#------------------------------------------------------------------------------ #$Date: 2025-02-12 01:08:47 +0200 (Wed, 12 Feb 2025) $ #$Revision: 297685 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/38/1573888.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_1573888 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 'C64 H88 K N4 Ni O2 S4, C4 H8 O' _chemical_formula_sum 'C68 H96 K N4 Ni O3 S4' _chemical_formula_weight 1243.53 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _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 90 _cell_formula_units_Z 4 _cell_length_a 12.25160(10) _cell_length_b 19.85030(10) _cell_length_c 27.24960(10) _cell_measurement_reflns_used 76595 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 76.7870 _cell_measurement_theta_min 2.7030 _cell_volume 6627.05(7) _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 1.000 _diffrn_measured_fraction_theta_max 1.000 _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 0.0445 _diffrn_reflns_av_unetI/netI 0.0212 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 119594 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 67.069 _diffrn_reflns_theta_max 67.069 _diffrn_reflns_theta_min 2.754 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 2.524 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.160 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.92a (Rigaku Oxford Diffraction, 2020) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.246 _exptl_crystal_description block _exptl_crystal_F_000 2668 _exptl_crystal_size_max 0.360 _exptl_crystal_size_mid 0.270 _exptl_crystal_size_min 0.210 _refine_diff_density_max 1.192 _refine_diff_density_min -0.704 _refine_diff_density_rms 0.055 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.436(13) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 823 _refine_ls_number_reflns 11832 _refine_ls_number_restraints 296 _refine_ls_restrained_S_all 1.081 _refine_ls_R_factor_all 0.0336 _refine_ls_R_factor_gt 0.0327 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+4.2696P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0908 _refine_ls_wR_factor_ref 0.0914 _reflns_Friedel_coverage 0.813 _reflns_Friedel_fraction_full 0.999 _reflns_Friedel_fraction_max 0.999 _reflns_number_gt 11513 _reflns_number_total 11832 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc08449g2.cif _cod_data_source_block Compound_4bK _cod_database_code 1573888 _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 0.463 _shelx_estimated_absorpt_t_max 0.619 _shelx_res_file ; TITL MaLu108_ref2_filter08_b.res in P2(1)2(1)2(1) MaLu108_ref2_filter08_b.res created by SHELXL-2018/3 at 12:13:50 on 22-Mar-2023 REM Old TITL MaLu108_ref2_filter08 in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.083, Rweak 0.016, Alpha 0.011, Orientation as input REM Flack x = 0.441 ( 0.003 ) from Parsons' quotients REM Formula found by SHELXT: C68 N6 O S4 K Ni CELL 1.54184 12.2516 19.8503 27.2496 90.000 90.000 90.000 ZERR 4.000 0.0001 0.0001 0.0001 0.000 0.000 0.000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H N O S K NI UNIT 272 384 16 12 16 4 4 TEMP -173 SIZE 0.21 0.27 0.36 L.S. 10 OMIT 12 1 0 OMIT 1 1 9 BOND $H LIST 4 ACTA 144 SHEL 0.837 99999999999999999999991 FMAP 2 TWIN PLAN 20 REM ##### SIMU 0.01 O1_101 > C5_102 RIGU 0.005 O1_101 > C5_102 DFIX 1.516 0.001 C8_6 C1_41 C8_6 C1_42 WGHT 0.047000 4.269599 BASF 0.43626 FVAR 0.14092 0.81265 0.43335 PART 1 21 RESI 101 THF O1 4 0.112985 0.568278 0.246307 21.00000 0.02661 0.02327 = 0.06058 -0.00110 -0.00190 0.00365 C2 1 0.092028 0.499664 0.250898 21.00000 0.03515 0.02513 = 0.07471 0.00356 0.00255 -0.00242 AFIX 23 H02V 2 0.136020 0.480096 0.277833 21.00000 -1.20000 H02W 2 0.110123 0.475822 0.220042 21.00000 -1.20000 AFIX 0 C3 1 -0.031315 0.493275 0.262321 21.00000 0.04584 0.04087 = 0.09705 0.02211 -0.00834 -0.01702 AFIX 23 H03E 2 -0.061240 0.450534 0.249301 21.00000 -1.20000 H03F 2 -0.044982 0.495375 0.298096 21.00000 -1.20000 AFIX 0 C4 1 -0.079478 0.551823 0.237014 21.00000 0.04016 0.05383 = 0.10787 0.00888 -0.00572 -0.00558 AFIX 23 H03C 2 -0.145462 0.567960 0.254382 21.00000 -1.20000 H03D 2 -0.099186 0.540423 0.202773 21.00000 -1.20000 AFIX 0 C5 1 0.010326 0.604302 0.238433 21.00000 0.03204 0.03047 = 0.07383 0.00770 0.00043 0.00261 AFIX 23 H030 2 0.012786 0.629499 0.207100 21.00000 -1.20000 H031 2 -0.002758 0.636659 0.265446 21.00000 -1.20000 AFIX 0 RESI 0 PART 0 PART 2 -21 RESI 102 THF O1 4 0.096872 0.574432 0.244119 -21.00000 0.03282 0.02357 = 0.07104 0.00242 0.00048 -0.00655 C2 1 0.075241 0.496842 0.255605 -21.00000 0.03543 0.02540 = 0.08016 0.00694 -0.00307 -0.00411 AFIX 23 H02V 2 0.130711 0.466825 0.240779 -21.00000 -1.20000 H02W 2 0.068260 0.487509 0.291155 -21.00000 -1.20000 AFIX 0 C3 1 -0.032827 0.494426 0.229049 -21.00000 0.03839 0.03484 = 0.08934 0.00345 -0.00262 -0.00604 AFIX 23 H03E 2 -0.024832 0.468664 0.198149 -21.00000 -1.20000 H03F 2 -0.087700 0.471325 0.249739 -21.00000 -1.20000 AFIX 0 C4 1 -0.061134 0.547144 0.220633 -21.00000 0.03602 0.04256 = 0.08684 0.01191 -0.00707 -0.00169 AFIX 23 H03C 2 -0.141238 0.549812 0.224999 -21.00000 -1.20000 H03D 2 -0.044414 0.557872 0.185958 -21.00000 -1.20000 AFIX 0 C5 1 -0.001357 0.603322 0.256755 -21.00000 0.03418 0.03307 = 0.08218 0.00591 -0.00344 0.00097 AFIX 23 H030 2 -0.009741 0.650493 0.245578 -21.00000 -1.20000 H031 2 -0.020296 0.598633 0.291909 -21.00000 -1.20000 AFIX 0 RESI 0 PART 0 RESI 2 THF O1 4 0.428561 0.572331 0.256424 11.00000 0.03312 0.02987 = 0.06696 -0.00848 -0.00583 0.01030 C2 1 0.542598 0.572026 0.267478 11.00000 0.03673 0.03577 = 0.06347 -0.00980 -0.00878 0.00760 AFIX 23 H02R 2 0.554578 0.565966 0.303135 11.00000 -1.20000 H02S 2 0.576994 0.614849 0.257102 11.00000 -1.20000 AFIX 0 C3 1 0.589040 0.514209 0.239468 11.00000 0.03390 0.02939 = 0.07281 -0.00116 0.00899 0.00604 AFIX 23 H02P 2 0.657523 0.497737 0.254564 11.00000 -1.20000 H02Q 2 0.603119 0.526494 0.204830 11.00000 -1.20000 AFIX 0 C4 1 0.499285 0.462814 0.243545 11.00000 0.03308 0.03030 = 0.05104 -0.00479 -0.00324 0.00324 AFIX 23 H024 2 0.500656 0.431185 0.215462 11.00000 -1.20000 H025 2 0.505332 0.436895 0.274465 11.00000 -1.20000 AFIX 0 C5 1 0.397686 0.505029 0.243005 11.00000 0.03591 0.02930 = 0.06106 -0.00479 -0.00960 0.00702 AFIX 23 H032 2 0.364529 0.504729 0.209874 11.00000 -1.20000 H033 2 0.343729 0.487028 0.266658 11.00000 -1.20000 AFIX 0 RESI 0 RESI 3 THF O1 4 0.733481 0.774931 0.295508 11.00000 0.03946 0.04370 = 0.04027 0.00692 0.01332 0.01382 C2 1 0.809996 0.728031 0.274470 11.00000 0.03721 0.04036 = 0.03897 -0.00138 0.00635 0.01061 AFIX 23 H02T 2 0.778244 0.682194 0.273382 11.00000 -1.20000 H02U 2 0.877919 0.726606 0.294124 11.00000 -1.20000 AFIX 0 C3 1 0.833108 0.752876 0.223790 11.00000 0.02785 0.04389 = 0.03505 -0.00033 0.00458 0.00676 AFIX 23 H020 2 0.777528 0.736835 0.200147 11.00000 -1.20000 H021 2 0.906387 0.738672 0.212504 11.00000 -1.20000 AFIX 0 C4 1 0.827021 0.828627 0.230646 11.00000 0.03793 0.03857 = 0.03709 0.00398 0.00251 -0.00256 AFIX 23 H034 2 0.812006 0.852014 0.199276 11.00000 -1.20000 H035 2 0.895024 0.846724 0.245183 11.00000 -1.20000 AFIX 0 C5 1 0.731294 0.834467 0.265997 11.00000 0.03709 0.03795 = 0.03606 0.00057 0.00128 0.01034 AFIX 23 H022 2 0.739028 0.875105 0.286769 11.00000 -1.20000 H023 2 0.661652 0.837536 0.247708 11.00000 -1.20000 AFIX 0 RESI 0 RESI 4 MAIN NI1 7 0.198808 0.826578 0.249781 11.00000 0.01591 0.01682 = 0.01358 -0.00029 0.00045 -0.00231 S2 5 0.269637 0.877668 0.313055 11.00000 0.02272 0.02112 = 0.01563 0.00134 -0.00048 -0.00827 S3 5 0.120612 0.771230 0.310198 11.00000 0.01718 0.01880 = 0.01527 -0.00008 -0.00017 -0.00349 S4 5 0.134380 0.771415 0.186765 11.00000 0.01594 0.01845 = 0.01497 -0.00012 0.00059 -0.00453 S5 5 0.290932 0.873166 0.190423 11.00000 0.02439 0.02775 = 0.01567 -0.00421 0.00332 -0.01286 K6 6 0.268203 0.662911 0.250822 11.00000 0.02700 0.02196 = 0.03257 -0.00080 -0.00084 0.00447 RESI 0 RESI 5 NHC C1 1 0.227534 0.816832 0.149991 11.00000 0.01409 0.01845 = 0.01894 -0.00108 0.00152 -0.00204 C2 1 0.247511 0.808697 0.101193 11.00000 0.01412 0.01292 = 0.01826 -0.00201 -0.00171 -0.00128 N3 3 0.187516 0.771290 0.066940 11.00000 0.01584 0.01479 = 0.01597 -0.00153 0.00065 -0.00029 C4 1 0.237369 0.775628 0.020954 11.00000 0.02340 0.01805 = 0.01331 -0.00141 0.00118 0.00265 AFIX 43 H4 2 0.212407 0.754448 -0.008225 11.00000 -1.20000 AFIX 0 C5 1 0.325507 0.814293 0.024780 11.00000 0.02201 0.01792 = 0.01642 -0.00210 0.00507 -0.00046 AFIX 43 H5 2 0.374469 0.825287 -0.001041 11.00000 -1.20000 AFIX 0 N6 3 0.333600 0.836092 0.073771 11.00000 0.01737 0.02164 = 0.01524 -0.00186 0.00348 -0.00541 C7 1 0.434394 0.862445 0.092842 11.00000 0.01553 0.02212 = 0.01756 -0.00498 0.00403 -0.00327 C8 1 0.459016 0.930343 0.083721 11.00000 0.02094 0.01967 = 0.02644 -0.00349 0.00283 -0.00149 C9 1 0.558963 0.954550 0.100981 11.00000 0.02309 0.02174 = 0.03950 -0.00040 -0.00115 -0.00615 AFIX 43 H01I 2 0.577942 1.000344 0.095521 11.00000 -1.20000 AFIX 0 C10 1 0.630238 0.913372 0.125683 11.00000 0.01836 0.03369 = 0.03525 -0.00256 -0.00075 -0.00685 AFIX 43 H01F 2 0.697583 0.931045 0.137209 11.00000 -1.20000 AFIX 0 C11 1 0.605047 0.846446 0.133966 11.00000 0.01862 0.03225 = 0.02855 0.00160 0.00087 0.00186 AFIX 43 H01H 2 0.655165 0.818528 0.151114 11.00000 -1.20000 AFIX 0 C12 1 0.506283 0.819561 0.117272 11.00000 0.01813 0.02199 = 0.02364 0.00083 0.00368 -0.00024 C13 1 0.086021 0.738132 0.076694 11.00000 0.01549 0.01863 = 0.01350 -0.00077 -0.00148 -0.00387 C14 1 0.086846 0.668050 0.083197 11.00000 0.02186 0.01843 = 0.01773 -0.00116 -0.00198 -0.00148 C15 1 -0.011090 0.637220 0.096650 11.00000 0.02425 0.01752 = 0.02375 0.00025 -0.00136 -0.00283 AFIX 43 H15 2 -0.013260 0.589821 0.101368 11.00000 -1.20000 AFIX 0 C16 1 -0.105001 0.674824 0.103196 11.00000 0.01960 0.02562 = 0.02237 0.00015 -0.00003 -0.00716 AFIX 43 H16 2 -0.170112 0.653311 0.113819 11.00000 -1.20000 AFIX 0 C17 1 -0.105021 0.743764 0.094384 11.00000 0.01837 0.02281 = 0.02094 -0.00230 -0.00052 -0.00022 AFIX 43 H01D 2 -0.170763 0.768665 0.097950 11.00000 -1.20000 AFIX 0 C18 1 -0.009549 0.776763 0.080362 11.00000 0.01957 0.01820 = 0.01583 -0.00162 -0.00138 -0.00203 RESI 0 RESI 6 NHC C1 1 0.202125 0.819256 0.350105 11.00000 0.01700 0.01539 = 0.01899 0.00131 0.00087 -0.00279 C2 1 0.216660 0.810066 0.399816 11.00000 0.01266 0.01217 = 0.01891 -0.00242 0.00118 0.00100 N3 3 0.297636 0.837713 0.429258 11.00000 0.01758 0.02026 = 0.01646 0.00109 -0.00045 -0.00301 C4 1 0.286443 0.812725 0.477279 11.00000 0.02260 0.02228 = 0.01609 0.00028 -0.00429 0.00241 AFIX 43 H4 2 0.332479 0.822889 0.504338 11.00000 -1.20000 AFIX 0 C5 1 0.199792 0.772276 0.478038 11.00000 0.02141 0.02048 = 0.01722 0.00393 0.00144 0.00354 AFIX 43 H5 2 0.172749 0.749020 0.505977 11.00000 -1.20000 AFIX 0 N6 3 0.155516 0.769762 0.431124 11.00000 0.01866 0.01886 = 0.01334 0.00306 -0.00052 -0.00117 C7 1 0.056287 0.735576 0.419292 11.00000 0.01772 0.01885 = 0.01496 0.00336 0.00124 -0.00223 C8 1 0.059236 0.664882 0.413901 11.00000 0.02568 0.01709 = 0.02287 0.00192 0.00568 0.00035 C9 1 -0.037419 0.632671 0.401251 11.00000 0.03329 0.01893 = 0.02681 -0.00093 0.00425 -0.00664 AFIX 43 H9 2 -0.038251 0.585061 0.397728 11.00000 -1.20000 AFIX 0 C10 1 -0.132495 0.668838 0.393702 11.00000 0.02367 0.02819 = 0.02415 0.00076 -0.00121 -0.00720 AFIX 43 H10 2 -0.197362 0.646146 0.384130 11.00000 -1.20000 AFIX 0 C11 1 -0.133272 0.738071 0.400074 11.00000 0.01785 0.03003 = 0.02238 0.00304 0.00040 -0.00096 AFIX 43 H11 2 -0.199103 0.762366 0.394957 11.00000 -1.20000 AFIX 0 C12 1 -0.039709 0.772536 0.413783 11.00000 0.02209 0.01842 = 0.01568 0.00324 0.00466 0.00112 C13 1 0.399963 0.865327 0.413200 11.00000 0.01414 0.01964 = 0.01714 -0.00211 -0.00470 -0.00218 C14 1 0.476595 0.823418 0.390435 11.00000 0.01936 0.02396 = 0.02013 0.00031 -0.00285 -0.00024 C15 1 0.577054 0.851501 0.377178 11.00000 0.01827 0.02838 = 0.02651 -0.00258 -0.00023 0.00286 AFIX 43 H15 2 0.630496 0.824354 0.361462 11.00000 -1.20000 AFIX 0 C16 1 0.599142 0.918733 0.386833 11.00000 0.01693 0.03038 = 0.03032 0.00106 0.00118 -0.00435 AFIX 43 H16 2 0.667572 0.937273 0.377535 11.00000 -1.20000 AFIX 0 C17 1 0.522753 0.959047 0.409820 11.00000 0.02228 0.02089 = 0.02929 -0.00074 -0.00290 -0.00317 AFIX 43 H17 2 0.539723 1.004875 0.416356 11.00000 -1.20000 AFIX 0 C18 1 0.421315 0.933660 0.423573 11.00000 0.01910 0.02147 = 0.02083 -0.00004 -0.00250 -0.00064 RESI 0 RESI 7 IPR C1 1 0.335693 0.977379 0.448158 11.00000 0.02257 0.02069 = 0.03427 -0.00295 0.00258 -0.00132 AFIX 13 H01G 2 0.289469 0.947137 0.468882 11.00000 -1.20000 AFIX 0 C2 1 0.384527 1.030453 0.481876 11.00000 0.03230 0.03478 = 0.03540 -0.01020 0.00615 0.00072 AFIX 137 H01P 2 0.427981 1.062208 0.462469 11.00000 -1.50000 H01Q 2 0.431359 1.008567 0.506286 11.00000 -1.50000 H01R 2 0.325713 1.054792 0.498604 11.00000 -1.50000 AFIX 0 C3 1 0.261378 1.009988 0.410618 11.00000 0.05018 0.04894 = 0.05355 -0.02006 -0.01706 0.03222 AFIX 137 H02X 2 0.304443 1.039430 0.389205 11.00000 -1.50000 H02Y 2 0.205533 1.036664 0.427511 11.00000 -1.50000 H02Z 2 0.226077 0.974970 0.390851 11.00000 -1.50000 AFIX 0 RESI 0 RESI 8 IPR C1 1 0.453917 0.749357 0.380148 11.00000 0.02058 0.02288 = 0.03166 -0.00641 -0.00233 0.00208 AFIX 13 H1 2 0.377673 0.739542 0.391125 11.00000 -1.20000 AFIX 0 C2 1 0.460782 0.733517 0.325469 11.00000 0.04167 0.03139 = 0.03952 -0.01198 -0.00537 0.00628 AFIX 137 H02J 2 0.411397 0.763353 0.307358 11.00000 -1.50000 H02K 2 0.439588 0.686533 0.319883 11.00000 -1.50000 H02L 2 0.535773 0.740486 0.314030 11.00000 -1.50000 AFIX 0 C3 1 0.529861 0.704191 0.409008 11.00000 0.03571 0.02461 = 0.05341 -0.00098 -0.01001 0.00126 AFIX 137 H02G 2 0.605721 0.716177 0.401668 11.00000 -1.50000 H02H 2 0.516897 0.657117 0.399869 11.00000 -1.50000 H02I 2 0.516169 0.710015 0.444186 11.00000 -1.50000 AFIX 0 RESI 0 RESI 9 IPR C1 1 -0.044835 0.848301 0.422042 11.00000 0.01814 0.01960 = 0.02946 0.00091 0.00402 -0.00021 AFIX 13 H1 2 0.027756 0.863399 0.434713 11.00000 -1.20000 AFIX 0 C2 1 -0.068231 0.886600 0.374303 11.00000 0.04177 0.02350 = 0.03173 0.00865 0.01257 0.01232 AFIX 137 H01V 2 -0.012710 0.875150 0.349794 11.00000 -1.50000 H01W 2 -0.066438 0.935177 0.380672 11.00000 -1.50000 H01X 2 -0.140493 0.873945 0.361940 11.00000 -1.50000 AFIX 0 C3 1 -0.131416 0.865435 0.460808 11.00000 0.02804 0.02191 = 0.02657 0.00003 0.00362 0.00354 AFIX 137 H01A 2 -0.128314 0.913679 0.468315 11.00000 -1.50000 H01B 2 -0.117226 0.839474 0.490725 11.00000 -1.50000 H01C 2 -0.203979 0.854089 0.448130 11.00000 -1.50000 AFIX 0 RESI 0 SIMU 0.007 C1_41 > C3_42 RIGU 0.004 C1_41 > C3_42 PART 1 31 RESI 41 IPR C1 1 0.164617 0.625755 0.420178 31.00000 0.02998 0.02004 = 0.03661 0.00360 0.00430 0.00379 AFIX 13 H01E 2 0.213327 0.659432 0.436465 31.00000 -1.20000 AFIX 0 C2 1 0.222756 0.612447 0.372981 31.00000 0.03169 0.02234 = 0.03713 0.00688 0.00628 0.00948 AFIX 137 H039 2 0.175622 0.585902 0.351292 31.00000 -1.50000 H03A 2 0.290077 0.587367 0.379574 31.00000 -1.50000 H03B 2 0.240713 0.655341 0.357111 31.00000 -1.50000 AFIX 0 C3 1 0.145726 0.574072 0.460996 31.00000 0.03539 0.02486 = 0.02992 0.00704 -0.00518 0.01032 AFIX 137 H01J 2 0.087590 0.542969 0.451158 31.00000 -1.50000 H01K 2 0.124334 0.597428 0.491186 31.00000 -1.50000 H01L 2 0.213160 0.548733 0.466778 31.00000 -1.50000 AFIX 0 RESI 0 PART 0 PART 2 -31 RESI 42 IPR C1 1 0.164652 0.625543 0.419318 -31.00000 0.02961 