# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1576 data_global #============================================================================ # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof Malcolm L.H.Green' _publ_contact_author_address ; Inorganic Chemistry Laboratory, University of Oxford, South Parks Road, Oxford. OX1 3QR ; _publ_contact_author_phone '(01865) 272649' _publ_contact_author_fax '(01865) 272690 ' _publ_contact_author_email 'Malcolm.Green@chemistry.ox.ac.uk' _publ_requested_journal 'J. Chem. Soc., Chem. Commun.' _publ_requested_category CO _publ_requested_coeditor_name ' ? ' #============================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Weakly-coordinating Anions Stabilise the Unprecedented Monovalent and Divalent eta-Benzene Nickel Cations [(eta-C5H5)Ni(eta-C6H6)Ni(eta-C5H5)]2+ and [Ni(eta-C6H6)2]2+ ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Priego, Jose L.' ; Inorganic Chemistry Laboratory, University of Oxford, South Parks Road, Oxford. OX1 3QR ; ; ? #footnote for author 1 ; ; 'Doerrer, Linda H.' # Author 2 ; ; Inorganic Chemistry Laboratory, University of Oxford, South Parks Road, Oxford. OX1 3QR ; ; ? # footnote 2 ; ; 'Rees, Leigh H.' # Author 2 ; ; Inorganic Chemistry Laboratory, University of Oxford, South Parks Road, Oxford. OX1 3QR ; ; ? # footnote 2 ; ; 'Green, Malcolm L. H.' # Author 2 ; ; Inorganic Chemistry Laboratory, University of Oxford, South Parks Road, Oxford. OX1 3QR ; ; ? # footnote 2 ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; ? ; _publ_section_comment #Text of the paper ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions #Captions to figures ; ? ; _publ_section_exptl_refinement # see also _refine_ls_hydrogen for refinement keywords. ; H atoms placed geometrically after each cycle ; _publ_section_exptl_prep ; ? ; ## -----------------REFERENCES ----------------------## _publ_section_references ; # SIR92 # Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 # Chebychev Weights # Carruthers, J.R. and Watkin, D.J. (1979), Acta Cryst, A35, 698-699 # Denzo # Otwinowski, Z. & Minor, W. (1996), Processing of X-ray Diffraction Data Collected in Oscillation Mode. Methods Enzymol. 276, 1997, 307-326. Ed Carter, C.W. & Sweet, R.M., Academic Press. # Extinction correction # Larson, A.C. (1970), Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294 # Azimutal absorption correction # North, A.C.T., Phillips, D.C. and Mathews, F.S., (1968), Acta Cryst, A24, 351-359 # SHELXS 86 # Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of Gottingen, Federal Republic of Germany. # DIFABS # Walker, N., and Stuart, D. Acta Cryst, (1983) A39, 158-166 # CRYSTALS # Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10. Chemical Crystallography Laboratory, OXFORD, UK. #CAMERON # Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. # RC93 # Watkin, D.J., Prout, C.K., Lilley, P.M.deQ. (1994), RC93, Chemical Crystallography Laboratory, Oxford, UK. ; #========================================================================== # Diffractometer details #========================================================================== _diffrn_measurement_device_type ; Enraf-nonius DIP2000 ; _diffrn_radiation_monochromator graphite _computing_data_collection ; DIP2000 software 'Xpress' (MAC Science, 1989) ; _computing_data_reduction ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; _computing_cell_refinement ; DIP2000 software 'DENZO' (Otwinowski & Minor, 1996) ; #========================================================================= data_complex1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C32 H12 B F24, C10 H10 Ni' _chemical_formula_structural 'C42 H22 B F24 Ni' _chemical_formula_analytical ? _chemical_formula_sum 'C42 H22 B F24 Ni' _chemical_formula_weight 1052.12 _chemical_melting_point ? _chemical_compound_source 'synthesis as described' 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' 'B' 'B' 0.0013 0.0007 '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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.792(3) _cell_length_b 12.679(3) _cell_length_c 21.434(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.52(3) _cell_angle_gamma 90.00 _cell_volume 4290.1(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour 'blue green' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method none _exptl_crystal_F_000 2092 _exptl_absorpt_coefficient_mu 0.588 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.8297 _exptl_absorpt_correction_T_max 1.0214 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2802 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 22.50 _reflns_number_total 2802 _reflns_number_observed 2760 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Enraf-Nonius DIP2000 Software - XPRESS' _computing_cell_refinement DENZO _computing_data_reduction 'DENZO & SCALEPACK' _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1998)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+31.9699P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2801 _refine_ls_number_parameters 393 _refine_ls_number_restraints 471 _refine_ls_R_factor_all 0.0948 _refine_ls_R_factor_obs 0.0921 _refine_ls_wR_factor_all 0.1973 _refine_ls_wR_factor_obs 0.1857 _refine_ls_goodness_of_fit_all 1.451 _refine_ls_goodness_of_fit_obs 1.457 _refine_ls_restrained_S_all 1.516 _refine_ls_restrained_S_obs 1.450 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 1.0000 0.5000 0.5000 0.0327(4) Uani 1 d S . B1 B 1.0000 0.1755(8) 0.7500 0.020(2) Uani 1 d S . C1 C 1.0771(4) 0.2486(5) 0.7251(3) 0.0197(14) Uani 1 d . . C2 C 1.1031(4) 0.3402(5) 0.7551(3) 0.028(2) Uani 1 d . . H2 H 1.0722(4) 0.3641(5) 0.7886(3) 0.034 Uiso 1 calc R . C3 C 1.1728(4) 0.3980(6) 0.7375(3) 0.034(2) Uani 1 d . . C4 C 1.1973(6) 0.4918(8) 0.7727(4) 0.071(3) Uani 1 d D . F41 F 1.2189(6) 0.4703(7) 0.8332(3) 0.108(3) Uani 0.838(9) d PDU 1 F42 F 1.1347(6) 0.5601(6) 0.7797(4) 0.103(3) Uani 0.838(9) d PDU 1 F43 F 1.2625(6) 0.5431(7) 0.7513(4) 0.117(3) Uani 0.838(9) d PDU 1 C5 C 1.2199(4) 0.3657(5) 0.6879(3) 0.030(2) Uani 1 d . . H5 H 1.2678(4) 0.4028(5) 0.6763(3) 0.036 Uiso 1 calc R . C6 C 1.1941(4) 0.2770(5) 0.6561(3) 0.0255(15) Uani 1 d . . C7 C 1.2391(5) 0.2462(5) 0.5997(3) 0.041(2) Uani 1 d D . F71 F 1.3225(3) 0.2410(5) 0.6093(3) 0.092(2) Uani 1 d D . F72 F 1.2184(4) 0.1537(4) 0.5772(2) 0.075(2) Uani 1 d D . F73 F 1.2301(4) 0.3158(4) 0.5550(2) 0.094(2) Uani 1 d D . C8 C 1.1252(4) 0.2198(5) 0.6744(3) 0.0226(14) Uani 1 d . . H8 H 1.1101(4) 0.1595(5) 0.6521(3) 0.027 Uiso 1 calc R . C9 C 0.9644(4) 0.1016(5) 0.6925(3) 0.0243(15) Uani 1 d . . C10 C 0.8951(4) 0.1271(5) 0.6548(3) 0.028(2) Uani 1 d . . H10 H 0.8636(4) 0.1864(5) 0.6647(3) 0.033 Uiso 1 calc R . C11 C 0.8702(4) 0.0681(6) 0.6025(3) 0.038(2) Uani 1 d . . C12 C 0.7950(6) 0.0999(7) 0.5662(4) 0.058(2) Uani 1 d D . F121 F 0.7883(5) 0.2014(5) 0.5570(4) 0.102(3) Uani 0.870(8) d PDU 1 F122 F 0.7234(4) 0.0724(6) 0.5909(3) 0.084(2) Uani 0.870(8) d PDU 1 F123 F 0.7904(5) 0.0558(8) 0.5095(3) 0.111(3) Uani 0.870(8) d PDU 1 C13 C 0.9144(5) -0.0203(6) 0.5863(4) 0.049(2) Uani 1 d . . H13 H 0.8983(5) -0.0598(6) 0.5514(4) 0.058 Uiso 1 calc R . C14 C 0.9835(5) -0.0489(6) 0.6233(4) 0.044(2) Uani 1 d . . C15 C 1.0321(6) -0.1431(9) 0.6085(6) 0.087(4) Uani 1 d D . F151 F 1.1144(5) -0.1276(7) 0.6100(5) 0.117(3) Uani 0.839(9) d PDU 1 F152 F 1.0194(6) -0.2225(6) 0.6480(5) 0.114(3) Uani 0.839(9) d PDU 1 F153 F 1.0127(6) -0.1848(7) 0.5532(4) 0.124(3) Uani 0.839(9) d PDU 1 C16 C 1.0067(4) 0.0107(5) 0.6753(3) 0.035(2) Uani 1 d . . H16 H 1.0528(4) -0.0114(5) 0.6999(3) 0.041 Uiso 1 calc R . C21 C 0.9962(6) 0.3551(7) 0.5595(4) 0.054(2) Uani 1 d . . H21 H 1.0208(6) 0.2885(7) 0.5588(4) 0.065 Uiso 1 calc R . C22 C 0.9190(5) 0.3860(7) 0.5316(4) 0.051(2) Uani 1 d . . H22 H 0.8870(5) 0.3460(7) 0.5032(4) 0.062 Uiso 1 calc R . C23 C 0.8976(5) 0.4862(7) 0.5529(4) 0.051(2) Uani 1 d . . H23 H 0.8465(5) 0.5208(7) 0.5448(4) 0.061 Uiso 1 calc R . C24 C 0.9661(6) 0.5260(6) 0.5885(3) 0.048(2) Uani 1 d . . H24 H 0.9692(6) 0.5915(6) 0.6080(3) 0.057 Uiso 1 calc R . C25 C 1.0292(5) 0.4474(7) 0.5891(4) 0.050(2) Uani 1 d . . H25 H 1.0837(5) 0.4547(7) 0.6061(4) 0.060 Uiso 1 calc R . F41A F 1.1600(20) 0.5220(29) 0.8241(10) 0.105(5) Uani 0.162(9) d PDU 2 F42B F 1.1896(15) 0.5758(22) 0.7386(13) 0.110(5) Uani 0.162(9) d PDU 2 F43C F 1.2747(14) 0.4892(28) 0.7960(11) 0.115(5) Uani 0.162(9) d PDU 2 F12A F 0.7402(19) 0.1651(17) 0.5927(16) 0.096(5) Uani 0.130(8) d PDU 2 F12B F 0.7471(21) 0.0196(25) 0.5489(13) 0.096(5) Uani 0.130(8) d PDU 2 F12C F 0.8038(30) 0.1479(17) 0.5124(10) 0.104(5) Uani 0.130(8) d PDU 2 F15A F 