#------------------------------------------------------------------------------ #$Date: 2025-02-12 01:08:47 +0200 (Wed, 12 Feb 2025) $ #$Revision: 297685 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/38/1573887.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_1573887 loop_ _publ_author_name 'Luff, Martin Simon' 'Filipovic, Tin M.' 'Corsei, Celine S.' 'Oppel, Kai' 'Krummenacher, Ivo' 'Bertermann, R\"udiger' 'Finze, Maik' 'Braunschweig, Holger' 'Radius, Udo' _publ_section_title ; Azolium-2-dithiocarboxylates as redox active ligands in nickel chemistry ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC08449G _journal_year 2025 _chemical_formula_moiety '4(C28 H42 N6 Ni S2), C4 H8 O' _chemical_formula_sum 'C116 H176 N24 Ni4 O S8' _chemical_formula_weight 2414.05 _space_group_crystal_system trigonal _space_group_IT_number 148 _space_group_name_Hall '-R 3' _space_group_name_H-M_alt 'R -3 :H' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2024-12-12 deposited with the CCDC. 2025-02-10 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 9 _cell_length_a 41.9148(2) _cell_length_b 41.9148(2) _cell_length_c 19.73740(10) _cell_measurement_reflns_used 48822 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 77.0460 _cell_measurement_theta_min 2.1120 _cell_volume 30030.0(3) _computing_cell_refinement 'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)' _computing_molecular_graphics 'ShelXLe (Huebschle et all, 2011)' _computing_publication_material 'SHELXL-2014/6 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 10.0000 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.983 _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_unetI/netI 0.0179 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.983 _diffrn_reflns_limit_h_max 53 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_k_max 53 _diffrn_reflns_limit_k_min -51 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 67581 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.983 _diffrn_reflns_theta_full 72.000 _diffrn_reflns_theta_max 77.486 _diffrn_reflns_theta_min 3.308 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 2.192 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.77883 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.201 _exptl_crystal_description block _exptl_crystal_F_000 11592 _exptl_crystal_size_max 0.470 _exptl_crystal_size_mid 0.350 _exptl_crystal_size_min 0.240 _refine_diff_density_max 1.162 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.074 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 720 _refine_ls_number_reflns 13943 _refine_ls_number_restraints 15 _refine_ls_restrained_S_all 1.037 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0490 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0845P)^2^+68.7143P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1418 _refine_ls_wR_factor_ref 0.1432 _reflns_Friedel_coverage 0.000 _reflns_number_gt 13223 _reflns_number_total 13943 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc08449g2.cif _cod_data_source_block Compound_2d _cod_database_code 1573887 _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 0.423 _shelx_estimated_absorpt_t_max 0.619 _shelx_res_file ; TITL MaLu120_ref_a.res in R-3 MaLu120_ref_a.res created by SHELXL-2018/3 at 16:36:44 on 22-May-2023 REM Old TITL MaLu120_ref in R3 REM SHELXT solution in R-3 REM R1 0.145, Rweak 0.011, Alpha 0.037, Orientation as input REM Formula found by SHELXT: C56 N12 S4 Ni2 CELL 1.54184 41.9148 41.9148 19.7374 90.000 90.000 120.000 ZERR 36.000 0.0002 0.0002 0.0001 0.000 0.000 0.000 LATT 3 SYMM -Y, X-Y, Z SYMM -X+Y, -X, Z SFAC C H N S NI O UNIT 1044 1584 216 72 36 9 TEMP -173 SIZE 0.24 0.35 0.47 L.S. 10 BOND $H LIST 4 ACTA 144 FMAP 2 PLAN 20 OMIT -4 5 0 OMIT -4 6 0 OMIT 1 14 11 OMIT -1 1 1 OMIT -3 5 1 OMIT 0 12 0 OMIT -13 8 3 OMIT -1 2 0 OMIT 6 7 2 OMIT 1 11 11 OMIT -4 4 4 OMIT 5 21 5 OMIT -7 4 4 OMIT -5 19 0 OMIT -1 17 0 OMIT -2 7 0 OMIT 3 4 2 OMIT 7 24 7 WGHT 0.084500 68.714294 FVAR 0.06471 NI01 5 0.373264 0.482205 0.639203 11.00000 0.02229 0.02382 = 0.02780 0.00076 0.00051 0.01013 NI02 5 0.542258 0.431064 0.732593 11.00000 0.03381 0.02433 = 0.02740 0.00442 0.00512 0.00856 SIMU 0.005 O1_9 > C5_9 RIGU 0.002 O1_9 > C5_9 PART -1 10.125 RESI 9 THF AFIX 6 O1 6 0.682070 0.319702 0.775683 10.12500 0.18753 C2 1 0.684169 0.319734 0.703794 10.12500 0.18363 AFIX 23 H2A 2 0.669781 0.294221 0.686408 10.12500 -1.20000 H2B 2 0.710110 0.330031 0.689392 10.12500 -1.20000 AFIX 5 C3 1 0.668660 0.343167 0.675278 10.12500 0.18453 AFIX 23 H3A 2 0.688573 0.366366 0.655684 10.12500 -1.20000 H3B 2 0.650109 0.329546 0.639687 10.12500 -1.20000 AFIX 5 C4 1 0.650995 0.351109 0.735767 10.12500 0.18478 AFIX 23 H4A 2 0.624293 0.340942 0.728105 10.12500 -1.20000 H4B 2 0.662650 0.377963 0.743680 10.12500 -1.20000 AFIX 5 C5 1 0.657579 0.332129 0.795989 10.12500 0.18798 AFIX 23 H5A 2 0.668360 0.349634 0.834211 10.12500 -1.20000 H5B 2 0.633923 0.310978 0.811192 10.12500 -1.20000 AFIX 6 RESI 0 PART 0 SIMU 0.005 O1_7 > C5_7 RIGU 0.002 O1_7 > C5_7 PART -1 10.25 RESI 7 THF O1 6 0.411965 0.677156 0.641620 10.25000 0.12335 C2 1 0.379142 0.652887 0.677198 10.25000 0.11784 AFIX 23 H2A 2 0.362501 0.663270 0.678517 10.25000 -1.20000 H2B 2 0.385121 0.649750 0.724375 10.25000 -1.20000 AFIX 5 C3 1 0.360199 0.615623 0.640937 10.25000 0.12187 AFIX 23 H3A 2 0.361848 0.596705 0.668304 10.25000 -1.20000 H3B 2 0.333910 0.607365 0.632535 10.25000 -1.20000 AFIX 5 C4 1 0.381012 0.622243 0.574193 10.25000 0.12226 AFIX 23 H4A 2 0.364319 0.617226 0.535163 10.25000 -1.20000 H4B 2 0.392029 0.606205 0.570755 10.25000 -1.20000 AFIX 5 C5 1 0.411036 0.662870 0.575869 10.25000 0.12837 AFIX 23 H5A 2 0.435237 0.665323 0.565134 10.25000 -1.20000 H5B 2 0.405726 0.676851 0.541628 10.25000 -1.20000 AFIX 6 RESI 0 PART 0 SIMU 0.005 O1_8 > C5_8 RIGU 0.002 O1_8 > C5_8 PART -2 10.125 RESI 8 O1 6 0.318709 0.667402 0.493423 10.12500 0.13860 C2 1 0.311834 0.632854 0.467674 10.12500 0.13393 AFIX 23 H2A 2 0.312211 0.633405 0.417526 10.12500 -1.20000 H2B 2 0.287251 0.613122 0.482583 10.12500 -1.20000 AFIX 5 C3 1 0.341650 0.625157 0.494138 10.12500 0.13042 AFIX 23 H3A 2 0.331262 0.604905 0.527729 10.12500 -1.20000 H3B 2 0.352673 0.618305 0.456515 10.12500 -1.20000 AFIX 5 C4 1 0.370375 0.661156 0.527043 10.12500 0.12888 AFIX 23 H4A 2 0.394528 0.670938 0.504260 10.12500 -1.20000 H4B 2 0.373329 0.657376 0.575641 10.12500 -1.20000 AFIX 5 C5 1 0.355394 0.687543 0.518336 10.12500 0.13613 AFIX 23 H5A 2 0.355733 0.699009 0.562382 10.12500 -1.20000 H5B 2 0.371006 0.707363 0.486078 10.12500 -1.20000 AFIX 0 RESI 0 PART 0 RESI 1 CS S1 4 0.332968 0.447430 0.563458 11.00000 0.02940 0.02584 = 0.04139 -0.00306 -0.00812 0.01209 C2 1 0.324156 0.483675 0.545990 11.00000 0.03414 0.03592 = 0.03570 0.00155 -0.00036 0.02218 S3 4 0.352327 0.518033 0.605614 11.00000 0.04396 0.03088 = 0.03193 0.00175 0.00194 0.02294 C4 1 0.303975 0.486190 