#------------------------------------------------------------------------------ #$Date: 2019-11-17 11:39:28 +0200 (Sun, 17 Nov 2019) $ #$Revision: 229647 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/80/7048012.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_7048012 loop_ _publ_author_name 'LaPierre, Etienne A.' 'Piers, Warren E.' 'Gendy, Chris' _publ_section_title ; Redox-state dependent activation of silanes and ammonia with reverse polarity (PCcarbeneP)Ni complexes: electrophilic vs. nucleophilic carbenes. ; _journal_issue 46 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 16789 _journal_page_last 16797 _journal_paper_doi 10.1039/c8dt04409k _journal_volume 47 _journal_year 2018 _chemical_formula_moiety 'C28 H45 N2 Ni P2, F6 Sb' _chemical_formula_sum 'C28 H45 F6 N2 Ni P2 Sb' _chemical_formula_weight 766.06 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2018-08-22 deposited with the CCDC. 2018-11-07 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.9790(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.9965(3) _cell_length_b 16.1517(4) _cell_length_c 18.8351(4) _cell_measurement_reflns_used 9968 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.51 _cell_measurement_theta_min 2.55 _cell_volume 3272.49(14) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'LinXTL v. 5.9.1 (Spasyuk, 2009)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_unetI/netI 0.0340 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 33471 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 25.000 _diffrn_reflns_theta_min 3.154 _exptl_absorpt_coefficient_mu 1.553 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6064 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_crystal_colour Purple _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Block _exptl_crystal_F_000 1560 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.25 _refine_diff_density_max 1.322 _refine_diff_density_min -0.962 _refine_diff_density_rms 0.081 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 372 _refine_ls_number_reflns 5713 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.016 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0315 _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^)+(0.0377P)^2^+4.4682P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0727 _refine_ls_wR_factor_ref 0.0812 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4715 _reflns_number_total 5713 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8dt04409k2.cif _cod_data_source_block CGEL180219020_0m _cod_depositor_comments 'Adding full bibliography for 7048006--7048012.cif.' _cod_database_code 7048012 _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_res_file ; CGEL180219020_0m_a.res created by SHELXL-2014/7 TITL CGEL180219020_0m_a.res in P2(1)/n CELL 0.71073 10.9965 16.1517 18.8351 90.000 101.979 90.000 ZERR 4.000 0.0003 0.0004 0.0004 0.000 0.001 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H N F P NI SB UNIT 112 180 8 24 8 4 4 OMIT 0 9 17 OMIT -1 15 10 OMIT 2 8 8 OMIT 2 5 4 OMIT -1 14 3 OMIT -5 4 3 OMIT 1 3 10 OMIT -1 2 13 OMIT -7 8 5 OMIT -2 14 3 OMIT -1 16 9 OMIT 0 1 10 OMIT -2 5 1 OMIT 7 