1.0871(15) -0.1779(25) 0.6520(13) 0.113(5) Uani 0.161(9) d PDU 2 F15B F 0.9901(27) -0.2304(23) 0.5971(11) 0.119(5) Uani 0.161(9) d PDU 2 F15C F 1.0771(16) -0.1308(30) 0.5589(10) 0.122(5) Uani 0.161(9) d PDU 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 Ni1 0.0275(7) 0.0454(8) 0.0253(7) -0.0041(6) 0.0018(5) -0.0029(6) B1 0.017(5) 0.021(5) 0.022(5) 0.000 0.001(4) 0.000 C1 0.017(3) 0.026(3) 0.016(3) 0.003(3) -0.002(3) 0.003(3) C2 0.022(3) 0.040(4) 0.022(3) -0.007(3) 0.006(3) -0.007(3) C3 0.037(4) 0.040(4) 0.026(4) -0.007(3) 0.004(3) -0.015(3) C4 0.073(7) 0.089(8) 0.053(6) -0.041(6) 0.033(5) -0.051(6) F41 0.120(6) 0.134(6) 0.069(5) -0.061(4) 0.011(4) -0.049(5) F42 0.119(6) 0.069(5) 0.122(6) -0.059(5) 0.029(5) -0.037(4) F43 0.126(6) 0.128(6) 0.102(5) -0.076(4) 0.083(5) -0.112(5) C5 0.023(4) 0.036(4) 0.033(4) 0.004(3) 0.004(3) -0.004(3) C6 0.025(4) 0.028(4) 0.025(4) 0.003(3) 0.010(3) 0.002(3) C7 0.046(5) 0.033(4) 0.047(5) -0.003(4) 0.028(4) -0.001(4) F71 0.050(3) 0.119(5) 0.109(5) -0.026(4) 0.050(3) 0.004(3) F72 0.102(4) 0.057(3) 0.070(3) -0.026(3) 0.063(3) -0.023(3) F73 0.170(6) 0.070(4) 0.044(3) 0.021(3) 0.065(4) 0.039(4) C8 0.025(4) 0.025(3) 0.018(3) 0.000(3) 0.002(3) 0.004(3) C9 0.024(4) 0.028(4) 0.021(3) 0.004(3) 0.006(3) -0.005(3) C10 0.031(4) 0.029(4) 0.022(4) 0.006(3) 0.002(3) -0.009(3) C11 0.035(4) 0.051(5) 0.027(4) 0.008(4) -0.006(3) -0.023(4) C12 0.077(7) 0.056(6) 0.042(5) 0.009(4) -0.030(5) -0.027(5) F121 0.106(5) 0.077(5) 0.116(6) 0.054(4) -0.082(4) -0.043(4) F122 0.046(3) 0.109(5) 0.095(5) 0.050(4) -0.027(3) -0.024(4) F123 0.110(5) 0.157(7) 0.064(4) -0.008(5) -0.047(4) -0.018(5) C13 0.054(5) 0.051(5) 0.040(5) -0.017(4) 0.006(4) -0.025(4) C14 0.042(5) 0.039(4) 0.051(5) -0.019(4) 0.016(4) -0.013(4) C15 0.059(7) 0.072(8) 0.130(11) -0.062(8) 0.033(7) -0.017(6) F151 0.073(5) 0.095(5) 0.185(8) -0.090(6) 0.026(5) 0.004(4) F152 0.127(7) 0.062(5) 0.151(7) -0.042(5) 0.003(6) 0.024(5) F153 0.137(7) 0.106(6) 0.130(7) -0.096(6) -0.004(5) 0.017(5) C16 0.030(4) 0.034(4) 0.040(4) -0.003(3) 0.007(3) -0.010(3) C21 0.068(6) 0.049(5) 0.046(5) 0.007(4) -0.014(4) 0.003(4) C22 0.045(5) 0.052(5) 0.057(5) 0.005(4) -0.008(4) -0.014(4) C23 0.038(4) 0.068(6) 0.046(5) -0.006(4) 0.012(4) 0.003(4) C24 0.075(6) 0.042(5) 0.027(4) -0.003(3) 0.014(4) -0.008(4) C25 0.047(5) 0.064(6) 0.039(4) 0.012(4) -0.016(4) -0.010(5) F41A 0.119(9) 0.103(9) 0.095(9) -0.061(8) 0.028(9) -0.044(8) F42B 0.127(9) 0.093(8) 0.113(9) -0.067(8) 0.050(9) -0.067(9) F43C 0.121(9) 0.131(9) 0.094(9) -0.064(8) 0.037(8) -0.082(9) F12A 0.077(8) 0.100(9) 0.106(9) 0.045(8) -0.055(8) -0.028(8) F12B 0.075(8) 0.130(9) 0.082(9) 0.021(8) -0.041(8) -0.025(8) F12C 0.108(9) 0.115(9) 0.085(9) 0.031(9) -0.061(8) -0.027(9) F15A 0.100(9) 0.074(9) 0.165(10) -0.067(9) 0.011(9) 0.022(8) F15B 0.130(9) 0.082(9) 0.144(10) -0.069(9) -0.002(9) 0.014(8) F15C 0.105(9) 0.104(9) 0.157(10) -0.087(9) 0.020(9) 0.016(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Ni1 C23 2.007(7) . ? Ni1 C23 2.007(7) 5_766 ? Ni1 C24 2.012(7) 5_766 ? Ni1 C24 2.012(7) . ? Ni1 C22 2.056(8) 5_766 ? Ni1 C22 2.056(8) . ? Ni1 C25 2.063(7) . ? Ni1 C25 2.063(7) 5_766 ? Ni1 C21 2.238(8) . ? Ni1 C21 2.238(8) 5_766 ? B1 C1 1.631(8) . ? B1 C1 1.631(8) 2_756 ? B1 C9 1.636(8) 2_756 ? B1 C9 1.637(8) . ? C1 C2 1.384(9) . ? C1 C8 1.391(8) . ? C2 C3 1.383(9) . ? C3 C5 1.376(9) . ? C3 C4 1.455(11) . ? C4 F42B 1.30(2) . ? C4 F43C 1.31(2) . ? C4 F43 1.310(10) . ? C4 F41A 1.32(2) . ? C4 F42 1.325(11) . ? C4 F41 1.359(11) . ? C5 C6 1.371(9) . ? C6 C8 1.375(9) . ? C6 C7 1.469(9) . ? C7 F72 1.306(8) . ? C7 F73 1.308(8) . ? C7 F71 1.330(9) . ? C9 C10 1.381(9) . ? C9 C16 1.386(9) . ? C10 C11 1.395(9) . ? C11 C13 1.370(11) . ? C11 C12 1.459(11) . ? C12 F121 1.306(10) . ? C12 F122 1.307(10) . ? C12 F12C 1.31(2) . ? C12 F12B 1.32(2) . ? C12 F12A 1.34(2) . ? C12 F123 1.339(10) . ? C13 C14 1.381(11) . ? C14 C16 1.387(10) . ? C14 C15 1.459(13) . ? C15 F15C 1.31(2) . ? C15 F15B 1.31(2) . ? C15 F151 1.315(11) . ? C15 F153 1.327(12) . ? C15 F15A 1.33(2) . ? C15 F152 1.334(13) . ? C21 C22 1.400(11) . ? C21 C25 1.423(11) . ? C22 C23 1.394(12) . ? C23 C24 1.401(11) . ? C24 C25 1.409(12) . ? 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 C23 Ni1 C23 179.999(1) . 5_766 ? C23 Ni1 C24 139.2(3) . 5_766 ? C23 Ni1 C24 40.8(3) 5_766 5_766 ? C23 Ni1 C24 40.8(3) . . ? C23 Ni1 C24 139.2(3) 5_766 . ? C24 Ni1 C24 179.999(2) 5_766 . ? C23 Ni1 C22 139.9(3) . 5_766 ? C23 Ni1 C22 40.1(3) 5_766 5_766 ? C24 Ni1 C22 67.8(3) 5_766 5_766 ? C24 Ni1 C22 112.3(3) . 5_766 ? C23 Ni1 C22 40.1(3) . . ? C23 Ni1 C22 139.9(3) 5_766 . ? C24 Ni1 C22 112.3(3) 5_766 . ? C24 Ni1 C22 67.7(3) . . ? C22 Ni1 C22 179.998(1) 5_766 . ? C23 Ni1 C25 67.2(3) . . ? C23 Ni1 C25 112.8(3) 5_766 . ? C24 Ni1 C25 139.6(3) 5_766 . ? C24 Ni1 C25 40.4(3) . . ? C22 Ni1 C25 113.9(3) 5_766 . ? C22 Ni1 C25 66.0(3) . . ? C23 Ni1 C25 112.8(3) . 5_766 ? C23 Ni1 C25 67.2(3) 5_766 5_766 ? C24 Ni1 C25 40.4(3) 5_766 5_766 ? C24 Ni1 C25 139.6(3) . 5_766 ? C22 Ni1 C25 66.1(3) 5_766 5_766 ? C22 Ni1 C25 113.9(3) . 5_766 ? C25 Ni1 C25 179.998(1) . 5_766 ? C23 Ni1 C21 64.7(3) . . ? C23 Ni1 C21 115.3(3) 5_766 . ? C24 Ni1 C21 114.5(3) 5_766 . ? C24 Ni1 C21 65.5(3) . . ? C22 Ni1 C21 142.2(3) 5_766 . ? C22 Ni1 C21 37.8(3) . . ? C25 Ni1 C21 38.4(3) . . ? C25 Ni1 C21 141.6(3) 5_766 . ? C23 Ni1 C21 115.3(3) . 5_766 ? C23 Ni1 C21 64.7(3) 5_766 5_766 ? C24 Ni1 C21 65.5(3) 5_766 5_766 ? C24 Ni1 C21 114.5(3) . 5_766 ? C22 Ni1 C21 37.8(3) 5_766 5_766 ? C22 Ni1 C21 142.2(3) . 5_766 ? C25 Ni1 C21 141.6(3) . 5_766 ? C25 Ni1 C21 38.4(3) 5_766 5_766 ? C21 Ni1 C21 179.998(1) . 5_766 ? C1 B1 C1 110.8(7) . 2_756 ? C1 B1 C9 109.1(3) . 2_756 ? C1 B1 C9 108.9(3) 2_756 2_756 ? C1 B1 C9 108.9(3) . . ? C1 B1 C9 109.1(3) 2_756 . ? C9 B1 C9 110.1(7) 2_756 . ? C2 C1 C8 115.0(5) . . ? C2 C1 B1 122.6(5) . . ? C8 C1 B1 122.3(5) . . ? C3 C2 C1 123.1(6) . . ? C5 C3 C2 120.2(6) . . ? C5 C3 C4 120.1(6) . . ? C2 C3 C4 119.7(6) . . ? F42B C4 F43C 108.0(17) . . ? F42B C4 F41A 101.3(19) . . ? F43C C4 F41A 97.0(19) . . ? F43 C4 F42 108.1(9) . . ? F43 C4 F41 104.6(8) . . ? F42 C4 F41 101.1(7) . . ? F42B C4 C3 111.1(17) . . ? F43C C4 C3 114.2(19) . . ? F43 C4 C3 115.2(7) . . ? F41A C4 C3 123.4(20) . . ? F42 C4 C3 113.8(8) . . ? F41 C4 C3 112.7(8) . . ? C6 C5 C3 118.0(6) . . ? C5 C6 C8 121.1(6) . . ? C5 C6 C7 118.9(6) . . ? C8 C6 C7 119.9(6) . . ? F72 C7 F73 108.3(7) . . ? F72 C7 F71 104.4(6) . . ? F73 C7 F71 103.6(6) . . ? F72 C7 C6 114.9(6) . . ? F73 C7 C6 112.2(6) . . ? F71 C7 C6 112.6(6) . . ? C6 C8 C1 122.5(6) . . ? C10 C9 C16 114.8(6) . . ? C10 C9 B1 123.9(6) . . ? C16 C9 B1 121.2(6) . . ? C9 C10 C11 123.1(7) . . ? C13 C11 C10 120.5(7) . . ? C13 C11 C12 120.2(7) . . ? C10 C11 C12 119.2(7) . . ? F121 C12 F122 104.9(8) . . ? F12C C12 F12B 100.6(20) . . ? F12C C12 F12A 99.9(21) . . ? F12B C12 F12A 103.0(19) . . ? F121 C12 F123 105.8(7) . . ? F122 C12 F123 103.2(7) . . ? F121 C12 C11 114.5(7) . . ? F122 C12 C11 114.2(7) . . ? F12C C12 C11 119.5(23) . . ? F12B C12 C11 113.0(21) . . ? F12A C12 C11 118.2(19) . . ? F123 C12 C11 113.1(8) . . ? C11 C13 C14 118.0(7) . . ? C13 C14 C16 120.4(7) . . ? C13 C14 C15 120.1(8) . . ? C16 C14 C15 119.5(8) . . ? F15C C15 F15B 103.4(19) . . ? F151 C15 F153 106.6(8) . . ? F15C C15 F15A 104.5(19) . . ? F15B C15 F15A 99.7(20) . . ? F151 C15 F152 105.2(11) . . ? F153 C15 F152 103.4(9) . . ? F15C C15 C14 112.4(21) . . ? F15B C15 C14 117.8(22) . . ? F151 C15 C14 113.4(8) . . ? F153 C15 C14 114.3(10) . . ? F15A C15 C14 117.1(19) . . ? F152 C15 C14 113.1(8) . . ? C9 C16 C14 123.2(7) . . ? C22 C21 C25 105.3(7) . . ? C22 C21 Ni1 64.1(4) . . ? C25 C21 Ni1 64.2(4) . . ? C23 C22 C21 109.3(8) . . ? C23 C22 Ni1 68.0(4) . . ? C21 C22 Ni1 78.2(5) . . ? C22 C23 C24 108.4(7) . . ? C22 C23 Ni1 71.8(5) . . ? C24 C23 Ni1 69.8(4) . . ? C23 C24 C25 106.6(7) . . ? C23 C24 Ni1 69.4(4) . . ? C25 C24 Ni1 71.7(4) . . ? C24 C25 C21 109.1(7) . . ? C24 C25 Ni1 67.8(4) . . ? C21 C25 Ni1 77.5(5) . . ? _refine_diff_density_max 0.563 _refine_diff_density_min -0.419 _refine_diff_density_rms 0.073 #==END data_complex2 #========================================================================== # General computing #========================================================================== _computing_structure_refinement ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_publication_material ; CRYSTALS Issue 10 (Watkin, Prout, Carruthers & Betteridge, 1996) ; _computing_molecular_graphics ; CAMERON (Watkin, Prout & Pearce, 1996) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1992)' #========================================================================== _chemical_name_systematic ; ? ; _chemical_melting_point 'not measured' _refine_ls_matrix_type full _atom_sites_solution_primary direct # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref #**************************************************************************** _cell_length_a 11.873(7) _cell_angle_alpha 73.658(6) _cell_length_b 13.526(8) _cell_angle_beta 75.969(6) _cell_length_c 16.304(8) _cell_angle_gamma 71.607(6) _cell_volume 2350.0(5) _symmetry_cell_setting 'Triclinic ' _symmetry_space_group_name_H-M 'P -1 ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'Ni ' 0.2850 1.1130 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421 1.0341 'International_Tables_Vol_IV_Table_2.2B' 'C ' 0.0020 0.0020 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International_Tables_Vol_IV_Table_2.2B' 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7997 0.0030 'International_Tables_Vol_IV_Table_2.2B' 'B ' 0.0000 0.0010 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International_Tables_Vol_IV_Table_2.2B' 'O ' 0.0080 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International_Tables_Vol_IV_Table_2.2B' 'F ' 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International_Tables_Vol_IV_Table_2.2B' 'Cl ' 0.1320 0.1590 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International_Tables_Vol_IV_Table_2.2B' _chemical_formula_sum 'C47 H18 B3 Cl2 F25 Ni2 O3' _chemical_formula_moiety 'C30 B3 F25 O3, C16 H16 Ni2, C H2 Cl2' _chemical_compound_source ; ? ; _chemical_formula_weight 1326.37 _cell_measurement_reflns_used 12916 _cell_measurement_theta_min 0 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _cell_formula_units_Z 2 _exptl_crystal_description ' thinblock ' _exptl_crystal_colour ' orange-brown ' _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.40 _exptl_crystal_density_diffrn 1.87 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 1310.44 _exptl_absorpt_coefficient_mu 1.06 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.85 # Sheldrick geometric definitions 0.81 0.85 _diffrn_standards_interval_time 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 150 _diffrn_reflns_number 8130 _reflns_number_total 8130 _diffrn_reflns_av_R_equivalents 0.03 # Number of reflections with Friedels Law is 8130 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 9815 _diffrn_measured_fraction_theta_max 0.828 _reflns_number_gt 6045 _diffrn_reflns_theta_min 0.00 _diffrn_reflns_theta_max 26.57 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min -16 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _refine_diff_density_min -0.55 _refine_diff_density_max 0.43 _reflns_threshold_expression >3.00\s(I) _refine_ls_number_reflns 6045 _refine_ls_number_parameters 739 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.0572 _refine_ls_goodness_of_fit_ref 1.0715 _refine_ls_shift/su_max 0.000535 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979, 2.17 0.844 1.64 ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # Uequiv = arithmetic mean of Ui # i.e. Ueqiv = (U1+U2+U3)/3 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type Ni1 0.00622(5) -0.51634(4) 0.39333(3) 0.0400 1.0000 Uani Ni2 0.07721(5) -0.39669(4) -0.04302(3) 0.0458 1.0000 Uani Cl1 0.84653(17) -0.17519(14) 0.1233(1) 0.0855 1.0000 Uani Cl2 0.8692(3) -0.1406(3) 0.28345(17) 0.1579 1.0000 Uani F22 0.03141(19) -0.20838(15) 0.48497(16) 0.0442 1.0000 Uani F23 -0.2041(2) -0.16113(19) 0.53969(18) 0.0558 1.0000 Uani F24 -0.34433(19) 0.0408(2) 0.49267(18) 0.0541 1.0000 Uani F25 -0.23945(19) 0.19702(18) 0.38844(15) 0.0482 1.0000 Uani F26 -0.00657(19) 0.15206(15) 0.33173(13) 0.0399 1.0000 Uani F32 0.2330(2) 0.20018(17) 0.15102(15) 0.0451 1.0000 Uani F33 0.3105(2) 0.37680(17) 0.10794(16) 0.0496 1.0000 Uani F34 0.4966(2) 0.38098(18) 0.17306(18) 0.0553 1.0000 Uani F35 0.6100(3) 0.2035(2) 0.2808(2) 0.0750 1.0000 Uani F36 0.5404(3) 0.0249(2) 0.32085(18) 0.0628 1.0000 Uani F42 0.1148(2) 0.00723(19) 0.18350(15) 0.0476 1.0000 Uani F43 0.1280(3) -0.0543(2) 0.04066(18) 0.0648 1.0000 Uani F44 0.3453(3) -0.1330(2) -0.05343(16) 0.0684 1.0000 Uani F45 0.5512(3) -0.14850(19) 0.00002(16) 0.0591 1.0000 Uani F46 0.5406(2) -0.07841(18) 0.14023(14) 0.0431 1.0000 Uani F52 0.56433(18) -0.17411(16) 0.42755(13) 0.0376 1.0000 Uani F53 0.6410(2) -0.29409(18) 0.57358(15) 0.0482 1.0000 Uani F54 0.5460(2) -0.45710(18) 0.66852(15) 0.0508 1.0000 Uani F55 0.3694(2) -0.49913(17) 0.61393(15) 0.0457 1.0000 Uani F56 0.29242(19) -0.38148(16) 0.46693(14) 0.0391 1.0000 Uani F62 0.60497(18) -0.28174(17) 0.27837(15) 0.0408 1.0000 Uani F63 0.6834(2) -0.3796(2) 0.14599(19) 0.0624 1.0000 Uani F64 0.5248(3) -0.42147(19) 0.07284(15) 0.0592 1.0000 Uani F65 0.2858(2) -0.3734(2) 0.14214(14) 0.0519 1.0000 Uani F66 0.20525(18) -0.27531(19) 0.27306(14) 0.0424 1.0000 Uani O1 0.21111(19) 0.02155(17) 0.31325(14) 0.0280 1.0000 Uani O2 0.23177(19) -0.16262(16) 0.37954(14) 0.0259 1.0000 Uani O3 0.41024(19) -0.10018(16) 0.31270(13) 0.0259 1.0000 Uani C1 0.1079(7) -0.2704(5) -0.1491(3) 0.0791 1.0000 Uani C2 0.0585(5) -0.2291(4) -0.0732(4) 0.0692 1.0000 Uani C3 0.1407(5) -0.2817(4) -0.0147(3) 0.0560 1.0000 Uani C4 0.2384(4) -0.3542(4) -0.0531(3) 0.0556 1.0000 Uani C5 0.2176(6) -0.3468(5) -0.1369(3) 0.0667 1.0000 Uani C11 0.0673(5) -0.6233(3) 0.3077(3) 0.0524 1.0000 Uani C12 -0.0591(5) -0.5811(4) 0.3156(3) 0.0515 1.0000 Uani C13 -0.0849(5) -0.4685(4) 0.2861(3) 0.0548 1.0000 Uani C14 0.0264(5) -0.4404(3) 0.2604(2) 0.0501 1.0000 Uani C15 0.1198(4) -0.5345(4) 0.2731(2) 0.0500 1.0000 Uani C21 0.0249(3) -0.0317(2) 0.40098(19) 0.0255 1.0000 Uani C22 -0.0327(3) -0.1071(3) 0.4564(2) 0.0313 1.0000 Uani C23 -0.1547(3) -0.0844(3) 0.4870(2) 0.0380 1.0000 Uani C24 -0.2260(3) 0.0182(3) 0.4631(2) 0.0373 1.0000 Uani C25 -0.1730(3) 0.0961(3) 0.4101(2) 0.0340 1.0000 Uani C26 -0.0503(3) 0.0698(3) 0.3809(2) 0.0302 1.0000 Uani C31 0.3836(3) 0.1027(2) 0.2375(2) 0.0273 1.0000 Uani C32 0.3289(3) 0.1952(3) 0.1848(2) 0.0304 1.0000 Uani C33 0.3658(3) 0.2886(2) 0.1612(2) 0.0335 1.0000 Uani C34 0.4611(3) 0.2914(3) 0.1935(2) 0.0366 1.0000 Uani C35 0.5183(4) 0.2019(3) 0.2472(3) 0.0422 1.0000 Uani C36 0.4800(3) 0.1097(3) 0.2678(2) 0.0370 1.0000 Uani C41 0.3282(3) -0.0337(2) 0.1701(2) 0.0305 1.0000 Uani C42 0.2262(3) -0.0294(3) 0.1406(2) 0.0368 1.0000 Uani C43 0.2298(4) -0.0607(3) 0.0655(3) 0.0482 1.0000 Uani C44 0.3400(5) -0.1014(3) 0.0177(2) 0.0484 1.0000 Uani C45 0.4435(4) -0.1076(3) 0.0449(2) 0.0432 1.0000 Uani C46 0.4358(4) -0.0725(3) 0.1186(2) 0.0358 1.0000 Uani C51 0.4216(3) -0.2695(2) 0.4404(2) 0.0263 1.0000 Uani C52 0.5123(3) -0.2541(2) 0.4715(2) 0.0289 1.0000 Uani C53 0.5538(3) -0.3144(3) 0.5466(2) 0.0328 1.0000 Uani C54 0.5060(3) -0.3976(3) 0.5957(2) 0.0341 1.0000 Uani C55 0.4170(3) -0.4179(2) 0.5675(2) 0.0315 1.0000 Uani C56 0.3784(3) -0.3559(2) 0.4921(2) 0.0281 1.0000 Uani C61 0.4015(3) -0.2714(2) 0.2810(2) 0.0273 1.0000 Uani C62 0.5215(3) -0.3025(2) 0.2464(2) 0.0337 1.0000 Uani C63 0.5652(3) -0.3533(3) 0.1776(3) 0.0404 1.0000 Uani C64 0.4851(4) -0.3755(3) 0.1413(2) 0.0419 1.0000 Uani C65 0.3650(4) -0.3492(3) 0.1755(2) 0.0364 1.0000 Uani C66 0.3247(3) -0.2988(2) 0.2442(2) 0.0294 1.0000 Uani C81 -0.0639(6) -0.4082(5) 0.4810(3) 0.0674 1.0000 Uani C82 0.0470(6) -0.4289(4) 0.4685(3) 0.0595 1.0000 Uani C83 0.1099(6) -0.5203(6) 0.4876(4) 0.0735 1.0000 Uani C84 -0.0943(5) -0.4328(5) -0.0045(5) 0.0731 1.0000 Uani C85 -0.0510(6) -0.4588(7) 0.0614(4) 0.0823 1.0000 Uani C86 0.0424(7) -0.5233(6) 0.0653(4) 0.0771 1.0000 Uani C200 0.8196(13) -0.0928(8) 0.1901(7) 0.1617 1.0000 Uani B1 0.1659(3) -0.0601(3) 0.3626(2) 0.0235 1.0000 Uani B2 0.3600(3) -0.1998(3) 0.3547(2) 0.0259 1.0000 Uani B3 0.3289(3) -0.0011(3) 0.2603(2) 0.0269 1.0000 Uani H11 0.0696 -0.2487 -0.2015 0.0600 1.0000 Uiso H21 -0.0177 -0.1743 -0.0627 0.0600 1.0000 Uiso H31 0.1305 -0.2705 0.0444 0.0600 1.0000 Uiso H41 0.3088 -0.4012 -0.0266 0.0600 1.0000 Uiso H51 0.2714 -0.3889 -0.1789 0.0600 1.0000 Uiso H111 0.1111 -0.6994 0.3232 0.0600 1.0000 Uiso H121 -0.1187 -0.6234 0.3378 0.0600 1.0000 Uiso H131 -0.1661 -0.4180 0.2840 0.0600 1.0000 Uiso H141 0.0364 -0.3674 0.2374 0.0600 1.0000 Uiso H151 0.2067 -0.5393 0.2604 0.0600 1.0000 Uiso H811 -0.1139 -0.3309 0.4640 0.0600 1.0000 Uiso H821 0.0877 -0.3702 0.4427 0.0600 1.0000 Uiso H831 0.2011 -0.5354 0.4766 0.0600 1.0000 Uiso H841 -0.1728 -0.3757 -0.0085 0.0600 1.0000 Uiso H851 -0.0939 -0.4247 0.1116 0.0600 1.0000 Uiso H861 0.0797 -0.5419 0.1189 0.0600 1.0000 Uiso H2001 0.8584 -0.0357 0.1579 0.0600 1.0000 Uiso H2002 0.7327 -0.0655 0.2032 0.0600 1.0000 Uiso 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 0.0559(3) 0.0462(3) 0.0265(2) -0.01548(18) -0.0030(2) -0.0218(2) Ni2 0.0453(3) 0.0506(3) 