0.495643 11.00000 0.03743 0.05131 = 0.03546 0.00115 0.00085 0.02988 N5 3 0.285510 0.460890 0.442129 11.00000 0.04099 0.06101 = 0.03549 -0.00385 -0.00456 0.03208 C6 1 0.270188 0.475547 0.398654 11.00000 0.04036 0.08825 = 0.03168 0.00546 0.00338 0.04198 C7 1 0.249860 0.461073 0.340304 11.00000 0.05045 0.10337 = 0.03655 -0.00253 -0.00105 0.05004 AFIX 43 H024 2 0.244575 0.437733 0.323271 11.00000 -1.20000 AFIX 0 C8 1 0.237341 0.482430 0.307249 11.00000 0.07169 0.15381 = 0.03189 0.00257 -0.00322 0.08014 AFIX 43 H02O 2 0.223329 0.473409 0.266823 11.00000 -1.20000 AFIX 0 C9 1 0.244954 0.516084 0.332206 11.00000 0.09249 0.14800 = 0.03489 0.01420 0.00726 0.09874 AFIX 43 H02P 2 0.236103 0.529884 0.308672 11.00000 -1.20000 AFIX 0 C10 1 0.265450 0.530483 0.391508 11.00000 0.07852 0.11277 = 0.04049 0.01567 0.00961 0.07822 AFIX 43 H029 2 0.270572 0.553731 0.408768 11.00000 -1.20000 AFIX 0 C11 1 0.278007 0.509658 0.424155 11.00000 0.05411 0.08555 = 0.03415 0.00932 0.00593 0.05271 N12 3 0.298507 0.516378 0.483109 11.00000 0.06023 0.06828 = 0.03849 0.00355 -0.00023 0.04986 C13 1 0.280400 0.424664 0.432177 11.00000 0.06575 0.08188 = 0.05356 -0.02913 -0.02309 0.05507 AFIX 137 H014 2 0.254067 0.406878 0.427316 11.00000 -1.50000 H017 2 0.290208 0.417952 0.471311 11.00000 -1.50000 H018 2 0.293441 0.424456 0.391117 11.00000 -1.50000 AFIX 0 C14 1 0.294771 0.537708 0.537196 11.00000 0.13825 0.10361 = 0.06757 -0.02499 -0.03573 0.10353 AFIX 137 H02W 2 0.279502 0.547906 0.521620 11.00000 -1.50000 H02X 2 0.319186 0.557860 0.550020 11.00000 -1.50000 H02Y 2 0.283100 0.521770 0.576494 11.00000 -1.50000 AFIX 0 RESI 0 RESI 2 NHC C1 1 0.380799 0.443149 0.667739 11.00000 0.03366 0.03895 = 0.02985 0.00171 0.00091 0.02254 N2 3 0.356275 0.412220 0.701938 11.00000 0.05257 0.04478 = 0.04890 0.01826 0.01618 0.03511 C3 1 0.371061 0.389718 0.713999 11.00000 0.10364 0.07956 = 0.07239 0.03958 0.03395 0.07608 AFIX 43 H012 2 0.359253 0.366616 0.736609 11.00000 -1.20000 AFIX 0 C4 1 0.404872 0.406441 0.688060 11.00000 0.09215 0.09992 = 0.06166 0.03073 0.02279 0.08321 AFIX 43 H01W 2 0.421804 0.397628 0.688780 11.00000 -1.20000 AFIX 0 N5 3 0.410674 0.439174 0.659787 11.00000 0.04629 0.06518 = 0.03656 0.00697 0.00377 0.04201 C6 1 0.444653 0.465623 0.624674 11.00000 0.03301 0.07423 = 0.03293 -0.00756 -0.00134 0.03257 AFIX 13 H6 2 0.440657 0.485045 0.603607 11.00000 -1.20000 AFIX 0 C7 1 0.453778 0.446376 0.568568 11.00000 0.05241 0.08063 = 0.03413 -0.00694 -0.00143 0.04666 AFIX 137 H01A 2 0.473787 0.464862 0.540519 11.00000 -1.50000 H01B 2 0.431919 0.431967 0.540380 11.00000 -1.50000 H01C 2 0.461484 0.429947 0.588799 11.00000 -1.50000 AFIX 0 C8 1 0.476054 0.484006 0.675647 11.00000 0.04526 0.13971 = 0.05019 -0.03834 -0.01457 0.05406 AFIX 137 H026 2 0.497874 0.503724 0.653172 11.00000 -1.50000 H027 2 0.481831 0.465700 0.693720 11.00000 -1.50000 H028 2 0.468644 0.494412 0.712817 11.00000 -1.50000 AFIX 0 C9 1 0.318800 0.402717 0.722373 11.00000 0.04861 0.03572 = 0.05262 0.01431 0.01936 0.02290 AFIX 13 H9 2 0.315386 0.424128 0.711542 11.00000 -1.20000 AFIX 0 C10 1 0.290663 0.369761 0.682265 11.00000 0.06741 0.03433 = 0.08153 0.00315 0.02913 0.01040 AFIX 137 H02A 2 0.265795 0.363957 0.695509 11.00000 -1.50000 H02B 2 0.293794 0.348522 0.691584 11.00000 -1.50000 H02C 2 0.294205 0.375493 0.633767 11.00000 -1.50000 AFIX 0 C11 1 0.313763 0.395864 0.798743 11.00000 0.07393 0.06119 = 0.05764 0.02981 0.03026 0.04106 AFIX 137 H01Y 2 0.289406 0.391563 0.812116 11.00000 -1.50000 H01Z 2 0.332840 0.417430 0.822868 11.00000 -1.50000 H010 2 0.315815 0.374209 0.810187 11.00000 -1.50000 AFIX 0 RESI 0 RESI 3 NHC C1 1 0.412729 0.518550 0.692945 11.00000 0.03207 0.03925 = 0.03089 -0.00609 0.00284 0.01309 N2 3 0.418475 0.518775 0.760679 11.00000 0.03960 0.05385 = 0.03024 -0.01234 -0.00152 0.01843 C3 1 0.451046 0.549521 0.779816 11.00000 0.04856 0.07302 = 0.04153 -0.02829 -0.00767 0.01466 AFIX 43 H025 2 0.460707 0.555591 0.824472 11.00000 -1.20000 AFIX 0 C4 1 0.466313 0.568988 0.724153 11.00000 0.04393 0.06676 = 0.04911 -0.02941 -0.00022 -0.00286 AFIX 43 H01X 2 0.488933 0.591619 0.721327 11.00000 -1.20000 AFIX 0 N5 3 0.442814 0.549874 0.670737 11.00000 0.03701 0.04513 = 0.03651 -0.01403 0.00315 -0.00231 C6 1 0.393498 0.490492 0.808086 11.00000 0.05485 0.06056 = 0.02868 -0.00083 0.00499 0.03119 AFIX 13 H6 2 0.371963 0.471631 0.781574 11.00000 -1.20000 AFIX 0 C7 1 0.411992 0.471162 0.841365 11.00000 0.08970 0.10760 = 0.03884 0.00831 0.00474 0.06737 AFIX 137 H02Q 2 0.394339 0.451555 0.871151 11.00000 -1.50000 H02R 2 0.433158 0.489005 0.868054 11.00000 -1.50000 H02S 2 0.420386 0.460478 0.806315 11.00000 -1.50000 AFIX 0 C8 1 0.379010 0.507267 0.859664 11.00000 0.07867 0.06868 = 0.04835 0.00157 0.02283 0.03856 AFIX 137 H01T 2 0.360715 0.487769 0.888820 11.00000 -1.50000 H01U 2 0.367532 0.519479 0.835859 11.00000 -1.50000 H01V 2 0.399473 0.525333 0.887453 11.00000 -1.50000 AFIX 0 C9 1 0.449064 0.563497 0.600814 11.00000 0.06063 0.04993 = 0.03757 -0.00794 0.01005 -0.01592 AFIX 13 H011 2 0.428348 0.544884 0.572387 11.00000 -1.20000 AFIX 0 C10 1 0.484781 0.567742 0.572872 11.00000 0.06027 0.09952 = 0.06113 -0.02715 0.02961 -0.02882 AFIX 137 H032 2 0.488386 0.577060 0.526325 11.00000 -1.50000 H033 2 0.483537 0.543764 0.573194 11.00000 -1.50000 H034 2 0.505446 0.585137 0.601083 11.00000 -1.50000 AFIX 0 C11 1 0.448091 0.599183 0.598033 11.00000 0.13143 0.04199 = 0.05756 0.00604 0.00571 -0.00845 AFIX 137 H02Z 2 0.451529 0.607972 0.551130 11.00000 -1.50000 H030 2 0.467869 0.617754 0.626359 11.00000 -1.50000 H031 2 0.424248 0.594867 0.614814 11.00000 -1.50000 AFIX 0 RESI 0 RESI 4 CS S1 4 0.505152 0.406085 0.818681 11.00000 0.03166 0.03295 = 0.02470 0.00146 0.00122 0.00233 C2 1 0.469014 0.379407 0.761360 11.00000 0.03756 0.02461 = 0.02317 0.00167 -0.00158 0.01075 S3 4 0.491486 0.390439 0.681216 11.00000 0.04176 0.03274 = 0.02419 0.00266 0.00137 0.01173 C4 1 0.433238 0.356596 0.774725 11.00000 0.03605 0.02379 = 0.02629 0.00111 -0.00575 0.01070 N5 3 0.405506 0.332422 0.728846 11.00000 0.04427 0.02787 = 0.03357 0.00177 -0.01436 0.00840 C6 1 0.371287 0.316775 0.759856 11.00000 0.03768 0.02635 = 0.05416 0.01275 -0.01404 0.00758 C7 1 0.336268 0.293771 0.734958 11.00000 0.05171 0.03615 = 0.07683 0.01404 -0.03245 0.00446 AFIX 43 H020 2 0.332425 0.284204 0.690201 11.00000 -1.20000 AFIX 0 C8 1 0.306451 0.285110 0.778953 11.00000 0.03221 0.04245 = 0.12458 0.03417 -0.02366 -0.00063 AFIX 43 H02M 2 0.282036 0.269676 0.763030 11.00000 -1.20000 AFIX 0 C9 1 0.311686 0.298294 0.843860 11.00000 0.03191 0.05006 = 0.10512 0.03253 -0.00138 0.00875 AFIX 43 H02N 2 0.290912 0.292020 0.871802 11.00000 -1.20000 AFIX 0 C10 1 0.347052 0.320807 0.869663 11.00000 0.03437 0.04156 = 0.07441 0.02189 0.00694 0.01249 AFIX 43 H01M 2 0.350857 0.329730 0.914889 11.00000 -1.20000 AFIX 0 C11 1 0.376493 0.329618 0.826306 11.00000 0.03165 0.02662 = 0.05306 0.01218 -0.00376 0.00891 N12 3 0.414137 