.5446(4) 0.5927(3) 0.43972(19) 0.0610(13) Uani 1 1 d . . . . . C71 C 0.5783(4) 0.6575(4) 0.6481(2) 0.0772(18) Uani 1 1 d . . . . . H71A H 0.520717 0.661112 0.652645 0.116 Uiso 1 1 calc GR . . . . H71B H 0.613490 0.670651 0.678019 0.116 Uiso 1 1 calc GR . . . . H71C H 0.590412 0.610135 0.639818 0.116 Uiso 1 1 calc GR . . . . C22 C -0.0489(3) 0.6394(3) 0.59919(19) 0.0638(14) Uani 1 1 d . . . . . H22 H -0.067092 0.602373 0.616911 0.077 Uiso 1 1 calc R . . . . C57 C 0.0518(7) 0.5646(5) 0.7723(3) 0.131(4) Uani 1 1 d . . . . . H57A H 0.093364 0.596608 0.764103 0.196 Uiso 1 1 calc GR . . . . H57B H 0.051810 0.564715 0.807320 0.196 Uiso 1 1 calc GR . . . . H57C H -0.002322 0.578599 0.755900 0.196 Uiso 1 1 calc GR . . . . C46 C 0.1095(3) 0.4159(3) 0.6386(2) 0.0630(13) Uani 1 1 d . . . . . C45 C 0.1054(3) 0.4728(3) 0.60918(19) 0.0590(12) Uani 1 1 d . . . . . H45 H 0.113470 0.467498 0.576444 0.071 Uiso 1 1 calc R . . . . C41 C -0.1461(4) 0.9806(4) 0.6568(2) 0.0796(17) Uani 1 1 d . . . . . H41A H -0.092924 0.958236 0.656526 0.119 Uiso 1 1 calc GR . . . . H41B H -0.145880 1.004576 0.687640 0.119 Uiso 1 1 calc GR . . . . H41C H -0.155878 1.013547 0.630188 0.119 Uiso 1 1 calc GR . . . . C43 C -0.2954(4) 0.9586(3) 0.6576(2) 0.0700(15) Uani 1 1 d . . . . . H43A H -0.308264 0.995669 0.634049 0.105 Uiso 1 1 calc GR . . . . H43B H -0.291382 0.977260 0.690403 0.105 Uiso 1 1 calc GR . . . . H43C H -0.338784 0.923967 0.652723 0.105 Uiso 1 1 calc GR . . . . C47 C 0.0964(4) 0.4269(3) 0.6872(2) 0.0680(14) Uani 1 1 d . . . . . H47 H 0.101135 0.389039 0.708818 0.082 Uiso 1 1 calc R . . . . C65 C 0.5399(6) 0.6455(4) 0.3987(2) 0.090(2) Uani 1 1 d . . . . . H65A H 0.483698 0.647593 0.381577 0.136 Uiso 1 1 calc GR . . . . H65B H 0.577141 0.632017 0.376102 0.136 Uiso 1 1 calc GR . . . . H65C H 0.555872 0.690673 0.412282 0.136 Uiso 1 1 calc GR . . . . C70 C 0.5773(3) 0.7800(4) 0.6197(2) 0.0756(17) Uani 1 1 d . . . . . H70A H 0.600601 0.810757 0.597514 0.113 Uiso 1 1 calc GR . . . . H70B H 0.602393 0.789679 0.652965 0.113 Uiso 1 1 calc GR . . . . H70C H 0.518008 0.787319 0.616532 0.113 Uiso 1 1 calc GR . . . . C50 C 0.1332(4) 0.3438(3) 0.6204(2) 0.0759(16) Uani 1 1 d . . . . . C67 C 0.4974(5) 0.5290(4) 0.4244(3) 0.092(2) Uani 1 1 d . . . . . H67A H 0.499862 0.497617 0.451916 0.138 Uiso 1 1 calc GR . . . . H67B H 0.521320 0.506668 0.398291 0.138 Uiso 1 1 calc GR . . . . H67C H 0.440185 0.540869 0.412808 0.138 Uiso 1 1 