0.01951 = 0.03782 0.00415 0.00433 0.00204 AFIX 13 H01E 2 0.227024 0.655857 0.427845 -31.00000 -1.20000 AFIX 0 C2 1 0.186158 0.586880 0.369083 -31.00000 0.03965 0.03029 = 0.03718 0.00700 0.00695 0.01711 AFIX 137 H039 2 0.126524 0.555059 0.362982 -31.00000 -1.50000 H03A 2 0.255338 0.562265 0.371187 -31.00000 -1.50000 H03B 2 0.189856 0.619505 0.342142 -31.00000 -1.50000 AFIX 0 C3 1 0.159978 0.565115 0.453222 -31.00000 0.02664 0.02719 = 0.02713 0.00519 -0.00056 0.00435 AFIX 137 H01J 2 0.108548 0.531911 0.440044 -31.00000 -1.50000 H01K 2 0.135677 0.579529 0.485837 -31.00000 -1.50000 H01L 2 0.232685 0.544821 0.455714 -31.00000 -1.50000 AFIX 0 RESI 0 PART 0 RESI 11 IPR C1 1 0.378991 0.976046 0.057242 11.00000 0.02175 0.02121 = 0.03787 -0.00187 -0.00328 0.00022 AFIX 13 H1 2 0.333440 0.946748 0.035522 11.00000 -1.20000 AFIX 0 C2 1 0.302332 1.009779 0.093195 11.00000 0.04878 0.05901 = 0.05331 0.02344 0.02097 0.03202 AFIX 137 H036 2 0.250501 1.038173 0.075236 11.00000 -1.50000 H037 2 0.344524 1.037690 0.116002 11.00000 -1.50000 H038 2 0.262330 0.975320 0.111628 11.00000 -1.50000 AFIX 0 C3 1 0.434170 1.027916 0.024471 11.00000 0.03620 0.03732 = 0.04095 0.00944 -0.00061 0.00471 AFIX 137 H026 2 0.479461 1.004820 0.000064 11.00000 -1.50000 H027 2 0.480135 1.057486 0.044528 11.00000 -1.50000 H028 2 0.378459 1.054853 0.007710 11.00000 -1.50000 AFIX 0 RESI 0 RESI 12 IPR C1 1 0.481371 0.745039 0.125908 11.00000 0.01973 0.02190 = 0.03462 0.00370 0.00373 0.00000 AFIX 13 H02C 2 0.405396 0.736452 0.114044 11.00000 -1.20000 AFIX 0 C2 1 0.557827 0.700402 0.096134 11.00000 0.04277 0.02334 = 0.05236 -0.00110 0.01731 0.00188 AFIX 137 H01Y 2 0.551118 0.711595 0.061237 11.00000 -1.50000 H01Z 2 0.538314 0.653028 0.101183 11.00000 -1.50000 H013 2 0.633235 0.707867 0.106828 11.00000 -1.50000 AFIX 0 C3 1 0.484804 0.727379 0.180343 11.00000 0.05583 0.03286 = 0.03943 0.01279 0.00485 -0.00249 AFIX 137 H029 2 0.461056 0.680657 0.184925 11.00000 -1.50000 H02A 2 0.436034 0.757564 0.198484 11.00000 -1.50000 H02B 2 0.559529 0.732566 0.192606 11.00000 -1.50000 AFIX 0 RESI 0 RESI 13 IPR C1 1 -0.010981 0.851922 0.068607 11.00000 0.01993 0.01542 = 0.02570 -0.00144 0.00079 -0.00116 AFIX 13 H1 2 0.059990 0.863327 0.052498 11.00000 -1.20000 AFIX 0 C2 1 -0.020951 0.895161 0.114682 11.00000 0.04061 0.02041 = 0.03126 -0.00440 -0.00923 0.00784 AFIX 137 H01S 2 -0.014068 0.942819 0.105819 11.00000 -1.50000 H01T 2 0.037037 0.883035 0.137826 11.00000 -1.50000 H01U 2 -0.092226 0.887403 0.129996 11.00000 -1.50000 AFIX 0 C3 1 -0.101903 0.868435 0.032465 11.00000 0.03142 0.02246 = 0.02703 0.00148 -0.00539 0.00196 AFIX 137 H01M 2 -0.098800 0.916371 0.023975 11.00000 -1.50000 H01N 2 -0.172703 0.858238 0.047463 11.00000 -1.50000 H01O 2 -0.092729 0.841324 0.002693 11.00000 -1.50000 AFIX 0 RESI 0 RESI 14 IPR C1 1 0.191549 0.627173 0.078196 11.00000 0.02181 0.01591 = 0.02790 -0.00099 0.00349 0.00285 AFIX 13 H1 2 0.246823 0.656723 0.061895 11.00000 -1.20000 AFIX 0 C2 1 0.236870 0.608005 0.128115 11.00000 0.04511 0.04644 = 0.03424 -0.00428 -0.00527 0.02299 AFIX 137 H02M 2 0.305742 0.583581 0.123874 11.00000 -1.50000 H02N 2 0.184303 0.579189 0.145267 11.00000 -1.50000 H02O 2 0.249830 0.648867 0.147438 11.00000 -1.50000 AFIX 0 C3 1 0.176277 0.565162 0.045641 11.00000 0.03485 0.02420 = 0.04351 -0.00957 0.00762 -0.00173 AFIX 137 H02D 2 0.151720 0.579315 0.013004 11.00000 -1.50000 H02E 2 0.121519 0.535341 0.060317 11.00000 -1.50000 H02F 2 0.245802 0.541077 0.042733 11.00000 -1.50000 RESI 0 AFIX 0 HKLF 4 REM MaLu108_ref2_filter08_b.res in P2(1)2(1)2(1) REM wR2 = 0.091403, GooF = S = 1.08781, Restrained GooF = 1.08065 for all data REM R1 = 0.032683 for 11513 Fo > 4sig(Fo) and 0.033597 for all 11832 data REM 823 parameters refined using 296 restraints END WGHT 0.0470 4.2694 REM Highest difference peak 1.192, deepest hole -0.704, 1-sigma level 0.055 Q1 1 0.5139 0.3643 0.2487 11.00000 0.05 1.19 Q2 1 -0.0714 0.5429 0.2731 11.00000 0.05 0.40 Q3 1 0.3230 0.8496 0.3090 11.00000 0.05 0.32 Q4 1 0.3359 0.8450 0.1879 11.00000 0.05 0.31 Q5 1 0.6785 0.8053 0.2518 11.00000 0.05 0.28 Q6 1 0.1670 0.7432 0.3138 11.00000 0.05 0.27 Q7 1 0.2752 1.0170 0.3761 11.00000 0.05 0.25 Q8 1 0.1875 0.7935 0.1645 11.00000 0.05 0.24 Q9 1 0.2549 0.8426 0.1665 11.00000 0.05 0.24 Q10 1 0.1785 0.7804 0.2890 11.00000 0.05 0.24 Q11 1 0.1676 0.7957 0.3334 11.00000 0.05 0.24 Q12 1 0.2566 0.8051 0.2559 11.00000 0.05 0.24 Q13 1 0.1773 0.7785 0.2095 11.00000 0.05 0.23 Q14 1 0.1798 0.7427 0.1936 11.00000 0.05 0.23 Q15 1 0.8687 0.7466 0.2508 11.00000 0.05 0.23 Q16 1 0.1770 0.7799 0.3304 11.00000 0.05 0.23 Q17 1 0.5162 0.5386 0.2992 11.00000 0.05 0.22 Q18 1 -0.0538 0.7607 0.0796 11.00000 0.05 0.22 Q19 1 0.2610 0.7979 0.1369 11.00000 0.05 0.21 Q20 1 0.7352 0.7537 0.2518 11.00000 0.05 0.21 ; _shelx_res_checksum 14251 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 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 O1_101 O 0.1130(8) 0.5683(5) 0.2463(6) 0.0368(14) Uani 0.813(14) 1 d . U P A 1 C2_101 C 0.0920(10) 0.4997(8) 0.2509(7) 0.045(2) Uani 0.813(14) 1 d . U P A 1 H02V_101 H 0.136020 0.480096 0.277833 0.054 Uiso 0.813(14) 1 calc R U P A 1 H02W_101 H 0.110123 0.475822 0.220042 0.054 Uiso 0.813(14) 1 calc R U P A 1 C3_101 C -0.0313(5) 0.4933(3) 0.2623(4) 0.061(2) Uani 0.813(14) 1 d . U P A 1 H03E_101 H -0.061240 0.450534 0.249301 0.074 Uiso 0.813(14) 1 calc R U P A 1 H03F_101 H -0.044982 0.495375 0.298096 0.074 Uiso 0.813(14) 1 calc R U P A 1 C4_101 C -0.0795(8) 0.5518(6) 0.2370(4) 0.067(2) Uani 0.813(14) 1 d . U P A 1 H03C_101 H -0.145462 0.567960 0.254382 0.081 Uiso 0.813(14) 1 calc R U P A 1 H03D_101 H -0.099186 0.540423 0.202773 0.081 Uiso 0.813(14) 1 calc R U P A 1 C5_101 C 0.0103(7) 0.6043(4) 0.2384(3) 0.0454(18) Uani 0.813(14) 1 d . U P A 1 H030_101 H 0.012786 0.629499 0.207100 0.055 Uiso 0.813(14) 1 calc R U P A 1 H031_101 H -0.002758 0.636659 0.265446 0.055 Uiso 0.813(14) 1 calc R U P A 1 O1_102 O 0.097(4) 0.574(3) 0.244(3) 0.042(3) Uani 0.187(14) 1 d . U P A 2 C2_102 C 0.075(5) 0.497(4) 0.256(3) 0.047(3) Uani 0.187(14) 1 d . U P A 2 H02V_102 H 0.130711 0.466825 0.240779 0.056 Uiso 0.187(14) 1 calc R U P A 2 H02W_102 H 0.068260 0.487509 0.291155 0.056 Uiso 0.187(14) 1 calc R U P A 2 C3_102 C -0.033(2) 0.4944(15) 0.2290(18) 0.054(3) Uani 0.187(14) 1 d . U P A 2 H03E_102 H -0.024832 0.468664 0.198149 0.065 Uiso 0.187(14) 1 calc R U P A 2 H03F_102 H -0.087700 0.471325 0.249739 0.065 Uiso 0.187(14) 1 calc R U P A 2 C4_102 C -0.061(4) 0.547(2) 0.2206(17) 0.055(4) Uani 0.187(14) 1 d . U P A 2 H03C_102 H -0.141238 0.549812 0.224999 0.066 Uiso 0.187(14) 1 calc R U P A 2 H03D_102 H -0.044414 0.557872 0.185958 0.066 Uiso 0.187(14) 1 calc R U P A 2 C5_102 C -0.001(4) 0.603(2) 0.2568(17) 0.050(3) Uani 0.187(14) 1 d . U P A 2 H030_102 H -0.009741 0.650493 0.245578 0.060 Uiso 0.187(14) 1 calc R U P A 2 H031_102 H -0.020296 0.598633 0.291909 0.060 Uiso 0.187(14) 1 calc R U P A 2 O1_2 O 0.4286(2) 0.57233(13) 0.25642(14) 0.0433(7) Uani 1 1 d . . . . . C2_2 C 0.5426(4) 0.5720(2) 0.26748(19) 0.0453(11) Uani 1 1 d . . . . . H02R_2 H 0.554578 0.565966 0.303135 0.054 Uiso 1 1 calc R U . . . H02S_2 H 0.576994 0.614849 0.257102 0.054 Uiso 1 1 calc R U . . . C3_2 C 0.5890(3) 0.51421(19) 0.2395(2) 0.0454(12) Uani 1 1 d . . . . . H02P_2 H 0.657523 0.497737 0.254564 0.054 Uiso 1 1 calc R U . . . H02Q_2 H 0.603119 0.526494 0.204830 0.054 Uiso 1 1 calc R U . . . C4_2 C 0.4993(3) 0.46281(18) 0.24354(19) 0.0381(10) Uani 1 1 d . . . . . H024_2 H 0.500656 0.431185 0.215462 0.046 Uiso 1 1 calc R U . . . H025_2 H 0.505332 0.436895 0.274465 0.046 Uiso 1 1 calc R U . . . C5_2 C 0.3977(3) 0.50503(18) 0.2430(2) 0.0421(11) Uani 1 1 d . . . . . H032_2 H 0.364529 