#============================================================================== data_global #============================================================================== _publ_contact_author 'Simon Aldridge' _publ_contact_author_email Simon.Aldridge@chem.ox.ac.uk loop_ _publ_author_name _publ_author_address 'Pierce, Glesni A.' ; Inorganic Chemistry, University of Oxford, South Parks Road, Oxford OX1 3QR. UK. ; 'Vidovic, Drasko' ; Inorganic Chemistry, University of Oxford, South Parks Road, Oxford OX1 3QR. UK. ; 'Kays, Deborah L.' ; Inorganic Chemistry, University of Oxford, South Parks Road, Oxford OX1 3QR. UK. ; 'Coombs, Natalie D.' ; Inorganic Chemistry, University of Oxford, South Parks Road, Oxford OX1 3QR. UK. ; 'Thompson, Amber L.' ; Chemical Crystallography Department, Inorganic Chemistry, University of Oxford, South Parks Road, Oxford OX1 3QR. UK. ; 'Willock, David J.' ; Cardiff School of Chemistry, Main Building, Park Place, Cardiff, CF10 3AT. UK. ; 'Jemmis, Eluvathingal D.' ; Department of Inorganic and Physical Chemistry, Indian Institute of Science, Bangalore, 560 012. India. ; 'De, Susmita' ; Department of Inorganic and Physical Chemistry, Indian Institute of Science, Bangalore, 560 012. India. ; 'Aldridge, Simon' ; Inorganic Chemistry, University of Oxford, South Parks Road, Oxford OX1 3QR. UK. ; _journal_name_full 'Organometallics' _journal_volume '?' _journal_page_first '?' _journal_page_last '?' _journal_year '2008' _ccdc_journal_depnumber '?' _publ_section_title ; Half-sandwich group 8 borylene complexes: synthetic and structural studies, and oxygen atom abstraction chemistry ; _publ_section_abstract ; Cationic terminal borylene complexes, synthesized by halide abstraction, offer a versatile platform on which to gauge the effects on the electronic structure of the metal-ligand bond brought about by variation in the borylene substituent and the metal/ligand framework. While the borylene substituent exerts a strong influence on boron-centred electrophilicity and hence on metal-ligand \p character and bond length (e.g. from 1.792(8) \%A for [Cp^*^Fe(CO)~2~(BMes)]^+^ to 2.049(4) \%A for [CpFe(CO)~2~{B(NCy~2~)(4-pic)}]^+^), much smaller changes are effected by changes in the metal/ligand set. Introduction of stronger \p donor ruthenium and/or phosphine containing fragments is readily brought about by extension of the halide abstraction approach; phosphines are readily introduced by carbonyl ligand substitution at the boryl precursor stage. Thus, the novel systems [CpRu(CO)~2~{B(NCy~2~)}]^+^[BArf~4~]^-^ and [CpM(CO)(PMe~3~){B(NCy~2~)}]^+^[BArf~4~]^-^ (M = Fe, Ru) (have been synthesized and structurally characterized. The utility of cationic complexes containing formally sub-valent boron based ligands in oxygen atom abstraction chemistry has been demonstrated by the conversion of a range of isocyanates, RNCO, to the corresponding (metal-coordinated) isonitriles, [CpFe(CO)~2~(CNR)]^+^. Moreover, with a view to modeling potential intermediates, the mechanism of related chemistry with carbodiimide substrates, R'NCNR', has been investigated by structural and in situ ESI-MS approaches. While such studies reveal the formation of a novel spirocyclic boronium complex, [CpFe(CO)~2~C(NCy)~2~B(NCy)~2~CNCy~2~]^+^[BArf~4~]^-^ (for R' = Cy), by a double insertion process, DFT studies imply that the analogous product of isocyanate insertion is unlikely to be an intermediate on the pathway to isonitrile formation. The presence of a number of facile competing reaction pathways, and the thermodynamic stability of the spirocyclic product mean that the product distribution is better explained in terms of competing pathways, rather than differing extents of reaction along similar trajectories. ; #============================================================================== data_2 #============================================================================== _audit_creation_date 07-11-30 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title '5622' _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 11.8422(2) _cell_length_b 11.8546(2) _cell_length_c 14.4183(2) _cell_angle_alpha 90 _cell_angle_beta 98.7952(7) _cell_angle_gamma 90 _cell_volume 2000.31(6) _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x,y+1/2,-z+1/2' 'x,-y+1/2,z+1/2' 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 C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ru -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C19 H27 B1 Cl1 N1 O2 Ru1 # Dc = 1.49 Fooo = 920.00 Mu = 9.29 M = 448.76 # Found Formula = C19 H27 B1 Cl1 N1 O2 Ru1 # Dc = 1.49 FOOO = 920.00 Mu = 9.29 M = 448.76 _chemical_formula_sum 'C19 H27 B1 Cl1 N1 O2 Ru1' _chemical_formula_moiety 'C19 H27 B1 Cl1 N1 O2 Ru1' _chemical_compound_source . _chemical_formula_weight 448.76 _cell_measurement_reflns_used 4743 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description 'block' _exptl_crystal_colour 'clear_pale_yellow' _exptl_crystal_size_min 0.20 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_max 0.43 _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 0.929 # Sheldrick geometric approximatio 0.70 0.86 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 0.83 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type 'Area' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 27804 _reflns_number_total 4565 _diffrn_reflns_av_R_equivalents 0.033 # Number of reflections with Friedels Law is 4565 # Number of reflections without Friedels Law is 9118 # Theoretical number of reflections is about 4592 _diffrn_reflns_theta_min 5.132 _diffrn_reflns_theta_max 27.494 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.944 _diffrn_measured_fraction_theta_full 0.993 _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 -18 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.71 _refine_diff_density_max 0.68 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 4565 _refine_ls_number_restraints 0 _refine_ls_number_parameters 226 _oxford_refine_ls_R_factor_ref 0.0312 _refine_ls_wR_factor_ref 0.0648 _refine_ls_goodness_of_fit_ref 0.9859 _refine_ls_shift/su_max 0.001929 # The values computed from all data _oxford_reflns_number_all 4565 _refine_ls_R_factor_all 0.0312 _refine_ls_wR_factor_all 0.0648 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3984 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_gt 0.0636 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration '.' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 0.71P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Ru1 Ru 0.680534(11) 0.339532(12) 0.855283(9) 0.0187 1.0000 Uani . . . . . . . C2 C 0.83438(16) 0.30028(16) 0.88123(12) 0.0217 1.0000 Uani . . . . . . . O3 O 0.92886(11) 0.27344(12) 0.89795(9) 0.0308 1.0000 Uani . . . . . . . C4 C 0.65555(17) 0.20385(17) 0.79034(14) 0.0285 1.0000 Uani . . . . . . . O5 O 0.64144(15) 0.12017(13) 0.74998(11) 0.0444 1.0000 Uani . . . . . . . C6 C 0.58356(18) 0.50281(18) 0.86818(14) 0.0336 1.0000 Uani . . . . . . . C7 C 0.66102(17) 0.48739(18) 0.95166(14) 0.0325 1.0000 Uani . . . . . . . C8 C 0.62854(17) 0.3889(2) 0.99733(13) 0.0319 1.0000 Uani . . . . . . . C9 C 0.53299(18) 0.34201(19) 0.94038(15) 0.0341 1.0000 Uani . . . . . . . C10 C 0.50515(17) 0.4121(2) 0.85989(14) 0.0337 1.0000 Uani . . . . . . . B11 B 0.70187(17) 0.41169(17) 0.72293(13) 0.0192 1.0000 Uani . . . . . . . Cl12 Cl 0.58453(4) 0.37603(4) 0.62930(3) 0.0271 1.0000 Uani . . . . . . . N13 N 0.78403(12) 0.48740(12) 0.70112(9) 0.0178 1.0000 Uani . . . . . . . C14 C 0.87578(14) 0.52831(14) 0.77526(12) 0.0187 1.0000 Uani . . . . . . . C15 C 0.99455(15) 0.48891(16) 0.76042(12) 0.0225 1.0000 Uani . . . . . . . C16 C 1.08549(16) 0.52605(17) 0.84185(14) 0.0278 1.0000 Uani . . . . . . . C17 C 1.08150(17) 0.65354(17) 0.85701(15) 0.0286 1.0000 Uani . . . . . . . C18 C 0.96283(17) 0.69088(17) 0.87236(13) 0.0270 1.0000 Uani . . . . . . . C19 C 0.87221(16) 0.65615(14) 0.78983(13) 0.0230 1.0000 Uani . . . . . . . C20 C 0.79257(15) 0.53671(15) 0.60698(11) 0.0189 1.0000 Uani . . . . . . . C21 C 0.80951(15) 0.44832(15) 0.53297(12) 0.0210 1.0000 Uani . . . . . . . C22 C 0.83305(15) 0.50692(16) 0.44323(12) 0.0228 1.0000 Uani . . . . . . . C23 C 0.73750(16) 0.58916(16) 0.40650(12) 0.0251 1.0000 Uani . . . . . . . C24 C 0.72082(17) 0.67689(16) 0.48127(13) 0.0256 1.0000 Uani . . . . . . . C25 C 0.69625(16) 0.61923(16) 0.57092(12) 0.0224 1.0000 Uani . . . . . . . H61 H 0.5828 0.5661 0.8262 0.0421 1.0000 Uiso R . . . . . . H71 H 0.7233 0.5383 0.9786 0.0377 1.0000 Uiso R . . . . . . H81 H 0.6669 0.3600 1.0581 0.0371 1.0000 Uiso R . . . . . . H91 H 0.4909 0.2740 0.9583 0.0434 1.0000 Uiso R . . . . . . H101 H 0.4373 0.4007 0.8101 0.0419 1.0000 Uiso R . . . . . . H141 H 0.8628 0.4961 0.8352 0.0211 1.0000 Uiso R . . . . . . H151 H 1.0101 0.5234 0.7026 0.0254 1.0000 Uiso R . . . . . . H152 H 0.9943 0.4090 0.7534 0.0254 1.0000 Uiso R . . . . . . H162 H 1.1609 0.5045 0.8276 0.0323 1.0000 Uiso R . . . . . . H161 H 1.0716 0.4871 0.9002 0.0318 1.0000 Uiso R . . . . . . H172 H 1.1374 0.6726 0.9133 0.0318 1.0000 Uiso R . . . . . . H171 H 1.1016 0.6936 0.8013 0.0317 1.0000 Uiso R . . . . . . H181 H 0.9587 0.7728 0.8793 0.0345 1.0000 Uiso R . . . . . . H182 H 0.9407 0.6527 0.9277 0.0337 1.0000 Uiso R . . . . . . H192 H 0.8923 0.6967 0.7326 0.0278 1.0000 Uiso R . . . . . . H191 H 0.7961 0.6762 0.8038 0.0276 1.0000 Uiso R . . . . . . H201 H 0.8642 0.5784 0.6145 0.0216 1.0000 Uiso R . . . . . . H212 H 0.8728 0.4004 0.5568 0.0267 1.0000 Uiso R . . . . . . H211 H 0.7419 0.4029 0.5196 0.0267 1.0000 Uiso R . . . . . . H221 H 0.9031 0.5496 0.4609 0.0277 1.0000 Uiso R . . . . . . H222 H 0.8398 0.4478 0.3956 0.0270 1.0000 Uiso R . . . . . . H232 H 0.7553 0.6278 0.3510 0.0298 1.0000 Uiso R . . . . . . H231 H 0.6667 0.5454 0.3909 0.0304 1.0000 Uiso R . . . . . . H242 H 0.7935 0.7183 0.4976 0.0291 1.0000 Uiso R . . . . . . H241 H 0.6583 0.7298 0.4573 0.0294 1.0000 Uiso R . . . . . . H251 H 0.6911 0.6742 0.6191 0.0276 1.0000 Uiso R . . . . . . H252 H 0.6254 0.5781 0.5590 0.0276 1.0000 Uiso R . . . . . . 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 Ru1 0.01818(9) 0.02104(9) 0.01704(9) 0.00182(5) 0.00294(6) -0.00214(5) C2 0.0269(10) 0.0206(9) 0.0176(8) 0.0008(7) 0.0033(7) -0.0023(8) O3 0.0245(7) 0.0346(8) 0.0325(7) 0.0027(6) 0.0026(6) 0.0027(6) C4 0.0273(10) 0.0285(10) 0.0276(10) 0.0054(8) -0.0020(8) -0.0032(8) O5 0.0595(11) 0.0260(8) 0.0418(9) -0.0044(7) -0.0108(8) -0.0078(7) C6 0.0366(11) 0.0321(11) 0.0349(11) 0.0037(9) 0.0145(9) 0.0125(9) C7 0.0306(10) 0.0347(11) 0.0340(11) -0.0116(9) 0.0109(8) 0.0025(9) C8 0.0286(10) 0.0486(13) 0.0199(9) 0.0003(9) 0.0088(8) 0.0070(9) C9 0.0244(10) 0.0481(13) 0.0329(11) 0.0041(9) 0.0145(9) 0.0006(9) C10 0.0209(10) 0.0508(13) 0.0301(10) 0.0025(9) 0.0058(8) 0.0083(9) B11 0.0198(9) 0.0205(10) 0.0169(9) -0.0004(7) 0.0012(7) 0.0015(8) Cl12 0.0231(2) 0.0361(3) 0.0204(2) 0.00210(18) -0.00205(17) -0.00961(19) N13 0.0189(7) 0.0197(7) 0.0145(7) -0.0002(5) 0.0022(5) -0.0014(6) C14 0.0179(8) 0.0211(9) 0.0168(8) -0.0019(7) 0.0020(6) -0.0020(7) C15 0.0200(8) 0.0248(9) 0.0227(9) -0.0021(7) 0.0036(7) 0.0006(7) C16 0.0181(9) 0.0356(11) 0.0285(10) -0.0021(8) 0.0000(7) -0.0003(8) C17 0.0212(9) 0.0337(11) 0.0298(10) -0.0046(8) 0.0002(8) -0.0072(8) C18 0.0280(10) 0.0262(10) 0.0268(10) -0.0084(8) 0.0037(8) -0.0062(8) C19 0.0218(9) 0.0214(9) 0.0258(9) -0.0049(7) 0.0030(7) -0.0006(7) C20 0.0195(8) 0.0207(9) 0.0171(8) 0.0020(7) 0.0043(7) -0.0015(7) C21 0.0240(9) 0.0201(9) 0.0198(8) 0.0010(7) 0.0061(7) 0.0029(7) C22 0.0251(9) 0.0241(9) 0.0205(9) -0.0007(7) 0.0075(7) 0.0009(7) C23 0.0283(10) 0.0260(10) 0.0212(9) 0.0047(7) 0.0039(7) 0.0016(8) C24 0.0289(10) 0.0233(10) 0.0247(10) 0.0056(7) 0.0046(8) 0.0035(8) C25 0.0254(9) 0.0206(9) 0.0217(9) 0.0008(7) 0.0054(7) 0.0030(7) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 0.3563(3) 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 Ru1 . C2 . 1.8621(19) yes Ru1 . C4 . 1.862(2) yes Ru1 . C6 . 2.273(2) yes Ru1 . C7 . 2.2704(19) yes Ru1 . C8 . 2.3025(18) yes Ru1 . C9 . 2.2836(19) yes Ru1 . C10 . 2.2586(19) yes Ru1 . B11 . 2.1412(19) yes C2 . O3 . 1.153(2) yes C4 . O5 . 1.149(3) yes C6 . C7 . 1.409(3) yes C6 . C10 . 1.413(3) yes C6 . H61 . 0.963 no C7 . C8 . 1.422(3) yes C7 . H71 . 0.986 no C8 . C9 . 1.407(3) yes C8 . H81 . 0.985 no C9 . C10 . 1.425(3) yes C9 . H91 . 1.003 no C10 . H101 . 1.002 no B11 . Cl12 . 1.833(2) yes B11 . N13 . 1.394(2) yes N13 . C14 . 1.484(2) yes N13 . C20 . 1.495(2) yes C14 . C15 . 1.528(2) yes C14 . C19 . 1.531(2) yes C14 . H141 . 0.978 no C15 . C16 . 1.531(2) yes C15 . H151 . 0.971 no C15 . H152 . 0.953 no C16 . C17 . 1.529(3) yes C16 . H162 . 0.981 no C16 . H161 . 0.995 no C17 . C18 . 1.522(3) yes C17 . H172 . 0.991 no C17 . H171 . 0.992 no C18 . C19 . 1.532(3) yes C18 . H181 . 0.979 no C18 . H182 . 0.987 no C19 . H192 . 1.014 no C19 . H191 . 0.982 no C20 . C21 . 1.530(2) yes C20 . C25 . 1.532(2) yes C20 . H201 . 0.974 no C21 . C22 . 1.531(2) yes C21 . H212 . 0.961 no C21 . H211 . 0.960 no C22 . C23 . 1.526(3) yes C22 . H221 . 0.972 no C22 . H222 . 0.993 no C23 . C24 . 1.532(3) yes C23 . H232 . 0.973 no C23 . H231 . 0.982 no C24 . C25 . 1.529(2) yes C24 . H242 . 0.988 no C24 . H241 . 0.991 no C25 . H251 . 0.962 no C25 . H252 . 0.963 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 C2 . Ru1 . C4 . 87.74(8) yes C2 . Ru1 . C6 . 133.43(8) yes C4 . Ru1 . C6 . 137.18(8) yes C2 . Ru1 . C7 . 104.95(8) yes C4 . Ru1 . C7 . 162.08(8) yes C6 . Ru1 . C7 . 36.14(8) yes C2 . Ru1 . C8 . 105.74(7) yes C4 . Ru1 . C8 . 128.56(8) yes C6 . Ru1 . C8 . 60.24(7) yes C7 . Ru1 . C8 . 36.23(8) yes C2 . Ru1 . C9 . 134.49(8) yes C4 . Ru1 . C9 . 101.86(8) yes C6 . Ru1 . C9 . 60.49(8) yes C7 . Ru1 . C9 . 60.22(8) yes C8 . Ru1 . C9 . 35.72(8) yes C2 . Ru1 . C10 . 164.84(8) yes C4 . Ru1 . C10 . 105.54(8) yes C6 . Ru1 . C10 . 36.35(8) yes C7 . Ru1 . C10 . 60.50(8) yes C8 . Ru1 . C10 . 60.32(7) yes C2 . Ru1 . B11 . 91.93(7) yes C4 . Ru1 . B11 . 85.88(8) yes C6 . Ru1 . B11 . 82.11(7) yes C7 . Ru1 . B11 . 105.90(7) yes C8 . Ru1 . B11 . 140.83(8) yes C9 . Ru1 . C10 . 36.56(7) yes C9 . Ru1 . B11 . 132.69(8) yes C10 . Ru1 . B11 . 96.22(7) yes Ru1 . C2 . O3 . 178.35(16) yes Ru1 . C4 . O5 . 179.17(18) yes Ru1 . C6 . C7 . 71.84(11) yes Ru1 . C6 . C10 . 71.28(12) yes C7 . C6 . C10 . 107.88(18) yes Ru1 . C6 . H61 . 124.6 no C7 . C6 . H61 . 125.5 no C10 . C6 . H61 . 126.6 no Ru1 . C7 . C6 . 72.02(11) yes Ru1 . C7 . C8 . 73.12(11) yes C6 . C7 . C8 . 108.37(19) yes Ru1 . C7 . H71 . 125.0 no C6 . C7 . H71 . 127.4 no C8 . C7 . H71 . 124.0 no Ru1 . C8 . C7 . 70.66(10) yes Ru1 . C8 . C9 . 71.41(11) yes C7 . C8 . C9 . 107.73(18) yes Ru1 . C8 . H81 . 123.6 no C7 . C8 . H81 . 125.2 no C9 . C8 . H81 . 127.0 no Ru1 . C9 . C8 . 72.87(11) yes Ru1 . C9 . C10 . 70.77(11) yes C8 . C9 . C10 . 108.07(19) yes Ru1 . C9 . H91 . 125.4 no C8 . C9 . H91 . 123.7 no C10 . C9 . H91 . 128.1 no Ru1 . C10 . C9 . 72.68(11) yes Ru1 . C10 . C6 . 72.37(11) yes C9 . C10 . C6 . 107.92(18) yes Ru1 . C10 . H101 . 124.6 no C9 . C10 . H101 . 124.4 no C6 . C10 . H101 . 127.5 no Ru1 . B11 . Cl12 . 112.64(10) yes Ru1 . B11 . N13 . 129.76(13) yes Cl12 . B11 . N13 . 117.32(13) yes B11 . N13 . C14 . 120.47(14) yes B11 . N13 . C20 . 127.05(14) yes C14 . N13 . C20 . 112.48(13) yes N13 . C14 . C15 . 112.79(14) yes N13 . C14 . C19 . 112.93(14) yes C15 . C14 . C19 . 111.53(15) yes N13 . C14 . H141 . 108.2 no C15 . C14 . H141 . 106.1 no C19 . C14 . H141 . 104.7 no C14 . C15 . C16 . 111.05(14) yes C14 . C15 . H151 . 106.9 no C16 . C15 . H151 . 109.5 no C14 . C15 . H152 . 109.3 no C16 . C15 . H152 . 111.0 no H151 . C15 . H152 . 109.0 no C15 . C16 . C17 . 111.12(16) yes C15 . C16 . H162 . 108.7 no C17 . C16 . H162 . 109.7 no C15 . C16 . H161 . 109.1 no C17 . C16 . H161 . 108.9 no H162 . C16 . H161 . 109.3 no C16 . C17 . C18 . 110.97(16) yes C16 . C17 . H172 . 108.1 no C18 . C17 . H172 . 109.3 no C16 . C17 . H171 . 109.9 no C18 . C17 . H171 . 108.6 no H172 . C17 . H171 . 109.9 no C17 . C18 . C19 . 111.21(15) yes C17 . C18 . H181 . 111.4 no C19 . C18 . H181 . 107.9 no C17 . C18 . H182 . 110.5 no C19 . C18 . H182 . 105.3 no H181 . C18 . H182 . 110.4 no C18 . C19 . C14 . 109.98(15) yes C18 . C19 . H192 . 106.4 no C14 . C19 . H192 . 110.0 no C18 . C19 . H191 . 109.4 no C14 . C19 . H191 . 108.3 no H192 . C19 . H191 . 112.8 no N13 . C20 . C21 . 113.55(14) yes N13 . C20 . C25 . 114.05(13) yes C21 . C20 . C25 . 111.77(14) yes N13 . C20 . H201 . 106.0 no C21 . C20 . H201 . 102.8 no C25 . C20 . H201 . 107.7 no C20 . C21 . C22 . 109.80(14) yes C20 . C21 . H212 . 109.5 no C22 . C21 . H212 . 109.7 no C20 . C21 . H211 . 109.3 no C22 . C21 . H211 . 109.8 no H212 . C21 . H211 . 108.8 no C21 . C22 . C23 . 111.22(14) yes C21 . C22 . H221 . 105.8 no C23 . C22 . H221 . 108.5 no C21 . C22 . H222 . 107.9 no C23 . C22 . H222 . 110.2 no H221 . C22 . H222 . 113.2 no C22 . C23 . C24 . 110.97(15) yes C22 . C23 . H232 . 110.1 no C24 . C23 . H232 . 109.0 no C22 . C23 . H231 . 107.7 no C24 . C23 . H231 . 108.8 no H232 . C23 . H231 . 110.2 no C23 . C24 . C25 . 110.67(15) yes C23 . C24 . H242 . 107.7 no C25 . C24 . H242 . 107.0 no C23 . C24 . H241 . 110.8 no C25 . C24 . H241 . 110.4 no H242 . C24 . H241 . 110.2 no C20 . C25 . C24 . 110.14(14) yes C20 . C25 . H251 . 108.3 no C24 . C25 . H251 . 110.5 no C20 . C25 . H252 . 108.7 no C24 . C25 . H252 . 110.4 no H251 . C25 . H252 . 108.8 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C14 . H141 . C2 . 131 0.98 2.45 3.180(3) yes #============================================================================== data_4 #============================================================================== _audit_creation_date 07-12-01 _audit_creation_method CRYSTALS_ver_12.85 _publ_section_exptl_refinement ; Residual electron density suggests that there is not only disorder in most of the CF~3~ groups, but also a small amount of rotational disorder of the RuCp(CO)~2~ moiety about the Ru---B bond. This is also explains the prolate ellipses for O(8), O(10) and to a lesser extent C(7) and C(9). The maximum difference electron density is only 1.15 which explains why it was not possible to model any of it. ; _oxford_structure_analysis_title '5635' _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 12.7397(2) _cell_length_b 14.7060(3) _cell_length_c 16.4103(3) _cell_angle_alpha 77.1667(9) _cell_angle_beta 74.0805(9) _cell_angle_gamma 74.4248(8) _cell_volume 2811.17(9) _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-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 C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ru -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C61 H41 B2 Cl6 F24 N1 O2 Ru1 # Dc = 1.90 Fooo = 1360.00 Mu = 6.95 M = 1611.36 # Found Formula = C52 H41 B2 Cl2 F24 N1 O2 Ru1 # Dc = 1.61 FOOO = 1360.00 Mu = 4.95 M = 1361.45 _chemical_formula_sum 'C52 H41 B2 Cl2 F24 N1 O2 Ru1' _chemical_formula_moiety 'C32 H12 B F24, C19 H27 B N1 O2 Ru1, C H2 Cl2' _chemical_compound_source . _chemical_formula_weight 1361.45 _cell_measurement_reflns_used 11340 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description 'plate' _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_min 0.16 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_max 0.25 _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 0.495 # Sheldrick geometric approximatio 0.88 0.92 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.92 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type 'Area' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 41940 _reflns_number_total 12755 _diffrn_reflns_av_R_equivalents 0.050 # Number of reflections with Friedels Law is 12755 # Number of reflections without Friedels Law is 21420 # Theoretical number of reflections is about 12867 _diffrn_reflns_theta_min 5.120 _diffrn_reflns_theta_max 27.480 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.831 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min -15 _reflns_limit_h_max 16 _reflns_limit_k_min -18 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.81 _refine_diff_density_max 1.15 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 7665 _refine_ls_number_restraints 12 _refine_ls_number_parameters 754 _oxford_refine_ls_R_factor_ref 0.0769 _refine_ls_wR_factor_ref 0.0774 _refine_ls_goodness_of_fit_ref 1.1384 _refine_ls_shift/su_max 0.002880 # The values computed from all data _oxford_reflns_number_all 12755 _refine_ls_R_factor_all 0.1233 _refine_ls_wR_factor_all 0.1068 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 7665 _refine_ls_R_factor_gt 0.0769 _refine_ls_wR_factor_gt 0.0774 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration '.' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.600 -0.283 0.420E-01 -0.351 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Ru1 Ru 0.61506(4) 0.24173(4) 0.40999(3) 0.0557 1.0000 Uani . . . . . . . C2 C 0.7214(6) 0.3418(6) 0.3220(6) 0.0785 1.0000 Uani . . . . . . . C3 C 0.7680(5) 0.2494(5) 0.3036(5) 0.0650 1.0000 Uani . . . . . . . C4 C 0.8004(6) 0.1918(7) 0.3757(8) 0.1048 1.0000 Uani . . . . . . . C5 C 0.7705(7) 0.2556(7) 0.4422(6) 0.0844 1.0000 Uani . . . . . . . C6 C 0.7253(7) 0.3443(7) 0.4022(6) 0.0840 1.0000 Uani . . . . . . . C7 C 0.4816(6) 0.3202(7) 0.4610(5) 0.0938 1.0000 Uani . . . . . . . O8 O 0.4002(6) 0.3677(8) 0.4930(5) 0.1630 1.0000 Uani . . . . . . . C9 C 0.5756(9) 0.1317(9) 0.4792(6) 0.1026 1.0000 Uani . . . . . . . O10 O 0.5569(9) 0.0617(7) 0.5197(5) 0.1588 1.0000 Uani . . . . . . . B11 B 0.5364(5) 0.2289(4) 0.3273(4) 0.0456 1.0000 Uani . . . . . . . N12 N 0.4895(3) 0.2233(3) 0.2667(3) 0.0399 1.0000 Uani . . . . . . . C13 C 0.4263(4) 0.3119(4) 0.2209(3) 0.0420 1.0000 Uani . . . . . . . C14 C 0.4884(5) 0.3356(4) 0.1287(3) 0.0507 1.0000 Uani . . . . . . . C15 C 0.4193(7) 0.4211(5) 0.0827(4) 0.0672 1.0000 Uani . . . . . . . C16 C 0.3895(6) 0.5079(4) 0.1280(4) 0.0629 1.0000 Uani . . . . . . . C17 C 0.3296(5) 0.4853(4) 0.2211(4) 0.0560 1.0000 Uani . . . . . . . C18 C 0.3974(4) 0.3968(4) 0.2686(3) 0.0468 1.0000 Uani . . . . . . . C19 C 0.4987(5) 0.1318(4) 0.2364(3) 0.0474 1.0000 Uani . . . . . . . C20 C 0.5793(6) 0.0499(5) 0.2772(5) 0.0680 1.0000 Uani . . . . . . . C21 C 0.5916(6) -0.0407(5) 0.2431(6) 0.0790 1.0000 Uani . . . . . . . C22 C 0.4797(6) -0.0666(4) 0.2565(5) 0.0659 1.0000 Uani . . . . . . . C23 C 0.4010(7) 0.0166(5) 0.2157(6) 0.0781 1.0000 Uani . . . . . . . C24 C 0.3880(5) 0.1069(5) 0.2523(6) 0.0700 1.0000 Uani . . . . . . . Cl25 Cl 0.76687(17) 0.18748(15) 0.67946(12) 0.0788 1.0000 Uani . . . . . . . C26 C 0.8942(7) 0.1080(7) 0.6767(5) 0.0855 1.0000 Uani . . . . . . . Cl27 Cl 0.9313(3) 0.0347(3) 0.6029(3) 0.1639 1.0000 Uani . . . . . . . F28 F 0.8351(3) 0.5280(2) 0.5667(2) 0.0621 1.0000 Uani . . . . . . . C29 C 0.8569(5) 0.4416(4) 0.5421(3) 0.0485 1.0000 Uani . . . . . . . F30 F 0.7595(3) 0.4132(3) 0.5722(2) 0.0586 1.0000 Uani . . . . . . . F31 F 0.8748(3) 0.4579(3) 0.4568(2) 0.0709 1.0000 Uani . . . . . . . C32 C 0.9507(4) 0.3726(4) 0.5757(3) 0.0391 1.0000 Uani . . . . . . . C33 C 0.9563(4) 0.3686(3) 0.6597(3) 0.0346 1.0000 Uani . . . . . . . C34 C 1.0433(4) 0.3076(3) 0.6954(3) 0.0332 1.0000 Uani . . . . . . . C35 C 1.1238(4) 0.2485(4) 0.6415(3) 0.0408 1.0000 Uani . . . . . . . C36 C 1.1167(5) 0.2497(4) 0.5579(3) 0.0494 1.0000 Uani . . . . . . . C37 C 1.0307(5) 0.3126(4) 0.5230(3) 0.0462 1.0000 Uani . . . . . . . C38 C 1.2008(4) 0.1873(3) 0.5021(3) 0.0676 1.0000 Uani D . . . . . . B42 B 1.0440(4) 0.2962(4) 0.7968(3) 0.0313 1.0000 Uani . . . . . . . C43 C 0.9780(3) 0.3924(3) 0.8396(3) 0.0326 1.0000 Uani . . . . . . . C44 C 0.9816(4) 0.4838(3) 0.7933(3) 0.0338 1.0000 Uani . . . . . . . C45 C 0.9354(4) 0.5661(3) 0.8316(3) 0.0362 1.0000 Uani . . . . . . . C46 C 0.8822(4) 0.5596(4) 0.9178(3) 0.0416 1.0000 Uani . . . . . . . C47 C 0.8783(4) 0.4694(4) 0.9652(3) 0.0364 1.0000 Uani . . . . . . . C48 C 0.9253(4) 0.3879(3) 0.9266(3) 0.0327 1.0000 Uani . . . . . . . C49 C 0.8177(5) 0.4606(4) 1.0578(3) 0.0459 1.0000 Uani . . . . . . . F50 F 0.8275(3) 0.5264(3) 1.0971(2) 0.0709 1.0000 Uani . . . . . . . F51 F 0.8599(4) 0.3784(3) 1.1040(2) 0.0848 1.0000 Uani . . . . . . . F52 F 0.7106(3) 0.4652(4) 1.0688(2) 0.0948 1.0000 Uani . . . . . . . C53 C 0.9385(4) 0.6623(4) 0.7773(4) 0.0454 1.0000 Uani . . . . . . . F54 F 1.0227(4) 0.6618(3) 0.7122(3) 0.0992 1.0000 Uani . . . . . . . F55 F 0.9446(8) 0.7257(3) 0.8174(3) 0.1559 1.0000 Uani . . . . . . . F56 F 0.8527(4) 0.6971(4) 0.7452(5) 0.1666 1.0000 Uani . . . . . . . C57 C 0.9851(4) 0.2049(3) 0.8422(3) 0.0315 1.0000 Uani . . . . . . . C58 C 1.0468(4) 0.1096(3) 0.8465(3) 0.0338 1.0000 Uani . . . . . . . C59 C 0.9939(4) 0.0330(3) 0.8786(3) 0.0358 1.0000 Uani . . . . . . . C60 C 0.8789(4) 0.0478(3) 0.9081(3) 0.0379 1.0000 Uani . . . . . . . C61 C 0.8175(4) 0.1415(3) 0.9032(3) 0.0347 1.0000 Uani . . . . . . . C62 C 0.8691(4) 0.2178(3) 0.8709(3) 0.0333 1.0000 Uani . . . . . . . C63 C 0.6914(4) 0.1589(4) 0.9353(3) 0.0426 1.0000 Uani . . . . . . . F64 F 0.6467(3) 0.1130(4) 0.8981(3) 0.0899 1.0000 Uani . . . . . . . F65 F 0.6607(3) 0.1255(5) 1.0167(3) 0.1129 1.0000 Uani . . . . . . . F66 F 0.6401(3) 0.2469(3) 0.9213(4) 0.1128 1.0000 Uani . . . . . . . C67 C 1.0614(5) -0.0667(4) 0.8747(3) 0.0472 1.0000 Uani . . . . . . . F68 F 1.0209(3) -0.1314(2) 0.9393(3) 0.0754 1.0000 Uani . . . . . . . F69 F 1.1665(3) -0.0777(3) 0.8805(3) 0.0775 1.0000 Uani . . . . . . . F70 F 1.0658(5) -0.0956(3) 0.8037(3) 0.1055 1.0000 Uani . . . . . . . C71 C 1.1709(4) 0.2790(3) 0.8121(3) 0.0334 1.0000 Uani . . . . . . . C72 C 1.2528(4) 0.3217(3) 0.7528(3) 0.0378 1.0000 Uani . . . . . . . C73 C 1.3546(4) 0.3189(4) 0.7719(3) 0.0400 1.0000 Uani . . . . . . . C74 C 1.3775(4) 0.2742(4) 0.8493(3) 0.0401 1.0000 Uani . . . . . . . C75 C 1.2982(4) 0.2298(3) 0.9091(3) 0.0372 1.0000 Uani . . . . . . . C76 C 1.1967(4) 0.2323(3) 0.8903(3) 0.0342 1.0000 Uani . . . . . . . C77 C 1.3234(4) 0.1773(4) 0.9928(3) 0.0433 1.0000 Uani . . . . . . . F78 F 1.3752(5) 0.2213(4) 1.0258(3) 0.1047 1.0000 Uani . . . . . . . F79 F 1.2362(3) 0.1599(4) 1.0522(2) 0.0841 1.0000 Uani . . . . . . . F80 F 1.3908(5) 0.0919(3) 0.9847(3) 0.1073 1.0000 Uani . . . . . . . C81 C 1.4405(5) 0.3645(5) 0.7060(4) 0.0536 1.0000 Uani . . . . . . . F82 F 1.3979(4) 0.4406(3) 0.6556(3) 0.0937 1.0000 Uani . . . . . . . F83 F 1.5058(4) 0.3076(4) 0.6506(3) 0.0979 1.0000 Uani . . . . . . . F84 F 1.5111(5) 0.3860(6) 0.7384(3) 0.1520 1.0000 Uani . . . . . . . F390 F 1.1799(8) 0.1089(5) 0.4937(6) 0.124(4) 0.5000 Uiso D . . . 