#------------------------------------------------------------------------------ #$Date: 2024-11-23 03:09:45 +0200 (Sat, 23 Nov 2024) $ #$Revision: 296077 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/32/1573257.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_1573257 loop_ _publ_author_name 'Abherv\'e, Alexandre' 'Mroweh, Nabil' 'Cui, Hengbo' 'Kato, Reizo' 'Vanthuyne, Nicolas' 'Alemany, Pere' 'Canadell, Enric' 'Avarvari, Narcis' _publ_section_title ; Enantiomorphic single component conducting nickel(II) and platinum(II) bis(diethyl-dddt) crystalline complexes† ; _journal_name_full Nanoscale _journal_paper_doi 10.1039/D4NR04048A _journal_year 2024 _chemical_formula_moiety 'C16 H36 N, C16 H24 Ni S8' _chemical_formula_sum 'C32 H60 N Ni S8' _chemical_formula_weight 774.00 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2016/4 _audit_update_record ; 2024-09-26 deposited with the CCDC. 2024-11-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 115.109(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.6673(5) _cell_length_b 17.9434(3) _cell_length_c 16.4154(5) _cell_measurement_reflns_used 12636 _cell_measurement_temperature 150.01(10) _cell_measurement_theta_max 73.3570 _cell_measurement_theta_min 3.7930 _cell_volume 3912.0(2) _computing_cell_refinement 'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)' _computing_molecular_graphics 'DIAMOND 3.2k (Crystal Impact GbR, 2014)' _computing_publication_material 'WinGX publication routines (Farrugia, 2012)' _computing_structure_refinement 'SHELXL-2016/4 (Sheldrick, 2016)' _computing_structure_solution 'SHELXS-2013/1 (Sheldrick, 2013)' _diffrn_ambient_temperature 150.01(10) _diffrn_detector_area_resol_mean 5.1990 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_device_type 'SuperNova, Single source at offset, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_unetI/netI 0.0271 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.986 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 35475 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.986 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.662 _diffrn_reflns_theta_min 3.328 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 4.868 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.56267 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.314 _exptl_crystal_description prism _exptl_crystal_F_000 1660 _exptl_crystal_size_max 0.050 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.010 _refine_diff_density_max 0.815 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.068 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 418 _refine_ls_number_reflns 7798 _refine_ls_number_restraints 56 _refine_ls_restrained_S_all 1.060 _refine_ls_R_factor_all 0.0706 _refine_ls_R_factor_gt 0.0619 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0739P)^2^+5.6892P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1601 _refine_ls_wR_factor_ref 0.1677 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6623 _reflns_number_total 7798 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4nr04048a2.cif _cod_data_source_block shelx _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 1573257 _shelx_shelxl_version_number 2016/4 _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 0.414 _shelx_estimated_absorpt_t_max 0.668 _oxdiff_exptl_absorpt_empirical_full_min 0.755 _oxdiff_exptl_absorpt_empirical_full_max 1.667 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _shelx_res_file ; TITL aa230 in P 21/c shelx.res created by SHELXL-2016/4 at 16:14:33 on 28-Sep-2020 CELL 1.54184 14.6673 17.9434 16.4154 90.000 115.109 90.000 ZERR 4.00 0.0005 0.0003 0.0005 0.000 0.004 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N S NI UNIT 128 240 4 32 4 MERG 2 DFIX 1.600 0.020 C1D C7B DFIX 1.500 0.020 C2D C5B DFIX 1.500 0.020 C1B C5B DFIX 1.600 0.020 C5A C2C DFIX 1.500 0.020 C1A C5A DFIX 1.600 0.020 C1C C7A DFIX 1.500 0.020 C2A C7A DFIX 1.440 0.010 C7B C8B ISOR 0.010 C1A C2A C1B C2B C1C C2C C1D C2D FMAP 2 PLAN 25 SIZE 0.090 0.210 0.220 ACTA BOND $H CONF L.S. 10 TEMP -123.00 WGHT 0.073900 5.689199 FVAR 2.15679 N1 3 -0.098936 0.783704 1.173917 11.00000 0.05370 0.06032 = 0.04190 0.00309 0.02149 -0.00398 C1 1 -0.153410 0.754411 1.078458 11.00000 0.05739 0.05586 = 0.04301 0.00026 0.01960 0.00216 AFIX 23 H1A 2 -0.102497 0.733919 1.059832 11.00000 -1.20000 H1B 2 -0.186042 0.797079 1.038429 11.00000 -1.20000 AFIX 0 C2 1 -0.233067 0.694701 1.062822 11.00000 