0.351799 0.836502 11.00000 0.02977 0.03114 = 0.03407 0.00294 0.00109 0.00895 C13 1 0.411655 0.319607 0.665450 11.00000 0.08463 0.05392 = 0.03085 -0.00772 -0.00853 -0.00471 AFIX 137 H02D 2 0.392994 0.293643 0.659150 11.00000 -1.50000 H02E 2 0.436213 0.322174 0.665504 11.00000 -1.50000 H02F 2 0.409956 0.334253 0.628400 11.00000 -1.50000 AFIX 0 C14 1 0.428293 0.374753 0.895614 11.00000 0.04055 0.06779 = 0.04781 -0.01794 0.01063 0.00633 AFIX 137 H01Q 2 0.412546 0.362050 0.934619 11.00000 -1.50000 H01R 2 0.428573 0.397983 0.887820 11.00000 -1.50000 H01S 2 0.453407 0.379869 0.904685 11.00000 -1.50000 AFIX 0 RESI 0 RESI 5 NHC C1 1 0.571899 0.444721 0.652668 11.00000 0.04087 0.02994 = 0.03431 0.00342 0.00716 0.01163 N2 3 0.583178 0.423947 0.618689 11.00000 0.05627 0.03782 = 0.04058 0.00237 0.01431 0.02049 C3 1 0.604775 0.443027 0.562988 11.00000 0.06021 0.05432 = 0.03942 0.00295 0.02039 0.02341 AFIX 43 H3 2 0.615646 0.434176 0.531420 11.00000 -1.20000 AFIX 0 C4 1 0.607313 0.476081 0.562337 11.00000 0.05496 0.04253 = 0.03543 0.00641 0.01730 0.01350 AFIX 43 H4 2 0.620390 0.495263 0.530442 11.00000 -1.20000 AFIX 0 N5 3 0.587165 0.476951 0.617218 11.00000 0.04250 0.03087 = 0.03179 0.00662 0.01051 0.00948 C6 1 0.571725 0.385397 0.635543 11.00000 0.06991 0.04121 = 0.04975 0.00046 0.01069 0.02957 AFIX 13 H6 2 0.558958 0.379491 0.680427 11.00000 -1.20000 AFIX 0 C7 1 0.544556 0.359778 0.582913 11.00000 0.08740 0.03902 = 0.05995 -0.00500 0.00473 0.02971 AFIX 137 H02T 2 0.534105 0.334193 0.597960 11.00000 -1.50000 H02U 2 0.557295 0.363098 0.539618 11.00000 -1.50000 H02V 2 0.524734 0.365511 0.577196 11.00000 -1.50000 AFIX 0 C8 1 0.604812 0.380093 0.641427 11.00000 0.09174 0.06638 = 0.07317 -0.00514 0.01175 0.05297 AFIX 137 H02J 2 0.596777 0.354983 0.656936 11.00000 -1.50000 H02K 2 0.622330 0.397808 0.674071 11.00000 -1.50000 H02L 2 0.616735 0.384057 0.597082 11.00000 -1.50000 AFIX 0 C9 1 0.583311 0.508786 0.634354 11.00000 0.04312 0.02779 = 0.03761 0.00681 0.00423 0.01024 AFIX 13 H9 2 0.564884 0.501431 0.671810 11.00000 -1.20000 AFIX 0 C10 1 0.568842 0.520124 0.573767 11.00000 0.05662 0.05218 = 0.04315 0.01190 0.00336 0.02508 AFIX 137 H01G 2 0.564054 0.539857 0.587179 11.00000 -1.50000 H01H 2 0.545937 0.498881 0.557687 11.00000 -1.50000 H01I 2 0.587209 0.528944 0.537383 11.00000 -1.50000 AFIX 0 C11 1 0.619997 0.540414 0.659890 11.00000 0.05065 0.02998 = 0.06071 0.00695 -0.00183 0.00902 AFIX 137 H01D 2 0.617258 0.561814 0.669982 11.00000 -1.50000 H01E 2 0.638900 0.547000 0.624964 11.00000 -1.50000 H01F 2 0.627349 0.532700 0.701091 11.00000 -1.50000 AFIX 0 RESI 0 RESI 6 NHC C1 1 0.580008 0.468317 0.786593 11.00000 0.03350 0.02729 = 0.03272 0.00600 0.00637 0.00949 N2 3 0.578018 0.495794 0.820364 11.00000 0.03331 0.03130 = 0.04035 -0.00337 -0.00089 0.00973 C3 1 0.610850 0.518095 0.853740 11.00000 0.03844 0.03238 = 0.05074 -0.00829 -0.00564 0.00790 AFIX 43 H3 2 0.616326 0.538964 0.880812 11.00000 -1.20000 AFIX 0 C4 1 0.633530 0.504918 0.840954 11.00000 0.03411 0.03861 = 0.04890 -0.00165 -0.00250 0.01084 AFIX 43 H4 2 0.658020 0.514658 0.857074 11.00000 -1.20000 AFIX 0 N5 3 0.614472 0.474516 0.799916 11.00000 0.03504 0.03376 = 0.03883 0.00420 0.00468 0.01264 C6 1 0.546138 0.501591 0.822531 11.00000 0.03754 0.03643 = 0.05153 -0.01010 -0.00277 0.01465 AFIX 13 H6 2 0.526619 0.482894 0.792231 11.00000 -1.20000 AFIX 0 C7 1 0.530677 0.495088 0.894300 11.00000 0.05115 0.06108 = 0.05812 -0.01167 0.00648 0.02763 AFIX 137 H021 2 0.508897 0.498008 0.895176 11.00000 -1.50000 H022 2 0.549415 0.512993 0.925108 11.00000 -1.50000 H023 2 0.523779 0.470083 0.908750 11.00000 -1.50000 AFIX 0 C8 1 0.556245 0.539707 0.796243 11.00000 0.05138 0.03908 = 0.06864 -0.01209 -0.00929 0.02240 AFIX 137 H01N 2 0.534216 0.542207 0.795619 11.00000 -1.50000 H01O 2 0.566176 0.542858 0.750234 11.00000 -1.50000 H01P 2 0.574839 0.558558 0.825980 11.00000 -1.50000 AFIX 0 C9 1 0.630418 0.452956 0.771501 11.00000 0.04897 0.05073 = 0.03812 0.00405 0.00810 0.02809 AFIX 13 H9 2 0.610763 0.431964 0.745079 11.00000 -1.20000 AFIX 0 C10 1 0.643029 0.437081 0.827968 11.00000 0.08544 0.08128 = 0.04731 0.00730 0.00882 0.06062 AFIX 137 H02G 2 0.652242 0.421757 0.808302 11.00000 -1.50000 H02H 2 0.622230 0.422033 0.858045 11.00000 -1.50000 H02I 2 0.662737 0.457232 0.853920 11.00000 -1.50000 AFIX 0 C11 1 0.661553 0.476895 0.723108 11.00000 0.04568 0.06669 = 0.04950 0.00551 0.01198 0.02734 AFIX 137 H01J 2 0.671865 0.462429 0.703891 11.00000 -1.50000 H01K 2 0.680841 0.498080 0.747732 11.00000 -1.50000 H01L 2 0.652018 0.485602 0.686516 11.00000 -1.50000 RESI 0 AFIX 0 HKLF 4 REM MaLu120_ref_a.res in R-3 REM wR2 = 0.143183, GooF = S = 1.03762, Restrained GooF = 1.03738 for all data REM R1 = 0.048963 for 13223 Fo > 4sig(Fo) and 0.050657 for all 13943 data REM 720 parameters refined using 15 restraints END WGHT 0.0838 68.5653 REM Highest difference peak 1.162, deepest hole -0.468, 1-sigma level 0.074 Q1 1 0.4125 0.6667 0.5320 11.00000 0.05 1.16 Q2 1 0.3828 0.6429 0.6318 11.00000 0.05 0.93 Q3 1 0.3333 0.6667 0.4189 10.33333 0.05 0.87 Q4 1 0.4178 0.6612 0.6059 11.00000 0.05 0.85 Q5 1 0.6667 0.3333 0.6213 10.33333 0.05 0.71 Q6 1 0.3822 0.6418 0.5599 11.00000 0.05 0.71 Q7 1 0.4384 0.6799 0.5867 11.00000 0.05 0.68 Q8 1 0.3253 0.4608 0.5612 11.00000 0.05 0.67 Q9 1 0.6667 0.3333 0.8333 10.16667 0.05 0.56 Q10 1 0.3333 0.6667 0.5154 10.33333 0.05 0.54 Q11 1 0.3195 0.5563 0.5088 11.00000 0.05 0.54 Q12 1 0.2083 0.4045 0.3821 11.00000 0.05 0.53 Q13 1 0.6667 0.3333 0.7175 10.33333 0.05 0.51 Q14 1 0.4954 0.4185 0.8245 11.00000 0.05 0.51 Q15 1 0.5448 0.4403 0.7700 11.00000 0.05 0.48 Q16 1 0.2939 0.6243 0.4932 11.00000 0.05 0.48 Q17 1 0.6735 0.3245 0.7246 11.00000 0.05 0.47 Q18 1 0.3341 0.5000 0.5804 11.00000 0.05 0.47 Q19 1 0.3185 0.6293 0.4431 11.00000 0.05 0.47 Q20 1 0.6462 0.3448 0.7886 11.00000 0.05 0.37 ; _shelx_res_checksum 50439 loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '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' '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' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-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' '-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' 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 Ni01 Ni 0.37326(2) 0.48221(2) 0.63920(2) 0.02525(9) Uani 1 1 d . . . . . Ni02 Ni 0.54226(2) 0.43106(2) 0.73259(2) 0.03117(10) Uani 1 1 d . . . . . O1_9 O 0.6821(14) 0.3197(15) 0.776(2) 0.188(12) Uiso 0.125 1 d G U P A -1 C2_9 C 0.684(2) 0.3197(19) 0.704(2) 0.184(12) Uiso 0.125 1 d G U P A -1 H2A_9 H 0.669781 0.294221 0.686408 0.220 Uiso 0.125 1 calc R U P A -1 H2B_9 H 0.710110 0.330031 0.689392 0.220 Uiso 0.125 1 calc R U P A -1 C3_9 C 0.669(2) 0.3432(18) 0.6753(17) 0.185(12) Uiso 0.125 1 d G U P A -1 H3A_9 H 0.688573 0.366366 0.655684 0.221 Uiso 0.125 1 calc R U P A -1 H3B_9 H 0.650109 0.329546 0.639687 0.221 Uiso 0.125 1 calc R U P A -1 C4_9 C 0.651(2) 