1 . . F391 F 1.1672(6) 0.1640(5) 0.4433(4) 0.078(2) 0.5000 Uiso D . . . 2 . . F400 F 1.2433(7) 0.2334(6) 0.4272(4) 0.106(3) 0.5000 Uiso D . . . 1 . . F401 F 1.3007(5) 0.2060(6) 0.4719(5) 0.102(3) 0.5000 Uiso D . . . 2 . . F410 F 1.3001(6) 0.1490(7) 0.5304(6) 0.108(3) 0.5000 Uiso D . . . 1 . . F411 F 1.2326(7) 0.0960(4) 0.5479(4) 0.083(2) 0.5000 Uiso D . . . 2 . . H21 H 0.6934 0.3979 0.2815 0.0983 1.0000 Uiso R . . . . . . H31 H 0.7797 0.2307 0.2473 0.0804 1.0000 Uiso R . . . . . . H41 H 0.8392 0.1248 0.3801 0.1174 1.0000 Uiso R . . . . . . H51 H 0.7852 0.2395 0.4996 0.1074 1.0000 Uiso R . . . . . . H61 H 0.6995 0.4032 0.4288 0.1076 1.0000 Uiso R . . . . . . H131 H 0.3554 0.2972 0.2195 0.0527 1.0000 Uiso R . . . . . . H142 H 0.5573 0.3498 0.1281 0.0623 1.0000 Uiso R . . . . . . H141 H 0.5024 0.2812 0.1000 0.0621 1.0000 Uiso R . . . . . . H152 H 0.4610 0.4352 0.0237 0.0864 1.0000 Uiso R . . . . . . H151 H 0.3508 0.4049 0.0815 0.0862 1.0000 Uiso R . . . . . . H161 H 0.4581 0.5258 0.1263 0.0781 1.0000 Uiso R . . . . . . H162 H 0.3420 0.5605 0.0986 0.0783 1.0000 Uiso R . . . . . . H171 H 0.3166 0.5392 0.2498 0.0695 1.0000 Uiso R . . . . . . H172 H 0.2583 0.4719 0.2232 0.0694 1.0000 Uiso R . . . . . . H181 H 0.4667 0.4101 0.2718 0.0552 1.0000 Uiso R . . . . . . H182 H 0.3551 0.3805 0.3266 0.0552 1.0000 Uiso R . . . . . . H191 H 0.5280 0.1398 0.1749 0.0573 1.0000 Uiso R . . . . . . H201 H 0.6517 0.0662 0.2646 0.0842 1.0000 Uiso R . . . . . . H202 H 0.5502 0.0401 0.3392 0.0845 1.0000 Uiso R . . . . . . H211 H 0.6393 -0.0930 0.2727 0.0944 1.0000 Uiso R . . . . . . H212 H 0.6253 -0.0317 0.1821 0.0944 1.0000 Uiso R . . . . . . H222 H 0.4472 -0.0781 0.3177 0.0823 1.0000 Uiso R . . . . . . H221 H 0.4901 -0.1238 0.2321 0.0820 1.0000 Uiso R . . . . . . H232 H 0.4322 0.0285 0.1533 0.1094 1.0000 Uiso R . . . . . . H231 H 0.3284 0.0016 0.2267 0.1094 1.0000 Uiso R . . . . . . H241 H 0.3599 0.0958 0.3130 0.0912 1.0000 Uiso R . . . . . . H242 H 0.3389 0.1593 0.2255 0.0911 1.0000 Uiso R . . . . . . H261 H 0.9524 0.1435 0.6651 0.1095 1.0000 Uiso R . . . . . . H262 H 0.8910 0.0673 0.7319 0.1092 1.0000 Uiso R . . . . . . H331 H 0.8994 0.4083 0.6939 0.0454 1.0000 Uiso R . . . . . . H351 H 1.1836 0.2069 0.6619 0.0503 1.0000 Uiso R . . . . . . H371 H 1.0251 0.3156 0.4677 0.0560 1.0000 Uiso R . . . . . . H441 H 1.0162 0.4906 0.7356 0.0433 1.0000 Uiso R . . . . . . H461 H 0.8507 0.6141 0.9427 0.0514 1.0000 Uiso R . . . . . . H481 H 0.9201 0.3280 0.9610 0.0435 1.0000 Uiso R . . . . . . H581 H 1.1246 0.0978 0.8282 0.0415 1.0000 Uiso R . . . . . . H601 H 0.8441 -0.0037 0.9302 0.0460 1.0000 Uiso R . . . . . . H621 H 0.8255 0.2787 0.8684 0.0437 1.0000 Uiso R . . . . . . H721 H 1.2382 0.3534 0.6997 0.0470 1.0000 Uiso R . . . . . . H741 H 1.4441 0.2735 0.8622 0.0491 1.0000 Uiso R . . . . . . H761 H 1.1452 0.2024 0.9310 0.0441 1.0000 Uiso R . . . . . . 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 Ru1 0.0444(2) 0.0775(4) 0.0482(2) -0.0247(2) -0.01254(19) -0.0044(2) C2 0.065(4) 0.088(5) 0.090(5) -0.027(4) -0.017(4) -0.019(4) C3 0.042(3) 0.069(4) 0.083(5) -0.017(4) -0.011(3) -0.010(3) C4 0.049(4) 0.085(6) 0.155(9) -0.010(6) -0.015(5) 0.011(4) C5 0.073(5) 0.107(6) 0.091(5) -0.011(5) -0.044(4) -0.029(5) C6 0.079(5) 0.093(6) 0.094(6) -0.012(5) -0.041(4) -0.023(4) C7 0.052(4) 0.160(8) 0.079(5) -0.081(5) -0.019(3) 0.017(4) O8 0.087(4) 0.285(11) 0.131(6) -0.155(7) -0.049(4) 0.060(6) C9 0.130(8) 0.132(8) 0.057(4) -0.002(5) -0.030(5) -0.050(7) O10 0.244(11) 0.173(8) 0.078(5) 0.037(5) -0.044(6) -0.115(8) B11 0.042(3) 0.044(3) 0.046(3) -0.014(3) -0.002(2) -0.003(3) N12 0.038(2) 0.041(2) 0.041(2) -0.0170(17) -0.0019(17) -0.0077(18) C13 0.040(3) 0.039(3) 0.054(3) -0.018(2) -0.011(2) -0.011(2) C14 0.056(3) 0.054(3) 0.045(3) -0.021(2) -0.008(2) -0.011(3) C15 0.093(5) 0.059(4) 0.059(4) -0.010(3) -0.030(3) -0.018(4) C16 0.075(4) 0.046(3) 0.074(4) -0.007(3) -0.030(3) -0.013(3) C17 0.044(3) 0.047(3) 0.084(4) -0.026(3) -0.017(3) -0.007(2) C18 0.043(3) 0.048(3) 0.047(3) -0.021(2) 0.002(2) -0.006(2) C19 0.055(3) 0.044(3) 0.042(3) -0.021(2) -0.004(2) -0.003(2) C20 0.056(4) 0.050(4) 0.100(5) -0.014(3) -0.025(4) -0.004(3) C21 0.058(4) 0.045(4) 0.124(7) -0.031(4) -0.012(4) 0.010(3) C22 0.081(5) 0.047(3) 0.074(4) -0.020(3) -0.020(4) -0.011(3) C23 0.095(5) 0.052(4) 0.107(6) -0.023(4) -0.049(5) -0.013(4) C24 0.053(3) 0.056(4) 0.117(6) -0.040(4) -0.034(4) -0.001(3) Cl25 0.0833(12) 0.0850(13) 0.0703(10) -0.0048(9) -0.0217(9) -0.0242(10) C26 0.081(5) 0.117(7) 0.073(5) -0.024(4) -0.030(4) -0.025(5) Cl27 0.162(3) 0.181(3) 0.159(3) -0.112(3) -0.068(2) 0.048(2) F28 0.070(2) 0.0457(19) 0.079(2) -0.0054(16) -0.0371(19) -0.0105(16) C29 0.049(3) 0.058(3) 0.045(3) -0.007(2) -0.014(2) -0.021(3) F30 0.0499(18) 0.063(2) 0.069(2) -0.0013(17) -0.0235(16) -0.0205(16) F31 0.081(3) 0.091(3) 0.0408(17) -0.0003(17) -0.0234(17) -0.018(2) C32 0.039(2) 0.048(3) 0.037(2) -0.007(2) -0.0097(19) -0.020(2) C33 0.036(2) 0.038(3) 0.033(2) -0.0094(19) -0.0029(18) -0.018(2) C34 0.028(2) 0.034(2) 0.040(2) -0.0099(19) -0.0041(18) -0.0110(18) C35 0.036(2) 0.046(3) 0.044(3) -0.015(2) -0.009(2) -0.009(2) C36 0.045(3) 0.060(3) 0.045(3) -0.022(2) -0.002(2) -0.012(3) C37 0.053(3) 0.058(3) 0.031(2) -0.014(2) -0.003(2) -0.021(3) C38 0.068(4) 0.084(5) 0.054(3) -0.035(3) 0.000(3) -0.016(4) B42 0.028(2) 0.031(3) 0.038(2) -0.009(2) -0.0077(19) -0.008(2) C43 0.026(2) 0.040(3) 0.037(2) -0.0126(19) -0.0114(17) -0.0064(18) C44 0.027(2) 0.043(3) 0.036(2) -0.0139(19) -0.0069(17) -0.0107(19) C45 0.031(2) 0.037(3) 0.045(3) -0.013(2) -0.0071(19) -0.0123(19) C46 0.044(3) 0.040(3) 0.046(3) -0.019(2) -0.008(2) -0.011(2) C47 0.035(2) 0.044(3) 0.037(2) -0.016(2) -0.0063(19) -0.014(2) C48 0.030(2) 0.037(2) 0.034(2) -0.0094(18) -0.0087(17) -0.0099(19) C49 0.051(3) 0.054(3) 0.038(3) -0.017(2) -0.008(2) -0.016(3) F50 0.088(3) 0.083(3) 0.0525(19) -0.0402(18) 0.0007(18) -0.030(2) F51 0.131(4) 0.069(3) 0.0387(18) -0.0055(17) -0.005(2) -0.012(2) F52 0.055(2) 0.193(5) 0.047(2) -0.022(3) 0.0045(17) -0.059(3) C53 0.044(3) 0.039(3) 0.052(3) -0.008(2) -0.004(2) -0.014(2) F54 0.087(3) 0.051(2) 0.117(4) 0.008(2) 0.035(3) -0.020(2) F55 0.347(11) 0.055(3) 0.083(3) -0.010(2) -0.037(5) -0.086(4) F56 0.078(3) 0.118(4) 0.281(8) 0.130(5) -0.096(4) -0.061(3) C57 0.030(2) 0.037(2) 0.032(2) -0.0133(18) -0.0092(17) -0.0065(18) C58 0.028(2) 0.039(3) 0.039(2) -0.0153(19) -0.0070(18) -0.0071(18) C59 0.038(2) 0.034(2) 0.038(2) -0.0129(19) -0.0114(19) -0.0050(19) C60 0.043(3) 0.038(3) 0.036(2) -0.0095(19) -0.005(2) -0.016(2) C61 0.033(2) 0.041(3) 0.034(2) -0.0148(19) -0.0051(18) -0.0111(19) C62 0.034(2) 0.033(2) 0.038(2) -0.0101(18) -0.0117(18) -0.0096(18) C63 0.041(3) 0.038(3) 0.052(3) -0.011(2) -0.007(2) -0.014(2) F64 0.0430(19) 0.129(4) 0.123(4) -0.071(3) -0.008(2) -0.031(2) F65 0.048(2) 0.216(6) 0.054(2) -0.007(3) 0.0024(18) -0.020(3) F66 0.0329(18) 0.056(2) 0.227(6) -0.007(3) -0.008(3) -0.0074(17) C67 0.048(3) 0.044(3) 0.048(3) -0.015(2) -0.010(2) -0.002(2) F68 0.075(2) 0.0379(18) 0.095(3) -0.0027(18) -0.001(2) -0.0073(17) F69 0.0458(19) 0.046(2) 0.132(4) -0.011(2) -0.022(2) 0.0029(16) F70 0.165(5) 0.066(3) 0.081(3) -0.051(2) -0.057(3) 0.042(3) C71 0.028(2) 0.030(2) 0.045(2) -0.0112(19) -0.0066(18) -0.0082(18) C72 0.034(2) 0.038(3) 0.043(2) -0.012(2) -0.0061(19) -0.010(2) C73 0.033(2) 0.039(3) 0.051(3) -0.014(2) -0.004(2) -0.013(2) C74 0.029(2) 0.041(3) 0.056(3) -0.017(2) -0.009(2) -0.012(2) C75 0.038(2) 0.034(2) 0.046(3) -0.014(2) -0.014(2) -0.0062(19) C76 0.031(2) 0.033(2) 0.043(2) -0.0115(19) -0.0083(18) -0.0104(19) C77 0.038(3) 0.045(3) 0.054(3) -0.011(2) -0.019(2) -0.009(2) F78 0.161(5) 0.114(4) 0.092(3) 0.026(3) -0.088(3) -0.093(4) F79 0.055(2) 0.145(4) 0.050(2) 0.008(2) -0.0192(17) -0.029(2) F80 0.144(4) 0.074(3) 0.070(3) -0.007(2) -0.035(3) 0.040(3) C81 0.041(3) 0.063(4) 0.063(3) -0.009(3) -0.011(3) -0.024(3) F82 0.063(2) 0.066(3) 0.122(4) 0.021(3) 0.004(2) -0.019(2) F83 0.084(3) 0.091(3) 0.086(3) -0.005(2) 0.026(2) -0.019(3) F84 0.149(5) 0.291(9) 0.077(3) 0.009(4) -0.023(3) -0.184(6) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 0.2992(5) 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 Ru1 . C2 . 2.267(8) yes Ru1 . C3 . 2.241(7) yes Ru1 . C4 . 2.226(8) yes Ru1 . C5 . 2.255(7) yes Ru1 . C6 . 2.284(8) yes Ru1 . C7 . 1.875(7) yes Ru1 . C9 . 1.862(11) yes Ru1 . B11 . 1.960(6) yes C2 . C3 . 1.394(10) yes C2 . C6 . 1.338(11) yes C2 . H21 . 0.989 no C3 . C4 . 1.387(12) yes C3 . H31 . 0.983 no C4 . C5 . 1.501(13) yes C4 . H41 . 0.973 no C5 . C6 . 1.374(12) yes C5 . H51 . 0.975 no C6 . H61 . 0.992 no C7 . O8 . 1.147(8) yes C9 . O10 . 1.140(11) yes B11 . N12 . 1.320(7) yes N12 . C13 . 1.498(7) yes N12 . C19 . 1.500(6) yes C13 . C14 . 1.515(8) yes C13 . C18 . 1.530(7) yes C13 . H131 . 0.990 no C14 . C15 . 1.508(9) yes C14 . H142 . 0.953 no C14 . H141 . 0.968 no C15 . C16 . 1.526(9) yes C15 . H152 . 0.974 no C15 . H151 . 0.971 no C16 . C17 . 1.517(9) yes C16 . H161 . 0.970 no C16 . H162 . 0.970 no C17 . C18 . 1.537(8) yes C17 . H171 . 0.964 no C17 . H172 . 0.970 no C18 . H181 . 0.970 no C18 . H182 . 0.969 no C19 . C20 . 1.519(8) yes C19 . C24 . 1.492(8) yes C19 . H191 . 0.968 no C20 . C21 . 1.512(9) yes C20 . H201 . 0.971 no C20 . H202 . 0.975 no C21 . C22 . 1.519(10) yes C21 . H211 . 0.970 no C21 . H212 . 0.970 no C22 . C23 . 1.515(10) yes C22 . H222 . 0.971 no C22 . H221 . 0.973 no C23 . C24 . 1.527(9) yes C23 . H232 . 0.985 no C23 . H231 . 0.967 no C24 . H241 . 0.954 no C24 . H242 . 0.960 no Cl25 . C26 . 1.722(9) yes C26 . Cl27 . 1.687(8) yes C26 . H261 . 0.972 no C26 . H262 . 0.967 no F28 . C29 . 1.353(7) yes C29 . F30 . 1.344(6) yes C29 . F31 . 1.332(6) yes C29 . C32 . 1.491(7) yes C32 . C33 . 1.387(6) yes C32 . C37 . 1.392(7) yes C33 . C34 . 1.401(7) yes C33 . H331 . 0.936 no C34 . C35 . 1.398(6) yes C34 . B42 . 1.637(7) yes C35 . C36 . 1.396(7) yes C35 . H351 . 0.931 no C36 . C37 . 1.396(8) yes C36 . C38 . 1.461(6) yes C37 . H371 . 0.920 no C38 . F390 . 1.295(2) yes C38 . F400 . 1.314(2) yes C38 . F410 . 1.399(2) yes B42 . C43 . 1.638(6) yes B42 . C57 . 1.646(7) yes B42 . C71 . 1.648(6) yes C43 . C44 . 1.395(7) yes C43 . C48 . 1.395(6) yes C44 . C45 . 1.399(6) yes C44 . H441 . 0.924 no C45 . C46 . 1.385(7) yes C45 . C53 . 1.499(7) yes C46 . C47 . 1.387(7) yes C46 . H461 . 0.924 no C47 . C48 . 1.394(6) yes C47 . C49 . 1.498(7) yes C48 . H481 . 0.943 no C49 . F50 . 1.324(6) yes C49 . F51 . 1.339(7) yes C49 . F52 . 1.312(6) yes C53 . F54 . 1.290(7) yes C53 . F55 . 1.285(7) yes C53 . F56 . 1.276(7) yes C57 . C58 . 1.408(6) yes C57 . C62 . 1.396(6) yes C58 . C59 . 1.397(7) yes C58 . H581 . 0.932 no C59 . C60 . 1.383(7) yes C59 . C67 . 1.493(7) yes C60 . C61 . 1.388(7) yes C60 . H601 . 0.933 no C61 . C62 . 1.383(6) yes C61 . C63 . 1.517(7) yes C62 . H621 . 0.917 no C63 . F64 . 1.316(6) yes C63 . F65 . 1.305(7) yes C63 . F66 . 1.286(7) yes C67 . F68 . 1.345(7) yes C67 . F69 . 1.332(6) yes C67 . F70 . 1.309(6) yes C71 . C72 . 1.398(7) yes C71 . C76 . 1.394(7) yes C72 . C73 . 1.404(7) yes C72 . H721 . 0.935 no C73 . C74 . 1.364(7) yes C73 . C81 . 1.497(7) yes C74 . C75 . 1.391(7) yes C74 . H741 . 0.926 no C75 . C76 . 1.399(6) yes C75 . C77 . 1.491(7) yes C76 . H761 . 0.924 no C77 . F78 . 1.314(6) yes C77 . F79 . 1.303(6) yes C77 . F80 . 1.328(7) yes C81 . F82 . 1.319(7) yes C81 . F83 . 1.330(8) yes C81 . F84 . 1.297(7) yes 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 C2 . Ru1 . C3 . 36.0(3) yes C2 . Ru1 . C4 . 60.3(3) yes C3 . Ru1 . C4 . 36.2(3) yes C2 . Ru1 . C5 . 59.5(3) yes C3 . Ru1 . C5 . 61.7(3) yes C4 . Ru1 . C5 . 39.2(4) yes C2 . Ru1 . C6 . 34.2(3) yes C3 . Ru1 . C6 . 59.0(3) yes C4 . Ru1 . C6 . 60.7(4) yes C5 . Ru1 . C6 . 35.2(3) yes C2 . Ru1 . C7 . 106.1(4) yes C3 . Ru1 . C7 . 140.8(4) yes C4 . Ru1 . C7 . 153.7(4) yes C5 . Ru1 . C7 . 115.0(3) yes C6 . Ru1 . C7 . 95.1(4) yes C2 . Ru1 . C9 . 160.4(4) yes C3 . Ru1 . C9 . 126.9(4) yes C4 . Ru1 . C9 . 100.2(4) yes C5 . Ru1 . C9 . 106.7(4) yes C6 . Ru1 . C9 . 139.3(3) yes C2 . Ru1 . B11 . 98.2(3) yes C3 . Ru1 . B11 . 89.2(3) yes C4 . Ru1 . B11 . 115.3(4) yes C5 . Ru1 . B11 . 150.9(3) yes C6 . Ru1 . B11 . 130.9(3) yes C7 . Ru1 . C9 . 92.2(5) yes C7 . Ru1 . B11 . 87.7(3) yes C9 . Ru1 . B11 . 89.3(3) yes Ru1 . C2 . C3 . 71.0(4) yes Ru1 . C2 . C6 . 73.6(5) yes C3 . C2 . C6 . 109.4(8) yes Ru1 . C2 . H21 . 124.2 no C3 . C2 . H21 . 125.6 no C6 . C2 . H21 . 124.9 no Ru1 . C3 . C2 . 73.0(4) yes Ru1 . C3 . C4 . 71.3(5) yes C2 . C3 . C4 . 108.4(8) yes Ru1 . C3 . H31 . 124.6 no C2 . C3 . H31 . 124.6 no C4 . C3 . H31 . 126.8 no Ru1 . C4 . C3 . 72.5(4) yes Ru1 . C4 . C5 . 71.5(4) yes C3 . C4 . C5 . 105.9(7) yes Ru1 . C4 . H41 . 124.0 no C3 . C4 . H41 . 126.4 no C5 . C4 . H41 . 127.6 no Ru1 . C5 . C4 . 69.4(4) yes Ru1 . C5 . C6 . 73.6(4) yes C4 . C5 . C6 . 104.7(8) yes Ru1 . C5 . H51 . 124.9 no C4 . C5 . H51 . 128.0 no C6 . C5 . H51 . 127.1 no Ru1 . C6 . C5 . 71.2(5) yes Ru1 . C6 . C2 . 72.2(5) yes C5 . C6 . C2 . 111.5(9) yes Ru1 . C6 . H61 . 124.5 no C5 . C6 . H61 . 124.5 no C2 . C6 . H61 . 124.0 no Ru1 . C7 . O8 . 179.3(8) yes Ru1 . C9 . O10 . 176.4(11) yes Ru1 . B11 . N12 . 175.3(5) yes B11 . N12 . C13 . 120.3(4) yes B11 . N12 . C19 . 123.9(5) yes C13 . N12 . C19 . 115.7(4) yes N12 . C13 . C14 . 111.5(4) yes N12 . C13 . C18 . 111.9(4) yes C14 . C13 . C18 . 111.4(4) yes N12 . C13 . H131 . 106.3 no C14 . C13 . H131 . 107.2 no C18 . C13 . H131 . 108.2 no C13 . C14 . C15 . 110.2(5) yes C13 . C14 . H142 . 109.1 no C15 . C14 . H142 . 109.1 no C13 . C14 . H141 . 109.0 no C15 . C14 . H141 . 109.2 no H142 . C14 . H141 . 110.2 no C14 . C15 . C16 . 111.5(5) yes C14 . C15 . H152 . 108.8 no C16 . C15 . H152 . 110.7 no C14 . C15 . H151 . 108.5 no C16 . C15 . H151 . 109.0 no H152 . C15 . H151 . 108.3 no C15 . C16 . C17 . 111.2(5) yes C15 . C16 . H161 . 108.7 no C17 . C16 . H161 . 108.4 no C15 . C16 . H162 . 109.4 no C17 . C16 . H162 . 109.5 no H161 . C16 . H162 . 109.7 no C16 . C17 . C18 . 111.5(5) yes C16 . C17 . H171 . 110.0 no C18 . C17 . H171 . 109.3 no C16 . C17 . H172 . 108.8 no C18 . C17 . H172 . 108.1 no H171 . C17 . H172 . 109.2 no C17 . C18 . C13 . 110.3(4) yes C17 . C18 . H181 . 109.8 no C13 . C18 . H181 . 108.4 no C17 . C18 . H182 . 110.2 no C13 . C18 . H182 . 109.5 no H181 . C18 . H182 . 108.5 no N12 . C19 . C20 . 110.9(5) yes N12 . C19 . C24 . 112.6(4) yes C20 . C19 . C24 . 110.3(5) yes N12 . C19 . H191 . 108.6 no C20 . C19 . H191 . 107.8 no C24 . C19 . H191 . 106.4 no C19 . C20 . C21 . 110.3(6) yes C19 . C20 . H201 . 109.4 no C21 . C20 . H201 . 109.8 no C19 . C20 . H202 . 108.8 no C21 . C20 . H202 . 109.5 no H201 . C20 . H202 . 109.0 no C20 . C21 . C22 . 112.1(6) yes C20 . C21 . H211 . 109.0 no C22 . C21 . H211 . 108.5 no C20 . C21 . H212 . 108.9 no C22 . C21 . H212 . 108.6 no H211 . C21 . H212 . 109.8 no C21 . C22 . C23 . 109.5(6) yes C21 . C22 . H222 . 108.7 no C23 . C22 . H222 . 108.1 no C21 . C22 . H221 . 110.1 no C23 . C22 . H221 . 110.6 no H222 . C22 . H221 . 109.6 no C22 . C23 . C24 . 110.4(6) yes C22 . C23 . H232 . 109.1 no C24 . C23 . H232 . 108.6 no C22 . C23 . H231 . 109.7 no C24 . C23 . H231 . 109.2 no H232 . C23 . H231 . 109.8 no C23 . C24 . C19 . 110.6(6) yes C23 . C24 . H241 . 109.6 no C19 . C24 . H241 . 107.1 no C23 . C24 . H242 . 109.8 no C19 . C24 . H242 . 108.8 no H241 . C24 . H242 . 110.9 no Cl25 . C26 . Cl27 . 115.3(4) yes Cl25 . C26 . H261 . 109.0 no Cl27 . C26 . H261 . 107.6 no Cl25 . C26 . H262 . 108.2 no Cl27 . C26 . H262 . 106.4 no H261 . C26 . H262 . 110.2 no F28 . C29 . F30 . 104.4(5) yes F28 . C29 . F31 . 106.3(5) yes F30 . C29 . F31 . 106.8(4) yes F28 . C29 . C32 . 112.1(4) yes F30 . C29 . C32 . 112.6(4) yes F31 . C29 . C32 . 113.9(5) yes C29 . C32 . C33 . 119.3(5) yes C29 . C32 . C37 . 119.8(4) yes C33 . C32 . C37 . 120.9(5) yes C32 . C33 . C34 . 122.7(4) yes C32 . C33 . H331 . 118.4 no C34 . C33 . H331 . 118.8 no C33 . C34 . C35 . 115.8(4) yes C33 . C34 . B42 . 122.6(4) yes C35 . C34 . B42 . 121.2(4) yes C34 . C35 . C36 . 121.8(5) yes C34 . C35 . H351 . 119.3 no C36 . C35 . H351 . 118.9 no C35 . C36 . C37 . 121.4(5) yes C35 . C36 . C38 . 121.5(5) yes C37 . C36 . C38 . 117.1(5) yes C36 . C37 . C32 . 117.3(4) yes C36 . C37 . H371 . 122.9 no C32 . C37 . H371 . 119.8 no C36 . C38 . F390 . 119.2(6) yes C36 . C38 . F400 . 113.4(5) yes F390 . C38 . F400 . 110.933(10) yes C36 . C38 . F410 . 113.4(5) yes F390 . C38 . F410 . 99.099(10) yes F400 . C38 . F410 . 97.918(10) yes C34 . B42 . C43 . 113.8(4) yes C34 . B42 . C57 . 103.4(3) yes C43 . B42 . C57 . 112.2(4) yes C34 . B42 . C71 . 112.7(4) yes C43 . B42 . C71 . 102.3(3) yes C57 . B42 . C71 . 112.9(4) yes B42 . C43 . C44 . 121.6(4) yes B42 . C43 . C48 . 122.1(4) yes C44 . C43 . C48 . 116.0(4) yes C43 . C44 . C45 . 122.2(4) yes C43 . C44 . H441 . 119.3 no C45 . C44 . H441 . 118.5 no C44 . C45 . C46 . 120.6(5) yes C44 . C45 . C53 . 119.4(4) yes C46 . C45 . C53 . 119.9(4) yes C45 . C46 . C47 . 118.2(4) yes C45 . C46 . H461 . 120.5 no C47 . C46 . H461 . 121.3 no C46 . C47 . C48 . 120.6(4) yes C46 . C47 . C49 . 119.3(4) yes C48 . C47 . C49 . 120.1(5) yes C43 . C48 . C47 . 122.4(4) yes C43 . C48 . H481 . 119.7 no C47 . C48 . H481 . 118.0 no C47 . C49 . F50 . 113.0(4) yes C47 . C49 . F51 . 112.2(5) yes F50 . C49 . F51 . 103.2(4) yes C47 . C49 . F52 . 112.9(4) yes F50 . C49 . F52 . 107.7(5) yes F51 . C49 . F52 . 107.2(5) yes C45 . C53 . F54 . 113.9(4) yes C45 . C53 . F55 . 114.1(5) yes F54 . C53 . F55 . 104.3(6) yes C45 . C53 . F56 . 112.6(4) yes F54 . C53 . F56 . 104.7(6) yes F55 . C53 . F56 . 106.3(7) yes B42 . C57 . C58 . 122.2(4) yes B42 . C57 . C62 . 121.2(4) yes C58 . C57 . C62 . 116.2(4) yes C57 . C58 . C59 . 121.3(4) yes C57 . C58 . H581 . 119.0 no C59 . C58 . H581 . 119.7 no C58 . C59 . C60 . 121.4(4) yes C58 . C59 . C67 . 119.4(4) yes C60 . C59 . C67 . 119.1(4) yes C59 . C60 . C61 . 117.6(4) yes C59 . C60 . H601 . 121.0 no C61 . C60 . H601 . 121.4 no C60 . C61 . C62 . 121.4(4) yes C60 . C61 . C63 . 118.2(4) yes C62 . C61 . C63 . 120.3(4) yes C57 . C62 . C61 . 122.1(4) yes C57 . C62 . H621 . 119.2 no C61 . C62 . H621 . 118.7 no C61 . C63 . F64 . 111.9(4) yes C61 . C63 . F65 . 112.7(4) yes F64 . C63 . F65 . 103.3(5) yes C61 . C63 . F66 . 114.2(4) yes F64 . C63 . F66 . 105.0(5) yes F65 . C63 . F66 . 108.9(5) yes C59 . C67 . F68 . 113.3(4) yes C59 . C67 . F69 . 113.4(5) yes F68 . C67 . F69 . 104.2(5) yes C59 . C67 . F70 . 112.0(4) yes F68 . C67 . F70 . 106.1(5) yes F69 . C67 . F70 . 107.2(5) yes B42 . C71 . C72 . 121.8(4) yes B42 . C71 . C76 . 121.2(4) yes C72 . C71 . C76 . 116.4(4) yes C71 . C72 . C73 . 121.5(5) yes C71 . C72 . H721 . 118.6 no C73 . C72 . H721 . 119.9 no C72 . C73 . C74 . 121.1(5) yes C72 . C73 . C81 . 119.7(5) yes C74 . C73 . C81 . 119.2(4) yes C73 . C74 . C75 . 118.6(4) yes C73 . C74 . H741 . 121.0 no C75 . C74 . H741 . 120.4 no C74 . C75 . C76 . 120.4(5) yes C74 . C75 . C77 . 119.4(4) yes C76 . C75 . C77 . 120.1(4) yes C75 . C76 . C71 . 121.9(4) yes C75 . C76 . H761 . 119.0 no C71 . C76 . H761 . 119.1 no C75 . C77 . F78 . 113.3(4) yes C75 . C77 . F79 . 114.6(4) yes F78 . C77 . F79 . 106.6(5) yes C75 . C77 . F80 . 111.6(4) yes F78 . C77 . F80 . 105.2(5) yes F79 . C77 . F80 . 104.8(5) yes C73 . C81 . F82 . 114.0(5) yes C73 . C81 . F83 . 113.1(5) yes F82 . C81 . F83 . 102.9(5) yes C73 . C81 . F84 . 113.4(5) yes F82 . C81 . F84 . 109.1(6) yes F83 . C81 . F84 . 103.3(6) yes #============================================================================== data_6 #============================================================================== _audit_creation_date 08-02-13 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title '710' _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 13.75620(10) _cell_length_b 12.30200(10) _cell_length_c 15.96190(10) _cell_angle_alpha 90 _cell_angle_beta 93.8710(4) _cell_angle_gamma 90 _cell_volume 2695.05(3) _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' 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 C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C21 H36 B1 Cl1 Fe1 N1 O1 P1 # Dc = 1.11 Fooo = 1044.00 Mu = 7.27 M = 451.61 # Found Formula = C23.50 H42 B1 Cl1 Fe1 N1 O1 P1 # Dc = 1.20 FOOO = 1044.00 Mu = 7.32 M = 487.68 _chemical_formula_sum 'C23.50 H42 B1 Cl1 Fe1 N1 O1 P1' _chemical_formula_moiety 'C21 H36 B1 Cl1 Fe1 N1 O1 P1, 0.5(C5 H12)' _chemical_compound_source . _chemical_formula_weight 487.68 _cell_measurement_reflns_used 6399 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description 'block' _exptl_crystal_colour 'clear_pale_yellow' _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_max 0.25 _exptl_crystal_density_diffrn 1.202 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1044 _exptl_absorpt_coefficient_mu 0.732 # Sheldrick geometric approximatio 0.88 0.90 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.90 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type 'Area' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 51592 _reflns_number_total 6134 _diffrn_reflns_av_R_equivalents 0.039 # Number of reflections with Friedels Law is 6134 # Number of reflections without Friedels Law is 12259 # Theoretical number of reflections is about 6193 _diffrn_reflns_theta_min 5.121 _diffrn_reflns_theta_max 27.503 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.952 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -17 _reflns_limit_h_max 17 _reflns_limit_k_min 0 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _oxford_diffrn_Wilson_B_factor 2.57 _oxford_diffrn_Wilson_scale 6.62 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.49 _refine_diff_density_max 0.62 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 6134 _refine_ls_number_restraints 24 _refine_ls_number_parameters 254 _oxford_refine_ls_R_factor_ref 0.0541 _refine_ls_wR_factor_ref 0.1123 _refine_ls_goodness_of_fit_ref 0.9653 _refine_ls_shift/su_max 0.001908 # The values computed from all data _oxford_reflns_number_all 6134 _refine_ls_R_factor_all 0.0541 _refine_ls_wR_factor_all 0.1123 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4993 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_gt 0.1068 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration '.' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.05P)^2^ + 2.36P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Fe1 Fe 0.098194(19) 0.53217(2) 0.285071(16) 0.0268 1.0000 Uani . . . . . . . P2 P 0.16072(4) 0.52714(5) 0.16428(3) 0.0399 1.0000 Uani . . . . . . . C3 C 0.29247(19) 0.5448(3) 0.17341(18) 0.0591 1.0000 Uani . . . . . . . C4 C 0.1244(2) 0.6327(3) 0.08772(17) 0.0652 1.0000 Uani . . . . . . . C5 C 0.1487(2) 0.4030(3) 0.10245(17) 0.0651 1.0000 Uani . . . . . . . C6 C 0.13607(14) 0.66449(18) 0.29227(13) 0.0356 1.0000 Uani . . . . . . . O7 O 0.16493(12) 0.75382(14) 0.29669(13) 0.0564 1.0000 Uani . . . . . . . C8 C 0.06789(18) 0.36787(18) 0.30698(16) 0.0444 1.0000 Uani . . . . . . . C9 C 0.01470(17) 0.43534(19) 0.36035(16) 0.0454 1.0000 Uani . . . . . . . C10 C 0.08206(19) 0.4948(2) 0.41192(14) 0.0438 1.0000 Uani . . . . . . . C11 C 0.17731(18) 0.46456(19) 0.39162(14) 0.0433 1.0000 Uani . . . . . . . C12 C 0.16825(16) 0.38735(18) 0.32691(15) 0.0412 1.0000 Uani . . . . . . . B13 B -0.03385(17) 0.5756(2) 0.23210(15) 0.0345 1.0000 Uani . . . . . . . Cl14 Cl -0.08550(5) 0.48090(6) 0.14896(5) 0.0602 1.0000 Uani . . . . . . . N15 N -0.09720(12) 0.66031(14) 0.25161(10) 0.0326 1.0000 Uani . . . . . . . C16 C -0.07657(14) 0.72480(15) 0.32898(12) 0.0286 1.0000 Uani . . . . . . . C17 C -0.05619(15) 0.84482(16) 0.31233(12) 0.0330 1.0000 Uani . . . . . . . C18 C -0.02624(17) 0.90207(17) 0.39481(14) 0.0412 1.0000 Uani . . . . . . . C19 C -0.10356(18) 0.8903(2) 0.45713(14) 0.0456 1.0000 Uani . . . . . . . C20 C -0.12651(17) 0.7714(2) 0.47312(13) 0.0421 1.0000 Uani . . . . . . . C21 C -0.15593(15) 0.71262(17) 0.39105(14) 0.0358 1.0000 Uani . . . . . . . C28 C -0.0259(7) 0.1160(8) 0.1147(6) 0.2607(7) 0.5000 Uiso D . . . . . . C29 C 0.0335(6) 0.0271(7) 0.0843(5) 0.2316(10) 0.5000 Uiso D . . . . . . C30 C 0.0000 0.0000 0.0000 0.1468(9) 1.0000 Uiso DS . . . . . . C31 C 0.0635(5) -0.0818(7) -0.0324(4) 0.1936(10) 0.5000 Uiso D . . . . . . C32 C 0.0246(7) -0.1164(8) -0.1153(6) 0.2607(7) 0.5000 Uiso D . . . . . . H31 H 0.3201 0.4876 0.2079 0.0893 1.0000 Uiso . . . . . . . H32 H 0.3095 0.6147 0.2001 0.0898 1.0000 Uiso . . . . . . . H33 H 0.3180 0.5404 0.1191 0.0896 1.0000 Uiso . . . . . . . H41 H 0.0559 0.6230 0.0724 0.0971 1.0000 Uiso . . . . . . . H42 H 0.1364 0.7046 0.1129 0.0974 1.0000 Uiso . . . . . . . H43 H 0.1609 0.6243 0.0397 0.0972 1.0000 Uiso . . . . . . . H51 H 0.0805 0.3898 0.0877 0.0972 1.0000 Uiso . . . . . . . H52 H 0.1828 0.4107 0.0533 0.0979 1.0000 Uiso . . . . . . . H53 H 0.1761 0.3439 0.1343 0.0976 1.0000 Uiso . . . . . . . H81 H 0.0408 0.3189 0.2634 0.0529 1.0000 Uiso . . . . . . . H91 H -0.0547 0.4393 0.3619 0.0553 1.0000 Uiso . . . . . . . H101 H 0.0651 0.5463 0.4528 0.0532 1.0000 Uiso . . . . . . . H111 H 0.2405 0.4921 0.4187 0.0521 1.0000 Uiso . . . . . . . H121 H 0.2204 0.3514 0.3009 0.0505 1.0000 Uiso . . . . . . . H161 H -0.0176 0.6939 0.3573 0.0332 1.0000 Uiso . . . . . . . H171 H -0.1137 0.8792 0.2868 0.0383 1.0000 Uiso . . . . . . . H172 H -0.0044 0.8498 0.2729 0.0391 1.0000 Uiso . . . . . . . H181 H -0.0159 0.9800 0.3840 0.0494 1.0000 Uiso . . . . . . . H182 H 0.0352 0.8701 0.4186 0.0491 1.0000 Uiso . . . . . . . H191 H -0.0821 0.9265 0.5087 0.0556 1.0000 Uiso . . . . . . . H192 H -0.1621 0.9261 0.4339 0.0545 1.0000 Uiso . . . . . . . H201 H -0.1788 0.7656 0.5107 0.0506 1.0000 Uiso . . . . . . . H202 H -0.0691 0.7348 0.4997 0.0503 1.0000 Uiso . . . . . . . H211 H -0.2151 0.7434 0.3664 0.0422 1.0000 Uiso . . . . . . . H212 H -0.1660 0.6363 0.4023 0.0429 1.0000 Uiso . . . . . . . H281 H 0.0013 0.1397 0.1666 0.3119 0.5000 Uiso . . . . . . . H282 H -0.0180 0.1819 0.0754 0.3119 0.5000 Uiso . . . . . . . H283 H -0.0873 0.0966 0.1111 0.3119 0.5000 Uiso . . . . . . . H291 H 0.0987 0.0531 0.0738 0.3412 0.5000 Uiso . . . . . . . H292 H 0.0364 -0.0217 0.1288 0.3410 0.5000 Uiso . . . . . . . H301 H -0.0104 0.0567 -0.0481 0.2644 0.5000 Uiso . . . . . . . H302 H -0.0607 -0.0382 0.0033 0.2261 0.5000 Uiso . . . . . . . H311 H 0.1219 -0.0416 -0.0411 0.3010 0.5000 Uiso . . . . . . . H312 H 0.0531 -0.1409 0.0042 0.3012 0.5000 Uiso . . . . . . . H321 H 0.0690 -0.1648 -0.1367 0.3119 0.5000 Uiso . . . . . . . H322 H 0.0229 -0.0509 -0.1527 0.3119 0.5000 Uiso . . . . . . . H323 H -0.0358 -0.1415 -0.1111 0.3119 0.5000 Uiso . . . . . . . C220 C -0.1906(3) 0.6892(4) 0.2103(3) 0.0275(11) 0.5000 Uiso . . . . 1 . . C230 C -0.2763(3) 0.6144(4) 0.2139(3) 0.0374(11) 0.5000 Uiso . . . . 1 . . C240 C -0.3674(4) 0.6730(5) 0.1777(4) 0.0486(12) 0.5000 Uiso . . . . 1 . . C250 C -0.3547(4) 0.7066(4) 0.0888(4) 0.0462(11) 0.5000 Uiso . . . . 1 . . C260 C -0.2688(5) 0.7769(5) 0.0788(4) 0.0512(13) 0.5000 Uiso . . . . 1 . . C270 C -0.1755(4) 0.7213(5) 0.1193(3) 0.0438(13) 0.5000 Uiso . . . . 1 . . C221 C -0.1802(3) 0.7099(4) 0.1936(3) 0.0253(11) 0.5000 Uiso . . . . 2 . . C231 C -0.2699(3) 0.6335(4) 0.1861(3) 0.0365(11) 0.5000 Uiso . . . . 2 . . C241 C -0.3572(3) 0.6947(4) 0.1442(4) 0.0380(10) 0.5000 Uiso . . . . 2 . . C251 C -0.3323(4) 0.7353(4) 0.0600(3) 0.0389(10) 0.5000 Uiso . . . . 2 . . C261 C -0.2414(4) 0.8075(4) 0.0647(3) 0.0396(10) 0.5000 Uiso . . . . 2 . . C271 C -0.1551(4) 0.7510(4) 0.1103(3) 0.0327(10) 0.5000 Uiso . . . . 2 . . H2201 H -0.2103 0.7551 0.2378 0.0329 0.5000 Uiso . . . . 1 . . H2301 H -0.2852 0.5946 0.2710 0.0442 0.5000 Uiso . . . . 1 . . H2302 H -0.2645 0.5484 0.1824 0.0447 0.5000 Uiso . . . . 1 . . H2401 H -0.3791 0.7377 0.2127 0.0579 0.5000 Uiso . . . . 1 . . H2402 H -0.4227 0.6238 0.1801 0.0580 0.5000 Uiso . . . . 1 . . H2501 H -0.4140 0.7478 0.0699 0.0568 0.5000 Uiso . . . . 1 . . H2502 H -0.3506 0.6417 0.0546 0.0562 0.5000 Uiso . . . . 1 . . H2601 H -0.2751 0.8493 0.1038 0.0604 0.5000 Uiso . . . . 1 . . H2602 H -0.2600 0.7857 0.0188 0.0617 0.5000 Uiso . . . . 1 . . H2701 H -0.1229 0.7749 0.1176 0.0518 0.5000 Uiso . . . . 1 . . H2702 H -0.1606 0.6572 0.0874 0.0522 0.5000 Uiso . . . . 1 . . H2211 H -0.2019 0.7725 0.2237 0.0305 0.5000 Uiso . . . . 2 . . H2311 H -0.2857 0.6057 0.2429 0.0422 0.5000 Uiso . . . . 2 . . H2312 H -0.2556 0.5710 0.1525 0.0431 0.5000 Uiso . . . . 2 . . H2411 H -0.3741 0.7563 0.1800 0.0448 0.5000 Uiso . . . . 2 . . H2412 H -0.4121 0.6452 0.1333 0.0454 0.5000 Uiso . . . . 2 . . H2511 H -0.3860 0.7785 0.0339 0.0474 0.5000 Uiso . . . . 2 . . H2512 H -0.3201 0.6748 0.0238 0.0473 0.5000 Uiso . . . . 2 . . H2611 H -0.2537 0.8751 0.0924 0.0472 0.5000 Uiso . . . . 2 . . H2612 H -0.2233 0.8261 0.0085 0.0478 0.5000 Uiso . . . . 2 . . H2711 H -0.1045 0.8040 0.1184 0.0384 0.5000 Uiso . . . . 2 . . H2712 H -0.1323 0.6926 0.0770 0.0388 0.5000 Uiso . . . . 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 Fe1 0.02408(15) 0.02869(15) 0.02811(15) -0.00191(10) 0.00485(10) 0.00081(10) P2 0.0398(3) 0.0515(3) 0.0294(3) 0.0018(2) 0.0095(2) 0.0127(2) C3 0.0442(14) 0.0783(19) 0.0576(16) 0.0156(14) 0.0249(12) 0.0118(13) C4 0.0705(18) 0.085(2) 0.0415(13) 0.0220(14) 0.0125(12) 0.0205(16) C5 0.0708(18) 0.080(2) 0.0442(14) -0.0229(14) 0.0046(13) 0.0264(16) C6 0.0257(9) 0.0396(11) 0.0423(11) -0.0021(9) 0.0083(8) -0.0004(8) O7 0.0428(9) 0.0381(9) 0.0903(14) -0.0091(9) 0.0191(9) -0.0130(7) C8 0.0486(13) 0.0317(11) 0.0532(13) 0.0002(10) 0.0066(10) -0.0023(10) C9 0.0387(12) 0.0399(12) 0.0596(14) 0.0115(11) 0.0175(10) -0.0015(10) C10 0.0579(14) 0.0445(12) 0.0304(11) 0.0040(9) 0.0132(10) 0.0019(11) C11 0.0447(12) 0.0478(13) 0.0366(11) 0.0102(9) -0.0031(9) 0.0014(10) C12 0.0405(12) 0.0367(11) 0.0473(12) 0.0088(9) 0.0101(9) 0.0102(9) B13 0.0295(11) 0.0366(12) 0.0372(12) -0.0116(10) -0.0001(9) 0.0002(9) Cl14 0.0455(3) 0.0610(4) 0.0711(4) -0.0411(3) -0.0191(3) 0.0170(3) N15 0.0264(8) 0.0356(9) 0.0349(9) -0.0117(7) -0.0033(6) 0.0036(7) C16 0.0274(9) 0.0294(9) 0.0289(9) -0.0050(7) 0.0022(7) 0.0019(7) C17 0.0359(10) 0.0319(10) 0.0309(10) -0.0014(8) 0.0012(8) -0.0002(8) C18 0.0489(13) 0.0325(10) 0.0414(11) -0.0077(9) -0.0026(10) -0.0042(9) C19 0.0566(14) 0.0450(13) 0.0352(11) -0.0151(10) 0.0025(10) 0.0053(11) C20 0.0445(12) 0.0508(13) 0.0320(11) 0.0018(9) 0.0104(9) 0.0087(10) C21 0.0339(10) 0.0329(10) 0.0417(11) -0.0011(9) 0.0096(9) 0.0007(8) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 0.3942(5) 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 Fe1 . P2 . 2.1645(6) yes Fe1 . C6 . 1.711(2) yes Fe1 . C8 . 2.098(2) yes Fe1 . C9 . 2.090(2) yes Fe1 . C10 . 2.103(2) yes Fe1 . C11 . 2.126(2) yes Fe1 . C12 . 2.112(2) yes Fe1 . B13 . 2.023(2) yes P2 . C3 . 1.821(3) yes P2 . C4 . 1.829(3) yes P2 . C5 . 1.820(3) yes C3 . H31 . 0.955 no C3 . H32 . 0.981 no C3 . H33 . 0.959 no C4 . H41 . 0.965 no C4 . H42 . 0.981 no C4 . H43 . 0.950 no C5 . H51 . 0.966 no C5 . H52 . 0.946 no C5 . H53 . 0.950 no C6 . O7 . 1.169(3) yes C8 . C9 . 1.426(3) yes C8 . C12 . 1.416(3) yes C8 . H81 . 0.976 no C9 . C10 . 1.403(4) yes C9 . H91 . 0.958 no C10 . C11 . 1.420(3) yes C10 . H101 . 0.950 no C11 . C12 . 1.403(3) yes C11 . H111 . 1.003 no C12 . H121 . 0.960 no B13 . Cl14 . 1.870(2) yes B13 . N15 . 1.406(3) yes N15 . C16 . 1.479(2) yes N15 . C220 . 1.448(5) yes C16 . C17 . 1.529(3) yes C16 . C21 . 1.530(3) yes C16 . H161 . 0.978 no C17 . C18 . 1.525(3) yes C17 . H171 . 0.964 no C17 . H172 . 0.984 no C18 . C19 . 1.512(3) yes C18 . H181 . 0.986 no C18 . H182 . 0.985 no C19 . C20 . 1.521(3) yes C19 . H191 . 0.964 no C19 . H192 . 0.969 no C20 . C21 . 1.527(3) yes C20 . H201 . 0.969 no C20 . H202 . 0.980 no C21 . H211 . 0.958 no C21 . H212 . 0.968 no C28 . H322 2_555 1.004 no C28 . C31 2_555 1.441(8) yes C28 . H321 2_555 0.928 no C28 . H323 2_555 0.910 no C28 . C29 . 1.468(8) yes C28 . H281 . 0.933 no C28 . H282 . 1.034 no C28 . H283 . 0.876 no C29 . C32 2_555 1.465(7) yes C29 . C31 2_555 1.664(5) yes C29 . H301 2_555 1.214 no C29 . C30 . 1.431(7) yes C29 . H291 . 0.977 no C29 . H292 . 0.929 no C30 . H301 2_555 1.040 no C30 . C31 2_555 1.451(7) yes C30 . H302 2_555 0.962 no C30 . C31 . 1.451(7) yes C30 . H301 . 1.040 no C30 . H302 . 0.962 no C31 . C32 . 1.457(8) yes C31 . H311 . 0.961 no C31 . H312 . 0.951 no C32 . H282 2_555 1.034 no C32 . H281 2_555 0.916 no C32 . H283 2_555 0.894 no C32 . H321 . 0.933 no C32 . H322 . 1.002 no C32 . H323 . 0.893 no C220 . C230 . 1.500(7) yes C220 . C270 . 1.532(7) yes C220 . H2201 . 0.970 no C230 . C240 . 1.526(7) yes C230 . H2301 . 0.959 no C230 . H2302 . 0.975 no C240 . C250 . 1.499(8) yes C240 . H2401 . 0.992 no C240 . H2402 . 0.975 no C250 . C260 . 1.482(8) yes C250 . H2501 . 0.989 no C250 . H2502 . 0.971 no C260 . C270 . 1.556(8) yes C260 . H2601 . 0.982 no C260 . H2602 . 0.979 no C270 . H2701 . 0.980 no C270 . H2702 . 0.969 no C221 . C231 . 1.549(7) yes C221 . C271 . 1.485(7) yes C221 . H2211 . 0.965 no C231 . C241 . 1.532(7) yes C231 . H2311 . 1.006 no C231 . H2312 . 0.966 no C241 . C251 . 1.495(7) yes C241 . H2411 . 0.986 no C241 . H2412 . 0.977 no C251 . C261 . 1.531(7) yes C251 . H2511 . 0.979 no C251 . H2512 . 0.964 no C261 . C271 . 1.518(6) yes C261 . H2611 . 0.963 no C261 . H2612 . 0.973 no C271 . H2711 . 0.957 no C271 . H2712 . 0.959 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 P2 . Fe1 . C6 . 87.11(7) yes P2 . Fe1 . C8 . 102.49(7) yes C6 . Fe1 . C8 . 165.62(10) yes P2 . Fe1 . C9 . 139.70(8) yes C6 . Fe1 . C9 . 132.88(10) yes C8 . Fe1 . C9 . 39.82(9) yes P2 . Fe1 . C10 . 157.77(7) yes C6 . Fe1 . C10 . 101.24(10) yes C8 . Fe1 . C10 . 66.03(10) yes C9 . Fe1 . C10 . 39.10(10) yes P2 . Fe1 . C11 . 119.25(7) yes C6 . Fe1 . C11 . 100.45(10) yes C8 . Fe1 . C11 . 65.57(9) yes C9 . Fe1 . C11 . 65.70(10) yes C10 . Fe1 . C11 . 39.25(10) yes P2 . Fe1 . C12 . 93.28(6) yes C6 . Fe1 . C12 . 130.61(10) yes C8 . Fe1 . C12 . 39.31(9) yes C9 . Fe1 . C12 . 66.06(9) yes C10 . Fe1 . C12 . 65.59(9) yes P2 . Fe1 . B13 . 92.00(7) yes C6 . Fe1 . B13 . 92.14(10) yes C8 . Fe1 . B13 . 98.13(10) yes C9 . Fe1 . B13 . 83.00(10) yes C10 . Fe1 . B13 . 108.06(10) yes C11 . Fe1 . C12 . 38.65(9) yes C11 . Fe1 . B13 . 146.57(10) yes C12 . Fe1 . B13 . 137.11(10) yes Fe1 . P2 . C3 . 112.24(9) yes Fe1 . P2 . C4 . 117.89(9) yes C3 . P2 . C4 . 101.20(14) yes Fe1 . P2 . C5 . 118.70(11) yes C3 . P2 . C5 . 101.35(14) yes C4 . P2 . C5 . 102.86(15) yes P2 . C3 . H31 . 108.2 no P2 . C3 . H32 . 110.3 no H31 . C3 . H32 . 108.7 no P2 . C3 . H33 . 110.1 no H31 . C3 . H33 . 108.9 no H32 . C3 . H33 . 110.5 no P2 . C4 . H41 . 107.4 no P2 . C4 . H42 . 109.7 no H41 . C4 . H42 . 110.4 no P2 . C4 . H43 . 109.1 no H41 . C4 . H43 . 110.0 no H42 . C4 . H43 . 110.1 no P2 . C5 . H51 . 108.9 no P2 . C5 . H52 . 109.5 no H51 . C5 . H52 . 110.0 no P2 . C5 . H53 . 109.5 no H51 . C5 . H53 . 110.2 no H52 . C5 . H53 . 108.6 no Fe1 . C6 . O7 . 177.82(18) yes Fe1 . C8 . C9 . 69.79(13) yes Fe1 . C8 . C12 . 70.89(13) yes C9 . C8 . C12 . 107.4(2) yes Fe1 . C8 . H81 . 123.1 no C9 . C8 . H81 . 126.8 no C12 . C8 . H81 . 125.8 no Fe1 . C9 . C8 . 70.39(13) yes Fe1 . C9 . C10 . 70.94(13) yes C8 . C9 . C10 . 108.0(2) yes Fe1 . C9 . H91 . 125.0 no C8 . C9 . H91 . 126.6 no C10 . C9 . H91 . 125.4 no Fe1 . C10 . C9 . 69.97(13) yes Fe1 . C10 . C11 . 71.25(12) yes C9 . C10 . C11 . 108.2(2) yes Fe1 . C10 . H101 . 124.2 no C9 . C10 . H101 . 124.6 no C11 . C10 . H101 . 127.2 no Fe1 . C11 . C10 . 69.49(13) yes Fe1 . C11 . C12 . 70.16(12) yes C10 . C11 . C12 . 107.9(2) yes Fe1 . C11 . H111 . 126.5 no C10 . C11 . H111 . 126.8 no C12 . C11 . H111 . 125.3 no Fe1 . C12 . C8 . 69.80(13) yes Fe1 . C12 . C11 . 71.19(13) yes C8 . C12 . C11 . 108.5(2) yes Fe1 . C12 . H121 . 126.1 no C8 . C12 . H121 . 124.8 no C11 . C12 . H121 . 126.7 no Fe1 . B13 . Cl14 . 114.79(12) yes Fe1 . B13 . N15 . 130.95(15) yes Cl14 . B13 . N15 . 114.04(15) yes B13 . N15 . C16 . 119.69(16) yes B13 . N15 . C220 . 128.7(2) yes C16 . N15 . C220 . 111.3(2) yes N15 . C16 . C17 . 113.57(16) yes N15 . C16 . C21 . 112.52(16) yes C17 . C16 . C21 . 110.74(16) yes N15 . C16 . H161 . 106.5 no C17 . C16 . H161 . 107.4 no C21 . C16 . H161 . 105.6 no C16 . C17 . C18 . 109.75(16) yes C16 . C17 . H171 . 110.0 no C18 . C17 . H171 . 109.2 no C16 . C17 . H172 . 108.7 no C18 . C17 . H172 . 111.0 no H171 . C17 . H172 . 108.1 no C17 . C18 . C19 . 111.26(18) yes C17 . C18 . H181 . 109.4 no C19 . C18 . H181 . 109.0 no C17 . C18 . H182 . 108.8 no C19 . C18 . H182 . 109.4 no H181 . C18 . H182 . 109.0 no C18 . C19 . C20 . 111.48(18) yes C18 . C19 . H191 . 109.2 no C20 . C19 . H191 . 110.9 no C18 . C19 . H192 . 108.0 no C20 . C19 . H192 . 108.9 no H191 . C19 . H192 . 108.3 no C19 . C20 . C21 . 110.94(18) yes C19 . C20 . H201 . 110.2 no C21 . C20 . H201 . 109.3 no C19 . C20 . H202 . 110.1 no C21 . C20 . H202 . 108.2 no H201 . C20 . H202 . 108.0 no C16 . C21 . C20 . 110.47(17) yes C16 . C21 . H211 . 108.6 no C20 . C21 . H211 . 109.5 no C16 . C21 . H212 . 109.5 no C20 . C21 . H212 . 109.4 no H211 . C21 . H212 . 109.3 no H322 2_555 C28 . C31 2_555 108.4 no H322 2_555 C28 . H321 2_555 106.7 no C31 2_555 C28 . H321 2_555 109.5 no H322 2_555 C28 . H323 2_555 108.1 no C31 2_555 C28 . H323 2_555 108.8 no H321 2_555 C28 . H323 2_555 115.1 no H322 2_555 C28 . C29 . 66.7 no C31 2_555 C28 . C29 . 69.8(4) yes H321 2_555 C28 . C29 . 172.0 no H323 2_555 C28 . C29 . 72.1 no H322 2_555 C28 . H281 . 73.3 no C31 2_555 C28 . H281 . 176.9 no H321 2_555 C28 . H281 . 72.0 no H323 2_555 C28 . H281 . 68.2 no C29 . C28 . H281 . 109.1 no H322 2_555 C28 . H282 . 171.5 no C31 2_555 C28 . H282 . 73.9 no H321 2_555 C28 . H282 . 79.6 no H323 2_555 C28 . H282 . 63.6 no C29 . C28 . H282 . 107.4 no H322 2_555 C28 . H283 . 79.8 no C31 2_555 C28 . H283 . 64.9 no H321 2_555 C28 . H283 . 64.2 no H323 2_555 C28 . H283 . 171.5 no C29 . C28 . H283 . 109.3 no H281 . C28 . H282 . 104.0 no H281 . C28 . H283 . 118.1 no H282 . C28 . H283 . 108.4 no C28 . C29 . C31 2_555 54.4(3) yes C32 2_555 C29 . C31 2_555 55.1(4) yes C28 . C29 . H301 2_555 131.1 no C32 2_555 C29 . H301 2_555 131.9 no C31 2_555 C29 . H301 2_555 86.1 no C28 . C29 . C30 . 109.500(10) yes C32 2_555 C29 . C30 . 110.2(4) yes C31 2_555 C29 . C30 . 55.3(3) yes H301 2_555 C29 . C30 . 45.4 no C28 . C29 . H291 . 110.5 no C32 2_555 C29 . H291 . 109.9 no C31 2_555 C29 . H291 . 119.9 no H301 2_555 C29 . H291 . 114.2 no C30 . C29 . H291 . 99.0 no C28 . C29 . H292 . 103.0 no C32 2_555 C29 . H292 . 102.8 no C31 2_555 C29 . H292 . 129.3 no H301 2_555 C29 . H292 . 79.2 no C30 . C29 . H292 . 124.3 no H291 . C29 . H292 . 110.4 no H301 2_555 C30 . C31 2_555 105.0 no H301 2_555 C30 . C29 2_555 123.8 no C31 2_555 C30 . C29 2_555 109.502(10) yes H301 2_555 C30 . C29 . 56.2 no C31 2_555 C30 . C29 . 70.498(10) yes C29 2_555 C30 . C29 . 179.992 yes H301 2_555 C30 . H302 2_555 106.9 no C31 2_555 C30 . H302 2_555 103.1 no C29 2_555 C30 . H302 2_555 106.7 no C29 . C30 . H302 2_555 73.3 no H301 2_555 C30 . C31 . 75.0 no C31 2_555 C30 . C31 . 179.992 yes C29 2_555 C30 . C31 . 70.498(10) yes C29 . C30 . C31 . 109.502(10) yes H302 2_555 C30 . C31 . 76.9 no H301 2_555 C30 . H301 . 180.0 no C31 2_555 C30 . H301 . 75.0 no C29 2_555 C30 . H301 . 56.2 no C29 . C30 . H301 . 123.8 no H302 2_555 C30 . H301 . 73.1 no H301 2_555 C30 . H302 . 73.1 no C31 2_555 C30 . H302 . 76.9 no C29 2_555 C30 . H302 . 73.3 no C29 . C30 . H302 . 106.7 no H302 2_555 C30 . H302 . 180.0 no C31 . C30 . H301 . 105.0 no C31 . C30 . H302 . 103.1 no H301 . C30 . H302 . 106.9 no C30 . C31 . C28 2_555 109.9(4) yes C30 . C31 . C29 2_555 54.2(3) yes C28 2_555 C31 . C29 2_555 55.9(4) yes C30 . C31 . C32 . 109.500(10) yes C29 2_555 C31 . C32 . 55.5(3) yes C30 . C31 . H311 . 102.9 no C28 2_555 C31 . H311 . 105.8 no C29 2_555 C31 . H311 . 111.8 no C32 . C31 . H311 . 106.2 no C30 . C31 . H312 . 101.0 no C28 2_555 C31 . H312 . 106.1 no C29 2_555 C31 . H312 . 117.8 no C32 . C31 . H312 . 105.9 no H311 . C31 . H312 . 130.1 no H282 2_555 C32 . C29 2_555 107.6 no H282 2_555 C32 . C31 . 73.2 no C29 2_555 C32 . C31 . 69.4(4) yes H282 2_555 C32 . H281 2_555 105.2 no C29 2_555 C32 . H281 2_555 110.4 no C31 . C32 . H281 2_555 178.1 no H282 2_555 C32 . H283 2_555 106.9 no C29 2_555 C32 . H283 2_555 108.3 no C31 . C32 . H283 2_555 63.8 no H281 2_555 C32 . H283 2_555 117.9 no H282 2_555 C32 . H321 . 79.4 no C29 2_555 C32 . H321 . 170.8 no C31 . C32 . H321 . 108.0 no H281 2_555 C32 . H321 . 72.5 no H283 2_555 C32 . H321 . 63.3 no H282 2_555 C32 . H322 . 173.3 no C29 2_555 C32 . H322 . 66.9 no C31 . C32 . H322 . 107.4 no H281 2_555 C32 . H322 . 74.1 no H283 2_555 C32 . H322 . 79.0 no H282 2_555 C32 . H323 . 64.1 no C29 2_555 C32 . H323 . 72.7 no C31 . C32 . H323 . 108.6 no H281 2_555 C32 . H323 . 69.6 no H283 2_555 C32 . H323 . 170.3 no H321 . C32 . H322 . 106.5 no H321 . C32 . H323 . 116.3 no H322 . C32 . H323 . 109.8 no C30 . H301 . C29 2_555 78.4 no N15 . C220 . C230 . 120.5(4) yes N15 . C220 . C270 . 108.8(4) yes C230 . C220 . C270 . 110.6(4) yes N15 . C220 . H2201 . 105.4 no C230 . C220 . H2201 . 104.5 no C270 . C220 . H2201 . 105.9 no C220 . C230 . C240 . 108.9(4) yes C220 . C230 . H2301 . 110.2 no C240 . C230 . H2301 . 109.0 no C220 . C230 . H2302 . 109.4 no C240 . C230 . H2302 . 111.1 no H2301 . C230 . H2302 . 108.3 no C230 . C240 . C250 . 110.1(5) yes C230 . C240 . H2401 . 109.0 no C250 . C240 . H2401 . 110.2 no C230 . C240 . H2402 . 108.3 no C250 . C240 . H2402 . 110.5 no H2401 . C240 . H2402 . 108.6 no C240 . C250 . C260 . 114.0(5) yes C240 . C250 . H2501 . 106.5 no C260 . C250 . H2501 . 108.4 no C240 . C250 . H2502 . 108.7 no C260 . C250 . H2502 . 110.0 no H2501 . C250 . H2502 . 109.1 no C250 . C260 . C270 . 109.9(5) yes C250 . C260 . H2601 . 113.1 no C270 . C260 . H2601 . 108.9 no C250 . C260 . H2602 . 108.7 no C270 . C260 . H2602 . 107.6 no H2601 . C260 . H2602 . 108.6 no C220 . C270 . C260 . 110.3(4) yes C220 . C270 . H2701 . 110.3 no C260 . C270 . H2701 . 106.3 no C220 . C270 . H2702 . 109.6 no C260 . C270 . H2702 . 109.8 no H2701 . C270 . H2702 . 110.4 no N15 . C221 . C231 . 111.1(4) yes N15 . C221 . C271 . 117.6(3) yes C231 . C221 . C271 . 111.7(4) yes N15 . C221 . H2211 . 104.9 no C231 . C221 . H2211 . 104.5 no C271 . C221 . H2211 . 105.8 no C221 . C231 . C241 . 109.4(4) yes C221 . C231 . H2311 . 110.9 no C241 . C231 . H2311 . 110.5 no C221 . C231 . H2312 . 109.6 no C241 . C231 . H2312 . 109.4 no H2311 . C231 . H2312 . 107.0 no C231 . C241 . C251 . 109.7(4) yes C231 . C241 . H2411 . 109.4 no C251 . C241 . H2411 . 110.0 no C231 . C241 . H2412 . 110.2 no C251 . C241 . H2412 . 105.6 no H2411 . C241 . H2412 . 111.9 no C241 . C251 . C261 . 112.6(4) yes C241 . C251 . H2511 . 110.6 no C261 . C251 . H2511 . 107.3 no C241 . C251 . H2512 . 109.9 no C261 . C251 . H2512 . 107.6 no H2511 . C251 . H2512 . 108.7 no C251 . C261 . C271 . 111.6(4) yes C251 . C261 . H2611 . 110.8 no C271 . C261 . H2611 . 109.4 no C251 . C261 . H2612 . 110.5 no C271 . C261 . H2612 . 108.0 no H2611 . C261 . H2612 . 106.5 no C261 . C271 . C221 . 111.3(4) yes C261 . C271 . H2711 . 107.0 no C221 . C271 . H2711 . 108.8 no C261 . C271 . H2712 . 110.6 no C221 . C271 . H2712 . 110.3 no H2711 . C271 . H2712 . 108.8 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C12 . H121 . O7 3_545 168 0.96 2.59 3.531(6) yes C16 . H161 . C6 . 125 0.98 2.44 3.111(6) yes #============================================================================== data_9 #============================================================================== _audit_creation_date 08-01-17 _audit_creation_method CRYSTALS_ver_12.85 _oxford_structure_analysis_title '5669' _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 17.48100(10) _cell_length_b 18.27830(10) _cell_length_c 37.2971(3) _cell_angle_alpha 90 _cell_angle_beta 96.0302(3) _cell_angle_gamma 90 _cell_volume 11851.34(13) _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'C 1 2/c 1 ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 'x+1/2,y+1/2,z' '-x+1/2,-y+1/2,-z' '-x,y,-z+1/2' 'x,-y,z+1/2' '-x+1/2,y+1/2,-z+1/2' 'x+1/2,-y+1/2,z+1/2' 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 C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 # Given Formula = C53 H48 B2 Cl2 F24 Fe1 N1 O1 P1 # Dc = 1.51 Fooo = 5520.00 Mu = 4.86 M = 1350.27 # Found Formula = C54 H50 B2 Cl2 F24 Fe1 N1 O1 P1 # Dc = 1.53 FOOO = 5520.00 Mu = 4.87 M = 1364.30 _chemical_formula_sum 'C54 H50 B2 Cl2 F24 Fe1 N1 O1 P1' _chemical_formula_moiety 'C32 H12 B F24 C21 H36 B Fe1 N1 O1 P1, C H2 Cl2' _chemical_compound_source . _chemical_formula_weight 1364.30 _cell_measurement_reflns_used 13288 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description 'block' _exptl_crystal_colour 'clear_pale_yellow' _exptl_crystal_size_min 0.24 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 5520 _exptl_absorpt_coefficient_mu 0.487 # Sheldrick geometric approximatio 0.88 0.89 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.89 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type 'Area' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 63388 _reflns_number_total 13462 _diffrn_reflns_av_R_equivalents 0.053 # Number of reflections with Friedels Law is 13462 # Number of reflections without Friedels Law is 25599 # Theoretical number of reflections is about 13611 _diffrn_reflns_theta_min 5.097 _diffrn_reflns_theta_max 27.498 _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.848 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 48 _reflns_limit_h_min -22 _reflns_limit_h_max 22 _reflns_limit_k_min 0 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 48 _oxford_diffrn_Wilson_B_factor 2.75 _oxford_diffrn_Wilson_scale 86.59 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.70 _refine_diff_density_max 0.92 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 13461 _refine_ls_number_restraints 12 _refine_ls_number_parameters 787 _oxford_refine_ls_R_factor_ref 0.1025 _refine_ls_wR_factor_ref 0.1711 _refine_ls_goodness_of_fit_ref 0.9550 _refine_ls_shift/su_max 0.000378 # The values computed from all data _oxford_reflns_number_all 13462 _refine_ls_R_factor_all 0.1025 _refine_ls_wR_factor_all 0.1711 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 8800 _refine_ls_R_factor_gt 0.0636 _refine_ls_wR_factor_gt 0.1516 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration '.' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.08P)^2^ +38.92P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Fe1 Fe 0.31911(3) 0.13136(3) 0.405790(13) 0.0348 1.0000 Uani . . . . . . . P2 P 0.40531(5) 0.21763(5) 0.41401(2) 0.0358 1.0000 Uani . . . . . . . C3 C 0.4319(2) 0.2369(2) 0.46151(11) 0.0528 1.0000 Uani . . . . . . . C4 C 0.3788(2) 0.3066(2) 0.39553(11) 0.0500 1.0000 Uani . . . . . . . C5 C 0.4973(2) 0.2015(2) 0.39673(11) 0.0530 1.0000 Uani . . . . . . . C6 C 0.2751(4) 0.0371(3) 0.4261(2) 0.0945 1.0000 Uani . . . . . . . C7 C 0.3438(5) 0.0520(3) 0.44625(15) 0.0864 1.0000 Uani . . . . . . . C8 C 0.3992(3) 0.0505(2) 0.42408(15) 0.0639 1.0000 Uani . . . . . . . C9 C 0.3697(3) 0.0353(2) 0.38904(12) 0.0543 1.0000 Uani . . . . . . . C10 C 0.2896(3) 0.0256(2) 0.38937(17) 0.0776 1.0000 Uani . . . . . . . C11 C 0.25289(19) 0.1884(2) 0.42373(10) 0.0419 1.0000 Uani . . . . . . . O12 O 0.20952(15) 0.22535(16) 0.43567(9) 0.0599 1.0000 Uani . . . . . . . B13 B 0.2872(2) 0.1667(2) 0.36108(11) 0.0356 1.0000 Uani . . . . . . . N14 N 0.26341(15) 0.19006(16) 0.32749(7) 0.0366 1.0000 Uani . . . . . . . C15 C 0.1812(2) 0.2002(2) 0.31397(10) 0.0424 1.0000 Uani . . . . . . . C16 C 0.1354(2) 0.1320(2) 0.31869(16) 0.0685 1.0000 Uani . . . . . . . C17 C 0.0513(2) 0.1424(3) 0.30403(19) 0.0876 1.0000 Uani . . . . . . . C18 C 0.0160(2) 0.2073(3) 0.32107(13) 0.0601 1.0000 Uani . . . . . . . C19 C 0.0619(2) 0.2753(3) 0.31690(15) 0.0708 1.0000 Uani . . . . . . . C20 C 0.1461(2) 0.2649(2) 0.33136(14) 0.0635 1.0000 Uani . . . . . . . C21 C 0.32388(19) 0.1972(2) 0.30229(9) 0.0394 1.0000 Uani . . . . . . . C22 C 0.3188(2) 0.1364(2) 0.27460(11) 0.0535 1.0000 Uani . . . . . . . C23 C 0.3843(3) 0.1430(3) 0.25095(12) 0.0617 1.0000 Uani . . . . . . . C24 C 0.3846(2) 0.2175(3) 0.23330(11) 0.0659 1.0000 Uani . . . . . . . C25 C 0.3901(2) 0.2773(3) 0.26105(11) 0.0588 1.0000 Uani . . . . . . . C26 C 0.3247(2) 0.2728(2) 0.28509(10) 0.0497 1.0000 Uani . . . . . . . Cl27 Cl 0.72605(7) 0.62230(6) 0.52050(3) 0.0697 1.0000 Uani . . . . . . . C28 C 0.6779(3) 0.5523(2) 0.54052(12) 0.0569 1.0000 Uani . . . . . . . Cl29 Cl 0.72286(8) 0.52852(6) 0.58326(3) 0.0753 1.0000 Uani . . . . . . . F30 F 0.85644(17) 0.38602(12) 0.47575(6) 0.0660 1.0000 Uani . . . . . . . C31 C 0.8581(2) 0.39340(18) 0.51120(9) 0.0364 1.0000 Uani . . . . . . . F32 F 0.92969(16) 0.41237(15) 0.52255(8) 0.0850 1.0000 Uani . . . . . . . F33 F 0.81564(17) 0.45090(12) 0.51661(7) 0.0767 1.0000 Uani . . . . . . . C34 C 0.83446(17) 0.32559(16) 0.52940(8) 0.0277 1.0000 Uani . . . . . . . C35 C 0.79352(16) 0.33019(16) 0.55952(8) 0.0268 1.0000 Uani . . . . . . . C36 C 0.77425(15) 0.26885(16) 0.57888(7) 0.0241 1.0000 Uani . . . . . . . C37 C 0.79773(16) 0.20152(16) 0.56585(8) 0.0252 1.0000 Uani . . . . . . . C38 C 0.83926(17) 0.19607(16) 0.53612(8) 0.0264 1.0000 Uani . . . . . . . C39 C 0.85821(17) 0.25771(17) 0.51756(8) 0.0294 1.0000 Uani . . . . . . . C40 C 0.86955(19) 0.12365(18) 0.52587(9) 0.0355 1.0000 Uani . . . . . . . F41 F 0.87181(18) 0.11604(12) 0.49086(6) 0.0710 1.0000 Uani . . . . . . . F42 F 0.83088(17) 0.06739(11) 0.53621(8) 0.0753 1.0000 Uani . . . . . . . F43 F 0.94111(16) 0.11283(15) 0.54056(9) 0.0910 1.0000 Uani . . . . . . . B44 B 0.72460(18) 0.27533(18) 0.61403(8) 0.0240 1.0000 Uani . . . . . . . C45 C 0.74746(16) 0.34929(15) 0.63744(7) 0.0241 1.0000 Uani . . . . . . . C46 C 0.82123(16) 0.38026(16) 0.64010(8) 0.0264 1.0000 Uani . . . . . . . C47 C 0.84056(17) 0.44300(17) 0.66003(9) 0.0320 1.0000 Uani . . . . . . . C48 C 0.78699(19) 0.47751(18) 0.67905(9) 0.0352 1.0000 Uani . . . . . . . C49 C 0.71464(17) 0.44721(17) 0.67799(8) 0.0310 1.0000 Uani . . . . . . . C50 C 0.69549(16) 0.38427(17) 0.65804(8) 0.0282 1.0000 Uani . . . . . . . C51 C 0.6546(2) 0.4820(2) 0.69835(10) 0.0461 1.0000 Uani . . . . . . . F52 F 0.59056(14) 0.49472(19) 0.67823(8) 0.0927 1.0000 Uani . . . . . . . F53 F 0.67683(15) 0.54350(17) 0.71425(10) 0.0989 1.0000 Uani . . . . . . . F54 F 0.6334(2) 0.4390(2) 0.72416(9) 0.1046 1.0000 Uani . . . . . . . C55 C 0.9203(2) 0.4725(2) 0.66062(12) 0.0491 1.0000 Uani . . . . . . . F56 F 0.94015(15) 0.48288(18) 0.62718(8) 0.0853 1.0000 Uani . . . . . . . F57 F 0.93020(17) 0.53428(19) 0.67763(13) 0.1385 1.0000 Uani . . . . . . . F58 F 0.97332(12) 0.42600(16) 0.67446(7) 0.0732 1.0000 Uani . . . . . . . C59 C 0.74451(16) 0.20763(15) 0.64259(7) 0.0236 1.0000 Uani . . . . . . . C60 C 0.81809(16) 0.17672(16) 0.64828(8) 0.0256 1.0000 Uani . . . . . . . C61 C 0.83666(17) 0.12206(16) 0.67362(8) 0.0290 1.0000 Uani . . . . . . . C62 C 0.78283(18) 0.09706(17) 0.69518(8) 0.0305 1.0000 Uani . . . . . . . C63 C 0.71028(17) 0.12795(17) 0.69091(8) 0.0289 1.0000 Uani . . . . . . . C64 C 0.69148(16) 0.18177(16) 0.66510(8) 0.0265 1.0000 Uani . . . . . . . C65 C 0.65009(19) 0.10328(19) 0.71383(9) 0.0415 1.0000 Uani D . . . . . . C69 C 0.91535(19) 0.08920(19) 0.67609(9) 0.0378 1.0000 Uani . . . . . . . F70 F 0.93468(13) 0.05468(15) 0.70711(6) 0.0695 1.0000 Uani . . . . . . . F71 F 0.92189(13) 0.03986(14) 0.65047(7) 0.0678 1.0000 Uani . . . . . . . F72 F 0.97001(12) 0.13847(13) 0.67300(8) 0.0703 1.0000 Uani . . . . . . . C73 C 0.63411(16) 0.27635(16) 0.59714(7) 0.0244 1.0000 Uani . . . . . . . C74 C 0.59152(16) 0.21217(16) 0.59015(8) 0.0265 1.0000 Uani . . . . . . . C75 C 0.51547(16) 0.21345(16) 0.57444(8) 0.0274 1.0000 Uani . . . . . . . C76 C 0.47959(17) 0.27901(18) 0.56476(8) 0.0312 1.0000 Uani . . . . . . . C77 C 0.52064(17) 0.34284(17) 0.57110(8) 0.0297 1.0000 Uani . . . . . . . C78 C 0.59657(16) 0.34177(16) 0.58685(8) 0.0264 1.0000 Uani . . . . . . . C79 C 0.48153(19) 0.41460(19) 0.56199(10) 0.0411 1.0000 Uani . . . . . . . F80 F 0.42535(19) 0.42724(16) 0.58135(10) 0.1053 1.0000 Uani . . . . . . . F81 F 0.4479(2) 0.41636(17) 0.52867(8) 0.1133 1.0000 Uani . . . . . . . F82 F 0.52653(15) 0.47054(13) 0.56410(12) 0.1066 1.0000 Uani . . . . . . . C83 C 0.47009(18) 0.14437(19) 0.56884(9) 0.0356 1.0000 Uani . . . . . . . F84 F 0.51010(14) 0.08471(12) 0.57576(10) 0.0856 1.0000 Uani . . . . . . . F85 F 0.41306(15) 0.14124(14) 0.58923(9) 0.0809 1.0000 Uani . . . . . . . F86 F 0.4360(2) 0.13747(17) 0.53592(8) 0.1077 1.0000 Uani . . . . . . . H31 H 0.4527 0.1924 0.4718 0.0768 1.0000 Uiso . . . . . . . H33 H 0.4700 0.2753 0.4626 0.0768 1.0000 Uiso . . . . . . . H32 H 0.3869 0.2515 0.4720 0.0768 1.0000 Uiso . . . . . . . H41 H 0.3767 0.3046 0.3696 0.0731 1.0000 Uiso . . . . . . . H43 H 0.4166 0.3419 0.4045 0.0728 1.0000 Uiso . . . . . . . H42 H 0.3282 0.3191 0.4030 0.0714 1.0000 Uiso . . . . . . . H51 H 0.4878 0.1979 0.3715 0.0783 1.0000 Uiso . . . . . . . H53 H 0.5301 0.2418 0.4036 0.0788 1.0000 Uiso . . . . . . . H52 H 0.5179 0.1569 0.4069 0.0788 1.0000 Uiso . . . . . . . H61 H 0.2251 0.0331 0.4353 0.1178 1.0000 Uiso . . . . . . . H71 H 0.3507 0.0636 0.4724 0.1052 1.0000 Uiso . . . . . . . H81 H 0.4528 0.0608 0.4318 0.0746 1.0000 Uiso . . . . . . . H91 H 0.3982 0.0305 0.3684 0.0655 1.0000 Uiso . . . . . . . H101 H 0.2528 0.0143 0.3693 0.0892 1.0000 Uiso . . . . . . . H151 H 0.1777 0.2101 0.2883 0.0503 1.0000 Uiso . . . . . . . H161 H 0.1380 0.1226 0.3445 0.0800 1.0000 Uiso . . . . . . . H162 H 0.1577 0.0906 0.3067 0.0803 1.0000 Uiso . . . . . . . H171 H 0.0219 0.0992 0.3089 0.1024 1.0000 Uiso . . . . . . . H172 H 0.0479 0.1503 0.2782 0.1021 1.0000 Uiso . . . . . . . H182 H 0.0146 0.1980 0.3469 0.0710 1.0000 Uiso . . . . . . . H181 H -0.0352 0.2142 0.3092 0.0704 1.0000 Uiso . . . . . . . H191 H 0.0406 0.3153 0.3298 0.0831 1.0000 Uiso . . . . . . . H192 H 0.0577 0.2869 0.2913 0.0827 1.0000 Uiso . . . . . . . H201 H 0.1491 0.2552 0.3572 0.0740 1.0000 Uiso . . . . . . . H202 H 0.1757 0.3083 0.3280 0.0741 1.0000 Uiso . . . . . . . H211 H 0.3741 0.1913 0.3170 0.0468 1.0000 Uiso . . . . . . . H222 H 0.3205 0.0885 0.2863 0.0642 1.0000 Uiso . . . . . . . H221 H 0.2700 0.1422 0.2593 0.0637 1.0000 Uiso . . . . . . . H231 H 0.4326 0.1359 0.2660 0.0747 1.0000 Uiso . . . . . . . H232 H 0.3776 0.1054 0.2324 0.0755 1.0000 Uiso . . . . . . . H241 H 0.4276 0.2215 0.2188 0.0791 1.0000 Uiso . . . . . . . H242 H 0.3361 0.2230 0.2176 0.0786 1.0000 Uiso . . . . . . . H252 H 0.4397 0.2731 0.2757 0.0681 1.0000 Uiso . . . . . . . H251 H 0.3871 0.3246 0.2494 0.0691 1.0000 Uiso . . . . . . . H261 H 0.3304 0.3105 0.3038 0.0590 1.0000 Uiso . . . . . . . H262 H 0.2769 0.2801 0.2700 0.0592 1.0000 Uiso . . . . . . . H281 H 0.6262 0.5691 0.5434 0.0670 1.0000 Uiso . . . . . . . H282 H 0.6776 0.5101 0.5248 0.0670 1.0000 Uiso . . . . . . . H351 H 0.7782 0.3767 0.5667 0.0318 1.0000 Uiso . . . . . . . H371 H 0.7850 0.1582 0.5772 0.0296 1.0000 Uiso . . . . . . . H391 H 0.8852 0.2552 0.4977 0.0347 1.0000 Uiso . . . . . . . H461 H 0.8591 0.3587 0.6282 0.0311 1.0000 Uiso . . . . . . . H481 H 0.7996 0.5203 0.6917 0.0410 1.0000 Uiso . . . . . . . H501 H 0.6462 0.3642 0.6585 0.0326 1.0000 Uiso . . . . . . . H601 H 0.8558 0.1927 0.6347 0.0299 1.0000 Uiso . . . . . . . H621 H 0.7955 0.0610 0.7119 0.0360 1.0000 Uiso . . . . . . . H641 H 0.6418 0.2016 0.6629 0.0307 1.0000 Uiso . . . . . . . H741 H 0.6148 0.1678 0.5957 0.0311 1.0000 Uiso . . . . . . . H761 H 0.4288 0.2792 0.5548 0.0366 1.0000 Uiso . . . . . . . H781 H 0.6236 0.3855 0.5904 0.0307 1.0000 Uiso . . . . . . . F660 F 0.67468(18) 0.0552(2) 0.73844(11) 0.0669 0.7000 Uani D . . . 1 . . F670 F 0.6220(3) 0.1594(2) 0.73100(13) 0.0865 0.7000 Uani D . . . 1 . . F680 F 0.5909(2) 0.0746(3) 0.69492(9) 0.0916 0.7000 Uani D . . . 1 . . F661 F 0.6754(6) 0.0967(6) 0.7482(2) 0.076(3) 0.3000 Uiso D . . . 2 . . F671 F 0.5892(5) 0.1438(5) 0.7146(3) 0.064(3) 0.3000 Uiso D . . . 2 . . F681 F 0.6211(7) 0.0388(4) 0.7044(3) 0.092(4) 0.3000 Uiso D . . . 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 Fe1 0.0312(2) 0.0352(3) 0.0394(3) 0.0071(2) 0.01010(19) 0.0041(2) P2 0.0278(4) 0.0433(5) 0.0368(5) 0.0012(4) 0.0062(3) 0.0041(4) C3 0.043(2) 0.068(3) 0.046(2) -0.0054(19) -0.0012(17) 0.0047(19) C4 0.052(2) 0.041(2) 0.057(2) -0.0016(17) 0.0018(19) -0.0068(17) C5 0.0287(18) 0.078(3) 0.053(2) -0.009(2) 0.0109(16) -0.0006(18) C6 0.087(4) 0.043(3) 0.168(7) 0.040(3) 0.081(4) 0.011(3) C7 0.139(6) 0.057(3) 0.067(3) 0.027(3) 0.026(4) 0.028(3) C8 0.057(3) 0.042(2) 0.089(4) 0.001(2) -0.010(2) 0.019(2) C9 0.061(3) 0.036(2) 0.069(3) -0.0019(19) 0.020(2) 0.0075(18) C10 0.078(3) 0.034(2) 0.112(4) 0.006(2) -0.034(3) -0.011(2) C11 0.0307(17) 0.045(2) 0.052(2) 0.0036(17) 0.0103(16) -0.0017(15) O12 0.0371(14) 0.0607(18) 0.086(2) -0.0118(15) 0.0254(14) 0.0071(13) B13 0.0267(18) 0.038(2) 0.043(2) 0.0015(17) 0.0073(16) -0.0010(15) N14 0.0303(14) 0.0450(16) 0.0346(15) 0.0031(12) 0.0047(11) -0.0037(12) C15 0.0323(17) 0.056(2) 0.0386(19) 0.0065(16) 0.0046(14) 0.0037(16) C16 0.0293(19) 0.054(3) 0.122(4) -0.016(3) 0.003(2) -0.0010(18) C17 0.030(2) 0.069(3) 0.160(6) -0.019(3) -0.005(3) 0.001(2) C18 0.0313(19) 0.074(3) 0.076(3) 0.020(2) 0.0085(19) 0.0077(19) C19 0.043(2) 0.064(3) 0.104(4) 0.005(3) 0.001(2) 0.018(2) C20 0.046(2) 0.045(2) 0.097(4) -0.005(2) -0.004(2) 0.0043(19) C21 0.0327(17) 0.050(2) 0.0360(18) 0.0060(15) 0.0054(14) -0.0030(15) C22 0.056(2) 0.061(3) 0.046(2) -0.0093(19) 0.0151(18) -0.009(2) C23 0.055(2) 0.082(3) 0.050(2) -0.013(2) 0.017(2) -0.004(2) C24 0.047(2) 0.112(4) 0.041(2) 0.009(2) 0.0120(18) -0.007(2) C25 0.051(2) 0.076(3) 0.050(2) 0.024(2) 0.0062(19) -0.009(2) C26 0.048(2) 0.055(2) 0.045(2) 0.0148(18) 0.0058(17) -0.0007(18) Cl27 0.0728(7) 0.0622(7) 0.0770(8) 0.0017(6) 0.0216(6) 0.0020(6) C28 0.065(3) 0.047(2) 0.058(3) -0.0119(19) 0.002(2) -0.003(2) Cl29 0.1045(10) 0.0542(6) 0.0650(7) 0.0008(5) -0.0006(6) 0.0269(6) F30 0.116(2) 0.0492(13) 0.0364(12) 0.0107(10) 0.0273(13) -0.0037(13) C31 0.0407(19) 0.0343(17) 0.0357(18) 0.0054(14) 0.0108(15) 0.0094(15) F32 0.0700(17) 0.0759(18) 0.103(2) 0.0449(16) -0.0195(15) -0.0343(15) F33 0.108(2) 0.0416(13) 0.0918(19) 0.0293(13) 0.0630(17) 0.0302(13) C34 0.0266(15) 0.0312(16) 0.0250(15) 0.0033(12) 0.0024(12) 0.0041(12) C35 0.0263(15) 0.0286(15) 0.0251(15) 0.0004(12) 0.0015(12) 0.0065(12) C36 0.0190(13) 0.0296(15) 0.0232(14) 0.0022(11) -0.0001(11) 0.0042(11) C37 0.0236(14) 0.0282(15) 0.0237(14) 0.0006(11) 0.0017(11) 0.0012(12) C38 0.0267(15) 0.0266(15) 0.0259(15) -0.0019(12) 0.0025(12) 0.0041(12) C39 0.0277(15) 0.0355(17) 0.0259(15) 0.0005(12) 0.0066(12) 0.0040(13) C40 0.0408(18) 0.0336(17) 0.0338(17) -0.0025(14) 0.0126(14) 0.0048(14) F41 0.130(2) 0.0472(13) 0.0419(13) -0.0052(10) 0.0373(14) 0.0212(14) F42 0.111(2) 0.0289(11) 0.0982(19) -0.0072(12) 0.0686(17) -0.0036(12) F43 0.0664(17) 0.0588(16) 0.139(3) -0.0326(17) -0.0307(17) 0.0375(14) B44 0.0218(15) 0.0285(17) 0.0220(16) 0.0000(13) 0.0029(12) 0.0041(13) C45 0.0217(14) 0.0274(15) 0.0231(14) 0.0042(11) 0.0028(11) 0.0052(11) C46 0.0222(14) 0.0295(15) 0.0284(15) 0.0009(12) 0.0062(12) 0.0043(12) C47 0.0259(15) 0.0328(16) 0.0377(17) -0.0022(13) 0.0044(13) -0.0041(13) C48 0.0356(17) 0.0315(17) 0.0381(18) -0.0091(14) 0.0018(14) 0.0007(14) C49 0.0287(16) 0.0343(16) 0.0301(16) -0.0053(13) 0.0036(13) 0.0051(13) C50 0.0235(14) 0.0353(16) 0.0261(15) -0.0016(12) 0.0044(12) 0.0010(12) C51 0.0355(19) 0.055(2) 0.048(2) -0.0224(18) 0.0079(16) 0.0050(17) F52 0.0463(14) 0.148(3) 0.0815(19) -0.0513(19) -0.0053(13) 0.0471(16) F53 0.0617(16) 0.097(2) 0.144(3) -0.088(2) 0.0368(17) -0.0113(15) F54 0.113(3) 0.115(3) 0.100(2) 0.015(2) 0.078(2) 0.041(2) C55 0.037(2) 0.044(2) 0.068(3) -0.0105(19) 0.0131(18) -0.0096(17) F56 0.0575(16) 0.109(2) 0.092(2) 0.0311(17) 0.0225(14) -0.0256(15) F57 0.0586(18) 0.106(2) 0.259(5) -0.118(3) 0.059(2) -0.0485(17) F58 0.0279(11) 0.101(2) 0.0886(19) 0.0158(16) -0.0045(11) -0.0101(13) C59 0.0238(14) 0.0236(14) 0.0233(14) -0.0042(11) 0.0018(11) 0.0029(11) C60 0.0243(14) 0.0266(15) 0.0260(15) -0.0013(12) 0.0028(11) 0.0012(12) C61 0.0266(15) 0.0309(16) 0.0284(15) -0.0022(12) -0.0025(12) 0.0054(13) C62 0.0332(16) 0.0309(16) 0.0266(15) 0.0036(12) -0.0015(13) 0.0045(13) C63 0.0298(15) 0.0340(16) 0.0227(14) 0.0026(12) 0.0020(12) -0.0006(13) C64 0.0215(14) 0.0308(15) 0.0271(15) 0.0014(12) 0.0022(11) 0.0032(12) C65 0.0409(19) 0.046(2) 0.0387(19) 0.0117(16) 0.0078(16) 0.0042(16) C69 0.0330(17) 0.0407(19) 0.0388(19) 0.0020(15) -0.0006(14) 0.0112(15) F70 0.0542(14) 0.0993(19) 0.0546(14) 0.0281(13) 0.0040(11) 0.0456(14) F71 0.0540(14) 0.0804(17) 0.0679(16) -0.0266(13) 0.0005(12) 0.0350(13) F72 0.0236(10) 0.0630(15) 0.122(2) 0.0171(15) -0.0039(12) 0.0057(10) C73 0.0219(14) 0.0301(15) 0.0217(14) -0.0005(11) 0.0052(11) 0.0026(12) C74 0.0250(14) 0.0309(15) 0.0241(15) 0.0021(12) 0.0045(11) 0.0061(12) C75 0.0240(14) 0.0333(16) 0.0251(15) -0.0001(12) 0.0034(12) 0.0019(12) C76 0.0212(14) 0.0417(18) 0.0303(16) 0.0021(13) 0.0009(12) 0.0045(13) C77 0.0252(15) 0.0350(16) 0.0289(16) 0.0030(13) 0.0027(12) 0.0079(13) C78 0.0241(14) 0.0296(15) 0.0257(15) 0.0006(12) 0.0032(12) 0.0028(12) C79 0.0280(17) 0.040(2) 0.054(2) 0.0020(16) -0.0023(15) 0.0107(15) F80 0.107(2) 0.0717(19) 0.152(3) 0.0409(19) 0.083(2) 0.0602(17) F81 0.158(3) 0.086(2) 0.082(2) 0.0017(17) -0.054(2) 0.069(2) F82 0.0492(15) 0.0375(14) 0.225(4) 0.0355(19) -0.0222(19) 0.0097(12) C83 0.0242(15) 0.0420(19) 0.0401(19) 0.0020(15) 0.0005(13) -0.0007(14) F84 0.0430(13) 0.0345(12) 0.175(3) -0.0065(15) -0.0067(16) -0.0040(11) F85 0.0636(16) 0.0595(15) 0.129(2) -0.0140(15) 0.0551(17) -0.0219(13) F86 0.153(3) 0.096(2) 0.0630(18) 0.0129(16) -0.0405(19) -0.081(2) F660 0.049(2) 0.084(3) 0.071(2) 0.060(2) 0.0234(17) 0.0149(19) F670 0.108(3) 0.073(3) 0.094(3) -0.013(2) 0.084(3) -0.012(3) F680 0.042(2) 0.177(5) 0.054(2) 0.037(3) -0.0090(17) -0.064(3) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 0.12328(5) 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 Fe1 . P2 . 2.1804(10) yes Fe1 . C6 . 2.063(4) yes Fe1 . C7 . 2.105(5) yes Fe1 . C8 . 2.100(4) yes Fe1 . C9 . 2.091(4) yes Fe1 . C10 . 2.077(4) yes Fe1 . C11 . 1.743(4) yes Fe1 . B13 . 1.821(4) yes P2 . C3 . 1.818(4) yes P2 . C4 . 1.807(4) yes P2 . C5 . 1.818(4) yes C3 . H31 . 0.955 no C3 . H33 . 0.966 no C3 . H32 . 0.952 no C4 . H41 . 0.963 no C4 . H43 . 0.959 no C4 . H42 . 0.984 no C5 . H51 . 0.941 no C5 . H53 . 0.951 no C5 . H52 . 0.954 no C6 . C7 . 1.376(9) yes C6 . C10 . 1.434(8) yes C6 . H61 . 0.974 no C7 . C8 . 1.339(8) yes C7 . H71 . 0.992 no C8 . C9 . 1.383(6) yes C8 . H81 . 0.969 no C9 . C10 . 1.412(7) yes C9 . H91 . 0.965 no C10 . H101 . 0.956 no C11 . O12 . 1.140(4) yes B13 . N14 . 1.347(5) yes N14 . C15 . 1.483(4) yes N14 . C21 . 1.492(4) yes C15 . C16 . 1.503(6) yes C15 . C20 . 1.510(6) yes C15 . H151 . 0.969 no C16 . C17 . 1.525(6) yes C16 . H161 . 0.973 no C16 . H162 . 0.979 no C17 . C18 . 1.508(7) yes C17 . H171 . 0.970 no C17 . H172 . 0.971 no C18 . C19 . 1.497(6) yes C18 . H182 . 0.981 no C18 . H181 . 0.965 no C19 . C20 . 1.525(6) yes C19 . H191 . 0.971 no C19 . H192 . 0.974 no C20 . H201 . 0.977 no C20 . H202 . 0.964 no C21 . C22 . 1.514(5) yes C21 . C26 . 1.523(5) yes C21 . H211 . 0.991 no C22 . C23 . 1.521(6) yes C22 . H222 . 0.977 no C22 . H221 . 0.981 no C23 . C24 . 1.514(7) yes C23 . H231 . 0.972 no C23 . H232 . 0.971 no C24 . C25 . 1.501(7) yes C24 . H241 . 0.973 no C24 . H242 . 0.983 no C25 . C26 . 1.527(6) yes C25 . H252 . 0.979 no C25 . H251 . 0.968 no C26 . H261 . 0.978 no C26 . H262 . 0.966 no Cl27 . C28 . 1.742(5) yes C28 . Cl29 . 1.756(4) yes C28 . H281 . 0.972 no C28 . H282 . 0.969 no F30 . C31 . 1.326(4) yes C31 . F32 . 1.324(4) yes C31 . F33 . 1.315(4) yes C31 . C34 . 1.492(4) yes C34 . C35 . 1.396(4) yes C34 . C39 . 1.395(4) yes C35 . C36 . 1.394(4) yes C35 . H351 . 0.939 no C36 . C37 . 1.400(4) yes C36 . B44 . 1.651(4) yes C37 . C38 . 1.391(4) yes C37 . H371 . 0.935 no C38 . C39 . 1.381(4) yes C38 . C40 . 1.490(4) yes C39 . H391 . 0.921 no C40 . F41 . 1.318(4) yes C40 . F42 . 1.311(4) yes C40 . F43 . 1.327(4) yes B44 . C45 . 1.636(4) yes B44 . C59 . 1.646(4) yes B44 . C73 . 1.640(4) yes C45 . C46 . 1.402(4) yes C45 . C50 . 1.404(4) yes C46 . C47 . 1.389(4) yes C46 . H461 . 0.924 no C47 . C48 . 1.385(4) yes C47 . C55 . 1.493(5) yes C48 . C49 . 1.377(4) yes C48 . H481 . 0.929 no C49 . C50 . 1.392(4) yes C49 . C51 . 1.500(4) yes C50 . H501 . 0.938 no C51 . F52 . 1.301(4) yes C51 . F53 . 1.312(4) yes C51 . F54 . 1.324(5) yes C55 . F56 . 1.343(5) yes C55 . F57 . 1.298(5) yes C55 . F58 . 1.322(5) yes C59 . C60 . 1.401(4) yes C59 . C64 . 1.397(4) yes C60 . C61 . 1.390(4) yes C60 . H601 . 0.920 no C61 . C62 . 1.379(4) yes C61 . C69 . 1.495(4) yes C62 . C63 . 1.382(4) yes C62 . H621 . 0.918 no C63 . C64 . 1.391(4) yes C63 . C65 . 1.493(4) yes C64 . H641 . 0.937 no C65 . F660 . 1.311(4) yes C65 . F670 . 1.330(4) yes C65 . F680 . 1.301(4) yes C69 . F70 . 1.330(4) yes C69 . F71 . 1.328(4) yes C69 . F72 . 1.327(4) yes C73 . C74 . 1.399(4) yes C73 . C78 . 1.398(4) yes C74 . C75 . 1.395(4) yes C74 . H741 . 0.921 no C75 . C76 . 1.383(4) yes C75 . C83 . 1.494(4) yes C76 . C77 . 1.377(5) yes C76 . H761 . 0.926 no C77 . C78 . 1.394(4) yes C77 . C79 . 1.502(4) yes C78 . H781 . 0.931 no C79 . F80 . 1.299(4) yes C79 . F81 . 1.318(4) yes C79 . F82 . 1.287(4) yes C83 . F84 . 1.307(4) yes C83 . F85 . 1.317(4) yes C83 . F86 . 1.313(4) yes 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 P2 . Fe1 . C6 . 146.2(3) yes P2 . Fe1 . C7 . 108.1(2) yes C6 . Fe1 . C7 . 38.5(3) yes P2 . Fe1 . C8 . 92.03(13) yes C6 . Fe1 . C8 . 63.6(2) yes C7 . Fe1 . C8 . 37.1(2) yes P2 . Fe1 . C9 . 109.99(12) yes C6 . Fe1 . C9 . 66.04(19) yes C7 . Fe1 . C9 . 64.8(2) yes C8 . Fe1 . C9 . 38.53(18) yes P2 . Fe1 . C10 . 149.45(18) yes C6 . Fe1 . C10 . 40.5(2) yes C7 . Fe1 . C10 . 66.1(2) yes C8 . Fe1 . C10 . 64.99(18) yes C9 . Fe1 . C10 . 39.6(2) yes P2 . Fe1 . C11 . 89.45(12) yes C6 . Fe1 . C11 . 94.05(18) yes C7 . Fe1 . C11 . 103.4(2) yes C8 . Fe1 . C11 . 138.0(2) yes C9 . Fe1 . C11 . 159.38(16) yes P2 . Fe1 . B13 . 90.74(12) yes C6 . Fe1 . B13 . 122.8(3) yes C7 . Fe1 . B13 . 157.1(2) yes C8 . Fe1 . B13 . 132.63(19) yes C9 . Fe1 . B13 . 97.07(18) yes C10 . Fe1 . C11 . 121.1(2) yes C10 . Fe1 . B13 . 91.0(2) yes C11 . Fe1 . B13 . 89.26(17) yes Fe1 . P2 . C3 . 112.30(14) yes Fe1 . P2 . C4 . 116.84(13) yes C3 . P2 . C4 . 103.06(19) yes Fe1 . P2 . C5 . 117.21(14) yes C3 . P2 . C5 . 103.41(18) yes C4 . P2 . C5 . 102.2(2) yes P2 . C3 . H31 . 105.9 no P2 . C3 . H33 . 106.5 no H31 . C3 . H33 . 111.7 no P2 . C3 . H32 . 108.5 no H31 . C3 . H32 . 111.6 no H33 . C3 . H32 . 112.2 no P2 . C4 . H41 . 109.3 no P2 . C4 . H43 . 109.5 no H41 . C4 . H43 . 109.2 no P2 . C4 . H42 . 107.7 no H41 . C4 . H42 . 110.6 no H43 . C4 . H42 . 110.5 no P2 . C5 . H51 . 107.2 no P2 . C5 . H53 . 108.0 no H51 . C5 . H53 . 111.3 no P2 . C5 . H52 . 108.0 no H51 . C5 . H52 . 110.9 no H53 . C5 . H52 . 111.2 no Fe1 . C6 . C7 . 72.4(3) yes Fe1 . C6 . C10 . 70.2(3) yes C7 . C6 . C10 . 108.6(4) yes Fe1 . C6 . H61 . 125.1 no C7 . C6 . H61 . 125.8 no C10 . C6 . H61 . 125.6 no Fe1 . C7 . C6 . 69.1(3) yes Fe1 . C7 . C8 . 71.2(3) yes C6 . C7 . C8 . 107.8(5) yes Fe1 . C7 . H71 . 123.4 no C6 . C7 . H71 . 126.0 no C8 . C7 . H71 . 126.2 no Fe1 . C8 . C7 . 71.6(3) yes Fe1 . C8 . C9 . 70.4(2) yes C7 . C8 . C9 . 111.4(5) yes Fe1 . C8 . H81 . 123.5 no C7 . C8 . H81 . 123.7 no C9 . C8 . H81 . 124.9 no Fe1 . C9 . C8 . 71.1(2) yes Fe1 . C9 . C10 . 69.7(2) yes C8 . C9 . C10 . 106.8(4) yes Fe1 . C9 . H91 . 125.8 no C8 . C9 . H91 . 126.8 no C10 . C9 . H91 . 126.3 no C6 . C10 . Fe1 . 69.2(3) yes C6 . C10 . C9 . 105.4(4) yes Fe1 . C10 . C9 . 70.7(2) yes C6 . C10 . H101 . 127.3 no Fe1 . C10 . H101 . 123.8 no C9 . C10 . H101 . 127.4 no Fe1 . C11 . O12 . 179.5(3) yes Fe1 . B13 . N14 . 177.7(3) yes B13 . N14 . C15 . 123.3(3) yes B13 . N14 . C21 . 116.4(3) yes C15 . N14 . C21 . 120.0(3) yes N14 . C15 . C16 . 111.5(3) yes N14 . C15 . C20 . 112.0(3) yes C16 . C15 . C20 . 110.7(3) yes N14 . C15 . H151 . 108.5 no C16 . C15 . H151 . 107.0 no C20 . C15 . H151 . 106.9 no C15 . C16 . C17 . 111.1(4) yes C15 . C16 . H161 . 106.9 no C17 . C16 . H161 . 108.6 no C15 . C16 . H162 . 110.1 no C17 . C16 . H162 . 110.3 no H161 . C16 . H162 . 109.6 no C16 . C17 . C18 . 111.6(4) yes C16 . C17 . H171 . 110.0 no C18 . C17 . H171 . 108.2 no C16 . C17 . H172 . 109.4 no C18 . C17 . H172 . 108.3 no H171 . C17 . H172 . 109.3 no C17 . C18 . C19 . 111.2(4) yes C17 . C18 . H182 . 109.3 no C19 . C18 . H182 . 108.3 no C17 . C18 . H181 . 108.1 no C19 . C18 . H181 . 108.9 no H182 . C18 . H181 . 110.9 no C18 . C19 . C20 . 111.5(4) yes C18 . C19 . H191 . 109.6 no C20 . C19 . H191 . 108.9 no C18 . C19 . H192 . 107.2 no C20 . C19 . H192 . 110.2 no H191 . C19 . H192 . 109.3 no C19 . C20 . C15 . 111.5(4) yes C19 . C20 . H201 . 108.8 no C15 . C20 . H201 . 107.5 no C19 . C20 . H202 . 111.3 no C15 . C20 . H202 . 109.9 no H201 . C20 . H202 . 107.6 no N14 . C21 . C22 . 111.8(3) yes N14 . C21 . C26 . 112.5(3) yes C22 . C21 . C26 . 112.4(3) yes N14 . C21 . H211 . 106.6 no C22 . C21 . H211 . 106.4 no C26 . C21 . H211 . 106.6 no C21 . C22 . C23 . 110.1(3) yes C21 . C22 . H222 . 110.8 no C23 . C22 . H222 . 110.0 no C21 . C22 . H221 . 107.5 no C23 . C22 . H221 . 108.4 no H222 . C22 . H221 . 109.9 no C22 . C23 . C24 . 111.1(4) yes C22 . C23 . H231 . 108.3 no C24 . C23 . H231 . 109.2 no C22 . C23 . H232 . 108.4 no C24 . C23 . H232 . 109.4 no H231 . C23 . H232 . 110.4 no C23 . C24 . C25 . 111.0(3) yes C23 . C24 . H241 . 110.2 no C25 . C24 . H241 . 109.4 no C23 . C24 . H242 . 108.0 no C25 . C24 . H242 . 109.0 no H241 . C24 . H242 . 109.2 no C24 . C25 . C26 . 111.5(4) yes C24 . C25 . H252 . 108.5 no C26 . C25 . H252 . 