calc GR . . . . C52 C 0.2135(6) 0.3279(5) 0.6401(4) 0.119(3) Uani 1 1 d . . . . . H52A H 0.218682 0.328499 0.675479 0.179 Uiso 1 1 calc R . . . . H52B H 0.227526 0.282231 0.629277 0.179 Uiso 1 1 calc R . . . . H52C H 0.250908 0.361834 0.629482 0.179 Uiso 1 1 calc R . . . . C55 C 0.1474(5) 0.4734(5) 0.7890(3) 0.101(2) Uani 1 1 d . . . . . H55A H 0.145354 0.423608 0.793427 0.152 Uiso 1 1 calc GR . . . . H55B H 0.151363 0.496027 0.820574 0.152 Uiso 1 1 calc GR . . . . H55C H 0.195349 0.485240 0.773792 0.152 Uiso 1 1 calc GR . . . . C66 C 0.6361(4) 0.5738(5) 0.4516(3) 0.110(3) Uani 1 1 d . . . . . H66A H 0.667549 0.614455 0.463608 0.165 Uiso 1 1 calc GR . . . . H66B H 0.655712 0.557110 0.422258 0.165 Uiso 1 1 calc GR . . . . H66C H 0.643140 0.537921 0.476323 0.165 Uiso 1 1 calc GR . . . . C56 C 0.0004(5) 0.4487(5) 0.7683(3) 0.107(3) Uani 1 1 d . . . . . H56A H -0.047156 0.453274 0.743014 0.161 Uiso 1 1 calc GR . . . . H56B H -0.015370 0.461157 0.799628 0.161 Uiso 1 1 calc GR . . . . H56C H 0.019841 0.401202 0.769474 0.161 Uiso 1 1 calc GR . . . . C51 C 0.1271(5) 0.3425(5) 0.5655(3) 0.111(3) Uani 1 1 d . . . . . H51A H 0.069756 0.336175 0.551089 0.167 Uiso 1 1 calc GR . . . . H51B H 0.160119 0.304600 0.555817 0.167 Uiso 1 1 calc GR . . . . H51C H 0.147489 0.385926 0.554264 0.167 Uiso 1 1 calc GR . . . . C53 C 0.0729(8) 0.2911(5) 0.6387(4) 0.156(5) Uani 1 1 d . . . . . H53A H 0.073652 0.296877 0.673601 0.234 Uiso 1 1 calc GR . . . . H53B H 0.090019 0.244379 0.632102 0.234 Uiso 1 1 calc GR . . . . H53C H 0.017243 0.299077 0.621921 0.234 Uiso 1 1 calc GR . . . . 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 0.0151(4) 0.0670(6) 0.0154(4) 0.000 -0.0027(3) 0.000 Ni2 0.0294(4) 0.1012(6) 0.0212(4) 0.0081(4) 0.0003(3) -0.0116(3) N1 0.0163(13) 0.065(2) 0.0211(16) 0.0004(14) -0.0043(11) -0.0031(12) N2 0.0185(13) 0.077(2) 0.0181(16) -0.0001(15) -0.0031(11) 0.0005(13) N3 0.0194(14) 0.082(2) 0.0220(17) 0.0039(16) -0.0012(12) -0.0028(14) N4 0.0271(15) 0.104(3) 0.0239(18) 0.0089(18) 0.0016(13) -0.0109(17) N6 0.0333(17) 0.096(3) 0.0282(19) 0.0059(19) -0.0004(14) -0.0038(18) N7 0.0245(15) 0.104(3) 0.0259(18) 0.0078(19) -0.0034(13) -0.0073(17) C5 0.0205(16) 0.070(3) 0.0217(19) 0.0024(17) -0.0014(14) -0.0010(15) C2 0.0163(15) 0.067(2) 0.0226(19) 0.0017(17) -0.0024(13) 0.0004(15) C6 0.0215(16) 0.077(3) 0.0212(19) 0.0083(18) -0.0003(14) -0.0002(16) N5 0.0389(18) 0.093(3) 0.030(2) 0.0078(19) 