#------------------------------------------------------------------------------ #$Date: 2019-11-10 07:58:01 +0200 (Sun, 10 Nov 2019) $ #$Revision: 225926 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/58/4515823.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_4515823 loop_ _publ_author_name 'Beromi, Megan Mohadjer' 'Banerjee, Gourab' 'Brudvig, Gary W.' 'Hazari, Nilay' 'Mercado, Brandon Q.' _publ_section_title ; Nickel(I) Aryl Species: Synthesis, Properties, and Catalytic Activity. ; _journal_issue 3 _journal_name_full 'ACS catalysis' _journal_page_first 2526 _journal_page_last 2533 _journal_paper_doi 10.1021/acscatal.8b00546 _journal_volume 8 _journal_year 2018 _chemical_formula_moiety 'C56 H53 Fe Ni P2' _chemical_formula_sum 'C56 H53 Fe Ni P2' _chemical_formula_weight 902.48 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-I 2ya' _space_group_name_H-M_alt 'I 1 2/a 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary SHELXT _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 95.985(7) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.0344(9) _cell_length_b 13.3580(9) _cell_length_c 23.5713(19) _cell_measurement_reflns_used 5482 _cell_measurement_temperature 93(2) _cell_measurement_theta_max 26.2760 _cell_measurement_theta_min 2.2310 _cell_volume 4394.9(5) _computing_cell_refinement 'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.16b (Rigaku OD, 2015)' _computing_molecular_graphics ; Dolomanov, O.V.; Bourhis, L.J.; Gildea, R.J.; Howard, J.A.K.; Puschmann, H., OLEX2: A complete structure solution, refinement and analysis program (2009). J. Appl. Cryst., 42, 339-341. ; _computing_publication_material 'CIFTAB-2013/2 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT-2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 93(2) _diffrn_detector_area_resol_mean 6.8 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Rigaku Mercury275R CCD' _diffrn_measurement_method \w _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0764 _diffrn_reflns_av_unetI/netI 0.0463 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 28371 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.425 _diffrn_reflns_theta_min 2.635 _diffrn_source 'fine-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.870 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.84705 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.16b (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour Orange _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Plate _exptl_crystal_F_000 1892 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.050 _refine_diff_density_max 0.641 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.081 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 311 _refine_ls_number_reflns 4514 _refine_ls_number_restraints 76 _refine_ls_restrained_S_all 1.030 _refine_ls_R_factor_all 0.0778 _refine_ls_R_factor_gt 0.0475 _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^)+(0.0563P)^2^+8.6511P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1098 _refine_ls_wR_factor_ref 0.1246 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3209 _reflns_number_total 4514 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs8b00546_si_002.cif _cod_data_source_block '_(dppf)NiI(2,6-xylyl)' _cod_original_sg_symbol_H-M 'I 2/a' _cod_database_code 4515823 _shelx_shelxl_version_number 2014/7 _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 0.780 _shelx_estimated_absorpt_t_max 0.958 _shelx_res_file ; mini-17045.res created by SHELXL-2014/7 TITL mini-17045 CELL 0.71073 14.0344 13.358 23.5713 90 95.985 90 ZERR 4 0.0009 0.0009 0.0019 0 0.007 0 LATT 2 SYMM 0.5-X,+Y,-Z SFAC C H Fe Ni P UNIT 224 212 4 4 8 DFIX 1.395 0.002 C31 C26 C31 C30 C30 C29 C29 C28 C28 C27 C27 C26 SADI C2 C1 C3 C2 C4 C3 C6 C5 C6 C1 C4 C5 SADI C6 C8 C2 C7 RIGU C1 C2 C3 C4 C5 C6 C7 C8 L.S. 10 SIZE 0.3 0.05 0.05 TEMP -180 BOND $H CONF MORE -1 ACTA OMIT 1 1 0 OMIT 0 1 1 OMIT 0 0 2 WGHT 0.056300 8.651102 FVAR 0.17087 NI1 4 0.750000 0.258210 0.500000 10.50000 0.02385 0.01872 = 0.03517 0.00000 0.00233 0.00000 FE1 3 0.750000 0.580651 0.500000 10.50000 0.01976 0.01928 = 0.02581 0.00000 0.00226 0.00000 P1 5 0.706312 0.359501 0.565608 11.00000 0.02130 0.02314 = 0.02573 0.00320 0.00022 -0.00096 PART -1 C1 1 0.767457 0.113056 0.500077 10.50000 0.04712 0.02393 = 0.02555 -0.00145 0.00924 0.00182 C2 1 0.856510 0.068051 0.520150 10.50000 0.05067 0.02998 = 0.02991 0.00302 0.01101 0.00818 C3 1 0.865197 -0.035925 0.522456 10.50000 0.08374 0.03139 = 0.05025 0.00581 0.02322 0.01367 AFIX 43 H3 2 0.925394 -0.065979 0.534170 10.50000 -1.20000 AFIX 0 C4 1 0.783836 -0.096219 0.507248 10.50000 0.09802 0.02222 = 0.03695 -0.00195 0.03137 -0.00135 AFIX 43 H4 2 0.790042 -0.166855 0.510542 10.50000 -1.20000 AFIX 0 C5 1 0.695584 -0.056417 0.487768 10.50000 0.09554 0.02428 = 0.04813 -0.00111 