0.06155 0.06524 = 0.05793 -0.00081 0.01935 -0.00215 AFIX 23 H2A 2 -0.201982 0.651063 1.101615 11.00000 -1.20000 H2B 2 -0.286214 0.714527 1.078984 11.00000 -1.20000 AFIX 0 C3 1 -0.279318 0.670960 0.964701 11.00000 0.06434 0.06473 = 0.07076 -0.01493 0.02277 0.00452 AFIX 23 H3A 2 -0.308302 0.715265 0.926475 11.00000 -1.20000 H3B 2 -0.225637 0.650891 0.949421 11.00000 -1.20000 AFIX 0 C4 1 -0.360480 0.612802 0.943619 11.00000 0.06021 0.09220 = 0.08820 -0.02522 0.02131 -0.00489 AFIX 33 H4A 2 -0.387496 0.599654 0.879713 11.00000 -1.50000 H4B 2 -0.331979 0.568286 0.980204 11.00000 -1.50000 H4C 2 -0.414683 0.632691 0.957247 11.00000 -1.50000 AFIX 0 C5 1 -0.040340 0.722805 1.238906 11.00000 0.05624 0.07093 = 0.04709 0.01422 0.02264 -0.00501 AFIX 23 H5A 2 -0.010804 0.744020 1.300388 11.00000 -1.20000 H5B 2 -0.088299 0.683428 1.237424 11.00000 -1.20000 AFIX 0 C6 1 0.041977 0.687283 1.222348 11.00000 0.06952 0.09321 = 0.06431 0.03063 0.03693 0.02224 AFIX 23 H6A 2 0.090660 0.725561 1.222500 11.00000 -1.20000 H6B 2 0.013863 0.662292 1.162968 11.00000 -1.20000 AFIX 0 C7 1 0.094209 0.630845 1.296096 11.00000 0.06603 0.06740 = 0.06846 0.01718 0.02683 0.00540 AFIX 23 H7A 2 0.113638 0.655684 1.354969 11.00000 -1.20000 H7B 2 0.045588 0.590953 1.291382 11.00000 -1.20000 AFIX 0 C8 1 0.183766 0.596603 1.294560 11.00000 0.09594 0.11494 = 0.09312 0.03978 0.05102 0.04015 AFIX 33 H8A 2 0.212623 0.561022 1.344312 11.00000 -1.50000 H8B 2 0.165299 0.570471 1.237310 11.00000 -1.50000 H8C 2 0.233489 0.635334 1.301027 11.00000 -1.50000 AFIX 0 C9 1 -0.029492 0.845093 1.170402 11.00000 0.06087 0.06345 = 0.04253 0.00526 0.02372 -0.00916 AFIX 23 H9A 2 0.018093 0.823310 1.148593 11.00000 -1.20000 H9B 2 -0.070559 0.882568 1.125588 11.00000 -1.20000 AFIX 0 C10 1 0.030889 0.884810 1.258524 11.00000 0.08142 0.08843 = 0.04836 0.00049 0.02584 -0.03146 AFIX 23 H10A 2 -0.015539 0.909075 1.279942 11.00000 -1.20000 H10B 2 0.071989 0.848096 1.304454 11.00000 -1.20000 AFIX 0 C11 1 0.098207 0.942179 1.246823 11.00000 0.08851 0.06304 = 0.06352 -0.00322 0.04227 -0.01667 AFIX 23 H11A 2 0.057131 0.975159 1.196133 11.00000 -1.20000 H11B 2 0.147896 0.916710 1.230364 11.00000 -1.20000 AFIX 0 C12 1 0.153949 0.989442 1.328693 11.00000 0.09230 0.09383 = 0.07261 -0.01021 0.03406 -0.03224 AFIX 33 H12A 2 0.196258 1.025513 1.315792 11.00000 -1.50000 H12B 2 0.105504 1.016078 1.344678 11.00000 -1.50000 H12C 2 0.196410 0.957538 1.378963 11.00000 -1.50000 AFIX 0 C13 1 -0.173040 0.813842 1.209017 11.00000 0.05684 0.08169 = 0.05449 -0.01510 0.02991 -0.01208 AFIX 23 H13A 2 -0.215736 0.772086 1.211821 11.00000 -1.20000 H13B 2 -0.134159 0.831972 1.271245 11.00000 -1.20000 AFIX 0 C14 1 -0.241305 0.876264 1.154316 11.00000 0.07759 0.06335 = 0.09529 -0.00879 0.04300 0.00863 AFIX 23 H14A 2 -0.282079 0.858536 1.092237 11.00000 -1.20000 H14B 2 -0.199655 0.918588 1.151098 11.00000 -1.20000 AFIX 0 C15 1 -0.311900 0.903033 1.195939 11.00000 0.07871 0.11729 = 0.09644 -0.03615 0.03302 0.00096 AFIX 23 H15A 2 -0.270295 0.918999 1.258613 11.00000 -1.20000 H15B 2 -0.349227 0.947274 1.162127 11.00000 -1.20000 AFIX 0 C16 1 -0.384715 0.847678 1.196760 11.00000 0.10056 0.14690 = 0.16339 0.03197 0.06823 0.03349 AFIX 33 H16A 2 -0.426246 0.869394 1.224275 11.00000 -1.50000 H16B 2 -0.427893 0.832445 1.134931 11.00000 -1.50000 H16C 2 -0.348792 0.804110 1.231624 11.00000 -1.50000 AFIX 0 NI1 5 0.000000 1.000000 1.000000 10.50000 0.05299 0.04480 = 0.03576 -0.00184 0.01585 0.00841 C3A 1 -0.229815 0.980719 0.928546 11.00000 0.05462 0.06781 = 0.05247 -0.01018 0.01570 0.00959 C4A 1 -0.203536 0.921100 0.894956 11.00000 0.05814 0.05341 = 0.04778 -0.00292 0.02144 0.00074 C5A 1 -0.450754 0.866958 0.893497 11.00000 0.11955 0.12809 = 0.08239 -0.02312 0.03220 -0.02816 AFIX 23 H5A1 2 -0.384421 0.849857 0.938834 11.00000 -1.20000 H5A2 2 -0.482328 0.825876 0.850412 11.00000 -1.20000 AFIX 0 C6A 1 -0.516768 0.889523 0.938334 11.00000 0.08590 0.20959 = 0.31329 0.01600 0.08300 0.02037 AFIX 33 H6A1 2 -0.526748 0.846813 0.970873 11.00000 -1.50000 H6A2 2 -0.484627 0.930186 0.980723 11.00000 -1.50000 H6A3 2 -0.582076 0.906318 0.892713 11.00000 -1.50000 AFIX 0 C7A 1 -0.403996 0.975370 0.713392 11.00000 0.08656 0.13825 = 0.07780 0.00942 0.02402 0.02300 AFIX 23 H7A1 2 -0.453935 1.012961 0.712241 11.00000 -1.20000 H7A2 2 -0.336465 0.998677 0.740694 11.00000 -1.20000 AFIX 0 C8A 1 -0.425631 0.952859 0.625654 11.00000 0.12923 0.18287 = 0.08307 0.01620 0.00856 -0.06308 AFIX 33 H8A1 2 -0.423607 0.996193 