0 1 OMIT 1 6 6 OMIT 4 3 5 OMIT -7 7 15 OMIT -4 2 2 OMIT 0 2 6 OMIT -1 5 8 OMIT -10 9 4 OMIT 3 0 3 OMIT -1 6 6 OMIT 1 4 7 OMIT 0 0 20 OMIT -1 1 11 OMIT 7 0 15 OMIT -3 2 9 OMIT 3 17 7 OMIT -3 14 7 OMIT -1 14 1 OMIT 0 2 0 OMIT 1 0 1 OMIT -1 0 1 OMIT 0 0 2 OMIT 0 1 2 OMIT 0 2 1 OMIT -1 1 1 OMIT 2 0 0 OMIT 1 1 0 OMIT 1 1 1 OMIT 0 1 1 OMIT -4 50 ACTA 50 L.S. 10 BOND $H FMAP 2 PLAN 50 LIST 6 WGHT 0.037700 4.468200 FVAR 0.26287 C1 1 0.662140 0.620046 0.383443 11.00000 0.02200 0.01711 = 0.02116 0.00321 0.00239 -0.00095 C2 1 0.670945 0.627086 0.463811 11.00000 0.01622 0.02285 = 0.02762 0.00244 0.00361 -0.00074 C3 1 0.712251 0.558804 0.508178 11.00000 0.02012 0.02332 = 0.02568 0.00190 0.00181 -0.00276 C4 1 0.742758 0.477772 0.473781 11.00000 0.02487 0.02068 = 0.02802 0.00456 0.00047 -0.00283 C5 1 0.803846 0.497413 0.409884 11.00000 0.02170 0.01951 = 0.02753 -0.00162 -0.00005 -0.00476 C6 1 0.762437 0.566249 0.365818 11.00000 0.01596 0.02170 = 0.02299 -0.00055 0.00060 -0.00131 C7 1 0.642536 0.701846 0.492218 11.00000 0.02136 0.02362 = 0.02332 0.00257 -0.00038 -0.00174 C8 1 0.653736 0.709565 0.567336 11.00000 0.03306 0.02658 = 0.02691 -0.00600 0.00056 -0.00113 AFIX 43 H8 2 0.635266 0.759563 0.587198 11.00000 -1.20000 AFIX 0 C9 1 0.692209 0.642772 0.611554 11.00000 0.03549 0.03629 = 0.01897 0.00196 0.00019 -0.00034 AFIX 43 H9 2 0.698512 0.647504 0.661395 11.00000 -1.20000 AFIX 0 C10 1 0.721627 0.568556 0.582478 11.00000 0.02563 0.02990 = 0.02652 0.00715 -0.00094 0.00110 AFIX 43 H10 2 0.748254 0.524227 0.613302 11.00000 -1.20000 AFIX 0 C11 1 0.815595 0.586549 0.307022 11.00000 0.02211 0.02407 = 0.02612 -0.00207 0.00335 -0.00134 C12 1 0.908248 0.536892 0.290061 11.00000 0.02555 0.02895 = 0.03329 -0.00538 0.00801 -0.00322 AFIX 43 H12 2 0.942412 0.549091 0.250066 11.00000 -1.20000 AFIX 0 C13 1 0.949396 0.469216 0.332984 11.00000 0.02418 0.02303 = 0.04310 -0.00676 0.00635 0.00246 AFIX 43 H13 2 1.012137 0.436139 0.321892 11.00000 -1.20000 AFIX 0 C14 1 0.898697 0.449704 0.392423 11.00000 0.02693 0.01595 = 0.03816 -0.00081 -0.00096 -0.00078 AFIX 43 H14 2 0.928519 0.404138 0.420959 11.00000 -1.20000 AFIX 0 C15 1 0.619018 0.430661 0.445423 11.00000 0.02643 0.02800 = 0.03427 0.00303 0.00568 -0.00457 AFIX 137 H15A 2 0.567559 0.462334 0.407622 11.00000 -1.50000 H15B 2 0.576408 0.422771 0.484529 11.00000 -1.50000 H15C 2 0.636634 0.377769 0.426596 11.00000 -1.50000 AFIX 0 C16 1 0.825793 0.420681 0.528838 11.00000 0.03398 0.02426 = 0.03303 0.00498 -0.00005 0.00111 AFIX 137 H16A 2 0.837210 0.368976 0.505945 11.00000 -1.50000 H16B 2 0.786887 0.410856 0.569213 11.00000 -1.50000 H16C 2 0.905103 0.446583 0.545715 11.00000 -1.50000 AFIX 0 C17 1 0.705700 0.870365 0.463698 11.00000 0.04206 0.03099 = 0.03111 -0.00804 0.00925 -0.01090 AFIX 13 H17 2 0.687451 0.883465 0.511210 11.00000 -1.20000 AFIX 0 C18 1 0.842046 0.846150 0.475533 11.00000 0.03837 0.05279 = 0.05134 -0.00659 0.00056 -0.01647 AFIX 137 H18A 2 0.863671 0.835948 0.429483 11.00000 -1.50000 H18B 2 0.856062 0.796918 0.504643 11.00000 -1.50000 H18C 2 0.892490 0.890294 0.499944 11.00000 -1.50000 AFIX 0 C19 1 0.676046 0.946365 0.416247 11.00000 0.06400 0.02374 = 0.05730 -0.00110 0.01895 -0.00927 AFIX 137 H19A 2 0.730322 0.990822 0.436374 11.00000 -1.50000 H19B 2 0.591291 0.962440 0.414021 11.00000 -1.50000 H19C 2 0.687719 0.934038 0.368248 11.00000 -1.50000 AFIX 0 C20 1 0.446971 0.821727 0.429103 11.00000 0.03174 0.02566 = 0.02854 0.00383 0.00615 0.00837 AFIX 13 H20 2 0.427300 0.865832 0.392801 11.00000 -1.20000 AFIX 0 C21 1 0.431349 0.858978 0.501137 11.00000 0.04723 0.05304 = 0.03577 -0.00549 0.01324 0.01764 AFIX 137 H21A 2 0.348396 0.880082 0.496168 11.00000 -1.50000 H21B 2 0.489911 0.903230 0.514494 11.00000 -1.50000 H21C 2 0.445913 0.817055 0.538061 11.00000 -1.50000 AFIX 0 C22 1 0.351741 0.753388 0.405510 11.00000 0.02863 0.04104 = 0.05551 0.00014 0.01030 0.00379 AFIX 137 H22A 2 0.367147 0.708741 0.439850 11.00000 -1.50000 H22B 2 0.358368 0.733436 0.358451 11.00000 -1.50000 H22C 2 0.269677 0.774907 0.403355 11.00000 -1.50000 AFIX 0 C23 1 0.896669 0.747137 0.261462 11.00000 0.02858 0.03255 = 0.04759 0.00265 0.00799 -0.00504 AFIX 13 H23 2 0.930114 0.731366 0.219045 11.00000 -1.20000 AFIX 0 C24 1 0.997355 0.735022 0.327101 11.00000 0.03944 0.04326 = 0.08764 -0.00576 -0.00816 -0.00674 AFIX 137 H24A 2 1.061156 0.775712 0.327581 11.00000 -1.50000 H24B 2 1.032123 0.680627 0.326054 11.00000 -1.50000 H24C 2 0.963593 0.740930 0.369918 11.00000 -1.50000 AFIX 0 C25 1 0.857532 0.838540 0.252325 11.00000 0.03789 0.03449 = 0.05983 0.01034 0.00612 -0.00602 AFIX 137 H25A 2 0.828873 0.856716 0.294536 11.00000 -1.50000 H25B 2 0.791849 0.844466 0.210237 11.00000 -1.50000 H25C 2 0.927435 0.871514 0.246497 11.00000 -1.50000 AFIX 0 C26 1 0.714516 0.645613 0.165331 11.00000 0.03260 0.03384 = 0.02638 -0.00364 0.01002 0.00215 AFIX 13 H26 2 0.787701 0.618641 0.153578 11.00000 -1.20000 AFIX 0 C27 1 0.676198 0.715959 0.111542 11.00000 0.05987 0.04805 = 0.02859 0.00622 0.00852 0.00388 AFIX 137 H27A 2 0.653674 0.693819 0.063295 11.00000 -1.50000 H27B 2 0.744397 0.753755 0.114303 11.00000 -1.50000 H27C 2 0.606362 0.744662 0.123109 11.00000 -1.50000 AFIX 0 C28 1 0.611634 0.582030 0.157375 11.00000 0.03386 0.04355 = 0.03352 -0.01024 0.00472 -0.00277 AFIX 137 H28A 2 0.539239 0.606831 0.169482 11.00000 -1.50000 H28B 2 0.638490 0.536360 0.189418 11.00000 -1.50000 H28C 2 0.591861 0.562534 0.108173 11.00000 -1.50000 AFIX 0 F1 4 0.153214 0.447775 0.225096 11.00000 0.05015 0.04815 = 0.03681 0.00741 0.00546 -0.02532 F2 4 0.388843 0.490001 0.233842 11.00000 0.03518 0.03340 = 0.05638 0.00090 0.00193 0.00263 F3 4 0.316713 0.637177 0.176711 11.00000 0.03826 0.03584 = 0.04801 0.01109 0.00967 -0.00799 F4 4 0.244198 0.584580 0.293305 11.00000 0.05770 0.04446 = 0.03025 0.00165 0.00914 0.00091 F5 4 0.228479 0.499299 0.107819 11.00000 0.09141 0.06501 = 0.02335 -0.00459 0.01156 -0.03063 F6 4 0.082607 0.594876 0.168133 11.00000 0.02945 0.08506 = 0.06477 0.03577 -0.00248 -0.00080 N1 3 0.539780 0.603324 0.341044 11.00000 0.02141 0.02445 = 0.02366 -0.00255 0.00309 -0.00213 AFIX 23 H1A 2 0.477071 0.602855 0.364267 11.00000 -1.20000 H1B 2 0.533568 0.565832 0.305845 11.00000 -1.20000 AFIX 0 N2 3 0.488932 0.779597 0.250515 11.00000 0.03798 0.02816 = 0.02980 0.00209 0.00531 0.00521 AFIX 137 H2A 2 0.434749 0.744447 0.224803 11.00000 -1.50000 