0.351(3) 0.736(2) 0.185(12) Uiso 0.125 1 d G U P A -1 H4A_9 H 0.624293 0.340942 0.728105 0.222 Uiso 0.125 1 calc R U P A -1 H4B_9 H 0.662650 0.377963 0.743680 0.222 Uiso 0.125 1 calc R U P A -1 C5_9 C 0.6576(19) 0.332(2) 0.7960(16) 0.188(12) Uiso 0.125 1 d G U P A -1 H5A_9 H 0.668360 0.349634 0.834211 0.226 Uiso 0.125 1 calc R U P A -1 H5B_9 H 0.633923 0.310978 0.811192 0.226 Uiso 0.125 1 calc R U P A -1 O1_7 O 0.4120(4) 0.6772(3) 0.6416(8) 0.123(4) Uiso 0.25 1 d G U P B -1 C2_7 C 0.3791(4) 0.6529(4) 0.6772(7) 0.118(4) Uiso 0.25 1 d G U P B -1 H2A_7 H 0.362501 0.663270 0.678517 0.141 Uiso 0.25 1 calc R U P B -1 H2B_7 H 0.385121 0.649750 0.724375 0.141 Uiso 0.25 1 calc R U P B -1 C3_7 C 0.3602(4) 0.6156(4) 0.6409(9) 0.122(4) Uiso 0.25 1 d G U P B -1 H3A_7 H 0.361848 0.596705 0.668304 0.146 Uiso 0.25 1 calc R U P B -1 H3B_7 H 0.333910 0.607365 0.632535 0.146 Uiso 0.25 1 calc R U P B -1 C4_7 C 0.3810(5) 0.6222(4) 0.5742(8) 0.122(4) Uiso 0.25 1 d G U P B -1 H4A_7 H 0.364319 0.617226 0.535163 0.147 Uiso 0.25 1 calc R U P B -1 H4B_7 H 0.392029 0.606205 0.570755 0.147 Uiso 0.25 1 calc R U P B -1 C5_7 C 0.4110(5) 0.6629(5) 0.5759(7) 0.128(4) Uiso 0.25 1 d G U P B -1 H5A_7 H 0.435237 0.665323 0.565134 0.154 Uiso 0.25 1 calc R U P B -1 H5B_7 H 0.405726 0.676851 0.541628 0.154 Uiso 0.25 1 calc R U P B -1 O1_8 O 0.3187(8) 0.6674(9) 0.4934(15) 0.139(8) Uiso 0.125 1 d G U P C -2 C2_8 C 0.3118(8) 0.6329(10) 0.4677(18) 0.134(8) Uiso 0.125 1 d G U P C -2 H2A_8 H 0.312211 0.633405 0.417526 0.161 Uiso 0.125 1 calc R U P C -2 H2B_8 H 0.287251 0.613122 0.482583 0.161 Uiso 0.125 1 calc R U P C -2 C3_8 C 0.3416(11) 0.6252(9) 0.494(2) 0.130(8) Uiso 0.125 1 d G U P C -2 H3A_8 H 0.331262 0.604905 0.527729 0.157 Uiso 0.125 1 calc R U P C -2 H3B_8 H 0.352673 0.618305 0.456515 0.157 Uiso 0.125 1 calc R U P C -2 C4_8 C 0.3704(9) 0.6612(11) 0.527(2) 0.129(8) Uiso 0.125 1 d G U P C -2 H4A_8 H 0.394528 0.670938 0.504260 0.155 Uiso 0.125 1 calc R U P C -2 H4B_8 H 0.373329 0.657376 0.575641 0.155 Uiso 0.125 1 calc R U P C -2 C5_8 C 0.3554(8) 0.6875(8) 0.5183(19) 0.136(8) Uiso 0.125 1 d G U P C -2 H5A_8 H 0.355733 0.699009 0.562382 0.163 Uiso 0.125 1 calc R U P C -2 H5B_8 H 0.371006 0.707363 0.486078 0.163 Uiso 0.125 1 calc R U P C -2 S1_1 S 0.33297(2) 0.44743(2) 0.56346(3) 0.03298(12) Uani 1 1 d . . . . . C2_1 C 0.32416(6) 0.48368(6) 0.54599(11) 0.0332(4) Uani 1 1 d . . . . . S3_1 S 0.35233(2) 0.51803(2) 0.60561(3) 0.03371(12) Uani 1 1 d . . . . . C4_1 C 0.30398(6) 0.48619(7) 0.49564(12) 0.0380(5) Uani 1 1 d . . . . . N5_1 N 0.28551(6) 0.46089(6) 0.44213(10) 0.0429(5) Uani 1 1 d . . . . . C6_1 C 0.27019(7) 0.47555(9) 0.39865(12) 0.0491(6) Uani 1 1 d . . . . . C7_1 C 0.24986(8) 0.46107(11) 0.34030(14) 0.0583(8) Uani 1 1 d . . . . . H024_1 H 0.244575 0.437733 0.323271 0.070 Uiso 1 1 calc R U . . . C8_1 C 0.23734(10) 0.48243(13) 0.30725(15) 0.0752(11) Uani 1 1 d . . . . . H02O_1 H 0.223329 0.473409 0.266823 0.090 Uiso 1 1 calc R U . . . C9_1 C 0.24495(11) 0.51608(13) 0.33221(15) 0.0746(11) Uani 1 1 d . . . . . H02P_1 H 0.236103 0.529884 0.308672 0.090 Uiso 1 1 calc R U . . . C10_1 C 0.26545(10) 0.53048(11) 0.39151(15) 0.0637(9) Uani 1 1 d . . . . . H029_1 H 0.270572 0.553731 0.408768 0.076 Uiso 1 1 calc R U . . . C11_1 C 0.27801(8) 0.50966(9) 0.42416(13) 0.0500(6) Uani 1 1 d . . . . . N12_1 N 0.29851(7) 0.51638(7) 0.48311(11) 0.0478(5) Uani 1 1 d . . . . . C13_1 C 0.28040(9) 0.42466(9) 0.43218(16) 0.0590(8) Uani 1 1 d . . . . . H014_1 H 0.254067 0.406878 0.427316 0.088 Uiso 1 1 calc R U . . . H017_1 H 0.290208 0.417952 0.471311 0.088 Uiso 1 1 calc R U . . . H018_1 H 0.293441 0.424456 0.391117 0.088 Uiso 1 1 calc R U . . . C14_1 C 0.29477(14) 0.53771(12) 0.53720(19) 0.0840(13) Uani 1 1 d . . . . . H02W_1 H 0.279502 0.547906 0.521620 0.126 Uiso 1 1 calc R U . . . H02X_1 H 0.319186 0.557860 0.550020 0.126 Uiso 1 1 calc R U . . . H02Y_1 H 0.283100 0.521770 0.576494 0.126 Uiso 1 1 calc R U . . . C1_2 C 0.38080(6) 0.44315(6) 0.66774(11) 0.0322(4) Uani 1 1 d . . . . . N2_2 N 0.35627(6) 0.41222(6) 0.70194(11) 0.0440(5) Uani 1 1 d . . . . . C3_2 C 0.37106(11) 0.38972(10) 0.71400(18) 0.0717(10) Uani 1 1 d . . . . . H012_2 H 0.359253 0.366616 0.736609 0.086 Uiso 1 1 calc R U . . . C4_2 C 0.40487(11) 0.40644(11) 0.68806(17) 0.0689(10) Uani 1 1 d . . . . . H01W_2 H 0.421804 0.397628 0.688780 0.083 Uiso 1 1 calc R U . . . N5_2 N 0.41067(6) 0.43917(7) 0.65979(10) 0.0431(5) Uani 1 1 d . . . . . C6_2 C 0.44465(6) 0.46562(8) 0.62467(12) 0.0442(6) Uani 1 1 d . . . . . H6_2 H 0.440657 0.485045 0.603607 0.053 Uiso 1 1 calc R U . . . C7_2 C 0.45378(8) 0.44638(9) 0.56857(13) 0.0498(6) Uani 1 1 d . . . . . H01A_2 H 0.473787 0.464862 0.540519 0.075 Uiso 1 1 calc R U . . . H01B_2 H 0.431919 0.431967 0.540380 0.075 Uiso 1 1 calc R U . . . H01C_2 H 0.461484 0.429947 0.588799 0.075 Uiso 1 1 calc R U . . . C8_2 C 0.47605(8) 0.48401(13) 0.67565(16) 0.0749(11) Uani 1 1 d . . . . . H026_2 H 0.497874 0.503724 0.653172 0.112 Uiso 1 1 calc R U . . . H027_2 H 0.481831 0.465700 0.693720 0.112 Uiso 1 1 calc R U . . . H028_2 H 0.468644 0.494412 0.712817 0.112 Uiso 1 1 calc R U . . . C9_2 C 0.31880(7) 0.40272(7) 0.72237(14) 0.0448(6) Uani 1 1 d . . . . . H9_2 H 0.315386 0.424128 0.711542 0.054 Uiso 1 1 calc R U . . . C10_2 C 0.29066(10) 0.36976(8) 0.68227(19) 0.0678(9) Uani 1 1 d . . . . . H02A_2 H 0.265795 0.363957 0.695509 0.102 Uiso 1 1 calc R U . . . H02B_2 H 0.293794 0.348522 0.691584 0.102 Uiso 1 1 calc R U . . . H02C_2 H 0.294205 0.375493 0.633767 0.102 Uiso 1 1 calc R U . . . C11_2 C 0.31376(10) 0.39586(9) 0.79874(16) 0.0610(8) Uani 1 1 d . . . . . H01Y_2 H 0.289406 0.391563 0.812116 0.092 Uiso 1 1 calc R U . . . H01Z_2 H 0.332840 0.417430 0.822868 0.092 Uiso 1 1 calc R U . . . H010_2 H 0.315815 0.374209 0.810187 0.092 Uiso 1 1 calc R U . . . C1_3 C 0.41273(6) 0.51855(6) 0.69295(11) 0.0362(5) Uani 1 1 d . . . . . N2_3 N 0.41848(6) 0.51877(6) 0.76068(10) 0.0434(5) Uani 1 1 d . . . . . C3_3 C 0.45105(8) 0.54952(9) 0.77982(15) 0.0614(8) Uani 1 1 d . . . . . H025_3 H 0.460707 0.555591 0.824472 0.074 Uiso 1 1 calc R U . . . C4_3 C 0.46631(8) 0.56899(9) 0.72415(16) 0.0668(9) Uani 1 1 d . . . . . H01X_3 H 0.488933 0.591619 0.721327 0.080 Uiso 1 1 calc R U . . . N5_3 N 0.44281(6) 0.54987(6) 0.67074(11) 0.0497(6) Uani 1 1 d . . . . . C6_3 C 0.39350(8) 0.49049(8) 0.80809(12) 0.0470(6) Uani 1 1 d . . . . . H6_3 H 0.371963 0.471631 0.781574 0.056 Uiso 1 1 calc R U . . . C7_3 C 0.41199(11) 0.47116(12) 0.84136(16) 0.0707(9) Uani 1 1 d . . . . . H02Q_3 H 0.394339 0.451555 0.871151 0.106 Uiso 1 1 calc R U . . . H02R_3 H 0.433158 0.489005 0.868054 0.106 Uiso 1 1 calc R U . . . H02S_3 H 0.420386 0.460478 0.806315 0.106 Uiso 1 1 calc R U . . . C8_3 C 0.37901(10) 0.50727(10) 0.85966(16) 0.0645(8) Uani 1 1 d . . . . . H01T_3 H 0.360715 0.487769 0.888820 0.097 Uiso 1 1 calc R U . . . H01U_3 H 0.367532 0.519479 0.835859 0.097 Uiso 1 1 calc R U . . . H01V_3 H 