0.590121 11.00000 -1.50000 H8A2 2 -0.375595 0.916163 0.626839 11.00000 -1.50000 H8A3 2 -0.492872 0.930424 0.598433 11.00000 -1.50000 AFIX 0 S1A 4 -0.351833 1.006126 0.915400 11.00000 0.05287 0.11226 = 0.11895 -0.05699 0.01472 0.01286 S2A 4 -0.286696 0.854307 0.821000 11.00000 0.07079 0.05962 = 0.08767 -0.02168 0.03203 -0.00826 S3A 4 -0.138512 1.043396 0.994955 11.00000 0.05449 0.06685 = 0.06011 -0.02283 0.01138 0.01475 S4A 4 -0.078014 0.905376 0.919572 11.00000 0.06008 0.04416 = 0.05407 -0.00487 0.02757 0.00389 NI2 5 0.000000 1.000000 1.500000 10.50000 0.05090 0.04920 = 0.04047 0.00058 0.02079 -0.00765 C3B 1 0.111129 0.849769 1.524562 11.00000 0.05453 0.05401 = 0.05132 -0.00215 0.02926 -0.00685 C4B 1 0.186454 0.898398 1.564428 11.00000 0.05426 0.05616 = 0.04992 0.00012 0.02391 -0.00502 C5B 1 0.280238 0.720001 1.679599 11.00000 0.11403 0.15215 = 0.11588 0.06163 0.03886 0.00890 AFIX 23 H5B1 2 0.277377 0.769498 1.705060 11.00000 -1.20000 H5B2 2 0.230203 0.687509 1.687775 11.00000 -1.20000 AFIX 0 C6B 1 0.380348 0.688517 1.729447 11.00000 0.28679 0.15984 = 0.15731 0.03355 -0.04851 0.06913 AFIX 33 H6B1 2 0.394378 0.684454 1.793209 11.00000 -1.50000 H6B2 2 0.383378 0.638939 1.705673 11.00000 -1.50000 H6B3 2 0.430590 0.720993 1.722971 11.00000 -1.50000 AFIX 0 C7B 1 0.294095 0.791332 1.462493 11.00000 0.12408 0.10414 = 0.12591 -0.02803 0.09201 -0.02612 AFIX 23 H7B1 2 0.232127 0.821131 1.431093 11.00000 -1.20000 H7B2 2 0.282108 0.740540 1.436483 11.00000 -1.20000 AFIX 0 C8B 1 0.378639 0.826079 1.451798 11.00000 0.23361 0.49006 = 0.31944 -0.20917 0.22841 -0.18464 AFIX 33 H8B1 2 0.363379 0.829106 1.387696 11.00000 -1.50000 H8B2 2 0.389681 0.876335 1.477583 11.00000 -1.50000 H8B3 2 0.439466 0.796061 1.482952 11.00000 -1.50000 AFIX 0 S1B 4 0.118977 0.752674 1.513975 11.00000 0.05694 0.05410 = 0.08720 -0.01389 0.03202 -0.00835 S2B 4 0.315737 0.877398 1.615917 11.00000 0.04811 0.06550 = 0.10266 -0.01078 0.01501 -0.00578 S3B 4 -0.012299 0.881929 1.474431 11.00000 0.05033 0.05339 = 0.05713 -0.00660 0.02322 -0.01056 S4B 4 0.160633 0.992550 1.567624 11.00000 0.05136 0.05147 = 0.05746 -0.00085 0.01743 -0.01006 PART 1 C1A 1 -0.438921 0.932280 0.846717 10.50000 0.03493 0.05405 = 0.04749 -0.00739 0.01044 0.00400 AFIX 13 H1A1 2 -0.506961 0.955769 0.816287 10.50000 -1.20000 AFIX 0 C2A 1 -0.406702 0.908896 0.769955 10.50000 0.04384 0.04436 = 0.04524 -0.01351 0.00719 -0.00822 AFIX 13 H2A1 2 -0.459747 0.874252 0.728984 10.50000 -1.20000 AFIX 0 C1B 1 0.251264 0.728584 1.578915 10.50000 0.03839 0.03333 = 0.05013 -0.00543 0.01884 -0.00908 AFIX 13 H1B1 2 0.262588 0.679229 1.556438 10.50000 -1.20000 AFIX 0 C2B 1 0.319877 0.787930 1.558626 10.50000 0.02955 0.03897 = 0.06217 -0.01071 0.02400 -0.01254 AFIX 13 H2B1 2 0.390680 0.769212 1.588773 10.50000 -1.20000 AFIX 0 PART 2 C1C 1 -0.419453 0.959657 0.803290 10.50000 0.11136 0.14834 = 0.13416 -0.00642 0.02162 -0.00109 AFIX 13 H1C 2 -0.492672 0.968376 0.786058 10.50000 -1.20000 AFIX 0 C2C 1 -0.407766 0.889827 0.811785 10.50000 0.09887 0.13036 = 0.13666 -0.00180 0.02959 -0.02184 AFIX 13 H2C 2 -0.459124 0.868589 0.754293 10.50000 -1.20000 AFIX 0 C1D 1 0.259728 0.751617 1.542274 10.50000 0.12960 0.13516 = 0.12846 -0.02686 0.04947 0.04821 AFIX 13 H1D 2 0.277728 0.697698 1.544067 10.50000 -1.20000 AFIX 0 C2D 1 0.310514 0.774886 1.618564 10.50000 0.15937 0.16621 = 0.17730 0.01445 0.06299 0.04076 AFIX 13 H2D 2 0.380562 0.759207 1.630793 10.50000 -1.20000 AFIX 0 HKLF 4 REM aa230 in P 21/c REM R1 = 0.0619 for 6623 Fo > 4sig(Fo) and 0.0706 for all 7798 data REM 418 parameters refined using 56 restraints END WGHT 0.0772 5.5320 REM Highest difference peak 0.815, deepest hole -0.697, 1-sigma level 0.068 Q1 1 0.0870 0.5889 1.2549 11.00000 0.05 0.81 Q2 1 -0.3677 0.9426 1.1974 11.00000 0.05 0.71 Q3 1 -0.3489 1.0190 0.8612 11.00000 0.05 0.62 Q4 1 0.3493 0.8454 1.4277 11.00000 0.05 0.52 Q5 1 0.0805 0.9938 1.5355 11.00000 0.05 0.50 Q6 1 -0.2946 0.8605 1.2385 11.00000 0.05 0.49 Q7 1 0.3785 0.7531 1.4822 11.00000 0.05 0.48 Q8 1 -0.5382 0.8660 0.8649 11.00000 0.05 0.44 Q9 1 -0.4709 1.0133 0.6508 11.00000 0.05 0.44 Q10 1 -0.3574 0.9463 0.6995 11.00000 0.05 0.43 Q11 1 0.1882 0.6341 1.3412 11.00000 0.05 0.39 Q12 1 -0.3460 1.0516 0.8999 11.00000 0.05 0.38 Q13 1 0.1180 0.7537 1.4636 11.00000 0.05 0.38 Q14 1 0.2970 0.6708 1.7162 11.00000 0.05 0.37 Q15 1 0.3154 0.9040 1.6541 11.00000 0.05 0.37 Q16 1 0.4044 0.6899 1.7096 11.00000 0.05 0.37 Q17 1 -0.2437 0.8305 0.8573 11.00000 0.05 0.36 Q18 1 