0.504729 0.209874 0.051 Uiso 1 1 calc R U . . . H033_2 H 0.343729 0.487028 0.266658 0.051 Uiso 1 1 calc R U . . . O1_3 O 0.7335(2) 0.77493(15) 0.29551(11) 0.0411(7) Uani 1 1 d . . . . . C2_3 C 0.8100(4) 0.7280(2) 0.27447(16) 0.0388(9) Uani 1 1 d . . . . . H02T_3 H 0.778244 0.682194 0.273382 0.047 Uiso 1 1 calc R U . . . H02U_3 H 0.877919 0.726606 0.294124 0.047 Uiso 1 1 calc R U . . . C3_3 C 0.8331(3) 0.7529(2) 0.22379(15) 0.0356(9) Uani 1 1 d . . . . . H020_3 H 0.777528 0.736835 0.200147 0.043 Uiso 1 1 calc R U . . . H021_3 H 0.906387 0.738672 0.212504 0.043 Uiso 1 1 calc R U . . . C4_3 C 0.8270(3) 0.8286(2) 0.23065(16) 0.0379(9) Uani 1 1 d . . . . . H034_3 H 0.812006 0.852014 0.199276 0.045 Uiso 1 1 calc R U . . . H035_3 H 0.895024 0.846724 0.245183 0.045 Uiso 1 1 calc R U . . . C5_3 C 0.7313(3) 0.8345(2) 0.26600(15) 0.0370(9) Uani 1 1 d . . . . . H022_3 H 0.739028 0.875105 0.286769 0.044 Uiso 1 1 calc R U . . . H023_3 H 0.661652 0.837536 0.247708 0.044 Uiso 1 1 calc R U . . . Ni1_4 Ni 0.19881(4) 0.82658(2) 0.24978(2) 0.01543(12) Uani 1 1 d . . . . . S2_4 S 0.26964(6) 0.87767(4) 0.31306(3) 0.01983(17) Uani 1 1 d . . . . . S3_4 S 0.12061(6) 0.77123(4) 0.31020(3) 0.01708(16) Uani 1 1 d . . . . . S4_4 S 0.13438(6) 0.77142(4) 0.18676(3) 0.01645(16) Uani 1 1 d . . . . . S5_4 S 0.29093(7) 0.87317(4) 0.19042(3) 0.02260(18) Uani 1 1 d . . . . . K6_4 K 0.26820(6) 0.66291(3) 0.25082(3) 0.02718(16) Uani 1 1 d . . . . . C1_5 C 0.2275(3) 0.81683(16) 0.14999(12) 0.0172(6) Uani 1 1 d . . . . . C2_5 C 0.2475(2) 0.80870(15) 0.10119(12) 0.0151(6) Uani 1 1 d . . . . . N3_5 N 0.1875(2) 0.77129(13) 0.06694(10) 0.0155(5) Uani 1 1 d . . . . . C4_5 C 0.2374(3) 0.77563(17) 0.02095(11) 0.0183(6) Uani 1 1 d . . . . . H4_5 H 0.212407 0.754448 -0.008225 0.022 Uiso 1 1 calc R U . . . C5_5 C 0.3255(3) 0.81429(16) 0.02478(12) 0.0188(7) Uani 1 1 d . . . . . H5_5 H 0.374469 0.825287 -0.001041 0.023 Uiso 1 1 calc R U . . . N6_5 N 0.3336(2) 0.83609(14) 0.07377(10) 0.0181(6) Uani 1 1 d . . . . . C7_5 C 0.4344(3) 0.86244(17) 0.09284(12) 0.0184(7) Uani 1 1 d . . . . . C8_5 C 0.4590(3) 0.93034(17) 0.08372(13) 0.0224(7) Uani 1 1 d . . . . . C9_5 C 0.5590(3) 0.95455(19) 0.10098(15) 0.0281(8) Uani 1 1 d . . . . . H01I_5 H 0.577942 1.000344 0.095521 0.034 Uiso 1 1 calc R U . . . C10_5 C 0.6302(3) 0.91337(19) 0.12568(15) 0.0291(8) Uani 1 1 d . . . . . H01F_5 H 0.697583 0.931045 0.137209 0.035 Uiso 1 1 calc R U . . . C11_5 C 0.6050(3) 0.84645(19) 0.13397(14) 0.0265(8) Uani 1 1 d . . . . . H01H_5 H 0.655165 0.818528 0.151114 0.032 Uiso 1 1 calc R U . . . C12_5 C 0.5063(3) 0.81956(17) 0.11727(13) 0.0213(7) Uani 1 1 d . . . . . C13_5 C 0.0860(3) 0.73813(17) 0.07669(11) 0.0159(6) Uani 1 1 d . . . . . C14_5 C 0.0868(3) 0.66805(17) 0.08320(12) 0.0193(7) Uani 1 1 d . . . . . C15_5 C -0.0111(3) 0.63722(17) 0.09665(13) 0.0218(7) Uani 1 1 d . . . . . H15_5 H -0.013260 0.589821 0.101368 0.026 Uiso 1 1 calc R U . . . C16_5 C -0.1050(3) 0.67482(18) 0.10320(13) 0.0225(7) Uani 1 1 d . . . . . H16_5 H -0.170112 0.653311 0.113819 0.027 Uiso 1 1 calc R U . . . C17_5 C -0.1050(3) 0.74376(18) 0.09438(12) 0.0207(7) Uani 1 1 d . . . . . H01D_5 H -0.170763 0.768665 0.097950 0.025 Uiso 1 1 calc R U . . . C18_5 C -0.0095(3) 0.77676(17) 0.08036(12) 0.0179(7) Uani 1 1 d . . . . . C1_6 C 0.2021(2) 0.81926(16) 0.35010(12) 0.0171(6) Uani 1 1 d . . . . . C2_6 C 0.2167(2) 0.81007(15) 0.39982(12) 0.0146(6) Uani 1 1 d . . . . . N3_6 N 0.2976(2) 0.83771(14) 0.42926(10) 0.0181(6) Uani 1 1 d . . . . . C4_6 C 0.2864(3) 0.81272(17) 0.47728(12) 0.0203(7) Uani 1 1 d . . . . . H4_6 H 0.332479 0.822889 0.504338 0.024 Uiso 1 1 calc R U . . . C5_6 C 0.1998(3) 0.77228(17) 0.47804(12) 0.0197(7) Uani 1 1 d . . . . . H5_6 H 0.172749 0.749020 0.505977 0.024 Uiso 1 1 calc R U . . . N6_6 N 0.1555(2) 0.76976(14) 0.43112(10) 0.0170(5) Uani 1 1 d . . . . . C7_6 C 0.0563(3) 0.73558(17) 0.41929(12) 0.0172(7) Uani 1 1 d . . . . . C8_6 C 0.0592(2) 0.66488(17) 0.41390(13) 0.0219(7) Uani 1 1 d D . . . . C9_6 C -0.0374(3) 0.63267(18) 0.40125(14) 0.0263(8) Uani 1 1 d . . . . . H9_6 H -0.038251 0.585061 0.397728 0.032 Uiso 1 1 calc R U . . . C10_6 C -0.1325(3) 0.66884(19) 0.39370(13) 0.0253(7) Uani 1 1 d . . . . . H10_6 H -0.197362 0.646146 0.384130 0.030 Uiso 1 1 calc R U . . . C11_6 C -0.1333(3) 0.73807(19) 0.40007(13) 0.0234(7) Uani 1 1 d . . . . . H11_6 H -0.199103 0.762366 0.394957 0.028 Uiso 1 1 calc R U . . . C12_6 C -0.0397(3) 0.77254(17) 0.41378(12) 0.0187(7) Uani 1 1 d . . . . . C13_6 C 0.4000(3) 0.86533(17) 0.41320(12) 0.0170(6) Uani 1 1 d . . . . . C14_6 C 0.4766(3) 0.82342(18) 0.39044(13) 0.0212(7) Uani 1 1 d . . . . . C15_6 C 0.5771(3) 0.85150(18) 0.37718(13) 0.0244(7) Uani 1 1 d . . . . . H15_6 H 0.630496 0.824354 0.361462 0.029 Uiso 1 1 calc R U . . . C16_6 C 0.5991(3) 0.91873(19) 0.38683(14) 0.0259(8) Uani 1 1 d . . . . . H16_6 H 0.667572 0.937273 0.377535 0.031 Uiso 1 1 calc R U . . . C17_6 C 0.5228(3) 0.95905(18) 0.40982(14) 0.0242(7) Uani 1 1 d . . . . . H17_6 H 0.539723 1.004875 0.416356 0.029 Uiso 1 1 calc R U . . . C18_6 C 0.4213(3) 0.93366(17) 0.42357(12) 0.0205(7) Uani 1 1 d . . . . . C1_7 C 0.3357(3) 0.97738(18) 0.44816(14) 0.0258(8) Uani 1 1 d . . . . . H01G_7 H 0.289469 0.947137 0.468882 0.031 Uiso 1 1 calc R U . . . C2_7 C 0.3845(3) 1.0305(2) 0.48188(15) 0.0342(9) Uani 1 1 d . . . . . H01P_7 H 0.427981 1.062208 0.462469 0.051 Uiso 1 1 calc R U . . . H01Q_7 H 0.431359 1.008567 0.506286 0.051 Uiso 1 1 calc R U . . . H01R_7 H 0.325713 1.054792 0.498604 0.051 Uiso 1 1 calc R U . . . C3_7 C 0.2614(4) 1.0100(3) 0.41062(19) 0.0509(13) Uani 1 1 d . . . . . H02X_7 H 0.304443 1.039430 0.389205 0.076 Uiso 1 1 calc R U . . . H02Y_7 H 0.205533 1.036664 0.427511 0.076 Uiso 1 1 calc R U . . . H02Z_7 H 0.226077 0.974970 0.390851 0.076 Uiso 1 1 calc R U . . . C1_8 C 0.4539(3) 0.74936(18) 0.38015(14) 0.0250(8) Uani 1 1 d . . . . . H1_8 H 0.377673 0.739542 0.391125 0.030 Uiso 1 1 calc R U . . . C2_8 C 0.4608(4) 0.7335(2) 0.32547(16) 0.0375(9) Uani 1 1 d . . . . . H02J_8 H 0.411397 0.763353 0.307358 0.056 Uiso 1 1 calc R U . . . H02K_8 H 0.439588 0.686533 0.319883 0.056 Uiso 1 1 calc R U . . . H02L_8 H 0.535773 0.740486 0.314030 0.056 Uiso 1 1 calc R U . . . C3_8 C 0.5299(3) 0.7042(2) 0.40901(18) 0.0379(10) Uani 1 1 d . . . . . H02G_8 H 0.605721 0.716177 0.401668 0.057 Uiso 1 1 calc R U . . . H02H_8 H 0.516897 0.657117 0.399869 0.057 Uiso 1 1 calc R U . . . H02I_8 H 0.516169 0.710015 0.444186 0.057 Uiso 1 1 calc R U . . . C1_9 C -0.0448(3) 0.84830(17) 0.42204(13) 0.0224(7) Uani 1 1 d . . . . . H1_9 H 0.027756 0.863399 0.434713 0.027 Uiso 1 1 calc R U . . . C2_9 C -0.0682(3) 0.88660(19) 0.37430(14) 0.0323(9) Uani 1 1 d . . . . . H01V_9 H -0.012710 0.875150 0.349794 0.049 Uiso 1 1 calc R U . . . H01W_9 H -0.066438 0.935177 0.380672 0.049 Uiso 1 1 calc R U . . . H01X_9 H -0.140493 0.873945 0.361940 0.049 Uiso 1 1 calc R U . . . C3_9 C -0.1314(3) 0.86543(18) 0.46081(13) 0.0255(8) Uani 1 1 d . . . . . H01A_9 H -0.128314 0.913679 0.468315 0.038 Uiso 1 1 calc R U . . . H01B_9 H -0.117226 0.839474 0.490725 0.038 Uiso 1 1 calc R U . . . H01C_9 H -0.203979 0.854089 0.448130 0.038 Uiso 1 1 calc R U . . . C1_41 C 0.165(3) 0.626(3) 0.420(3) 0.029(2) Uani 0.43(3) 1 d D U P A 1 H01E_41 H 0.213327 0.659432 0.436465 0.035 Uiso 0.43(3) 1 calc R U P A 1 C2_41 C 0.2228(13) 0.6124(8) 0.3730(5) 0.030(3) Uani 0.43(3) 1 d . U P A 1 H039_41 H 0.175622 0.585902 0.351292 0.046 Uiso 0.43(3) 1 calc R U P A 1 H03A_41 H 0.290077 0.587367 0.379574 0.046 Uiso 0.43(3) 1 calc R U P A 1 H03B_41 H 0.240713 0.655341 0.357111 0.046 Uiso 0.43(3) 1 calc R U P A 1 C3_41 C 0.146(3) 0.5741(17) 0.4610(11) 0.030(4) Uani 0.43(3) 1 d . U P A 1 H01J_41 H 0.087590 