H2B 2 0.528051 0.807073 0.220926 11.00000 -1.50000 H2C 2 0.448781 0.815282 0.273408 11.00000 -1.50000 AFIX 0 NI1 6 0.613833 0.716239 0.323825 11.00000 0.02368 0.01916 = 0.02034 0.00108 0.00299 0.00149 P1 5 0.603997 0.783530 0.424788 11.00000 0.02590 0.01807 = 0.02281 -0.00064 0.00322 0.00004 P2 5 0.756768 0.682127 0.261327 11.00000 0.02288 0.02359 = 0.02387 0.00119 0.00631 0.00021 SB1 7 0.235845 0.541886 0.200075 11.00000 0.02673 0.03630 = 0.02125 0.00591 -0.00023 -0.00937 HKLF 4 REM CGEL180219020_0m_a.res in P2(1)/n REM R1 = 0.0315 for 4715 Fo > 4sig(Fo) and 0.0434 for all 5713 data REM 372 parameters refined using 0 restraints END WGHT 0.0341 4.5411 REM Highest difference peak 1.322, deepest hole -0.962, 1-sigma level 0.081 Q1 1 0.2660 0.5005 0.1838 11.00000 0.05 1.32 Q2 1 0.9982 0.7397 0.2429 11.00000 0.05 0.64 Q3 1 0.6366 0.7361 0.3807 11.00000 0.05 0.51 Q4 1 0.2072 0.5371 0.2057 11.00000 0.05 0.48 Q5 1 0.7898 0.7447 0.2793 11.00000 0.05 0.43 Q6 1 0.6896 0.7010 0.2865 11.00000 0.05 0.41 Q7 1 0.8013 0.6333 0.2944 11.00000 0.05 0.38 Q8 1 0.1834 0.5708 0.2494 11.00000 0.05 0.37 Q9 1 0.2080 0.4143 0.2100 11.00000 0.05 0.36 Q10 1 0.5965 0.7458 0.4631 11.00000 0.05 0.35 Q11 1 0.7252 0.5172 0.4917 11.00000 0.05 0.34 Q12 1 0.5547 0.7421 0.2724 11.00000 0.05 0.32 Q13 1 0.5150 0.8035 0.4373 11.00000 0.05 0.31 Q14 1 0.7741 0.4939 0.4439 11.00000 0.05 0.31 Q15 1 0.0709 0.5381 0.1551 11.00000 0.05 0.31 Q16 1 0.6840 0.4588 0.4601 11.00000 0.05 0.30 Q17 1 0.6945 0.6785 0.1422 11.00000 0.05 0.30 Q18 1 0.7940 0.5414 0.3988 11.00000 0.05 0.30 Q19 1 0.3993 0.5343 0.2626 11.00000 0.05 0.30 Q20 1 0.6568 0.8354 0.4450 11.00000 0.05 0.30 Q21 1 0.7268 0.6631 0.2050 11.00000 0.05 0.29 Q22 1 0.6995 0.6936 0.3562 11.00000 0.05 0.28 Q23 1 0.8107 0.5876 0.3404 11.00000 0.05 0.28 Q24 1 0.5956 0.9550 0.3559 11.00000 0.05 0.27 Q25 1 0.5393 0.7232 0.0953 11.00000 0.05 0.27 Q26 1 0.7398 0.5658 0.5387 11.00000 0.05 0.27 Q27 1 0.7200 0.9406 0.3795 11.00000 0.05 0.27 Q28 1 0.6019 0.7769 0.3516 11.00000 0.05 0.27 Q29 1 0.7048 0.6784 0.5923 11.00000 0.05 0.27 Q30 1 0.8303 0.4701 0.3754 11.00000 0.05 0.27 Q31 1 0.8524 0.5582 0.2949 11.00000 0.05 0.27 Q32 1 0.8861 0.8728 0.1730 11.00000 0.05 0.26 Q33 1 0.8359 0.7646 0.1448 11.00000 0.05 0.26 Q34 1 0.5397 0.7191 0.3623 11.00000 0.05 0.25 Q35 1 0.5378 0.7193 0.1469 11.00000 0.05 0.25 Q36 1 0.7733 0.8512 0.4609 11.00000 0.05 0.24 Q37 1 0.5513 0.4750 0.4343 11.00000 0.05 0.24 Q38 1 0.7114 0.7244 0.3370 11.00000 0.05 0.24 Q39 1 0.5157 0.7602 0.2075 11.00000 0.05 0.23 Q40 1 0.8893 0.4948 0.2922 11.00000 0.05 0.23 Q41 1 0.9780 0.7226 0.1873 11.00000 0.05 0.23 Q42 1 0.6670 0.6245 0.1729 11.00000 0.05 0.23 Q43 1 0.6343 0.7458 0.1324 11.00000 0.05 0.23 Q44 1 0.9023 0.7646 0.3031 11.00000 0.05 0.23 Q45 1 0.3648 0.8872 0.4972 11.00000 0.05 0.23 Q46 1 0.7533 0.5625 0.3436 11.00000 0.05 0.22 Q47 1 0.5614 0.4573 0.4851 11.00000 0.05 0.22 Q48 1 0.6605 0.6577 0.7092 11.00000 0.05 0.22 Q49 1 0.1916 0.5272 0.1458 11.00000 0.05 0.22 Q50 1 0.6467 0.5838 0.5891 11.00000 0.05 0.22 ; _shelx_res_checksum 54326 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -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 