0.0378(3) -0.0023(2) -0.0107(2) -0.0114(2) Cl1 0.0938(11) 0.092(1) 0.0721(8) -0.0251(8) -0.0138(8) -0.0212(9) Cl2 0.190(3) 0.183(3) 0.1247(18) -0.0752(19) -0.0895(18) 0.001(2) F22 0.0365(11) 0.0257(9) 0.0631(14) -0.0088(9) 0.0080(11) -0.0114(9) F23 0.0401(12) 0.0487(13) 0.0812(17) -0.0231(12) 0.0175(13) -0.0286(11) F24 0.023(1) 0.0687(15) 0.0755(17) -0.0371(14) 0.0052(11) -0.0103(11) F25 0.0314(11) 0.0482(12) 0.0517(13) -0.0142(11) -0.009(1) 0.012(1) F26 0.0343(11) 0.0309(9) 0.039(1) 0.0027(8) -0.0005(9) -0.0006(9) F32 0.0371(12) 0.0354(11) 0.0621(14) 0.0038(9) -0.0238(11) -0.0099(9) F33 0.0454(13) 0.030(1) 0.0644(14) 0.007(1) -0.0145(12) -0.009(1) F34 0.0615(16) 0.0368(12) 0.0737(16) -0.0024(11) -0.0142(13) -0.0282(12) F35 0.086(2) 0.0664(17) 0.096(2) 0.0176(15) -0.0578(18) -0.0507(17) F36 0.0667(17) 0.0456(13) 0.0837(18) 0.0234(12) -0.0496(15) -0.0309(13) F42 0.0375(12) 0.0554(13) 0.0551(13) -0.0203(11) -0.0160(11) -0.006(1) F43 0.0783(19) 0.0648(17) 0.0668(16) -0.0199(13) -0.0376(15) -0.0166(15) F44 0.114(2) 0.0632(16) 0.0408(12) -0.0231(12) -0.0098(15) -0.0340(17) F45 0.0771(18) 0.0493(13) 0.0414(12) -0.0186(11) 0.0209(13) -0.0196(13) F46 0.0346(11) 0.0473(12) 0.0440(11) -0.0116(9) 0.004(1) -0.013(1) F52 0.0347(11) 0.035(1) 0.0438(11) 0.0063(8) -0.0137(9) -0.0182(9) F53 0.0513(14) 0.0450(12) 0.0553(13) 0.001(1) -0.0287(12) -0.0183(11) F54 0.0629(15) 0.0437(12) 0.0423(11) 0.0100(9) -0.0254(11) -0.0139(11) F55 0.0483(13) 0.034(1) 0.0484(12) 0.0106(9) -0.0088(11) -0.019(1) F56 0.0364(11) 0.033(1) 0.0508(12) 0.0014(9) -0.012(1) -0.0184(9) F62 0.024(1) 0.0385(11) 0.0559(13) -0.012(1) -0.001(1) -0.0064(9) F63 0.0403(13) 0.0570(14) 0.0769(18) -0.0304(14) 0.0227(14) -0.0060(12) F64 0.090(2) 0.0404(12) 0.0387(11) -0.020(1) 0.0154(13) -0.0159(13) F65 0.0709(16) 0.0555(14) 0.0408(11) -0.017(1) -0.0152(12) -0.0227(13) F66 0.029(1) 0.0587(13) 0.0468(12) -0.024(1) -0.0040(9) -0.014(1) O1 0.0234(11) 0.025(1) 0.0323(11) -0.0048(8) -0.0023(9) -0.0048(9) O2 0.022(1) 0.023(1) 0.0308(11) -0.0056(8) -0.0021(9) -0.0050(9) O3 0.024(1) 0.022(1) 0.028(1) -0.0016(8) -0.0021(9) -0.0063(9) C1 0.101(5) 0.085(4) 0.051(3) 0.029(3) -0.030(3) -0.052(4) C2 0.070(3) 0.047(2) 0.077(3) 0.005(2) -0.024(3) -0.005(2) C3 0.060(3) 0.049(2) 0.058(3) -0.008(2) -0.017(2) -0.011(2) C4 0.047(2) 0.059(3) 0.062(3) -0.013(2) -0.010(2) -0.016(2) C5 0.080(4) 0.071(3) 0.054(3) -0.012(2) -0.002(3) -0.034(3) C11 0.079(3) 0.051(2) 0.0330(18) -0.0202(17) -0.002(2) -0.022(2) C12 0.071(3) 0.063(3) 0.0347(19) -0.0187(18) -0.005(2) -0.033(2) C13 0.069(3) 0.070(3) 0.0359(19) -0.0203(19) -0.012(2) -0.023(2) C14 0.077(3) 0.053(2) 0.0273(16) -0.0103(16) -0.0061(19) -0.028(2) C15 0.063(3) 0.065(3) 0.0286(17) -0.0196(17) 0.0068(19) -0.028(2) C21 0.0247(15) 0.0282(14) 0.0262(14) -0.0115(11) -0.0036(13) -0.0062(12) C22 0.0279(16) 0.0286(15) 0.0413(17) -0.0158(13) -0.0042(15) -0.0071(13) C23 0.0334(17) 0.0403(19) 0.049(2) -0.0230(16) 0.0055(17) -0.0200(16) C24 0.0185(14) 0.053(2) 0.049(2) -0.0284(17) -0.0011(15) -0.0088(15) C25 0.0252(16) 0.0427(18) 0.0340(17) -0.0176(14) -0.0083(14) 0.0014(14) C26 0.0269(16) 0.0374(17) 0.0274(15) -0.0131(13) -0.0013(14) -0.0074(14) C31 0.0264(15) 0.0269(14) 0.0260(14) -0.0053(11) -0.0002(13) -0.0073(13) C32 0.0245(15) 0.0326(16) 0.0334(16) -0.0091(13) -0.0017(14) -0.0075(13) C33 0.0354(18) 0.0228(14) 0.0346(16) -0.0019(12) -0.0006(15) -0.0052(14) C34 0.0392(19) 0.0288(16) 0.0421(18) -0.0056(14) 0.0004(16) -0.0166(15) C35 0.042(2) 0.045(2) 0.047(2) -0.0023(16) -0.0140(18) -0.0241(18) C36 0.0392(19) 0.0328(17) 0.0397(18) 0.0030(14) -0.0147(16) -0.0145(16) C41 0.0377(18) 0.0234(14) 0.0283(15) -0.0001(11) -0.0062(14) -0.0096(13) C42 0.041(2) 0.0305(16) 0.0386(18) -0.0075(14) -0.0099(16) -0.0072(15) C43 0.069(3) 0.038(2) 0.045(2) -0.0055(16) -0.027(2) -0.015(2) C44 0.083(3) 0.0351(18) 0.0293(17) -0.0055(14) -0.010(2) -0.021(2) C45 0.063(3) 0.0307(17) 0.0312(17) -0.0063(14) 0.0060(19) -0.0172(18) C46 0.043(2) 0.0302(16) 0.0307(16) -0.0017(13) -0.0035(16) -0.0119(15) C51 0.0225(14) 0.0224(13) 0.0302(15) -0.0048(11) -0.0011(13) -0.0042(12) C52 0.0275(16) 0.0248(14) 0.0328(15) -0.0021(12) -0.0041(14) -0.0090(13) C53 0.0324(17) 0.0312(16) 0.0358(17) -0.0051(13) -0.0089(15) -0.0094(14) C54 0.0376(19) 0.0277(15) 0.0303(16) 0.0003(12) -0.0114(15) -0.0015(14) C55 0.0339(17) 0.0205(14) 0.0328(16) 0.0009(12) -0.0008(15) -0.0069(13) C56 0.0255(15) 0.0229(14) 0.0342(16) -0.0053(12) -0.0035(14) -0.0059(13) C61 0.0256(15) 0.0215(13) 0.0300(15) -0.0017(11) -0.0015(13) -0.0056(12) C62 0.0299(17) 0.0240(15) 0.0419(18) -0.0051(13) -0.0007(16) -0.0059(14) C63 0.0349(19) 0.0273(16) 0.046(2) -0.0101(15) 0.0133(18) -0.0045(15) C64 0.061(2) 0.0242(15) 0.0321(17) -0.0077(13) 0.0071(18) -0.0095(17) C65 0.053(2) 0.0266(15) 0.0311(16) -0.0041(13) -0.0090(17) -0.0129(16) C66 0.0311(16) 0.0257(14) 0.0276(15) -0.0021(12) -0.0040(14) -0.0064(13) C81 0.075(4) 0.081(4) 0.054(3) -0.033(3) -0.020(3) -0.007(3) C82 0.087(4) 0.064(3) 0.041(2) -0.022(2) -0.006(2) -0.034(3) C83 0.079(4) 0.097(5) 0.060(3) -0.045(3) -0.011(3) -0.020(4) C84 0.055(3) 0.060(3) 0.107(5) -0.019(3) -0.029(3) -0.009(3) C85 0.069(4) 0.119(6) 0.077(4) -0.040(4) 0.005(4) -0.047(4) C86 0.083(5) 0.104(5) 0.052(3) -0.001(3) -0.014(3) -0.048(4) C200 0.227(13) 0.117(7) 0.131(7) -0.060(6) -0.105(8) 0.053(7) B1 0.0218(15) 0.0283(16) 0.0226(15) -0.0092(12) -0.0033(13) -0.0067(13) B2 0.0224(16) 0.0216(15) 0.0310(17) -0.0033(13) -0.0002(15) -0.0077(13) B3 0.0260(17) 0.0227(15) 0.0294(16) -0.0028(13) -0.0043(15) -0.0060(14) _refine_ls_extinction_method 'None' loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ni1 . C11 . 2.133(3) yes Ni1 . C12 . 2.122(4) yes Ni1 . C13 . 2.117(4) yes Ni1 . C14 . 2.112(4) yes Ni1 . C15 . 2.122(4) yes Ni1 . C81 . 2.169(5) yes Ni1 . C81 2_546 2.185(5) yes Ni1 . C82 . 2.145(4) yes Ni1 . C82 2_546 2.165(5) yes Ni1 . C83 . 2.170(5) yes Ni1 . C83 2_546 2.174(5) yes Ni2 . C1 . 2.113(5) yes Ni2 . C2 . 2.130(5) yes Ni2 . C3 . 2.124(4) yes Ni2 . C4 . 2.123(4) yes Ni2 . C5 . 2.114(5) yes Ni2 . C84 . 2.148(6) yes Ni2 . C84 2_545 2.177(6) yes Ni2 . C85 . 2.160(6) yes Ni2 . C85 2_545 2.184(6) yes Ni2 . C86 . 2.148(6) yes Ni2 . C86 2_545 2.182(6) yes Cl1 . C200 . 1.679(8) yes Cl2 . C200 . 1.65(1) yes F22 . C22 . 1.352(4) yes F23 . C23 . 1.341(4) yes F24 . C24 . 1.336(4) yes F25 . C25 . 1.340(4) yes F26 . C26 . 1.345(4) yes F32 . C32 . 1.357(4) yes F33 . C33 . 1.344(4) yes F34 . C34 . 1.335(4) yes F35 . C35 . 1.341(4) yes F36 . C36 . 1.343(4) yes F42 . C42 . 1.348(4) yes F43 . C43 . 1.336(5) yes F44 . C44 . 1.326(4) yes F45 . C45 . 1.343(5) yes F46 . C46 . 1.346(4) yes F52 . C52 . 1.356(3) yes F53 . C53 . 1.345(4) yes F54 . C54 . 1.333(4) yes F55 . C55 . 1.348(4) yes F56 . C56 . 1.354(4) yes F62 . C62 . 1.357(4) yes F63 . C63 . 1.341(4) yes F64 . C64 . 1.344(4) yes F65 . C65 . 1.352(4) yes F66 . C66 . 1.346(4) yes O1 . B1 . 1.349(4) yes O1 . B3 . 1.445(4) yes O2 . B1 . 1.348(4) yes O2 . B2 . 1.438(4) yes O3 . B2 . 1.558(4) yes O3 . B3 . 1.549(4) yes C1 . C2 . 1.421(9) yes C1 . C5 . 1.402(9) yes C1 . H11 . 0.993(5) no C2 . C3 . 1.413(8) yes C2 . H21 . 0.985(6) no C3 . C4 . 1.405(7) yes C3 . H31 . 0.991(5) no C4 . C5 . 1.417(7) yes C4 . H41 . 0.988(5) no C5 . H51 . 0.989(5) no C11 . C12 . 1.415(7) yes C11 . C15 . 1.438(6) yes C11 . H111 . 0.987(5) no C12 . C13 . 1.418(7) yes C12 . H121 . 0.986(4) no C13 . C14 . 1.423(7) yes C13 . H131 . 0.992(5) no C14 . C15 . 1.402(7) yes C14 . H141 . 0.987(4) no C15 . H151 . 0.986(5) no C21 . C22 . 1.395(4) yes C21 . C26 . 1.380(5) yes C21 . B1 . 1.601(4) yes C22 . C23 . 1.377(5) yes C23 . C24 . 1.380(6) yes C24 . C25 . 1.376(5) yes C25 . C26 . 1.382(5) yes C31 . C32 . 1.371(5) yes C31 . C36 . 1.390(5) yes C31 . B3 . 1.641(4) yes C32 . C33 . 1.389(4) yes C33 . C34 . 1.374(5) yes C34 . C35 . 1.365(6) yes C35 . C36 . 1.386(5) yes C41 . C42 . 1.387(5) yes C41 . C46 . 1.384(5) yes C41 . B3 . 1.653(4) yes C42 . C43 . 1.391(5) yes C43 . C44 . 1.384(7) yes C44 . C45 . 1.376(7) yes C45 . C46 . 1.385(5) yes C51 . C52 . 1.388(4) yes C51 . C56 . 1.397(4) yes C51 . B2 . 1.642(5) yes C52 . C53 . 1.373(5) yes C53 . C54 . 1.380(5) yes C54 . C55 . 1.375(5) yes C55 . C56 . 1.370(5) yes C61 . C62 . 1.375(5) yes C61 . C66 . 1.390(5) yes C61 . B2 . 1.641(4) yes C62 . C63 . 1.388(5) yes C63 . C64 . 1.377(6) yes C64 . C65 . 1.369(6) yes C65 . C66 . 1.382(4) yes C81 . C82 . 1.234(8) yes C81 . C83 2_546 1.190(8) yes C81 . H811 . 1.023(6) no C82 . C83 . 1.223(8) yes C82 . H821 . 0.998(5) no C83 . H831 . 1.016(6) no C84 . C85 . 1.22(1) yes C84 . C86 2_545 1.233(9) yes C84 . H841 . 1.008(6) no C85 . C86 . 1.18(1) yes C85 . H851 . 