0.02335 -0.00036 AFIX 43 H5 2 0.641708 -0.097970 0.477211 10.50000 -1.20000 AFIX 0 C6 1 0.689268 0.048740 0.484300 10.50000 0.05494 0.02303 = 0.03748 -0.00105 0.00674 -0.00690 C7 1 0.942608 0.133326 0.538830 10.50000 0.04848 0.04078 = 0.04766 0.00689 -0.00465 0.01092 AFIX 137 H7A 2 0.942305 0.192136 0.513956 10.50000 -1.50000 H7B 2 1.001536 0.094976 0.536276 10.50000 -1.50000 H7C 2 0.939579 0.155015 0.578319 10.50000 -1.50000 AFIX 0 C8 1 0.594367 0.091137 0.461981 10.50000 0.05448 0.02577 = 0.05750 -0.00097 0.00089 -0.01682 AFIX 137 H8A 2 0.569356 0.132039 0.491604 10.50000 -1.50000 H8B 2 0.549591 0.036433 0.451172 10.50000 -1.50000 H8C 2 0.601810 0.132793 0.428504 10.50000 -1.50000 AFIX 0 PART 0 C9 1 0.682564 0.491463 0.553507 11.00000 0.02267 0.02228 = 0.02391 -0.00183 0.00659 -0.00320 C10 1 0.724518 0.575653 0.584112 11.00000 0.02586 0.03000 = 0.02592 -0.00324 0.00470 -0.00442 AFIX 43 H10 2 0.771269 0.572320 0.616244 11.00000 -1.20000 AFIX 0 C11 1 0.685325 0.664816 0.558927 11.00000 0.03603 0.02137 = 0.03197 -0.00628 0.01269 0.00028 AFIX 43 H11 2 0.701298 0.731098 0.571051 11.00000 -1.20000 AFIX 0 C12 1 0.617755 0.637523 0.512226 11.00000 0.02399 0.02331 = 0.03635 0.00379 0.00794 0.00505 AFIX 43 H12 2 0.580525 0.682611 0.487882 11.00000 -1.20000 AFIX 0 C13 1 0.615439 0.531480 0.508201 11.00000 0.01867 0.02656 = 0.02640 0.00035 0.00455 -0.00133 AFIX 43 H13 2 0.576699 0.493395 0.480651 11.00000 -1.20000 AFIX 0 C14 1 0.803463 0.359785 0.624110 11.00000 0.02595 0.02605 = 0.02984 0.00313 -0.00476 0.00059 C15 1 0.897393 0.351107 0.610700 11.00000 0.03167 0.03205 = 0.03247 0.00787 0.00139 -0.00224 AFIX 43 H15 2 0.909760 0.346824 0.571910 11.00000 -1.20000 AFIX 0 C16 1 0.973180 0.348660 0.653571 11.00000 0.02481 0.03691 = 0.04413 0.00784 -0.00500 0.00052 AFIX 43 H16 2 1.037037 0.343136 0.643944 11.00000 -1.20000 AFIX 0 C17 1 0.956165 0.354200 0.709872 11.00000 0.03314 0.05276 = 0.04449 0.00402 -0.01424 0.00418 AFIX 43 H17 2 1.008235 0.352586 0.739043 11.00000 -1.20000 AFIX 0 C18 1 0.863495 0.362105 0.724055 11.00000 0.04326 0.06870 = 0.03009 -0.00399 -0.00959 0.01039 AFIX 43 H18 2 0.851684 0.365519 0.762966 11.00000 -1.20000 AFIX 0 C19 1 0.787470 0.365060 0.681256 11.00000 0.03172 0.05059 = 0.03553 -0.00129 0.00011 0.00730 AFIX 43 H19 2 0.723806 0.370754 0.691186 11.00000 -1.20000 AFIX 0 C20 1 0.601935 0.321512 0.601142 11.00000 0.02540 0.03050 = 0.01834 0.00367 -0.00150 -0.00086 C21 1 0.580730 0.220027 0.604366 11.00000 0.04160 0.02953 = 0.02567 0.00156 0.00773 -0.00125 AFIX 43 H21 2 0.620480 0.172029 0.588657 11.00000 -1.20000 AFIX 0 C22 1 0.501911 0.188827 0.630388 11.00000 0.04886 0.03702 = 0.03542 0.00717 0.01049 -0.01167 AFIX 43 H22 2 0.487669 0.119445 0.632189 11.00000 -1.20000 AFIX 0 C23 1 0.444179 0.257100 0.653596 11.00000 0.03261 0.05465 = 0.02979 0.01155 0.00661 -0.00582 AFIX 43 H23 2 0.389609 0.235042 0.670797 11.00000 -1.20000 AFIX 0 C24 1 0.465332 0.357668 0.651962 11.00000 0.02711 0.04727 = 0.02788 0.00461 0.00480 0.00707 AFIX 43 H24 2 0.426676 0.404870 0.669179 11.00000 -1.20000 AFIX 0 C25 1 0.543881 0.390167 0.624887 11.00000 0.02599 0.03282 = 0.02842 0.00230 0.00084 0.00074 AFIX 43 H25 2 0.557398 0.459678 0.622804 11.00000 -1.20000 AFIX 0 C26 1 0.687357 0.498192 0.803646 11.00000 0.05887 0.06066 = 0.05960 -0.00446 0.01829 0.01202 C27 1 0.756466 0.509175 0.849840 11.00000 0.08997 0.09485 = 0.05236 0.00002 0.01069 0.02784 AFIX 43 H27 2 0.753124 0.470034 0.883224 11.00000 -1.20000 AFIX 0 C28 1 0.830550 0.577514 0.847175 11.00000 0.05013 0.16509 = 0.06672 -0.05188 -0.00688 0.01492 AFIX 43 H28 2 0.877734 0.584067 0.878912 11.00000 -1.20000 AFIX 0 C29 1 0.837232 0.636535 0.799136 11.00000 0.07939 0.09111 = 0.10681 -0.04239 0.03634 -0.02650 AFIX 43 H29 2 0.886933 0.684681 0.798517 11.00000 -1.20000 AFIX 0 C30 1 0.769979 0.623917 0.752036 11.00000 0.08625 0.05631 = 0.07563 -0.01308 0.02063 -0.00070 AFIX 43 H30 2 0.775335 0.659960 0.717770 11.00000 -1.20000 AFIX 0 C31 1 0.694866 0.557599 0.756097 11.00000 0.04265 0.06061 = 0.07457 0.00953 0.00047 0.00812 AFIX 43 H31 2 0.646445 0.552699 0.724903 11.00000 -1.20000 AFIX 0 C32 1 0.607540 0.424042 0.802660 11.00000 0.10508 0.08618 = 0.12590 -0.01104 0.05131 -0.02844 AFIX 137 H32A 2 0.573099 0.433614 0.836344 11.00000 -1.50000 H32B 2 0.633815 0.356053 0.802899 11.00000 -1.50000 H32C 2 0.563338 0.433809 0.768091 11.00000 -1.50000 AFIX 0 HKLF 4 REM mini-17045 REM R1 = 0.0475 for 3209 Fo > 4sig(Fo) and 0.0778 for all 4514 data REM 311 parameters refined using 76 restraints END WGHT 0.0563 8.6593 REM Highest difference peak 0.641, deepest hole -0.486, 1-sigma level 0.081 Q1 1 0.6866 0.5974 0.7917 11.00000 0.05 0.64 Q2 1 0.7051 0.7990 0.5662 11.00000 0.05 0.37 Q3 1 0.7500 0.4820 0.5000 10.50000 0.05 0.37 Q4 1 0.5041 0.3726 0.6310 11.00000 0.05 0.34 Q5 1 0.7279 0.5394 0.8302 11.00000 