0.399473 0.525333 0.887453 0.097 Uiso 1 1 calc R U . . . C9_3 C 0.44906(9) 0.56350(8) 0.60081(14) 0.0687(10) Uani 1 1 d . . . . . H011_3 H 0.428348 0.544884 0.572387 0.082 Uiso 1 1 calc R U . . . C10_3 C 0.48478(10) 0.56774(13) 0.57287(19) 0.1042(19) Uani 1 1 d . . . . . H032_3 H 0.488386 0.577060 0.526325 0.156 Uiso 1 1 calc R U . . . H033_3 H 0.483537 0.543764 0.573194 0.156 Uiso 1 1 calc R U . . . H034_3 H 0.505446 0.585137 0.601083 0.156 Uiso 1 1 calc R U . . . C11_3 C 0.44809(14) 0.59918(9) 0.5980(2) 0.1000(17) Uani 1 1 d . . . . . H02Z_3 H 0.451529 0.607972 0.551130 0.150 Uiso 1 1 calc R U . . . H030_3 H 0.467869 0.617754 0.626359 0.150 Uiso 1 1 calc R U . . . H031_3 H 0.424248 0.594867 0.614814 0.150 Uiso 1 1 calc R U . . . S1_4 S 0.50515(2) 0.40608(2) 0.81868(2) 0.03591(13) Uani 1 1 d . . . . . C2_4 C 0.46901(6) 0.37941(5) 0.76136(10) 0.0306(4) Uani 1 1 d . . . . . S3_4 S 0.49149(2) 0.39044(2) 0.68122(3) 0.03596(13) Uani 1 1 d . . . . . C4_4 C 0.43324(6) 0.35660(5) 0.77472(10) 0.0306(4) Uani 1 1 d . . . . . N5_4 N 0.40551(6) 0.33242(5) 0.72885(10) 0.0395(4) Uani 1 1 d . . . . . C6_4 C 0.37129(7) 0.31678(6) 0.75986(14) 0.0431(6) Uani 1 1 d . . . . . C7_4 C 0.33627(8) 0.29377(7) 0.73496(18) 0.0627(9) Uani 1 1 d . . . . . H020_4 H 0.332425 0.284204 0.690201 0.075 Uiso 1 1 calc R U . . . C8_4 C 0.30645(8) 0.28511(8) 0.7790(2) 0.0750(12) Uani 1 1 d . . . . . H02M_4 H 0.282036 0.269676 0.763030 0.090 Uiso 1 1 calc R U . . . C9_4 C 0.31169(8) 0.29829(9) 0.8439(2) 0.0676(10) Uani 1 1 d . . . . . H02N_4 H 0.290912 0.292020 0.871802 0.081 Uiso 1 1 calc R U . . . C10_4 C 0.34705(7) 0.32081(7) 0.86966(17) 0.0530(7) Uani 1 1 d . . . . . H01M_4 H 0.350857 0.329730 0.914889 0.064 Uiso 1 1 calc R U . . . C11_4 C 0.37649(6) 0.32962(6) 0.82631(13) 0.0396(5) Uani 1 1 d . . . . . N12_4 N 0.41414(5) 0.35180(5) 0.83650(10) 0.0344(4) Uani 1 1 d . . . . . C13_4 C 0.41165(11) 0.31961(9) 0.66545(14) 0.0740(11) Uani 1 1 d . . . . . H02D_4 H 0.392994 0.293643 0.659150 0.111 Uiso 1 1 calc R U . . . H02E_4 H 0.436213 0.322174 0.665504 0.111 Uiso 1 1 calc R U . . . H02F_4 H 0.409956 0.334253 0.628400 0.111 Uiso 1 1 calc R U . . . C14_4 C 0.42829(8) 0.37475(9) 0.89561(15) 0.0613(8) Uani 1 1 d . . . . . H01Q_4 H 0.412546 0.362050 0.934619 0.092 Uiso 1 1 calc R U . . . H01R_4 H 0.428573 0.397983 0.887820 0.092 Uiso 1 1 calc R U . . . H01S_4 H 0.453407 0.379869 0.904685 0.092 Uiso 1 1 calc R U . . . C1_5 C 0.57190(7) 0.44472(6) 0.65267(12) 0.0377(5) Uani 1 1 d . . . . . N2_5 N 0.58318(6) 0.42395(6) 0.61869(11) 0.0462(5) Uani 1 1 d . . . . . C3_5 C 0.60477(8) 0.44303(8) 0.56299(14) 0.0536(7) Uani 1 1 d . . . . . H3_5 H 0.615646 0.434176 0.531420 0.064 Uiso 1 1 calc R U . . . C4_5 C 0.60731(8) 0.47608(7) 0.56234(13) 0.0491(6) Uani 1 1 d . . . . . H4_5 H 0.620390 0.495263 0.530442 0.059 Uiso 1 1 calc R U . . . N5_5 N 0.58716(6) 0.47695(5) 0.61722(10) 0.0390(4) Uani 1 1 d . . . . . C6_5 C 0.57173(9) 0.38540(7) 0.63554(15) 0.0528(6) Uani 1 1 d . . . . . H6_5 H 0.558958 0.379491 0.680427 0.063 Uiso 1 1 calc R U . . . C7_5 C 0.54456(10) 0.35978(8) 0.58291(17) 0.0630(8) Uani 1 1 d . . . . . H02T_5 H 0.534105 0.334193 0.597960 0.094 Uiso 1 1 calc R U . . . H02U_5 H 0.557295 0.363098 0.539618 0.094 Uiso 1 1 calc R U . . . H02V_5 H 0.524734 0.365511 0.577196 0.094 Uiso 1 1 calc R U . . . C8_5 C 0.60481(11) 0.38009(10) 0.6414(2) 0.0711(9) Uani 1 1 d . . . . . H02J_5 H 0.596777 0.354983 0.656936 0.107 Uiso 1 1 calc R U . . . H02K_5 H 0.622330 0.397808 0.674071 0.107 Uiso 1 1 calc R U . . . H02L_5 H 0.616735 0.384057 0.597082 0.107 Uiso 1 1 calc R U . . . C9_5 C 0.58331(7) 0.50879(6) 0.63435(12) 0.0395(5) Uani 1 1 d . . . . . H9_5 H 0.564884 0.501431 0.671810 0.047 Uiso 1 1 calc R U . . . C10_5 C 0.56884(8) 0.52012(8) 0.57377(14) 0.0516(6) Uani 1 1 d . . . . . H01G_5 H 0.564054 0.539857 0.587179 0.077 Uiso 1 1 calc R U . . . H01H_5 H 0.545937 0.498881 0.557687 0.077 Uiso 1 1 calc R U . . . H01I_5 H 0.587209 0.528944 0.537383 0.077 Uiso 1 1 calc R U . . . C11_5 C 0.62000(8) 0.54041(7) 0.65989(16) 0.0521(6) Uani 1 1 d . . . . . H01D_5 H 0.617258 0.561814 0.669982 0.078 Uiso 1 1 calc R U . . . H01E_5 H 0.638900 0.547000 0.624964 0.078 Uiso 1 1 calc R U . . . H01F_5 H 0.627349 0.532700 0.701091 0.078 Uiso 1 1 calc R U . . . C1_6 C 0.58001(6) 0.46832(6) 0.78659(11) 0.0337(4) Uani 1 1 d . . . . . N2_6 N 0.57802(5) 0.49579(5) 0.82036(10) 0.0378(4) Uani 1 1 d . . . . . C3_6 C 0.61085(7) 0.51810(7) 0.85374(14) 0.0449(5) Uani 1 1 d . . . . . H3_6 H 0.616326 0.538964 0.880812 0.054 Uiso 1 1 calc R U . . . C4_6 C 0.63353(7) 0.50492(7) 0.84095(13) 0.0438(5) Uani 1 1 d . . . . . H4_6 H 0.658020 0.514658 0.857074 0.053 Uiso 1 1 calc R U . . . N5_6 N 0.61447(5) 0.47452(5) 0.79992(10) 0.0379(4) Uani 1 1 d . . . . . C6_6 C 0.54614(7) 0.50159(7) 0.82253(14) 0.0435(5) Uani 1 1 d . . . . . H6_6 H 0.526619 0.482894 0.792231 0.052 Uiso 1 1 calc R U . . . C7_6 C 0.53068(8) 0.49509(9) 0.89430(16) 0.0570(7) Uani 1 1 d . . . . . H021_6 H 0.508897 0.498008 0.895176 0.085 Uiso 1 1 calc R U . . . H022_6 H 0.549415 0.512993 0.925108 0.085 Uiso 1 1 calc R U . . . H023_6 H 0.523779 0.470083 0.908750 0.085 Uiso 1 1 calc R U . . . C8_6 C 0.55624(8) 0.53971(7) 0.79624(17) 0.0531(6) Uani 1 1 d . . . . . H01N_6 H 0.534216 0.542207 0.795619 0.080 Uiso 1 1 calc R U . . . H01O_6 H 0.566176 0.542858 0.750234 0.080 Uiso 1 1 calc R U . . . H01P_6 H 0.574839 0.558558 0.825980 0.080 Uiso 1 1 calc R U . . . C9_6 C 0.63042(7) 0.45296(7) 0.77150(13) 0.0445(5) Uani 1 1 d . . . . . H9_6 H 0.610763 0.431964 0.745079 0.053 Uiso 1 1 calc R U . . . C10_6 C 0.64303(10) 0.43708(10) 0.82797(16) 0.0629(8) Uani 1 1 d . . . . . H02G_6 H 0.652242 0.421757 0.808302 0.094 Uiso 1 1 calc R U . . . H02H_6 H 0.622230 0.422033 0.858045 0.094 Uiso 1 1 calc R U . . . H02I_6 H 0.662737 0.457232 0.853920 0.094 Uiso 1 1 calc R U . . . C11_6 C 0.66155(8) 0.47689(9) 0.72311(15) 0.0543(7) Uani 1 1 d . . . . . H01J_6 H 0.671865 0.462429 0.703891 0.081 Uiso 1 1 calc R U . . . H01K_6 H 0.680841 0.498080 0.747732 0.081 Uiso 1 1 calc R U . . . H01L_6 H 0.652018 0.485602 0.686516 0.081 Uiso 1 1 calc R U . . . 