1.002(6) no C86 . H861 . 1.008(6) no C200 . H2001 . 0.982(15) no C200 . H2002 . 0.971(14) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C11 . Ni1 . C12 . 38.85(19) yes C11 . Ni1 . C13 . 65.44(18) yes C12 . Ni1 . C13 . 39.08(18) yes C11 . Ni1 . C14 . 65.68(16) yes C12 . Ni1 . C14 . 65.71(16) yes C13 . Ni1 . C14 . 39.32(18) yes C11 . Ni1 . C15 . 39.50(16) yes C12 . Ni1 . C15 . 65.52(16) yes C13 . Ni1 . C15 . 65.34(19) yes C14 . Ni1 . C15 . 38.69(19) yes C11 . Ni1 . C81 . 177.5(2) yes C12 . Ni1 . C81 . 138.8(2) yes C13 . Ni1 . C81 . 113.1(2) yes C14 . Ni1 . C81 . 114.6(2) yes C15 . Ni1 . C81 . 142.2(2) yes C11 . Ni1 . C81 2_546 111.89(19) yes C12 . Ni1 . C81 2_546 128.9(2) yes C13 . Ni1 . C81 2_546 164.0(2) yes C14 . Ni1 . C81 2_546 155.8(2) yes C15 . Ni1 . C81 2_546 123.6(2) yes C11 . Ni1 . C82 . 149.2(2) yes C12 . Ni1 . C82 . 170.6(2) yes C13 . Ni1 . C82 . 132.9(2) yes C14 . Ni1 . C82 . 111.08(17) yes C15 . Ni1 . C82 . 118.07(18) yes C11 . Ni1 . C82 2_546 121.73(17) yes C12 . Ni1 . C82 2_546 114.13(16) yes C13 . Ni1 . C82 2_546 133.5(2) yes C14 . Ni1 . C82 2_546 169.0(2) yes C15 . Ni1 . C82 2_546 152.2(2) yes C11 . Ni1 . C83 . 122.7(2) yes C12 . Ni1 . C83 . 156.0(2) yes C13 . Ni1 . C83 . 163.3(2) yes C14 . Ni1 . C83 . 127.3(2) yes C15 . Ni1 . C83 . 110.6(2) yes C11 . Ni1 . C83 2_546 146.4(2) yes C12 . Ni1 . C83 2_546 117.9(2) yes C13 . Ni1 . C83 2_546 113.7(2) yes C14 . Ni1 . C83 2_546 136.7(2) yes C15 . Ni1 . C83 2_546 173.8(2) yes C81 . Ni1 . C81 2_546 68.9(3) yes C81 . Ni1 . C82 . 33.2(2) yes C81 2_546 Ni1 . C82 . 57.6(2) yes C81 . Ni1 . C82 2_546 57.6(2) yes C81 2_546 Ni1 . C82 2_546 33.0(2) yes C82 . Ni1 . C82 2_546 67.2(2) yes C81 . Ni1 . C83 . 59.3(2) yes C81 2_546 Ni1 . C83 . 31.7(2) yes C82 . Ni1 . C83 . 32.9(2) yes C82 2_546 Ni1 . C83 . 57.4(2) yes C81 . Ni1 . C83 2_546 31.8(2) yes C81 2_546 Ni1 . C83 2_546 59.0(2) yes C82 . Ni1 . C83 2_546 57.7(2) yes C82 2_546 Ni1 . C83 2_546 32.7(2) yes C83 . Ni1 . C83 2_546 68.5(3) yes C1 . Ni2 . C2 . 39.1(2) yes C1 . Ni2 . C3 . 64.8(2) yes C2 . Ni2 . C3 . 38.8(2) yes C1 . Ni2 . C4 . 65.1(2) yes C2 . Ni2 . C4 . 65.4(2) yes C3 . Ni2 . C4 . 38.63(18) yes C1 . Ni2 . C5 . 38.7(3) yes C2 . Ni2 . C5 . 65.5(2) yes C3 . Ni2 . C5 . 64.93(19) yes C4 . Ni2 . C5 . 39.1(2) yes C1 . Ni2 . C84 . 121.4(3) yes C2 . Ni2 . C84 . 111.9(2) yes C3 . Ni2 . C84 . 131.5(2) yes C4 . Ni2 . C84 . 167.3(2) yes C5 . Ni2 . C84 . 152.7(3) yes C1 . Ni2 . C84 2_545 147.6(3) yes C2 . Ni2 . C84 2_545 172.9(2) yes C3 . Ni2 . C84 2_545 135.9(2) yes C4 . Ni2 . C84 2_545 113.4(2) yes C5 . Ni2 . C84 2_545 118.5(2) yes C1 . Ni2 . C85 . 147.2(3) yes C2 . Ni2 . C85 . 117.7(3) yes C3 . Ni2 . C85 . 113.6(2) yes C4 . Ni2 . C85 . 135.9(2) yes C5 . Ni2 . C85 . 173.6(3) yes C1 . Ni2 . C85 2_545 121.6(3) yes C2 . Ni2 . C85 2_545 153.6(3) yes C3 . Ni2 . C85 2_545 166.3(3) yes C4 . Ni2 . C85 2_545 130.2(2) yes C5 . Ni2 . C85 2_545 111.5(2) yes C1 . Ni2 . C86 . 178.9(3) yes C2 . Ni2 . C86 . 140.2(3) yes C3 . Ni2 . C86 . 115.2(2) yes C4 . Ni2 . C86 . 115.6(2) yes C5 . Ni2 . C86 . 142.4(3) yes C1 . Ni2 . C86 2_545 111.8(2) yes C2 . Ni2 . C86 2_545 126.9(3) yes C3 . Ni2 . C86 2_545 161.7(3) yes C4 . Ni2 . C86 2_545 158.5(3) yes C5 . Ni2 . C86 2_545 124.8(2) yes C84 . Ni2 . C84 2_545 67.6(3) yes C84 . Ni2 . C85 . 32.9(3) yes C84 2_545 Ni2 . C85 . 57.7(3) yes C84 . Ni2 . C85 2_545 57.8(2) yes C84 2_545 Ni2 . C85 2_545 32.5(3) yes C85 . Ni2 . C85 2_545 68.3(3) yes C84 . Ni2 . C86 . 57.6(3) yes C84 2_545 Ni2 . C86 . 33.1(2) yes C85 . Ni2 . C86 . 31.7(3) yes C85 2_545 Ni2 . C86 . 58.7(2) yes C84 . Ni2 . C86 2_545 33.1(2) yes C84 2_545 Ni2 . C86 2_545 56.7(2) yes C85 . Ni2 . C86 2_545 58.5(2) yes C85 2_545 Ni2 . C86 2_545 31.3(3) yes C86 . Ni2 . C86 2_545 67.8(3) yes B1 . O1 . B3 . 119.5(2) yes B1 . O2 . B2 . 125.7(2) yes B2 . O3 . B3 . 117.4(2) yes Ni2 . C1 . C2 . 71.1(3) yes Ni2 . C1 . C5 . 70.6(3) yes C2 . C1 . C5 . 108.8(5) yes Ni2 . C1 . H11 . 123.7(4) no C2 . C1 . H11 . 125.0(7) no C5 . C1 . H11 . 126.3(7) no Ni2 . C2 . C1 . 69.8(3) yes Ni2 . C2 . C3 . 70.4(3) yes C1 . C2 . C3 . 106.6(5) yes Ni2 . C2 . H21 . 125.0(4) no C1 . C2 . H21 . 127.4(6) no C3 . C2 . H21 . 126.1(6) no Ni2 . C3 . C2 . 70.8(3) yes Ni2 . C3 . C4 . 70.6(2) yes C2 . C3 . C4 . 109.2(4) yes Ni2 . C3 . H31 . 123.8(4) no C2 . C3 . H31 . 125.6(5) no C4 . C3 . H31 . 125.2(5) no Ni2 . C4 . C3 . 70.7(3) yes Ni2 . C4 . C5 . 70.1(3) yes C3 . C4 . C5 . 107.5(5) yes Ni2 . C4 . H41 . 124.8(4) no C3 . C4 . H41 . 126.2(5) no C5 . C4 . H41 . 126.3(5) no Ni2 . C5 . C1 . 70.6(3) yes Ni2 . C5 . C4 . 70.8(3) yes C1 . C5 . C4 . 108.0(5) yes Ni2 . C5 . H51 . 123.9(4) no C1 . C5 . H51 . 126.4(6) no C4 . C5 . H51 . 125.6(6) no Ni1 . C11 . C12 . 70.2(2) yes Ni1 . C11 . C15 . 69.8(2) yes C12 . C11 . C15 . 107.2(4) yes Ni1 . C11 . H111 . 125.2(3) no C12 . C11 . H111 . 126.2(4) no C15 . C11 . H111 . 126.5(5) no Ni1 . C12 . C11 . 71.0(2) yes Ni1 . C12 . C13 . 70.3(2) yes C11 . C12 . C13 . 108.4(4) yes Ni1 . C12 . H121 . 124.7(3) no C11 . C12 . H121 . 125.5(5) no C13 . C12 . H121 . 126.2(5) no Ni1 . C13 . C12 . 70.7(2) yes Ni1 . C13 . C14 . 70.2(2) yes C12 . C13 . C14 . 107.9(4) yes Ni1 . C13 . H131 . 124.5(3) no C12 . C13 . H131 . 126.2(5) no C14 . C13 . H131 . 125.8(5) no Ni1 . C14 . C13 . 70.5(2) yes Ni1 . C14 . C15 . 71.0(2) yes C13 . C14 . C15 . 108.1(4) yes Ni1 . C14 . H141 . 124.3(3) no C13 . C14 . H141 . 126.1(5) no C15 . C14 . H141 . 125.7(5) no Ni1 . C15 . C11 . 70.7(2) yes Ni1 . C15 . C14 . 70.3(2) yes C11 . C15 . C14 . 108.3(4) yes Ni1 . C15 . H151 . 124.9(3) no C11 . C15 . H151 . 125.7(5) no C14 . C15 . H151 . 125.9(4) no C22 . C21 . C26 . 114.4(3) yes C22 . C21 . B1 . 123.2(3) yes C26 . C21 . B1 . 122.5(3) yes F22 . C22 . C21 . 120.5(3) yes F22 . C22 . C23 . 116.0(3) yes C21 . C22 . C23 . 123.6(3) yes F23 . C23 . C22 . 120.3(3) yes F23 . C23 . C24 . 120.2(3) yes C22 . C23 . C24 . 119.5(3) yes F24 . C24 . C23 . 119.9(3) yes F24 . C24 . C25 . 121.0(3) yes C23 . C24 . C25 . 119.1(3) yes F25 . C25 . C24 . 120.4(3) yes F25 . C25 . C26 . 120.2(3) yes C24 . C25 . C26 . 119.4(3) yes F26 . C26 . C21 . 121.1(3) yes F26 . C26 . C25 . 114.9(3) yes C21 . C26 . C25 . 123.9(3) yes C32 . C31 . C36 . 114.2(3) yes C32 . C31 . B3 . 118.6(3) yes C36 . C31 . B3 . 127.2(3) yes F32 . C32 . C31 . 120.6(3) yes F32 . C32 . C33 . 115.2(3) yes C31 . C32 . C33 . 124.2(3) yes F33 . C33 . C32 . 122.0(3) yes F33 . C33 . C34 . 118.9(3) yes C32 . C33 . C34 . 119.2(3) yes F34 . C34 . C33 . 120.2(3) yes F34 . C34 . C35 . 120.6(3) yes C33 . C34 . C35 . 119.2(3) yes F35 . C35 . C34 . 120.2(3) yes F35 . C35 . C36 . 120.1(4) yes C34 . C35 . C36 . 119.8(3) yes F36 . C36 . C31 . 120.1(3) yes F36 . C36 . C35 . 116.4(3) yes C31 . C36 . C35 . 123.4(3) yes C42 . C41 . C46 . 114.5(3) yes C42 . C41 . B3 . 125.4(3) yes C46 . C41 . B3 . 120.1(3) yes F42 . C42 . C41 . 121.4(3) yes F42 . C42 . C43 . 115.1(3) yes C41 . C42 . C43 . 123.5(4) yes F43 . C43 . C42 . 120.5(4) yes F43 . C43 . C44 . 120.0(3) yes C42 . C43 . C44 . 119.5(4) yes F44 . C44 . C43 . 120.4(4) yes F44 . C44 . C45 . 120.7(4) yes C43 . C44 . C45 . 118.9(3) yes F45 . C45 . C44 . 119.6(3) yes F45 . C45 . C46 . 120.7(4) yes C44 . C45 . C46 . 119.7(4) yes F46 . C46 . C41 . 119.6(3) yes F46 . C46 . C45 . 116.6(3) yes C41 . C46 . C45 . 123.8(4) yes C52 . C51 . C56 . 113.1(3) yes C52 . C51 . B2 . 128.8(3) yes C56 . C51 . B2 . 118.1(3) yes F52 . C52 . C51 . 119.9(3) yes F52 . C52 . C53 . 115.8(3) yes C51 . C52 . C53 . 124.3(3) yes F53 . C53 . C52 . 121.1(3) yes F53 . C53 . C54 . 119.0(3) yes C52 . C53 . C54 . 119.9(3) yes F54 . C54 . C53 . 120.4(3) yes F54 . C54 . C55 . 121.0(3) yes C53 . C54 . C55 . 118.6(3) yes F55 . C55 . C54 . 119.7(3) yes F55 . C55 . C56 . 120.6(3) yes C54 . C55 . C56 . 119.7(3) yes F56 . C56 . C51 . 118.8(3) yes F56 . C56 . C55 . 116.8(3) yes C51 . C56 . C55 . 124.5(3) yes C62 . C61 . C66 . 114.8(3) yes C62 . C61 . B2 . 119.2(3) yes C66 . C61 . B2 . 125.9(3) yes F62 . C62 . C61 . 119.9(3) yes F62 . C62 . C63 . 116.0(3) yes C61 . C62 . C63 . 124.0(3) yes F63 . C63 . C62 . 120.8(4) yes F63 . C63 . C64 . 120.2(3) yes C62 . C63 . C64 . 119.0(3) yes F64 . C64 . C63 . 120.1(4) yes F64 . C64 . C65 . 120.8(4) yes C63 . C64 . C65 . 119.1(3) yes F65 . C65 . C64 . 119.7(3) yes F65 . C65 . C66 . 120.0(3) yes C64 . C65 . C66 . 120.3(3) yes F66 . C66 . C61 . 121.1(3) yes F66 . C66 . C65 . 116.2(3) yes C61 . C66 . C65 . 122.7(3) yes Ni1 . C81 . Ni1 2_546 111.1(3) yes Ni1 . C81 . C82 . 72.3(3) yes Ni1 2_546 C81 . C82 . 72.6(3) yes Ni1 . C81 . C83 2_546 74.3(3) yes Ni1 2_546 C81 . C83 2_546 73.5(4) yes C82 . C81 . C83 2_546 118.5(6) yes Ni1 . C81 . H811 . 123.8(4) no Ni1 2_546 C81 . H811 . 