0.05 0.32 Q6 1 0.7500 -0.0803 0.5000 10.50000 0.05 0.32 Q7 1 0.5521 0.0369 0.4283 11.00000 0.05 0.30 Q8 1 0.7309 0.3372 0.5288 11.00000 0.05 0.30 Q9 1 0.7180 0.5471 0.7632 11.00000 0.05 0.29 Q10 1 0.7140 0.4191 0.8274 11.00000 0.05 0.29 Q11 1 0.7158 0.2655 0.5319 11.00000 0.05 0.28 Q12 1 0.4506 0.2578 0.6765 11.00000 0.05 0.28 Q13 1 0.8124 0.5295 0.8293 11.00000 0.05 0.27 Q14 1 0.9786 0.4449 0.6800 11.00000 0.05 0.27 Q15 1 0.8214 0.6293 0.7887 11.00000 0.05 0.26 Q16 1 0.5386 0.4325 0.6198 11.00000 0.05 0.26 Q17 1 0.9766 0.0912 0.5502 11.00000 0.05 0.25 Q18 1 0.4061 0.2471 0.6991 11.00000 0.05 0.25 Q19 1 0.5792 0.3845 0.6485 11.00000 0.05 0.25 Q20 1 0.9319 0.3206 0.6290 11.00000 0.05 0.24 ; _shelx_res_checksum 69568 _shelx_hkl_file ; 0 0 -2 -0.53 0.69 0 0 2 -0.37 0.53 0 0 2 -1.49 0.92 0 0 4 835.91 13.81 0 0 -4 875.63 14.02 0 0 4 845.30 13.48 0 0 -4 838.86 10.46 0 0 6 2188.96 27.38 0 0 -6 2331.24 21.37 0 0 6 2342.36 27.66 0 0 -6 2297.55 27.98 0 0 8 1824.86 28.93 0 0 8 1729.14 28.07 0 0 -8 1840.03 28.98 0 0 -8 1845.23 22.37 0 0 10 593.39 18.67 0 0 10 587.12 18.79 0 0 -10 607.49 14.54 0 0 -10 592.78 18.70 0 0 12 713.40 22.45 0 0 -12 709.41 22.48 0 0 12 688.16 22.14 0 0 -12 690.03 17.04 0 0 -14 1253.07 24.77 0 0 14 1251.22 32.34 0 0 14 1253.72 32.75 0 0 -14 1241.69 32.25 0 0 16 783.55 28.40 0 0 -16 797.11 28.46 0 0 -16 793.14 21.28 0 0 16 800.31 28.29 0 0 18 496.59 24.19 0 0 18 517.32 24.78 0 0 -18 515.77 18.54 0 0 -18 488.62 23.70 0 0 20 332.84 21.29 0 0 -20 357.94 22.12 0 0 -20 313.78 16.37 0 0 20 336.60 21.76 0 0 -22 -1.13 5.10 0 0 22 2.85 6.84 0 0 -22 -5.06 6.08 0 0 22 -4.95 6.76 0 0 -24 -0.26 6.39 0 0 24 3.06 7.89 0 0 24 4.34 6.83 0 0 26 58.66 13.01 0 0 -26 32.13 9.82 0 0 26 57.54 12.44 0 0 -28 64.90 13.20 0 0 28 46.83 11.49 0 0 28 26.44 11.44 0 1 1 -0.34 0.50 0 -1 1 -1.33 0.82 0 -1 -1 -0.76 0.70 0 1 -1 -1.85 1.05 0 1 -3 248.51 6.87 0 -1 -3 254.19 7.48 0 1 3 248.92 6.51 0 1 3 252.94 6.91 0 -1 3 250.34 7.05 0 -1 3 248.29 6.78 0 1 -3 257.04 7.09 0 -1 -5 446.37 6.92 0 1 -5 450.94 11.60 0 -1 5 445.74 11.56 0 1 5 442.98 11.26 0 1 -5 489.23 11.59 0 -1 5 431.80 11.99 0 1 5 483.09 12.33 0 -1 -5 449.45 11.97 0 1 -7 14.55 3.30 0 1 7 13.27 3.38 0 -1 -7 12.04 1.94 0 -1 7 11.13 3.67 0 1 7 9.72 3.68 0 -1 7 14.53 3.19 0 1 -7 14.95 3.57 0 -1 -7 14.40 3.74 0 -1 9 38.37 5.63 0 -1 -9 44.21 5.65 0 1 9 42.03 5.67 0 1 -9 49.10 5.84 0 -1 9 53.39 6.06 0 -1 -9 46.63 3.91 0 1 9 50.35 6.34 0 1 -9 47.32 5.34 0 -1 -11 61.81 5.03 0 1 11 62.13 7.05 0 1 -11 56.30 7.00 0 -1 11 57.53 7.00 0 1 -11 66.65 7.11 0 1 11 60.89 7.18 0 -1 11 66.91 7.90 0 -1 -11 56.98 6.64 0 -1 -13 218.23 13.20 0 1 -13 234.19 13.59 0 1 -13 236.83 12.59 0 -1 13 221.20 13.69 0 -1 13 210.97 13.60 0 -1 -13 231.08 9.81 0 1 13 215.18 13.13 0 1 13 234.16 14.03 0 -1 -15 258.81 11.20 0 1 15 273.05 16.33 0 -1 -15 237.45 15.49 0 -1 15 269.96 16.36 0 1 15 268.95 15.65 0 1 -15 279.62 15.83 0 -1 15 293.14 17.03 0 1 -15 232.84 13.59 0 1 -17 352.62 19.38 0 1 17 373.28 20.54 0 -1 17 378.66 21.00 0 -1 17 363.40 20.06 0 1 -17 359.77 16.45 0 1 17 344.72 19.37 0 -1 -17 380.32 20.07 0 -1 -17 368.64 14.16 0 1 19 98.44 11.61 0 1 -19 80.56 10.78 0 -1 -19 91.49 11.57 0 1 19 87.78 12.00 0 -1 19 81.59 11.97 0 -1 19 88.75 11.70 0 -1 -19 81.00 8.16 0 1 -19 79.94 9.90 0 -1 21 -3.69 6.65 0 1 -21 11.08 7.29 0 -1 -21 -8.74 5.81 0 1 21 -1.71 6.06 0 -1 21 -5.00 5.86 0 1 -21 18.20 8.72 0 1 21 2.73 6.97 0 -1 -21 -0.30 5.11 0 1 -23 26.73 7.38 0 -1 -23 18.98 7.94 0 1 -23 25.94 7.74 0 -1 23 33.27 10.57 0 -1 23 16.23 8.36 0 1 23 28.50 9.26 0 1 23 20.03 8.93 0 1 25 -0.97 6.44 0 1 -25 -9.43 7.40 0 1 25 7.81 8.84 0 -1 -25 -3.04 6.25 0 -1 25 -2.39 6.82 0 -1 25 4.67 8.67 0 -1 27 31.32 11.07 0 1 27 10.81 8.28 0 1 27 12.95 9.18 0 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12 5.81 4.02 0 2 -12 10.19 5.23 0 -2 12 7.25 4.41 0 2 12 3.47 5.10 0 2 -12 8.33 4.21 0 -2 -12 8.79 2.54 0 -2 12 7.22 4.70 0 -2 -12 4.90 4.55 0 2 -14 7.95 4.42 0 -2 14 7.33 4.20 0 2 14 12.54 4.94 0 -2 14 15.01 5.44 0 2 -14 19.08 6.28 0 -2 -14 12.15 3.20 0 -2 -14 15.08 5.50 0 2 14 6.44 4.55 0 2 -16 -3.86 5.19 0 2 -16 1.19 5.44 0 -2 -16 -1.82 4.30 0 2 16 -4.96 5.33 0 -2 16 -0.45 4.46 0 -2 -16 -5.90 3.87 0 2 16 8.32 5.49 0 -2 16 -1.56 4.86 0 -2 -18 77.73 7.40 0 -2 -18 63.78 10.13 0 -2 18 83.69 11.51 0 -2 18 58.42 9.46 0 2 18 68.47 10.33 0 2 -18 77.93 10.39 0 2 18 54.43 8.70 0 2 -18 65.59 9.50 0 -2 -20 -10.07 7.77 0 2 -20 10.04 5.29 0 2 20 -1.65 5.70 0 -2 20 8.27 6.76 0 2 20 13.03 6.76 0 2 -20 4.86 7.03 0 -2 20 1.11 6.07 0 2 -22 -3.57 7.17 0 -2 -22 0.73 6.83 0 2 -22 6.98 7.06 0 -2 22 5.93 7.09 0 2 22 7.71 8.21 0 -2 22 -1.27 6.60 0 2 22 -8.99 7.66 0 -2 -24 -6.41 7.24 0 2 -24 -0.17 5.85 0 -2 24 -13.02 8.98 0 -2 24 10.21 7.90 0 2 24 -10.72 8.78 0 2 24 10.71 7.28 0 2 -24 -5.96 6.78 0 2 26 10.48 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-7 -4 9.80 10.67 15 -7 4 8.24 7.49 -15 -7 -4 3.87 9.78 -15 7 -6 7.61 9.06 15 7 6 6.80 8.66 15 -7 6 -12.13 9.08 -15 -7 -6 -11.95 11.90 -15 -8 7 4.81 9.36 -15 8 7 8.06 9.39 -15 -8 7 5.47 8.80 15 8 -7 9.73 8.83 15 -8 -7 6.26 8.16 -15 -8 5 21.95 10.63 -15 8 5 0.54 10.91 -15 -8 5 18.67 11.63 15 8 -5 15.38 8.36 15 -8 -5 10.51 8.53 -15 -8 3 9.02 9.86 -15 8 3 1.30 9.41 -15 -8 3 8.75 8.09 15 -8 -3 6.11 7.36 15 8 -3 -3.50 7.38 -15 8 1 24.93 12.08 -15 -8 1 6.25 9.07 -15 -8 1 7.51 9.59 15 -8 -1 5.54 7.06 15 8 -1 10.46 8.05 -15 8 -1 24.80 14.12 -15 -8 -1 5.75 10.29 -15 -8 -1 24.96 9.76 15 -8 1 22.06 10.81 15 8 1 13.52 8.19 -15 8 -3 -2.41 10.69 -15 -8 -3 18.16 12.23 -15 -8 -3 -1.25 9.54 15 -8 3 15.24 8.67 16 0 -14 39.08 10.95 -16 0 14 7.80 9.86 16 0 -12 28.26 10.67 -16 0 12 8.45 9.05 16 0 -10 15.99 9.13 -16 0 10 -6.56 8.80 -16 0 8 64.97 12.78 16 0 -8 89.77 13.69 16 0 -6 186.28 18.52 -16 0 6 177.04 18.90 -16 0 4 287.43 22.91 -16 0 4 305.64 29.45 -16 0 2 116.21 14.72 -16 0 2 109.65 18.12 16 0 -2 115.93 12.67 -16 0 0 42.88 10.12 -16 0 0 51.12 12.80 -16 0 0 64.89 15.09 16 0 0 72.17 10.91 -16 0 -2 98.55 14.77 -16 0 -2 81.12 16.47 -16 0 -2 54.70 11.01 16 0 2 97.42 12.49 -16 0 -4 86.96 15.72 -16 0 -4 43.78 11.06 16 0 4 58.78 9.87 16 0 4 76.14 11.34 16 0 4 64.35 11.07 16 0 6 22.35 7.62 16 0 6 26.26 7.94 -16 0 -8 105.07 17.58 16 0 8 155.73 17.82 16 0 8 113.01 14.02 16 -1 -13 -6.39 8.65 16 1 -13 -4.34 7.25 -16 1 13 3.83 8.93 -16 -1 13 -5.77 9.10 16 -1 -11 6.30 7.36 16 1 -11 -1.08 6.92 -16 1 11 7.63 9.29 -16 -1 11 -2.75 8.86 16 -1 -9 15.47 8.16 16 1 -9 29.88 11.19 -16 1 9 13.86 9.20 -16 -1 9 -1.96 7.52 -16 1 7 23.28 9.25 -16 -1 7 10.18 8.52 -16 1 7 13.47 11.03 16 1 -7 22.89 7.67 -16 -1 5 83.82 14.94 -16 1 5 38.49 9.54 -16 1 5 59.84 14.88 16 1 -5 76.39 12.50 -16 -1 3 63.89 11.34 -16 1 3 78.61 17.11 16 -1 -3 45.07 8.55 16 1 -3 64.62 11.95 -16 -1 1 21.58 8.37 -16 1 1 1.49 8.49 -16 -1 1 10.33 9.00 16 1 -1 5.10 4.89 16 -1 -1 -1.52 5.51 -16 -1 1 5.40 6.24 -16 -1 -1 7.66 7.58 -16 1 -1 27.11 12.42 -16 -1 -1 12.71 9.04 -16 -1 -1 10.67 10.41 16 1 1 8.32 5.63 16 -1 1 13.37 6.47 -16 -1 -1 3.47 7.14 -16 1 -3 58.30 14.51 -16 1 -3 57.70 11.89 -16 -1 -3 64.04 13.56 -16 -1 -3 53.74 10.98 -16 -1 -3 42.79 12.66 16 1 3 32.33 8.59 16 1 3 42.49 9.09 16 -1 3 47.46 9.81 -16 1 -5 14.05 12.24 -16 -1 -5 16.51 8.59 16 1 5 7.56 6.29 16 1 5 14.72 7.89 16 1 5 3.51 6.02 16 -1 5 1.03 5.76 -16 1 -7 6.97 10.94 -16 -1 -7 19.45 11.01 16 1 7 2.62 5.58 16 1 7 13.05 7.89 16 1 7 18.74 7.84 16 -1 7 8.88 8.03 -16 1 -9 36.88 13.34 16 -1 9 25.34 9.94 -16 -1 -9 21.38 12.06 16 -2 -14 -1.54 8.15 16 2 -14 -7.15 8.84 -16 2 14 2.03 8.16 -16 -2 14 12.83 11.08 16 -2 -12 -18.84 10.70 16 2 -12 3.00 6.77 -16 2 12 1.68 7.19 -16 -2 12 -0.37 8.75 16 2 -10 -1.93 6.88 -16 -2 10 8.34 10.25 -16 -2 8 6.49 9.06 -16 2 8 -1.36 11.57 16 2 -8 18.29 8.82 -16 -2 6 10.84 9.39 -16 -2 6 8.47 11.01 -16 2 6 6.40 10.45 -16 -2 6 2.67 6.70 16 2 -6 13.27 8.94 -16 -2 4 11.35 9.11 -16 2 4 0.88 9.63 -16 -2 4 15.94 10.26 -16 -2 4 -6.37 7.04 16 -2 -4 2.23 5.87 16 2 -4 5.96 6.95 -16 -2 2 18.57 9.10 -16 2 2 26.81 12.20 -16 -2 2 23.31 9.53 16 -2 -2 17.32 6.86 -16 -2 2 16.68 8.53 16 2 -2 13.89 7.29 -16 -2 0 -2.98 7.58 -16 2 0 0.59 8.24 -16 -2 0 6.79 9.22 16 2 0 5.17 5.21 16 -2 0 -1.76 5.04 -16 -2 0 -0.63 7.01 16 2 0 4.45 6.63 -16 2 -2 2.00 8.52 -16 -2 -2 9.14 8.24 -16 -2 -2 -8.27 8.36 16 2 2 11.27 7.06 16 -2 2 1.50 5.51 -16 -2 -2 16.78 9.74 16 2 2 4.33 5.67 -16 2 -4 10.09 9.53 -16 2 -4 8.13 8.02 16 2 4 0.69 5.75 16 2 4 10.25 8.09 16 2 4 -3.52 5.67 16 -2 4 6.27 7.25 16 2 4 2.41 5.93 -16 2 -6 20.85 11.76 16 2 6 14.27 8.34 16 2 6 2.98 7.27 16 -2 6 -11.45 8.25 -16 -2 -6 5.93 8.93 16 2 6 0.19 6.07 -16 2 -8 -3.33 9.60 16 2 8 12.58 8.24 16 2 8 0.71 7.39 16 -2 8 1.17 7.19 16 -3 -13 -0.20 6.71 16 3 -13 32.66 11.01 -16 -3 13 29.22 12.38 -16 -3 11 12.71 12.92 -16 3 11 7.60 11.19 -16 -3 11 6.05 7.72 16 3 -11 23.84 9.10 -16 -3 11 7.34 8.95 -16 -3 9 -5.68 10.25 -16 -3 9 2.70 10.69 -16 3 9 29.63 13.93 -16 -3 9 6.40 8.42 16 3 -9 -3.58 7.66 -16 -3 7 8.28 9.82 -16 3 7 -11.77 10.97 -16 -3 7 28.59 13.48 -16 -3 7 13.63 9.33 16 3 -7 -3.92 6.88 16 -3 -7 11.66 6.42 -16 -3 5 41.17 11.79 -16 3 5 55.25 14.47 -16 -3 5 40.50 12.91 -16 -3 5 60.45 12.34 16 -3 -5 36.74 8.50 16 3 -5 54.59 11.25 -16 -3 3 15.76 9.27 -16 3 3 10.75 11.20 -16 -3 3 9.76 7.61 16 -3 -3 3.14 4.96 16 3 -3 17.42 7.53 -16 -3 1 -6.67 7.95 -16 3 1 -5.73 9.64 -16 -3 1 -1.36 7.59 16 -3 -1 8.48 6.90 -16 -3 1 5.49 6.99 16 3 -1 7.89 6.74 -16 3 -1 10.83 8.93 -16 -3 -1 11.31 8.40 -16 -3 -1 3.81 7.69 16 -3 1 -1.19 5.42 -16 -3 -1 17.02 9.46 16 3 1 5.84 5.44 -16 3 -3 8.30 9.71 -16 -3 -3 4.90 7.58 16 3 3 10.44 6.98 16 -3 3 6.93 6.22 -16 -3 -3 6.33 8.64 16 3 3 0.93 5.57 -16 -3 -5 -1.73 7.88 -16 3 -5 -4.96 8.82 16 3 5 18.98 8.74 16 -3 5 9.78 6.60 16 3 5 7.31 5.97 -16 3 -7 -5.47 8.87 16 3 7 3.87 6.44 16 3 7 9.82 9.35 16 -3 7 10.57 7.36 -16 -3 -7 -3.43 10.00 -16 -4 12 30.27 12.09 -16 4 12 60.34 17.04 -16 -4 12 28.98 10.13 16 4 -12 72.08 13.26 -16 -4 12 31.94 11.89 -16 -4 10 9.95 11.04 -16 4 10 11.82 13.19 -16 -4 10 -5.02 10.78 -16 -4 10 6.84 9.70 16 4 -10 14.21 8.06 -16 -4 8 5.80 8.78 -16 4 8 -9.25 10.67 -16 -4 8 -0.53 8.55 -16 -4 8 6.94 9.85 16 4 -8 4.98 7.34 16 -4 -8 1.02 5.26 -16 -4 6 14.28 10.81 -16 4 6 9.56 11.20 -16 -4 6 -2.93 8.29 -16 -4 6 -4.58 7.83 16 4 -6 4.65 6.08 16 -4 -6 13.83 8.01 -16 -4 4 15.53 9.70 -16 4 4 20.54 10.83 -16 -4 4 29.20 12.14 -16 -4 4 9.32 8.51 16 -4 -4 7.84 6.34 16 4 -4 24.79 8.93 -16 -4 2 2.96 8.27 -16 4 2 18.59 11.84 -16 -4 2 5.19 10.19 -16 -4 2 3.35 8.29 16 -4 -2 2.50 5.62 16 4 -2 -5.78 6.78 -16 -4 0 65.13 13.60 -16 4 0 80.70 16.09 16 -4 0 89.82 13.35 -16 -4 0 76.07 13.82 16 4 0 88.75 12.55 -16 4 -2 7.81 10.98 -16 -4 -2 -0.87 8.70 16 -4 2 0.87 6.24 -16 -4 -2 2.53 8.72 16 4 2 1.79 6.36 -16 4 -4 8.35 9.28 -16 -4 -4 10.13 7.55 -16 -4 -4 1.93 7.80 16 -4 4 21.02 9.04 -16 -4 -4 28.81 10.90 16 4 4 21.68 7.62 -16 4 -6 48.54 14.98 16 4 6 32.39 9.85 -16 -4 -6 35.95 12.00 16 -4 6 42.82 11.63 -16 -5 11 7.47 10.30 -16 5 11 27.21 15.55 -16 -5 11 -3.18 9.70 -16 -5 11 9.04 10.01 -16 -5 9 -0.74 8.94 -16 5 9 -0.15 11.36 -16 -5 9 12.02 11.03 -16 -5 9 17.52 10.36 16 5 -9 16.61 8.41 16 -5 -9 17.68 7.97 -16 -5 7 18.50 12.47 -16 5 7 -1.26 10.18 -16 -5 7 14.72 10.10 -16 -5 7 -3.08 9.94 16 5 -7 14.80 8.12 16 -5 -7 8.33 6.17 -16 -5 5 34.71 13.32 -16 5 5 25.62 14.18 -16 -5 5 7.73 10.54 -16 -5 5 42.04 12.83 16 5 -5 34.03 9.90 16 -5 -5 40.53 10.88 -16 -5 3 -5.30 8.58 -16 5 3 1.31 11.66 -16 -5 3 0.79 7.62 16 -5 -3 5.03 6.20 16 5 -3 9.72 7.67 -16 -5 1 -3.77 8.88 -16 5 1 3.61 9.50 -16 -5 1 -3.83 8.80 16 -5 -1 6.99 6.89 16 5 -1 9.26 7.02 -16 5 -1 7.71 10.84 -16 -5 -1 -0.35 7.59 16 -5 1 -6.74 7.50 -16 -5 -1 -11.67 8.19 16 5 1 -5.00 5.95 -16 5 -3 19.38 13.59 -16 -5 -3 6.83 8.48 16 -5 3 3.47 6.48 -16 -5 -3 12.87 9.24 16 5 3 0.98 5.32 -16 5 -5 6.66 12.84 16 5 5 2.20 7.40 16 -5 5 5.89 7.07 -16 -5 -5 -8.80 9.37 -16 -6 8 58.32 14.84 -16 6 8 52.30 15.20 -16 -6 8 63.36 15.61 -16 -6 8 64.05 14.48 16 6 -8 107.11 16.11 16 -6 -8 58.01 11.70 -16 -6 6 82.03 17.17 -16 6 6 40.95 14.67 -16 -6 6 66.98 15.78 16 6 -6 70.40 13.04 16 -6 -6 58.08 11.57 -16 -6 4 11.46 11.47 -16 6 4 23.88 12.43 -16 -6 4 33.27 12.11 16 -6 -4 12.48 8.44 16 6 -4 15.87 8.93 -16 -6 2 25.62 10.25 -16 6 2 11.80 10.86 -16 -6 2 24.16 10.78 16 -6 -2 19.61 8.94 16 6 -2 8.18 6.56 -16 6 0 29.01 10.99 -16 -6 0 51.81 13.76 -16 -6 0 40.08 10.20 16 -6 0 35.51 9.94 16 6 0 60.70 11.30 -16 6 -2 27.07 13.15 -16 -6 -2 52.55 13.63 16 -6 2 28.49 9.56 -16 -6 -2 58.82 15.02 16 6 2 31.32 8.73 -17 0 9 -2.68 7.98 17 0 -9 -6.02 7.80 -17 0 7 19.84 10.90 17 0 -7 -0.15 6.68 -17 0 5 -0.10 7.87 17 0 -5 -0.39 7.80 -17 0 1 5.94 9.21 -17 0 1 -18.71 11.08 -17 0 -1 7.37 9.33 -17 0 -1 6.07 10.93 17 0 1 0.32 5.22 -17 0 -3 -9.88 10.58 -17 0 -3 10.25 8.78 17 0 3 4.82 6.69 -17 -1 10 14.60 10.23 17 -1 -10 10.32 7.64 -17 -1 8 -2.09 8.35 17 -1 -8 -4.26 7.21 17 1 -8 1.66 7.29 -17 -1 6 43.09 11.44 -17 1 6 40.78 16.05 17 1 -6 41.95 10.92 -17 -1 4 21.42 9.26 -17 -1 4 66.81 15.82 -17 1 4 34.84 13.90 17 1 -4 71.41 13.11 -17 -1 2 12.47 9.23 -17 -1 2 -6.61 8.99 -17 1 2 -2.00 9.41 17 -1 -2 6.95 6.04 17 1 -2 -3.62 7.38 -17 -1 0 0.68 7.58 -17 1 0 -12.38 12.12 -17 -1 0 -9.83 10.66 17 -1 0 13.60 7.17 17 1 0 3.40 6.44 -17 1 -2 2.13 9.62 -17 1 -2 -6.21 8.60 -17 -1 -2 -11.67 10.57 17 1 2 0.37 5.92 17 -1 2 7.60 6.43 -17 1 -4 17.60 10.61 -17 -1 -4 10.15 8.64 -17 -2 9 37.06 11.65 17 2 -9 22.48 9.09 -17 -2 7 12.49 10.00 -17 -2 7 -16.30 11.26 -17 2 7 3.73 10.09 17 2 -7 -8.95 8.23 -17 -2 5 11.81 10.61 -17 -2 5 21.61 11.81 -17 2 5 27.42 11.76 17 2 -5 38.42 10.95 -17 -2 3 11.55 9.39 -17 -2 3 20.73 11.45 17 -2 -3 9.06 6.72 17 2 -3 2.85 6.48 -17 -2 1 17.26 9.63 -17 2 1 25.72 12.71 -17 -2 1 25.51 11.79 17 -2 -1 13.38 7.56 17 2 -1 13.53 7.85 -17 2 -1 3.04 10.38 -17 -2 -1 -1.18 7.77 -17 -2 -1 6.48 8.10 17 -2 1 17.68 7.70 17 2 1 17.29 8.05 -17 2 -3 51.59 14.93 17 2 3 22.85 8.03 17 2 3 15.15 7.06 17 -2 3 20.52 7.67 17 2 3 38.19 9.94 -17 3 8 12.97 11.72 -17 -3 6 47.01 12.80 -17 3 6 32.84 13.57 -17 -3 6 27.79 12.36 17 3 -6 42.32 10.45 -17 -3 4 20.35 9.70 -17 3 4 25.75 12.96 -17 -3 4 28.08 12.13 -17 -3 4 22.51 10.49 17 -3 -4 28.16 8.49 17 3 -4 27.79 9.55 -17 -3 2 29.58 11.83 -17 3 2 9.36 9.47 -17 -3 2 22.92 12.23 -17 -3 2 19.11 9.54 17 -3 -2 14.13 7.39 17 3 -2 10.39 7.30 -17 -3 0 32.37 11.14 -17 3 0 51.23 14.35 -17 -3 0 22.78 8.79 17 -3 0 56.79 11.68 -17 -3 0 49.02 12.68 17 3 0 47.98 10.23 -17 3 -2 78.31 16.94 -17 4 5 41.71 15.38 -17 -4 3 38.74 12.25 -17 4 3 31.80 13.67 -17 -4 3 0.97 8.60 -17 -4 3 22.34 10.20 17 -4 -3 29.28 9.46 17 4 -3 10.53 6.75 0 0 0 0.00 0.00 TITL abs in I2/a REM I2/a (#15 in standard setting) CELL 0.71073 14.034385 13.358000 23.571293 90.0000 95.9855 90.0000 ZERR 19.00 0.000919 0.000854 0.001901 0.0000 0.0067 0.0000 LATT 2 SYMM -x+1/2, y,-z SFAC C H N O UNIT 209.00 190.00 19.00 19.