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 Ni01 0.02229(16) 0.02382(16) 0.02780(18) 0.00076(12) 0.00051(12) 0.01013(13) Ni02 0.03381(19) 0.02433(17) 0.02740(19) 0.00442(13) 0.00512(13) 0.00856(14) S1_1 0.0294(2) 0.0258(2) 0.0414(3) -0.00306(19) -0.00812(19) 0.01209(19) C2_1 0.0341(10) 0.0359(10) 0.0357(11) 0.0015(8) -0.0004(8) 0.0222(9) S3_1 0.0440(3) 0.0309(2) 0.0319(3) 0.00175(18) 0.0019(2) 0.0229(2) C4_1 0.0374(11) 0.0513(13) 0.0355(11) 0.0012(9) 0.0009(9) 0.0299(10) N5_1 0.0410(10) 0.0610(13) 0.0355(10) -0.0039(9) -0.0046(8) 0.0321(10) C6_1 0.0404(12) 0.088(2) 0.0317(11) 0.0055(12) 0.0034(9) 0.0420(14) C7_1 0.0505(15) 0.103(2) 0.0366(13) -0.0025(14) -0.0011(11) 0.0500(17) C8_1 0.072(2) 0.154(4) 0.0319(13) 0.0026(18) -0.0032(13) 0.080(2) C9_1 0.092(2) 0.148(4) 0.0349(14) 0.0142(18) 0.0073(14) 0.099(3) C10_1 0.079(2) 0.113(3) 0.0405(14) 0.0157(15) 0.0096(13) 0.078(2) C11_1 0.0541(15) 0.086(2) 0.0341(12) 0.0093(12) 0.0059(10) 0.0527(15) N12_1 0.0602(13) 0.0683(14) 0.0385(11) 0.0035(10) -0.0002(9) 0.0499(12) C13_1 0.0658(18) 0.082(2) 0.0536(16) -0.0291(15) -0.0231(14) 0.0551(17) C14_1 0.138(4) 0.104(3) 0.068(2) -0.025(2) -0.036(2) 0.104(3) C1_2 0.0337(10) 0.0389(11) 0.0298(10) 0.0017(8) 0.0009(8) 0.0225(9) N2_2 0.0526(12) 0.0448(11) 0.0489(11) 0.0183(9) 0.0162(9) 0.0351(10) C3_2 0.104(3) 0.080(2) 0.072(2) 0.0396(18) 0.0340(19) 0.076(2) C4_2 0.092(2) 0.100(3) 0.0617(18) 0.0307(17) 0.0228(17) 0.083(2) N5_2 0.0463(11) 0.0652(13) 0.0366(10) 0.0070(9) 0.0038(8) 0.0420(11) C6_2 0.0330(11) 0.0742(17) 0.0329(11) -0.0076(11) -0.0013(9) 0.0326(12) C7_2 0.0524(14) 0.0806(19) 0.0341(12) -0.0069(12) -0.0014(10) 0.0467(14) C8_2 0.0453(15) 0.140(3) 0.0502(16) -0.0383(19) -0.0146(13) 0.054(2) C9_2 0.0486(13) 0.0357(11) 0.0526(14) 0.0143(10) 0.0194(11) 0.0229(10) C10_2 0.0674(19) 0.0343(13) 0.082(2) 0.0032(13) 0.0291(17) 0.0104(13) C11_2 0.074(2) 0.0612(17) 0.0576(17) 0.0298(14) 0.0303(15) 0.0411(16) C1_3 0.0321(10) 0.0393(11) 0.0309(10) -0.0061(8) 0.0028(8) 0.0131(9) N2_3 0.0396(10) 0.0538(12) 0.0302(9) -0.0123(8) -0.0015(8) 0.0184(9) C3_3 0.0486(15) 0.0730(19) 0.0415(14) -0.0283(14) -0.0077(11) 0.0147(14) C4_3 0.0439(14) 0.0668(19) 0.0491(16) -0.0294(14) -0.0002(12) -0.0029(13) N5_3 0.0370(10) 0.0451(11) 0.0365(10) -0.0140(9) 0.0032(8) -0.0023(9) C6_3 0.0548(14) 0.0606(15) 0.0287(11) -0.0008(10) 0.0050(10) 0.0312(13) C7_3 0.090(2) 0.108(3) 0.0388(14) 0.0083(16) 0.0047(15) 0.067(2) C8_3 0.079(2) 0.0687(19) 0.0484(16) 0.0016(14) 0.0228(15) 0.0386(17) C9_3 0.0606(17) 0.0499(16) 0.0376(14) -0.0079(11) 0.0100(12) -0.0159(13) C10_3 0.060(2) 0.100(3) 0.061(2) -0.027(2) 0.0296(17) -0.029(2) C11_3 0.131(4) 0.0420(17) 0.058(2) 0.0060(14) 0.006(2) -0.008(2) S1_4 0.0317(2) 0.0329(3) 0.0247(2) 0.00146(18) 0.00122(18) 0.0023(2) C2_4 0.0376(10) 0.0246(9) 0.0232(9) 0.0017(7) -0.0016(8) 0.0107(8) S3_4 0.0418(3) 0.0327(3) 0.0242(2) 0.00266(18) 0.00137(19) 0.0117(2) C4_4 0.0360(10) 0.0238(9) 0.0263(9) 0.0011(7) -0.0057(8) 0.0107(8) N5_4 0.0443(10) 0.0279(8) 0.0336(9) 0.0018(7) -0.0144(8) 0.0084(8) C6_4 0.0377(12) 0.0264(10) 0.0542(14) 0.0128(9) -0.0140(10) 0.0076(9) C7_4 0.0517(16) 0.0362(13) 0.077(2) 0.0140(13) -0.0325(15) 0.0045(12) C8_4 0.0322(13) 0.0424(15) 0.125(3) 0.0342(18) -0.0237(16) -0.0006(11) C9_4 0.0319(13) 0.0501(16) 0.105(3) 0.0325(17) -0.0014(15) 0.0088(12) C10_4 0.0344(12) 0.0416(13) 0.0744(19) 0.0219(13) 0.0069(12) 0.0125(10) C11_4 0.0317(11) 0.0266(10) 0.0531(14) 0.0122(9) -0.0038(9) 0.0089(8) N12_4 0.0298(9) 0.0311(9) 0.0341(9) 0.0029(7) 0.0011(7) 0.0090(7) C13_4 0.085(2) 0.0539(17) 0.0308(13) -0.0077(12) -0.0085(14) -0.0047(16) C14_4 0.0405(13) 0.0678(18) 0.0478(15) -0.0179(13) 0.0106(11) 0.0063(13) C1_5 0.0409(11) 0.0299(10) 0.0343(11) 0.0034(8) 0.0072(9) 0.0116(9) N2_5 0.0563(13) 0.0378(10) 0.0406(11) 0.0024(8) 0.0143(9) 0.0205(9) C3_5 0.0602(16) 0.0543(15) 0.0394(13) 0.0030(11) 0.0204(12) 0.0234(13) C4_5 0.0550(15) 0.0425(13) 0.0354(12) 0.0064(10) 0.0173(11) 0.0135(11) N5_5 0.0425(10) 0.0309(9) 0.0318(9) 0.0066(7) 0.0105(8) 0.0095(8) C6_5 0.0699(18) 0.0412(13) 0.0497(15) 0.0005(11) 0.0107(13) 0.0296(13) C7_5 0.087(2) 0.0390(14) 0.0599(18) -0.0050(12) 0.0047(16) 0.0297(15) C8_5 0.092(2) 0.066(2) 0.073(2) -0.0051(16) 0.0117(18) 0.0530(19) C9_5 0.0431(12) 0.0278(10) 0.0376(11) 0.0068(8) 0.0042(9) 0.0102(9) C10_5 0.0566(15) 0.0522(15) 0.0431(14) 0.0119(11) 0.0034(11) 0.0251(13) C11_5 0.0507(15) 0.0300(11) 0.0607(16) 0.0069(11) -0.0018(12) 0.0090(11) C1_6 0.0335(10) 0.0273(9) 0.0327(10) 0.0060(8) 0.0064(8) 0.0095(8) N2_6 0.0333(9) 0.0313(9) 0.0404(10) -0.0034(7) -0.0009(8) 0.0097(7) C3_6 0.0384(12) 0.0324(11) 0.0507(14) -0.0083(10) -0.0056(10) 0.0079(9) C4_6 0.0341(11) 0.0386(12) 0.0489(13) -0.0017(10) -0.0025(10) 0.0108(10) N5_6 0.0350(9) 0.0338(9) 0.0388(10) 0.0042(7) 0.0047(8) 0.0126(8) C6_6 0.0375(12) 0.0364(11) 0.0515(14) -0.0101(10) -0.0028(10) 0.0147(10) C7_6 0.0511(15) 0.0611(17) 0.0581(17) -0.0117(13) 0.0065(13) 0.0276(14) C8_6 0.0514(15) 0.0391(13) 0.0686(18) -0.0121(12) -0.0093(13) 0.0224(12) C9_6 0.0490(13) 0.0507(14) 0.0381(12) 0.0041(10) 0.0081(10) 0.0281(12) C10_6 0.085(2) 0.081(2) 0.0473(15) 0.0073(14) 0.0088(15) 0.0606(19) C11_6 0.0457(14) 0.0667(17) 0.0495(15) 0.0055(13) 0.0120(12) 0.0273(13) 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' S S 0.3331 0.5567 '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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1_2 Ni01 C1_3 94.11(10) . . ? C1_2 Ni01 S1_1 91.96(7) . . ? C1_3 Ni01 S1_1 170.04(7) . . ? C1_2 Ni01 S3_1 167.86(7) . . ? C1_3 Ni01 S3_1 96.05(8) . . ? S1_1 Ni01 S3_1 78.96(2) . . ? C1_6 Ni02 C1_5 93.87(10) . . ? C1_6 Ni02 S1_4 93.35(6) . . ? C1_5 Ni02 S1_4 170.52(7) . . ? C1_6 Ni02 S3_4 168.98(7) . . ? C1_5 Ni02 S3_4 94.81(7) . . ? S1_4 Ni02 S3_4 78.82(2) . . ? C5_9 O1_9 C2_9 109.7 . . ? O1_9 C2_9 C3_9 108.8 . . ? O1_9 C2_9 H2A_9 109.9 . . ? C3_9 C2_9 H2A_9 109.9 . . ? O1_9 C2_9 H2B_9 109.9 . . ? C3_9 C2_9 H2B_9 109.9 . . ? H2A_9 C2_9 H2B_9 108.3 . . ? C4_9 C3_9 C2_9 105.1 . . ? C4_9 C3_9 H3A_9 110.7 . . ? C2_9 C3_9 H3A_9 110.7 . . ? C4_9 C3_9 H3B_9 110.7 . . ? C2_9 C3_9 H3B_9 110.7 . . ? H3A_9 C3_9 H3B_9 108.8 . . ? C3_9 C4_9 C5_9 105.1 . . ? C3_9 C4_9 H4A_9 110.7 . . ? C5_9 C4_9 H4A_9 110.7 . . ? C3_9 C4_9 H4B_9 110.7 . . ? C5_9 C4_9 H4B_9 110.7 . . ? H4A_9 C4_9 H4B_9 108.8 . . ? O1_9 C5_9 C4_9 108.8 . . ? O1_9 C5_9 H5A_9 109.9 . . ? C4_9 C5_9 H5A_9 109.9 . . ? O1_9 C5_9 H5B_9 109.9 . . ? C4_9 C5_9 H5B_9 109.9 . . ? H5A_9 C5_9 H5B_9 108.3 . . ? C5_7 O1_7 C2_7 109.7 . . ? O1_7 C2_7 C3_7 108.8 . . ? O1_7 C2_7 H2A_7 109.9 . . ? C3_7 C2_7 H2A_7 109.9 . . ? O1_7 C2_7 H2B_7 109.9 . . ? C3_7 C2_7 H2B_7 109.9 . . ? H2A_7 C2_7 H2B_7 108.3 . . ? C4_7 C3_7 C2_7 105.1 . . ? C4_7 C3_7 H3A_7 110.7 . . ? C2_7 C3_7 H3A_7 110.7 . . ? C4_7 C3_7 H3B_7 110.7 . . ? C2_7 C3_7 H3B_7 110.7 . . ? H3A_7 C3_7 H3B_7 108.8 . . ? C3_7 C4_7 C5_7 105.1 . . ? C3_7 C4_7 H4A_7 110.7 . . ? C5_7 C4_7 H4A_7 110.7 . . ? C3_7 C4_7 H4B_7 110.7 . . ? C5_7 C4_7 H4B_7 110.7 . . ? H4A_7 C4_7 H4B_7 108.8 . . ? O1_7 C5_7 C4_7 108.8 . . ? O1_7 C5_7 H5A_7 109.9 . . ? C4_7 C5_7 H5A_7 109.9 . . ? O1_7 C5_7 H5B_7 109.9 . . ? C4_7 C5_7 H5B_7 109.9 . . ? H5A_7 C5_7 H5B_7 108.3 . . ? C5_8 O1_8 C2_8 109.7 . . ? O1_8 C2_8 C3_8 108.8 . . ? O1_8 C2_8 H2A_8 109.9 . . ? C3_8 C2_8 H2A_8 109.9 . . ? O1_8 C2_8 H2B_8 109.9 . . ? C3_8 C2_8 H2B_8 109.9 . . ? H2A_8 C2_8 H2B_8 108.3 . . ? C4_8 C3_8 C2_8 105.1 . . ? C4_8 C3_8 H3A_8 110.7 . . ? C2_8 C3_8 H3A_8 110.7 . . ? C4_8 C3_8 H3B_8 110.7 . . ? C2_8 C3_8 H3B_8 110.7 . . ? H3A_8 C3_8 H3B_8 108.8 . . ? C3_8 C4_8 C5_8 105.1 . . ? C3_8 C4_8 H4A_8 110.7 . . ? C5_8 C4_8 H4A_8 110.7 . . ? C3_8 C4_8 H4B_8 110.7 . . ? C5_8 C4_8 H4B_8 110.7 . . ? H4A_8 C4_8 H4B_8 108.8 . . ? O1_8 