C1 C 0.6621(3) 0.62005(19) 0.38344(16) 0.0204(7) Uani 1 1 d . . C2 C 0.6709(3) 0.6271(2) 0.46381(17) 0.0224(7) Uani 1 1 d . . C3 C 0.7123(3) 0.5588(2) 0.50818(17) 0.0235(7) Uani 1 1 d . . C4 C 0.7428(3) 0.4778(2) 0.47378(18) 0.0252(7) Uani 1 1 d . . C5 C 0.8038(3) 0.4974(2) 0.40988(17) 0.0237(7) Uani 1 1 d . . C6 C 0.7624(3) 0.5662(2) 0.36582(16) 0.0207(7) Uani 1 1 d . . C7 C 0.6425(3) 0.7018(2) 0.49222(17) 0.0235(7) Uani 1 1 d . . C8 C 0.6537(3) 0.7096(2) 0.56734(18) 0.0297(8) Uani 1 1 d . . H8 H 0.6353 0.7596 0.5872 0.036 Uiso 1 1 calc R U C9 C 0.6922(3) 0.6428(2) 0.61155(18) 0.0310(8) Uani 1 1 d . . H9 H 0.6985 0.6475 0.6614 0.037 Uiso 1 1 calc R U C10 C 0.7216(3) 0.5686(2) 0.58248(18) 0.0283(8) Uani 1 1 d . . H10 H 0.7483 0.5242 0.6133 0.034 Uiso 1 1 calc R U C11 C 0.8156(3) 0.5865(2) 0.30702(17) 0.0243(7) Uani 1 1 d . . C12 C 0.9082(3) 0.5369(2) 0.29006(19) 0.0290(8) Uani 1 1 d . . H12 H 0.9424 0.5491 0.2501 0.035 Uiso 1 1 calc R U C13 C 0.9494(3) 0.4692(2) 0.3330(2) 0.0302(8) Uani 1 1 d . . H13 H 1.0121 0.4361 0.3219 0.036 Uiso 1 1 calc R U C14 C 0.8987(3) 0.4497(2) 0.39242(19) 0.0281(8) Uani 1 1 d . . H14 H 0.9285 0.4041 0.4210 0.034 Uiso 1 1 calc R U C15 C 0.6190(3) 0.4307(2) 0.44542(19) 0.0297(8) Uani 1 1 d . . H15A H 0.5676 0.4623 0.4076 0.044 Uiso 1 1 calc R U H15B H 0.5764 0.4228 0.4845 0.044 Uiso 1 1 calc R U H15C H 0.6366 0.3778 0.4266 0.044 Uiso 1 1 calc R U C16 C 0.8258(4) 0.4207(2) 0.52884(19) 0.0314(8) Uani 1 1 d . . H16A H 0.8372 0.3690 0.5059 0.047 Uiso 1 1 calc R U H16B H 0.7869 0.4109 0.5692 0.047 Uiso 1 1 calc R U H16C H 0.9051 0.4466 0.5457 0.047 Uiso 1 1 calc R U C17 C 0.7057(4) 0.8704(2) 0.46370(19) 0.0345(9) Uani 1 1 d . . H17 H 0.6875 0.8835 0.5112 0.041 Uiso 1 1 calc R U C18 C 0.8420(4) 0.8461(3) 0.4755(2) 0.0488(11) Uani 1 1 d . . H18A H 0.8637 0.8359 0.4295 0.073 Uiso 1 1 calc R U H18B H 0.8561 0.7969 0.5046 0.073 Uiso 1 1 calc R U H18C H 0.8925 0.8903 0.4999 0.073 Uiso 1 1 calc R U C19 C 0.6760(5) 0.9464(2) 0.4162(2) 0.0474(11) Uani 1 1 d . . H19A H 0.7303 0.9908 0.4364 0.071 Uiso 1 1 calc R U H19B H 0.5913 0.9624 0.4140 0.071 Uiso 1 1 calc R U H19C H 0.6877 0.9340 0.3682 0.071 Uiso 1 1 calc R U C20 C 0.4470(3) 0.8217(2) 0.42910(18) 0.0287(8) Uani 1 1 d . . H20 H 0.4273 0.8658 0.3928 0.034 Uiso 1 1 calc R U C21 C 0.4313(4) 0.8590(3) 0.5011(2) 0.0447(11) Uani 1 1 d . . H21A H 0.3484 0.8801 0.4962 0.067 Uiso 1 1 calc R U H21B H 0.4899 0.9032 0.5145 0.067 Uiso 1 1 calc R U H21C H 0.4459 0.8171 0.5381 0.067 Uiso 1 1 calc R U C22 C 0.3517(4) 0.7534(3) 0.4055(2) 0.0415(10) Uani 1 1 d . . H22A H 0.3671 0.7087 0.4399 0.062 Uiso 1 1 calc R U H22B H 0.3584 0.7334 0.3585 0.062 Uiso 1 1 calc R U H22C H 0.2697 0.7749 0.4034 0.062 Uiso 1 1 calc R U C23 C 0.8967(3) 0.7471(2) 0.2615(2) 0.0362(9) Uani 1 1 d . . H23 H 0.9301 0.7314 0.2190 0.043 Uiso 1 1 calc R U C24 C 0.9974(4) 0.7350(3) 0.3271(3) 0.0599(13) Uani 1 1 d . . H24A H 1.0612 0.7757 0.3276 0.090 Uiso 1 1 calc R U H24B H 1.0321 0.6806 0.3261 0.090 Uiso 1 1 calc R U H24C H 0.9636 0.7409 0.3699 0.090 Uiso 1 1 calc R U C25 C 0.8575(4) 0.8385(2) 0.2523(2) 0.0447(10) Uani 1 1 d . . H25A H 0.8289 0.8567 0.2945 0.067 Uiso 1 1 