110.0 no C24 . C25 . H251 . 110.1 no C26 . C25 . H251 . 107.7 no H252 . C25 . H251 . 109.0 no C25 . C26 . C21 . 109.7(3) yes C25 . C26 . H261 . 110.7 no C21 . C26 . H261 . 110.1 no C25 . C26 . H262 . 107.8 no C21 . C26 . H262 . 109.0 no H261 . C26 . H262 . 109.6 no Cl27 . C28 . Cl29 . 112.4(2) yes Cl27 . C28 . H281 . 108.3 no Cl29 . C28 . H281 . 108.0 no Cl27 . C28 . H282 . 107.4 no Cl29 . C28 . H282 . 108.9 no H281 . C28 . H282 . 111.9 no F30 . C31 . F32 . 105.5(3) yes F30 . C31 . F33 . 106.3(3) yes F32 . C31 . F33 . 105.8(3) yes F30 . C31 . C34 . 113.0(3) yes F32 . C31 . C34 . 111.7(3) yes F33 . C31 . C34 . 113.9(3) yes C31 . C34 . C35 . 120.4(3) yes C31 . C34 . C39 . 119.3(3) yes C35 . C34 . C39 . 120.2(3) yes C34 . C35 . C36 . 122.7(3) yes C34 . C35 . H351 . 118.1 no C36 . C35 . H351 . 119.2 no C35 . C36 . C37 . 115.6(2) yes C35 . C36 . B44 . 122.0(2) yes C37 . C36 . B44 . 122.4(2) yes C36 . C37 . C38 . 122.4(3) yes C36 . C37 . H371 . 119.6 no C38 . C37 . H371 . 118.0 no C37 . C38 . C39 . 120.9(3) yes C37 . C38 . C40 . 119.8(3) yes C39 . C38 . C40 . 119.1(3) yes C34 . C39 . C38 . 118.2(3) yes C34 . C39 . H391 . 119.6 no C38 . C39 . H391 . 122.2 no C38 . C40 . F41 . 113.4(3) yes C38 . C40 . F42 . 114.4(3) yes F41 . C40 . F42 . 106.2(3) yes C38 . C40 . F43 . 111.8(3) yes F41 . C40 . F43 . 105.6(3) yes F42 . C40 . F43 . 104.7(3) yes C36 . B44 . C45 . 111.3(2) yes C36 . B44 . C59 . 111.5(2) yes C45 . B44 . C59 . 104.6(2) yes C36 . B44 . C73 . 105.2(2) yes C45 . B44 . C73 . 111.6(2) yes C59 . B44 . C73 . 112.8(2) yes B44 . C45 . C46 . 122.9(2) yes B44 . C45 . C50 . 122.2(2) yes C46 . C45 . C50 . 114.9(3) yes C45 . C46 . C47 . 122.8(3) yes C45 . C46 . H461 . 119.5 no C47 . C46 . H461 . 117.7 no C46 . C47 . C48 . 120.7(3) yes C46 . C47 . C55 . 118.7(3) yes C48 . C47 . C55 . 120.6(3) yes C47 . C48 . C49 . 118.1(3) yes C47 . C48 . H481 . 120.5 no C49 . C48 . H481 . 121.4 no C48 . C49 . C50 . 121.1(3) yes C48 . C49 . C51 . 120.3(3) yes C50 . C49 . C51 . 118.6(3) yes C45 . C50 . C49 . 122.4(3) yes C45 . C50 . H501 . 118.6 no C49 . C50 . H501 . 119.0 no C49 . C51 . F52 . 112.9(3) yes C49 . C51 . F53 . 113.7(3) yes F52 . C51 . F53 . 107.7(3) yes C49 . C51 . F54 . 112.4(3) yes F52 . C51 . F54 . 103.7(3) yes F53 . C51 . F54 . 105.8(3) yes C47 . C55 . F56 . 111.7(3) yes C47 . C55 . F57 . 113.5(3) yes F56 . C55 . F57 . 107.3(4) yes C47 . C55 . F58 . 112.9(3) yes F56 . C55 . F58 . 102.4(3) yes F57 . C55 . F58 . 108.5(4) yes B44 . C59 . C60 . 122.0(2) yes B44 . C59 . C64 . 122.3(2) yes C60 . C59 . C64 . 115.4(3) yes C59 . C60 . C61 . 122.6(3) yes C59 . C60 . H601 . 119.2 no C61 . C60 . H601 . 118.2 no C60 . C61 . C62 . 120.7(3) yes C60 . C61 . C69 . 118.6(3) yes C62 . C61 . C69 . 120.7(3) yes C61 . C62 . C63 . 118.1(3) yes C61 . C62 . H621 . 120.2 no C63 . C62 . H621 . 121.6 no C62 . C63 . C64 . 121.1(3) yes C62 . C63 . C65 . 120.3(3) yes C64 . C63 . C65 . 118.7(3) yes C59 . C64 . C63 . 122.1(3) yes C59 . C64 . H641 . 118.9 no C63 . C64 . H641 . 119.0 no C63 . C65 . F660 . 113.9(3) yes C63 . C65 . F670 . 111.2(3) yes F660 . C65 . F670 . 106.9(4) yes C63 . C65 . F680 . 112.3(3) yes F660 . C65 . F680 . 107.0(4) yes F670 . C65 . F680 . 105.0(4) yes C61 . C69 . F70 . 113.1(3) yes C61 . C69 . F71 . 112.1(3) yes F70 . C69 . F71 . 105.7(3) yes C61 . C69 . F72 . 112.8(3) yes F70 . C69 . F72 . 106.2(3) yes F71 . C69 . F72 . 106.3(3) yes B44 . C73 . C74 . 122.3(2) yes B44 . C73 . C78 . 121.4(3) yes C74 . C73 . C78 . 116.1(3) yes C73 . C74 . C75 . 121.9(3) yes C73 . C74 . H741 . 118.8 no C75 . C74 . H741 . 119.2 no C74 . C75 . C76 . 120.7(3) yes C74 . C75 . C83 . 120.9(3) yes C76 . C75 . C83 . 118.4(3) yes C75 . C76 . C77 . 118.4(3) yes C75 . C76 . H761 . 119.9 no C77 . C76 . H761 . 121.7 no C76 . C77 . C78 . 121.1(3) yes C76 . C77 . C79 . 119.0(3) yes C78 . C77 . C79 . 119.9(3) yes C73 . C78 . C77 . 121.8(3) yes C73 . C78 . H781 . 118.6 no C77 . C78 . H781 . 119.6 no C77 . C79 . F80 . 112.5(3) yes C77 . C79 . F81 . 112.5(3) yes F80 . C79 . F81 . 103.4(3) yes C77 . C79 . F82 . 114.8(3) yes F80 . C79 . F82 . 108.5(4) yes F81 . C79 . F82 . 104.3(4) yes C75 . C83 . F84 . 114.4(3) yes C75 . C83 . F85 . 112.3(3) yes F84 . C83 . F85 . 105.8(3) yes C75 . C83 . F86 . 113.2(3) yes F84 . C83 . F86 . 106.6(3) yes F85 . C83 . F86 . 103.8(3) yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C76 . H761 . O12 4_556 148 0.93 2.48 3.305(5) yes #============================================================================== data_10 #============================================================================== _audit_creation_date 08-09-17 _audit_creation_method CRYSTALS_ver_12.86 _oxford_structure_analysis_title '016dvdv08' _chemical_name_systematic . _chemical_melting_point . _cell_length_a 12.23900(10) _cell_length_b 17.1260(2) _cell_length_c 27.0465(3) _cell_angle_alpha 90 _cell_angle_beta 99.1154(4) _cell_angle_gamma 90 _cell_volume 5597.49(10) _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' '-x,y+1/2,-z+1/2' 'x,-y+1/2,z+1/2' 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 C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ru -1.2594 0.8363 19.2674 0.8085 12.9182 8.4347 4.8634 24.7997 1.5676 94.2928 5.3787 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C53 H36 B2 F24 N1 O1 P1 Ru1 # Dc = 1.56 Fooo = 2664.00 Mu = 4.28 M = 1312.49 # Found Formula = C53 H48 B2 F24.00 N1 O1 P1 Ru1 # Dc = 1.57 FOOO = 2664.00 Mu = 4.28 M = 1324.59 _chemical_formula_sum 'C53 H48 B2 F24 N1 O1 P1 Ru1' _chemical_formula_moiety 'C32 H12 B F24, C21 H36 B N1 O1 P1 Ru1' _chemical_compound_source . _chemical_formula_weight 1324.59 _cell_measurement_reflns_used 11864 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description 'block' _exptl_crystal_colour 'pale_yellow' _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.25 _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2664 _exptl_absorpt_coefficient_mu 0.428 # Sheldrick geometric approximatio 0.92 0.94 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 0.94 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type 'Area' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 50002 _reflns_number_total 12677 _diffrn_reflns_av_R_equivalents 0.042 # Number of reflections with Friedels Law is 12677 # Number of reflections without Friedels Law is 23770 # Theoretical number of reflections is about 12824 _diffrn_reflns_theta_min 5.126 _diffrn_reflns_theta_max 27.475 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.552 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 35 _oxford_diffrn_Wilson_B_factor 2.11 _oxford_diffrn_Wilson_scale 28.18 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.93 _refine_diff_density_max 1.88 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 9103 _refine_ls_number_restraints 168 _refine_ls_number_parameters 800 _oxford_refine_ls_R_factor_ref 0.0584 _refine_ls_wR_factor_ref 0.0587 _refine_ls_goodness_of_fit_ref 1.1619 _refine_ls_shift/su_max 0.001242 # The values computed from all data _oxford_reflns_number_all 12677 _refine_ls_R_factor_all 0.0910 _refine_ls_wR_factor_all 0.0782 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 9103 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_gt 0.0587 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration '.' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.04 0.283 0.679 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Ru1 Ru 0.03291(2) 0.730779(17) 0.394332(10) 0.0268 1.0000 Uani . . . . . . . P2 P -0.14941(8) 0.77040(6) 0.38050(3) 0.0287 1.0000 Uani . . . . . . . C3 C -0.2108(4) 0.7652(3) 0.43730(16) 0.0430 1.0000 Uani . . . . . . . C4 C -0.1755(4) 0.8701(3) 0.35971(17) 0.0419 1.0000 Uani . . . . . . . C5 C -0.2472(4) 0.7161(3) 0.33599(19) 0.0505 1.0000 Uani . . . . . . . C6 C -0.0164(4) 0.6284(2) 0.37942(15) 0.0385 1.0000 Uani . . . . . . . O7 O -0.0458(4) 0.56648(19) 0.37036(15) 0.0640 1.0000 Uani . . . . . . . C8 C 0.2132(3) 0.7559(3) 0.42098(17) 0.0451 1.0000 Uani . . . . . . . C9 C 0.1742(4) 0.7075(3) 0.45711(17) 0.0497 1.0000 Uani . . . . . . . C10 C 0.0917(4) 0.7499(3) 0.47804(15) 0.0481 1.0000 Uani . . . . . . . C11 C 0.0796(4) 0.8227(3) 0.45434(16) 0.0446 1.0000 Uani . . . . . . . C12 C 0.1547(4) 0.8275(3) 0.41951(17) 0.0429 1.0000 Uani . . . . . . . B13 B 0.0535(3) 0.7405(2) 0.32541(15) 0.0284 1.0000 Uani . . . . . . . N14 N 0.0853(3) 0.74774(18) 0.28023(11) 0.0315 1.0000 Uani . . . . . . . C15 C 0.0416(3) 0.8084(2) 0.24318(13) 0.0293 1.0000 Uani . . . . . . . C16 C 0.0485(3) 0.8892(2) 0.26731(15) 0.0363 1.0000 Uani . . . . . . . C17 C 0.0025(4) 0.9521(3) 0.22994(18) 0.0457 1.0000 Uani . . . . . . . C18 C -0.1130(4) 0.9337(3) 0.20429(19) 0.0553 1.0000 Uani . . . . . . . C19 C -0.1185(4) 0.8532(3) 0.17989(17) 0.0494 1.0000 Uani . . . . . . . C20 C -0.0760(3) 0.7895(3) 0.21803(16) 0.0400 1.0000 Uani . . . . . . . C21 C 0.1747(3) 0.6942(2) 0.26849(13) 0.0318 1.0000 Uani . . . . . . . C22 C 0.1374(3) 0.6491(2) 0.22039(15) 0.0361 1.0000 Uani . . . . . . . C23 C 0.2295(4) 0.5943(3) 0.20926(17) 0.0445 1.0000 Uani . . . . . . . C24 C 0.3355(4) 0.6381(3) 0.20690(17) 0.0476 1.0000 Uani . . . . . . . C25 C 0.3736(4) 0.6828(3) 0.25493(19) 0.0513 1.0000 Uani . . . . . . . C26 C 0.2825(3) 0.7386(3) 0.26697(16) 0.0411 1.0000 Uani . . . . . . . F27 F 0.2744(2) 1.05547(13) 0.53447(10) 0.0470 1.0000 Uani . . . . . . . C28 C 0.2657(3) 0.9790(2) 0.54456(14) 0.0309 1.0000 Uani . . . . . . . F29 F 0.2782(3) 0.97384(17) 0.59427(9) 0.0570 1.0000 Uani . . . . . . . F30 F 0.1620(2) 0.95979(17) 0.52735(13) 0.0624 1.0000 Uani . . . . . . . C31 C 0.3481(3) 0.93081(19) 0.52260(12) 0.0230 1.0000 Uani . . . . . . . C32 C 0.4050(3) 0.87109(19) 0.55029(11) 0.0204 1.0000 Uani . . . . . . . C33 C 0.4811(3) 0.82337(18) 0.53112(11) 0.0192 1.0000 Uani . . . . . . . C34 C 0.4957(3) 0.83898(18) 0.48180(12) 0.0207 1.0000 Uani . . . . . . . C35 C 0.4379(3) 0.8978(2) 0.45327(12) 0.0232 1.0000 Uani . . . . . . . C36 C 0.3636(3) 0.94516(19) 0.47324(13) 0.0242 1.0000 Uani . . . . . . . C37 C 0.4508(3) 0.9096(2) 0.39943(13) 0.0281 1.0000 Uani . . . . . . . F38 F 0.5356(3) 0.8700(2) 0.38642(9) 0.0672 1.0000 Uani . . . . . . . F39 F 0.4673(3) 0.98296(15) 0.38780(9) 0.0583 1.0000 Uani . . . . . . . F40 F 0.3618(2) 0.8874(2) 0.36813(9) 0.0627 1.0000 Uani . . . . . . . B41 B 0.5567(3) 0.7596(2) 0.56691(12) 0.0188 1.0000 Uani . . . . . . . C42 C 0.6564(3) 0.81249(18) 0.59819(12) 0.0212 1.0000 Uani . . . . . . . C43 C 0.7515(3) 0.83375(19) 0.57890(12) 0.0218 1.0000 Uani . . . . . . . C44 C 0.8314(3) 0.8837(2) 0.60448(13) 0.0251 1.0000 Uani . . . . . . . C45 C 0.8195(3) 0.9149(2) 0.65056(13) 0.0259 1.0000 Uani . . . . . . . C46 C 0.7249(3) 0.8955(2) 0.67044(12) 0.0258 1.0000 Uani . . . . . . . C47 C 0.6452(3) 0.84622(19) 0.64470(12) 0.0224 1.0000 Uani . . . . . . . C48 C 0.7122(3) 0.9284(2) 0.72049(14) 0.0346 1.0000 Uani . . . . . . . F49 F 0.8019(2) 0.91369(19) 0.75496(9) 0.0553 1.0000 Uani . . . . . . . F50 F 0.7043(3) 1.00598(15) 0.71997(10) 0.0603 1.0000 Uani . . . . . . . F51 F 0.6274(2) 0.89910(19) 0.73907(10) 0.0577 1.0000 Uani . . . . . . . C52 C 0.9340(2) 0.90289(18) 0.58297(11) 0.0331 1.0000 Uani D U . . . . . C56 C 0.6010(3) 0.69010(18) 0.53286(11) 0.0192 1.0000 Uani . . . . . . . C57 C 0.7054(3) 0.6554(2) 0.54402(12) 0.0241 1.0000 Uani . . . . . . . C58 C 0.7367(3) 0.5938(2) 0.51583(14) 0.0297 1.0000 Uani . . . . . . . C59 C 0.6653(3) 0.5635(2) 0.47546(14) 0.0316 1.0000 Uani . . . . . . . C60 C 0.5613(3) 0.5968(2) 0.46406(13) 0.0291 1.0000 Uani . . . . . . . C61 C 0.5298(3) 0.65780(19) 0.49213(12) 0.0241 1.0000 Uani . . . . . . . C62 C 0.4827(3) 0.5666(2) 0.41961(11) 0.0430 1.0000 Uani D U . . . . . C66 C 0.8514(2) 0.5608(2) 0.52716(14) 0.0460 1.0000 Uani D U . . . . . C70 C 0.4874(2) 0.71292(17) 0.60461(11) 0.0194 1.0000 Uani . . . . . . . C71 C 0.3741(3) 0.69699(19) 0.59280(12) 0.0215 1.0000 Uani . . . . . . . C72 C 0.3182(3) 0.6517(2) 0.62392(12) 0.0242 1.0000 Uani . . . . . . . C73 C 0.3734(3) 0.6211(2) 0.66841(13) 0.0282 1.0000 Uani . . . . . . . C74 C 0.4858(3) 0.6371(2) 0.68122(12) 0.0269 1.0000 Uani . . . . . . . C75 C 0.5409(3) 0.6810(2) 0.64986(12) 0.0252 1.0000 Uani . . . . . . . C76 C 0.5464(3) 0.60507(19) 0.72940(9) 0.0416 1.0000 Uani D U . . . . . C80 C 0.1981(3) 0.6375(2) 0.60827(14) 0.0336 1.0000 Uani . . . . . . . F81 F 0.1377(2) 0.70261(19) 0.60777(14) 0.0698 1.0000 Uani . . . . . . . F82 F 0.1734(2) 0.6093(2) 0.56232(10) 0.0595 1.0000 Uani . . . . . . . F83 F 0.1551(2) 0.5897(2) 0.63848(13) 0.0857 1.0000 Uani . . . . . . . H31 H -0.2069 0.7120 0.4495 0.0710 1.0000 Uiso . . . . . . . H32 H -0.1705 0.7978 0.4626 0.0711 1.0000 Uiso . . . . . . . H33 H -0.2863 0.7816 0.4311 0.0710 1.0000 Uiso . . . . . . . H42 H -0.1622 0.8773 0.3262 0.0699 1.0000 Uiso . . . . . . . H43 H -0.1257 0.9055 0.3815 0.0701 1.0000 Uiso . . . . . . . H41 H -0.2508 0.8844 0.3621 0.0700 1.0000 Uiso . . . . . . . H51 H -0.2242 0.7157 0.3033 0.0790 1.0000 Uiso . . . . . . . H53 H -0.3195 0.7395 0.3333 0.0789 1.0000 Uiso . . . . . . . H52 H -0.2518 0.6629 0.3473 0.0791 1.0000 Uiso . . . . . . . H101 H 0.0515 0.7304 0.5048 0.0559 1.0000 Uiso . . . . . . . H111 H 0.0282 0.8648 0.4617 0.0571 1.0000 Uiso . . . . . . . H151 H 0.0895 0.8096 0.2169 0.0359 1.0000 Uiso . . . . . . . H162 H 0.0035 0.8894 0.2944 0.0471 1.0000 Uiso . . . . . . . H161 H 0.1250 0.9014 0.2822 0.0475 1.0000 Uiso . . . . . . . H172 H 0.0042 1.0028 0.2476 0.0593 1.0000 Uiso . . . . . . . H171 H 0.0515 0.9562 0.2046 0.0590 1.0000 Uiso . . . . . . . H181 H -0.1382 0.9735 0.1786 0.0671 1.0000 Uiso . . . . . . . H182 H -0.1645 0.9341 0.2290 0.0671 1.0000 Uiso . . . . . . . H191 H -0.1950 0.8407 0.1647 0.0611 1.0000 Uiso . . . . . . . H192 H -0.0723 0.8521 0.1533 0.0612 1.0000 Uiso . . . . . . . H201 H -0.1250 0.7869 0.2434 0.0508 1.0000 Uiso . . . . . . . H202 H -0.0784 0.7373 0.2017 0.0509 1.0000 Uiso . . . . . . . H211 H 0.1888 0.6551 0.2963 0.0401 1.0000 Uiso . . . . . . . H221 H 0.1200 0.6868 0.1920 0.0469 1.0000 Uiso . . . . . . . H222 H 0.0684 0.6188 0.2223 0.0471 1.0000 Uiso . . . . . . . H231 H 0.2425 0.5548 0.2357 0.0570 1.0000 Uiso . . . . . . . H232 H 0.2045 0.5660 0.1776 0.0571 1.0000 Uiso . . . . . . . H241 H 0.3230 0.6750 0.1783 0.0607 1.0000 Uiso . . . . . . . H242 H 0.3932 0.6017 0.2000 0.0610 1.0000 Uiso . . . . . . . H252 H 0.4415 0.7127 0.2528 0.0620 1.0000 Uiso . . . . . . . H251 H 0.3908 0.6451 0.2830 0.0618 1.0000 Uiso . . . . . . . H262 H 0.3062 0.7642 0.2986 0.0509 1.0000 Uiso . . . . . . . H261 H 0.2691 0.7784 0.2404 0.0512 1.0000 Uiso . . . . . . . H321 H 0.3908 0.8629 0.5833 0.0270 1.0000 Uiso . . . . . . . H341 H 0.5464 0.8078 0.4676 0.0265 1.0000 Uiso . . . . . . . H361 H 0.3259 0.9865 0.4542 0.0321 1.0000 Uiso . . . . . . . H431 H 0.7609 0.8141 0.5472 0.0271 1.0000 Uiso . . . . . . . H451 H 0.8734 0.9481 0.6677 0.0310 1.0000 Uiso . . . . . . . H471 H 0.5819 0.8345 0.6585 0.0302 1.0000 Uiso . . . . . . . H571 H 0.7566 0.6750 0.5712 0.0288 1.0000 Uiso . . . . . . . H591 H 0.6875 0.5207 0.4574 0.0372 1.0000 Uiso . . . . . . . H611 H 0.4576 0.6783 0.4838 0.0323 1.0000 Uiso . . . . . . . H711 H 0.3340 0.7170 0.5627 0.0283 1.0000 Uiso . . . . . . . H731 H 0.3354 0.5911 0.6896 0.0349 1.0000 Uiso . . . . . . . H751 H 0.6178 0.6896 0.6594 0.0313 1.0000 Uiso . . . . . . . H121 H 0.1653 0.8750 0.3986 0.0520 1.0000 Uiso . . . . . . . H81 H 0.2754 0.7441 0.4024 0.0532 1.0000 Uiso . . . . . . . H91 H 0.1988 0.6553 0.4656 0.0613 1.0000 Uiso . . . . . . . F530 F 0.9269(2) 0.8897(2) 0.53504(10) 0.0632 0.900(4) Uani D U P . 1 . . F540 F 0.9623(4) 0.9764(2) 0.58893(18) 0.1263 0.900(4) Uani D U P . 1 . . F550 F 1.0192(2) 0.8624(3) 0.60317(14) 0.1166 0.900(4) Uani D U P . 1 . . F531 F 0.9742(14) 0.8453(8) 0.5610(6) 0.0374(12) 0.100(4) Uiso D U P . 2 . . F541 F 0.9209(15) 0.9584(8) 0.5504(6) 0.0371(12) 0.100(4) Uiso D U P . 2 . . F551 F 1.0131(12) 0.9239(10) 0.6170(5) 0.0333(12) 0.100(4) Uiso D U P . 2 . . F630 F 0.4851(4) 0.4912(2) 0.41408(17) 0.0883 0.854(5) Uani D U P . 1 . . F640 F 0.3802(3) 0.5833(3) 0.42047(19) 0.1317 0.854(5) Uani D U P . 1 . . F650 F 0.5058(5) 0.5938(4) 0.37826(14) 0.1616 0.854(5) Uani D U P . 1 . . F631 F 0.5292(12) 0.5244(8) 0.3890(5) 0.0466(13) 0.146(5) Uiso D U P . 2 . . F641 F 0.4011(10) 0.5262(8) 0.4291(6) 0.0496(13) 0.146(5) Uiso D U P . 2 . . F651 F 0.4408(13) 0.6255(7) 0.3926(5) 0.0459(13) 0.146(5) Uiso D U P . 2 . . F670 F 0.9266(10) 0.5976(7) 0.5079(5) 0.0523(13) 0.174(5) Uiso D U P . 1 . . F680 F 0.8847(11) 0.5622(8) 0.5755(3) 0.0526(13) 0.174(5) Uiso D U P . 1 . . F690 F 0.8602(11) 0.4905(6) 0.5135(5) 0.0466(13) 0.174(5) Uiso D U P . 1 . . F671 F 0.9216(3) 0.6042(3) 0.55512(18) 0.0879 0.826(5) Uani D U P . 2 . . F681 F 0.8538(3) 0.4951(3) 0.5497(3) 0.1669 0.826(5) Uani D U P . 2 . . F691 F 0.8967(3) 0.5491(4) 0.48669(17) 0.1226 0.826(5) Uani D U P . 2 . . F770 F 0.560(3) 0.6523(17) 0.7674(9) 0.0480(14) 0.057(4) Uiso D U P . 1 . . F780 F 0.497(3) 0.5447(13) 0.7441(13) 0.0442(13) 0.057(4) Uiso D U P . 1 . . F790 F 0.6450(14) 0.583(2) 0.7250(13) 0.0457(13) 0.057(4) Uiso D U P . 1 . . F771 F 0.6404(3) 0.6413(2) 0.74526(11) 0.0816 0.943(4) Uani D U P . 2 . . F781 F 0.4902(3) 0.6090(3) 0.76662(11) 0.0951 0.943(4) Uani D U P . 2 . . F791 F 0.5745(4) 0.5323(2) 0.72588(15) 0.1187 0.943(4) Uani D U P . 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 Ru1 0.02966(15) 0.02915(15) 0.02282(13) -0.00077(13) 0.00779(10) 0.00038(13) P2 0.0303(4) 0.0287(4) 0.0291(4) -0.0048(4) 0.0107(3) -0.0002(4) C3 0.044(2) 0.047(2) 0.043(2) 0.005(2) 0.0243(18) 0.004(2) C4 0.045(2) 0.037(2) 0.048(2) 0.0050(18) 0.0190(19) 0.0082(18) C5 0.034(2) 0.062(3) 0.055(3) -0.015(2) 0.0043(19) -0.009(2) C6 0.049(2) 0.031(2) 0.036(2) 0.0013(16) 0.0086(18) 0.0075(18) O7 0.093(3) 0.0290(17) 0.068(2) -0.0064(16) 0.006(2) -0.0070(17) C8 0.0267(19) 0.066(3) 0.042(2) -0.004(2) 0.0038(16) -0.0062(19) C9 0.047(3) 0.061(3) 0.036(2) 0.007(2) -0.0071(19) 0.008(2) C10 0.050(3) 0.068(3) 0.0249(18) -0.0046(18) 0.0022(17) -0.005(2) C11 0.041(2) 0.050(3) 0.041(2) -0.020(2) 0.0020(18) -0.0121(19) C12 0.037(2) 0.048(2) 0.044(2) -0.0036(19) 0.0065(18) -0.0104(19) B13 0.0288(19) 0.029(2) 0.0283(18) -0.0026(16) 0.0060(15) -0.0001(16) N14 0.0360(17) 0.0332(17) 0.0271(14) -0.0006(12) 0.0102(13) -0.0018(12) C15 0.0335(18) 0.0312(18) 0.0249(16) -0.0009(14) 0.0105(14) -0.0039(15) C16 0.043(2) 0.0315(19) 0.036(2) -0.0042(16) 0.0100(17) -0.0030(17) C17 0.056(3) 0.035(2) 0.051(2) 0.0078(19) 0.022(2) 0.007(2) C18 0.049(3) 0.066(3) 0.052(3) 0.014(2) 0.014(2) 0.024(2) C19 0.033(2) 0.074(3) 0.039(2) 0.008(2) -0.0014(18) 0.004(2) C20 0.033(2) 0.049(2) 0.039(2) 0.0001(17) 0.0066(17) -0.0102(17) C21 0.039(2) 0.0307(18) 0.0275(17) 0.0010(15) 0.0110(15) 0.0015(16) C22 0.042(2) 0.0307(19) 0.038(2) -0.0074(16) 0.0148(17) -0.0024(17) C23 0.056(3) 0.039(2) 0.041(2) -0.0011(18) 0.018(2) 0.011(2) C24 0.051(3) 0.053(3) 0.044(2) 0.006(2) 0.022(2) 0.019(2) C25 0.039(2) 0.061(3) 0.056(3) 0.004(2) 0.012(2) 0.009(2) C26 0.036(2) 0.049(2) 0.039(2) -0.0038(19) 0.0090(16) -0.0028(19) F27 0.0563(15) 0.0224(11) 0.0668(16) -0.0003(11) 0.0238(13) 0.0109(11) C28 0.0308(19) 0.0261(17) 0.0372(19) -0.0012(15) 0.0097(15) 0.0055(15) F29 0.0786(19) 0.0596(17) 0.0383(13) 0.0052(12) 0.0261(13) 0.0382(15) F30 0.0249(12) 0.0615(18) 0.103(2) -0.0321(17) 0.0176(13) -0.0006(12) C31 0.0242(16) 0.0196(15) 0.0256(16) -0.0020(12) 0.0049(13) 0.0004(13) C32 0.0209(15) 0.0227(15) 0.0184(14) -0.0018(12) 0.0059(12) -0.0024(12) C33 0.0177(14) 0.0189(14) 0.0212(14) 0.0007(12) 0.0037(11) -0.0020(12) C34 0.0199(15) 0.0200(15) 0.0225(15) 0.0004(12) 0.0045(12) -0.0026(12) C35 0.0213(15) 0.0250(16) 0.0232(15) 0.0033(13) 0.0026(12) -0.0026(13) C36 0.0242(16) 0.0202(15) 0.0277(16) 0.0035(13) 0.0021(13) 0.0023(13) C37 0.0290(18) 0.0299(18) 0.0251(16) 0.0043(14) 0.0031(14) 0.0011(14) F38 0.079(2) 0.095(2) 0.0342(14) 0.0235(14) 0.0289(14) 0.0475(18) F39 0.102(2) 0.0398(14) 0.0356(13) 0.0112(11) 0.0172(14) -0.0185(15) F40 0.0571(17) 0.103(2) 0.0251(12) 0.0035(13) -0.0021(11) -0.0348(16) B41 0.0208(16) 0.0186(16) 0.0172(14) 0.0013(13) 0.0038(12) -0.0006(13) C42 0.0224(15) 0.0205(15) 0.0206(14) 0.0021(12) 0.0033(12) 0.0027(12) C43 0.0228(15) 0.0224(15) 0.0202(14) 0.0005(12) 0.0037(12) 0.0025(12) C44 0.0241(16) 0.0237(16) 0.0276(16) 0.0016(13) 0.0046(13) -0.0042(13) C45 0.0277(17) 0.0226(16) 0.0252(16) 0.0015(13) -0.0023(13) -0.0052(13) C46 0.0279(17) 0.0250(16) 0.0247(16) 0.0012(13) 0.0044(13) -0.0011(13) C47 0.0211(15) 0.0254(16) 0.0212(15) 0.0014(12) 0.0050(12) 0.0010(13) C48 0.041(2) 0.037(2) 0.0258(17) -0.0039(15) 0.0064(15) -0.0053(17) F49 0.0563(16) 0.082(2) 0.0244(11) -0.0033(12) -0.0036(11) -0.0060(15) F50 0.102(2) 0.0377(14) 0.0429(14) -0.0135(12) 0.0170(15) 0.0059(15) F51 0.0564(16) 0.083(2) 0.0393(14) -0.0261(14) 0.0246(12) -0.0261(15) C52 0.0273(15) 0.0377(14) 0.0356(12) -0.0005(9) 0.0086(11) -0.0068(11) C56 0.0206(15) 0.0179(15) 0.0200(14) 0.0011(12) 0.0055(12) 0.0011(12) C57 0.0221(16) 0.0244(16) 0.0256(16) 0.0009(13) 0.0029(13) -0.0002(13) C58 0.0255(17) 0.0278(18) 0.0360(19) -0.0019(15) 0.0055(14) 0.0049(14) C59 0.0364(19) 0.0246(17) 0.0343(18) -0.0075(15) 0.0074(15) 0.0057(15) C60 0.0317(18) 0.0256(17) 0.0292(17) -0.0039(14) 0.0021(14) -0.0024(14) C61 0.0255(16) 0.0224(16) 0.0240(16) 0.0006(13) 0.0023(13) -0.0005(13) C62 0.0472(15) 0.0407(14) 0.0372(16) -0.0086(11) -0.0058(14) -0.0044(11) C66 0.0339(18) 0.0433(14) 0.0576(15) 0.0018(13) -0.0027(12) 0.0062(13) C70 0.0206(15) 0.0190(15) 0.0193(13) -0.0017(11) 0.0053(12) 0.0014(11) C71 0.0216(15) 0.0231(15) 0.0195(14) -0.0025(12) 0.0028(12) -0.0020(13) C72 0.0236(16) 0.0251(16) 0.0250(16) -0.0011(13) 0.0073(13) -0.0036(13) C73 0.0324(18) 0.0272(17) 0.0271(17) 0.0028(14) 0.0112(14) -0.0050(14) C74 0.0302(17) 0.0261(17) 0.0241(16) 0.0035(13) 0.0030(13) 0.0032(14) C75 0.0213(16) 0.0275(17) 0.0258(16) 0.0038(13) 0.0004(13) 0.0009(13) C76 0.0423(13) 0.0476(15) 0.0327(15) 0.0112(12) -0.0010(13) 0.0033(11) C80 0.0308(19) 0.036(2) 0.0362(19) 0.0011(16) 0.0123(15) -0.0080(16) F81 0.0288(13) 0.0676(19) 0.111(3) -0.0260(19) 0.0039(15) 0.0070(13) F82 0.0345(13) 0.093(2) 0.0488(15) -0.0283(15) -0.0001(11) -0.0174(14) F83 0.0408(16) 0.134(3) 0.078(2) 0.056(2) -0.0015(15) -0.0403(18) F530 0.0382(15) 0.119(3) 0.0366(12) -0.0096(15) 0.0173(11) -0.0294(17) F540 0.144(4) 0.0728(19) 0.199(5) -0.073(3) 0.140(4) -0.079(2) F550 0.0276(16) 0.223(5) 0.104(3) 0.101(4) 0.0242(17) 0.035(2) F630 0.100(3) 0.0475(15) 0.099(3) -0.0412(19) -0.040(3) 0.0040(18) F640 0.0495(17) 0.169(5) 0.155(4) -0.128(4) -0.051(2) 0.037(2) F650 0.214(6) 0.221(6) 0.0309(17) 0.030(3) -0.039(2) -0.149(5) F671 0.0249(16) 0.100(3) 0.129(4) -0.066(3) -0.0176(19) 0.0260(16) F681 0.045(2) 0.101(3) 0.344(9) 0.136(5) -0.001(4) 0.021(2) F691 0.053(2) 0.221(6) 0.092(3) -0.066(3) 0.007(2) 0.060(3) F771 0.0594(17) 0.126(3) 0.0486(18) 0.0437(19) -0.0243(14) -0.033(2) F781 0.066(2) 0.183(4) 0.0381(16) 0.050(2) 0.0143(14) 0.012(2) F791 0.185(5) 0.0576(17) 0.090(3) 0.014(2) -0.053(3) 0.051(2) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 0.2149(3) 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 Ru1 . P2 . 2.3055(10) yes Ru1 . C6 . 1.877(4) yes Ru1 . C8 . 2.252(4) yes Ru1 . C9 . 2.259(4) yes Ru1 . C10 . 2.288(4) yes Ru1 . C11 . 2.268(4) yes Ru1 . C12 . 2.260(4) yes Ru1 . B13 . 1.928(4) yes P2 . C3 . 1.816(4) yes P2 . C4 . 1.811(4) yes P2 . C5 . 1.813(5) yes C3 . H31 . 0.968 no C3 . H32 . 0.958 no C3 . H33 . 0.955 no C4 . H42 . 0.954 no C4 . H43 . 0.987 no C4 . H41 . 0.965 no C5 . H51 . 0.968 no C5 . H53 . 0.964 no C5 . H52 . 0.965 no C6 . O7 . 1.135(5) yes C8 . C9 . 1.420(7) yes C8 . C12 . 1.417(7) yes C8 . H81 . 0.996 no C9 . C10 . 1.432(7) yes C9 . H91 . 0.960 no C10 . C11 . 1.399(7) yes C10 . H101 . 0.996 no C11 . C12 . 1.419(6) yes C11 . H111 . 0.998 no C12 . H121 . 1.011 no B13 . N14 . 1.345(5) yes N14 . C15 . 1.483(5) yes N14 . C21 . 1.500(5) yes C15 . C16 . 1.526(5) yes C15 . C20 . 1.527(5) yes C15 . H151 . 0.991 no C16 . C17 . 1.523(6) yes C16 . H162 . 0.984 no C16 . H161 . 0.982 no C17 . C18 . 