C5_8 C4_8 108.8 . . ? O1_8 C5_8 H5A_8 109.9 . . ? C4_8 C5_8 H5A_8 109.9 . . ? O1_8 C5_8 H5B_8 109.9 . . ? C4_8 C5_8 H5B_8 109.9 . . ? H5A_8 C5_8 H5B_8 108.3 . . ? C2_1 S1_1 Ni01 89.09(8) . . ? C4_1 C2_1 S1_1 128.49(18) . . ? C4_1 C2_1 S3_1 128.05(18) . . ? S1_1 C2_1 S3_1 103.17(11) . . ? C2_1 S3_1 Ni01 88.65(7) . . ? C2_1 C4_1 N12_1 126.1(2) . . ? C2_1 C4_1 N5_1 128.4(2) . . ? N12_1 C4_1 N5_1 105.42(19) . . ? C6_1 N5_1 C4_1 109.2(2) . . ? C6_1 N5_1 C13_1 121.8(2) . . ? C4_1 N5_1 C13_1 128.9(2) . . ? C7_1 C6_1 N5_1 130.0(3) . . ? C7_1 C6_1 C11_1 122.0(3) . . ? N5_1 C6_1 C11_1 108.0(2) . . ? C6_1 C7_1 C8_1 116.9(3) . . ? C6_1 C7_1 H024_1 121.5 . . ? C8_1 C7_1 H024_1 121.5 . . ? C9_1 C8_1 C7_1 121.3(3) . . ? C9_1 C8_1 H02O_1 119.4 . . ? C7_1 C8_1 H02O_1 119.4 . . ? C8_1 C9_1 C10_1 121.4(3) . . ? C8_1 C9_1 H02P_1 119.3 . . ? C10_1 C9_1 H02P_1 119.3 . . ? C11_1 C10_1 C9_1 117.6(3) . . ? C11_1 C10_1 H029_1 121.2 . . ? C9_1 C10_1 H029_1 121.2 . . ? C10_1 C11_1 N12_1 130.9(3) . . ? C10_1 C11_1 C6_1 120.8(3) . . ? N12_1 C11_1 C6_1 108.4(2) . . ? C11_1 N12_1 C4_1 109.0(2) . . ? C11_1 N12_1 C14_1 119.7(2) . . ? C4_1 N12_1 C14_1 122.5(2) . . ? N5_1 C13_1 H014_1 109.5 . . ? N5_1 C13_1 H017_1 109.5 . . ? H014_1 C13_1 H017_1 109.5 . . ? N5_1 C13_1 H018_1 109.5 . . ? H014_1 C13_1 H018_1 109.5 . . ? H017_1 C13_1 H018_1 109.5 . . ? N12_1 C14_1 H02W_1 109.5 . . ? N12_1 C14_1 H02X_1 109.5 . . ? H02W_1 C14_1 H02X_1 109.5 . . ? N12_1 C14_1 H02Y_1 109.5 . . ? H02W_1 C14_1 H02Y_1 109.5 . . ? H02X_1 C14_1 H02Y_1 109.5 . . ? N5_2 C1_2 N2_2 104.15(19) . . ? N5_2 C1_2 Ni01 129.38(17) . . ? N2_2 C1_2 Ni01 126.47(16) . . ? C1_2 N2_2 C3_2 110.6(2) . . ? C1_2 N2_2 C9_2 126.05(18) . . ? C3_2 N2_2 C9_2 123.4(2) . . ? C4_2 C3_2 N2_2 107.3(3) . . ? C4_2 C3_2 H012_2 126.4 . . ? N2_2 C3_2 H012_2 126.4 . . ? C3_2 C4_2 N5_2 106.9(2) . . ? C3_2 C4_2 H01W_2 126.6 . . ? N5_2 C4_2 H01W_2 126.6 . . ? C1_2 N5_2 C4_2 111.1(2) . . ? C1_2 N5_2 C6_2 124.7(2) . . ? C4_2 N5_2 C6_2 124.1(2) . . ? N5_2 C6_2 C8_2 109.7(2) . . ? N5_2 C6_2 C7_2 110.4(2) . . ? C8_2 C6_2 C7_2 111.4(2) . . ? N5_2 C6_2 H6_2 108.5 . . ? C8_2 C6_2 H6_2 108.5 . . ? C7_2 C6_2 H6_2 108.5 . . ? C6_2 C7_2 H01A_2 109.5 . . ? C6_2 C7_2 H01B_2 109.5 . . ? H01A_2 C7_2 H01B_2 109.5 . . ? C6_2 C7_2 H01C_2 109.5 . . ? H01A_2 C7_2 H01C_2 109.5 . . ? H01B_2 C7_2 H01C_2 109.5 . . ? C6_2 C8_2 H026_2 109.5 . . ? C6_2 C8_2 H027_2 109.5 . . ? H026_2 C8_2 H027_2 109.5 . . ? C6_2 C8_2 H028_2 109.5 . . ? H026_2 C8_2 H028_2 109.5 . . ? H027_2 C8_2 H028_2 109.5 . . ? N2_2 C9_2 C10_2 110.0(2) . . ? N2_2 C9_2 C11_2 110.5(2) . . ? C10_2 C9_2 C11_2 111.9(2) . . ? N2_2 C9_2 H9_2 108.1 . . ? C10_2 C9_2 H9_2 108.1 . . ? C11_2 C9_2 H9_2 108.1 . . ? C9_2 C10_2 H02A_2 109.5 . . ? C9_2 C10_2 H02B_2 109.5 . . ? H02A_2 C10_2 H02B_2 109.5 . . ? C9_2 C10_2 H02C_2 109.5 . . ? H02A_2 C10_2 H02C_2 109.5 . . ? H02B_2 C10_2 H02C_2 109.5 . . ? C9_2 C11_2 H01Y_2 109.5 . . ? C9_2 C11_2 H01Z_2 109.5 . . ? H01Y_2 C11_2 H01Z_2 109.5 . . ? C9_2 C11_2 H010_2 109.5 . . ? H01Y_2 C11_2 H010_2 109.5 . . ? H01Z_2 C11_2 H010_2 109.5 . . ? N2_3 C1_3 N5_3 103.59(19) . . ? N2_3 C1_3 Ni01 129.13(17) . . ? N5_3 C1_3 Ni01 127.22(17) . . ? C1_3 N2_3 C3_3 111.4(2) . . ? C1_3 N2_3 C6_3 124.9(2) . . ? C3_3 N2_3 C6_3 123.7(2) . . ? C4_3 C3_3 N2_3 107.2(2) . . ? C4_3 C3_3 H025_3 126.4 . . ? N2_3 C3_3 H025_3 126.4 . . ? C3_3 C4_3 N5_3 106.8(2) . . ? C3_3 C4_3 H01X_3 126.6 . . ? N5_3 C4_3 H01X_3 126.6 . . ? C1_3 N5_3 C4_3 111.1(2) . . ? C1_3 N5_3 C9_3 125.3(2) . . ? C4_3 N5_3 C9_3 123.5(2) . . ? N2_3 C6_3 C7_3 111.0(2) . . ? N2_3 C6_3 C8_3 110.0(2) . . ? C7_3 C6_3 C8_3 112.5(2) . . ? N2_3 C6_3 H6_3 107.7 . . ? C7_3 C6_3 H6_3 107.7 . . ? C8_3 C6_3 H6_3 107.7 . . ? C6_3 C7_3 H02Q_3 109.5 . . ? C6_3 C7_3 H02R_3 109.5 . . ? H02Q_3 C7_3 H02R_3 109.5 . . ? C6_3 C7_3 H02S_3 109.5 . . ? H02Q_3 C7_3 H02S_3 109.5 . . ? H02R_3 C7_3 H02S_3 109.5 . . ? C6_3 C8_3 H01T_3 109.5 . . ? C6_3 C8_3 H01U_3 109.5 . . ? H01T_3 C8_3 H01U_3 109.5 . . ? C6_3 C8_3 H01V_3 109.5 . . ? H01T_3 C8_3 H01V_3 109.5 . . ? H01U_3 C8_3 H01V_3 109.5 . . ? N5_3 C9_3 C11_3 109.3(3) . . ? N5_3 C9_3 C10_3 111.1(4) . . ? C11_3 C9_3 C10_3 112.4(3) . . ? N5_3 C9_3 H011_3 107.9 . . ? C11_3 C9_3 H011_3 107.9 . . ? C10_3 C9_3 H011_3 107.9 . . ? C9_3 C10_3 H032_3 109.5 . . ? C9_3 C10_3 H033_3 109.5 . . ? H032_3 C10_3 H033_3 109.5 . . ? C9_3 C10_3 H034_3 109.5 . . ? H032_3 C10_3 H034_3 109.5 . . ? H033_3 C10_3 H034_3 109.5 . . ? C9_3 C11_3 H02Z_3 109.5 . . ? C9_3 C11_3 H030_3 109.5 . . ? H02Z_3 C11_3 H030_3 109.5 . . ? C9_3 C11_3 H031_3 109.5 . . ? H02Z_3 C11_3 H031_3 109.5 . . ? H030_3 C11_3 H031_3 109.5 . . ? C2_4 S1_4 Ni02 89.14(7) . . ? C4_4 C2_4 S1_4 128.57(16) . . ? C4_4 C2_4 S3_4 128.16(16) . . ? S1_4 C2_4 S3_4 103.26(11) . . ? C2_4 S3_4 Ni02 88.45(7) . . ? C2_4 C4_4 N12_4 128.43(19) . . ? C2_4 C4_4 N5_4 127.4(2) . . ? N12_4 C4_4 N5_4 104.15(18) . . ? C6_4 N5_4 C4_4 109.9(2) . . ? C6_4 N5_4 C13_4 123.0(2) . . ? C4_4 N5_4 C13_4 125.9(2) . . ? C7_4 C6_4 N5_4 131.3(3) . . ? C7_4 C6_4 C11_4 120.7(3) . . ? N5_4 C6_4 C11_4 107.93(19) . . ? C6_4 C7_4 C8_4 117.1(3) . . ? C6_4 C7_4 H020_4 121.5 . . ? C8_4 C7_4 H020_4 121.5 . . ? C9_4 C8_4 C7_4 121.9(3) . . ? C9_4 C8_4 H02M_4 119.0 . . ? C7_4 C8_4 H02M_4 119.0 . . ? C8_4 C9_4 C10_4 121.1(3) . . ? C8_4 C9_4 H02N_4 119.5 . . ? C10_4 C9_4 H02N_4 119.5 . . ? C11_4 C10_4 C9_4 117.1(3) . . ? C11_4 C10_4 H01M_4 121.4 . . ? C9_4 C10_4 H01M_4 121.4 . . ? N12_4 C11_4 C10_4 130.5(3) . . ? N12_4 C11_4 C6_4 107.5(2) . . ? C10_4 C11_4 C6_4 122.0(2) . . ? C11_4 N12_4 C4_4 110.04(19) . . ? C11_4 N12_4 C14_4 121.1(2) . . ? C4_4 N12_4 C14_4 126.05(19) . . ? N5_4 C13_4 H02D_4 109.5 . . ? N5_4 C13_4 H02E_4 109.5 . . ? H02D_4 C13_4 H02E_4 109.5 . . ? N5_4 C13_4 H02F_4 109.5 . . ? H02D_4 C13_4 H02F_4 109.5 . . ? H02E_4 C13_4 H02F_4 109.5 . . ? N12_4 C14_4 H01Q_4 109.5 . . ? N12_4 C14_4 H01R_4 109.5 . . ? H01Q_4 C14_4 H01R_4 109.5 . . ? N12_4 C14_4 H01S_4 109.5 . . ? H01Q_4 C14_4 H01S_4 109.5 . . ? H01R_4 C14_4 H01S_4 109.5 . . ? N2_5 C1_5 N5_5 103.92(19) . . ? N2_5 C1_5 Ni02 126.77(17) . . ? N5_5 C1_5 Ni02 129.30(18) . . ? C1_5 N2_5 C3_5 110.9(2) . . ? C1_5 N2_5 C6_5 124.3(2) . . ? C3_5 N2_5 C6_5 124.6(2) . . ? C4_5 C3_5 N2_5 107.1(2) . . ? C4_5 C3_5 H3_5 126.4 . . ? N2_5 C3_5 H3_5 126.4 . . ? C3_5 C4_5 N5_5 106.6(2) . . ? C3_5 C4_5 H4_5 126.7 . . ? N5_5 C4_5 H4_5 126.7 . . ? C1_5 N5_5 C4_5 111.4(2) . . ? C1_5 N5_5 C9_5 125.05(19) . . ? C4_5 N5_5 C9_5 123.51(19) . . ? N2_5 C6_5 C8_5 111.0(3) . . ? N2_5 C6_5 C7_5 109.8(2) . . ? C8_5 C6_5 C7_5 111.5(3) . . ? N2_5 C6_5 H6_5 108.2 . . ? C8_5 C6_5 H6_5 108.2 . . ? C7_5 C6_5 H6_5 108.2 . . ? C6_5 C7_5 H02T_5 109.5 . . ? C6_5 C7_5 H02U_5 109.5 . . ? H02T_5 C7_5 H02U_5 109.5 . . ? C6_5 C7_5 H02V_5 109.5 . . ? H02T_5 C7_5 H02V_5 109.5 . . ? H02U_5 C7_5 H02V_5 109.5 . . ? C6_5 C8_5 H02J_5 109.5 . . ? C6_5 C8_5 H02K_5 109.5 . . ? H02J_5 C8_5 H02K_5 109.5 . . ? C6_5 C8_5 H02L_5 109.5 . . ? H02J_5 