calc R U H25B H 0.7918 0.8445 0.2102 0.067 Uiso 1 1 calc R U H25C H 0.9274 0.8715 0.2465 0.067 Uiso 1 1 calc R U C26 C 0.7145(4) 0.6456(2) 0.16533(18) 0.0304(8) Uani 1 1 d . . H26 H 0.7877 0.6186 0.1536 0.036 Uiso 1 1 calc R U C27 C 0.6762(4) 0.7160(3) 0.1115(2) 0.0456(11) Uani 1 1 d . . H27A H 0.6537 0.6938 0.0633 0.068 Uiso 1 1 calc R U H27B H 0.7444 0.7538 0.1143 0.068 Uiso 1 1 calc R U H27C H 0.6064 0.7447 0.1231 0.068 Uiso 1 1 calc R U C28 C 0.6116(4) 0.5820(3) 0.1574(2) 0.0373(9) Uani 1 1 d . . H28A H 0.5392 0.6068 0.1695 0.056 Uiso 1 1 calc R U H28B H 0.6385 0.5364 0.1894 0.056 Uiso 1 1 calc R U H28C H 0.5919 0.5625 0.1082 0.056 Uiso 1 1 calc R U F1 F 0.1532(2) 0.44777(14) 0.22510(11) 0.0456(6) Uani 1 1 d . . F2 F 0.3888(2) 0.49000(14) 0.23384(12) 0.0427(5) Uani 1 1 d . . F3 F 0.3167(2) 0.63718(13) 0.17671(12) 0.0406(5) Uani 1 1 d . . F4 F 0.2442(2) 0.58458(15) 0.29331(11) 0.0441(6) Uani 1 1 d . . F5 F 0.2285(3) 0.49930(17) 0.10782(11) 0.0600(8) Uani 1 1 d . . F6 F 0.0826(2) 0.59488(18) 0.16813(14) 0.0615(8) Uani 1 1 d . . N1 N 0.5398(3) 0.60332(17) 0.34104(14) 0.0234(6) Uani 1 1 d . . H1A H 0.4771 0.6029 0.3643 0.028 Uiso 1 1 calc R U H1B H 0.5336 0.5658 0.3058 0.028 Uiso 1 1 calc R U N2 N 0.4889(3) 0.77960(18) 0.25052(15) 0.0322(7) Uani 1 1 d . . H2A H 0.4347 0.7444 0.2248 0.048 Uiso 1 1 calc R U H2B H 0.5281 0.8071 0.2209 0.048 Uiso 1 1 calc R U H2C H 0.4488 0.8153 0.2734 0.048 Uiso 1 1 calc R U Ni1 Ni 0.61383(4) 0.71624(3) 0.32382(2) 0.02129(11) Uani 1 1 d . . P1 P 0.60400(8) 0.78353(5) 0.42479(4) 0.02252(19) Uani 1 1 d . . P2 P 0.75677(8) 0.68213(6) 0.26133(4) 0.0232(2) Uani 1 1 d . . Sb1 Sb 0.23584(2) 0.54189(2) 0.20007(2) 0.02885(9) Uani 1 1 d . . 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 C1 0.0220(17) 0.0171(16) 0.0212(15) 0.0032(13) 0.0024(13) -0.0009(14) C2 0.0162(17) 0.0228(17) 0.0276(17) 0.0024(14) 0.0036(14) -0.0007(14) C3 0.0201(17) 0.0233(18) 0.0257(17) 0.0019(14) 0.0018(14) -0.0028(14) C4 0.0249(18) 0.0207(18) 0.0280(17) 0.0046(14) 0.0005(15) -0.0028(15) C5 0.0217(18) 0.0195(17) 0.0275(17) -0.0016(13) -0.0001(14) -0.0048(14) C6 0.0160(16) 0.0217(17) 0.0230(16) -0.0006(13) 0.0006(13) -0.0013(14) C7 0.0214(18) 0.0236(18) 0.0233(17) 0.0026(14) -0.0004(14) -0.0017(14) C8 0.033(2) 0.0266(19) 0.0269(18) -0.0060(15) 0.0006(15) -0.0011(16) C9 0.035(2) 0.036(2) 0.0190(17) 0.0020(15) 0.0002(15) -0.0003(17) C10 0.0256(19) 0.0299(19) 0.0265(18) 0.0071(15) -0.0009(15) 0.0011(16) C11 0.0221(18) 0.0241(18) 0.0261(17) -0.0021(14) 0.0033(14) -0.0013(15) C12 0.0255(19) 0.0289(19) 0.0333(19) -0.0054(15) 0.0080(15) -0.0032(16) C13 0.0242(19) 0.0230(19) 0.043(2) -0.0068(16) 0.0064(16) 0.0025(15) C14 0.0269(19) 0.0159(17) 0.038(2) -0.0008(14) -0.0010(16) -0.0008(15) C15 0.026(2) 0.0280(19) 0.0343(19) 0.0030(15) 0.0057(16) -0.0046(16) C16 0.034(2) 0.0243(19) 0.0330(19) 0.0050(15) 0.0000(16) 0.0011(17) C17 0.042(2) 0.031(2) 0.0311(19) -0.0080(16) 0.0092(17) -0.0109(18) C18 0.038(2) 0.053(3) 0.051(3) -0.007(2) 0.001(2) -0.016(2) C19 0.064(3) 0.024(2) 0.057(3) -0.0011(18) 0.019(2) -0.009(2) C20 0.032(2) 0.0257(19) 0.0285(18) 0.0038(14) 0.0062(16) 0.0084(16) C21 0.047(3) 0.053(3) 0.036(2) -0.0055(19) 