0.0010(15) -0.0121(18) C11 0.0233(17) 0.094(3) 0.0177(18) 0.0093(19) -0.0024(14) -0.0055(18) C10 0.0240(17) 0.091(3) 0.0200(19) 0.005(2) -0.0057(14) -0.0096(18) C31 0.0299(19) 0.095(4) 0.030(2) 0.004(2) 0.0007(16) -0.003(2) C30 0.032(2) 0.111(4) 0.022(2) 0.005(2) 0.0013(16) -0.005(2) C9 0.0138(15) 0.073(3) 0.0235(19) 0.0023(17) -0.0030(13) -0.0022(15) C29 0.0243(17) 0.105(4) 0.020(2) 0.002(2) 0.0020(15) -0.0063(19) C1 0.0129(15) 0.071(3) 0.027(2) 0.0044(18) -0.0042(13) 0.0039(15) C14 0.0292(18) 0.083(3) 0.025(2) 0.014(2) -0.0059(15) -0.0088(18) C77 0.0226(18) 0.109(4) 0.021(2) -0.002(2) -0.0055(15) 0.016(2) C4 0.0198(16) 0.081(3) 0.0166(18) 0.0013(17) -0.0035(13) 0.0010(16) C26 0.0267(18) 0.118(4) 0.022(2) -0.005(2) 0.0018(16) -0.009(2) C58 0.038(2) 0.063(3) 0.022(2) 0.0083(17) -0.0037(15) -0.0053(18) C34 0.0265(18) 0.094(3) 0.032(2) 0.009(2) -0.0040(16) -0.0122(19) C8 0.0156(15) 0.085(3) 0.027(2) -0.0064(19) 0.0002(14) -0.0031(16) C72 0.0168(16) 0.096(3) 0.0194(19) 0.0037(19) -0.0013(13) -0.0039(18) C25 0.029(2) 0.107(4) 0.038(3) -0.014(3) 0.0014(18) -0.005(2) C3 0.0180(15) 0.073(3) 0.0204(18) 0.0034(17) -0.0067(13) 0.0007(15) C12 0.0244(17) 0.090(3) 0.0209(19) 0.010(2) -0.0031(14) -0.0068(18) C7 0.0195(16) 0.084(3) 0.0214(19) 0.0036(18) -0.0007(14) -0.0066(17) C73 0.0283(19) 0.097(4) 0.030(2) 0.008(2) -0.0026(16) -0.010(2) C59 0.043(2) 0.057(2) 0.027(2) 0.0058(18) -0.0015(16) -0.0029(18) C15 0.043(2) 0.080(3) 0.025(2) 0.004(2) 0.0003(17) -0.011(2) C63 0.063(3) 0.057(3) 0.026(2) 0.0010(18) -0.0021(19) -0.010(2) C28 0.034(2) 0.107(4) 0.023(2) 0.002(2) 0.0042(16) -0.006(2) C74 0.034(2) 0.117(4) 0.036(3) -0.002(3) 0.0004(18) -0.021(3) C32 0.034(2) 0.092(3) 0.027(2) 0.006(2) 0.0015(16) -0.010(2) C13 0.0249(17) 0.086(3) 0.028(2) 0.013(2) 0.0007(15) -0.0034(18) C78 0.019(2) 0.217(9) 0.041(3) -0.010(4) -0.0024(19) -0.020(3) C49 0.039(2) 0.074(3) 0.036(2) 0.006(2) 0.0116(18) 0.0077(19) C16 0.040(2) 0.081(3) 0.029(2) 0.009(2) 0.0012(17) -0.004(2) C24 0.031(2) 0.124(5) 0.027(2) 0.011(3) -0.0014(17) -0.005(2) C35 0.033(2) 0.112(4) 0.029(2) 0.000(2) -0.0030(17) -0.006(2) C27 0.0293(19) 0.110(4) 0.033(2) -0.007(2) 0.0064(17) 0.005(2) C60 0.040(2) 0.059(3) 0.033(2) 0.0095(19) -0.0031(17) 0.0029(18) C19 0.054(3) 0.094(4) 0.026(2) 0.006(2) 0.0072(19) -0.018(2) C36 0.033(2) 0.092(4) 0.033(2) 0.007(2) -0.0098(17) -0.008(2) C75 0.020(2) 0.176(7) 0.024(2) 0.001(3) -0.0008(16) -0.009(3) C61 0.045(2) 0.068(3) 0.040(3) 