0.0597 0.7527 1.4869 11.00000 0.05 0.36 Q19 1 0.0722 0.8427 1.2675 11.00000 0.05 0.36 Q20 1 -0.0744 0.9895 0.9789 11.00000 0.05 0.35 Q21 1 -0.3719 0.8894 0.7645 11.00000 0.05 0.34 Q22 1 -0.2923 0.8748 0.8718 11.00000 0.05 0.33 Q23 1 -0.1410 1.0545 0.9439 11.00000 0.05 0.31 Q24 1 0.3364 0.8152 1.5744 11.00000 0.05 0.29 Q25 1 -0.0811 0.7479 1.1847 11.00000 0.05 0.29 ; _shelx_res_checksum 99664 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group N1 N -0.0989(2) 0.78370(19) 1.17392(19) 0.0516(7) Uani 1 1 d . . . . . C1 C -0.1534(3) 0.7544(2) 1.0785(2) 0.0527(8) Uani 1 1 d . . . . . H1A H -0.102497 0.733919 1.059832 0.063 Uiso 1 1 calc R U . . . H1B H -0.186042 0.797079 1.038429 0.063 Uiso 1 1 calc R U . . . C2 C -0.2331(3) 0.6947(3) 1.0628(3) 0.0636(10) Uani 1 1 d . . . . . H2A H -0.201982 0.651063 1.101615 0.076 Uiso 1 1 calc R U . . . H2B H -0.286214 0.714527 1.078984 0.076 Uiso 1 1 calc R U . . . C3 C -0.2793(3) 0.6710(3) 0.9647(3) 0.0686(11) Uani 1 1 d . . . . . H3A H -0.308302 0.715265 0.926475 0.082 Uiso 1 1 calc R U . . . H3B H -0.225637 0.650891 0.949421 0.082 Uiso 1 1 calc R U . . . C4 C -0.3605(4) 0.6128(3) 0.9436(4) 0.0837(15) Uani 1 1 d . . . . . H4A H -0.387496 0.599654 0.879713 0.126 Uiso 1 1 calc R U . . . H4B H -0.331979 0.568286 0.980204 0.126 Uiso 1 1 calc R U . . . H4C H -0.414683 0.632691 0.957247 0.126 Uiso 1 1 calc R U . . . C5 C -0.0403(3) 0.7228(2) 1.2389(3) 0.0578(9) Uani 1 1 d . . . . . H5A H -0.010804 0.744020 1.300388 0.069 Uiso 1 1 calc R U . . . H5B H -0.088299 0.683428 1.237424 0.069 Uiso 1 1 calc R U . . . C6 C 0.0420(4) 0.6873(3) 1.2223(3) 0.0727(13) Uani 1 1 d . . . . . H6A H 0.090660 0.725561 1.222500 0.087 Uiso 1 1 calc R U . . . H6B H 0.013863 0.662292 1.162968 0.087 Uiso 1 1 calc R U . . . C7 C 0.0942(3) 0.6308(3) 1.2961(3) 0.0679(11) Uani 1 1 d . . . . . H7A H 0.113638 0.655684 1.354969 0.081 Uiso 1 1 calc R U . . . H7B H 0.045588 0.590953 1.291382 0.081 Uiso 1 1 calc R U . . . C8 C 0.1838(5) 0.5966(4) 1.2946(4) 0.0976(19) Uani 1 1 d . . . . . H8A H 0.212623 0.561022 1.344312 0.146 Uiso 1 1 calc R U . . . H8B H 0.165299 0.570471 1.237310 0.146 Uiso 1 1 calc R U . . . H8C H 0.233489 0.635334 1.301027 0.146 Uiso 1 1 calc R U . . . C9 C -0.0295(3) 0.8451(2) 1.1704(2) 0.0550(9) Uani 1 1 d . . . . . H9A H 0.018093 0.823310 1.148593 0.066 Uiso 1 1 calc R U . . . H9B H -0.070559 0.882568 1.125588 0.066 Uiso 1 1 calc R U . . . C10 C 0.0309(4) 0.8848(3) 1.2585(3) 0.0733(13) Uani 1 1 d . . . . . H10A H -0.015539 0.909075 1.279942 0.088 Uiso 1 1 calc R U . . . H10B H 0.071989 0.848096 1.304454 0.088 Uiso 1 1 calc R U . . . C11 C 0.0982(4) 0.9422(3) 1.2468(3) 0.0682(11) Uani 1 1 d . . . . . H11A H 0.057131 0.975159 1.196133 0.082 Uiso 1 1 calc R U . . . H11B H 0.147896 0.916710 1.230364 0.082 Uiso 1 1 calc R U . . . C12 C 0.1539(4) 0.9894(3) 1.3287(4) 0.0866(15) Uani 1 1 d . . . . . H12A H 0.196258 1.025513 1.315792 0.130 Uiso 1 1 calc R U . . . H12B H 0.105504 1.016078 1.344678 0.130 Uiso 1 1 calc R U . . . H12C H 0.196410 0.957538 1.378963 0.130 Uiso 1 1 calc R U . . . C13 C -0.1730(3) 0.8138(3) 1.2090(3) 0.0622(10) Uani 1 1 d . . . . . H13A H -0.215736 0.772086 1.211821 0.075 Uiso 1 1 calc R U . . . H13B H -0.134159 0.831972 1.271245 0.075 Uiso 1 1 calc R U . . . C14 C -0.2413(4) 0.8763(3) 1.1543(4) 0.0766(13) Uani 1 1 d . . . . . H14A H -0.282079 0.858536 1.092237 0.092 Uiso 1 1 calc R U . . . H14B H -0.199655 0.918588 1.151098 0.092 Uiso 1 1 calc R U . . . C15 C -0.3119(4) 0.9030(4) 1.1959(4) 0.0989(19) Uani 1 1 d . . . . . H15A H -0.270295 0.918999 1.258613 0.119 Uiso 1 1 calc R U . . . H15B H -0.349227 0.947274 1.162127 0.119 Uiso 1 1 calc R U . . . C16 C -0.3847(6) 0.8477(5) 1.1968(6) 0.133(3) Uani 1 1 d . . . . . H16A H -0.426246 0.869394 1.224275 0.199 Uiso 1 1 calc R U . . . H16B H -0.427893 0.832445 1.134931 0.199 Uiso 1 1 calc R U . . . H16C H -0.348792 0.804110 1.231624 0.199 Uiso 1 1 calc R U . . . NI1 Ni 0.000000 1.000000 1.000000 0.0455(2) Uani 1 2 d S . P . . C3A C -0.2298(3) 0.9807(2) 0.9285(3) 0.0607(10) Uani 1 1 d . . . . . C4A C -0.2035(3) 0.9211(2) 0.8950(2) 0.0535(8) Uani 1 1 d . . . . . C5A C -0.4508(6) 0.8670(4) 0.8935(4) 0.114(2) Uani 1 1 d D . . . . H5A1 H -0.384421 0.849857 0.938834 0.136 Uiso 1 1 calc R U . A 1 H5A2 H -0.482328 0.825876 0.850412 0.136 Uiso 1 1 calc R U . A 1 C6A C -0.5168(6) 0.8895(7) 0.9383(10) 0.204(6) Uani 1 1 d . . . . . H6A1 H -0.526748 0.846813 0.970873 0.305 Uiso 1 1 calc R U . . . H6A2 H -0.484627 0.930186 0.980723 0.305 Uiso 1 1 calc R U . . . H6A3 H -0.582076 0.906318 0.892713 0.305 Uiso 1 1 calc R U . . . C7A C -0.4040(5) 0.9754(4) 0.7134(4) 0.105(2) Uani 1 1 d D . . . . H7A1 H -0.453935 1.012961 0.712241 0.126 Uiso 1 1 calc R U . B 1 H7A2 H -0.336465 0.998677 0.740694 0.126 Uiso 1 1 calc R U . B 1 C8A C -0.4256(6) 0.9529(5) 0.6257(5) 0.144(4) Uani 1 1 d . . . . . H8A1 H -0.423607 0.996193 0.590121 0.216 Uiso 1 1 calc R U . . . H8A2 H -0.375595 0.916163 0.626839 0.216 Uiso 1 1 calc R U . . . H8A3 H -0.492872 0.930424 0.598433 0.216 Uiso 1 1 calc R U . . . S1A S -0.35183(9) 1.00613(9) 0.91540(12) 0.1022(6) Uani 1 1 d . . . . . S2A S -0.28670(9) 0.85431(6) 0.82100(9) 0.0732(3) Uani 1 1 d . . . . . S3A S -0.13851(8) 1.04340(6) 0.99496(7) 0.0649(3) Uani 1 1 d . . . . . S4A S -0.07801(7) 0.90538(5) 0.91957(6) 0.0516(2) Uani 1 1 d . . . . . NI2 Ni 0.000000 1.000000 1.500000 0.0464(2) Uani 1 2 d S . P . . C3B C 0.1111(3) 0.8498(2) 1.5246(2) 0.0509(8) Uani 1 1 d . . . . . C4B C 0.1865(3) 0.8984(2) 1.5644(3) 0.0528(8) Uani 1 1 d . . . . . C5B C 0.2802(6) 0.7200(5) 1.6796(5) 0.131(3) Uani 1 1 d D . . . . H5B1 H 0.277377 0.769498 1.705060 0.157 Uiso 1 1 calc R U . C 1 H5B2 H 0.230203 0.687509 1.687775 0.157 Uiso 1 1 calc R U . C 1 C6B C 0.3803(10) 0.6885(7) 1.7294(8) 0.251(8) Uani 1 1 d . . . . . H6B1 H 0.394378 0.684454 1.793209 0.376 Uiso 1 1 calc R U . . . H6B2 H 0.383378 0.638939 1.705673 0.376 Uiso 1 1 calc R U . . . H6B3 H 0.430590 0.720993 1.722971 0.376 Uiso 1 1 calc R U . . . C7B C 0.2941(5) 0.7913(4) 1.4625(5) 0.105(2) Uani 1 1 d D . . . . H7B1 H 0.232127 0.821131 1.431093 0.126 Uiso 1 1 calc R U . D 1 H7B2 H 0.282108 0.740540 1.436483 0.126 Uiso 1 1 calc R U . D 1 C8B C 0.3786(10) 0.8261(10) 1.4518(11) 0.309(11) Uani 1 1 d D . . . . H8B1 H 0.363379 0.829106 1.387696 0.464 Uiso 1 1 calc R U . . . H8B2 H 0.389681 0.876335 1.477583 0.464 Uiso 1 1 calc R U . . . H8B3 H 0.439466 0.796061 1.482952 0.464 Uiso 1 1 calc R U . . . S1B S 0.11898(8) 0.75267(6) 1.51397(9) 0.0656(3) Uani 1 1 d . . . . . S2B S 0.31574(8) 0.87740(7) 1.61592(10) 0.0779(4) Uani 1 1 d . . . . . S3B S -0.01230(7) 0.88193(5) 1.47443(7) 0.0535(2) Uani 1 1 d . . . . . S4B S 0.16063(7) 0.99255(5) 1.56762(7) 0.0554(2) Uani 1 1 d . . . . . C1A C -0.4389(5) 0.9323(4) 0.8467(5) 0.0479(16) Uani 0.5 1 d D U P E 1 H1A1 H -0.506961 0.955769 0.816287 0.058 Uiso 0.5 1 calc R U P E 1 C2A C -0.4067(6) 0.9089(4) 0.7700(5) 0.0485(17) Uani 0.5 1 d D U P E 1 H2A1 H -0.459747 0.874252 0.728984 0.058 Uiso 0.5 1 calc R U P E 1 C1B C 0.2513(5) 0.7286(4) 1.5789(5) 0.0406(14) Uani 0.5 1 d D U P F 1 H1B1 H 0.262588 0.679229 1.556438 0.049 Uiso 0.5 1 calc R U P F 1 C2B C 0.3199(5) 0.7879(4) 1.5586(5) 0.0420(14) Uani 0.5 1 d . U P F 1 H2B1 H 0.390680 0.769212 1.588773 0.050 Uiso 0.5 1 calc R U P F 1 C1C C -0.4195(14) 0.9597(12) 0.8033(11) 0.142(6) Uani 0.5 1 d D U P E 2 H1C H -0.492672 0.968376 0.786058 0.170 Uiso 0.5 1 calc R U P E 2 C2C C -0.4078(13) 0.8898(11) 0.8118(12) 0.129(6) Uani 0.5 1 d D U P E 2 H2C H -0.459124 0.868589 0.754293 0.155 Uiso 0.5 1 calc R U P E 2 C1D C 0.2597(14) 0.7516(10) 1.5423(12) 0.133(6) Uani 0.5 1 d D U P F 2 H1D H 0.277728 0.697698 1.544067 0.159 Uiso 0.5 1 calc R U P F 2 C2D C 0.3105(17) 0.7749(12) 1.6186(15) 0.171(8) Uani 0.5 1 d D U P F 2 H2D H 0.380562 0.759207 1.630793 0.205 Uiso 0.5 1 calc R U P F 2 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 N1 0.0537(17) 0.0603(18) 0.0419(15) 0.0031(13) 0.0215(13) -0.0040(14) C1 0.057(2) 0.056(2) 0.0430(18) 0.0003(15) 0.0196(16) 0.0022(16) C2 0.062(2) 0.065(3) 0.058(2) -0.0008(19) 0.0193(19) -0.0021(19) C3 0.064(2) 0.065(3) 0.071(3) -0.015(2) 0.023(2) 0.005(2) C4 0.060(3) 0.092(4) 0.088(3) -0.025(3) 0.021(2) -0.005(2) C5 0.056(2) 0.071(2) 0.0471(19) 0.0142(18) 0.0226(17) -0.0050(18) C6 0.070(3) 0.093(3) 0.064(3) 0.031(2) 0.037(2) 0.022(2) C7 0.066(3) 0.067(3) 0.068(3) 0.017(2) 0.027(2) 0.005(2) C8 0.096(4) 0.115(5) 0.093(4) 0.040(3) 0.051(3) 0.040(3) C9 0.061(2) 0.063(2) 0.0425(18) 0.0053(16) 0.0237(16) -0.0092(18) C10 0.081(3) 0.088(3) 0.048(2) 0.000(2) 0.026(2) -0.031(3) C11 0.089(3) 0.063(3) 0.064(2) -0.003(2) 0.042(2) -0.017(2) C12 0.092(4) 0.094(4) 0.073(3) -0.010(3) 0.034(3) -0.032(3) C13 0.057(2) 0.082(3) 0.054(2) -0.015(2) 0.0299(18) -0.012(2) C14 0.078(3) 0.063(3) 0.095(3) -0.009(2) 0.043(3) 0.009(2) C15 0.079(3) 0.117(5) 0.096(4) -0.036(4) 0.033(3) 0.001(3) C16 0.101(5) 0.147(7) 0.163(8) 0.032(6) 0.068(5) 0.033(5) NI1 0.0530(5) 