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 66969 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' '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 Ni1 Ni 0.7500 0.25821(4) 0.5000 0.02597(17) Uani 1 2 d S T P . . Fe1 Fe 0.7500 0.58065(5) 0.5000 0.02163(16) Uani 1 2 d S T P . . P1 P 0.70631(6) 0.35950(6) 0.56561(3) 0.02355(19) Uani 1 1 d . . . . . C1 C 0.7675(6) 0.1131(5) 0.5001(8) 0.032(2) Uani 0.5 1 d D U P A -1 C2 C 0.8565(8) 0.0681(6) 0.5202(4) 0.036(2) Uani 0.5 1 d D U P A -1 C3 C 0.8652(7) -0.0359(6) 0.5225(4) 0.054(2) Uani 0.5 1 d D U P A -1 H3 H 0.9254 -0.0660 0.5342 0.065 Uiso 0.5 1 calc R U P A -1 C4 C 0.7838(7) -0.0962(6) 0.5072(5) 0.051(2) Uani 0.5 1 d D U P A -1 H4 H 0.7900 -0.1669 0.5105 0.061 Uiso 0.5 1 calc R U P A -1 C5 C 0.6956(9) -0.0564(6) 0.4878(5) 0.055(3) Uani 0.5 1 d D U P A -1 H5 H 0.6417 -0.0980 0.4772 0.066 Uiso 0.5 1 calc R U P A -1 C6 C 0.6893(7) 0.0487(6) 0.4843(4) 0.038(2) Uani 0.5 1 d D U P A -1 C7 C 0.9426(7) 0.1333(7) 0.5388(4) 0.046(2) Uani 0.5 1 d D U P A -1 H7A H 0.9423 0.1921 0.5140 0.069 Uiso 0.5 1 calc R U P A -1 H7B H 1.0015 0.0950 0.5363 0.069 Uiso 0.5 1 calc R U P A -1 H7C H 0.9396 0.1550 0.5783 0.069 Uiso 0.5 1 calc R U P A -1 C8 C 0.5944(8) 0.0911(7) 0.4620(5) 0.046(2) Uani 0.5 1 d D U P A -1 H8A H 0.5694 0.1320 0.4916 0.069 Uiso 0.5 1 calc R U P A -1 H8B H 0.5496 0.0364 0.4512 0.069 Uiso 0.5 1 calc R U P A -1 H8C H 0.6018 0.1328 0.4285 0.069 Uiso 0.5 1 calc R U P A -1 C9 C 0.6826(2) 0.4915(2) 0.55351(13) 0.0227(7) Uani 1 1 d . . . . . C10 C 0.7245(2) 0.5757(2) 0.58411(13) 0.0271(7) Uani 1 1 d . . . . . H10 H 0.7713 0.5723 0.6162 0.033 Uiso 1 1 calc R U . . . C11 C 0.6853(2) 0.6648(2) 0.55893(14) 0.0291(7) Uani 1 1 d . . . . . H11 H 0.7013 0.7311 0.5711 0.035 Uiso 1 1 calc R U . . . C12 C 0.6178(2) 0.6375(2) 0.51223(14) 0.0275(7) Uani 1 1 d . . . . . H12 H 0.5805 0.6826 0.4879 0.033 Uiso 1 1 calc R U . . . C13 C 0.6154(2) 0.5315(2) 0.50820(13) 0.0237(7) Uani 1 1 d . . . . . H13 H 0.5767 0.4934 0.4807 0.028 Uiso 1 1 calc R U . . . C14 C 0.8035(2) 0.3598(2) 0.62411(14) 0.0278(7) Uani 1 1 d . . . . . C15 C 0.8974(2) 0.3511(3) 0.61070(15) 0.0322(8) Uani 1 1 d . . . . . H15 H 0.9098 0.3468 0.5719 0.039 Uiso 1 1 calc R U . . . C16 C 0.9732(2) 0.3487(3) 0.65357(16) 0.0359(8) Uani 1 1 d . . . . . H16 H 1.0370 0.3431 0.6439 0.043 Uiso 1 1 calc R U . . . C17 C 0.9562(3) 0.3542(3) 0.70987(17) 0.0447(10) Uani 1 1 d . . . . . H17 H 1.0082 0.3526 0.7390 0.054 Uiso 1 1 calc R U . . . C18 C 0.8635(3) 0.3621(3) 0.72405(16) 0.0483(10) Uani 1 1 d . . . . . H18 H 0.8517 0.3655 0.7630 0.058 Uiso 1 1 calc R U . . . C19 C 0.7875(3) 0.3651(3) 0.68126(15) 0.0395(9) Uani 1 1 d . . . . . H19 H 0.7238 0.3708 0.6912 0.047 Uiso 1 1 calc R U . . . C20 C 0.6019(2) 0.3215(2) 0.60114(12) 0.0250(7) Uani 1 1 d . . . . . C21 C 0.5807(3) 0.2200(3) 0.60437(14) 0.0320(8) Uani 1 1 d . . . . . H21 H 0.6205 0.1720 0.5887 0.038 Uiso 1 1 calc R U . . . C22 C 0.5019(3) 0.1888(3) 0.63039(15) 0.0400(9) Uani 1 1 d . . . . . H22 H 0.4877 0.1194 0.6322 0.048 Uiso 1 1 calc R U . . . C23 C 0.4442(3) 0.2571(3) 0.65360(15) 0.0388(9) Uani 1 1 d . . . . . H23 H 0.3896 0.2350 0.6708 0.047 Uiso 1 1 calc R U . . . C24 C 0.4653(2) 0.3577(3) 0.65196(14) 0.0339(8) Uani 1 1 d . . . . . H24 H 0.4267 0.4049 0.6692 0.041 Uiso 1 1 calc R U . . . C25 C 0.5439(2) 0.3902(3) 0.62489(14) 0.0292(7) Uani 1 1 d . . . . . H25 H 0.5574 0.4597 0.6228 0.035 Uiso 1 1 calc R U . . . C26 C 0.6874(3) 0.4982(3) 0.80365(16) 0.0589(12) Uani 1 1 d D . . . . C27 C 0.7565(3) 0.5092(4) 0.84984(19) 0.0788(16) Uani 1 1 d D . . . . H27 H 0.7531 0.4700 0.8832 0.095 Uiso 1 1 calc R U . . . C28 C 0.8306(3) 0.5775(4) 0.8472(2) 0.095(2) Uani 1 1 d D . . . . H28 H 0.8777 0.5841 0.8789 0.114 Uiso 1 1 calc R U . . . C29 C 0.8372(4) 0.6365(4) 0.7991(2) 0.091(2) Uani 1 1 d D . . . . H29 H 0.8869 0.6847 0.7985 0.109 Uiso 1 1 calc R U . . . C30 C 0.7700(3) 0.6239(3) 0.7520(2) 0.0719(14) Uani 1 1 d D . . . . H30 H 0.7753 0.6600 0.7178 0.086 Uiso 1 1 calc R U . . . C31 C 0.6949(3) 0.5576(3) 0.75610(19) 0.0597(12) Uani 1 1 d D . . . . H31 H 0.6464 0.5527 0.7249 0.072 Uiso 1 1 calc R U . . . C32 C 0.6075(5) 0.4240(5) 0.8027(3) 0.103(2) Uani 1 1 d . . . . . H32A H 0.5731 0.4336 0.8363 0.154 Uiso 1 1 calc R U . . . H32B H 0.6338 0.3561 0.8029 0.154 Uiso 1 1 calc R U . . . H32C H 0.5633 0.4338 0.7681 0.154 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 Ni1 0.0239(3) 0.0187(3) 0.0352(3) 0.000 0.0023(2) 0.000 Fe1 0.0198(3) 0.0193(3) 0.0258(3) 0.000 0.0023(2) 0.000 P1 0.0213(4) 0.0231(4) 0.0257(4) 0.0032(3) 0.0002(3) -0.0010(3) C1 0.047(6) 0.024(2) 0.026(3) -0.001(4) 0.009(5) 0.002(3) C2 0.051(6) 0.030(4) 0.030(5) 0.003(3) 0.011(5) 0.008(3) C3 0.084(6) 