0.009(2) 0.0031(19) 0.004(2) C33 0.033(2) 0.090(3) 0.035(2) 0.010(2) 0.0010(17) -0.013(2) C38 0.042(2) 0.094(4) 0.047(3) 0.015(3) -0.017(2) -0.012(2) C21 0.055(3) 0.085(3) 0.033(2) 0.004(2) 0.014(2) -0.020(2) C76 0.0218(19) 0.129(5) 0.040(3) -0.010(3) 0.0002(18) 0.009(2) C62 0.055(3) 0.057(3) 0.036(2) 0.0063(19) 0.008(2) 0.0036(19) C40 0.051(2) 0.084(3) 0.028(2) -0.001(2) -0.0056(19) -0.012(2) C68 0.040(2) 0.091(4) 0.035(2) 0.011(2) -0.0038(18) -0.005(2) C20 0.046(2) 0.095(4) 0.027(2) 0.007(2) 0.0025(18) -0.005(2) C17 0.048(2) 0.084(3) 0.037(3) 0.015(2) 0.0042(19) -0.006(2) C42 0.052(2) 0.089(4) 0.027(2) -0.008(2) 0.0080(19) 0.002(2) C37 0.048(3) 0.105(4) 0.038(3) 0.010(3) -0.013(2) -0.022(3) C79 0.050(3) 0.075(3) 0.072(4) 0.008(3) -0.006(2) -0.015(2) C39 0.043(2) 0.127(5) 0.043(3) 0.008(3) -0.012(2) -0.003(3) C80 0.041(2) 0.094(4) 0.064(4) -0.007(3) -0.006(2) 0.018(2) C54 0.080(4) 0.088(4) 0.032(3) 0.013(3) 0.003(2) 0.006(3) C48 0.071(3) 0.077(3) 0.044(3) -0.005(2) 0.019(2) -0.011(3) C69 0.043(3) 0.140(6) 0.051(3) -0.007(4) -0.013(2) -0.005(3) C18 0.055(3) 0.092(4) 0.041(3) 0.020(3) 0.008(2) -0.002(3) C23 0.043(2) 0.079(3) 0.061(3) -0.003(3) 0.030(2) 0.000(2) C44 0.044(2) 0.088(4) 0.042(3) 0.003(2) 0.005(2) -0.002(2) C64 0.076(3) 0.065(3) 0.043(3) 0.001(2) 0.013(2) 0.002(2) C71 0.066(3) 0.120(5) 0.040(3) 0.017(3) -0.010(2) -0.014(3) C22 0.039(2) 0.108(4) 0.044(3) 0.020(3) 0.008(2) 0.008(3) C57 0.211(11) 0.146(8) 0.047(4) -0.004(4) 0.059(6) 0.001(7) C46 0.058(3) 0.080(4) 0.051(3) 0.005(3) 0.008(2) -0.003(2) C45 0.054(3) 0.077(3) 0.047(3) 0.002(2) 0.011(2) 0.000(2) C41 0.073(4) 0.100(5) 0.060(4) -0.007(3) -0.009(3) -0.025(3) C43 0.076(4) 0.083(4) 0.048(3) -0.001(3) -0.003(3) 0.015(3) C47 0.072(3) 0.073(3) 0.059(3) 0.017(3) 0.010(3) -0.002(3) C65 0.151(7) 0.082(4) 0.046(3) -0.001(3) 0.042(4) 0.013(4) C70 0.051(3) 0.107(5) 0.065(4) -0.012(3) -0.004(3) -0.016(3) C50 0.091(4) 0.068(4) 0.067(4) -0.004(3) 0.006(3) -0.011(3) C67 0.120(6) 0.082(4) 0.078(5) -0.009(4) 0.032(4) -0.013(4) C52 0.130(7) 0.097(6) 0.129(8) -0.041(5) 0.014(6) 0.011(5) C55 0.090(5) 0.144(7) 0.072(5) 0.013(5) 0.015(4) -0.004(5) C66 0.070(4) 0.159(8) 0.104(6) -0.039(6) 0.019(4) 0.035(4) C56 0.124(6) 0.149(7) 0.055(4) 0.007(4) 0.031(4) -0.027(6) C51 0.089(5) 0.136(7) 0.101(6) -0.039(5) -0.013(4) 0.006(5) C53 0.225(12) 0.083(5) 0.185(11) -0.047(6) 0.112(10) -0.064(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 '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 N1 178.5(2) . 