0.0448(4) 0.0358(4) -0.0018(3) 0.0159(3) 0.0084(3) C3A 0.055(2) 0.068(2) 0.052(2) -0.0102(18) 0.0157(17) 0.0096(18) C4A 0.058(2) 0.053(2) 0.0478(19) -0.0029(16) 0.0214(16) 0.0007(16) C5A 0.120(5) 0.128(6) 0.082(4) -0.023(4) 0.032(4) -0.028(4) C6A 0.086(5) 0.210(12) 0.313(17) 0.016(11) 0.083(8) 0.020(6) C7A 0.087(4) 0.138(6) 0.078(4) 0.009(4) 0.024(3) 0.023(4) C8A 0.129(6) 0.183(9) 0.083(4) 0.016(5) 0.009(4) -0.063(6) S1A 0.0529(6) 0.1123(11) 0.1190(12) -0.0570(9) 0.0147(7) 0.0129(6) S2A 0.0708(7) 0.0596(6) 0.0877(8) -0.0217(5) 0.0320(6) -0.0083(5) S3A 0.0545(5) 0.0668(6) 0.0601(6) -0.0228(5) 0.0114(4) 0.0147(4) S4A 0.0601(5) 0.0442(4) 0.0541(5) -0.0049(4) 0.0276(4) 0.0039(4) NI2 0.0509(5) 0.0492(5) 0.0405(4) 0.0006(3) 0.0208(4) -0.0077(3) C3B 0.055(2) 0.054(2) 0.0513(19) -0.0022(15) 0.0293(17) -0.0068(16) C4B 0.054(2) 0.056(2) 0.0499(19) 0.0001(16) 0.0239(16) -0.0050(16) C5B 0.114(5) 0.152(7) 0.116(6) 0.062(5) 0.039(5) 0.009(5) C6B 0.287(16) 0.160(10) 0.157(10) 0.034(8) -0.049(10) 0.069(10) C7B 0.124(5) 0.104(4) 0.126(5) -0.028(4) 0.092(5) -0.026(4) C8B 0.234(14) 0.49(3) 0.319(19) -0.209(19) 0.228(15) -0.185(17) S1B 0.0569(6) 0.0541(6) 0.0872(7) -0.0139(5) 0.0320(5) -0.0084(4) S2B 0.0481(5) 0.0655(7) 0.1027(9) -0.0108(6) 0.0150(6) -0.0058(5) S3B 0.0503(5) 0.0534(5) 0.0571(5) -0.0066(4) 0.0232(4) -0.0106(4) S4B 0.0514(5) 0.0515(5) 0.0575(5) -0.0008(4) 0.0174(4) -0.0101(4) C1A 0.035(3) 0.054(4) 0.047(4) -0.007(3) 0.010(3) 0.004(3) C2A 0.044(3) 0.044(4) 0.045(4) -0.014(3) 0.007(3) -0.008(3) C1B 0.038(3) 0.033(3) 0.050(4) -0.005(3) 0.019(3) -0.009(2) C2B 0.030(3) 0.039(3) 0.062(4) -0.011(3) 0.024(3) -0.013(2) C1C 0.111(9) 0.148(10) 0.134(9) -0.006(8) 0.022(7) -0.001(8) C2C 0.099(8) 0.130(10) 0.137(10) -0.002(8) 0.030(7) -0.022(7) C1D 0.130(9) 0.135(10) 0.128(9) -0.027(7) 0.049(8) 0.048(7) C2D 0.159(11) 0.166(11) 0.177(11) 0.014(9) 0.063(8) 0.041(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' 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 C5 N1 C9 111.2(3) . . ? C5 N1 C1 111.7(3) . . ? C9 N1 C1 106.2(3) . . ? C5 N1 C13 105.8(3) . . ? C9 N1 C13 110.7(3) . . ? C1 N1 C13 111.4(3) . . ? N1 C1 C2 116.5(3) . . ? N1 C1 H1A 108.2 . . ? C2 C1 H1A 108.2 . . ? N1 C1 H1B 108.2 . . ? C2 C1 H1B 108.2 . . ? H1A C1 H1B 107.3 . . ? C3 C2 C1 109.9(4) . . ? C3 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? C3 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C4 C3 C2 113.0(4) . . ? C4 C3 H3A 109.0 . . ? C2 C3 H3A 109.0 . . ? C4 C3 H3B 109.0 . . ? C2 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 N1 116.2(3) . . ? C6 C5 H5A 108.2 . . ? N1 C5 H5A 108.2 . . ? C6 C5 H5B 108.2 . . ? N1 C5 H5B 108.2 . . ? H5A C5 H5B 107.4 . . ? C5 C6 C7 108.4(3) . . ? C5 C6 H6A 110.0 . . ? C7 C6 H6A 110.0 . . ? C5 C6 H6B 110.0 . . ? C7 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? C8 C7 C6 114.9(4) . . ? C8 C7 H7A 108.5 . . ? C6 C7 H7A 108.5 . . ? C8 C7 H7B 108.5 . . ? C6 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 N1 115.8(3) . . ? C10 C9 H9A 108.3 . . ? N1 C9 H9A 108.3 . . ? C10 C9 H9B 108.3 . . ? N1 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? C11 C10 C9 110.6(3) . . ? C11 C10 H10A 109.5 . . ? C9 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? C10 C11 C12 114.3(4) . . ? C10 C11 H11A 108.7 . . ? C12 C11 H11A 108.7 . . ? C10 C11 H11B 108.7 . . ? C12 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 N1 115.7(3) . . ? C14 C13 H13A 108.3 . . ? N1 C13 H13A 108.3 . . ? C14 C13 H13B 108.3 . . ? N1 C13 H13B 108.3 . . ? H13A C13 H13B 107.4 . . ? C13 C14 C15 111.5(5) . . ? C13 C14 H14A 109.3 . . ? C15 C14 H14A 109.3 . . ? C13 C14 H14B 109.3 . . ? C15 C14 H14B 109.3 . . ? H14A C14 H14B 108.0 . . ? C16 C15 C14 115.1(6) . . ? C16 C15 H15A 108.5 . . ? C14 C15 H15A 108.5 . . ? C16 C15 H15B 108.5 . . ? C14 C15 H15B 108.5 . . ? H15A C15 H15B 107.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? S3A NI1 S3A 180.0 3_577 . ? S3A NI1 S4A 89.18(4) 3_577 . ? S3A NI1 S4A 90.82(4) . . ? S3A NI1 S4A 90.82(4) 3_577 3_577 ? S3A NI1 S4A 89.18(4) . 3_577 ? S4A NI1 S4A 180.0 . 