0.542969 0.451158 0.045 Uiso 0.43(3) 1 calc R U P A 1 H01K_41 H 0.124334 0.597428 0.491186 0.045 Uiso 0.43(3) 1 calc R U P A 1 H01L_41 H 0.213160 0.548733 0.466778 0.045 Uiso 0.43(3) 1 calc R U P A 1 C1_42 C 0.165(2) 0.626(2) 0.419(3) 0.029(2) Uani 0.57(3) 1 d D U P A 2 H01E_42 H 0.227024 0.655857 0.427845 0.035 Uiso 0.57(3) 1 calc R U P A 2 C2_42 C 0.1862(11) 0.5869(7) 0.3691(3) 0.036(3) Uani 0.57(3) 1 d . U P A 2 H039_42 H 0.126524 0.555059 0.362982 0.054 Uiso 0.57(3) 1 calc R U P A 2 H03A_42 H 0.255338 0.562265 0.371187 0.054 Uiso 0.57(3) 1 calc R U P A 2 H03B_42 H 0.189856 0.619505 0.342142 0.054 Uiso 0.57(3) 1 calc R U P A 2 C3_42 C 0.160(2) 0.5651(13) 0.4532(8) 0.027(3) Uani 0.57(3) 1 d . U P A 2 H01J_42 H 0.108548 0.531911 0.440044 0.040 Uiso 0.57(3) 1 calc R U P A 2 H01K_42 H 0.135677 0.579529 0.485837 0.040 Uiso 0.57(3) 1 calc R U P A 2 H01L_42 H 0.232685 0.544821 0.455714 0.040 Uiso 0.57(3) 1 calc R U P A 2 C1_11 C 0.3790(3) 0.97605(18) 0.05724(14) 0.0269(8) Uani 1 1 d . . . . . H1_11 H 0.333440 0.946748 0.035522 0.032 Uiso 1 1 calc R U . . . C2_11 C 0.3023(4) 1.0098(3) 0.09319(19) 0.0537(14) Uani 1 1 d . . . . . H036_11 H 0.250501 1.038173 0.075236 0.081 Uiso 1 1 calc R U . . . H037_11 H 0.344524 1.037690 0.116002 0.081 Uiso 1 1 calc R U . . . H038_11 H 0.262330 0.975320 0.111628 0.081 Uiso 1 1 calc R U . . . C3_11 C 0.4342(4) 1.0279(2) 0.02447(16) 0.0382(10) Uani 1 1 d . . . . . H026_11 H 0.479461 1.004820 0.000064 0.057 Uiso 1 1 calc R U . . . H027_11 H 0.480135 1.057486 0.044528 0.057 Uiso 1 1 calc R U . . . H028_11 H 0.378459 1.054853 0.007710 0.057 Uiso 1 1 calc R U . . . C1_12 C 0.4814(3) 0.74504(18) 0.12591(14) 0.0254(8) Uani 1 1 d . . . . . H02C_12 H 0.405396 0.736452 0.114044 0.031 Uiso 1 1 calc R U . . . C2_12 C 0.5578(4) 0.7004(2) 0.09613(18) 0.0395(10) Uani 1 1 d . . . . . H01Y_12 H 0.551118 0.711595 0.061237 0.059 Uiso 1 1 calc R U . . . H01Z_12 H 0.538314 0.653028 0.101183 0.059 Uiso 1 1 calc R U . . . H013_12 H 0.633235 0.707867 0.106828 0.059 Uiso 1 1 calc R U . . . C3_12 C 0.4848(4) 0.7274(2) 0.18034(16) 0.0427(10) Uani 1 1 d . . . . . H029_12 H 0.461056 0.680657 0.184925 0.064 Uiso 1 1 calc R U . . . H02A_12 H 0.436034 0.757564 0.198484 0.064 Uiso 1 1 calc R U . . . H02B_12 H 0.559529 0.732566 0.192606 0.064 Uiso 1 1 calc R U . . . C1_13 C -0.0110(3) 0.85192(16) 0.06861(13) 0.0204(7) Uani 1 1 d . . . . . H1_13 H 0.059990 0.863327 0.052498 0.024 Uiso 1 1 calc R U . . . C2_13 C -0.0210(3) 0.89516(18) 0.11468(14) 0.0308(8) Uani 1 1 d . . . . . H01S_13 H -0.014068 0.942819 0.105819 0.046 Uiso 1 1 calc R U . . . H01T_13 H 0.037037 0.883035 0.137826 0.046 Uiso 1 1 calc R U . . . H01U_13 H -0.092226 0.887403 0.129996 0.046 Uiso 1 1 calc R U . . . C3_13 C -0.1019(3) 0.86844(19) 0.03246(13) 0.0270(8) Uani 1 1 d . . . . . H01M_13 H -0.098800 0.916371 0.023975 0.040 Uiso 1 1 calc R U . . . H01N_13 H -0.172703 0.858238 0.047463 0.040 Uiso 1 1 calc R U . . . H01O_13 H -0.092729 0.841324 0.002693 0.040 Uiso 1 1 calc R U . . . C1_14 C 0.1915(3) 0.62717(17) 0.07820(13) 0.0219(7) Uani 1 1 d . . . . . H1_14 H 0.246823 0.656723 0.061895 0.026 Uiso 1 1 calc R U . . . C2_14 C 0.2369(4) 0.6080(2) 0.12812(16) 0.0419(11) Uani 1 1 d . . . . . H02M_14 H 0.305742 0.583581 0.123874 0.063 Uiso 1 1 calc R U . . . H02N_14 H 0.184303 0.579189 0.145267 0.063 Uiso 1 1 calc R U . . . H02O_14 H 0.249830 0.648867 0.147438 0.063 Uiso 1 1 calc R U . . . C3_14 C 0.1763(3) 0.5652(2) 0.04564(16) 0.0342(9) Uani 1 1 d . . . . . H02D_14 H 0.151720 0.579315 0.013004 0.051 Uiso 1 1 calc R U . . . H02E_14 H 0.121519 0.535341 0.060317 0.051 Uiso 1 1 calc R U . . . H02F_14 H 0.245802 0.541077 0.042733 0.051 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 O1_101 0.027(3) 0.023(2) 0.061(3) -0.001(2) -0.002(3) 0.0036(19) C2_101 0.035(5) 0.025(3) 0.075(4) 0.004(3) 0.003(4) -0.002(3) C3_101 0.046(3) 0.041(3) 0.097(5) 0.022(3) -0.008(3) -0.017(2) C4_101 0.040(4) 0.054(3) 0.108(6) 0.009(5) -0.006(4) -0.006(3) C5_101 0.032(3) 0.030(2) 0.074(5) 0.008(3) 0.000(3) 0.003(2) O1_102 0.033(6) 0.024(6) 0.071(6) 0.002(6) 0.000(6) -0.007(5) C2_102 0.035(7) 0.025(6) 0.080(7) 0.007(6) -0.003(6) -0.004(6) C3_102 0.038(6) 0.035(5) 0.089(7) 0.003(6) -0.003(6) -0.006(5) C4_102 0.036(6) 0.043(6) 0.087(7) 0.012(6) -0.007(6) -0.002(6) C5_102 0.034(6) 0.033(6) 0.082(7) 0.006(7) -0.003(7) 0.001(5) O1_2 0.0331(14) 0.0299(13) 0.067(2) -0.0085(16) -0.0058(15) 0.0103(11) C2_2 0.037(2) 0.036(2) 0.063(3) -0.010(2) -0.009(2) 0.0076(18) C3_2 0.034(2) 0.0294(19) 0.073(4) -0.001(2) 0.009(2) 0.0060(16) C4_2 0.033(2) 0.0303(17) 0.051(3) -0.005(2) -0.003(2) 0.0032(15) C5_2 0.036(2) 0.0293(18) 0.061(3) -0.005(2) -0.010(2) 0.0070(16) O1_3 0.0395(15) 0.0437(16) 0.0403(16) 0.0069(13) 0.0133(13) 0.0138(13) C2_3 0.037(2) 0.040(2) 0.039(2) -0.0014(19) 0.0063(18) 0.0106(19) C3_3 0.0278(19) 0.044(2) 0.035(2) -0.0003(18) 0.0046(17) 0.0068(17) C4_3 0.038(2) 0.039(2) 0.037(2) 0.0040(17) 0.0025(17) -0.0026(18) C5_3 0.037(2) 0.038(2) 0.036(2) 0.0006(16) 0.0013(16) 0.0103(18) Ni1_4 0.0159(2) 0.0168(2) 0.0136(2) -0.0003(2) 0.0005(2) -0.00231(18) S2_4 0.0227(4) 0.0211(4) 0.0156(4) 0.0013(3) -0.0005(3) -0.0083(3) S3_4 0.0172(3) 0.0188(4) 0.0153(4) -0.0001(3) -0.0002(3) -0.0035(3) S4_4 0.0159(3) 0.0184(4) 0.0150(4) -0.0001(3) 0.0006(3) -0.0045(3) S5_4 0.0244(4) 0.0278(4) 0.0157(4) -0.0042(3) 0.0033(3) -0.0129(3) K6_4 0.0270(3) 0.0220(3) 0.0326(4) -0.0008(4) -0.0008(4) 0.0045(3) C1_5 0.0141(14) 0.0184(16) 0.0189(16) -0.0011(13) 0.0015(12) -0.0020(12) C2_5 0.0141(14) 0.0129(14) 0.0183(16) -0.0020(12) -0.0017(12) -0.0013(11) N3_5 0.0158(12) 0.0148(13) 0.0160(13) -0.0015(10) 0.0007(10) -0.0003(11) C4_5 0.0234(16) 0.0180(15) 0.0133(15) -0.0014(13) 0.0012(12) 0.0026(13) C5_5 0.0220(16) 0.0179(15) 0.0164(16) -0.0021(12) 0.0051(12) -0.0005(13) N6_5 0.0174(13) 0.0216(14) 0.0152(13) -0.0019(11) 0.0035(10) -0.0054(11) C7_5 0.0155(15) 0.0221(17) 0.0176(16) -0.0050(13) 0.0040(13) -0.0033(13) C8_5 0.0209(17) 0.0197(16) 0.0264(18) -0.0035(14) 0.0028(14) -0.0015(14) C9_5 0.0231(18) 0.0217(17) 0.039(2) -0.0004(16) -0.0012(16) -0.0061(14) C10_5 0.0184(17) 0.034(2) 0.035(2) -0.0026(16) -0.0008(15) -0.0069(15) C11_5 0.0186(16) 0.0322(19) 0.0286(19) 0.0016(15) 0.0009(14) 0.0019(14) C12_5 0.0181(15) 0.0220(17) 0.0236(17) 0.0008(14) 0.0037(13) -0.0002(13) C13_5 0.0155(15) 0.0186(16) 0.0135(15) -0.0008(12) -0.0015(12) -0.0039(13) C14_5 0.0219(16) 0.0184(16) 0.0177(16) -0.0012(13) -0.0020(13) -0.0015(14) C15_5 0.0242(17) 0.0175(16) 0.0238(18) 0.0003(13) -0.0014(14) -0.0028(13) C16_5 0.0196(15) 0.0256(18) 0.0224(17) 0.0001(14) 0.0000(13) -0.0072(14) C17_5 0.0184(15) 0.0228(17) 0.0209(17) -0.0023(14) -0.0005(13) -0.0002(13) C18_5 0.0196(16) 0.0182(16) 0.0158(15) -0.0016(12) -0.0014(12) -0.0020(13) C1_6 0.0170(15) 0.0154(15) 0.0190(16) 0.0013(12) 0.0009(12) -0.0028(13) C2_6 0.0127(14) 0.0122(14) 0.0189(16) -0.0024(12) 0.0012(12) 0.0010(11) N3_6 0.0176(13) 0.0203(14) 0.0165(13) 0.0011(11) -0.0005(11) -0.0030(11) C4_6 0.0226(17) 0.0223(16) 0.0161(16) 0.0003(13) -0.0043(13) 0.0024(14) C5_6 0.0214(15) 0.0205(16) 0.0172(16) 0.0039(13) 0.0014(13) 0.0035(14) N6_6 0.0187(13) 0.0189(13) 0.0133(13) 0.0031(11) -0.0005(10) -0.0012(11) C7_6 0.0177(15) 0.0189(16) 0.0150(15) 0.0034(12) 0.0012(12) -0.0022(13) C8_6 0.0257(17) 0.0171(16) 0.0229(17) 0.0019(14) 0.0057(14) 0.0004(14) C9_6 0.033(2) 0.0189(17) 0.0268(19) -0.0009(14) 0.0043(16) -0.0066(14) C10_6 0.0237(17) 0.0282(18) 0.0241(17) 0.0008(15) -0.0012(14) -0.0072(15) C11_6 0.0178(16) 0.0300(19) 0.0224(17) 0.0030(15) 0.0004(13) -0.0010(14) C12_6 0.0221(16) 0.0184(16) 0.0157(15) 0.0032(13) 0.0047(13) 0.0011(13) C13_6 0.0141(15) 0.0196(16) 0.0171(15) -0.0021(13) -0.0047(12) -0.0022(12) C14_6 