C8_5 H02L_5 109.5 . . ? H02K_5 C8_5 H02L_5 109.5 . . ? N5_5 C9_5 C10_5 110.3(2) . . ? N5_5 C9_5 C11_5 110.2(2) . . ? C10_5 C9_5 C11_5 111.9(2) . . ? N5_5 C9_5 H9_5 108.1 . . ? C10_5 C9_5 H9_5 108.1 . . ? C11_5 C9_5 H9_5 108.1 . . ? C9_5 C10_5 H01G_5 109.5 . . ? C9_5 C10_5 H01H_5 109.5 . . ? H01G_5 C10_5 H01H_5 109.5 . . ? C9_5 C10_5 H01I_5 109.5 . . ? H01G_5 C10_5 H01I_5 109.5 . . ? H01H_5 C10_5 H01I_5 109.5 . . ? C9_5 C11_5 H01D_5 109.5 . . ? C9_5 C11_5 H01E_5 109.5 . . ? H01D_5 C11_5 H01E_5 109.5 . . ? C9_5 C11_5 H01F_5 109.5 . . ? H01D_5 C11_5 H01F_5 109.5 . . ? H01E_5 C11_5 H01F_5 109.5 . . ? N5_6 C1_6 N2_6 104.53(19) . . ? N5_6 C1_6 Ni02 129.39(17) . . ? N2_6 C1_6 Ni02 126.07(17) . . ? C1_6 N2_6 C3_6 110.0(2) . . ? C1_6 N2_6 C6_6 126.49(19) . . ? C3_6 N2_6 C6_6 123.5(2) . . ? C4_6 C3_6 N2_6 107.6(2) . . ? C4_6 C3_6 H3_6 126.2 . . ? N2_6 C3_6 H3_6 126.2 . . ? C3_6 C4_6 N5_6 106.8(2) . . ? C3_6 C4_6 H4_6 126.6 . . ? N5_6 C4_6 H4_6 126.6 . . ? C1_6 N5_6 C4_6 111.1(2) . . ? C1_6 N5_6 C9_6 124.9(2) . . ? C4_6 N5_6 C9_6 123.9(2) . . ? N2_6 C6_6 C7_6 109.7(2) . . ? N2_6 C6_6 C8_6 111.3(2) . . ? C7_6 C6_6 C8_6 112.0(2) . . ? N2_6 C6_6 H6_6 107.9 . . ? C7_6 C6_6 H6_6 107.9 . . ? C8_6 C6_6 H6_6 107.9 . . ? C6_6 C7_6 H021_6 109.5 . . ? C6_6 C7_6 H022_6 109.5 . . ? H021_6 C7_6 H022_6 109.5 . . ? C6_6 C7_6 H023_6 109.5 . . ? H021_6 C7_6 H023_6 109.5 . . ? H022_6 C7_6 H023_6 109.5 . . ? C6_6 C8_6 H01N_6 109.5 . . ? C6_6 C8_6 H01O_6 109.5 . . ? H01N_6 C8_6 H01O_6 109.5 . . ? C6_6 C8_6 H01P_6 109.5 . . ? H01N_6 C8_6 H01P_6 109.5 . . ? H01O_6 C8_6 H01P_6 109.5 . . ? N5_6 C9_6 C11_6 109.7(2) . . ? N5_6 C9_6 C10_6 110.6(2) . . ? C11_6 C9_6 C10_6 112.2(2) . . ? N5_6 C9_6 H9_6 108.1 . . ? C11_6 C9_6 H9_6 108.1 . . ? C10_6 C9_6 H9_6 108.1 . . ? C9_6 C10_6 H02G_6 109.5 . . ? C9_6 C10_6 H02H_6 109.5 . . ? H02G_6 C10_6 H02H_6 109.5 . . ? C9_6 C10_6 H02I_6 109.5 . . ? H02G_6 C10_6 H02I_6 109.5 . . ? H02H_6 C10_6 H02I_6 109.5 . . ? C9_6 C11_6 H01J_6 109.5 . . ? C9_6 C11_6 H01K_6 109.5 . . ? H01J_6 C11_6 H01K_6 109.5 . . ? C9_6 C11_6 H01L_6 109.5 . . ? H01J_6 C11_6 H01L_6 109.5 . . ? H01K_6 C11_6 H01L_6 109.5 . . ? 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 Ni01 C1_2 1.901(2) . ? Ni01 C1_3 1.914(2) . ? Ni01 S1_1 2.1796(6) . ? Ni01 S3_1 2.1869(6) . ? Ni02 C1_6 1.899(2) . ? Ni02 C1_5 1.910(2) . ? Ni02 S1_4 2.1849(6) . ? Ni02 S3_4 2.1984(6) . ? O1_9 C5_9 1.4214 . ? O1_9 C2_9 1.4216 . ? C2_9 C3_9 1.5305 . ? C2_9 H2A_9 0.9900 . ? C2_9 H2B_9 0.9900 . ? C3_9 C4_9 1.5267 . ? C3_9 H3A_9 0.9900 . ? C3_9 H3B_9 0.9900 . ? C4_9 C5_9 1.5302 . ? C4_9 H4A_9 0.9900 . ? C4_9 H4B_9 0.9900 . ? C5_9 H5A_9 0.9900 . ? C5_9 H5B_9 0.9900 . ? O1_7 C5_7 1.4216 . ? O1_7 C2_7 1.4217 . ? C2_7 C3_7 1.5304 . ? C2_7 H2A_7 0.9900 . ? C2_7 H2B_7 0.9900 . ? C3_7 C4_7 1.5269 . ? C3_7 H3A_7 0.9900 . ? C3_7 H3B_7 0.9900 . ? C4_7 C5_7 1.5302 . ? C4_7 H4A_7 0.9900 . ? C4_7 H4B_7 0.9900 . ? C5_7 H5A_7 0.9900 . ? C5_7 H5B_7 0.9900 . ? O1_8 C5_8 1.4215 . ? O1_8 C2_8 1.4216 . ? C2_8 C3_8 1.5303 . ? C2_8 H2A_8 0.9900 . ? C2_8 H2B_8 0.9900 . ? C3_8 C4_8 1.5269 . ? C3_8 H3A_8 0.9900 . ? C3_8 H3B_8 0.9900 . ? C4_8 C5_8 1.5302 . ? C4_8 H4A_8 0.9900 . ? C4_8 H4B_8 0.9900 . ? C5_8 H5A_8 0.9900 . ? C5_8 H5B_8 0.9900 . ? S1_1 C2_1 1.768(2) . ? C2_1 C4_1 1.343(3) . ? C2_1 S3_1 1.776(2) . ? C4_1 N12_1 1.416(3) . ? C4_1 N5_1 1.421(3) . ? N5_1 C6_1 1.386(3) . ? N5_1 C13_1 1.437(4) . ? C6_1 C7_1 1.380(4) . ? C6_1 C11_1 1.392(4) . ? C7_1 C8_1 1.404(5) . ? C7_1 H024_1 0.9500 . ? C8_1 C9_1 1.373(6) . ? C8_1 H02O_1 0.9500 . ? C9_1 C10_1 1.398(5) . ? C9_1 H02P_1 0.9500 . ? C10_1 C11_1 1.383(4) . ? C10_1 H029_1 0.9500 . ? C11_1 N12_1 1.389(3) . ? N12_1 C14_1 1.450(4) . ? C13_1 H014_1 0.9800 . ? C13_1 H017_1 0.9800 . ? C13_1 H018_1 0.9800 . ? C14_1 H02W_1 0.9800 . ? C14_1 H02X_1 0.9800 . ? C14_1 H02Y_1 0.9800 . ? C1_2 N5_2 1.352(3) . ? C1_2 N2_2 1.364(3) . ? N2_2 C3_2 1.384(3) . ? N2_2 C9_2 1.471(3) . ? C3_2 C4_2 1.330(5) . ? C3_2 H012_2 0.9500 . ? C4_2 N5_2 1.385(4) . ? C4_2 H01W_2 0.9500 . ? N5_2 C6_2 1.469(3) . ? C6_2 C8_2 1.524(4) . ? C6_2 C7_2 1.527(3) . ? C6_2 H6_2 1.0000 . ? C7_2 H01A_2 0.9800 . ? C7_2 H01B_2 0.9800 . ? C7_2 H01C_2 0.9800 . ? C8_2 H026_2 0.9800 . ? C8_2 H027_2 0.9800 . ? C8_2 H028_2 0.9800 . ? C9_2 C10_2 1.515(4) . ? C9_2 C11_2 1.529(4) . ? C9_2 H9_2 1.0000 . ? C10_2 H02A_2 0.9800 . ? C10_2 H02B_2 0.9800 . ? C10_2 H02C_2 0.9800 . ? C11_2 H01Y_2 0.9800 . ? C11_2 H01Z_2 0.9800 . ? C11_2 H010_2 0.9800 . ? C1_3 N2_3 1.358(3) . ? C1_3 N5_3 1.360(3) . ? N2_3 C3_3 1.381(3) . ? N2_3 C6_3 1.461(3) . ? C3_3 C4_3 1.327(5) . ? C3_3 H025_3 0.9500 . ? C4_3 N5_3 1.391(3) . ? C4_3 H01X_3 0.9500 . ? N5_3 C9_3 1.466(4) . ? C6_3 C7_3 1.522(4) . ? C6_3 C8_3 1.525(4) . ? C6_3 H6_3 1.0000 . ? C7_3 H02Q_3 0.9800 . ? C7_3 H02R_3 0.9800 . ? C7_3 H02S_3 0.9800 . ? C8_3 H01T_3 0.9800 . ? C8_3 H01U_3 0.9800 . ? C8_3 H01V_3 0.9800 . ? C9_3 C11_3 1.518(6) . ? C9_3 C10_3 1.520(6) . ? C9_3 H011_3 1.0000 . ? C10_3 H032_3 0.9800 . ? C10_3 H033_3 0.9800 . ? C10_3 H034_3 0.9800 . ? C11_3 H02Z_3 0.9800 . ? C11_3 H030_3 0.9800 . ? C11_3 H031_3 0.9800 . ? S1_4 C2_4 1.769(2) . ? C2_4 C4_4 1.341(3) . ? C2_4 S3_4 1.780(2) . ? C4_4 N12_4 1.417(3) . ? C4_4 N5_4 1.421(3) . ? N5_4 C6_4 1.386(3) . ? N5_4 C13_4 1.435(4) . ? C6_4 C7_4 1.382(3) . ? C6_4 C11_4 1.393(4) . ? C7_4 C8_4 1.412(6) . ? C7_4 H020_4 0.9500 . ? C8_4 C9_4 1.369(6) . ? C8_4 H02M_4 0.9500 . ? C9_4 C10_4 1.396(4) . ? C9_4 H02N_4 0.9500 . ? C10_4 C11_4 1.391(4) . ? C10_4 H01M_4 0.9500 . ? C11_4 N12_4 1.388(3) . ? N12_4 C14_4 1.438(3) . ? C13_4 H02D_4 0.9800 . ? C13_4 H02E_4 0.9800 . ? C13_4 H02F_4 0.9800 . ? C14_4 H01Q_4 0.9800 . ? C14_4 H01R_4 0.9800 . ? C14_4 H01S_4 0.9800 . ? C1_5 N2_5 1.358(3) . ? C1_5 N5_5 1.364(3) . ? N2_5 C3_5 1.394(3) . ? N2_5 C6_5 1.475(3) . ? C3_5 C4_5 1.336(4) . ? C3_5 H3_5 0.9500 . ? C4_5 N5_5 1.385(3) . ? C4_5 H4_5 0.9500 . ? N5_5 C9_5 1.462(3) . ? C6_5 C8_5 1.515(5) . ? C6_5 C7_5 1.519(4) . ? C6_5 H6_5 1.0000 . ? C7_5 H02T_5 0.9800 . ? C7_5 H02U_5 0.9800 . ? C7_5 H02V_5 0.9800 . ? C8_5 H02J_5 0.9800 . ? C8_5 H02K_5 0.9800 . ? C8_5 H02L_5 0.9800 . ? C9_5 C10_5 1.520(3) . ? C9_5 C11_5 1.529(3) . ? C9_5 H9_5 1.0000 . ? C10_5 H01G_5 0.9800 . ? C10_5 H01H_5 0.9800 . ? C10_5 H01I_5 0.9800 . ? C11_5 H01D_5 0.9800 . ? C11_5 H01E_5 0.9800 . ? C11_5 H01F_5 0.9800 . ? C1_6 N5_6 1.359(3) . ? C1_6 N2_6 1.369(3) . ? N2_6 C3_6 1.384(3) . ? N2_6 C6_6 1.473(3) . ? C3_6 C4_6 1.341(4) . ? C3_6 H3_6 0.9500 . ? C4_6 N5_6 1.378(3) . ? C4_6 H4_6 0.9500 . ? N5_6 C9_6 1.477(3) . ? C6_6 C7_6 1.525(4) . ? C6_6 C8_6 1.525(4) . ? C6_6 H6_6 1.0000 . ? C7_6 H021_6 0.9800 . ? C7_6 H022_6 0.9800 . ? C7_6 H023_6 0.9800 . ? C8_6 H01N_6 0.9800 . ? C8_6 H01O_6 0.9800 . ? C8_6 H01P_6 0.9800 . ? C9_6 C11_6 1.521(4) . ? C9_6 C10_6 1.522(4) . ? C9_6 H9_6 1.0000 . ? C10_6 H02G_6 0.9800 . ? C10_6 H02H_6 0.9800 . ? C10_6 H02I_6 0.9800 . ? C11_6 H01J_6 0.9800 . ? C11_6 H01K_6 0.9800 . ? C11_6 H01L_6 0.9800 . ?