3_577 ? C4A C3A S3A 119.9(3) . . ? C4A C3A S1A 127.7(3) . . ? S3A C3A S1A 112.4(2) . . ? C3A C4A S4A 120.0(3) . . ? C3A C4A S2A 126.2(3) . . ? S4A C4A S2A 113.8(2) . . ? C1Aa C5A C6A 106.8(8) . . ? C6A C5A C2C 145.9(10) . . ? C1Aa C5A H5A1 110.4 . . ? C6A C5A H5A1 110.4 . . ? C1Aa C5A H5A2 110.4 . . ? C6A C5A H5A2 110.4 . . ? H5A1a C5A H5A2 108.6 . . ? C5A C6A H6A1 109.5 . . ? C5A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? C5A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C8A C7A C2A 110.4(7) . . ? C8A C7A C1C 146.7(10) . . ? C8A C7A H7A1 109.6 . . ? C2Aa C7A H7A1 109.6 . . ? C8A C7A H7A2 109.6 . . ? C2Aa C7A H7A2 109.6 . . ? H7A1a C7A H7A2 108.1 . . ? C7A C8A H8A1 109.5 . . ? C7A C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C7A C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? C3A S1A C1A 106.9(3) . . ? C3A S1A C1C 95.3(6) . . ? C4A S2A C2C 100.5(6) . . ? C4A S2A C2A 101.3(3) . . ? C3A S3A NI1 104.78(14) . . ? C4A S4A NI1 104.47(13) . . ? S4B NI2 S4B 180.00(5) 3_578 . ? S4B NI2 S3B 88.72(4) 3_578 . ? S4B NI2 S3B 91.28(4) . . ? S4B NI2 S3B 91.28(4) 3_578 3_578 ? S4B NI2 S3B 88.72(4) . 3_578 ? S3B NI2 S3B 180.0 . 3_578 ? C4B C3B S3B 119.5(3) . . ? C4B C3B S1B 128.2(3) . . ? S3B C3B S1B 112.4(2) . . ? C3B C4B S4B 120.2(3) . . ? C3B C4B S2B 126.3(3) . . ? S4B C4B S2B 113.5(2) . . ? C6B C5B C1B 113.4(9) . . ? C6B C5B C2D 96.3(11) . . ? C6B C5B H5B1 108.9 . . ? C1Ba C5B H5B1 108.9 . . ? C6B C5B H5B2 108.9 . . ? C1Ba C5B H5B2 108.9 . . ? H5B1a C5B H5B2 107.7 . . ? C5B C6B H6B1 109.5 . . ? C5B C6B H6B2 109.5 . . ? H6B1 C6B H6B2 109.5 . . ? C5B C6B H6B3 109.5 . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? C2Ba C7B C8B 107.7(8) . . ? C8B C7B C1D 142.6(11) . . ? C2Ba C7B H7B1 110.2 . . ? C8B C7B H7B1 110.2 . . ? C2Ba C7B H7B2 110.2 . . ? C8B C7B H7B2 110.2 . . ? H7B1a C7B H7B2 108.5 . . ? C7B C8B H8B1 109.5 . . ? C7B C8B H8B2 109.5 . . ? H8B1 C8B H8B2 109.5 . . ? C7B C8B H8B3 109.5 . . ? H8B1 C8B H8B3 109.5 . . ? H8B2 C8B H8B3 109.5 . . ? C3B S1B C1B 105.9(3) . . ? C3B S1B C1D 95.4(6) . . ? C4B S2B C2D 100.3(7) . . ? C4B S2B C2B 101.6(2) . . ? C3B S3B NI2 104.48(13) . . ? C4B S4B NI2 104.55(14) . . ? C5A C1Aa C2A 110.6(6) . . ? C5A C1Aa S1A 117.5(5) . . ? C2Aa C1Aa S1A 108.2(5) . . ? C5A C1Aa H1A1 106.7 . . ? C2Aa C1Aa H1A1 106.7 . . ? S1A C1Aa H1A1 106.7 . . ? C7A C2Aa C1A 111.9(6) . . ? C7A C2Aa S2A 114.8(5) . . ? C1Aa C2Aa S2A 108.9(5) . . ? C7A C2Aa H2A1 106.9 . . ? C1Aa C2Aa H2A1 106.9 . . ? S2A C2Aa H2A1 106.9 . . ? C5B C1Ba C2B 112.5(6) . . ? C5B C1Ba S1B 113.2(5) . . ? C2Ba C1Ba S1B 109.2(5) . . ? C5B C1Ba H1B1 107.2 . . ? C2Ba C1Ba H1B1 107.2 . . ? S1B C1Ba H1B1 107.2 . . ? C7B C2Ba C1B 110.9(5) . . ? C7B C2Ba S2B 117.3(5) . . ? C1Ba C2Ba S2B 108.0(4) . . ? C7B C2Ba H2B1 106.7 . . ? C1Ba C2Ba H2B1 106.7 . . ? S2B C2Ba H2B1 106.7 . . ? C2Cb C1Cb C7A 102.1(15) . . ? C2Cb C1Cb S1A 110.0(14) . . ? C7A C1Cb S1A 126.9(12) . . ? C2Cb C1Cb H1C 105.4 . . ? C7A C1Cb H1C 105.4 . . ? S1A C1Cb H1C 105.4 . . ? C1Cb C2Cb C5A 103.9(15) . . ? C1Cb C2Cb S2A 115.8(14) . . ? C5A C2Cb S2A 120.4(11) . . ? C1Cb C2Cb H2C 105.1 . . ? C5A C2Cb H2C 105.1 . . ? S2A C2Cb H2C 105.1 . . ? C2Db C1Db C7B 112.6(17) . . ? C2Db C1Db S1B 111.7(15) . . ? C7B C1Db S1B 116.1(10) . . ? C2Db C1Db H1D 105.1 . . ? C7B C1Db H1D 105.1 . . ? S1B C1Db H1D 105.1 . . ? C1Db C2Db C5B 102.7(17) . . ? C1Db C2Db S2B 109.2(15) . . ? C5B C2Db S2B 131.0(15) . . ? C1Db C2Db H2D 103.7 . . ? C5B C2Db H2D 103.7 . . ? S2B C2Db H2D 103.7 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C5 1.514(5) . ? N1 C9 1.518(5) . ? N1 C1 1.519(5) . ? N1 C13 1.529(5) . ? C1 C2 1.525(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.519(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.509(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.489(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.514(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.460(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.516(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.494(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.504(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.517(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.540(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.463(10) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? NI1 S3A 2.1442(10) 3_577 ? NI1 S3A 2.1442(10) . ? NI1 S4A 2.1571(9) . ? NI1 S4A 2.1572(9) 3_577 ? C3A C4A 1.333(6) . ? C3A S3A 1.734(4) . ? C3A S1A 1.769(4) . ? C4A S4A 1.732(4) . ? C4A S2A 1.772(4) . ? C5A C1A 1.451(10) . ? C5A C6A 1.499(12) . ? C5A C2C 1.756(15) . ? C5A H5A1 0.9900 . ? C5A H5A2 0.9900 . ? C6A H6A1 0.9800 . ? C6A H6A2 0.9800 . ? C6A H6A3 0.9800 . ? C7A C8A 1.397(10) . ? C7A C2A 1.522(10) . ? C7A C1C 1.610(16) . ? C7A H7A1 0.9900 . ? C7A H7A2 0.9900 . ? C8A H8A1 0.9800 . ? C8A H8A2 0.9800 . ? C8A H8A3 0.9800 . ? S1A C1A 