0.0194(15) 0.0240(17) 0.0201(16) 0.0003(14) -0.0028(13) -0.0002(14) C15_6 0.0183(16) 0.0284(18) 0.0265(18) -0.0026(14) -0.0002(14) 0.0029(14) C16_6 0.0169(16) 0.0304(19) 0.0303(19) 0.0011(15) 0.0012(14) -0.0043(14) C17_6 0.0223(17) 0.0209(16) 0.0293(19) -0.0007(14) -0.0029(15) -0.0032(14) C18_6 0.0191(16) 0.0215(16) 0.0208(17) 0.0000(13) -0.0025(13) -0.0006(13) C1_7 0.0226(17) 0.0207(17) 0.034(2) -0.0030(15) 0.0026(15) -0.0013(14) C2_7 0.032(2) 0.035(2) 0.035(2) -0.0102(17) 0.0062(17) 0.0007(17) C3_7 0.050(3) 0.049(3) 0.054(3) -0.020(2) -0.017(2) 0.032(2) C1_8 0.0206(16) 0.0229(18) 0.032(2) -0.0064(15) -0.0023(15) 0.0021(14) C2_8 0.042(2) 0.031(2) 0.040(2) -0.0120(18) -0.0054(18) 0.0063(18) C3_8 0.036(2) 0.0246(19) 0.053(3) -0.0010(18) -0.010(2) 0.0013(17) C1_9 0.0181(16) 0.0196(17) 0.0295(19) 0.0009(14) 0.0040(14) -0.0002(13) C2_9 0.042(2) 0.0235(18) 0.032(2) 0.0086(15) 0.0126(17) 0.0123(16) C3_9 0.0280(18) 0.0219(17) 0.0266(18) 0.0000(14) 0.0036(15) 0.0035(14) C1_41 0.030(4) 0.020(4) 0.037(5) 0.004(4) 0.004(4) 0.004(4) C2_41 0.032(5) 0.022(5) 0.037(4) 0.007(4) 0.006(4) 0.009(4) C3_41 0.035(9) 0.025(7) 0.030(8) 0.007(6) -0.005(6) 0.010(6) C1_42 0.030(4) 0.020(4) 0.038(4) 0.004(3) 0.004(3) 0.002(3) C2_42 0.040(5) 0.030(5) 0.037(4) 0.007(4) 0.007(4) 0.017(4) C3_42 0.027(6) 0.027(6) 0.027(6) 0.005(5) -0.001(4) 0.004(5) C1_11 0.0217(17) 0.0212(17) 0.038(2) -0.0019(15) -0.0033(15) 0.0002(14) C2_11 0.049(3) 0.059(3) 0.053(3) 0.023(2) 0.021(2) 0.032(2) C3_11 0.036(2) 0.037(2) 0.041(2) 0.0094(18) -0.0006(19) 0.0047(18) C1_12 0.0197(16) 0.0219(17) 0.035(2) 0.0037(15) 0.0037(15) 0.0000(13) C2_12 0.043(2) 0.0233(19) 0.052(3) -0.0011(18) 0.017(2) 0.0019(17) C3_12 0.056(3) 0.033(2) 0.039(2) 0.0128(19) 0.005(2) -0.002(2) C1_13 0.0199(16) 0.0154(16) 0.0257(17) -0.0014(13) 0.0008(14) -0.0012(12) C2_13 0.041(2) 0.0204(17) 0.031(2) -0.0044(15) -0.0092(17) 0.0078(16) C3_13 0.0314(19) 0.0225(17) 0.0270(19) 0.0015(15) -0.0054(15) 0.0020(15) C1_14 0.0218(16) 0.0159(16) 0.0279(18) -0.0010(14) 0.0035(14) 0.0029(13) C2_14 0.045(2) 0.046(3) 0.034(2) -0.0043(19) -0.0053(19) 0.023(2) C3_14 0.035(2) 0.0242(19) 0.044(2) -0.0096(18) 0.0076(18) -0.0017(16) 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' O O 0.0492 0.0322 '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' K K 0.3868 1.0657 '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 C2_101 O1_101 C5_101 109.5(9) . . ? C2_101 O1_101 K6_4 144.5(7) . . ? C5_101 O1_101 K6_4 105.9(6) . . ? O1_101 C2_101 C3_101 106.2(10) . . ? O1_101 C2_101 H02V_101 110.5 . . ? C3_101 C2_101 H02V_101 110.5 . . ? O1_101 C2_101 H02W_101 110.5 . . ? C3_101 C2_101 H02W_101 110.5 . . ? H02V_101 C2_101 H02W_101 108.7 . . ? C4_101 C3_101 C2_101 103.4(8) . . ? C4_101 C3_101 H03E_101 111.1 . . ? C2_101 C3_101 H03E_101 111.1 . . ? C4_101 C3_101 H03F_101 111.1 . . ? C2_101 C3_101 H03F_101 111.1 . . ? H03E_101 C3_101 H03F_101 109.0 . . ? C3_101 C4_101 C5_101 103.8(7) . . ? C3_101 C4_101 H03C_101 111.0 . . ? C5_101 C4_101 H03C_101 111.0 . . ? C3_101 C4_101 H03D_101 111.0 . . ? C5_101 C4_101 H03D_101 111.0 . . ? H03C_101 C4_101 H03D_101 109.0 . . ? O1_101 C5_101 C4_101 107.0(8) . . ? O1_101 C5_101 K6_4 49.5(5) . . ? C4_101 C5_101 K6_4 156.4(6) . . ? O1_101 C5_101 H030_101 110.3 . . ? C4_101 C5_101 H030_101 110.3 . . ? K6_4 C5_101 H030_101 83.3 . . ? O1_101 C5_101 H031_101 110.3 . . ? C4_101 C5_101 H031_101 110.3 . . ? K6_4 C5_101 H031_101 81.6 . . ? H030_101 C5_101 H031_101 108.6 . . ? C5_102 O1_102 C2_102 102(4) . . ? C5_102 O1_102 K6_4 113(3) . . ? C2_102 O1_102 K6_4 137(3) . . ? C3_102 C2_102 O1_102 95(5) . . ? C3_102 C2_102 H02V_102 112.8 . . ? O1_102 C2_102 H02V_102 112.8 . . ? C3_102 C2_102 H02W_102 112.8 . . ? O1_102 C2_102 H02W_102 112.8 . . ? H02V_102 C2_102 H02W_102 110.2 . . ? C4_102 C3_102 C2_102 110(4) . . ? C4_102 C3_102 H03E_102 109.7 . . ? C2_102 C3_102 H03E_102 109.7 . . ? C4_102 C3_102 H03F_102 109.7 . . ? C2_102 C3_102 H03F_102 109.7 . . ? H03E_102 C3_102 H03F_102 108.2 . . ? C3_102 C4_102 C5_102 112(4) . . ? C3_102 C4_102 H03C_102 109.3 . . ? C5_102 C4_102 H03C_102 109.3 . . ? C3_102 C4_102 H03D_102 109.3 . . ? C5_102 C4_102 H03D_102 109.3 . . ? H03C_102 C4_102 H03D_102 108.0 . . ? O1_102 C5_102 C4_102 88(4) . . ? O1_102 C5_102 K6_4 46(3) . . ? C4_102 C5_102 K6_4 128(3) . . ? O1_102 C5_102 H030_102 114.1 . . ? C4_102 C5_102 H030_102 114.1 . . ? K6_4 C5_102 H030_102 76.4 . . ? O1_102 C5_102 H031_102 114.1 . . ? C4_102 C5_102 H031_102 114.1 . . ? K6_4 C5_102 H031_102 107.3 . . ? H030_102 C5_102 H031_102 111.2 . . ? C2_2 O1_2 C5_2 107.9(3) . . ? C2_2 O1_2 K6_4 137.3(2) . . ? C5_2 O1_2 K6_4 114.7(2) . . ? O1_2 C2_2 C3_2 105.6(4) . . ? O1_2 C2_2 H02R_2 110.6 . . ? C3_2 C2_2 H02R_2 110.6 . . ? O1_2 C2_2 H02S_2 110.6 . . ? C3_2 C2_2 H02S_2 110.6 . . ? H02R_2 C2_2 H02S_2 108.8 . . ? C2_2 C3_2 C4_2 101.8(4) . . ? C2_2 C3_2 H02P_2 111.4 . . ? C4_2 C3_2 H02P_2 111.4 . . ? C2_2 C3_2 H02Q_2 111.4 . . ? C4_2 C3_2 H02Q_2 111.4 . . ? H02P_2 C3_2 H02Q_2 109.3 . . ? C5_2 C4_2 C3_2 103.1(3) . . ? C5_2 C4_2 H024_2 111.1 . . ? C3_2 C4_2 H024_2 111.1 . . ? C5_2 C4_2 H025_2 111.1 . . ? C3_2 C4_2 H025_2 111.1 . . ? H024_2 C4_2 H025_2 109.1 . . ? O1_2 C5_2 C4_2 107.4(3) . . ? O1_2 C5_2 K6_4 43.51(16) . . ? C4_2 C5_2 K6_4 150.5(3) . . ? O1_2 C5_2 H032_2 110.2 . . ? C4_2 C5_2 H032_2 110.2 . . ? K6_4 C5_2 H032_2 82.9 . . ? O1_2 C5_2 H033_2 110.2 . . ? C4_2 C5_2 H033_2 110.2 . . ? K6_4 C5_2 H033_2 88.9 . . ? H032_2 C5_2 H033_2 108.5 . . ? C5_3 O1_3 C2_3 108.8(3) . . ? O1_3 C2_3 C3_3 106.1(3) . . ? O1_3 C2_3 H02T_3 110.5 . . ? C3_3 C2_3 H02T_3 110.5 . . ? O1_3 C2_3 H02U_3 110.5 . . ? C3_3 C2_3 H02U_3 110.5 . . ? H02T_3 C2_3 H02U_3 108.7 . . ? C2_3 C3_3 C4_3 101.8(3) . . ? C2_3 C3_3 H020_3 111.4 . . ? C4_3 C3_3 H020_3 111.4 . . ? C2_3 C3_3 H021_3 111.4 . . ? C4_3 C3_3 H021_3 111.4 . . ? H020_3 C3_3 H021_3 109.3 . . ? C3_3 C4_3 C5_3 101.0(3) . . ? C3_3 C4_3 H034_3 111.6 . . ? C5_3 C4_3 H034_3 111.6 . . ? C3_3 C4_3 H035_3 111.6 . . ? C5_3 C4_3 H035_3 111.6 . . ? H034_3 C4_3 H035_3 109.4 . . ? O1_3 C5_3 C4_3 106.2(3) . . ? O1_3 C5_3 H022_3 110.5 . . ? C4_3 C5_3 H022_3 110.5 . . ? O1_3 C5_3 H023_3 110.5 . . ? C4_3 C5_3 H023_3 110.5 . . ? H022_3 C5_3 H023_3 108.7 . . ? S5_4 Ni1_4 S2_4 100.57(3) . . ? S5_4 Ni1_4 S4_4 79.42(3) . . ? S2_4 Ni1_4 S4_4 177.04(4) . . ? S5_4 Ni1_4 S3_4 173.60(4) . . ? S2_4 Ni1_4 S3_4 79.27(3) . . ? S4_4 Ni1_4 S3_4 100.41(3) . . ? S5_4 Ni1_4 K6_4 106.61(3) . . ? S2_4 Ni1_4 K6_4 110.03(3) . . ? S4_4 Ni1_4 K6_4 67.24(3) . . ? S3_4 Ni1_4 K6_4 67.70(3) . . ? C1_6 S2_4 Ni1_4 87.70(11) . . ? C1_6 S3_4 Ni1_4 86.83(11) . . ? C1_6 S3_4 K6_4 110.59(11) . . ? Ni1_4 S3_4 K6_4 73.43(3) . . ? C1_5 S4_4 Ni1_4 87.51(11) . . ? C1_5 S4_4 K6_4 108.66(11) . . ? Ni1_4 S4_4 K6_4 74.05(3) . . ? C1_5 S5_4 Ni1_4 88.07(11) . . ? O1_2 K6_4 O1_101 93.03(18) . . ? O1_2 K6_4 O1_102 97.8(10) . . ? O1_2 K6_4 S4_4 148.94(9) . . ? O1_101 K6_4 S4_4 94.7(2) . . ? O1_102 K6_4 S4_4 90.1(12) . . ? O1_2 K6_4 S3_4 146.02(9) . . ? O1_101 K6_4 S3_4 95.3(2) . . ? O1_102 K6_4 S3_4 91.8(13) . . ? S4_4 K6_4 S3_4 62.81(2) . . ? O1_2 K6_4 Ni1_4 147.03(6) . . ? O1_101 K6_4 Ni1_4 119.92(17) . . ? O1_102 K6_4 Ni1_4 115.2(10) . . ? S4_4 K6_4 Ni1_4 38.707(18) . . ? S3_4 K6_4 Ni1_4 38.870(18) . . ? O1_2 K6_4 C5_101 117.49(16) . . ? O1_101 K6_4 C5_101 24.6(2) . . ? S4_4 K6_4 C5_101 72.58(14) . . ? S3_4 K6_4 C5_101 75.94(16) . . ? Ni1_4 K6_4 C5_101 95.47(15) . . ? O1_2 K6_4 C2_8 74.56(10) . . ? O1_101 K6_4 C2_8 143.7(3) . . ? O1_102 K6_4 C2_8 146.2(16) . . ? S4_4 K6_4 C2_8 113.57(8) . . ? S3_4 K6_4 C2_8 79.39(7) . . ? Ni1_4 K6_4 C2_8 77.47(7) . . ? C5_101 K6_4 C2_8 147.72(18) . . ? O1_2 K6_4 C5_102 117.6(7) . . ? O1_102 K6_4 C5_102 21.2(13) . . ? S4_4 