0.031(4) 0.050(5) 0.006(3) 0.023(5) 0.014(4) C4 0.098(6) 0.022(4) 0.037(5) -0.002(4) 0.031(5) -0.001(3) C5 0.096(6) 0.024(4) 0.048(6) -0.001(4) 0.023(5) 0.000(4) C6 0.055(6) 0.023(4) 0.037(4) -0.001(3) 0.007(4) -0.007(3) C7 0.048(5) 0.041(5) 0.048(5) 0.007(4) -0.005(4) 0.011(4) C8 0.054(6) 0.026(5) 0.058(6) -0.001(4) 0.001(5) -0.017(4) C9 0.0227(15) 0.0223(16) 0.0239(15) -0.0018(12) 0.0066(12) -0.0032(13) C10 0.0259(15) 0.0300(17) 0.0259(16) -0.0032(14) 0.0047(13) -0.0044(14) C11 0.0360(18) 0.0214(17) 0.0320(18) -0.0063(13) 0.0127(15) 0.0003(14) C12 0.0240(15) 0.0233(16) 0.0364(18) 0.0038(14) 0.0079(14) 0.0051(14) C13 0.0187(14) 0.0266(16) 0.0264(16) 0.0003(13) 0.0045(12) -0.0013(13) C14 0.0260(16) 0.0260(17) 0.0298(17) 0.0031(14) -0.0048(13) 0.0006(14) C15 0.0317(17) 0.0320(18) 0.0325(18) 0.0079(15) 0.0014(14) -0.0022(15) C16 0.0248(16) 0.037(2) 0.044(2) 0.0078(17) -0.0050(15) 0.0005(15) C17 0.0331(19) 0.053(2) 0.044(2) 0.0040(19) -0.0142(17) 0.0042(18) C18 0.043(2) 0.069(3) 0.0301(19) -0.0040(19) -0.0096(17) 0.010(2) C19 0.0317(18) 0.051(2) 0.0355(19) -0.0013(18) 0.0001(15) 0.0073(17) C20 0.0254(15) 0.0305(17) 0.0183(15) 0.0037(13) -0.0015(12) -0.0009(14) C21 0.042(2) 0.0295(18) 0.0257(17) 0.0016(14) 0.0077(15) -0.0013(16) C22 0.049(2) 0.037(2) 0.035(2) 0.0072(17) 0.0105(17) -0.0117(18) C23 0.0326(19) 0.055(2) 0.0298(18) 0.0116(17) 0.0066(15) -0.0058(18) C24 0.0271(17) 0.047(2) 0.0279(17) 0.0046(16) 0.0048(14) 0.0071(16) C25 0.0260(16) 0.0328(18) 0.0284(17) 0.0023(14) 0.0008(14) 0.0007(14) C26 0.059(3) 0.061(3) 0.060(3) -0.004(2) 0.018(2) 0.012(2) C27 0.090(4) 0.095(4) 0.052(3) 0.000(3) 0.011(3) 0.028(4) C28 0.050(3) 0.165(7) 0.067(4) -0.052(4) -0.007(3) 0.015(4) C29 0.079(4) 0.091(5) 0.107(5) -0.042(4) 0.036(4) -0.027(3) C30 0.086(4) 0.056(3) 0.076(4) -0.013(3) 0.021(3) -0.001(3) C31 0.043(2) 0.061(3) 0.075(3) 0.010(2) 0.000(2) 0.008(2) C32 0.105(5) 0.086(5) 0.126(6) -0.011(4) 0.051(4) -0.028(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 C1 Ni1 P1 131.0(5) . . C1 Ni1 P1 124.7(5) . 2_656 P1 Ni1 P1 103.69(5) . 2_656 C13 Fe1 C13 142.20(18) . 2_656 C13 Fe1 C9 41.80(12) . . C13 Fe1 C9 111.52(13) 2_656 . C13 Fe1 C9 111.52(13) . 2_656 C13 Fe1 C9 41.80(12) 2_656 2_656 C9 Fe1 C9 108.47(17) . 2_656 C13 Fe1 C10 109.84(13) . 2_656 C13 Fe1 C10 68.87(12) 2_656 2_656 C9 Fe1 C10 135.87(13) . 2_656 C9 Fe1 C10 40.91(12) 2_656 2_656 C13 Fe1 C10 68.87(12) . . C13 Fe1 C10 109.84(13) 2_656 . C9 Fe1 C10 40.91(12) . . C9 Fe1 C10 135.87(13) 2_656 . C10 Fe1 C10 176.27(18) 2_656 . C13 Fe1 C12 40.71(12) . . C13 Fe1 C12 176.10(13) 2_656 . C9 Fe1 C12 69.18(12) . . C9 Fe1 C12 141.99(13) 2_656 . C10 Fe1 C12 113.50(13) 2_656 . C10 Fe1 C12 68.00(13) . . C13 Fe1 C12 176.10(13) . 2_656 C13 Fe1 C12 40.71(12) 2_656 2_656 C9 Fe1 C12 141.99(13) . 2_656 C9 Fe1 C12 69.18(12) 2_656 2_656 C10 Fe1 C12 67.99(13) 2_656 2_656 C10 Fe1 C12 113.50(13) . 2_656 C12 Fe1 C12 136.57(18) . 2_656 C13 Fe1 C11 135.91(13) . 2_656 C13 Fe1 C11 68.52(13) 2_656 2_656 C9 Fe1 C11 176.02(13) . 2_656 C9 Fe1 C11 68.75(12) 2_656 2_656 C10 Fe1 C11 40.19(13) 2_656 2_656 C10 Fe1 C11 143.05(13) . 2_656 C12 Fe1 C11 111.07(13) . 2_656 C12 Fe1 C11 40.40(13) 2_656 2_656 C13 Fe1 C11 68.52(13) . . C13 Fe1 C11 135.91(13) 2_656 . C9 Fe1 C11 68.76(12) . . C9 Fe1 C11 176.02(13) 2_656 . C10 Fe1 C11 143.05(13) 2_656 . C10 Fe1 C11 40.20(13) . . C12 Fe1 C11 40.40(13) . . C12 Fe1 C11 111.07(13) 2_656 . C11 Fe1 C11 114.17(18) 2_656 . C9 P1 C20 101.46(14) . . C9 P1 C14 103.09(14) . . C20 P1 C14 102.93(14) . . C9 P1 Ni1 123.41(10) . . C20 P1 Ni1 116.58(11) . . C14 P1 Ni1 106.92(11) . . C6 C1 C2 117.5(9) . . C6 C1 Ni1 120.6(7) . . C2 C1 Ni1 121.7(7) . . C3 C2 C1 120.3(9) . . C3 C2 C7 119.8(8) . . C1 C2 C7 119.9(7) . . C2 C3 C4 119.5(9) . . C2 C3 H3 120.2 . . C4 C3 H3 120.2 . . C5 C4 C3 122.5(8) . . C5 C4 H4 118.7 . . C3 C4 H4 118.7 . . C4 C5 C6 116.8(9) . . C4 C5 H5 121.6 . . C6 C5 H5 121.6 . . C5 C6 C1 123.3(9) . . C5 C6 C8 116.6(8) . . C1 C6 C8 120.2(8) . . C2 C7 H7A 109.5 . . C2 C7 H7B 109.5 . . H7A C7 H7B 109.5 . . C2 C7 H7C 109.5 . . H7A C7 H7C 109.5 . . H7B C7 H7C 109.5 . . C6 C8 H8A 109.5 . . C6 C8 H8B 109.5 . . H8A C8 H8B 109.5 . . C6 C8 H8C 109.5 . . H8A C8 H8C 109.5 . . H8B C8 H8C 109.5 . . C10 C9 C13 106.5(3) . . C10 C9 P1 128.8(2) . . C13 C9 P1 124.7(2) . . C10 C9 Fe1 70.06(17) . . C13 C9 Fe1 68.71(17) . . P1 C9 Fe1 125.22(16) . . C11 C10 C9 109.2(3) . . C11 C10 Fe1 70.54(18) . . C9 C10 Fe1 69.03(17) . . C11 C10 H10 125.4 . . C9 C10 H10 125.4 . . Fe1 C10 H10 126.6 . . C10 C11 C12 107.9(3) . . C10 C11 Fe1 69.27(18) . . C12 C11 Fe1 69.22(17) . . C10 C11 H11 126.1 . . C12 C11 H11 126.1 . . Fe1 C11 H11 127.0 . . C13 C12 C11 108.4(3) . . C13 C12 Fe1 68.67(17) . . C11 C12 Fe1 70.38(17) . . C13 C12 H12 125.8 . . C11 C12 H12 125.8 . . Fe1 C12 H12 126.7 . . C12 C13 C9 108.1(3) . . C12 C13 Fe1 70.62(18) . . C9 C13 