1.854(7) . ? S1A C1C 1.875(18) . ? S2A C2C 1.832(19) . ? S2A C2A 1.873(8) . ? NI2 S4B 2.1404(10) 3_578 ? NI2 S4B 2.1404(10) . ? NI2 S3B 2.1524(10) . ? NI2 S3B 2.1524(10) 3_578 ? C3B C4B 1.340(5) . ? C3B S3B 1.739(4) . ? C3B S1B 1.759(4) . ? C4B S4B 1.737(4) . ? C4B S2B 1.758(4) . ? C5B C6B 1.458(12) . ? C5B C1B 1.530(9) . ? C5B C2D 1.596(16) . ? C5B H5B1 0.9900 . ? C5B H5B2 0.9900 . ? C6B H6B1 0.9800 . ? C6B H6B2 0.9800 . ? C6B H6B3 0.9800 . ? C7B C2B 1.460(10) . ? C7B C8B 1.464(8) . ? C7B C1D 1.743(16) . ? C7B H7B1 0.9900 . ? C7B H7B2 0.9900 . ? C8B H8B1 0.9800 . ? C8B H8B2 0.9800 . ? C8B H8B3 0.9800 . ? S1B C1B 1.826(7) . ? S1B C1D 1.914(18) . ? S2B C2D 1.84(2) . ? S2B C2B 1.875(7) . ? C1Aa C2A 1.579(11) . ? C1Aa H1A1 1.0000 . ? C2Aa H2A1 1.0000 . ? C1Ba C2B 1.594(9) . ? C1Ba H1B1 1.0000 . ? C2Ba H2B1 1.0000 . ? C1Cb C2C 1.26(3) . ? C1Cb H1C 1.0000 . ? C2Cb H2C 1.0000 . ? C1Db C2D 1.23(3) . ? C1Db H1D 1.0000 . ? C2Db H2D 1.0000 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N1 C1 C2 62.1(4) . . . . ? C9 N1 C1 C2 -176.5(3) . . . . ? C13 N1 C1 C2 -55.9(4) . . . . ? N1 C1 C2 C3 -179.4(3) . . . . ? C1 C2 C3 C4 -178.9(4) . . . . ? C9 N1 C5 C6 -56.2(5) . . . . ? C1 N1 C5 C6 62.3(5) . . . . ? C13 N1 C5 C6 -176.4(4) . . . . ? N1 C5 C6 C7 177.5(4) . . . . ? C5 C6 C7 C8 -173.9(5) . . . . ? C5 N1 C9 C10 -60.2(5) . . . . ? C1 N1 C9 C10 178.1(4) . . . . ? C13 N1 C9 C10 57.0(5) . . . . ? N1 C9 C10 C11 178.3(4) . . . . ? C9 C10 C11 C12 174.5(5) . . . . ? C5 N1 C13 C14 -179.9(4) . . . . ? C9 N1 C13 C14 59.6(4) . . . . ? C1 N1 C13 C14 -58.4(5) . . . . ? N1 C13 C14 C15 -179.4(4) . . . . ? C13 C14 C15 C16 -64.6(7) . . . . ? S3A C3A C4A S4A 1.3(5) . . . . ? S1A C3A C4A S4A -177.8(3) . . . . ? S3A C3A C4A S2A -176.2(2) . . . . ? S1A C3A C4A S2A 4.7(6) . . . . ? C4A C3A S1A C1Aa 1.1(5) . . . . ? S3A C3A S1A C1Aa -178.0(3) . . . . ? C4A C3A S1A C1Cb -28.4(8) . . . . ? S3A C3A S1A C1Cb 152.4(6) . . . . ? C3A C4A S2A C2Cb -2.1(7) . . . . ? S4A C4A S2A C2Cb -179.7(6) . . . . ? C3A C4A S2A C2Aa 22.4(5) . . . . ? S4A C4A S2A C2Aa -155.2(3) . . . . ? C4A C3A S3A NI1 0.7(4) . . . . ? S1A C3A S3A NI1 179.9(2) . . . . ? C3A C4A S4A NI1 -2.5(4) . . . . ? S2A C4A S4A NI1 175.25(17) . . . . ? S3B C3B C4B S4B 1.1(5) . . . . ? S1B C3B C4B S4B -179.5(2) . . . . ? S3B C3B C4B S2B -178.2(2) . . . . ? S1B C3B C4B S2B 1.2(6) . . . . ? C4B C3B S1B C1Ba 5.7(5) . . . . ? S3B C3B S1B C1Ba -174.9(3) . . . . ? C4B C3B S1B C1Db -16.3(6) . . . . ? S3B C3B S1B C1Db 163.2(5) . . . . ? C3B C4B S2B C2Db -11.1(8) . . . . ? S4B C4B S2B C2Db 169.6(7) . . . . ? C3B C4B S2B C2Ba 23.2(4) . . . . ? S4B C4B S2B C2Ba -156.2(3) . . . . ? C4B C3B S3B NI2 -1.8(3) . . . . ? S1B C3B S3B NI2 178.66(15) . . . . ? C3B C4B S4B NI2 0.2(3) . . . . ? S2B C4B S4B NI2 179.62(16) . . . . ? C6A C5A C1Aa C2Aa -158.9(7) . . . . ? C6A C5A C1Aa S1A 76.2(8) . . . . ? C3A S1A C1Aa C5A 85.6(6) . . . . ? C3A S1A C1Aa C2Aa -40.4(6) . . . . ? C8A C7A C2Aa C1Aa -150.4(7) . . . . ? C8A C7A C2Aa S2A 84.8(7) . . . . ? C5A C1Aa C2Aa C7A 174.2(6) . . . . ? S1A C1Aa C2Aa C7A -55.8(7) . . . . ? C5A C1Aa C2Aa S2A -57.8(7) . . . . ? S1A C1Aa C2Aa S2A 72.2(5) . . . . ? C4A S2A C2Aa C7A 64.5(5) . . . . ? C4A S2A C2Aa C1Aa -61.8(5) . . . . ? C6B C5B C1Ba C2Ba -65.6(10) . . . . ? C6B C5B C1Ba S1B 170.1(8) . . . . ? C3B S1B C1Ba C5B 82.5(6) . . . . ? C3B S1B C1Ba C2Ba -43.6(5) . . . . ? C8B C7B C2Ba C1Ba -161.3(9) . . . . ? C8B C7B C2Ba S2B 74.0(10) . . . . ? C5B C1Ba C2Ba C7B 176.6(6) . . . . ? S1B C1Ba C2Ba C7B -56.9(7) . . . . ? C5B C1Ba C2Ba S2B -53.6(7) . . . . ? S1B C1Ba C2Ba S2B 72.9(5) . . . . ? C4B S2B C2Ba C7B 66.2(5) . . . . ? C4B S2B C2Ba C1Ba -60.0(5) . . . . ? C8A C7A C1Cb C2Cb 44(2) . . . . ? C8A C7A C1Cb S1A 170.6(11) . . . . ? C3A S1A C1Cb C2Cb 65.8(14) . . . . ? C3A S1A C1Cb C7A -57.6(15) . . . . ? C7A C1Cb C2Cb C5A -167.5(9) . . . . ? S1A C1Cb C2Cb C5A 55.6(15) . . . . ? C7A C1Cb C2Cb S2A 58.3(17) . . . . ? S1A C1Cb C2Cb S2A -78.7(15) . . . . ? C6A C5A C2Cb C1Cb 24(2) . . . . ? C6A C5A C2Cb S2A 155.5(12) . . . . ? C4A S2A C2Cb C1Cb 42.5(16) . . . . ? C4A S2A C2Cb C5A -83.8(12) . . . . ? C8B C7B C1Db C2Db 26(3) . . . . ? C8B C7B C1Db S1B 156.1(14) . . . . ? C7B C1Db C2Db C5B -169.4(10) . . . . ? S1B C1Db C2Db C5B 57.9(17) . . . . ? C7B C1Db C2Db S2B 48.3(19) . . . . ? S1B C1Db C2Db S2B -84.4(15) . . . . ? C6B C5B C2Db C1Db 117.5(17) . . . . ? C6B C5B C2Db S2B -112.5(18) . . . . ? C4B S2B C2Db C1Db 54.5(17) . . . . ? C4B S2B C2Db C5B -73.3(19) . . . . ?