K6_4 C5_102 76.8(8) . . ? S3_4 K6_4 C5_102 71.1(7) . . ? Ni1_4 K6_4 C5_102 95.1(7) . . ? C2_8 K6_4 C5_102 139.5(8) . . ? O1_2 K6_4 C3_12 73.79(10) . . ? O1_101 K6_4 C3_12 140.0(3) . . ? O1_102 K6_4 C3_12 140.7(17) . . ? S4_4 K6_4 C3_12 81.07(8) . . ? S3_4 K6_4 C3_12 116.88(8) . . ? Ni1_4 K6_4 C3_12 80.47(8) . . ? C5_101 K6_4 C3_12 140.82(17) . . ? C2_8 K6_4 C3_12 69.80(10) . . ? C5_102 K6_4 C3_12 149.0(8) . . ? O1_2 K6_4 C5_2 21.75(9) . . ? O1_101 K6_4 C5_2 72.08(19) . . ? O1_102 K6_4 C5_2 76.7(10) . . ? S4_4 K6_4 C5_2 142.39(9) . . ? S3_4 K6_4 C5_2 150.72(10) . . ? Ni1_4 K6_4 C5_2 167.20(8) . . ? C5_101 K6_4 C5_2 96.24(16) . . ? C2_8 K6_4 C5_2 95.17(10) . . ? C5_102 K6_4 C5_2 97.3(7) . . ? C3_12 K6_4 C5_2 87.18(11) . . ? O1_2 K6_4 C2_41 82.56(19) . . ? O1_101 K6_4 C2_41 74.4(5) . . ? S4_4 K6_4 C2_41 128.48(18) . . ? S3_4 K6_4 C2_41 68.20(19) . . ? Ni1_4 K6_4 C2_41 104.1(2) . . ? C5_101 K6_4 C2_41 81.3(3) . . ? C2_8 K6_4 C2_41 70.3(3) . . ? C3_12 K6_4 C2_41 137.7(3) . . ? C5_2 K6_4 C2_41 82.8(2) . . ? C2_5 C1_5 S5_4 127.6(2) . . ? C2_5 C1_5 S4_4 127.6(3) . . ? S5_4 C1_5 S4_4 104.81(17) . . ? C1_5 C2_5 N3_5 128.3(3) . . ? C1_5 C2_5 N6_5 127.6(3) . . ? N3_5 C2_5 N6_5 104.2(3) . . ? C4_5 N3_5 C2_5 109.6(3) . . ? C4_5 N3_5 C13_5 125.1(3) . . ? C2_5 N3_5 C13_5 125.1(3) . . ? C5_5 C4_5 N3_5 108.7(3) . . ? C5_5 C4_5 H4_5 125.7 . . ? N3_5 C4_5 H4_5 125.7 . . ? C4_5 C5_5 N6_5 108.0(3) . . ? C4_5 C5_5 H5_5 126.0 . . ? N6_5 C5_5 H5_5 126.0 . . ? C2_5 N6_5 C5_5 109.5(3) . . ? C2_5 N6_5 C7_5 126.5(3) . . ? C5_5 N6_5 C7_5 121.0(3) . . ? C12_5 C7_5 C8_5 122.4(3) . . ? C12_5 C7_5 N6_5 119.5(3) . . ? C8_5 C7_5 N6_5 118.0(3) . . ? C9_5 C8_5 C7_5 117.3(3) . . ? C9_5 C8_5 C1_11 121.4(3) . . ? C7_5 C8_5 C1_11 121.3(3) . . ? C10_5 C9_5 C8_5 121.2(3) . . ? C10_5 C9_5 H01I_5 119.4 . . ? C8_5 C9_5 H01I_5 119.4 . . ? C9_5 C10_5 C11_5 120.7(3) . . ? C9_5 C10_5 H01F_5 119.7 . . ? C11_5 C10_5 H01F_5 119.7 . . ? C10_5 C11_5 C12_5 120.4(3) . . ? C10_5 C11_5 H01H_5 119.8 . . ? C12_5 C11_5 H01H_5 119.8 . . ? C7_5 C12_5 C11_5 118.0(3) . . ? C7_5 C12_5 C1_12 122.6(3) . . ? C11_5 C12_5 C1_12 119.5(3) . . ? C14_5 C13_5 C18_5 122.6(3) . . ? C14_5 C13_5 N3_5 118.2(3) . . ? C18_5 C13_5 N3_5 119.1(3) . . ? C15_5 C14_5 C13_5 117.5(3) . . ? C15_5 C14_5 C1_14 120.9(3) . . ? C13_5 C14_5 C1_14 121.5(3) . . ? C16_5 C15_5 C14_5 120.8(3) . . ? C16_5 C15_5 H15_5 119.6 . . ? C14_5 C15_5 H15_5 119.6 . . ? C15_5 C16_5 C17_5 120.6(3) . . ? C15_5 C16_5 H16_5 119.7 . . ? C17_5 C16_5 H16_5 119.7 . . ? C16_5 C17_5 C18_5 120.7(3) . . ? C16_5 C17_5 H01D_5 119.7 . . ? C18_5 C17_5 H01D_5 119.7 . . ? C17_5 C18_5 C13_5 117.6(3) . . ? C17_5 C18_5 C1_13 120.5(3) . . ? C13_5 C18_5 C1_13 121.9(3) . . ? C2_6 C1_6 S2_4 126.5(2) . . ? C2_6 C1_6 S3_4 127.6(2) . . ? S2_4 C1_6 S3_4 105.76(18) . . ? C1_6 C2_6 N6_6 127.6(3) . . ? C1_6 C2_6 N3_6 127.4(3) . . ? N6_6 C2_6 N3_6 105.0(3) . . ? C2_6 N3_6 C4_6 109.2(3) . . ? C2_6 N3_6 C13_6 126.7(3) . . ? C4_6 N3_6 C13_6 120.2(3) . . ? C5_6 C4_6 N3_6 107.8(3) . . ? C5_6 C4_6 H4_6 126.1 . . ? N3_6 C4_6 H4_6 126.1 . . ? C4_6 C5_6 N6_6 108.6(3) . . ? C4_6 C5_6 H5_6 125.7 . . ? N6_6 C5_6 H5_6 125.7 . . ? C2_6 N6_6 C5_6 109.5(3) . . ? C2_6 N6_6 C7_6 126.4(3) . . ? C5_6 N6_6 C7_6 123.8(3) . . ? C12_6 C7_6 C8_6 122.2(3) . . ? C12_6 C7_6 N6_6 119.5(3) . . ? C8_6 C7_6 N6_6 118.3(3) . . ? C9_6 C8_6 C7_6 117.5(3) . . ? C9_6 C8_6 C1_41 121(3) . . ? C7_6 C8_6 C1_41 121(3) . . ? C9_6 C8_6 C1_42 120.9(19) . . ? C7_6 C8_6 C1_42 121.6(19) . . ? C10_6 C9_6 C8_6 121.0(3) . . ? C10_6 C9_6 H9_6 119.5 . . ? C8_6 C9_6 H9_6 119.5 . . ? C9_6 C10_6 C11_6 120.1(3) . . ? C9_6 C10_6 H10_6 119.9 . . ? C11_6 C10_6 H10_6 119.9 . . ? C10_6 C11_6 C12_6 121.2(3) . . ? C10_6 C11_6 H11_6 119.4 . . ? C12_6 C11_6 H11_6 119.4 . . ? C11_6 C12_6 C7_6 117.8(3) . . ? C11_6 C12_6 C1_9 119.6(3) . . ? C7_6 C12_6 C1_9 122.6(3) . . ? C14_6 C13_6 C18_6 122.4(3) . . ? C14_6 C13_6 N3_6 119.6(3) . . ? C18_6 C13_6 N3_6 117.9(3) . . ? C15_6 C14_6 C13_6 117.9(3) . . ? C15_6 C14_6 C1_8 119.9(3) . . ? C13_6 C14_6 C1_8 122.2(3) . . ? C16_6 C15_6 C14_6 120.4(3) . . ? C16_6 C15_6 H15_6 119.8 . . ? C14_6 C15_6 H15_6 119.8 . . ? C17_6 C16_6 C15_6 120.7(3) . . ? C17_6 C16_6 H16_6 119.6 . . ? C15_6 C16_6 H16_6 119.6 . . ? C16_6 C17_6 C18_6 121.1(3) . . ? C16_6 C17_6 H17_6 119.4 . . ? C18_6 C17_6 H17_6 119.4 . . ? C17_6 C18_6 C13_6 117.4(3) . . ? C17_6 C18_6 C1_7 121.9(3) . . ? C13_6 C18_6 C1_7 120.7(3) . . ? C3_7 C1_7 C18_6 111.2(3) . . ? C3_7 C1_7 C2_7 110.4(3) . . ? C18_6 C1_7 C2_7 113.0(3) . . ? C3_7 C1_7 H01G_7 107.3 . . ? C18_6 C1_7 H01G_7 107.3 . . ? C2_7 C1_7 H01G_7 107.3 . . ? C1_7 C2_7 H01P_7 109.5 . . ? C1_7 C2_7 H01Q_7 109.5 . . ? H01P_7 C2_7 H01Q_7 109.5 . . ? C1_7 C2_7 H01R_7 109.5 . . ? H01P_7 C2_7 H01R_7 109.5 . . ? H01Q_7 C2_7 H01R_7 109.5 . . ? C1_7 C3_7 H02X_7 109.5 . . ? C1_7 C3_7 H02Y_7 109.5 . . ? H02X_7 C3_7 H02Y_7 109.5 . . ? C1_7 C3_7 H02Z_7 109.5 . . ? H02X_7 C3_7 H02Z_7 109.5 . . ? H02Y_7 C3_7 H02Z_7 109.5 . . ? C3_8 C1_8 C14_6 111.4(3) . . ? C3_8 C1_8 C2_8 110.6(3) . . ? C14_6 C1_8 C2_8 111.7(3) . . ? C3_8 C1_8 H1_8 107.7 . . ? C14_6 C1_8 H1_8 107.7 . . ? C2_8 C1_8 H1_8 107.7 . . ? C1_8 C2_8 K6_4 128.9(3) . . ? C1_8 C2_8 H02J_8 109.5 . . ? K6_4 C2_8 H02J_8 61.4 . . ? C1_8 C2_8 H02K_8 109.5 . . ? K6_4 C2_8 H02K_8 48.2 . . ? H02J_8 C2_8 H02K_8 109.5 . . ? C1_8 C2_8 H02L_8 109.5 . . ? K6_4 C2_8 H02L_8 121.1 . . ? H02J_8 C2_8 H02L_8 109.5 . . ? H02K_8 C2_8 H02L_8 109.5 . . ? C1_8 C3_8 H02G_8 109.5 . . ? C1_8 C3_8 H02H_8 109.5 . . ? H02G_8 C3_8 H02H_8 109.5 . . ? C1_8 C3_8 H02I_8 109.5 . . ? H02G_8 C3_8 H02I_8 109.5 . . ? H02H_8 C3_8 H02I_8 109.5 . . ? C12_6 C1_9 C2_9 111.8(3) . . ? C12_6 C1_9 C3_9 110.4(3) . . ? C2_9 C1_9 C3_9 110.2(3) . . ? C12_6 C1_9 H1_9 108.1 . . ? C2_9 C1_9 H1_9 108.1 . . ? C3_9 C1_9 H1_9 108.1 . . ? C1_9 C2_9 H01V_9 109.5 . . ? C1_9 C2_9 H01W_9 109.5 . . ? H01V_9 C2_9 H01W_9 109.5 . . ? C1_9 C2_9 H01X_9 109.5 . . ? H01V_9 C2_9 H01X_9 109.5 . . ? H01W_9 C2_9 H01X_9 109.5 . . ? C1_9 C3_9 H01A_9 109.5 . . ? C1_9 C3_9 H01B_9 109.5 . . ? H01A_9 C3_9 H01B_9 109.5 . . ? C1_9 C3_9 H01C_9 109.5 . . ? H01A_9 C3_9 H01C_9 109.5 . . ? H01B_9 C3_9 H01C_9 109.5 . . ? C2_41 C1_41 C8_6 114(5) . . ? C2_41 C1_41 C3_41 125(3) . . ? C8_6 C1_41 C3_41 107(4) . . ? C2_41 C1_41 H01E_41 102.5 . . ? C8_6 C1_41 H01E_41 102.5 . . ? C3_41 C1_41 H01E_41 102.5 . . ? C1_41 C2_41 K6_4 147.1(16) . . ? C1_41 C2_41 H039_41 109.5 . . ? K6_4 C2_41 H039_41 71.1 . . ? C1_41 C2_41 H03A_41 109.5 . . ? K6_4 C2_41 H03A_41 100.7 . . ? H039_41 C2_41 H03A_41 109.5 . . ? C1_41 C2_41 H03B_41 109.5 . . ? K6_4 C2_41 H03B_41 45.6 . . ? H039_41 C2_41 H03B_41 109.5 . . ? H03A_41 C2_41 H03B_41 109.5 . . ? C1_41 C3_41 H01J_41 109.5 . . ? C1_41 C3_41 H01K_41 109.5 . . ? H01J_41 C3_41 H01K_41 109.5 . . ? C1_41 C3_41 H01L_41 109.5 . . ? H01J_41 C3_41 H01L_41 109.5 . . ? H01K_41 C3_41 H01L_41 109.5 . . ? C3_42 C1_42 C8_6 116(3) . . ? C3_42 C1_42 C2_42 99(3) . . ? C8_6 C1_42 C2_42 108(4) . . ? C3_42 C1_42 H01E_42 111.3 . . ? C8_6 C1_42 H01E_42 111.3 . . ? C2_42 C1_42 H01E_42 111.3 . . ? C1_42 C2_42 H039_42 109.5 . . ? C1_42 C2_42 H03A_42 109.5 . . ? H039_42 C2_42 H03A_42 109.5 . . ? C1_42 C2_42 H03B_42 109.5 . . ? H039_42 C2_42 H03B_42 109.5 . . ? H03A_42 C2_42 H03B_42 109.5 . . ? C1_42 C3_42 H01J_42 109.5 . . ? C1_42 C3_42 H01K_42 109.5 . . ? H01J_42 C3_42 H01K_42 109.5 . . ? C1_42 C3_42 H01L_42 109.5 . . ? H01J_42 C3_42 H01L_42 109.5 . . ? H01K_42 C3_42 H01L_42 109.5 . . ? C2_11 C1_11 C8_5 110.9(3) . . ? C2_11 C1_11 C3_11 110.9(3) . . ? C8_5 C1_11 C3_11 113.4(3) . . ? C2_11 C1_11 H1_11 107.1 . . ? C8_5 C1_11 H1_11 107.1 . . ? C3_11 C1_11 H1_11 107.1 . . ? C1_11 C2_11 H036_11 109.5 . . ? C1_11 C2_11 H037_11 109.5 . . ? H036_11 C2_11 