1.506(7) yes C17 . H172 . 0.990 no C17 . H171 . 0.982 no C18 . C19 . 1.526(8) yes C18 . H181 . 0.988 no C18 . H182 . 0.988 no C19 . C20 . 1.535(6) yes C19 . H191 . 0.984 no C19 . H192 . 0.982 no C20 . H201 . 0.982 no C20 . H202 . 0.996 no C21 . C22 . 1.520(5) yes C21 . C26 . 1.528(6) yes C21 . H211 . 1.001 no C22 . C23 . 1.533(6) yes C22 . H221 . 1.000 no C22 . H222 . 1.000 no C23 . C24 . 1.509(7) yes C23 . H231 . 0.979 no C23 . H232 . 0.990 no C24 . C25 . 1.517(7) yes C24 . H241 . 0.992 no C24 . H242 . 0.982 no C25 . C26 . 1.542(6) yes C25 . H252 . 0.985 no C25 . H251 . 0.994 no C26 . H262 . 0.963 no C26 . H261 . 0.984 no F27 . C28 . 1.346(4) yes C28 . F29 . 1.332(4) yes C28 . F30 . 1.323(5) yes C28 . C31 . 1.496(5) yes C31 . C32 . 1.388(5) yes C31 . C36 . 1.400(5) yes C32 . C33 . 1.399(4) yes C32 . H321 . 0.946 no C33 . C34 . 1.399(4) yes C33 . B41 . 1.644(5) yes C34 . C35 . 1.391(5) yes C34 . H341 . 0.946 no C35 . C36 . 1.390(5) yes C35 . C37 . 1.503(5) yes C36 . H361 . 0.951 no C37 . F38 . 1.333(4) yes C37 . F39 . 1.319(4) yes C37 . F40 . 1.324(4) yes B41 . C42 . 1.642(5) yes B41 . C56 . 1.649(5) yes B41 . C70 . 1.635(4) yes C42 . C43 . 1.397(4) yes C42 . C47 . 1.411(4) yes C43 . C44 . 1.397(5) yes C43 . H431 . 0.946 no C44 . C45 . 1.385(5) yes C44 . C52 . 1.501(4) yes C45 . C46 . 1.392(5) yes C45 . H451 . 0.936 no C46 . C47 . 1.390(5) yes C46 . C48 . 1.497(5) yes C47 . H471 . 0.933 no C48 . F49 . 1.347(5) yes C48 . F50 . 1.333(5) yes C48 . F51 . 1.321(5) yes C52 . F530 . 1.305(4) yes C52 . F540 . 1.309(4) yes C52 . F550 . 1.298(4) yes C56 . C57 . 1.398(4) yes C56 . C61 . 1.405(4) yes C57 . C58 . 1.390(5) yes C57 . H571 . 0.949 no C58 . C59 . 1.386(5) yes C58 . C66 . 1.500(4) yes C59 . C60 . 1.384(5) yes C59 . H591 . 0.945 no C60 . C61 . 1.382(5) yes C60 . C62 . 1.508(4) yes C61 . H611 . 0.944 no C62 . F630 . 1.301(5) yes C62 . F640 . 1.290(5) yes C62 . F650 . 1.284(5) yes C66 . F670 . 1.290(9) yes C66 . F680 . 1.306(9) yes C66 . F690 . 1.267(9) yes C70 . C71 . 1.400(4) yes C70 . C75 . 1.404(4) yes C71 . C72 . 1.400(4) yes C71 . H711 . 0.946 no C72 . C73 . 1.385(5) yes C72 . C80 . 1.484(5) yes C73 . C74 . 1.391(5) yes C73 . H731 . 0.946 no C74 . C75 . 1.387(5) yes C74 . C76 . 1.498(4) yes C75 . H751 . 0.946 no C76 . F770 . 1.298(10) yes C76 . F780 . 1.290(10) yes C76 . F790 . 1.288(10) yes C80 . F81 . 1.337(5) yes C80 . F82 . 1.323(5) yes C80 . F83 . 1.324(5) yes 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 P2 . Ru1 . C6 . 88.29(13) yes P2 . Ru1 . C8 . 150.46(13) yes C6 . Ru1 . C8 . 120.83(19) yes P2 . Ru1 . C9 . 141.27(13) yes C6 . Ru1 . C9 . 100.27(19) yes C8 . Ru1 . C9 . 36.70(18) yes P2 . Ru1 . C10 . 105.25(13) yes C6 . Ru1 . C10 . 112.74(18) yes C8 . Ru1 . C10 . 61.12(16) yes C9 . Ru1 . C10 . 36.69(18) yes P2 . Ru1 . C11 . 92.25(12) yes C6 . Ru1 . C11 . 146.93(18) yes C8 . Ru1 . C11 . 61.02(17) yes C9 . Ru1 . C11 . 60.58(18) yes C10 . Ru1 . C11 . 35.75(18) yes P2 . Ru1 . C12 . 114.11(12) yes C6 . Ru1 . C12 . 157.44(18) yes C8 . Ru1 . C12 . 36.62(17) yes C9 . Ru1 . C12 . 60.85(18) yes C10 . Ru1 . C12 . 60.50(17) yes P2 . Ru1 . B13 . 95.12(13) yes C6 . Ru1 . B13 . 87.71(18) yes C8 . Ru1 . B13 . 91.22(17) yes C9 . Ru1 . B13 . 122.70(18) yes C10 . Ru1 . B13 . 151.11(18) yes C11 . Ru1 . C12 . 36.52(16) yes C11 . Ru1 . B13 . 125.10(18) yes C12 . Ru1 . B13 . 92.68(17) yes Ru1 . P2 . C3 . 111.57(15) yes Ru1 . P2 . C4 . 116.54(15) yes C3 . P2 . C4 . 103.4(2) yes Ru1 . P2 . C5 . 118.47(16) yes C3 . P2 . C5 . 102.6(2) yes C4 . P2 . C5 . 102.2(2) yes P2 . C3 . H31 . 109.3 no P2 . C3 . H32 . 110.0 no H31 . C3 . H32 . 108.2 no P2 . C3 . H33 . 110.8 no H31 . C3 . H33 . 109.3 no H32 . C3 . H33 . 109.1 no P2 . C4 . H42 . 111.5 no P2 . C4 . H43 . 109.4 no H42 . C4 . H43 . 107.9 no P2 . C4 . H41 . 110.0 no H42 . C4 . H41 . 109.9 no H43 . C4 . H41 . 108.1 no P2 . C5 . H51 . 110.7 no P2 . C5 . H53 . 109.8 no H51 . C5 . H53 . 109.3 no P2 . C5 . H52 . 109.9 no H51 . C5 . H52 . 108.6 no H53 . C5 . H52 . 108.5 no Ru1 . C6 . O7 . 179.8(4) yes Ru1 . C8 . C9 . 71.9(2) yes Ru1 . C8 . C12 . 72.0(2) yes C9 . C8 . C12 . 107.5(4) yes Ru1 . C8 . H81 . 126.0 no C9 . C8 . H81 . 126.5 no C12 . C8 . H81 . 125.7 no Ru1 . C9 . C8 . 71.4(2) yes Ru1 . C9 . C10 . 72.8(2) yes C8 . C9 . C10 . 108.1(4) yes Ru1 . C9 . H91 . 121.2 no C8 . C9 . H91 . 125.6 no C10 . C9 . H91 . 126.3 no Ru1 . C10 . C9 . 70.5(2) yes Ru1 . C10 . C11 . 71.4(2) yes C9 . C10 . C11 . 107.6(4) yes Ru1 . C10 . H101 . 123.8 no C9 . C10 . H101 . 125.3 no C11 . C10 . H101 . 127.1 no Ru1 . C11 . C10 . 72.9(2) yes Ru1 . C11 . C12 . 71.4(2) yes C10 . C11 . C12 . 108.8(4) yes Ru1 . C11 . H111 . 123.4 no C10 . C11 . H111 . 125.3 no C12 . C11 . H111 . 125.9 no Ru1 . C12 . C11 . 72.1(2) yes Ru1 . C12 . C8 . 71.4(2) yes C11 . C12 . C8 . 108.0(4) yes Ru1 . C12 . H121 . 124.0 no C11 . C12 . H121 . 124.8 no C8 . C12 . H121 . 127.1 no Ru1 . B13 . N14 . 170.8(3) yes B13 . N14 . C15 . 123.6(3) yes B13 . N14 . C21 . 117.5(3) yes C15 . N14 . C21 . 118.8(3) yes N14 . C15 . C16 . 110.9(3) yes N14 . C15 . C20 . 111.4(3) yes C16 . C15 . C20 . 111.6(3) yes N14 . C15 . H151 . 107.9 no C16 . C15 . H151 . 106.9 no C20 . C15 . H151 . 108.0 no C15 . C16 . C17 . 111.6(3) yes C15 . C16 . H162 . 108.8 no C17 . C16 . H162 . 107.5 no C15 . C16 . H161 . 110.7 no C17 . C16 . H161 . 110.5 no H162 . C16 . H161 . 107.7 no C16 . C17 . C18 . 112.3(4) yes C16 . C17 . H172 . 108.8 no C18 . C17 . H172 . 110.6 no C16 . C17 . H171 . 108.2 no C18 . C17 . H171 . 109.0 no H172 . C17 . H171 . 107.9 no C17 . C18 . C19 . 111.3(4) yes C17 . C18 . H181 . 110.2 no C19 . C18 . H181 . 109.4 no C17 . C18 . H182 . 109.9 no C19 . C18 . H182 . 108.0 no H181 . C18 . H182 . 108.0 no C18 . C19 . C20 . 111.4(4) yes C18 . C19 . H191 . 110.5 no C20 . C19 . H191 . 109.0 no C18 . C19 . H192 . 110.0 no C20 . C19 . H192 . 107.7 no H191 . C19 . H192 . 108.0 no C19 . C20 . C15 . 110.1(3) yes C19 . C20 . H201 . 108.8 no C15 . C20 . H201 . 109.6 no C19 . C20 . H202 . 110.9 no C15 . C20 . H202 . 110.3 no H201 . C20 . H202 . 107.0 no N14 . C21 . C22 . 111.2(3) yes N14 . C21 . C26 . 111.3(3) yes C22 . C21 . C26 . 111.9(3) yes N14 . C21 . H211 . 107.1 no C22 . C21 . H211 . 107.1 no C26 . C21 . H211 . 107.9 no C21 . C22 . C23 . 110.4(4) yes C21 . C22 . H221 . 109.1 no C23 . C22 . H221 . 108.6 no C21 . C22 . H222 . 111.2 no C23 . C22 . H222 . 110.2 no H221 . C22 . H222 . 107.3 no C22 . C23 . C24 . 111.6(4) yes C22 . C23 . H231 . 108.7 no C24 . C23 . H231 . 109.5 no C22 . C23 . H232 . 109.5 no C24 . C23 . H232 . 110.9 no H231 . C23 . H232 . 106.5 no C23 . C24 . C25 . 111.4(4) yes C23 . C24 . H241 . 108.8 no C25 . C24 . H241 . 109.5 no C23 . C24 . H242 . 110.0 no C25 . C24 . H242 . 110.5 no H241 . C24 . H242 . 106.5 no C24 . C25 . C26 . 111.1(4) yes C24 . C25 . H252 . 111.2 no C26 . C25 . H252 . 109.6 no C24 . C25 . H251 . 108.9 no C26 . C25 . H251 . 108.4 no H252 . C25 . H251 . 107.6 no C25 . C26 . C21 . 110.7(4) yes C25 . C26 . H262 . 110.0 no C21 . C26 . H262 . 110.0 no C25 . C26 . H261 . 108.4 no C21 . C26 . H261 . 108.6 no H262 . C26 . H261 . 109.0 no F27 . C28 . F29 . 105.6(3) yes F27 . C28 . F30 . 105.8(3) yes F29 . C28 . F30 . 106.8(3) yes F27 . C28 . C31 . 112.1(3) yes F29 . C28 . C31 . 112.8(3) yes F30 . C28 . C31 . 113.1(3) yes C28 . C31 . C32 . 120.3(3) yes C28 . C31 . C36 . 118.9(3) yes C32 . C31 . C36 . 120.8(3) yes C31 . C32 . C33 . 122.5(3) yes C31 . C32 . H321 . 117.7 no C33 . C32 . H321 . 119.8 no C32 . C33 . C34 . 115.8(3) yes C32 . C33 . B41 . 121.0(3) yes C34 . C33 . B41 . 122.9(3) yes C33 . C34 . C35 . 122.5(3) yes C33 . C34 . H341 . 118.1 no C35 . C34 . H341 . 119.5 no C34 . C35 . C36 . 120.9(3) yes C34 . C35 . C37 . 120.8(3) yes C36 . C35 . C37 . 118.3(3) yes C31 . C36 . C35 . 117.6(3) yes C31 . C36 . H361 . 121.3 no C35 . C36 . H361 . 121.0 no C35 . C37 . F38 . 113.1(3) yes C35 . C37 . F39 . 113.7(3) yes F38 . C37 . F39 . 105.5(3) yes C35 . C37 . F40 . 112.3(3) yes F38 . C37 . F40 . 106.3(3) yes F39 . C37 . F40 . 105.2(3) yes C33 . B41 . C42 . 103.9(2) yes C33 . B41 . C56 . 110.8(2) yes C42 . B41 . C56 . 113.8(3) yes C33 . B41 . C70 . 113.1(3) yes C42 . B41 . C70 . 111.4(2) yes C56 . B41 . C70 . 104.1(2) yes B41 . C42 . C43 . 123.1(3) yes B41 . C42 . C47 . 121.1(3) yes C43 . C42 . C47 . 115.5(3) yes C42 . C43 . C44 . 122.3(3) yes C42 . C43 . H431 . 118.3 no C44 . C43 . H431 . 119.4 no C43 . C44 . C45 . 121.1(3) yes C43 . C44 . C52 . 120.3(3) yes C45 . C44 . C52 . 118.6(3) yes C44 . C45 . C46 . 117.9(3) yes C44 . C45 . H451 . 120.8 no C46 . C45 . H451 . 121.2 no C45 . C46 . C47 . 120.8(3) yes C45 . C46 . C48 . 118.1(3) yes C47 . C46 . C48 . 121.1(3) yes C42 . C47 . C46 . 122.4(3) yes C42 . C47 . H471 . 118.2 no C46 . C47 . H471 . 119.4 no C46 . C48 . F49 . 111.5(3) yes C46 . C48 . F50 . 112.5(3) yes F49 . C48 . F50 . 104.1(3) yes C46 . C48 . F51 . 113.7(3) yes F49 . C48 . F51 . 105.6(3) yes F50 . C48 . F51 . 108.8(4) yes C44 . C52 . F530 . 114.8(3) yes C44 . C52 . F540 . 112.6(3) yes F530 . C52 . F540 . 105.30(10) yes C44 . C52 . F550 . 112.7(3) yes F530 . C52 . F550 . 104.34(10) yes F540 . C52 . F550 . 106.38(10) yes B41 . C56 . C57 . 123.8(3) yes B41 . C56 . C61 . 120.3(3) yes C57 . C56 . C61 . 115.7(3) yes C56 . C57 . C58 . 121.7(3) yes C56 . C57 . H571 . 119.0 no C58 . C57 . H571 . 119.3 no C57 . C58 . C59 . 121.5(3) yes C57 . C58 . C66 . 120.3(3) yes C59 . C58 . C66 . 118.2(3) yes C58 . C59 . C60 . 117.6(3) yes C58 . C59 . H591 . 120.1 no C60 . C59 . H591 . 122.2 no C59 . C60 . C61 . 121.1(3) yes C59 . C60 . C62 . 119.0(3) yes C61 . C60 . C62 . 119.9(3) yes C56 . C61 . C60 . 122.4(3) yes C56 . C61 . H611 . 118.7 no C60 . C61 . H611 . 118.9 no C60 . C62 . F630 . 114.2(3) yes C60 . C62 . F640 . 114.1(3) yes F630 . C62 . F640 . 105.24(10) yes C60 . C62 . F650 . 111.6(3) yes F630 . C62 . F650 . 104.38(10) yes F640 . C62 . F650 . 106.48(10) yes C58 . C66 . F670 . 115.9(6) yes C58 . C66 . F680 . 109.3(7) yes F670 . C66 . F680 . 105.35(10) yes C58 . C66 . F690 . 114.7(7) yes F670 . C66 . F690 . 104.37(10) yes F680 . C66 . F690 . 106.37(10) yes B41 . C70 . C71 . 123.1(3) yes B41 . C70 . C75 . 121.2(3) yes C71 . C70 . C75 . 115.6(3) yes C70 . C71 . C72 . 122.1(3) yes C70 . C71 . H711 . 119.1 no C72 . C71 . H711 . 118.8 no C71 . C72 . C73 . 120.9(3) yes C71 . C72 . C80 . 118.4(3) yes C73 . C72 . C80 . 120.7(3) yes C72 . C73 . C74 . 117.9(3) yes C72 . C73 . H731 . 120.9 no C74 . C73 . H731 . 121.1 no C73 . C74 . C75 . 120.8(3) yes C73 . C74 . C76 . 118.6(3) yes C75 . C74 . C76 . 120.5(3) yes C70 . C75 . C74 . 122.6(3) yes C70 . C75 . H751 . 118.9 no C74 . C75 . H751 . 118.5 no C74 . C76 . F770 . 116.5(16) yes C74 . C76 . F780 . 111.8(16) yes F770 . C76 . F780 . 105.33(10) yes C74 . C76 . F790 . 111.7(16) yes F770 . C76 . F790 . 104.35(10) yes F780 . C76 . F790 . 106.41(10) yes C72 . C80 . F81 . 112.8(3) yes C72 . C80 . F82 . 113.4(3) yes F81 . C80 . F82 . 104.5(4) yes C72 . C80 . F83 . 113.4(3) yes F81 . C80 . F83 . 104.4(4) yes F82 . C80 . F83 . 107.4(4) yes #============================================================================== data_13 #============================================================================== _audit_creation_date 08-09-27 _audit_creation_method CRYSTALS_ver_12.86 _publ_section_exptl_refinement ; The data were weak probably in part due to disordered solvent and disorder in the CF~3~ groups hence the low data to parameter ratio. The difference map indicated the presence of diffuse electron density believed to be disordered solvent. SQUEEZE was used leaving a voidelecron density was removed. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 88 8 ' ' 2 0.148 0.586 0.229 18 2 ' ' 3 0.200 0.094 0.977 7 1 ' ' 4 0.417 0.237 0.690 158 20 ' ' 5 0.583 0.763 0.310 158 19 ' ' 6 0.422 0.474 0.249 20 2 ' ' 7 0.578 0.526 0.751 20 2 ' ' 8 0.800 0.906 0.023 7 1 ' ' 9 0.852 0.415 0.771 18 2 ' ' _platon_squeeze_details ; The discrete Fourier transform of the void region were treated as contributions to the A and B parts of the calculated structure factors. ; _oxford_structure_analysis_title '5721' _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 12.60730(10) _cell_length_b 19.6463(2) _cell_length_c 26.4427(4) _cell_angle_alpha 70.5296(5) _cell_angle_beta 87.0531(5) _cell_angle_gamma 78.5273(5) _cell_volume 6050.80(12) _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-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 C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C55 H55 B2 Cl2 F24 Fe1 N1 O2 P2 # Dc = 1.57 Fooo = 2672.00 Mu = 5.07 M = 2856.64 # Found Formula = C53.50 H48 B2 Cl1 F24 Fe1 N1 O1 P1 # Dc = 1.45 FOOO = 2672.00 Mu = 4.31 M = 2641.65 _chemical_formula_sum 'C53.50 H48 B2 Cl1 F24 Fe1 N1 O1 P1' _chemical_formula_moiety 'C21 H35 B Fe N O P, C32 H12 B F24, 0.5(C H2 Cl2)' _chemical_compound_source . _chemical_formula_weight 1320.82 _cell_measurement_reflns_used 21943 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_min 0.12 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_max 0.22 _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2672 _exptl_absorpt_coefficient_mu 0.431 # Sheldrick geometric approximatio 0.93 0.95 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.95 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type 'Area' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 81455 _reflns_number_total 26654 _diffrn_reflns_av_R_equivalents 0.064 # Number of reflections with Friedels Law is 26654 # Number of reflections without Friedels Law is 26654 # Theoretical number of reflections is about 27649 _diffrn_reflns_theta_min 5.099 _diffrn_reflns_theta_max 27.445 _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 25.250 _diffrn_measured_fraction_theta_full 0.970 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 34 _reflns_limit_h_min -16 _reflns_limit_h_max 16 _reflns_limit_k_min -23 _reflns_limit_k_max 25 _reflns_limit_l_min 0 _reflns_limit_l_max 34 _oxford_diffrn_Wilson_B_factor 2.82 _oxford_diffrn_Wilson_scale 46.12 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.20 _refine_diff_density_max 1.97 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 12969 _refine_ls_number_restraints 76 _refine_ls_number_parameters 1522 _oxford_refine_ls_R_factor_ref 0.0847 _refine_ls_wR_factor_ref 0.0883 _refine_ls_goodness_of_fit_ref 1.1364 _refine_ls_shift/su_max 0.000365 # The values computed from all data _oxford_reflns_number_all 19386 _refine_ls_R_factor_all 0.1261 _refine_ls_wR_factor_all 0.1257 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 12969 _refine_ls_R_factor_gt 0.0847 _refine_ls_wR_factor_gt 0.0883 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration '.' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.985 0.390 0.536 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Fe1 Fe 0.43452(7) 0.86571(4) -0.04725(3) 0.0346 1.0000 Uani . . . . . . . P2 P 0.50079(13) 0.87843(8) 0.02243(6) 0.0386 1.0000 Uani . . . . . . . C3 C 0.5455(5) 0.9669(3) 0.0101(3) 0.0424 1.0000 Uani . . . . . . . C4 C 0.4092(6) 0.8750(4) 0.0785(2) 0.0518 1.0000 Uani . . . . . . . C5 C 0.6225(6) 0.8125(4) 0.0532(3) 0.0516 1.0000 Uani . . . . . . . C6 C 0.4384(5) 0.8305(3) -0.1132(2) 0.0406 1.0000 Uani . . . . . . . C7 C 0.4265(6) 0.9072(3) -0.1303(2) 0.0482 1.0000 Uani . . . . . . . C8 C 0.5164(6) 0.9252(4) -0.1136(3) 0.0503 1.0000 Uani . . . . . . . C9 C 0.5864(5) 0.8592(4) -0.0854(3) 0.0467 1.0000 Uani . . . . . . . C10 C 0.5372(5) 0.8002(3) -0.0855(2) 0.0426 1.0000 Uani . . . . . . . C11 C 0.3119(6) 0.9218(3) -0.0390(3) 0.0456 1.0000 Uani . . . . . . . O12 O 0.2310(4) 0.9570(3) -0.0324(2) 0.0630 1.0000 Uani . . . . . . . B13 B 0.3756(5) 0.7866(4) -0.0081(3) 0.0366 1.0000 Uani . . . . . . . N14 N 0.3220(4) 0.7314(3) 0.01415(19) 0.0392 1.0000 Uani . . . . . . . C15 C 0.3746(5) 0.6566(3) 0.0497(2) 0.0395 1.0000 Uani . . . . . . . C16 C 0.4806(5) 0.6573(3) 0.0730(3) 0.0436 1.0000 Uani . . . . . . . C17 C 0.5300(6) 0.5808(4) 0.1108(3) 0.0598 1.0000 Uani . . . . . . . C18 C 0.5441(6) 0.5233(4) 0.0836(3) 0.0630 1.0000 Uani . . . . . . . C19 C 0.4369(6) 0.5246(3) 0.0591(3) 0.0579 1.0000 Uani . . . . . . . C20 C 0.3900(6) 0.6006(3) 0.0210(3) 0.0488 1.0000 Uani . . . . . . . C21 C 0.2030(5) 0.7409(4) 0.0038(3) 0.0472 1.0000 Uani . . . . . . . C22 C 0.1692(6) 0.7849(4) -0.0539(3) 0.0555 1.0000 Uani . . . . . . . C23 C 0.0481(6) 0.7931(5) -0.0618(4) 0.0680 1.0000 Uani . . . . . . . C24 C -0.0167(6) 0.8271(5) -0.0246(4) 0.0806 1.0000 Uani . . . . . . . C25 C 0.0170(6) 0.7847(6) 0.0341(4) 0.0956 1.0000 Uani . . . . . . . C26 C 0.1375(6) 0.7758(5) 0.0421(3) 0.0685 1.0000 Uani . . . . . . . Fe27 Fe 0.47887(7) 0.18579(4) 0.41587(3) 0.0336 1.0000 Uani . . . . . . . P28 P 0.54227(15) 0.10852(8) 0.49392(7) 0.0456 1.0000 Uani . . . . . . . C29 C 0.5119(6) 0.1376(4) 0.5518(3) 0.0548 1.0000 Uani . . . . . . . C30 C 0.4881(7) 0.0222(4) 0.5184(3) 0.0611 1.0000 Uani . . . . . . . C31 C 0.6882(6) 0.0765(4) 0.4993(4) 0.0687 1.0000 Uani . . . . . . . C32 C 0.5778(5) 0.1414(3) 0.3828(3) 0.0449 1.0000 Uani . . . . . . . O33 O 0.6425(4) 0.1145(3) 0.3598(2) 0.0649 1.0000 Uani . . . . . . . C34 C 0.3679(6) 0.2764(4) 0.3693(4) 0.0698 1.0000 Uani . . . . . . . C35 C 0.3631(5) 0.2192(5) 0.3541(3) 0.0594 1.0000 Uani . . . . . . . C36 C 0.3342(6) 0.1642(4) 0.3957(5) 0.0745 1.0000 Uani . . . . . . . C37 C 0.3187(5) 0.1929(8) 0.4401(3) 0.0995 1.0000 Uani . . . . . . . C38 C 0.3434(6) 0.2641(6) 0.4199(5) 0.0778 1.0000 Uani . . . . . . . B39 B 0.5691(5) 0.2481(3) 0.4157(2) 0.0344 1.0000 Uani . . . . . . . N40 N 0.6317(4) 0.2978(2) 0.41205(18) 0.0342 1.0000 Uani . . . . . . . C41 C 0.6443(5) 0.3268(3) 0.4570(2) 0.0409 1.0000 Uani . . . . . . . C42 C 0.5378(5) 0.3388(3) 0.4849(2) 0.0430 1.0000 Uani . . . . . . . C43 C 0.5508(7) 0.3661(4) 0.5314(3) 0.0646 1.0000 Uani . . . . . . . C44 C 0.6380(7) 0.3159(4) 0.5703(3) 0.0626 1.0000 Uani . . . . . . . C45 C 0.7447(7) 0.3072(4) 0.5416(3) 0.0621 1.0000 Uani . . . . . . . C46 C 0.7336(5) 0.2779(4) 0.4957(3) 0.0490 1.0000 Uani . . . . . . . C47 C 0.6925(6) 0.3302(4) 0.3632(2) 0.0486 1.0000 Uani . . . . . . . C48 C 0.6326(6) 0.4067(4) 0.3311(3) 0.0548 1.0000 Uani . . . . . . . C49 C 0.7044(8) 0.4409(5) 0.2832(3) 0.0826 1.0000 Uani . . . . . . . C50 C 0.7344(9) 0.3924(7) 0.2493(3) 0.0956 1.0000 Uani . . . . . . . C51 C 0.7862(7) 0.3164(6) 0.2809(3) 0.0762 1.0000 Uani . . . . . . . C52 C 0.7178(6) 0.2821(5) 0.3285(3) 0.0602 1.0000 Uani . . . . . . . F53 F -0.1659(3) 0.46802(19) 0.12195(14) 0.0534 1.0000 Uani D . . . . . . C54 C -0.1562(4) 0.4133(3) 0.1020(2) 0.0424 1.0000 Uani D . . . . . . F55 F -0.1933(3) 0.4438(2) 0.05144(14) 0.0642 1.0000 Uani D . . . . . . F56 F -0.2234(3) 0.3699(2) 0.12866(18) 0.0634 1.0000 Uani D . . . . . . C57 C -0.0411(4) 0.3721(3) 0.1048(2) 0.0307 1.0000 Uani D . . . . . . C58 C -0.0003(4) 0.3207(3) 0.1535(2) 0.0284 1.0000 Uani . . . . . . . C59 C 0.1055(4) 0.2794(3) 0.1588(2) 0.0269 1.0000 Uani . . . . . . . C60 C 0.1653(4) 0.2928(3) 0.1126(2) 0.0289 1.0000 Uani . . . . . . . C61 C 0.1263(4) 0.3455(3) 0.0638(2) 0.0326 1.0000 Uani D . . . . . . C62 C 0.0221(4) 0.3855(3) 0.0596(2) 0.0330 1.0000 Uani . . . . . . . C63 C 0.1981(5) 0.3557(3) 0.0160(2) 0.0488 1.0000 Uani D . . . . . . F64 F 0.1494(3) 0.4030(2) -0.02852(14) 0.0706 1.0000 Uani D . . . . . . F65 F 0.2344(4) 0.2926(2) 0.00632(16) 0.0796 1.0000 Uani D . . . . . . F66 F 0.2864(3) 0.3785(3) 0.02306(17) 0.0781 1.0000 Uani D . . . . . . B67 B 0.1484(5) 0.2114(3) 0.2145(2) 0.0293 1.0000 Uani . . . . . . . C68 C 0.2807(4) 0.1941(3) 0.22138(19) 0.0260 1.0000 Uani . . . . . . . C69 C 0.3367(4) 0.1235(3) 0.24840(19) 0.0275 1.0000 Uani . . . . . . . C70 C 0.4484(4) 0.1078(3) 0.2576(2) 0.0298 1.0000 Uani D . . . . . . C71 C 0.5076(4) 0.1628(3) 0.24011(19) 0.0290 1.0000 Uani . . . . . . . C72 C 0.4551(4) 0.2335(3) 0.2137(2) 0.0296 1.0000 Uani D . . . . . . C73 C 0.3427(4) 0.2488(3) 0.2047(2) 0.0298 1.0000 Uani . . . . . . . C74 C 0.5148(4) 0.2953(3) 0.1937(2) 0.0425 1.0000 Uani D . . . . . . F75 F 0.6214(3) 0.2733(2) 0.19878(19) 0.0672 1.0000 Uani D . . . . . . F76 F 0.4939(4) 0.3340(2) 0.14241(17) 0.0754 1.0000 Uani D . . . . . . F77 F 0.4885(4) 0.3433(2) 0.2199(2) 0.0797 1.0000 Uani D . . . . . . C78 C 0.5016(4) 0.0307(3) 0.2875(2) 0.0416 1.0000 Uani D . . . . . . F79 F 0.6074(3) 0.0175(2) 0.28094(17) 0.0645 1.0000 Uani D . . . . . . F80 F 0.4636(4) -0.0177(2) 0.2724(2) 0.0874 1.0000 Uani D . . . . . . F81 F 0.4858(4) 0.0135(2) 0.33976(16) 0.0831 1.0000 Uani D . . . . . . C82 C 0.1030(4) 0.1421(3) 0.20816(19) 0.0267 1.0000 Uani . . . . . . . C83 C 0.0003(4) 0.1287(3) 0.2247(2) 0.0295 1.0000 Uani . . . . . . . C84 C -0.0411(4) 0.0728(3) 0.2171(2) 0.0332 1.0000 Uani D . . . . . . C85 C 0.0204(5) 0.0264(3) 0.1922(2) 0.0397 1.0000 Uani . . . . . . . C86 C 0.1225(4) 0.0387(3) 0.1741(2) 0.0348 1.0000 Uani D . . . . . . C87 C 0.1615(4) 0.0960(3) 0.1822(2) 0.0307 1.0000 Uani . . . . . . . C88 C 0.1915(5) -0.0083(3) 0.1465(3) 0.0564 1.0000 Uani D . . . . . . F89 F 0.2859(4) -0.0412(3) 0.1712(2) 0.0958 1.0000 Uani D . . . . . . F90 F 0.2235(4) 0.0298(3) 0.09832(19) 0.0883 1.0000 Uani D . . . . . . F91 F 0.1465(5) -0.0593(4) 0.1408(4) 0.1579 1.0000 Uani D . . . . . . C92 C -0.1534(4) 0.0629(3) 0.2347(2) 0.0466 1.0000 Uani D . . . . . . F93 F -0.1643(3) -0.0065(2) 0.2493(2) 0.0740 1.0000 Uani D . . . . . . F94 F -0.1829(4) 0.0838(3) 0.2767(2) 0.0907 1.0000 Uani D . . . . . . F95 F -0.2258(3) 0.1005(3) 0.1964(2) 0.0898 1.0000 Uani D . . . . . . C96 C 0.1058(4) 0.2317(3) 0.26820(19) 0.0266 1.0000 Uani . . . . . . . C97 C 0.0842(4) 0.1793(3) 0.3161(2) 0.0311 1.0000 Uani . . . . . . . C98 C 0.0555(4) 0.1969(3) 0.3623(2) 0.0363 1.0000 Uani D . . . . . . C99 C 0.0503(5) 0.2671(3) 0.3632(2) 0.0392 1.0000 Uani . . . . . . . C100 C 0.0717(4) 0.3205(3) 0.3166(2) 0.0341 1.0000 Uani D . . . . . . C101 C 0.0985(4) 0.3026(3) 0.2704(2) 0.0299 1.0000 Uani . . . . . . . C102 C 0.0646(5) 0.3979(3) 0.3156(2) 0.0467 1.0000 Uani D . . . . . . F103 F 0.0324(4) 0.4467(2) 0.26848(15) 0.0715 1.0000 Uani D . . . . . . F104 F -0.0062(4) 0.4151(2) 0.35052(17) 0.0721 1.0000 Uani D . . . . . . F105 F 0.1576(4) 0.4096(2) 0.3280(2) 0.0852 1.0000 Uani D . . . . . . C106 C 0.0312(5) 0.1379(3) 0.4114(2) 0.0509 1.0000 Uani D . . . . . . F107 F -0.0515(6) 0.1109(4) 0.4055(2) 0.1414 1.0000 Uani D . . . . . . F108 F 0.1079(5) 0.0805(3) 0.4269(2) 0.1266 1.0000 Uani D . . . . . . F109 F 0.0119(8) 0.1571(3) 0.4534(2) 0.1594 1.0000 Uani D . . . . . . F110 F 0.5526(3) 0.4857(2) 0.60869(17) 0.0642 1.0000 Uani D . . . . . . C111 C 0.6548(4) 0.4877(3) 0.6157(2) 0.0468 1.0000 Uani D . . . . . . F112 F 0.6957(4) 0.4977(3) 0.56731(18) 0.1007 1.0000 Uani D . . . . . . F113 F 0.6517(5) 0.5474(2) 0.6278(3) 0.1117 1.0000 Uani D . . . . . . C114 C 0.7130(5) 0.4208(3) 0.6570(2) 0.0358 1.0000 Uani D . . . . . . C115 C 0.8176(4) 0.3878(3) 0.6493(2) 0.0314 1.0000 Uani . . . . . . . C116 C 0.8742(5) 0.3246(3) 0.6871(2) 0.0324 1.0000 Uani . . . . . . . C117 C 0.8177(5) 0.2969(3) 0.7340(2) 0.0466 1.0000 Uani . . . . . . . C118 C 0.7115(6) 0.3284(4) 0.7422(2) 0.0520 1.0000 Uani D . . . . . . C119 C 0.6585(5) 0.3906(4) 0.7042(3) 0.0493 1.0000 Uani . . . . . . . C120 C 0.6579(6) 0.2930(4) 0.7932(3) 0.0859 1.0000 Uani D . . . . . . F121 F 0.5563(4) 0.3223(3) 0.7954(2) 0.1110 1.0000 Uani D . . . . . . F122 F 0.6629(7) 0.2224(4) 0.8034(3) 0.1612 1.0000 Uani D . . . . . . F123 F 0.7046(6) 0.2964(6) 0.8347(2) 0.1786 1.0000 Uani D . . . . . . B124 B 0.9957(5) 0.2830(3) 0.6785(2) 0.0307 1.0000 Uani . . . . . . . C125 C 1.0559(4) 0.3365(3) 0.6284(2) 0.0285 1.0000 Uani . . . . . . . C126 C 1.0317(4) 0.3449(3) 0.5755(2) 0.0301 1.0000 Uani . . . . . . . C127 C 1.0815(5) 0.3878(3) 0.5320(2) 0.0351 1.0000 Uani D . . . . . . C128 C 1.1568(5) 0.4267(3) 0.5395(2) 0.0423 1.0000 Uani . . . . . . . C129 C 1.1812(5) 0.4206(3) 0.5914(2) 0.0413 1.0000 Uani D . . . . . . C130 C 1.1311(5) 0.3761(3) 0.6347(2) 0.0357 1.0000 Uani . . . . . . . C131 C 1.2591(5) 0.4632(3) 0.6008(2) 0.0541 1.0000 Uani D . . . . . . F132 F 1.2108(4) 0.5232(3) 