2 ? N2 Ni1 N1 89.94(13) . 2 ? N2 Ni1 N1 90.06(13) . . ? N2 Ni1 N1 89.94(13) 2 . ? N2 Ni1 N1 90.06(13) 2 2 ? N2 Ni1 N2 179.7(2) . 2 ? N4 Ni2 N6 178.2(2) . . ? N4 Ni2 N7 89.95(16) . . ? N4 Ni2 N5 89.67(17) . . ? N6 Ni2 N7 90.96(16) . . ? N6 Ni2 N5 89.48(16) . . ? N5 Ni2 N7 177.94(19) . . ? C5 N1 Ni1 127.8(2) . . ? C5 N1 C2 105.5(3) . . ? C2 N1 Ni1 126.4(3) . . ? C6 N2 Ni1 126.4(2) . . ? C6 N2 C9 103.9(3) . . ? C9 N2 Ni1 129.6(3) . . ? C5 N3 C12 121.6(3) . . ? C6 N3 C5 121.0(3) . . ? C6 N3 C12 117.1(3) . . ? C11 N4 Ni2 126.0(3) . . ? C11 N4 C14 105.0(3) . . ? C14 N4 Ni2 129.1(3) . . ? C24 N6 Ni2 127.1(4) . . ? C24 N6 C21 106.0(4) . . ? C21 N6 Ni2 126.7(3) . . ? C29 N7 Ni2 128.8(3) . . ? C26 N7 Ni2 126.3(3) . . ? C26 N7 C29 104.6(4) . . ? N1 C5 N3 122.3(3) . . ? N1 C5 C4 112.3(3) . . ? N3 C5 C4 125.3(3) . . ? N1 C2 C3 108.3(3) . . ? C1 C2 N1 125.2(3) . . ? C1 C2 C3 125.7(3) . . ? N2 C6 N3 124.8(3) . . ? N2 C6 C7 113.9(3) . . ? N3 C6 C7 121.3(3) . . ? C16 N5 Ni2 127.7(3) . . ? C16 N5 C19 104.5(4) . . ? C19 N5 Ni2 127.8(3) . . ? N4 C11 C10 128.5(3) . . ? N4 C11 C12 109.6(3) . . ? C10 C11 C12 121.8(4) . . ? C11 C10 C7 115.4(3) . . ? C29 C10 C11 119.3(4) . . ? C29 C10 C7 125.1(4) . . ? C30 C31 C32 122.8(4) . . ? C31 C30 C25 120.7(4) . . ? C31 C30 C35 118.5(4) . . ? C35 C30 C25 120.8(4) . . ? C1 C9 N2 122.0(3) 2 . ? C1 C9 C8 127.0(3) 2 . ? C8 C9 N2 110.6(3) . . ? N7 C29 C28 111.2(4) . . ? C10 C29 N7 124.1(4) . . ? C10 C29 C28 124.4(4) . . ? C2 C1 C9 122.9(3) . 2 ? C2 C1 C72 116.4(3) . . ? C9 C1 C72 120.4(3) 2 . ? N4 C14 C13 111.3(4) . . ? C15 C14 N4 124.8(4) . . ? C15 C14 C13 123.8(4) . . ? C72 C77 C80 122.2(4) . . ? C76 C77 C72 118.3(5) . . ? C76 C77 C80 119.5(5) . . ? C3 C4 C5 105.8(3) . . ? N7 C26 C25 124.6(5) . . ? N7 C26 C27 109.9(4) . . ? C25 C26 C27 125.1(4) . . ? C59 C58 C15 120.2(4) . . ? C59 C58 C63 119.0(4) . . ? C63 C58 C15 120.8(4) . . ? C35 C34 C36 117.9(4) . . ? C33 C34 C35 118.8(4) . . ? C33 C34 C36 123.3(4) . . ? C7 C8 C9 108.0(3) . . ? C77 C72 C1 118.5(4) . . ? C73 C72 C1 120.4(4) . . ? C73 C72 C77 120.8(4) . . ? C26 C25 C30 118.7(5) . . ? C24 C25 C30 119.4(4) . . ? C24 C25 C26 121.6(5) . . ? C4 C3 C2 108.0(3) . . ? N3 C12 C11 120.7(4) . . ? C13 C12 N3 131.2(3) . . ? C13 C12 C11 108.0(3) . . ? C10 C7 C6 120.2(3) . . ? C8 C7 C6 103.7(3) . . ? C8 C7 C10 135.8(3) . . ? C72 C73 C74 118.6(5) . . ? C72 C73 C79 