Fe1 69.50(16) . . C12 C13 H13 126.0 . . C9 C13 H13 126.0 . . Fe1 C13 H13 125.5 . . C19 C14 C15 118.5(3) . . C19 C14 P1 123.1(3) . . C15 C14 P1 118.4(2) . . C16 C15 C14 120.5(3) . . C16 C15 H15 119.7 . . C14 C15 H15 119.7 . . C17 C16 C15 120.3(3) . . C17 C16 H16 119.9 . . C15 C16 H16 119.9 . . C16 C17 C18 120.1(3) . . C16 C17 H17 120.0 . . C18 C17 H17 120.0 . . C17 C18 C19 119.8(4) . . C17 C18 H18 120.1 . . C19 C18 H18 120.1 . . C14 C19 C18 120.8(3) . . C14 C19 H19 119.6 . . C18 C19 H19 119.6 . . C25 C20 C21 119.0(3) . . C25 C20 P1 122.3(2) . . C21 C20 P1 118.7(2) . . C22 C21 C20 120.2(3) . . C22 C21 H21 119.9 . . C20 C21 H21 119.9 . . C23 C22 C21 120.6(3) . . C23 C22 H22 119.7 . . C21 C22 H22 119.7 . . C22 C23 C24 120.0(3) . . C22 C23 H23 120.0 . . C24 C23 H23 120.0 . . C23 C24 C25 119.9(3) . . C23 C24 H24 120.1 . . C25 C24 H24 120.1 . . C20 C25 C24 120.3(3) . . C20 C25 H25 119.9 . . C24 C25 H25 119.9 . . C31 C26 C27 117.9(4) . . C31 C26 C32 119.2(4) . . C27 C26 C32 122.9(5) . . C26 C27 C28 119.9(5) . . C26 C27 H27 120.0 . . C28 C27 H27 120.0 . . C27 C28 C29 121.6(5) . . C27 C28 H28 119.2 . . C29 C28 H28 119.2 . . C30 C29 C28 118.9(5) . . C30 C29 H29 120.5 . . C28 C29 H29 120.5 . . C31 C30 C29 118.7(5) . . C31 C30 H30 120.7 . . C29 C30 H30 120.7 . . C26 C31 C30 122.9(4) . . C26 C31 H31 118.5 . . C30 C31 H31 118.5 . . C26 C32 H32A 109.5 . . C26 C32 H32B 109.5 . . H32A C32 H32B 109.5 . . C26 C32 H32C 109.5 . . H32A C32 H32C 109.5 . . H32B C32 H32C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ni1 C1 1.954(6) . Ni1 P1 2.1900(9) . Ni1 P1 2.1900(9) 2_656 Fe1 C13 2.028(3) . Fe1 C13 2.028(3) 2_656 Fe1 C9 2.038(3) . Fe1 C9 2.038(3) 2_656 Fe1 C10 2.052(3) 2_656 Fe1 C10 2.052(3) . Fe1 C12 2.053(3) . Fe1 C12 2.053(3) 2_656 Fe1 C11 2.069(3) 2_656 Fe1 C11 2.069(3) . P1 C9 1.811(3) . P1 C20 1.833(3) . P1 C14 1.835(3) . C1 C6 1.413(10) . C1 C2 1.423(10) . C2 C3 1.395(10) . C2 C7 1.518(12) . C3 C4 1.413(11) . C3 H3 0.9500 . C4 C5 1.382(10) . C4 H4 0.9500 . C5 C6 1.409(10) . C5 H5 0.9500 . C6 C8 1.492(12) . C7 H7A 0.9800 . C7 H7B 0.9800 . C7 H7C 0.9800 . C8 H8A 0.9800 . C8 H8B 0.9800 . C8 H8C 0.9800 . C9 C10 1.429(4) . C9 C13 1.450(4) . C10 C11 1.416(5) . C10 H10 0.9500 . C11 C12 1.423(5) . C11 H11 0.9500 . C12 C13 1.420(4) . C12 H12 0.9500 . C13 H13 0.9500 . C14 C19 1.390(5) . C14 C15 1.392(5) . C15 C16 1.389(5) . C15 H15 0.9500 . C16 C17 1.375(5) . C16 H16 0.9500 . C17 C18 1.380(5) . C17 H17 0.9500 . C18 C19 1.390(5) . C18 H18 0.9500 . C19 H19 0.9500 . C20 C25 1.383(4) . C20 C21 1.392(5) . C21 C22 1.384(5) . C21 H21 0.9500 . C22 C23 1.371(5) . C22 H22 0.9500 . C23 C24 1.377(5) . C23 H23 0.9500 . C24 C25 1.399(5) . C24 H24 0.9500 . C25 H25 0.9500 . C26 C31 1.386(2) . C26 C27 1.388(2) . C26 C32 1.494(7) . C27 C28 1.390(2) . C27 H27 0.9500 . C28 C29 1.391(2) . C28 H28 0.9500 . C29 C30 1.390(2) . C29 H29 0.9500 . C30 C31 1.388(2) . C30 H30 0.9500 . C31 H31 0.9500 . C32 H32A 0.9800 . C32 H32B 0.9800 . C32 H32C 0.9800 . 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 C6 C1 C2 C3 1.5(19) Ni1 C1 C2 C3 176.6(9) C6 C1 C2 C7 -178.8(10) Ni1 C1 C2 C7 -3.7(17) C1 C2 C3 C4 -2.9(15) C7 C2 C3 C4 177.4(9) C2 C3 C4 C5 2.6(15) C3 C4 C5 C6 -0.9(14) C4 C5 C6 C1 -0.6(16) C4 C5 C6 C8 178.6(8) C2 C1 C6 C5 0(2) Ni1 C1 C6 C5 -174.9(11) C2 C1 C6 C8 -179.0(11) Ni1 C1 C6 C8 5.9(16) C20 P1 C9 C10 102.8(3) C14 P1 C9 C10 -3.5(3) Ni1 P1 C9 C10 -124.3(3) C20 P1 C9 C13 -78.3(3) C14 P1 C9 C13 175.3(3) Ni1 P1 C9 C13 54.6(3) C20 P1 C9 Fe1 -165.34(18) C14 P1 C9 Fe1 88.3(2) Ni1 P1 C9 Fe1 -32.4(2) C13 C9 C10 C11 -0.1(3) P1 C9 C10 C11 179.0(2) Fe1 C9 C10 C11 59.3(2) C13 C9 C10 Fe1 -59.3(2) P1 C9 C10 Fe1 119.7(3) C9 C10 C11 C12 0.3(3) Fe1 C10 C11 C12 58.6(2) C9 C10 C11 Fe1 -58.3(2) C10 C11 C12 C13 -0.4(3) Fe1 C11 C12 C13 58.3(2) C10 C11 C12 Fe1 -58.6(2) C11 C12 C13 C9 0.3(3) Fe1 C12 C13 C9 59.7(2) C11 C12 C13 Fe1 -59.3(2) C10 C9 C13 C12 -0.1(3) P1 C9 C13 C12 -179.2(2) Fe1 C9 C13 C12 -60.4(2) C10 C9 C13 Fe1 60.2(2) P1 C9 C13 Fe1 -118.9(2) C9 P1 C14 C19 85.4(3) C20 P1 C14 C19 -19.9(3) Ni1 P1 C14 C19 -143.2(3) C9 P1 C14 C15 -96.7(3) C20 P1 C14 C15 158.0(3) Ni1 P1 C14 C15 34.7(3) C19 C14 C15 C16 -0.5(5) P1 C14 C15 C16 -178.5(3) C14 C15 C16 C17 0.4(5) C15 C16 C17 C18 0.1(6) C16 C17 C18 C19 -0.4(6) C15 C14 C19 C18 0.2(6) P1 C14 C19 C18 178.1(3) C17 C18 C19 C14 0.2(6) C9 P1 C20 C25 -16.6(3) C14 P1 C20 C25 89.9(3) Ni1 P1 C20 C25 -153.5(2) C9 P1 C20 C21 163.5(2) C14 P1 C20 C21 -90.0(3) Ni1 P1 C20 C21 26.7(3) C25 C20 C21 C22 0.8(5) P1 C20 C21 C22 -179.4(3) C20 C21 C22 C23 -0.4(5) C21 C22 C23 C24 -1.1(5) C22 C23 C24 C25 2.2(5) C21 C20 C25 C24 0.3(5) P1 C20 C25 C24 -179.5(2) C23 C24 C25 C20 -1.8(5) C31 C26 C27 C28 -0.5(7) C32 C26 C27 C28 178.0(5) C26 C27 C28 C29 0.5(8) C27 C28 C29 C30 -2.4(8) C28 C29 C30 C31 4.3(8) C27 C26 C31 C30 2.6(7) C32 C26 C31 C30 -175.9(5) C29 C30 C31 C26 -4.5(8)