0.6108(2) 0.0919 1.0000 Uani D . . . . . . F133 F 1.3208(4) 0.4874(3) 0.5596(2) 0.0884 1.0000 Uani D . . . . . . F134 F 1.3259(5) 0.4247(3) 0.6411(3) 0.1193 1.0000 Uani D . . . . . . C135 C 1.0575(5) 0.3914(3) 0.4765(2) 0.0458 1.0000 Uani D . . . . . . F136 F 1.0668(4) 0.4544(2) 0.43935(15) 0.0730 1.0000 Uani D . . . . . . F137 F 0.9586(4) 0.3836(3) 0.47025(16) 0.0891 1.0000 Uani D . . . . . . F138 F 1.1229(5) 0.3397(3) 0.46258(18) 0.0985 1.0000 Uani D . . . . . . C139 C 1.0647(5) 0.2620(3) 0.7345(2) 0.0402 1.0000 Uani . . . . . . . C140 C 1.0677(5) 0.3155(3) 0.7581(2) 0.0452 1.0000 Uani . . . . . . . C141 C 1.1286(7) 0.3016(4) 0.8038(3) 0.0626 1.0000 Uani D U . . . . . C142 C 1.1848(10) 0.2332(5) 0.8285(4) 0.1099 1.0000 Uani . . . . . . . C143 C 1.1874(11) 0.1780(4) 0.8057(4) 0.1214 1.0000 Uani D . . . . . . C144 C 1.1264(8) 0.1932(4) 0.7591(3) 0.0763 1.0000 Uani . . . . . . . C145 C 1.2567(9) 0.1012(5) 0.8274(4) 0.1319 1.0000 Uani D . . . . . . F146 F 1.3195(6) 0.0791(3) 0.7907(3) 0.1330 1.0000 Uani D . . . . . . F147 F 1.1931(8) 0.0513(3) 0.8464(3) 0.1468 1.0000 Uani D . . . . . . F148 F 1.3081(11) 0.0936(3) 0.8706(4) 0.2583 1.0000 Uani D . . . . . . C149 C 1.1313(8) 0.3603(4) 0.8262(3) 0.1105 1.0000 Uani D U . . . . . F150 F 1.1206(7) 0.4251(3) 0.7938(2) 0.1515 1.0000 Uani D U . . . . . F151 F 1.2130(10) 0.3495(4) 0.8557(5) 0.3101 1.0000 Uani D U . . . . . F152 F 1.0525(12) 0.3659(6) 0.8595(4) 0.2797 1.0000 Uani D U . . . . . C153 C 0.9903(4) 0.2086(3) 0.6638(2) 0.0317 1.0000 Uani . . . . . . . C154 C 0.8999(4) 0.1753(3) 0.6715(2) 0.0313 1.0000 Uani . . . . . . . C155 C 0.8991(4) 0.1136(3) 0.6565(2) 0.0363 1.0000 Uani D . . . . . . C156 C 0.9867(5) 0.0836(3) 0.6327(2) 0.0411 1.0000 Uani . . . . . . . C157 C 1.0779(5) 0.1153(3) 0.6247(2) 0.0376 1.0000 Uani D . . . . . . C158 C 1.0787(5) 0.1760(3) 0.6402(2) 0.0359 1.0000 Uani . . . . . . . C159 C 1.1745(5) 0.0863(3) 0.5978(2) 0.0535 1.0000 Uani D . . . . . . F160 F 1.2657(3) 0.0736(3) 0.6237(2) 0.0959 1.0000 Uani D . . . . . . F161 F 1.1895(5) 0.1325(3) 0.5504(2) 0.1162 1.0000 Uani D . . . . . . F162 F 1.1698(5) 0.0243(3) 0.5901(3) 0.1332 1.0000 Uani D . . . . . . C163 C 0.7995(4) 0.0824(3) 0.6640(2) 0.0457 1.0000 Uani D . . . . . . F164 F 0.7285(5) 0.1149(3) 0.6258(3) 0.1348 1.0000 Uani D . . . . . . F165 F 0.8160(4) 0.0121(2) 0.6708(3) 0.1249 1.0000 Uani D . . . . . . F166 F 0.7467(5) 0.0841(5) 0.7074(3) 0.1361 1.0000 Uani D . . . . . . Cl167 Cl 0.1306(2) 0.54146(15) 0.07649(10) 0.0961 1.0000 Uani . . . . . . . C168 C 0.1372(9) 0.4842(6) 0.1405(4) 0.0960 1.0000 Uani . . . . . . . Cl169 Cl 0.2419(3) 0.4699(3) 0.17855(14) 0.1647 1.0000 Uani . . . . . . . H31 H 0.5729 0.9670 0.0435 0.0480 1.0000 Uiso R . . . . . . H32 H 0.6029 0.9707 -0.0161 0.0481 1.0000 Uiso R . . . . . . H41 H 0.3987 0.8252 0.0952 0.0770 1.0000 Uiso R . . . . . . H42 H 0.4389 0.8909 0.1044 0.0771 1.0000 Uiso R . . . . . . H43 H 0.3409 0.9064 0.0652 0.0770 1.0000 Uiso R . . . . . . H51 H 0.6110 0.7635 0.0602 0.0760 1.0000 Uiso R . . . . . . H52 H 0.6375 0.8198 0.0861 0.0760 1.0000 Uiso R . . . . . . H53 H 0.6821 0.8211 0.0294 0.0761 1.0000 Uiso R . . . . . . H61 H 0.3881 0.8030 -0.1210 0.0492 1.0000 Uiso R . . . . . . H71 H 0.3646 0.9422 -0.1510 0.0521 1.0000 Uiso R . . . . . . H81 H 0.5301 0.9752 -0.1210 0.0630 1.0000 Uiso R . . . . . . H91 H 0.6570 0.8546 -0.0690 0.0592 1.0000 Uiso R . . . . . . H101 H 0.5677 0.7475 -0.0699 0.0499 1.0000 Uiso R . . . . . . H151 H 0.3261 0.6410 0.0797 0.0461 1.0000 Uiso R . . . . . . H161 H 0.4691 0.6925 0.0924 0.0531 1.0000 Uiso R . . . . . . H162 H 0.5303 0.6715 0.0436 0.0529 1.0000 Uiso R . . . . . . H172 H 0.6000 0.5825 0.1233 0.0680 1.0000 Uiso R . . . . . . H171 H 0.4817 0.5685 0.1409 0.0681 1.0000 Uiso R . . . . . . H181 H 0.5976 0.5328 0.0559 0.0722 1.0000 Uiso R . . . . . . H182 H 0.5683 0.4753 0.1103 0.0720 1.0000 Uiso R . . . . . . H191 H 0.3850 0.5095 0.0875 0.0672 1.0000 Uiso R . . . . . . H192 H 0.4504 0.4903 0.0392 0.0672 1.0000 Uiso R . . . . . . H202 H 0.4400 0.6147 -0.0080 0.0581 1.0000 Uiso R . . . . . . H201 H 0.3209 0.6001 0.0065 0.0580 1.0000 Uiso R . . . . . . H211 H 0.1859 0.6920 0.0123 0.0542 1.0000 Uiso R . . . . . . H222 H 0.1880 0.8332 -0.0628 0.0652 1.0000 Uiso R . . . . . . H221 H 0.2082 0.7591 -0.0770 0.0649 1.0000 Uiso R . . . . . . H231 H 0.0291 0.8238 -0.0985 0.0821 1.0000 Uiso R . . . . . . H232 H 0.0321 0.7445 -0.0553 0.0821 1.0000 Uiso R . . . . . . H241 H -0.0050 0.8768 -0.0336 0.0861 1.0000 Uiso R . . . . . . H242 H -0.0927 0.8276 -0.0295 0.0859 1.0000 Uiso R . . . . . . H252 H -0.0213 0.8119 0.0565 0.1050 1.0000 Uiso R . . . . . . H251 H -0.0010 0.7365 0.0445 0.1052 1.0000 Uiso R . . . . . . H261 H 0.1545 0.8239 0.0346 0.0780 1.0000 Uiso R . . . . . . H262 H 0.1583 0.7457 0.0787 0.0780 1.0000 Uiso R . . . . . . H292 H 0.5456 0.1787 0.5481 0.0779 1.0000 Uiso R . . . . . . H291 H 0.5392 0.0983 0.5836 0.0779 1.0000 Uiso R . . . . . . H293 H 0.4353 0.1514 0.5540 0.0780 1.0000 Uiso R . . . . . . H302 H 0.5213 -0.0079 0.5531 0.0720 1.0000 Uiso R . . . . . . H301 H 0.4099 0.0345 0.5222 0.0721 1.0000 Uiso R . . . . . . H311 H 0.7127 0.0605 0.4692 0.1041 1.0000 Uiso R . . . . . . H313 H 0.7235 0.1159 0.4991 0.1041 1.0000 Uiso R . . . . . . H312 H 0.7071 0.0360 0.5322 0.1041 1.0000 Uiso R . . . . . . H341 H 0.3878 0.3216 0.3447 0.0751 1.0000 Uiso R . . . . . . H351 H 0.3806 0.2157 0.3184 0.0722 1.0000 Uiso R . . . . . . H361 H 0.3220 0.1166 0.3953 0.0860 1.0000 Uiso R . . . . . . H372 H 0.3104 0.1659 0.4772 0.1123 1.0000 Uiso R . . . . . . H381 H 0.3384 0.2993 0.4396 0.1000 1.0000 Uiso R . . . . . . H411 H 0.6637 0.3751 0.4406 0.0502 1.0000 Uiso R . . . . . . H421 H 0.4838 0.3728 0.4592 0.0531 1.0000 Uiso R . . . . . . H422 H 0.5163 0.2915 0.4995 0.0530 1.0000 Uiso R . . . . . . H432 H 0.5727 0.4138 0.5169 0.0820 1.0000 Uiso R . . . . . . H431 H 0.4824 0.3717 0.5496 0.0821 1.0000 Uiso R . . . . . . H441 H 0.6457 0.3350 0.5988 0.0731 1.0000 Uiso R . . . . . . H442 H 0.6192 0.2675 0.5849 0.0729 1.0000 Uiso R . . . . . . H451 H 0.8008 0.2745 0.5666 0.0791 1.0000 Uiso R . . . . . . H452 H 0.7636 0.3551 0.5271 0.0791 1.0000 Uiso R . . . . . . H462 H 0.8016 0.2766 0.4761 0.0622 1.0000 Uiso R . . . . . . H461 H 0.7187 0.2280 0.5099 0.0623 1.0000 Uiso R . . . . . . H471 H 0.7623 0.3357 0.3751 0.0601 1.0000 Uiso R . . . . . . H482 H 0.6204 0.4374 0.3539 0.0631 1.0000 Uiso R . . . . . . H481 H 0.5637 0.4023 0.3187 0.0630 1.0000 Uiso R . . . . . . H491 H 0.7703 0.4485 0.2965 0.0971 1.0000 Uiso R . . . . . . H492 H 0.6625 0.4877 0.2611 0.0971 1.0000 Uiso R . . . . . . H501 H 0.7851 0.4140 0.2224 0.1120 1.0000 Uiso R . . . . . . H502 H 0.6694 0.3909 0.2316 0.1121 1.0000 Uiso R . . . . . . H512 H 0.8561 0.3170 0.2944 0.0901 1.0000 Uiso R . . . . . . H511 H 0.7965 0.2865 0.2576 0.0900 1.0000 Uiso R . . . . . . H521 H 0.7563 0.2339 0.3503 0.0771 1.0000 Uiso R . . . . . . H522 H 0.6496 0.2776 0.3157 0.0771 1.0000 Uiso R . . . . . . H581 H -0.0444 0.3136 0.1836 0.0360 1.0000 Uiso R . . . . . . H601 H 0.2349 0.2653 0.1142 0.0330 1.0000 Uiso R . . . . . . H621 H -0.0055 0.4208 0.0274 0.0360 1.0000 Uiso R . . . . . . H691 H 0.2981 0.0855 0.2604 0.0311 1.0000 Uiso R . . . . . . H711 H 0.5821 0.1525 0.2460 0.0370 1.0000 Uiso R . . . . . . H731 H 0.3088 0.2973 0.1877 0.0381 1.0000 Uiso R . . . . . . H831 H -0.0425 0.1588 0.2415 0.0331 1.0000 Uiso R . . . . . . H851 H -0.0062 -0.0119 0.1876 0.0452 1.0000 Uiso R . . . . . . H871 H 0.2296 0.1038 0.1693 0.0352 1.0000 Uiso R . . . . . . H971 H 0.0887 0.1308 0.3171 0.0361 1.0000 Uiso R . . . . . . H991 H 0.0332 0.2784 0.3944 0.0480 1.0000 Uiso R . . . . . . H1011 H 0.1122 0.3396 0.2394 0.0341 1.0000 Uiso R . . . . . . H1151 H 0.8524 0.4094 0.6176 0.0370 1.0000 Uiso R . . . . . . H1171 H 0.8524 0.2558 0.7611 0.0531 1.0000 Uiso R . . . . . . H1191 H 0.5887 0.4133 0.7107 0.0582 1.0000 Uiso R . . . . . . H1261 H 0.9799 0.3207 0.5689 0.0350 1.0000 Uiso R . . . . . . H1281 H 1.1908 0.4557 0.5103 0.0530 1.0000 Uiso R . . . . . . H1301 H 1.1492 0.3727 0.6695 0.0419 1.0000 Uiso R . . . . . . H1401 H 1.0261 0.3625 0.7429 0.0531 1.0000 Uiso R . . . . . . H1421 H 1.2204 0.2226 0.8611 0.1031 1.0000 Uiso R . . . . . . H1441 H 1.1299 0.1568 0.7435 0.0781 1.0000 Uiso R . . . . . . H1541 H 0.8380 0.1944 0.6867 0.0350 1.0000 Uiso R . . . . . . H1561 H 0.9845 0.0433 0.6220 0.0482 1.0000 Uiso R . . . . . . H1581 H 1.1412 0.1956 0.6350 0.0390 1.0000 Uiso R . . . . . . H1681 H 0.0752 0.5040 0.1580 0.1061 1.0000 Uiso R . . . . . . H1682 H 0.1307 0.4366 0.1390 0.1062 1.0000 Uiso R . . . . . . 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 Fe1 0.0440(5) 0.0337(4) 0.0307(4) -0.0129(3) 0.0078(4) -0.0163(4) P2 0.0456(9) 0.0320(8) 0.0372(8) -0.0097(6) -0.0084(7) -0.0058(7) C3 0.041(3) 0.044(3) 0.041(3) -0.013(3) -0.010(3) -0.004(3) C4 0.088(5) 0.045(4) 0.029(3) -0.015(3) 0.010(3) -0.022(4) C5 0.056(4) 0.042(4) 0.052(4) -0.012(3) -0.021(3) 0.001(3) C6 0.051(4) 0.044(3) 0.034(3) -0.022(3) 0.007(3) -0.010(3) C7 0.053(4) 0.045(4) 0.031(3) 0.001(3) 0.001(3) 0.001(3) C8 0.067(5) 0.045(4) 0.042(4) -0.012(3) 0.023(3) -0.028(3) C9 0.034(3) 0.068(4) 0.043(4) -0.023(3) 0.011(3) -0.017(3) C10 0.048(4) 0.037(3) 0.038(3) -0.010(3) 0.004(3) -0.002(3) C11 0.047(4) 0.036(3) 0.048(4) -0.007(3) 0.000(3) -0.007(3) O12 0.041(3) 0.052(3) 0.086(4) -0.021(3) 0.007(2) 0.009(2) B13 0.035(4) 0.041(4) 0.036(4) -0.018(3) 0.003(3) -0.006(3) N14 0.043(3) 0.030(2) 0.039(3) -0.002(2) 0.001(2) -0.010(2) C15 0.047(4) 0.033(3) 0.036(3) -0.005(2) 0.004(3) -0.015(3) C16 0.040(4) 0.041(3) 0.049(4) -0.015(3) 0.003(3) -0.007(3) C17 0.045(4) 0.053(4) 0.072(5) -0.003(4) -0.008(4) -0.015(3) C18 0.056(5) 0.038(4) 0.081(5) -0.006(4) 0.010(4) -0.003(3) C19 0.061(5) 0.033(3) 0.077(5) -0.015(3) 0.015(4) -0.013(3) C20 0.049(4) 0.039(3) 0.060(4) -0.013(3) 0.004(3) -0.017(3) C21 0.037(4) 0.043(3) 0.055(4) -0.002(3) -0.007(3) -0.014(3) C22 0.052(4) 0.050(4) 0.062(4) -0.009(3) -0.016(3) -0.016(3) C23 0.053(5) 0.064(5) 0.084(6) -0.013(4) -0.015(4) -0.020(4) C24 0.040(4) 0.075(6) 0.109(7) -0.008(5) -0.005(4) -0.009(4) C25 0.042(5) 0.125(8) 0.093(7) -0.010(6) 0.014(4) -0.003(5) C26 0.044(4) 0.093(6) 0.059(5) -0.013(4) 0.007(3) -0.013(4) Fe27 0.0331(5) 0.0312(4) 0.0360(5) -0.0102(3) -0.0044(3) -0.0053(3) P28 0.0600(11) 0.0283(8) 0.0465(9) -0.0029(7) -0.0146(8) -0.0165(7) C29 0.079(5) 0.043(4) 0.038(4) -0.001(3) -0.012(3) -0.023(3) C30 0.097(6) 0.039(4) 0.048(4) -0.005(3) -0.006(4) -0.029(4) C31 0.068(5) 0.046(4) 0.090(6) -0.020(4) -0.031(4) -0.001(4) C32 0.044(4) 0.038(3) 0.057(4) -0.021(3) -0.010(3) -0.006(3) O33 0.059(3) 0.066(3) 0.079(4) -0.046(3) 0.000(3) 0.002(3) C34 0.042(4) 0.047(4) 0.101(7) -0.002(4) -0.022(4) 0.005(3) C35 0.031(4) 0.100(7) 0.047(4) -0.031(4) -0.015(3) 0.004(4) C36 0.043(4) 0.053(5) 0.135(9) -0.036(5) -0.039(5) -0.008(4) C37 0.021(4) 0.185(11) 0.040(4) 0.025(6) 0.002(3) -0.009(5) C38 0.037(4) 0.099(7) 0.115(8) -0.074(7) -0.007(5) 0.017(4) B39 0.037(4) 0.033(3) 0.025(3) -0.006(3) 0.000(3) 0.004(3) N40 0.041(3) 0.032(2) 0.032(2) -0.011(2) 0.002(2) -0.014(2) C41 0.054(4) 0.036(3) 0.032(3) -0.004(3) -0.004(3) -0.021(3) C42 0.058(4) 0.031(3) 0.035(3) -0.009(3) -0.003(3) 0.000(3) C43 0.104(6) 0.047(4) 0.049(4) -0.022(3) 0.012(4) -0.021(4) C44 0.104(6) 0.056(4) 0.039(4) -0.017(3) 0.001(4) -0.039(4) C45 0.078(5) 0.066(5) 0.048(4) -0.010(3) -0.013(4) -0.039(4) C46 0.044(4) 0.055(4) 0.049(4) -0.015(3) -0.003(3) -0.016(3) C47 0.050(4) 0.063(4) 0.039(3) -0.016(3) 0.012(3) -0.028(3) C48 0.073(5) 0.059(4) 0.035(3) -0.008(3) 0.006(3) -0.034(4) C49 0.118(8) 0.096(6) 0.046(4) -0.010(4) 0.006(5) -0.073(6) C50 0.116(8) 0.158(10) 0.045(5) -0.038(6) 0.036(5) -0.101(8) C51 0.053(5) 0.138(9) 0.049(5) -0.036(5) 0.018(4) -0.040(5) C52 0.043(4) 0.088(5) 0.055(4) -0.034(4) 0.008(3) -0.011(4) F53 0.055(2) 0.045(2) 0.047(2) -0.0116(17) 0.0043(17) 0.0133(17) C54 0.033(3) 0.054(4) 0.035(3) -0.012(3) -0.003(3) 0.000(3) F55 0.043(2) 0.087(3) 0.042(2) -0.014(2) -0.0159(17) 0.024(2) F56 0.0277(19) 0.062(2) 0.087(3) -0.011(2) 0.0055(19) -0.0025(17) C57 0.028(3) 0.030(3) 0.031(3) -0.008(2) -0.004(2) -0.001(2) C58 0.021(3) 0.033(3) 0.030(3) -0.010(2) -0.001(2) -0.004(2) C59 0.030(3) 0.024(3) 0.026(3) -0.007(2) -0.004(2) -0.006(2) C60 0.022(3) 0.029(3) 0.032(3) -0.005(2) -0.002(2) -0.004(2) C61 0.035(3) 0.032(3) 0.026(3) -0.004(2) 0.003(2) -0.007(2) C62 0.033(3) 0.031(3) 0.028(3) 0.000(2) -0.005(2) -0.003(2) C63 0.050(4) 0.046(4) 0.035(3) 0.005(3) 0.005(3) -0.005(3) F64 0.062(3) 0.082(3) 0.032(2) 0.0157(19) 0.0095(18) 0.007(2) F65 0.103(4) 0.070(3) 0.047(2) -0.012(2) 0.031(2) 0.007(3) F66 0.048(2) 0.113(4) 0.061(3) -0.004(2) 0.020(2) -0.035(3) B67 0.022(3) 0.032(3) 0.028(3) -0.003(3) 0.003(2) -0.005(3) C68 0.025(3) 0.034(3) 0.019(2) -0.009(2) -0.002(2) -0.005(2) C69 0.028(3) 0.031(3) 0.022(3) -0.005(2) 0.002(2) -0.011(2) C70 0.029(3) 0.035(3) 0.022(3) -0.006(2) -0.001(2) -0.005(2) C71 0.024(3) 0.043(3) 0.020(3) -0.008(2) -0.002(2) -0.008(2) C72 0.026(3) 0.038(3) 0.029(3) -0.014(2) -0.003(2) -0.010(2) C73 0.037(3) 0.030(3) 0.022(3) -0.007(2) -0.001(2) -0.007(2) C74 0.038(4) 0.041(3) 0.052(4) -0.017(3) 0.000(3) -0.013(3) F75 0.032(2) 0.059(2) 0.108(3) -0.016(2) 0.002(2) -0.0221(18) F76 0.087(3) 0.066(3) 0.066(3) 0.012(2) -0.013(2) -0.053(2) F77 0.073(3) 0.069(3) 0.129(4) -0.063(3) 0.024(3) -0.040(2) C78 0.032(3) 0.044(3) 0.044(4) -0.006(3) -0.005(3) -0.010(3) F79 0.030(2) 0.051(2) 0.085(3) 0.006(2) -0.0029(19) 0.0066(16) F80 0.066(3) 0.035(2) 0.154(5) -0.023(3) -0.045(3) 0.002(2) F81 0.096(3) 0.063(3) 0.049(3) 0.017(2) 0.011(2) 0.013(2) C82 0.030(3) 0.026(3) 0.019(2) 0.000(2) -0.005(2) -0.005(2) C83 0.025(3) 0.032(3) 0.029(3) -0.007(2) 0.000(2) -0.003(2) C84 0.025(3) 0.040(3) 0.033(3) -0.008(2) -0.001(2) -0.009(2) C85 0.039(3) 0.034(3) 0.049(4) -0.012(3) -0.004(3) -0.015(3) C86 0.029(3) 0.035(3) 0.043(3) -0.016(3) 0.002(2) -0.007(2) C87 0.026(3) 0.033(3) 0.032(3) -0.007(2) 0.001(2) -0.011(2) C88 0.046(4) 0.055(4) 0.076(5) -0.031(4) 0.008(4) -0.014(3) F89 0.090(4) 0.099(4) 0.091(4) -0.050(3) -0.003(3) 0.034(3) F90 0.110(4) 0.082(3) 0.071(3) -0.036(3) 0.027(3) -0.001(3) F91 0.105(4) 0.163(6) 0.317(10) -0.205(7) 0.111(6) -0.088(4) C92 0.038(4) 0.046(4) 0.061(4) -0.017(3) 0.002(3) -0.020(3) F93 0.054(2) 0.063(3) 0.112(4) -0.025(2) 0.024(2) -0.037(2) F94 0.061(3) 0.143(5) 0.113(4) -0.084(4) 0.050(3) -0.062(3) F95 0.028(2) 0.117(4) 0.092(3) 0.010(3) -0.013(2) -0.014(2) C96 0.021(3) 0.032(3) 0.022(3) -0.004(2) -0.003(2) -0.001(2) C97 0.023(3) 0.035(3) 0.031(3) -0.006(2) -0.003(2) -0.003(2) C98 0.030(3) 0.051(4) 0.024(3) -0.008(3) 0.002(2) -0.007(3) C99 0.041(3) 0.056(4) 0.023(3) -0.016(3) -0.002(2) -0.006(3) C100 0.027(3) 0.042(3) 0.032(3) -0.012(3) -0.003(2) -0.001(2) C101 0.028(3) 0.030(3) 0.027(3) -0.004(2) 0.001(2) -0.004(2) C102 0.052(4) 0.048(4) 0.038(3) -0.017(3) -0.008(3) 0.003(3) F103 0.117(4) 0.041(2) 0.049(2) -0.0176(19) -0.012(2) 0.007(2) F104 0.096(3) 0.064(3) 0.064(3) -0.041(2) 0.015(2) -0.002(2) F105 0.061(3) 0.061(3) 0.148(5) -0.051(3) -0.027(3) -0.009(2) C106 0.054(4) 0.057(4) 0.034(4) -0.003(3) 0.005(3) -0.015(4) F107 0.142(5) 0.179(6) 0.074(4) 0.048(4) -0.015(4) -0.117(5) F108 0.108(4) 0.095(4) 0.096(4) 0.054(3) 0.030(3) 0.007(3) F109 0.345(12) 0.097(4) 0.044(3) -0.022(3) 0.079(5) -0.080(6) F110 0.045(2) 0.058(2) 0.073(3) -0.002(2) -0.0148(19) -0.0010(19) C111 0.037(4) 0.033(3) 0.057(4) -0.001(3) 0.004(3) -0.001(3) F112 0.069(3) 0.102(4) 0.062(3) 0.037(3) 0.016(2) 0.027(3) F113 0.135(5) 0.029(2) 0.163(5) -0.015(3) -0.089(4) -0.005(2) C114 0.037(3) 0.031(3) 0.036(3) -0.007(2) 0.002(3) -0.006(2) C115 0.029(3) 0.033(3) 0.029(3) -0.007(2) 0.002(2) -0.007(2) C116 0.039(3) 0.026(3) 0.029(3) -0.006(2) 0.003(2) -0.004(2) C117 0.055(4) 0.038(3) 0.031(3) 0.001(3) 0.002(3) 0.006(3) C118 0.058(4) 0.055(4) 0.032(3) -0.007(3) 0.014(3) 0.000(3) C119 0.045(4) 0.052(4) 0.044(4) -0.016(3) 0.009(3) 0.005(3) C120 0.079(6) 0.086(7) 0.058(5) 0.005(5) 0.027(5) 0.009(5) F121 0.082(4) 0.132(5) 0.075(3) 0.001(3) 0.049(3) 0.005(3) F122 0.186(7) 0.097(5) 0.128(6) 0.030(4) 0.106(6) -0.001(5) F123 0.116(5) 0.365(14) 0.032(3) -0.030(5) 0.020(3) -0.062(7) B124 0.034(3) 0.030(3) 0.024(3) -0.003(2) -0.006(3) -0.003(3) C125 0.027(3) 0.023(3) 0.031(3) -0.004(2) -0.004(2) -0.003(2) C126 0.029(3) 0.031(3) 0.029(3) -0.008(2) 0.001(2) -0.007(2) C127 0.040(3) 0.034(3) 0.035(3) -0.017(3) 0.003(3) -0.006(3) C128 0.043(4) 0.042(3) 0.041(3) -0.012(3) 0.011(3) -0.012(3) C129 0.039(3) 0.039(3) 0.048(4) -0.013(3) 0.003(3) -0.013(3) C130 0.037(3) 0.035(3) 0.035(3) -0.013(3) 0.001(2) -0.003(3) C131 0.057(4) 0.057(4) 0.049(4) -0.014(3) 0.001(4) -0.018(4) F132 0.069(3) 0.098(4) 0.152(5) -0.088(4) 0.009(3) -0.032(3) F133 0.083(3) 0.108(4) 0.104(4) -0.050(3) 0.035(3) -0.068(3) F134 0.110(4) 0.102(4) 0.133(5) 0.015(4) -0.067(4) -0.068(4) C135 0.052(4) 0.047(4) 0.037(3) -0.011(3) 0.004(3) -0.012(3) F136 0.120(4) 0.058(3) 0.039(2) -0.0028(19) -0.001(2) -0.035(3) F137 0.084(3) 0.155(5) 0.037(2) -0.023(3) -0.001(2) -0.057(3) F138 0.139(5) 0.090(3) 0.057(3) -0.045(3) -0.016(3) 0.040(3) C139 0.052(4) 0.033(3) 0.029(3) -0.002(3) -0.006(3) -0.007(3) C140 0.060(4) 0.035(3) 0.032(3) -0.006(3) -0.008(3) 0.004(3) C141 0.090(6) 0.043(3) 0.047(4) -0.010(3) -0.025(4) 0.003(4) C142 0.177(11) 0.055(5) 0.086(6) -0.014(5) -0.099(7) 0.012(6) C143 0.195(12) 0.042(5) 0.122(8) -0.026(5) -0.123(9) 0.019(6) C144 0.114(7) 0.035(4) 0.074(5) -0.013(4) -0.057(5) 0.007(4) C145 0.190(15) 0.093(9) 0.128(11) -0.070(9) -0.063(11) 0.014(9) F146 0.140(6) 0.076(4) 0.164(7) -0.035(4) -0.060(5) 0.028(4) F147 0.250(10) 0.058(3) 0.103(5) 0.004(3) -0.063(5) 0.000(5) F148 0.418(16) 0.063(4) 0.264(11) -0.028(5) -0.295(12) 0.052(6) C149 0.209(8) 0.062(4) 0.050(4) -0.027(3) -0.069(4) 0.033(6) F150 0.319(10) 0.060(3) 0.086(4) -0.030(2) -0.067(4) -0.033(4) F151 0.435(14) 0.135(6) 0.388(14) -0.182(9) -0.344(13) 0.138(9) F152 0.510(17) 0.189(9) 0.211(10) -0.154(8) 0.173(11) -0.117(12) C153 0.035(3) 0.028(3) 0.025(3) -0.002(2) -0.003(2) -0.003(2) C154 0.027(3) 0.029(3) 0.029(3) 0.000(2) 0.004(2) -0.004(2) C155 0.039(3) 0.028(3) 0.036(3) 0.001(2) -0.004(3) -0.011(2) C156 0.045(4) 0.030(3) 0.046(4) -0.009(3) -0.005(3) -0.007(3) C157 0.041(3) 0.031(3) 0.033(3) -0.006(2) -0.001(3) 0.003(3) C158 0.029(3) 0.030(3) 0.044(3) -0.005(3) -0.001(3) -0.006(2) C159 0.053(5) 0.045(4) 0.059(4) -0.019(3) 0.012(4) -0.004(3) F160 0.040(3) 0.143(5) 0.103(4) -0.062(4) -0.005(2) 0.024(3) F161 0.111(4) 0.117(4) 0.066(3) 0.003(3) 0.044(3) 0.034(3) F162 0.094(4) 0.117(5) 0.245(8) -0.136(6) 0.077(5) -0.035(3) C163 0.043(4) 0.039(4) 0.055(4) -0.011(3) 0.002(3) -0.016(3) F164 0.091(4) 0.128(5) 0.140(5) 0.058(4) -0.071(4) -0.078(4) F165 0.069(3) 0.050(3) 0.251(8) -0.033(4) 0.020(4) -0.035(2) F166 0.111(5) 0.228(8) 0.136(5) -0.102(5) 0.069(4) -0.127(5) Cl167 0.0971(18) 0.1046(18) 0.0787(15) -0.0060(13) -0.0004(13) -0.0434(15) C168 0.108(8) 0.091(7) 0.086(7) -0.009(5) 0.001(6) -0.046(6) Cl169 0.122(3) 0.244(5) 0.094(2) 0.009(3) 0.0024(19) -0.071(3) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 0.1914(3) 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 Fe1 . P2 . 2.1687(17) yes Fe1 . C6 . 2.073(6) yes Fe1 . C7 . 2.072(6) yes Fe1 . C8 . 2.106(6) yes Fe1 . C9 . 2.119(6) yes Fe1 . C10 . 2.104(6) yes Fe1 . C11 . 1.760(7) yes Fe1 . B13 . 1.830(7) yes P2 . C3 . 1.854(6) yes P2 . C4 . 1.823(6) yes P2 . C5 . 1.825(6) yes C3 . C3 2_675 1.516(12) yes C3 . H31 . 0.967 no C3 . H32 . 0.971 no C4 . H41 . 0.963 no C4 . H42 . 0.959 no C4 . H43 . 0.960 no C5 . H51 . 0.957 no C5 . H52 . 0.962 no C5 . H53 . 0.958 no C6 . C7 . 1.399(9) yes C6 . C10 . 1.396(9) yes C6 . H61 . 0.980 no C7 . C8 . 1.385(10) yes C7 . H71 . 0.981 no C8 . C9 . 1.410(10) yes C8 . H81 . 0.984 no C9 . C10 . 1.421(9) yes C9 . H91 . 0.984 no C10 . H101 . 0.980 no C11 . O12 . 1.154(7) yes B13 . N14 . 1.342(8) yes N14 . C15 . 1.496(7) yes N14 . C21 . 1.502(8) yes C15 . C16 . 1.504(9) yes C15 . C20 . 1.511(9) yes C15 . H151 . 0.979 no C16 . C17 . 1.528(9) yes C16 . H161 . 0.976 no C16 . H162 . 0.974 no C17 . C18 . 1.507(11) yes C17 . H172 . 0.970 no C17 . H171 . 0.972 no C18 . C19 . 1.521(11) yes C18 . H181 . 0.968 no C18 . H182 . 0.971 no C19 . C20 . 1.518(9) yes C19 . H191 . 0.979 no C19 . H192 . 0.969 no C20 . H202 . 0.970 no C20 . H201 . 0.972 no C21 . C22 . 1.515(9) yes C21 . C26 . 1.526(10) yes C21 . H211 . 0.977 no C22 . C23 . 1.521(10) yes C22 . H222 . 0.973 no C22 . H221 . 0.973 no C23 . C24 . 1.490(12) yes C23 . H231 . 0.970 no C23 . H232 . 0.972 no C24 . C25 . 1.532(13) yes C24 . H241 . 0.964 no C24 . H242 . 0.972 no C25 . C26 . 1.511(11) yes C25 . H252 . 0.974 no C25 . H251 . 0.965 no C26 . H261 . 0.965 no C26 . H262 . 0.969 no Fe27 . P28 . 2.1913(18) yes Fe27 . C32 . 1.745(7) yes Fe27 . C34 . 2.089(7) yes Fe27 . C35 . 2.092(6) yes Fe27 . C36 . 2.084(7) yes Fe27 . C37 . 2.079(7) yes Fe27 . C38 . 2.084(7) yes Fe27 . B39 . 1.828(7) yes P28 . C29 . 1.802(7) yes P28 . C30 . 1.855(6) yes P28 . C31 . 1.819(8) yes C29 . H292 . 0.960 no C29 . H291 . 0.956 no C29 . H293 . 0.954 no C30 . C30 2_656 1.492(14) yes C30 . H302 . 0.975 no C30 . H301 . 0.977 no C31 . H311 . 0.964 no C31 . H313 . 0.965 no C31 . H312 . 0.964 no C32 . O33 . 1.143(8) yes C34 . C35 . 1.325(11) yes C34 . C38 . 1.311(13) yes C34 . H341 . 0.982 no C35 . C36 . 1.354(12) yes C35 . H351 . 0.980 no C36 . C37 . 1.450(14) yes C36 . H361 . 0.982 no C37 . C38 . 1.413(14) yes C37 . H372 . 0.959 no C38 . H381 . 0.985 no B39 . N40 . 1.350(8) yes N40 . C41 . 1.507(7) yes N40 . C47 . 1.484(7) yes C41 . C42 . 1.513(9) yes C41 . C46 . 1.507(9) yes C41 . H411 . 0.977 no C42 . C43 . 1.524(9) yes C42 . H421 . 0.967 no C42 . H422 . 0.968 no C43 . C44 . 1.499(11) yes C43 . H432 . 0.977 no C43 . H431 . 0.971 no C44 . C45 . 1.518(11) yes C44 . H441 . 0.964 no C44 . H442 . 0.971 no C45 . C46 . 1.529(9) yes C45 . H451 . 0.966 no C45 . H452 . 0.962 no C46 . H462 . 0.979 no C46 . H461 . 0.979 no C47 . C48 . 1.522(10) yes C47 . C52 . 1.505(10) yes C47 . H471 . 0.987 no C48 . C49 . 1.557(10) yes C48 . H482 . 0.974 no C48 . H481 . 0.974 no C49 . C50 . 1.499(13) yes C49 . H491 . 0.975 no C49 . H492 . 0.974 no C50 . C51 . 1.480(14) yes C50 . H501 . 0.977 no C50 . H502 . 0.974 no C51 . C52 . 1.529(10) yes C51 . H512 . 0.971 no C51 . H511 . 0.972 no C52 . H521 . 0.972 no C52 . H522 . 0.970 no F53 . C54 . 1.329(6) yes C54 . F55 . 1.336(5) yes C54 . F56 . 1.330(6) yes C54 . C57 . 1.506(6) yes C57 . C58 . 1.392(7) yes C57 . C62 . 1.382(8) yes C58 . C59 . 1.404(7) yes C58 . H581 . 0.934 no C59 . C60 . 1.378(7) yes C59 . B67 . 1.652(7) yes C60 . C61 . 1.397(7) yes C60 . H601 . 0.930 no C61 . C62 . 1.378(8) yes C61 . C63 . 1.497(6) yes C62 . H621 . 0.932 no C63 . F64 . 1.321(6) yes C63 . F65 . 1.337(6) yes C63 . F66 . 1.323(6) yes B67 . C68 . 1.641(8) yes B67 . C82 . 1.638(8) yes B67 . C96 . 1.636(8) yes C68 . C69 . 1.391(7) yes C68 . C73 . 1.395(7) yes C69 . C70 . 1.396(7) yes C69 . H691 . 0.931 no C70 . C71 . 1.374(7) yes C70 . C78 . 1.491(6) yes C71 . C72 . 1.375(7) yes C71 . H711 . 0.931 no C72 . C73 . 1.404(8) yes C72 . C74 . 1.488(6) yes C73 . H731 . 0.929 no C74 . F75 . 1.326(6) yes C74 . F76 . 1.326(6) yes C74 . F77 . 1.328(6) yes C78 . F79 . 1.321(6) yes C78 . F80 . 1.321(6) yes C78 . F81 . 1.324(6) yes C82 . C83 . 1.392(7) yes C82 . C87 . 1.389(8) yes C83 . C84 . 1.379(8) yes C83 . H831 . 0.929 no C84 . C85 . 1.391(8) yes C84 . C92 . 1.497(6) yes C85 . C86 . 1.389(8) yes C85 . H851 . 0.927 no C86 . C87 . 1.395(7) yes C86 . C88 . 1.485(7) yes C87 . H871 . 0.931 no C88 . F89 . 1.324(6) yes C88 . F90 . 1.334(6) yes C88 . F91 . 1.300(6) yes C92 . F93 . 1.323(6) yes C92 . F94 . 1.318(6) yes C92 . F95 . 1.317(6) yes C96 . C97 . 1.396(7) yes C96 . C101 . 1.397(7) yes C97 . C98 . 1.389(8) yes C97 . H971 . 0.935 no C98 . C99 . 1.375(8) yes C98 . C106 . 1.490(6) yes C99 . C100 . 1.382(8) yes C99 . H991 . 0.928 no C100 . C101 . 1.388(8) yes C100 . C102 . 1.497(6) yes C101 . H1011 . 0.932 no C102 . F103 . 1.317(6) yes C102 . F104 . 1.329(6) yes C102 . F105 . 1.315(6) yes C106 . F107 . 