0.0132(19) 0.018(2) C22 0.029(2) 0.041(2) 0.056(2) 0.000(2) 0.0103(19) 0.0038(19) C23 0.029(2) 0.033(2) 0.048(2) 0.0026(17) 0.0080(18) -0.0050(17) C24 0.039(3) 0.043(3) 0.088(4) -0.006(2) -0.008(2) -0.007(2) C25 0.038(2) 0.034(2) 0.060(3) 0.010(2) 0.006(2) -0.0060(19) C26 0.033(2) 0.034(2) 0.0264(18) -0.0036(15) 0.0100(16) 0.0022(17) C27 0.060(3) 0.048(3) 0.029(2) 0.0062(18) 0.0085(19) 0.004(2) C28 0.034(2) 0.044(2) 0.034(2) -0.0102(17) 0.0047(17) -0.0028(19) F1 0.0501(15) 0.0482(14) 0.0368(12) 0.0074(10) 0.0055(11) -0.0253(12) F2 0.0352(13) 0.0334(12) 0.0564(14) 0.0009(10) 0.0019(11) 0.0026(10) F3 0.0383(13) 0.0358(12) 0.0480(13) 0.0111(10) 0.0097(10) -0.0080(10) F4 0.0577(16) 0.0445(14) 0.0303(11) 0.0017(10) 0.0091(11) 0.0009(12) F5 0.091(2) 0.0650(17) 0.0234(11) -0.0046(11) 0.0116(12) -0.0306(16) F6 0.0295(13) 0.085(2) 0.0648(16) 0.0358(15) -0.0025(12) -0.0008(13) N1 0.0214(15) 0.0244(15) 0.0237(14) -0.0025(11) 0.0031(12) -0.0021(12) N2 0.0380(19) 0.0282(16) 0.0298(16) 0.0021(13) 0.0053(14) 0.0052(14) Ni1 0.0237(2) 0.0192(2) 0.0203(2) 0.00108(16) 0.00299(17) 0.00149(18) P1 0.0259(5) 0.0181(4) 0.0228(4) -0.0006(3) 0.0032(4) 0.0000(4) P2 0.0229(5) 0.0236(5) 0.0239(4) 0.0012(3) 0.0063(4) 0.0002(4) Sb1 0.02673(14) 0.03630(15) 0.02125(13) 0.00591(10) -0.00023(10) -0.00937(11) 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 N1 C1 C6 114.5(3) N1 C1 C2 115.5(3) C6 C1 C2 111.8(3) N1 C1 Ni1 73.45(17) C6 C1 Ni1 117.8(2) C2 C1 Ni1 118.6(2) C7 C2 C3 121.9(3) C7 C2 C1 118.9(3) C3 C2 C1 119.1(3) C10 C3 C2 117.3(3) C10 C3 C4 123.1(3) C2 C3 C4 119.6(3) C3 C4 C5 109.1(3) C3 C4 C16 112.3(3) C5 C4 C16 111.0(3) C3 C4 C15 108.2(3) C5 C4 C15 109.1(3) C16 C4 C15 107.0(3) C14 C5 C6 117.8(3) C14 C5 C4 123.0(3) C6 C5 C4 119.2(3) C11 C6 C5 121.1(3) C11 C6 C1 119.3(3) C5 C6 C1 119.5(3) C2 C7 C8 119.3(3) C2 C7 P1 113.7(2) C8 C7 P1 126.9(3) C9 C8 C7 119.6(3) C9 C8 H8 120.2 C7 C8 H8 120.2 C8 C9 C10 120.5(3) C8 C9 H9 119.7 C10 C9 H9 119.7 C9 C10 C3 121.5(3) C9 C10 H10 119.3 C3 C10 H10 119.3 C12 C11 C6 119.8(3) C12 C11 P2 126.0(3) C6 C11 P2 114.1(2) C13 C12 C11 119.4(3) C13 C12 H12 120.3 C11 C12 H12 120.3 C12 C13 C14 121.0(3) C12 C13 H13 119.5 C14 C13 H13 119.5 C13 C14 C5 120.8(3) C13 C14 H14 119.6 C5 C14 H14 119.6 C4 C15 H15A 109.5 C4 C15 H15B 109.5 H15A C15 H15B 109.5 C4 C15 H15C 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 C4 C16 H16A 109.5 C4 C16 H16B 109.5 H16A C16 H16B 109.5 C4 C16 H16C 109.5 H16A C16 H16C 109.5 H16B C16 H16C 109.5 C19 C17 C18 112.3(4) C19 C17 P1 110.1(3) C18 C17 P1 111.1(3) C19 C17 H17 107.7 C18 C17 H17 107.7 P1 C17 H17 107.7 C17 C18 H18A 109.5 C17 C18 H18B 109.5 H18A C18 H18B 109.5 C17 C18 H18C 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 C17 C19 H19A 109.5 C17 C19 H19B 109.5 H19A C19 H19B 109.5 C17 C19 H19C 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 C22 C20 C21 110.3(3) C22 C20 P1 109.7(2) C21 C20 P1 116.7(3) C22 C20 H20 106.5 C21 C20 H20 106.5 P1 C20 H20 106.5 C20 C21 H21A 109.5 C20 C21 H21B 109.5 H21A C21 H21B 109.5 C20 C21 H21C 109.5 H21A C21 H21C 109.5 H21B C21 H21C 109.5 C20 C22 H22A 109.5 C20 C22 H22B 109.5 H22A C22 H22B 109.5 C20 C22 H22C 109.5 H22A C22 H22C 