122.6(4) . . ? C74 C73 C79 118.7(5) . . ? C60 C59 C58 121.1(4) . . ? C14 C15 C58 120.4(4) . . ? C14 C15 C16 121.6(4) . . ? C16 C15 C58 117.8(4) . . ? C62 C63 C58 121.0(4) . . ? C27 C28 C29 106.4(4) . . ? C75 C74 C73 121.9(6) . . ? C31 C32 C40 120.1(4) . . ? C33 C32 C31 116.4(4) . . ? C33 C32 C40 123.4(4) . . ? C12 C13 C14 106.1(3) . . ? C48 C49 C44 118.5(5) . . ? N5 C16 C15 125.3(4) . . ? N5 C16 C17 110.5(4) . . ? C15 C16 C17 123.6(4) . . ? N6 C24 C25 125.5(4) . . ? N6 C24 C23 107.4(5) . . ? C25 C24 C23 127.2(4) . . ? C34 C35 C30 120.4(5) . . ? C28 C27 C26 107.8(4) . . ? C59 C60 C61 118.9(4) . . ? C59 C60 C68 119.4(4) . . ? C61 C60 C68 121.7(4) . . ? N5 C19 C20 125.7(5) . . ? N5 C19 C18 110.4(4) . . ? C20 C19 C18 123.9(5) . . ? C34 C36 C39 112.1(4) . . ? C38 C36 C34 108.4(4) . . ? C38 C36 C37 110.2(4) . . ? C38 C36 C39 109.7(4) . . ? C37 C36 C34 108.9(3) . . ? C37 C36 C39 107.4(5) . . ? C74 C75 C78 120.1(7) . . ? C74 C75 C76 119.3(4) . . ? C76 C75 C78 120.6(6) . . ? C62 C61 C60 121.8(4) . . ? C34 C33 C32 123.1(5) . . ? N6 C21 C22 108.2(5) . . ? C20 C21 N6 126.7(4) . . ? C20 C21 C22 124.9(5) . . ? C75 C76 C77 121.1(5) . . ? C63 C62 C64 119.5(4) . . ? C61 C62 C63 118.2(4) . . ? C61 C62 C64 122.3(4) . . ? C42 C40 C32 109.0(4) . . ? C42 C40 C41 109.6(4) . . ? C42 C40 C43 108.4(4) . . ? C41 C40 C32 107.5(4) . . ? C43 C40 C32 112.4(4) . . ? C43 C40 C41 110.0(5) . . ? C69 C68 C60 112.2(4) . . ? C69 C68 C71 110.1(5) . . ? C69 C68 C70 107.1(5) . . ? C71 C68 C60 107.5(4) . . ? C71 C68 C70 110.4(5) . . ? C70 C68 C60 109.6(4) . . ? C19 C20 C44 115.7(5) . . ? C21 C20 C19 120.2(5) . . ? C21 C20 C44 123.8(4) . . ? C18 C17 C16 106.9(4) . . ? C48 C54 C55 111.9(5) . . ? C48 C54 C56 108.6(5) . . ? C57 C54 C48 114.8(5) . . ? C57 C54 C55 107.3(7) . . ? C57 C54 C56 107.7(7) . . ? C55 C54 C56 106.0(6) . . ? C49 C48 C54 122.2(5) . . ? C47 C48 C49 119.3(5) . . ? C47 C48 C54 118.0(5) . . ? C17 C18 C19 107.7(5) . . ? C22 C23 C24 109.4(4) . . ? C49 C44 C20 118.9(5) . . ? C45 C44 C49 121.0(5) . . ? C45 C44 C20 119.9(5) . . ? C62 C64 C65 106.9(4) . . ? C62 C64 C66 111.7(5) . . ? C65 C64 C66 105.1(6) . . ? C67 C64 C62 112.4(5) . . ? C67 C64 C65 112.1(6) . . ? C67 C64 C66 108.4(6) . . ? C23 C22 C21 108.6(5) . . ? C45 C46 C47 116.6(5) . . ? C45 C46 C50 121.5(5) . . ? C47 C46 C50 121.8(5) . . ? C46 C45 C44 121.8(5) . . ? C48 C47 C46 122.7(5) . . ? C46 C50 C53 106.3(6) . . ? C52 C50 C46 109.9(6) . . ? C52 C50 C51 108.3(7) . . ? C52 C50 C53 109.7(8) . . ? C51 C50 C46 111.1(6) . . ? C51 C50 C53 111.5(7) . . ? 