125.0(3) no C82 . C81 . H811 . 119.9(7) no C83 2_546 C81 . H811 . 121.6(7) no Ni1 . C82 . Ni1 2_546 112.8(2) yes Ni1 . C82 . C81 . 74.5(3) yes Ni1 2_546 C82 . C81 . 74.4(3) yes Ni1 . C82 . C83 . 74.7(3) yes Ni1 2_546 C82 . C83 . 74.1(3) yes C81 . C82 . C83 . 121.8(5) yes Ni1 . C82 . H821 . 123.6(3) no Ni1 2_546 C82 . H821 . 123.5(3) no C81 . C82 . H821 . 120.0(7) no C83 . C82 . H821 . 118.2(7) no Ni1 . C83 . Ni1 2_546 111.5(3) yes Ni1 . C83 . C81 2_546 74.8(3) yes Ni1 2_546 C83 . C81 2_546 73.9(4) yes Ni1 . C83 . C82 . 72.4(3) yes Ni1 2_546 C83 . C82 . 73.2(3) yes C81 2_546 C83 . C82 . 119.7(6) yes Ni1 . C83 . H831 . 124.0(4) no Ni1 2_546 C83 . H831 . 124.5(4) no C81 2_546 C83 . H831 . 119.9(7) no C82 . C83 . H831 . 120.3(7) no Ni2 . C84 . Ni2 2_545 112.4(3) yes Ni2 . C84 . C85 . 74.1(4) yes Ni2 2_545 C84 . C85 . 74.1(5) yes Ni2 . C84 . C86 2_545 75.0(4) yes Ni2 2_545 C84 . C86 2_545 72.2(4) yes C85 . C84 . C86 2_545 119.9(6) yes Ni2 . C84 . H841 . 122.5(4) no Ni2 2_545 C84 . H841 . 125.1(4) no C85 . C84 . H841 . 119.4(7) no C86 2_545 C84 . H841 . 120.8(7) no Ni2 . C85 . Ni2 2_545 111.7(3) yes Ni2 . C85 . C84 . 73.0(4) yes Ni2 2_545 C85 . C84 . 73.4(4) yes Ni2 . C85 . C86 . 73.6(4) yes Ni2 2_545 C85 . C86 . 74.3(5) yes C84 . C85 . C86 . 119.6(7) yes Ni2 . C85 . H851 . 124.0(5) no Ni2 2_545 C85 . H851 . 124.3(5) no C84 . C85 . H851 . 120.2(9) no C86 . C85 . H851 . 120.2(8) no Ni2 . C86 . Ni2 2_545 112.2(3) yes Ni2 . C86 . C84 2_545 74.7(4) yes Ni2 2_545 C86 . C84 2_545 72.0(4) yes Ni2 . C86 . C85 . 74.7(5) yes Ni2 2_545 C86 . C85 . 74.4(4) yes C84 2_545 C86 . C85 . 120.5(6) yes Ni2 . C86 . H861 . 121.8(4) no Ni2 2_545 C86 . H861 . 126.0(4) no C84 2_545 C86 . H861 . 120.3(8) no C85 . C86 . H861 . 119.1(8) no Cl1 . C200 . Cl2 . 118.9(6) yes Cl1 . C200 . H2001 . 106.2(8) no Cl2 . C200 . H2001 . 106.3(9) no Cl1 . C200 . H2002 . 106.6(9) no Cl2 . C200 . H2002 . 107.2(9) no H2001 . C200 . H2002 . 111.7(10) no O1 . B1 . O2 . 123.8(3) yes O1 . B1 . C21 . 117.0(3) yes O2 . B1 . C21 . 119.1(3) yes O2 . B2 . O3 . 108.0(2) yes O2 . B2 . C51 . 109.9(2) yes O3 . B2 . C51 . 109.8(2) yes O2 . B2 . C61 . 114.2(3) yes O3 . B2 . C61 . 105.6(2) yes C51 . B2 . C61 . 109.2(2) yes O1 . B3 . O3 . 107.6(2) yes O1 . B3 . C31 . 109.3(2) yes O3 . B3 . C31 . 110.6(2) yes O1 . B3 . C41 . 113.1(3) yes O3 . B3 . C41 . 105.9(2) yes C31 . B3 . C41 . 110.2(3) yes #==END #================================================================ data_complex3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C43 H23 B F24 Ni' _chemical_formula_structural 'C43 H23 B F24 Ni' _chemical_formula_analytical ? _chemical_formula_sum 'C43 H23 B F24 Ni' _chemical_formula_weight 1065.13 _chemical_melting_point ? _chemical_compound_source 'synthesis as described' 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' 'B' 'B' 0.0013 0.0007 '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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.889(5) _cell_length_b 13.191(6) _cell_length_c 14.420(4) _cell_angle_alpha 86.902(6) _cell_angle_beta 90.131(6) _cell_angle_gamma 61.171(6) _cell_volume 2143.55(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 98 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method none _exptl_crystal_F_000 1060 _exptl_absorpt_coefficient_mu 0.590 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.7811 _exptl_absorpt_correction_T_max 0.9481 _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7119 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7119 _reflns_number_observed 5856 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Enraf-Nonius DIP2000 Software - XPRESS' _computing_cell_refinement DENZO _computing_data_reduction 'DENZO & SCALEPACK' _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1998)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1350P)^2^+2.4124P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0026(19) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7114 _refine_ls_number_parameters 710 _refine_ls_number_restraints 840 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_obs 0.0630 _refine_ls_wR_factor_all 0.2037 _refine_ls_wR_factor_obs 0.1873 _refine_ls_goodness_of_fit_all 1.018 _refine_ls_goodness_of_fit_obs 1.069 _refine_ls_restrained_S_all 1.317 _refine_ls_restrained_S_obs 1.384 _refine_ls_shift/esd_max 0.194 _refine_ls_shift/esd_mean 0.005 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ni1 Ni 0.5000 1.0000 0.5000 0.0383(3) Uani 1 d S . Ni2 Ni 0.0000 1.0000 0.0000 0.0357(3) Uani 1 d S . B1 B 0.2330(4) 0.5058(4) 0.2581(3) 0.0265(10) Uani 1 d . . C11 C 0.2598(4) 0.5377(3) 0.1537(3) 0.0286(9) Uani 1 d . . C12 C 0.3346(4) 0.5855(4) 0.1394(3) 0.0308(9) Uani 1 d . . H12 H 0.3768(4) 0.5911(4) 0.1912(3) 0.037 Uiso 1 calc R . C13 C 0.3496(4) 0.6254(4) 0.0516(3) 0.0358(10) Uani 1 d . . C14 C 0.4246(4) 0.6827(4) 0.0409(4) 0.0444(12) Uani 1 d D . F141 F 0.5158(3) 0.6394(4) 0.1007(3) 0.0737(11) Uani 1 d D . F142 F 0.4709(4) 0.6739(4) -0.0418(3) 0.0853(13) Uani 1 d D . F143 F 0.3642(3) 0.7945(3) 0.0540(4) 0.0858(14) Uani 1 d D . C15 C 0.2909(4) 0.6175(4) -0.0262(3) 0.0413(11) Uani 1 d . . H15 H 0.3023(4) 0.6426(4) -0.0865(3) 0.050 Uiso 1 calc R . C16 C 0.2147(5) 0.5716(4) -0.0129(3) 0.0404(11) Uani 1 d . . C17 C 0.1462(6) 0.5665(6) -0.0944(4) 0.061(2) Uani 1 d D . F171 F 0.1992(15) 0.4679(12) -0.1314(11) 0.133(6) Uani 0.494(10) d PDU 1 F172 F 0.1216(15) 0.6467(14) -0.1597(8) 0.103(4) Uani 0.494(10) d PDU 1 F173 F 0.0397(11) 0.5823(17) -0.0749(7) 0.102(4) Uani 0.494(10) d PDU 1 C18 C 0.1995(4) 0.5335(4) 0.0747(3) 0.0338(10) Uani 1 d . 1 H18 H 0.1460(4) 0.5034(4) 0.0813(3) 0.041 Uiso 1 calc R 1 C21 C 0.1298(3) 0.6311(3) 0.2904(3) 0.0261(8) Uani 1 d . 1 C22 C 0.1576(4) 0.7099(3) 0.3289(3) 0.0275(9) Uani 1 d . 1 H22 H 0.2379(4) 0.6861(3) 0.3449(3) 0.033 Uiso 1 calc R 1 C23 C 0.0719(4) 0.8220(4) 0.3444(3) 0.0298(9) Uani 1 d . 1 C24 C 0.1099(4) 0.9025(4) 0.3816(3) 0.0362(10) Uani 1 d D 1 F241 F 0.1495(4) 0.8749(3) 0.4690(2) 0.0690(11) Uani 1 d D 1 F242 F 0.1995(4) 0.9014(3) 0.3357(3) 0.0706(11) Uani 1 d D 1 F243 F 0.0265(3) 1.0116(3) 0.3750(3) 0.0781(13) Uani 1 d D 1 C25 C -0.0466(4) 0.8597(3) 0.3237(3) 0.0306(9) Uani 1 d . 1 H25 H -0.1058(4) 0.9359(3) 0.3356(3) 0.037 Uiso 1 calc R 1 C26 C -0.0761(4) 0.7827(4) 0.2850(3) 0.0310(9) Uani 1 d . 1 C27 C -0.2021(4) 0.8185(4) 0.2604(4) 0.0415(11) Uani 1 d D 1 F271 F -0.2171(3) 0.7911(5) 0.1766(3) 0.0910(15) Uani 1 d D 1 F272 F -0.2723(3) 0.9304(3) 0.2591(5) 0.109(2) Uani 1 d D 1 F273 F -0.2464(3) 0.7699(5) 0.3164(4) 0.100(2) Uani 1 d D 1 C28 C 0.0103(4) 0.6715(3) 0.2683(3) 0.0296(9) Uani 1 d . 1 H28 H -0.0125(4) 0.6210(3) 0.2409(3) 0.035 Uiso 1 calc R 1 C31 C 0.1888(4) 0.4086(3) 0.2635(3) 0.0287(9) Uani 1 d . 1 C32 C 0.1133(4) 0.4061(4) 0.3307(3) 0.0323(9) Uani 1 d . 1 H32 H 0.0798(4) 0.4677(4) 0.3713(3) 0.039 Uiso 1 calc R 1 C33 C 0.0843(4) 0.3176(4) 0.3414(3) 0.0382(11) Uani 1 d . 1 C34 C 0.0039(5) 0.3210(5) 0.4152(4) 0.0515(14) Uani 1 d D 1 F341 F 0.0436(6) 0.3349(7) 0.5008(4) 0.077(2) Uani 0.723(9) d PDU 1 F342 F -0.0991(5) 0.4121(7) 0.4076(6) 0.099(3) Uani 0.723(9) d PDU 1 F343 F -0.0025(10) 0.2270(7) 0.4310(7) 0.111(3) Uani 0.723(9) d PDU 1 C35 C 0.1316(5) 0.2266(4) 0.2834(3) 0.0405(11) Uani 1 d . . H35 H 0.1115(5) 0.1662(4) 0.2894(3) 0.049 Uiso 1 calc R 1 C36 C 0.2086(5) 0.2256(4) 0.2167(3) 0.0402(11) Uani 1 d . . C37 C 0.2640(6) 0.1298(5) 0.1521(4) 0.059(2) Uani 1 d D . F371 F 0.3784(4) 0.0911(4) 0.1420(4) 0.097(2) Uani 1 d D . F372 F 0.2198(6) 0.1601(5) 0.0689(3) 0.146(3) Uani 1 d D . F373 F 0.2599(6) 0.0364(4) 0.1830(4) 0.115(2) Uani 1 d D . C38 C 0.2367(4) 0.3149(4) 0.2063(3) 0.0339(10) Uani 1 d . . H38 H 0.2894(4) 0.3124(4) 0.1594(3) 0.041 Uiso 1 calc R 1 C41 C 0.3504(3) 0.4479(3) 0.3273(3) 0.0252(8) Uani 1 d . . C42 C 0.3444(4) 0.4531(3) 0.4233(3) 0.0265(8) Uani 1 d . . H42 H 0.2701(4) 0.5009(3) 0.4496(3) 0.032 Uiso 1 calc R . C43 C 0.4442(4) 0.3903(3) 0.4826(3) 0.0276(9) Uani 1 d . . C44 C 0.4315(4) 0.3925(4) 0.5854(3) 0.0325(9) Uani 1 d D . F441 F 0.5322(3) 0.3637(4) 0.6311(2) 0.0731(12) Uani 1 d D . F442 F 0.3549(3) 0.4947(3) 0.6127(2) 0.0579(9) Uani 1 d D . F443 F 0.3948(4) 0.3204(3) 0.6172(2) 0.0701(11) Uani 1 d D . C45 C 0.5535(4) 0.3196(4) 0.4462(3) 0.0296(9) Uani 1 d . . H45 H 0.6218(4) 0.2769(4) 0.4858(3) 0.036 Uiso 1 calc R . C46 C 0.5609(4) 0.3129(3) 0.3510(3) 0.0295(9) Uani 1 d . . C47 C 0.6766(4) 0.2347(4) 0.3098(4) 0.0439(12) Uani 1 d D . F471 F 0.6653(6) 0.1958(8) 0.2294(4) 0.110(4) Uani 0.736(9) d PDU 1 F472 F 0.7352(6) 0.1357(5) 0.3584(4) 0.077(2) Uani 0.736(9) d PDU 1 F473 F 0.7468(7) 0.2755(7) 0.3043(11) 0.147(4) Uani 0.736(9) d PDU 1 C48 C 0.4617(4) 0.3750(3) 0.2927(3) 