109.5 H22B C22 H22C 109.5 C24 C23 C25 111.2(4) C24 C23 P2 113.5(3) C25 C23 P2 109.2(3) C24 C23 H23 107.6 C25 C23 H23 107.6 P2 C23 H23 107.6 C23 C24 H24A 109.5 C23 C24 H24B 109.5 H24A C24 H24B 109.5 C23 C24 H24C 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 C23 C25 H25A 109.5 C23 C25 H25B 109.5 H25A C25 H25B 109.5 C23 C25 H25C 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 C28 C26 C27 110.1(3) C28 C26 P2 110.0(2) C27 C26 P2 112.8(3) C28 C26 H26 108.0 C27 C26 H26 108.0 P2 C26 H26 108.0 C26 C27 H27A 109.5 C26 C27 H27B 109.5 H27A C27 H27B 109.5 C26 C27 H27C 109.5 H27A C27 H27C 109.5 H27B C27 H27C 109.5 C26 C28 H28A 109.5 C26 C28 H28B 109.5 H28A C28 H28B 109.5 C26 C28 H28C 109.5 H28A C28 H28C 109.5 H28B C28 H28C 109.5 C1 N1 Ni1 64.21(16) C1 N1 H1A 117.3 Ni1 N1 H1A 117.3 C1 N1 H1B 117.3 Ni1 N1 H1B 117.3 H1A N1 H1B 114.4 Ni1 N2 H2A 109.5 Ni1 N2 H2B 109.5 H2A N2 H2B 109.5 Ni1 N2 H2C 109.5 H2A N2 H2C 109.5 H2B N2 H2C 109.5 C1 Ni1 N2 151.20(13) C1 Ni1 N1 42.33(12) N2 Ni1 N1 108.89(12) C1 Ni1 P1 87.24(10) N2 Ni1 P1 101.05(9) N1 Ni1 P1 102.07(8) C1 Ni1 P2 88.22(10) N2 Ni1 P2 102.70(9) N1 Ni1 P2 102.20(8) P1 Ni1 P2 138.08(4) C7 P1 C17 103.85(16) C7 P1 C20 107.17(16) C17 P1 C20 102.88(17) C7 P1 Ni1 101.42(11) C17 P1 Ni1 125.47(12) C20 P1 Ni1 114.45(12) C11 P2 C23 105.38(17) C11 P2 C26 100.53(16) C23 P2 C26 102.65(17) C11 P2 Ni1 100.43(11) C23 P2 Ni1 122.34(13) C26 P2 Ni1 122.06(12) F5 Sb1 F2 90.79(12) F5 Sb1 F4 179.67(13) F2 Sb1 F4 88.88(10) F5 Sb1 F6 90.41(13) F2 Sb1 F6 178.81(11) F4 Sb1 F6 89.93(12) F5 Sb1 F3 90.87(10) F2 Sb1 F3 90.61(10) F4 Sb1 F3 89.11(10) F6 Sb1 F3 89.34(11) F5 Sb1 F1 90.32(10) F2 Sb1 F1 90.00(10) F4 Sb1 F1 89.71(10) F6 Sb1 F1 90.03(11) F3 Sb1 F1 178.66(10) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 N1 1.441(4) C1 C6 1.495(4) C1 C2 1.501(4) C1 Ni1 1.926(3) C2 C7 1.383(5) C2 C3 1.401(5) C3 C10 1.391(5) C3 C4 1.528(5) C4 C5 1.528(5) C4 C16 1.538(5) C4 C15 1.554(5) C5 C14 1.390(5) C5 C6 1.406(5) C6 C11 1.394(5) C7 C8 1.400(5) C7 P1 1.819(3) C8 C9 1.375(5) C8 H8 0.9300 C9 C10 1.384(5) C9 H9 0.9300 C10 H10 0.9300 C11 C12 1.385(5) C11 P2 1.820(3) C12 C13 1.379(5) C12 H12 0.9300 C13 C14 1.387(5) C13 H13 0.9300 C14 H14 0.9300 C15 H15A 0.9600 C15 H15B 0.9600 C15 H15C 0.9600 C16 H16A 0.9600 C16 H16B 0.9600 C16 H16C 0.9600 C17 C19 1.514(5) C17 C18 1.521(6) C17 P1 1.848(4) C17 H17 0.9800 C18 H18A 0.9600 C18 H18B 0.9600 C18 H18C 0.9600 C19 H19A 0.9600 C19 H19B 0.9600 C19 H19C 0.9600 C20 C22 1.523(5) C20 C21 1.526(5) C20 P1 1.851(4) C20 H20 0.9800 C21 H21A 0.9600 C21 H21B 0.9600 C21 H21C 0.9600 C22 H22A 0.9600 C22 H22B 0.9600 C22 H22C 0.9600 C23 C24 1.491(6) C23 C25 1.537(6) C23 P2 1.862(4) C23 H23 0.9800 C24 H24A 0.9600 C24 H24B 0.9600 C24 H24C 0.9600 C25 H25A 0.9600 C25 H25B 0.9600 C25 H25C 0.9600 C26 C28 1.512(5) C26 C27 1.522(5) C26 P2 1.867(3) C26 H26 0.9800 C27 H27A 0.9600 C27 H27B 0.9600 C27 H27C 0.9600 C28 H28A 0.9600 C28 H28B 0.9600 C28 H28C 0.9600 F1 Sb1 1.880(2) F2 Sb1 1.869(2) F3 Sb1 1.875(2) F4 Sb1 1.871(2) F5 Sb1 1.855(2) F6 Sb1 1.874(2) N1 Ni1 2.050(3) N1 H1A 0.8900 N1 H1B 0.8900 N2 Ni1 2.013(3) N2 H2A 0.8900 N2 H2B 0.8900 N2 H2C 0.8900 Ni1 P1 2.2124(9) Ni1 P2 2.2199(10)