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 1.904(3) . ? Ni1 N1 1.904(3) 2 ? Ni1 N2 1.895(3) . ? Ni1 N2 1.895(3) 2 ? Ni2 N4 1.906(3) . ? Ni2 N6 1.920(4) . ? Ni2 N7 1.942(4) . ? Ni2 N5 1.939(4) . ? N1 C5 1.340(5) . ? N1 C2 1.402(4) . ? N2 C6 1.333(5) . ? N2 C9 1.420(4) . ? N3 C5 1.377(5) . ? N3 C6 1.363(5) . ? N3 C12 1.410(5) . ? N4 C11 1.389(6) . ? N4 C14 1.389(5) . ? N6 C24 1.383(6) . ? N6 C21 1.398(7) . ? N7 C29 1.399(6) . ? N7 C26 1.379(6) . ? C5 C4 1.409(5) . ? C2 C1 1.372(5) . ? C2 C3 1.423(5) . ? C6 C7 1.443(5) . ? N5 C16 1.378(6) . ? N5 C19 1.382(6) . ? C11 C10 1.395(6) . ? C11 C12 1.428(5) . ? C10 C29 1.378(6) . ? C10 C7 1.443(6) . ? C31 C30 1.381(7) . ? C31 C32 1.409(7) . ? C30 C25 1.478(7) . ? C30 C35 1.412(6) . ? C9 C1 1.391(5) 2 ? C9 C8 1.398(5) . ? C29 C28 1.414(7) . ? C1 C72 1.506(4) . ? C14 C15 1.389(6) . ? C14 C13 1.417(6) . ? C77 C72 1.421(7) . ? C77 C76 1.403(6) . ? C77 C80 1.489(8) . ? C4 C3 1.359(5) . ? C26 C25 1.406(7) . ? C26 C27 1.436(8) . ? C58 C59 1.394(6) . ? C58 C15 1.476(6) . ? C58 C63 1.407(6) . ? C34 C35 1.399(7) . ? C34 C36 1.545(6) . ? C34 C33 1.381(7) . ? C8 C7 1.395(6) . ? C72 C73 1.364(7) . ? C25 C24 1.397(8) . ? C12 C13 1.368(6) . ? C73 C74 1.409(6) . ? C73 C79 1.523(8) . ? C59 C60 1.367(6) . ? C15 C16 1.391(6) . ? C63 C62 1.394(7) . ? C28 C27 1.361(6) . ? C74 C75 1.369(9) . ? C32 C33 1.397(6) . ? C32 C40 1.556(7) . ? C78 C75 1.535(6) . ? C49 C48 1.399(7) . ? C49 C44 1.406(7) . ? C16 C17 1.420(7) . ? C24 C23 1.463(7) . ? C60 C61 1.415(7) . ? C60 C68 1.540(6) . ? C19 C20 1.389(6) . ? C19 C18 1.410(8) . ? C36 C38 1.500(8) . ? C36 C37 1.538(7) . ? C36 C39 1.552(8) . ? C75 C76 1.373(10) . ? C61 C62 1.377(7) . ? C21 C20 1.368(8) . ? C21 C22 1.444(6) . ? C62 C64 1.529(7) . ? C40 C42 1.510(7) . ? C40 C41 1.540(7) . ? C40 C43 1.515(8) . ? C68 C69 1.529(7) . ? C68 C71 1.531(7) . ? C68 C70 1.537(9) . ? C20 C44 1.503(8) . ? C17 C18 1.340(7) . ? C54 C48 1.495(7) . ? C54 C57 1.431(11) . ? C54 C55 1.522(9) . ? C54 C56 1.553(10) . ? C48 C47 1.390(8) . ? C23 C22 1.267(8) . ? C44 C45 1.395(8) . ? C64 C65 1.536(8) . ? C64 C67 1.496(9) . ? C64 C66 1.541(9) . ? C46 C45 1.378(8) . ? C46 C47 1.424(8) . ? C46 C50 1.565(9) . ? C50 C52 1.393(11) . ? C50 C51 1.524(10) . ? C50 C53 1.569(10) . ? 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 -0.217 0.070 0.111 3102 142 ' '