0.0274(9) Uani 1 d . . H48 H 0.4696(4) 0.3678(3) 0.2275(3) 0.033 Uiso 1 calc R . C51 C 0.4476(11) 0.9887(11) 0.3693(8) 0.115(3) Uani 1 d U . H51 H 0.5008(11) 0.9245(11) 0.3360(8) 0.138 Uiso 1 calc R . C52 C 0.4533(9) 1.0602(10) 0.3603(7) 0.092(3) Uani 1 d U . H52 H 0.5011(9) 1.0645(10) 0.3119(7) 0.111 Uiso 1 calc R . C53 C 0.4037(7) 1.1425(6) 0.4067(5) 0.067(2) Uani 1 d U . H53 H 0.4162(7) 1.2077(6) 0.3986(5) 0.080 Uiso 1 calc R . C54 C 0.3338(7) 1.1382(7) 0.4670(6) 0.082(2) Uani 1 d U . H54 H 0.2921(7) 1.1988(7) 0.5073(6) 0.098 Uiso 1 calc R . C55 C 0.3237(6) 1.0453(8) 0.4694(6) 0.078(2) Uani 1 d U . H55 H 0.2729(6) 1.0325(8) 0.5102(6) 0.094 Uiso 1 calc R . C56 C 0.3852(8) 0.9757(7) 0.4145(7) 0.079(2) Uani 1 d U . H56 H 0.3794(8) 0.9070(7) 0.4101(7) 0.094 Uiso 1 calc R . C61 C 0.0701(7) 0.9386(7) 0.1322(4) 0.069(2) Uani 1 d . . H61 H 0.1472(7) 0.9236(7) 0.1509(4) 0.083 Uiso 1 calc R . C62 C -0.0275(11) 1.0392(7) 0.1382(5) 0.089(3) Uani 1 d . . H62 H -0.0309(11) 1.1061(7) 0.1628(5) 0.107 Uiso 1 calc R . C63 C -0.1195(7) 1.0325(9) 0.1047(6) 0.098(4) Uani 1 d . . H63 H -0.1996(7) 1.0926(9) 0.1012(6) 0.118 Uiso 1 calc R . C64 C -0.0762(10) 0.9187(11) 0.0751(5) 0.099(4) Uani 1 d . . H64 H -0.1205(10) 0.8876(11) 0.0468(5) 0.119 Uiso 1 calc R . C65 C 0.0455(7) 0.8618(5) 0.0965(4) 0.063(2) Uani 1 d . . H65 H 0.1002(7) 0.7831(5) 0.0872(4) 0.076 Uiso 1 calc R . F17A F 0.2047(12) 0.5489(16) -0.1724(6) 0.102(4) Uani 0.506(10) d PDU 2 F17C F 0.1175(16) 0.4873(14) -0.0873(7) 0.101(4) Uani 0.506(10) d PDU 2 F17B F 0.0494(14) 0.6644(13) -0.1089(11) 0.147(6) Uani 0.506(10) d PDU 2 F34A F -0.0451(17) 0.4090(15) 0.4607(13) 0.096(5) Uani 0.277(9) d PDU 2 F34B F -0.0834(13) 0.3042(17) 0.3824(12) 0.091(5) Uani 0.277(9) d PDU 2 F34C F 0.0553(15) 0.2424(16) 0.4778(11) 0.099(6) Uani 0.277(9) d PDU 2 F47A F 0.6850(18) 0.1378(15) 0.2947(15) 0.118(7) Uani 0.264(9) d PDU 2 F47B F 0.7649(11) 0.2100(19) 0.3641(11) 0.099(7) Uani 0.264(9) d PDU 2 F47C F 0.6966(13) 0.2750(14) 0.2389(10) 0.086(7) Uani 0.264(9) d PDU 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 Ni1 0.0344(5) 0.0308(5) 0.0493(6) 0.0092(4) -0.0144(4) -0.0167(4) Ni2 0.0361(5) 0.0339(5) 0.0257(5) 0.0042(3) 0.0038(3) -0.0085(4) B1 0.026(2) 0.022(2) 0.029(3) 0.000(2) -0.001(2) -0.010(2) C11 0.024(2) 0.021(2) 0.031(2) -0.001(2) 0.000(2) -0.003(2) C12 0.029(2) 0.027(2) 0.029(2) 0.001(2) 0.001(2) -0.009(2) C13 0.035(2) 0.027(2) 0.037(3) 0.003(2) 0.006(2) -0.008(2) C14 0.041(3) 0.042(3) 0.043(3) 0.008(2) 0.007(2) -0.016(2) F141 0.057(2) 0.089(3) 0.086(3) 0.028(2) -0.013(2) -0.047(2) F142 0.108(3) 0.116(3) 0.062(3) -0.004(2) 0.034(2) -0.078(3) F143 0.062(2) 0.041(2) 0.158(4) -0.009(2) 0.024(2) -0.027(2) C15 0.043(3) 0.038(3) 0.030(3) 0.005(2) 0.007(2) -0.011(2) C16 0.045(3) 0.037(2) 0.029(2) 0.002(2) -0.004(2) -0.012(2) C17 0.072(4) 0.071(4) 0.036(3) 0.005(3) -0.013(3) -0.033(4) F171 0.149(10) 0.127(9) 0.095(10) -0.047(7) -0.045(8) -0.042(9) F172 0.139(10) 0.146(9) 0.056(6) 0.062(6) -0.064(6) -0.101(8) F173 0.092(7) 0.186(11) 0.057(5) 0.027(7) -0.037(5) -0.094(7) C18 0.033(2) 0.030(2) 0.031(2) 0.001(2) -0.002(2) -0.011(2) C21 0.025(2) 0.024(2) 0.027(2) 0.0017(15) 0.002(2) -0.010(2) C22 0.026(2) 0.027(2) 0.024(2) 0.004(2) 0.000(2) -0.010(2) C23 0.035(2) 0.027(2) 0.025(2) 0.002(2) 0.001(2) -0.013(2) C24 0.038(2) 0.027(2) 0.037(3) -0.001(2) -0.004(2) -0.010(2) F241 0.109(3) 0.075(2) 0.039(2) 0.002(2) -0.022(2) -0.057(2) F242 0.087(3) 0.082(3) 0.079(3) -0.030(2) 0.023(2) -0.068(2) F243 0.068(2) 0.028(2) 0.123(3) -0.015(2) -0.032(2) -0.011(2) C25 0.028(2) 0.024(2) 0.032(2) 0.002(2) 0.006(2) -0.006(2) C26 0.026(2) 0.031(2) 0.033(2) 0.007(2) 0.001(2) -0.011(2) C27 0.029(2) 0.034(2) 0.057(3) 0.000(2) 0.002(2) -0.013(2) F271 0.039(2) 0.136(4) 0.083(3) -0.024(3) -0.014(2) -0.029(2) F272 0.029(2) 0.045(2) 0.235(6) -0.015(3) -0.021(3) -0.003(2) F273 0.050(2) 0.144(4) 0.117(4) 0.053(3) -0.011(2) -0.063(3) C28 0.029(2) 0.026(2) 0.033(2) 0.002(2) 0.001(2) -0.014(2) C31 0.026(2) 0.026(2) 0.030(2) 0.004(2) -0.006(2) -0.010(2) C32 0.030(2) 0.028(2) 0.037(2) 0.005(2) -0.004(2) -0.013(2) C33 0.033(2) 0.039(3) 0.042(3) 0.013(2) -0.009(2) -0.019(2) C34 0.044(3) 0.053(3) 0.061(4) 0.010(3) 0.004(3) -0.027(3) F341 0.085(4) 0.117(6) 0.051(3) -0.006(3) 0.016(3) -0.064(4) F342 0.040(3) 0.112(5) 0.101(5) 0.044(4) 0.020(3) -0.008(3) F343 0.169(8) 0.090(4) 0.128(7) -0.029(4) 0.079(6) -0.103(5) C35 0.049(3) 0.040(3) 0.043(3) 0.007(2) -0.015(2) -0.031(2) C36 0.050(3) 0.034(2) 0.039(3) 0.002(2) -0.013(2) -0.023(2) C37 0.084(5) 0.052(3) 0.054(4) -0.014(3) -0.003(3) -0.041(3) F371 0.091(3) 0.079(3) 0.124(4) -0.059(3) 0.036(3) -0.040(3) F372 0.185(6) 0.095(4) 0.077(3) -0.042(3) -0.059(4) 0.001(4) F373 0.179(5) 0.068(3) 0.134(4) -0.049(3) 0.072(4) -0.084(3) C38 0.038(2) 0.028(2) 0.034(2) 0.000(2) -0.007(2) -0.015(2) C41 0.025(2) 0.021(2) 0.029(2) 0.0013(15) 0.001(2) -0.012(2) C42 0.025(2) 0.022(2) 0.031(2) -0.002(2) 0.001(2) -0.011(2) C43 0.029(2) 0.024(2) 0.032(2) 0.002(2) -0.002(2) -0.015(2) C44 0.033(2) 0.035(2) 0.031(2) 0.000(2) 0.000(2) -0.019(2) F441 0.045(2) 0.131(3) 0.034(2) -0.001(2) -0.0068(14) -0.036(2) F442 0.074(2) 0.046(2) 0.036(2) -0.0079(13) 0.005(2) -0.015(2) F443 0.129(3) 0.081(2) 0.039(2) -0.002(2) 0.017(2) -0.081(3) C45 0.025(2) 0.028(2) 0.034(2) 0.006(2) -0.005(2) -0.012(2) C46 0.026(2) 0.024(2) 0.035(2) 0.003(2) 0.002(2) -0.009(2) C47 0.032(3) 0.032(3) 0.055(3) 0.002(2) 0.004(2) -0.006(2) F471 0.058(3) 0.132(6) 0.042(3) -0.037(4) -0.004(3) 0.035(4) F472 0.069(4) 0.045(3) 0.043(3) 0.006(2) 0.014(3) 0.029(3) F473 0.070(5) 0.082(5) 0.310(12) -0.068(6) 0.101(7) -0.049(4) C48 0.028(2) 0.023(2) 0.028(2) 0.001(2) 0.001(2) -0.010(2) C51 0.097(5) 0.095(5) 0.092(5) -0.002(5) -0.034(5) 0.001(5) C52 0.073(4) 0.094(5) 0.078(4) 0.021(5) -0.018(4) -0.018(4) C53 0.066(3) 0.056(3) 0.082(4) 0.024(3) -0.036(3) -0.036(3) C54 0.056(3) 0.077(4) 0.079(4) -0.002(4) -0.024(3) -0.006(3) C55 0.048(3) 0.088(4) 0.090(5) 0.024(4) -0.020(3) -0.029(3) C56 0.074(4) 0.061(3) 0.109(6) 0.020(4) -0.043(4) -0.042(3) C61 0.076(4) 0.106(6) 0.032(3) 0.020(3) -0.010(3) -0.051(4) C62 0.166(10) 0.061(4) 0.035(4) -0.006(3) 0.027(5) -0.049(6) C63 0.056(4) 0.107(7) 0.054(4) 0.039(4) 0.029(4) 0.019(4) C64 0.150(8) 0.201(11) 0.029(3) 0.012(4) -0.002(4) -0.153(9) C65 0.088(5) 0.039(3) 0.043(3) 0.009(2) 0.022(3) -0.016(3) F17A 0.138(8) 0.168(10) 0.025(4) -0.012(5) 0.000(5) -0.093(8) F17C 0.161(11) 0.137(9) 0.055(6) 0.021(6) -0.046(7) -0.116(8) F17B 0.120(9) 0.148(10) 0.103(10) -0.001(8) -0.076(7) -0.011(9) F34A 0.101(11) 0.101(10) 0.103(11) -0.015(9) 0.045(9) -0.062(9) F34B 0.062(8) 0.130(11) 0.105(10) 0.021(9) 0.012(7) -0.068(8) F34C 0.078(9) 0.129(11) 0.077(10) 0.048(9) 0.013(8) -0.045(9) F47A 0.090(11) 0.084(10) 0.145(13) -0.027(11) 0.048(11) -0.012(9) F47B 0.021(6) 0.142(13) 0.066(9) -0.026(9) -0.005(6) 0.018(9) F47C 0.048(8) 0.082(9) 0.038(8) 0.039(7) 0.040(6) 0.036(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Ni1 C51 2.037(11) 2_676 ? Ni1 C51 2.037(11) . ? Ni1 C54 2.068(7) . ? Ni1 C54 2.068(7) 2_676 ? Ni1 C56 2.074(7) 2_676 ? Ni1 C56 2.074(7) . ? Ni1 C53 2.086(6) . ? Ni1 C53 2.086(6) 2_676 ? Ni1 C55 2.092(7) . ? Ni1 C55 2.092(7) 2_676 ? Ni1 C52 2.100(9) 2_676 ? Ni1 C52 2.100(9) . ? Ni2 C64 2.045(6) 2_575 ? Ni2 C64 2.045(6) . ? Ni2 C61 2.055(6) . ? Ni2 C61 2.055(6) 2_575 ? Ni2 C63 2.069(6) 2_575 ? Ni2 C63 2.069(6) . ? Ni2 C65 2.072(5) 2_575 ? Ni2 C65 2.072(5) . ? Ni2 C62 2.074(6) 2_575 ? Ni2 C62 2.074(6) . ? B1 C11 1.625(6) . ? B1 C41 1.632(6) . ? B1 C31 1.633(6) . ? B1 C21 1.638(6) . ? C11 C12 1.393(6) . ? C11 C18 1.396(6) . ? C12 C13 1.395(6) . ? C13 C15 1.388(7) . ? C13 C14 1.491(7) . ? C14 F143 1.319(6) . ? C14 F142 1.320(7) . ? C14 F141 1.322(6) . ? C15 C16 1.389(7) . ? C16 C18 1.382(7) . ? C16 C17 1.492(7) . ? C17 F17C 1.266(11) . ? C17 F171 1.290(13) . ? C17 F172 1.294(10) . ? C17 F17B 1.297(13) . ? C17 F173 1.319(12) . ? C17 F17A 1.323(11) . ? C21 C22 1.391(6) . ? C21 C28 1.395(6) . ? C22 C23 1.385(6) . ? C23 C25 1.385(6) . ? C23 C24 1.488(6) . ? C24 F243 1.315(5) . ? C24 F241 1.323(6) . ? C24 F242 1.327(6) . ? C25 C26 1.386(6) . ? C26 C28 1.383(6) . ? C26 C27 1.492(6) . ? C27 F273 1.298(6) . ? C27 F272 1.307(6) . ? C27 F271 1.321(7) . ? C31 C32 1.386(6) . ? C31 C38 1.402(6) . ? C32 C33 1.389(6) . ? C33 C35 1.384(7) . ? C33 C34 1.474(8) . ? C34 F343 1.290(8) . ? C34 F342 1.290(8) . ? C34 F341 1.390(8) . ? C35 C36 1.379(8) . ? C36 C38 1.391(7) . ? C36 C37 1.494(8) . ? C37 F372 1.284(7) . ? C37 F373 1.312(7) . ? C37 F371 1.319(8) . ? C41 C42 1.391(6) . ? C41 C48 1.399(6) . ? C42 C43 1.401(6) . ? C43 C45 1.385(6) . ? C43 C44 1.493(6) . ? C44 F442 1.312(5) . ? C44 F443 1.314(5) . ? C44 F441 1.325(5) . ? C45 C46 1.381(6) . ? C46 C48 1.386(6) . ? C46 C47 1.493(6) . ? C47 F47C 1.211(12) . ? C47 F473 1.257(8) . ? C47 F47A 1.26(2) . ? C47 F47B 1.275(14) . ? C47 F472 1.310(7) . ? C47 F471 1.329(8) . ? C51 C52 0.98(2) . ? C51 C56 1.11(2) . ? C51 C53 1.933(15) . ? C51 C55 2.04(2) . ? C52 C53 1.202(13) . ? C52 C56 1.863(14) . ? C53 C54 1.273(11) . ? C54 C55 1.293(12) . ? C55 C56 1.215(12) . ? C61 C62 1.324(12) . ? C61 C65 1.325(10) . ? C62 C63 1.324(13) . ? C63 C64 1.417(13) . ? C64 C65 1.399(12) . ? 