H037_11 109.5 . . ? C1_11 C2_11 H038_11 109.5 . . ? H036_11 C2_11 H038_11 109.5 . . ? H037_11 C2_11 H038_11 109.5 . . ? C1_11 C3_11 H026_11 109.5 . . ? C1_11 C3_11 H027_11 109.5 . . ? H026_11 C3_11 H027_11 109.5 . . ? C1_11 C3_11 H028_11 109.5 . . ? H026_11 C3_11 H028_11 109.5 . . ? H027_11 C3_11 H028_11 109.5 . . ? C2_12 C1_12 C3_12 111.6(3) . . ? C2_12 C1_12 C12_5 111.0(3) . . ? C3_12 C1_12 C12_5 111.5(3) . . ? C2_12 C1_12 H02C_12 107.5 . . ? C3_12 C1_12 H02C_12 107.5 . . ? C12_5 C1_12 H02C_12 107.5 . . ? C1_12 C2_12 H01Y_12 109.5 . . ? C1_12 C2_12 H01Z_12 109.5 . . ? H01Y_12 C2_12 H01Z_12 109.5 . . ? C1_12 C2_12 H013_12 109.5 . . ? H01Y_12 C2_12 H013_12 109.5 . . ? H01Z_12 C2_12 H013_12 109.5 . . ? C1_12 C3_12 K6_4 126.4(3) . . ? C1_12 C3_12 H029_12 109.5 . . ? K6_4 C3_12 H029_12 50.4 . . ? C1_12 C3_12 H02A_12 109.5 . . ? K6_4 C3_12 H02A_12 59.1 . . ? H029_12 C3_12 H02A_12 109.5 . . ? C1_12 C3_12 H02B_12 109.5 . . ? K6_4 C3_12 H02B_12 123.8 . . ? H029_12 C3_12 H02B_12 109.5 . . ? H02A_12 C3_12 H02B_12 109.5 . . ? C3_13 C1_13 C2_13 110.6(3) . . ? C3_13 C1_13 C18_5 110.8(3) . . ? C2_13 C1_13 C18_5 112.2(3) . . ? C3_13 C1_13 H1_13 107.7 . . ? C2_13 C1_13 H1_13 107.7 . . ? C18_5 C1_13 H1_13 107.7 . . ? C1_13 C2_13 H01S_13 109.5 . . ? C1_13 C2_13 H01T_13 109.5 . . ? H01S_13 C2_13 H01T_13 109.5 . . ? C1_13 C2_13 H01U_13 109.5 . . ? H01S_13 C2_13 H01U_13 109.5 . . ? H01T_13 C2_13 H01U_13 109.5 . . ? C1_13 C3_13 H01M_13 109.5 . . ? C1_13 C3_13 H01N_13 109.5 . . ? H01M_13 C3_13 H01N_13 109.5 . . ? C1_13 C3_13 H01O_13 109.5 . . ? H01M_13 C3_13 H01O_13 109.5 . . ? H01N_13 C3_13 H01O_13 109.5 . . ? C2_14 C1_14 C14_5 111.2(3) . . ? C2_14 C1_14 C3_14 111.3(3) . . ? C14_5 C1_14 C3_14 112.2(3) . . ? C2_14 C1_14 H1_14 107.3 . . ? C14_5 C1_14 H1_14 107.3 . . ? C3_14 C1_14 H1_14 107.3 . . ? C1_14 C2_14 K6_4 144.1(3) . . ? C1_14 C2_14 H02M_14 109.5 . . ? K6_4 C2_14 H02M_14 99.8 . . ? C1_14 C2_14 H02N_14 109.5 . . ? K6_4 C2_14 H02N_14 78.5 . . ? H02M_14 C2_14 H02N_14 109.5 . . ? C1_14 C2_14 H02O_14 109.5 . . ? K6_4 C2_14 H02O_14 38.7 . . ? H02M_14 C2_14 H02O_14 109.5 . . ? H02N_14 C2_14 H02O_14 109.5 . . ? C1_14 C3_14 H02D_14 109.5 . . ? C1_14 C3_14 H02E_14 109.5 . . ? H02D_14 C3_14 H02E_14 109.5 . . ? C1_14 C3_14 H02F_14 109.5 . . ? H02D_14 C3_14 H02F_14 109.5 . . ? H02E_14 C3_14 H02F_14 109.5 . . ? 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 O1_101 C2_101 1.392(19) . ? O1_101 C5_101 1.463(11) . ? O1_101 K6_4 2.676(12) . ? C2_101 C3_101 1.548(13) . ? C2_101 H02V_101 0.9900 . ? C2_101 H02W_101 0.9900 . ? C3_101 C4_101 1.475(13) . ? C3_101 H03E_101 0.9900 . ? C3_101 H03F_101 0.9900 . ? C4_101 C5_101 1.516(15) . ? C4_101 H03C_101 0.9900 . ? C4_101 H03D_101 0.9900 . ? C5_101 K6_4 3.384(9) . ? C5_101 H030_101 0.9900 . ? C5_101 H031_101 0.9900 . ? O1_102 C5_102 1.38(6) . ? O1_102 C2_102 1.59(9) . ? O1_102 K6_4 2.74(5) . ? C2_102 C3_102 1.51(8) . ? C2_102 H02V_102 0.9900 . ? C2_102 H02W_102 0.9900 . ? C3_102 C4_102 1.13(5) . ? C3_102 H03E_102 0.9900 . ? C3_102 H03F_102 0.9900 . ? C4_102 C5_102 1.66(7) . ? C4_102 H03C_102 0.9900 . ? C4_102 H03D_102 0.9900 . ? C5_102 K6_4 3.51(4) . ? C5_102 H030_102 0.9900 . ? C5_102 H031_102 0.9900 . ? O1_2 C2_2 1.429(5) . ? O1_2 C5_2 1.436(5) . ? O1_2 K6_4 2.668(3) . ? C2_2 C3_2 1.491(6) . ? C2_2 H02R_2 0.9900 . ? C2_2 H02S_2 0.9900 . ? C3_2 C4_2 1.504(6) . ? C3_2 H02P_2 0.9900 . ? C3_2 H02Q_2 0.9900 . ? C4_2 C5_2 1.501(5) . ? C4_2 H024_2 0.9900 . ? C4_2 H025_2 0.9900 . ? C5_2 K6_4 3.519(4) . ? C5_2 H032_2 0.9900 . ? C5_2 H033_2 0.9900 . ? O1_3 C5_3 1.430(5) . ? O1_3 C2_3 1.440(5) . ? C2_3 C3_3 1.494(6) . ? C2_3 H02T_3 0.9900 . ? C2_3 H02U_3 0.9900 . ? C3_3 C4_3 1.517(6) . ? C3_3 H020_3 0.9900 . ? C3_3 H021_3 0.9900 . ? C4_3 C5_3 1.522(6) . ? C4_3 H034_3 0.9900 . ? C4_3 H035_3 0.9900 . ? C5_3 H022_3 0.9900 . ? C5_3 H023_3 0.9900 . ? Ni1_4 S5_4 2.1784(10) . ? Ni1_4 S2_4 2.1804(10) . ? Ni1_4 S4_4 2.1842(9) . ? Ni1_4 S3_4 2.1989(9) . ? Ni1_4 K6_4 3.3584(8) . ? S2_4 C1_6 1.746(3) . ? S3_4 C1_6 1.757(3) . ? S3_4 K6_4 3.2420(11) . ? S4_4 C1_5 1.766(3) . ? S4_4 K6_4 3.2209(11) . ? S5_4 C1_5 1.751(3) . ? K6_4 C2_8 3.416(4) . ? K6_4 C3_12 3.517(5) . ? K6_4 C2_41 3.521(12) . ? C1_5 C2_5 1.362(5) . ? C2_5 N3_5 1.401(4) . ? C2_5 N6_5 1.402(4) . ? N3_5 C4_5 1.397(4) . ? N3_5 C13_5 1.432(4) . ? C4_5 C5_5 1.329(5) . ? C4_5 H4_5 0.9500 . ? C5_5 N6_5 1.407(4) . ? C5_5 H5_5 0.9500 . ? N6_5 C7_5 1.438(4) . ? C7_5 C12_5 1.394(5) . ? C7_5 C8_5 1.403(5) . ? C8_5 C9_5 1.397(5) . ? C8_5 C1_11 1.518(5) . ? C9_5 C10_5 1.373(6) . ? C9_5 H01I_5 0.9500 . ? C10_5 C11_5 1.382(5) . ? C10_5 H01F_5 0.9500 . ? C11_5 C12_5 1.399(5) . ? C11_5 H01H_5 0.9500 . ? C12_5 C1_12 1.529(5) . ? C13_5 C14_5 1.402(5) . ? C13_5 C18_5 1.403(5) . ? C14_5 C15_5 1.396(5) . ? C14_5 C1_14 1.524(5) . ? C15_5 C16_5 1.383(5) . ? C15_5 H15_5 0.9500 . ? C16_5 C17_5 1.389(5) . ? C16_5 H16_5 0.9500 . ? C17_5 C18_5 1.394(5) . ? C17_5 H01D_5 0.9500 . ? C18_5 C1_13 1.526(5) . ? C1_6 C2_6 1.378(5) . ? C2_6 N6_6 1.389(4) . ? C2_6 N3_6 1.389(4) . ? N3_6 C4_6 1.406(4) . ? N3_6 C13_6 1.437(4) . ? C4_6 C5_6 1.331(5) . ? C4_6 H4_6 0.9500 . ? C5_6 N6_6 1.390(4) . ? C5_6 H5_6 0.9500 . ? N6_6 C7_6 1.429(4) . ? C7_6 C12_6 1.394(5) . ? C7_6 C8_6 1.411(5) . ? C8_6 C9_6 1.389(5) . ? C8_6 C1_41 1.5164(15) . ? C8_6 C1_42 1.5164(14) . ? C9_6 C10_6 1.384(5) . ? C9_6 H9_6 0.9500 . ? C10_6 C11_6 1.385(5) . ? C10_6 H10_6 0.9500 . ? C11_6 C12_6 1.386(5) . ? C11_6 H11_6 0.9500 . ? C12_6 C1_9 1.522(5) . ? C13_6 C14_6 1.399(5) . ? C13_6 C18_6 1.410(5) . ? C14_6 C15_6 1.399(5) . ? C14_6 C1_8 1.522(5) . ? C15_6 C16_6 1.387(5) . ? C15_6 H15_6 0.9500 . ? C16_6 C17_6 1.382(5) . ? C16_6 H16_6 0.9500 . ? C17_6 C18_6 1.392(5) . ? C17_6 H17_6 0.9500 . ? C18_6 C1_7 1.517(5) . ? C1_7 C3_7 1.515(6) . ? C1_7 C2_7 1.521(5) . ? C1_7 H01G_7 1.0000 . ? C2_7 H01P_7 0.9800 . ? C2_7 H01Q_7 0.9800 . ? C2_7 H01R_7 0.9800 . ? C3_7 H02X_7 0.9800 . ? C3_7 H02Y_7 0.9800 . ? C3_7 H02Z_7 0.9800 . ? C1_8 C3_8 1.513(5) . ? C1_8 C2_8 1.525(5) . ? C1_8 H1_8 1.0000 . ? C2_8 H02J_8 0.9800 . ? C2_8 H02K_8 0.9800 . ? C2_8 H02L_8 0.9800 . ? C3_8 H02G_8 0.9800 . ? C3_8 H02H_8 0.9800 . ? C3_8 H02I_8 0.9800 . ? C1_9 C2_9 1.534(5) . ? C1_9 C3_9 1.535(5) . ? C1_9 H1_9 1.0000 . ? C2_9 H01V_9 0.9800 . ? C2_9 H01W_9 0.9800 . ? C2_9 H01X_9 0.9800 . ? C3_9 H01A_9 0.9800 . ? C3_9 H01B_9 0.9800 . ? C3_9 H01C_9 0.9800 . ? C1_41 C2_41 1.49(9) . ? C1_41 C3_41 1.53(8) . ? C1_41 H01E_41 1.0000 . ? C2_41 H039_41 0.9800 . ? C2_41 H03A_41 0.9800 . ? C2_41 H03B_41 0.9800 . ? C3_41 H01J_41 0.9800 . ? C3_41 H01K_41 0.9800 . ? C3_41 H01L_41 0.9800 . ? C1_42 C3_42 1.52(5) . ? C1_42 C2_42 1.59(7) . ? C1_42 H01E_42 1.0000 . ? C2_42 H039_42 0.9800 . ? C2_42 H03A_42 0.9800 . ? C2_42 H03B_42 0.9800 . ? C3_42 H01J_42 0.9800 . ? C3_42 H01K_42 0.9800 . ? C3_42 H01L_42 0.9800 . ? C1_11 C2_11 1.513(6) . ? C1_11 C3_11 1.521(5) . ? C1_11 H1_11 1.0000 . ? C2_11 H036_11 0.9800 . ? C2_11 H037_11 0.9800 . ? C2_11 H038_11 0.9800 . ? C3_11 H026_11 0.9800 . ? C3_11 H027_11 0.9800 . ? C3_11 H028_11 0.9800 . ? C1_12 C2_12 1.523(5) . ? C1_12 C3_12 1.525(6) . ? C1_12 H02C_12 1.0000 . ? C2_12 H01Y_12 0.9800 . ? C2_12 H01Z_12 0.9800 . ? C2_12 H013_12 0.9800 . ? C3_12 H029_12 0.9800 . ? C3_12 H02A_12 0.9800 . ? C3_12 H02B_12 0.9800 . ? C1_13 C3_13 1.523(5) . ? C1_13 C2_13 1.526(5) . ? C1_13 H1_13 1.0000 . ? C2_13 H01S_13 0.9800 . ? C2_13 H01T_13 0.9800 . ? C2_13 H01U_13 0.9800 . ? C3_13 H01M_13 0.9800 . ? C3_13 H01N_13 0.9800 . ? C3_13 H01O_13 0.9800 . ? C1_14 C2_14 1.518(5) . ? C1_14 C3_14 1.529(5) . ? C1_14 H1_14 1.0000 . ? C2_14 H02M_14 0.9800 . ? C2_14 H02N_14 0.9800 . ? C2_14 H02O_14 0.9800 . ? C3_14 H02D_14 0.9800 . ? C3_14 H02E_14 0.9800 . ? C3_14 H02F_14 0.9800 . ?