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 C51 Ni1 C51 179.999(3) 2_676 . ? C51 Ni1 C54 110.0(4) 2_676 . ? C51 Ni1 C54 70.0(4) . . ? C51 Ni1 C54 70.0(4) 2_676 2_676 ? C51 Ni1 C54 110.0(4) . 2_676 ? C54 Ni1 C54 180.0 . 2_676 ? C51 Ni1 C56 31.2(4) 2_676 2_676 ? C51 Ni1 C56 148.8(4) . 2_676 ? C54 Ni1 C56 119.0(3) . 2_676 ? C54 Ni1 C56 61.0(3) 2_676 2_676 ? C51 Ni1 C56 148.8(4) 2_676 . ? C51 Ni1 C56 31.2(4) . . ? C54 Ni1 C56 61.0(3) . . ? C54 Ni1 C56 119.0(3) 2_676 . ? C56 Ni1 C56 179.998(3) 2_676 . ? C51 Ni1 C53 124.1(4) 2_676 . ? C51 Ni1 C53 55.9(4) . . ? C54 Ni1 C53 35.7(3) . . ? C54 Ni1 C53 144.3(3) 2_676 . ? C56 Ni1 C53 112.2(3) 2_676 . ? C56 Ni1 C53 67.8(3) . . ? C51 Ni1 C53 55.9(4) 2_676 2_676 ? C51 Ni1 C53 124.1(4) . 2_676 ? C54 Ni1 C53 144.3(3) . 2_676 ? C54 Ni1 C53 35.7(3) 2_676 2_676 ? C56 Ni1 C53 67.8(3) 2_676 2_676 ? C56 Ni1 C53 112.2(3) . 2_676 ? C53 Ni1 C53 179.999(1) . 2_676 ? C51 Ni1 C55 120.8(5) 2_676 . ? C51 Ni1 C55 59.2(5) . . ? C54 Ni1 C55 36.2(3) . . ? C54 Ni1 C55 143.8(3) 2_676 . ? C56 Ni1 C55 146.1(3) 2_676 . ? C56 Ni1 C55 33.9(3) . . ? C53 Ni1 C55 62.4(3) . . ? C53 Ni1 C55 117.6(3) 2_676 . ? C51 Ni1 C55 59.2(5) 2_676 2_676 ? C51 Ni1 C55 120.8(5) . 2_676 ? C54 Ni1 C55 143.8(3) . 2_676 ? C54 Ni1 C55 36.2(3) 2_676 2_676 ? C56 Ni1 C55 33.9(3) 2_676 2_676 ? C56 Ni1 C55 146.1(3) . 2_676 ? C53 Ni1 C55 117.6(3) . 2_676 ? C53 Ni1 C55 62.4(3) 2_676 2_676 ? C55 Ni1 C55 180.0 . 2_676 ? C51 Ni1 C52 27.4(4) 2_676 2_676 ? C51 Ni1 C52 152.6(4) . 2_676 ? C54 Ni1 C52 119.2(4) . 2_676 ? C54 Ni1 C52 60.8(4) 2_676 2_676 ? C56 Ni1 C52 53.0(4) 2_676 2_676 ? C56 Ni1 C52 127.0(4) . 2_676 ? C53 Ni1 C52 146.6(3) . 2_676 ? C53 Ni1 C52 33.4(3) 2_676 2_676 ? C55 Ni1 C52 111.3(4) . 2_676 ? C55 Ni1 C52 68.7(4) 2_676 2_676 ? C51 Ni1 C52 152.6(4) 2_676 . ? C51 Ni1 C52 27.4(4) . . ? C54 Ni1 C52 60.8(4) . . ? C54 Ni1 C52 119.2(4) 2_676 . ? C56 Ni1 C52 127.0(4) 2_676 . ? C56 Ni1 C52 53.0(4) . . ? C53 Ni1 C52 33.4(3) . . ? C53 Ni1 C52 146.6(3) 2_676 . ? C55 Ni1 C52 68.7(4) . . ? C55 Ni1 C52 111.3(4) 2_676 . ? C52 Ni1 C52 180.000(2) 2_676 . ? C64 Ni2 C64 180.000(1) 2_575 . ? C64 Ni2 C61 115.4(3) 2_575 . ? C64 Ni2 C61 64.6(3) . . ? C64 Ni2 C61 64.6(3) 2_575 2_575 ? C64 Ni2 C61 115.4(3) . 2_575 ? C61 Ni2 C61 179.999(2) . 2_575 ? C64 Ni2 C63 40.3(4) 2_575 2_575 ? C64 Ni2 C63 139.7(4) . 2_575 ? C61 Ni2 C63 116.7(3) . 2_575 ? C61 Ni2 C63 63.3(3) 2_575 2_575 ? C64 Ni2 C63 139.7(4) 2_575 . ? C64 Ni2 C63 40.3(4) . . ? C61 Ni2 C63 63.3(3) . . ? C61 Ni2 C63 116.7(3) 2_575 . ? C63 Ni2 C63 180.0 2_575 . ? C64 Ni2 C65 39.7(4) 2_575 2_575 ? C64 Ni2 C65 140.3(4) . 2_575 ? C61 Ni2 C65 142.5(3) . 2_575 ? C61 Ni2 C65 37.5(3) 2_575 2_575 ? C63 Ni2 C65 65.5(3) 2_575 2_575 ? C63 Ni2 C65 114.5(3) . 2_575 ? C64 Ni2 C65 140.3(4) 2_575 . ? C64 Ni2 C65 39.7(4) . . ? C61 Ni2 C65 37.5(3) . . ? C61 Ni2 C65 142.5(3) 2_575 . ? C63 Ni2 C65 114.5(3) 2_575 . ? C63 Ni2 C65 65.5(3) . . ? C65 Ni2 C65 180.0 2_575 . ? C64 Ni2 C62 64.7(3) 2_575 2_575 ? C64 Ni2 C62 115.3(3) . 2_575 ? C61 Ni2 C62 142.6(3) . 2_575 ? C61 Ni2 C62 37.4(3) 2_575 2_575 ? C63 Ni2 C62 37.3(4) 2_575 2_575 ? C63 Ni2 C62 142.7(4) . 2_575 ? C65 Ni2 C62 63.4(3) 2_575 2_575 ? C65 Ni2 C62 116.6(3) . 2_575 ? C64 Ni2 C62 115.3(3) 2_575 . ? C64 Ni2 C62 64.7(3) . . ? C61 Ni2 C62 37.4(3) . . ? C61 Ni2 C62 142.6(3) 2_575 . ? C63 Ni2 C62 142.7(4) 2_575 . ? C63 Ni2 C62 37.3(4) . . ? C65 Ni2 C62 116.6(3) 2_575 . ? C65 Ni2 C62 63.4(3) . . ? C62 Ni2 C62 179.999(1) 2_575 . ? C11 B1 C41 112.9(3) . . ? C11 B1 C31 114.0(3) . . ? C41 B1 C31 103.1(3) . . ? C11 B1 C21 102.8(3) . . ? C41 B1 C21 113.0(3) . . ? C31 B1 C21 111.5(3) . . ? C12 C11 C18 115.8(4) . . ? C12 C11 B1 120.7(4) . . ? C18 C11 B1 123.0(4) . . ? C11 C12 C13 122.2(4) . . ? C15 C13 C12 120.8(5) . . ? C15 C13 C14 119.1(4) . . ? C12 C13 C14 120.1(4) . . ? F143 C14 F142 106.4(5) . . ? F143 C14 F141 106.0(5) . . ? F142 C14 F141 105.2(5) . . ? F143 C14 C13 111.8(4) . . ? F142 C14 C13 113.7(5) . . ? F141 C14 C13 113.1(4) . . ? C13 C15 C16 117.6(4) . . ? C18 C16 C15 121.1(5) . . ? C18 C16 C17 119.9(5) . . ? C15 C16 C17 119.0(5) . . ? F171 C17 F172 107.6(10) . . ? F17C C17 F17B 107.4(11) . . ? F171 C17 F173 105.6(11) . . ? F172 C17 F173 101.5(9) . . ? F17C C17 F17A 104.8(9) . . ? F17B C17 F17A 106.0(10) . . ? F17C C17 C16 115.0(6) . . ? F171 C17 C16 112.2(7) . . ? F172 C17 C16 114.8(7) . . ? F17B C17 C16 110.2(7) . . ? F173 C17 C16 114.2(7) . . ? F17A C17 C16 112.8(7) . . ? C16 C18 C11 122.4(5) . . ? C22 C21 C28 116.1(4) . . ? C22 C21 B1 121.7(4) . . ? C28 C21 B1 121.6(4) . . ? C23 C22 C21 122.2(4) . . ? C22 C23 C25 120.8(4) . . ? C22 C23 C24 118.7(4) . . ? C25 C23 C24 120.5(4) . . ? F243 C24 F241 108.3(4) . . ? F243 C24 F242 104.7(4) . . ? F241 C24 F242 104.4(4) . . ? F243 C24 C23 113.4(4) . . ? F241 C24 C23 113.1(4) . . ? F242 C24 C23 112.1(4) . . ? C23 C25 C26 118.0(4) . . ? C28 C26 C25 120.8(4) . . ? C28 C26 C27 118.7(4) . . ? C25 C26 C27 120.5(4) . . ? F273 C27 F272 107.4(5) . . ? F273 C27 F271 105.3(5) . . ? F272 C27 F271 103.9(5) . . ? F273 C27 C26 112.6(4) . . ? F272 C27 C26 113.6(4) . . ? F271 C27 C26 113.3(4) . . ? C26 C28 C21 122.2(4) . . ? C32 C31 C38 116.1(4) . . ? C32 C31 B1 122.5(4) . . ? C38 C31 B1 121.0(4) . . ? C31 C32 C33 122.9(4) . . ? C35 C33 C32 119.9(5) . . ? C35 C33 C34 120.6(4) . . ? C32 C33 C34 119.4(5) . . ? F343 C34 F342 112.5(7) . . ? F343 C34 F341 102.3(7) . . ? F342 C34 F341 100.7(7) . . ? F343 C34 C33 115.5(6) . . ? F342 C34 C33 113.5(5) . . ? F341 C34 C33 110.8(5) . . ? C36 C35 C33 118.6(4) . . ? C35 C36 C38 121.0(5) . . ? C35 C36 C37 121.6(5) . . ? C38 C36 C37 117.4(5) . . ? F372 C37 F373 110.1(6) . . ? F372 C37 F371 104.0(7) . . ? F373 C37 F371 102.7(6) . . ? F372 C37 C36 113.1(5) . . ? F373 C37 C36 112.3(6) . . ? F371 C37 C36 113.9(5) . . ? C36 C38 C31 121.4(5) . . ? C42 C41 C48 116.4(4) . . ? C42 C41 B1 122.8(3) . . ? C48 C41 B1 120.1(4) . . ? C41 C42 C43 122.1(4) . . ? C45 C43 C42 120.2(4) . . ? C45 C43 C44 119.7(4) . . ? C42 C43 C44 120.0(4) . . ? F442 C44 F443 106.0(4) . . ? F442 C44 F441 105.6(4) . . ? F443 C44 F441 106.8(4) . . ? F442 C44 C43 113.4(4) . . ? F443 C44 C43 111.7(4) . . ? F441 C44 C43 112.8(4) . . ? C46 C45 C43 118.4(4) . . ? C45 C46 C48 121.2(4) . . ? C45 C46 C47 119.7(4) . . ? C48 C46 C47 119.1(4) . . ? F47C C47 F47A 108.9(13) . . ? F47C C47 F47B 104.5(12) . . ? F47A C47 F47B 104.4(13) . . ? F473 C47 F472 105.0(7) . . ? F473 C47 F471 111.3(8) . . ? F472 C47 F471 99.4(6) . . ? F47C C47 C46 114.2(7) . . ? F473 C47 C46 114.2(5) . . ? F47A C47 C46 111.4(10) . . ? F47B C47 C46 112.7(8) . . ? F472 C47 C46 112.4(5) . . ? F471 C47 C46 113.4(5) . . ? C46 C48 C41 121.7(4) . . ? C52 C51 C56 126.2(16) . . ? C52 C51 C53 30.9(9) . . ? C56 C51 C53 95.7(9) . . ? C52 C51 C55 96.7(12) . . ? C56 C51 C55 29.9(7) . . ? C53 C51 C55 65.9(5) . . ? C52 C51 Ni1 79.8(10) . . ? C56 C51 Ni1 76.3(7) . . ? C53 C51 Ni1 63.3(4) . . ? C55 C51 Ni1 61.7(4) . . ? C51 C52 C53 124.2(15) . . ? C51 C52 C56 28.6(10) . . ? C53 C52 C56 96.0(8) . . ? C51 C52 Ni1 72.8(9) . . ? C53 C52 Ni1 72.7(6) . . ? C56 C52 Ni1 62.8(4) . . ? C52 C53 C54 117.0(9) . . ? C52 C53 C51 24.8(7) . . ? C54 C53 C51 92.2(7) . . ? C52 C53 Ni1 73.9(5) . . ? C54 C53 Ni1 71.4(4) . . ? C51 C53 Ni1 60.8(4) . . ? C53 C54 C55 114.9(8) . . ? C53 C54 Ni1 72.9(4) . . ? C55 C54 Ni1 72.9(4) . . ? C56 C55 C54 113.8(9) . . ? C56 C55 C51 27.0(6) . . ? C54 C55 C51 86.9(7) . . ? C56 C55 Ni1 72.3(5) . . ? C54 C55 Ni1 70.9(4) . . ? C51 C55 Ni1 59.1(4) . . ? C51 C56 C55 123.1(11) . . ? C51 C56 C52 25.2(8) . . ? C55 C56 C52 98.2(7) . . ? C51 C56 Ni1 72.6(7) . . ? C55 C56 Ni1 73.8(5) . . ? C52 C56 Ni1 64.2(4) . . ? C62 C61 C65 110.8(7) . . ? C62 C61 Ni2 72.1(4) . . ? C65 C61 Ni2 71.9(4) . . ? C63 C62 C61 109.7(7) . . ? C63 C62 Ni2 71.2(4) . . ? C61 C62 Ni2 70.5(4) . . ? C62 C63 C64 107.1(7) . . ? C62 C63 Ni2 71.6(4) . . ? C64 C63 Ni2 69.0(4) . . ? C65 C64 C63 105.4(7) . . ? C65 C64 Ni2 71.2(4) . . ? C63 C64 Ni2 70.7(4) . . ? C61 C65 C64 107.0(7) . . ? C61 C65 Ni2 70.6(3) . . ? C64 C65 Ni2 69.1(4) . . ? _refine_diff_density_max 1.024 _refine_diff_density_min -0.791 _refine_diff_density_rms 0.081 #==END