1.298(6) yes C106 . F108 . 1.294(6) yes C106 . F109 . 1.284(6) yes F110 . C111 . 1.321(6) yes C111 . F112 . 1.320(6) yes C111 . F113 . 1.309(6) yes C111 . C114 . 1.484(6) yes C114 . C115 . 1.386(8) yes C114 . C119 . 1.402(8) yes C115 . C116 . 1.394(7) yes C115 . H1151 . 0.935 no C116 . C117 . 1.397(8) yes C116 . B124 . 1.630(8) yes C117 . C118 . 1.398(9) yes C117 . H1171 . 0.929 no C118 . C119 . 1.369(9) yes C118 . C120 . 1.492(7) yes C119 . H1191 . 0.939 no C120 . F121 . 1.303(7) yes C120 . F122 . 1.312(7) yes C120 . F123 . 1.300(8) yes B124 . C125 . 1.650(8) yes B124 . C139 . 1.644(8) yes B124 . C153 . 1.648(8) yes C125 . C126 . 1.394(7) yes C125 . C130 . 1.391(8) yes C126 . C127 . 1.385(8) yes C126 . H1261 . 0.934 no C127 . C128 . 1.391(8) yes C127 . C135 . 1.489(6) yes C128 . C129 . 1.381(9) yes C128 . H1281 . 0.936 no C129 . C130 . 1.397(8) yes C129 . C131 . 1.489(7) yes C130 . H1301 . 0.936 no C131 . F132 . 1.317(6) yes C131 . F133 . 1.316(6) yes C131 . F134 . 1.311(6) yes C135 . F136 . 1.322(6) yes C135 . F137 . 1.312(6) yes C135 . F138 . 1.317(6) yes C139 . C140 . 1.398(8) yes C139 . C144 . 1.378(9) yes C140 . C141 . 1.384(9) yes C140 . H1401 . 0.933 no C141 . C142 . 1.348(10) yes C141 . C149 . 1.466(7) yes C142 . C143 . 1.400(12) yes C142 . H1421 . 0.933 no C143 . C144 . 1.400(10) yes C143 . C145 . 1.522(8) yes C144 . H1441 . 0.932 no C145 . F146 . 1.350(8) yes C145 . F147 . 1.342(8) yes C145 . F148 . 1.293(8) yes C149 . F150 . 1.261(7) yes C149 . F151 . 1.266(7) yes C149 . F152 . 1.307(8) yes C153 . C154 . 1.397(8) yes C153 . C158 . 1.397(8) yes C154 . C155 . 1.397(8) yes C154 . H1541 . 0.929 no C155 . C156 . 1.371(8) yes C155 . C163 . 1.480(6) yes C156 . C157 . 1.389(8) yes C156 . H1561 . 0.931 no C157 . C158 . 1.385(8) yes C157 . C159 . 1.489(6) yes C158 . H1581 . 0.929 no C159 . F160 . 1.306(6) yes C159 . F161 . 1.311(6) yes C159 . F162 . 1.313(6) yes C163 . F164 . 1.290(6) yes C163 . F165 . 1.305(6) yes C163 . F166 . 1.304(6) yes Cl167 . C168 . 1.688(10) yes C168 . Cl169 . 1.622(11) yes C168 . H1681 . 0.970 no C168 . H1682 . 0.968 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 P2 . Fe1 . C6 . 155.61(19) yes P2 . Fe1 . C7 . 142.9(2) yes C6 . Fe1 . C7 . 39.5(2) yes P2 . Fe1 . C8 . 105.7(2) yes C6 . Fe1 . C8 . 65.7(3) yes C7 . Fe1 . C8 . 38.7(3) yes P2 . Fe1 . C9 . 92.98(18) yes C6 . Fe1 . C9 . 65.7(3) yes C7 . Fe1 . C9 . 65.3(3) yes C8 . Fe1 . C9 . 39.0(3) yes P2 . Fe1 . C10 . 116.68(18) yes C6 . Fe1 . C10 . 39.0(2) yes C7 . Fe1 . C10 . 65.6(2) yes C8 . Fe1 . C10 . 65.6(3) yes C9 . Fe1 . C10 . 39.3(2) yes P2 . Fe1 . C11 . 89.3(2) yes C6 . Fe1 . C11 . 115.0(3) yes C7 . Fe1 . C11 . 94.2(3) yes C8 . Fe1 . C11 . 109.4(3) yes C9 . Fe1 . C11 . 147.3(3) yes P2 . Fe1 . B13 . 94.2(2) yes C6 . Fe1 . B13 . 89.2(3) yes C7 . Fe1 . B13 . 122.9(3) yes C8 . Fe1 . B13 . 153.8(3) yes C9 . Fe1 . B13 . 125.0(3) yes C10 . Fe1 . C11 . 154.0(3) yes C10 . Fe1 . B13 . 90.4(3) yes C11 . Fe1 . B13 . 87.3(3) yes Fe1 . P2 . C3 . 115.0(2) yes Fe1 . P2 . C4 . 115.8(2) yes C3 . P2 . C4 . 102.5(3) yes Fe1 . P2 . C5 . 116.6(2) yes C3 . P2 . C5 . 101.2(3) yes C4 . P2 . C5 . 103.8(3) yes C3 2_675 C3 . P2 . 112.8(6) yes C3 2_675 C3 . H31 . 108.0 no P2 . C3 . H31 . 108.3 no C3 2_675 C3 . H32 . 109.3 no P2 . C3 . H32 . 108.8 no H31 . C3 . H32 . 109.6 no P2 . C4 . H41 . 108.9 no P2 . C4 . H42 . 110.5 no H41 . C4 . H42 . 109.5 no P2 . C4 . H43 . 109.0 no H41 . C4 . H43 . 109.2 no H42 . C4 . H43 . 109.7 no P2 . C5 . H51 . 109.6 no P2 . C5 . H52 . 108.2 no H51 . C5 . H52 . 110.3 no P2 . C5 . H53 . 109.3 no H51 . C5 . H53 . 110.0 no H52 . C5 . H53 . 109.5 no Fe1 . C6 . C7 . 70.2(3) yes Fe1 . C6 . C10 . 71.7(3) yes C7 . C6 . C10 . 108.0(6) yes Fe1 . C6 . H61 . 126.2 no C7 . C6 . H61 . 125.9 no C10 . C6 . H61 . 126.0 no Fe1 . C7 . C6 . 70.3(3) yes Fe1 . C7 . C8 . 72.0(4) yes C6 . C7 . C8 . 109.0(6) yes Fe1 . C7 . H71 . 124.2 no C6 . C7 . H71 . 125.2 no C8 . C7 . H71 . 125.9 no Fe1 . C8 . C7 . 69.3(3) yes Fe1 . C8 . C9 . 71.0(3) yes C7 . C8 . C9 . 107.9(6) yes Fe1 . C8 . H81 . 126.5 no C7 . C8 . H81 . 126.2 no C9 . C8 . H81 . 125.8 no Fe1 . C9 . C8 . 70.0(4) yes Fe1 . C9 . C10 . 69.8(3) yes C8 . C9 . C10 . 107.4(6) yes Fe1 . C9 . H91 . 126.1 no C8 . C9 . H91 . 126.4 no C10 . C9 . H91 . 126.2 no Fe1 . C10 . C9 . 70.9(3) yes Fe1 . C10 . C6 . 69.3(3) yes C9 . C10 . C6 . 107.7(5) yes Fe1 . C10 . H101 . 126.5 no C9 . C10 . H101 . 126.3 no C6 . C10 . H101 . 125.9 no Fe1 . C11 . O12 . 178.1(6) yes Fe1 . B13 . N14 . 171.2(5) yes B13 . N14 . C15 . 123.6(5) yes B13 . N14 . C21 . 121.3(5) yes C15 . N14 . C21 . 115.1(4) yes N14 . C15 . C16 . 112.0(5) yes N14 . C15 . C20 . 111.8(5) yes C16 . C15 . C20 . 110.3(5) yes N14 . C15 . H151 . 107.6 no C16 . C15 . H151 . 107.4 no C20 . C15 . H151 . 107.5 no C15 . C16 . C17 . 110.7(5) yes C15 . C16 . H161 . 109.5 no C17 . C16 . H161 . 109.8 no C15 . C16 . H162 . 108.2 no C17 . C16 . H162 . 108.4 no H161 . C16 . H162 . 110.3 no C16 . C17 . C18 . 112.1(6) yes C16 . C17 . H172 . 108.6 no C18 . C17 . H172 . 109.1 no C16 . C17 . H171 . 107.6 no C18 . C17 . H171 . 109.6 no H172 . C17 . H171 . 109.8 no C17 . C18 . C19 . 110.0(6) yes C17 . C18 . H181 . 109.6 no C19 . C18 . H181 . 109.7 no C17 . C18 . H182 . 108.6 no C19 . C18 . H182 . 109.3 no H181 . C18 . H182 . 109.7 no C18 . C19 . C20 . 111.5(5) yes C18 . C19 . H191 . 109.8 no C20 . C19 . H191 . 109.1 no C18 . C19 . H192 . 107.7 no C20 . C19 . H192 . 108.8 no H191 . C19 . H192 . 109.8 no C19 . C20 . C15 . 110.5(6) yes C19 . C20 . H202 . 109.1 no C15 . C20 . H202 . 108.0 no C19 . C20 . H201 . 109.7 no C15 . C20 . H201 . 109.7 no H202 . C20 . H201 . 109.8 no N14 . C21 . C22 . 113.2(5) yes N14 . C21 . C26 . 110.1(5) yes C22 . C21 . C26 . 110.6(6) yes N14 . C21 . H211 . 107.8 no C22 . C21 . H211 . 108.7 no C26 . C21 . H211 . 106.2 no C21 . C22 . C23 . 110.7(6) yes C21 . C22 . H222 . 108.8 no C23 . C22 . H222 . 109.8 no C21 . C22 . H221 . 108.5 no C23 . C22 . H221 . 109.4 no H222 . C22 . H221 . 109.7 no C22 . C23 . C24 . 112.2(7) yes C22 . C23 . H231 . 108.1 no C24 . C23 . H231 . 109.3 no C22 . C23 . H232 . 108.3 no C24 . C23 . H232 . 108.9 no H231 . C23 . H232 . 109.9 no C23 . C24 . C25 . 111.7(7) yes C23 . C24 . H241 . 107.9 no C25 . C24 . H241 . 109.2 no C23 . C24 . H242 . 108.6 no C25 . C24 . H242 . 109.5 no H241 . C24 . H242 . 109.9 no C24 . C25 . C26 . 111.0(7) yes C24 . C25 . H252 . 108.8 no C26 . C25 . H252 . 109.0 no C24 . C25 . H251 . 109.7 no C26 . C25 . H251 . 108.5 no H252 . C25 . H251 . 109.8 no C21 . C26 . C25 . 112.0(7) yes C21 . C26 . H261 . 107.2 no C25 . C26 . H261 . 108.4 no C21 . C26 . H262 . 109.2 no C25 . C26 . H262 . 110.0 no H261 . C26 . H262 . 109.9 no P28 . Fe27 . C32 . 90.9(2) yes P28 . Fe27 . C34 . 151.1(3) yes C32 . Fe27 . C34 . 118.0(4) yes P28 . Fe27 . C35 . 149.1(3) yes C32 . Fe27 . C35 . 94.8(3) yes C34 . Fe27 . C35 . 36.9(3) yes P28 . Fe27 . C36 . 111.4(3) yes C32 . Fe27 . C36 . 104.4(3) yes C34 . Fe27 . C36 . 63.6(3) yes C35 . Fe27 . C36 . 37.8(3) yes P28 . Fe27 . C37 . 93.6(2) yes C32 . Fe27 . C37 . 143.4(5) yes C34 . Fe27 . C37 . 63.5(4) yes C35 . Fe27 . C37 . 64.5(3) yes C36 . Fe27 . C37 . 40.8(4) yes P28 . Fe27 . C38 . 114.5(3) yes C32 . Fe27 . C38 . 154.6(4) yes C34 . Fe27 . C38 . 36.6(4) yes C35 . Fe27 . C38 . 63.0(3) yes C36 . Fe27 . C38 . 66.4(3) yes P28 . Fe27 . B39 . 92.0(2) yes C32 . Fe27 . B39 . 89.0(3) yes C34 . Fe27 . B39 . 88.8(3) yes C35 . Fe27 . B39 . 118.4(3) yes C36 . Fe27 . B39 . 152.4(3) yes C37 . Fe27 . C38 . 39.7(4) yes C37 . Fe27 . B39 . 127.0(5) yes C38 . Fe27 . B39 . 91.2(3) yes Fe27 . P28 . C29 . 117.6(2) yes Fe27 . P28 . C30 . 115.6(2) yes C29 . P28 . C30 . 98.2(3) yes Fe27 . P28 . C31 . 116.2(3) yes C29 . P28 . C31 . 103.0(4) yes C30 . P28 . C31 . 103.6(4) yes P28 . C29 . H292 . 109.1 no P28 . C29 . H291 . 109.9 no H292 . C29 . H291 . 109.1 no P28 . C29 . H293 . 109.0 no H292 . C29 . H293 . 110.2 no H291 . C29 . H293 . 109.5 no C30 2_656 C30 . P28 . 112.8(7) yes C30 2_656 C30 . H302 . 107.7 no P28 . C30 . H302 . 108.9 no C30 2_656 C30 . H301 . 109.1 no P28 . C30 . H301 . 109.0 no H302 . C30 . H301 . 109.4 no P28 . C31 . H311 . 109.2 no P28 . C31 . H313 . 109.9 no H311 . C31 . H313 . 109.1 no P28 . C31 . H312 . 110.2 no H311 . C31 . H312 . 109.3 no H313 . C31 . H312 . 109.1 no Fe27 . C32 . O33 . 177.7(6) yes Fe27 . C34 . C35 . 71.6(4) yes Fe27 . C34 . C38 . 71.5(5) yes C35 . C34 . C38 . 111.8(8) yes Fe27 . C34 . H341 . 124.2 no C35 . C34 . H341 . 122.5 no C38 . C34 . H341 . 125.8 no Fe27 . C35 . C34 . 71.4(4) yes Fe27 . C35 . C36 . 70.8(4) yes C34 . C35 . C36 . 110.4(8) yes Fe27 . C35 . H351 . 122.6 no C34 . C35 . H351 . 125.6 no C36 . C35 . H351 . 124.0 no Fe27 . C36 . C35 . 71.4(4) yes Fe27 . C36 . C37 . 69.4(4) yes C35 . C36 . C37 . 104.9(7) yes Fe27 . C36 . H361 . 126.2 no C35 . C36 . H361 . 127.4 no C37 . C36 . H361 . 127.5 no C36 . C37 . Fe27 . 69.8(4) yes C36 . C37 . C38 . 105.7(7) yes Fe27 . C37 . C38 . 70.4(4) yes C36 . C37 . H372 . 127.3 no Fe27 . C37 . H372 . 113.8 no C38 . C37 . H372 . 125.6 no Fe27 . C38 . C37 . 69.9(5) yes Fe27 . C38 . C34 . 71.9(4) yes C37 . C38 . C34 . 107.2(8) yes Fe27 . C38 . H381 . 126.4 no C37 . C38 . H381 . 126.4 no C34 . C38 . H381 . 126.2 no Fe27 . B39 . N40 . 175.6(5) yes B39 . N40 . C41 . 122.8(5) yes B39 . N40 . C47 . 123.4(5) yes C41 . N40 . C47 . 113.8(4) yes N40 . C41 . C42 . 110.9(5) yes N40 . C41 . C46 . 111.6(5) yes C42 . C41 . C46 . 112.1(5) yes N40 . C41 . H411 . 106.8 no C42 . C41 . H411 . 106.8 no C46 . C41 . H411 . 108.3 no C41 . C42 . C43 . 111.0(6) yes C41 . C42 . H421 . 109.7 no C43 . C42 . H421 . 111.3 no C41 . C42 . H422 . 107.0 no C43 . C42 . H422 . 107.9 no H421 . C42 . H422 . 109.8 no C42 . C43 . C44 . 112.0(6) yes C42 . C43 . H432 . 108.3 no C44 . C43 . H432 . 106.8 no C42 . C43 . H431 . 109.8 no C44 . C43 . H431 . 110.4 no H432 . C43 . H431 . 109.3 no C43 . C44 . C45 . 110.2(6) yes C43 . C44 . H441 . 110.3 no C45 . C44 . H441 . 109.9 no C43 . C44 . H442 . 108.9 no C45 . C44 . H442 . 107.5 no H441 . C44 . H442 . 110.0 no C44 . C45 . C46 . 110.6(6) yes C44 . C45 . H451 . 110.3 no C46 . C45 . H451 . 110.2 no C44 . C45 . H452 . 107.6 no C46 . C45 . H452 . 109.1 no H451 . C45 . H452 . 109.1 no C45 . C46 . C41 . 111.2(6) yes C45 . C46 . H462 . 109.0 no C41 . C46 . H462 . 108.3 no C45 . C46 . H461 . 110.2 no C41 . C46 . H461 . 109.3 no H462 . C46 . H461 . 108.8 no N40 . C47 . C48 . 110.7(5) yes N40 . C47 . C52 . 113.2(5) yes C48 . C47 . C52 . 110.8(6) yes N40 . C47 . H471 . 107.5 no C48 . C47 . H471 . 107.2 no C52 . C47 . H471 . 107.1 no C47 . C48 . C49 . 108.6(7) yes C47 . C48 . H482 . 109.2 no C49 . C48 . H482 . 108.9 no C47 . C48 . H481 . 108.4 no C49 . C48 . H481 . 111.6 no H482 . C48 . H481 . 110.1 no C48 . C49 . C50 . 111.3(6) yes C48 . C49 . H491 . 110.2 no C50 . C49 . H491 . 109.0 no C48 . C49 . H492 . 107.8 no C50 . C49 . H492 . 108.3 no H491 . C49 . H492 . 110.2 no C49 . C50 . C51 . 112.6(7) yes C49 . C50 . H501 . 107.6 no C51 . C50 . H501 . 108.9 no C49 . C50 . H502 . 109.1 no C51 . C50 . H502 . 109.0 no H501 . C50 . H502 . 109.7 no C50 . C51 . C52 . 112.2(7) yes C50 . C51 . H512 . 109.2 no C52 . C51 . H512 . 108.6 no C50 . C51 . H511 . 108.7 no C52 . C51 . H511 . 108.8 no H512 . C51 . H511 . 109.4 no C51 . C52 . C47 . 110.4(7) yes C51 . C52 . H521 . 110.5 no C47 . C52 . H521 . 108.5 no C51 . C52 . H522 . 109.9 no C47 . C52 . H522 . 107.7 no H521 . C52 . H522 . 109.8 no F53 . C54 . F55 . 106.2(4) yes F53 . C54 . F56 . 107.4(4) yes F55 . C54 . F56 . 106.9(5) yes F53 . C54 . C57 . 112.2(4) yes F55 . C54 . C57 . 111.6(4) yes F56 . C54 . C57 . 112.2(4) yes C54 . C57 . C58 . 118.8(5) yes C54 . C57 . C62 . 120.2(5) yes C58 . C57 . C62 . 121.0(5) yes C57 . C58 . C59 . 121.8(5) yes C57 . C58 . H581 . 119.1 no C59 . C58 . H581 . 119.1 no C58 . C59 . C60 . 115.5(5) yes C58 . C59 . B67 . 121.5(5) yes C60 . C59 . B67 . 122.4(5) yes C59 . C60 . C61 . 123.2(5) yes C59 . C60 . H601 . 118.0 no C61 . C60 . H601 . 118.8 no C60 . C61 . C62 . 120.1(5) yes C60 . C61 . C63 . 118.8(5) yes C62 . C61 . C63 . 121.0(5) yes C57 . C62 . C61 . 118.2(5) yes C57 . C62 . H621 . 120.3 no C61 . C62 . H621 . 121.5 no C61 . C63 . F64 . 113.1(5) yes C61 . C63 . F65 . 111.9(4) yes F64 . C63 . F65 . 106.7(5) yes C61 . C63 . F66 . 112.2(5) yes F64 . C63 . F66 . 107.5(5) yes F65 . C63 . F66 . 104.9(5) yes C59 . B67 . C68 . 112.3(4) yes C59 . B67 . C82 . 103.3(4) yes C68 . B67 . C82 . 112.3(4) yes C59 . B67 . C96 . 112.1(4) yes C68 . B67 . C96 . 103.5(4) yes C82 . B67 . C96 . 113.7(4) yes B67 . C68 . C69 . 121.0(4) yes B67 . C68 . C73 . 123.0(5) yes C69 . C68 . C73 . 115.9(5) yes C68 . C69 . C70 . 122.3(5) yes C68 . C69 . H691 . 118.5 no C70 . C69 . H691 . 119.2 no C69 . C70 . C71 . 120.5(5) yes C69 . C70 . C78 . 118.7(5) yes C71 . C70 . C78 . 120.8(5) yes C70 . C71 . C72 . 119.0(5) yes C70 . C71 . H711 . 120.7 no C72 . C71 . H711 . 120.2 no C71 . C72 . C73 . 120.1(5) yes C71 . C72 . C74 . 121.5(5) yes C73 . C72 . C74 . 118.4(5) yes C72 . C73 . C68 . 122.1(5) yes C72 . C73 . H731 . 118.5 no C68 . C73 . H731 . 119.3 no C72 . C74 . F75 . 113.1(4) yes C72 . C74 . F76 . 112.7(4) yes F75 . C74 . F76 . 106.6(5) yes C72 . C74 . F77 . 112.0(4) yes F75 . C74 . F77 . 106.3(5) yes F76 . C74 . F77 . 105.5(5) yes C70 . C78 . F79 . 113.4(4) yes C70 . C78 . F80 . 112.1(4) yes F79 . C78 . F80 . 106.2(5) yes C70 . C78 . F81 . 112.0(5) yes F79 . C78 . F81 . 106.6(5) yes F80 . C78 . F81 . 106.1(5) yes B67 . C82 . C83 . 122.5(5) yes B67 . C82 . C87 . 122.0(5) yes C83 . C82 . C87 . 115.4(5) yes C82 . C83 . C84 . 123.1(5) yes C82 . C83 . H831 . 118.6 no C84 . C83 . H831 . 118.3 no C83 . C84 . C85 . 120.2(5) yes C83 . C84 . C92 . 120.0(5) yes C85 . C84 . C92 . 119.7(5) yes C84 . C85 . C86 . 118.6(5) yes C84 . C85 . H851 . 120.8 no C86 . C85 . H851 . 120.6 no C85 . C86 . C87 . 119.5(5) yes C85 . C86 . C88 . 121.2(5) yes C87 . C86 . C88 . 119.2(5) yes C86 . C87 . C82 . 123.1(5) yes C86 . C87 . H871 . 118.1 no C82 . C87 . H871 . 118.8 no C86 . C88 . F89 . 113.0(5) yes C86 . C88 . F90 . 113.3(5) yes F89 . C88 . F90 . 101.0(5) yes C86 . C88 . F91 . 113.8(5) yes F89 . C88 . F91 . 107.0(6) yes F90 . C88 . F91 . 107.7(6) yes C84 . C92 . F93 . 112.6(5) yes C84 . C92 . F94 . 112.8(5) yes F93 . C92 . F94 . 105.3(5) yes C84 . C92 . F95 . 112.0(5) yes F93 . C92 . F95 . 106.7(5) yes F94 . C92 . F95 . 107.1(5) yes B67 . C96 . C97 . 123.1(5) yes B67 . C96 . C101 . 121.4(4) yes C97 . C96 . C101 . 115.2(5) yes C96 . C97 . C98 . 122.1(5) yes C96 . C97 . H971 . 118.9 no C98 . C97 . H971 . 119.0 no C97 . C98 . C99 . 121.1(5) yes C97 . C98 . C106 . 118.7(5) yes C99 . C98 . C106 . 120.3(5) yes C98 . C99 . C100 . 118.5(5) yes C98 . C99 . H991 . 121.0 no C100 . C99 . H991 . 120.5 no C99 . C100 . C101 . 119.9(5) yes C99 . C100 . C102 . 120.2(5) yes C101 . C100 . C102 . 119.9(5) yes C96 . C101 . C100 . 123.1(5) yes C96 . C101 . H1011 . 118.5 no C100 . C101 . H1011 . 118.4 no C100 . C102 . F103 . 112.5(4) yes C100 . C102 . F104 . 112.3(5) yes F103 . C102 . F104 . 105.5(5) yes C100 . C102 . F105 . 112.2(5) yes F103 . C102 . F105 . 107.9(5) yes F104 . C102 . F105 . 105.9(5) yes C98 . C106 . F107 . 113.4(5) yes C98 . C106 . F108 . 114.5(5) yes F107 . C106 . F108 . 103.3(6) yes C98 . C106 . F109 . 115.1(5) yes F107 . C106 . F109 . 105.6(7) yes F108 . C106 . F109 . 103.7(7) yes F110 . C111 . F112 . 103.5(5) yes F110 . C111 . F113 . 105.1(5) yes F112 . C111 . F113 . 108.5(6) yes F110 . C111 . C114 . 113.4(5) yes F112 . C111 . C114 . 113.2(5) yes F113 . C111 . C114 . 112.5(5) yes C111 . C114 . C115 . 121.6(5) yes C111 . C114 . C119 . 118.0(5) yes C115 . C114 . C119 . 120.3(5) yes C114 . C115 . C116 . 123.0(5) yes C114 . C115 . H1151 . 118.5 no C116 . C115 . H1151 . 118.4 no C115 . C116 . C117 . 114.9(5) yes C115 . C116 . B124 . 124.2(5) yes C117 . C116 . B124 . 120.8(5) yes C116 . C117 . C118 . 123.0(5) yes C116 . C117 . H1171 . 118.7 no C118 . C117 . H1171 . 118.3 no C117 . C118 . C119 . 120.4(5) yes C117 . C118 . C120 . 118.5(6) yes C119 . C118 . C120 . 121.0(6) yes C114 . C119 . C118 . 118.2(6) yes C114 . C119 . H1191 . 121.4 no C118 . C119 . H1191 . 120.3 no C118 . C120 . F121 . 114.3(6) yes C118 . C120 . F122 . 113.3(6) yes F121 . C120 . F122 . 106.8(7) yes C118 . C120 . F123 . 112.0(7) yes F121 . C120 . F123 . 105.7(7) yes F122 . C120 . F123 . 103.9(8) yes C116 . B124 . C125 . 111.1(4) yes C116 . B124 . C139 . 107.4(5) yes C125 . B124 . C139 . 109.8(5) yes C116 . B124 . C153 . 110.3(5) yes C125 . B124 . C153 . 107.2(4) yes C139 . B124 . C153 . 111.0(4) yes B124 . C125 . C126 . 120.4(5) yes B124 . C125 . C130 . 124.1(5) yes C126 . C125 . C130 . 115.5(5) yes C125 . C126 . C127 . 122.7(5) yes C125 . C126 . H1261 . 119.1 no C127 . C126 . H1261 . 118.3 no C126 . C127 . C128 . 120.6(5) yes C126 . C127 . C135 . 120.5(5) yes C128 . C127 . C135 . 118.9(5) yes C127 . C128 . C129 . 118.2(5) yes C127 . C128 . H1281 . 121.0 no C129 . C128 . H1281 . 120.8 no C128 . C129 . C130 . 120.3(5) yes C128 . C129 . C131 . 119.6(5) yes C130 . C129 . C131 . 120.1(5) yes C129 . C130 . C125 . 122.7(5) yes C129 . C130 . H1301 . 118.7 no C125 . C130 . H1301 . 118.6 no C129 . C131 . F132 . 112.8(5) yes C129 . C131 . F133 . 114.2(5) yes F132 . C131 . F133 . 103.9(5) yes C129 . C131 . F134 . 112.5(5) yes F132 . C131 . F134 . 107.0(6) yes F133 . C131 . F134 . 105.6(6) yes C127 . C135 . F136 . 114.0(5) yes C127 . C135 . F137 . 113.2(5) yes F136 . C135 . F137 . 104.7(5) yes C127 . C135 . F138 . 111.7(5) yes F136 . C135 . F138 . 106.1(5) yes F137 . C135 . F138 . 106.6(5) yes B124 . C139 . C140 . 120.5(5) yes B124 . C139 . C144 . 122.9(5) yes C140 . C139 . C144 . 116.6(6) yes C139 . C140 . C141 . 122.8(6) yes C139 . C140 . H1401 . 118.9 no C141 . C140 . H1401 . 118.3 no C140 . C141 . C142 . 119.6(6) yes C140 . C141 . C149 . 120.6(6) yes C142 . C141 . C149 . 119.7(6) yes C141 . C142 . C143 . 119.9(7) yes C141 . C142 . H1421 . 119.7 no C143 . C142 . H1421 . 120.3 no C142 . C143 . C144 . 119.6(7) yes C142 . C143 . C145 . 123.9(7) yes C144 . C143 . C145 . 116.4(7) yes C143 . C144 . C139 . 121.3(7) yes C143 . C144 . H1441 . 119.3 no C139 . C144 . H1441 . 119.3 no C143 . C145 . F146 . 114.8(9) yes C143 . C145 . F147 . 109.9(9) yes F146 . C145 . F147 . 105.2(8) yes C143 . C145 . F148 . 110.7(7) yes F146 . C145 . F148 . 114.1(11) yes F147 . C145 . F148 . 100.9(10) yes C141 . C149 . F150 . 117.4(6) yes C141 . C149 . F151 . 114.8(6) yes F150 . C149 . F151 . 107.1(7) yes C141 . C149 . F152 . 112.0(8) yes F150 . C149 . F152 . 102.4(7) yes F151 . C149 . F152 . 101.2(6) yes B124 . C153 . C154 . 124.5(5) yes B124 . C153 . C158 . 120.1(5) yes C154 . C153 . C158 . 115.4(5) yes C153 . C154 . C155 . 121.8(5) yes C153 . C154 . H1541 . 119.9 no C155 . C154 . H1541 . 118.3 no C154 . C155 . C156 . 121.4(5) yes C154 . C155 . C163 . 119.2(5) yes C156 . C155 . C163 . 119.3(5) yes C155 . C156 . C157 . 118.2(5) yes C155 . C156 . H1561 . 120.6 no C157 . C156 . H1561 . 121.2 no C156 . C157 . C158 . 120.2(5) yes C156 . C157 . C159 . 120.6(5) yes C158 . C157 . C159 . 119.2(5) yes C153 . C158 . C157 . 123.1(5) yes C153 . C158 . H1581 . 118.5 no C157 . C158 . H1581 . 118.4 no C157 . C159 . F160 . 114.1(5) yes C157 . C159 . F161 . 112.3(5) yes F160 . C159 . F161 . 104.4(6) yes C157 . C159 . F162 . 114.1(5) yes F160 . C159 . F162 . 105.4(6) yes F161 . C159 . F162 . 105.7(6) yes C155 . C163 . F164 . 114.3(5) yes C155 . C163 . F165 . 114.6(5) yes F164 . C163 . F165 . 107.1(6) yes C155 . C163 . F166 . 114.5(5) yes F164 . C163 . F166 . 104.3(7) yes F165 . C163 . F166 . 100.6(6) yes Cl167 . C168 . Cl169 . 121.1(6) yes Cl167 . C168 . H1681 . 105.6 no Cl169 . C168 . H1681 . 106.7 no Cl167 . C168 . H1682 . 106.3 no Cl169 . C168 . H1682 . 106.4 no H1681 . C168 . H1682 . 110.5 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C130 . H1301 . C140 . 131 0.94 2.50 3.198(10) yes #============================================================================== data_18b #============================================================================== _chemical_name_systematic ; . ; _chemical_name_common . _chemical_melting_point 'not measured' _chemical_formula_moiety 'C46 H22 B F24 Fe N O2, 0.5 (C6 H5 F)' _chemical_formula_sum 'C49 H24.50 B F24.50 Fe N O2' _chemical_formula_weight 1191.36 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.9155(2) _cell_length_b 16.2092(3) _cell_length_c 33.7381(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9797.4(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 356107 _cell_measurement_theta_min 5.097 _cell_measurement_theta_max 27.485 _exptl_crystal_description shapeless _exptl_crystal_colour clear_pale_yellow _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.615 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4744 _exptl_absorpt_coefficient_mu 0.443 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.904 _exptl_absorpt_correction_T_max 1.159 _exptl_absorpt_process_details ; Multi-scan from symmetry-related measurements using Sortav (Blessing 1995). ; _exptl_special_details ; The data collection nominally covered a hemisphere of reciprocal Space, by a combination of \w and \f scans. ; _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_type 'KappaCCD' _diffrn_measurement_method 'CCD' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 57876 _diffrn_reflns_av_R_equivalents 0.0786 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 5.12 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11086 _reflns_number_gt 6659 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0853P)^2^+11.5837P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 11086 _refine_ls_number_parameters 686 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1229 _refine_ls_R_factor_gt 0.0657 _refine_ls_wR_factor_ref 0.1883 _refine_ls_wR_factor_gt 0.1599 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.3451(2) 0.9837(2) 0.37483(11) 0.0301(8) Uani 1 1 d . . . C11 C 0.28990(18) 1.0565(2) 0.39200(9) 0.0312(7) Uani 1 1 d . . . C12 C 0.22064(18) 1.0745(2) 0.37475(10) 0.0328(7) Uani 1 1 d . . . H12 H 0.2047 1.0424 0.3528 0.039 Uiso 1 1 calc R . . C13 C 0.17430(19) 1.1370(2) 0.38834(10) 0.0317(7) Uani 1 1 d . . . C14 C 0.19594(19) 1.1873(2) 0.41939(10) 0.0346(8) Uani 1 1 d . . . H14 H 0.1648 1.2307 0.4286 0.042 Uiso 1 1 calc R . . C15 C 0.26519(19) 1.1719(2) 0.43674(10) 0.0339(8) Uani 1 1 d . . . C16 C 0.31046(19) 1.1088(2) 0.42335(10) 0.0330(8) Uani 1 1 d . . . H16 H 0.3574 1.1004 0.4358 0.040 Uiso 1 1 calc R . . C17 C 0.0988(2) 1.1474(2) 0.36998(11) 0.0389(8) Uani 1 1 d . . . C18 C 0.2876(2) 1.2233(2) 0.47167(11) 0.0446(9) Uani 1 1 d . . . F11 F 0.10115(16) 1.1761(2) 0.33357(9) 0.0977(12) Uani 1 1 d . . . F12 F 0.05380(17) 1.1934(3) 0.39038(11) 0.1200(16) Uani 1 1 d . . . F13 F 0.06320(13) 1.07601(17) 0.36545(10) 0.0723(8) Uani 1 1 d . . . F14 F 0.27395(15) 1.30329(14) 0.46658(8) 0.0639(7) Uani 1 1 d . . . F15 F 0.25077(18) 1.20151(19) 0.50446(7) 0.0813(9) Uani 1 1 d . . . F16 F 0.36032(13) 1.21767(15) 0.48022(7) 0.0576(6) Uani 1 1 d . . . C21 C 0.39319(18) 0.9368(2) 0.40967(10) 0.0309(7) Uani 1 1 d . . . C22 C 0.37141(19) 0.9315(2) 0.44931(10) 0.0350(8) Uani 1 1 d . . . H22 H 0.3264 0.9575 0.4574 0.042 Uiso 1 1 calc R . . C23 C 0.4135(2) 0.8893(2) 0.47744(10) 0.0391(8) Uani 1 1 d . . . C24 C 0.4792(2) 0.8506(2) 0.46729(11) 0.0401(9) Uani 1 1 d . . . H24 H 0.5083 0.8228 0.4867 0.048 Uiso 1 1 calc R . . C25 C 0.50173(18) 0.8533(2) 0.42792(10) 0.0330(8) Uani 1 1 d . . . C26 C 0.45911(18) 0.8948(2) 0.39994(10) 0.0319(7) Uani 1 1 d . . . H26 H 0.4753 0.8947 0.3731 0.038 Uiso 1 1 calc R . . C27 C 0.3903(3) 0.8872(3) 0.52018(12) 0.0530(11) Uani 1 1 d . . . C28 C 0.5738(2) 0.8132(2) 0.41675(11) 0.0430(9) Uani 1 1 d . . . F21 F 0.3898(2) 0.8110(2) 0.53490(9) 0.0980(11) Uani 1 1 d . . . F22 F 0.32094(19) 0.9107(3) 0.52630(8) 0.1022(12) Uani 1 1 d . . . F23 F 0.4347(2) 0.9275(3) 0.54288(8) 0.1347(18) Uani 1 1 d . . . F24 F 0.58618(13) 0.74221(15) 0.43475(7) 0.0597(6) Uani 1 1 d . . . F25 F 0.58026(14) 0.79803(18) 0.37808(7) 0.0664(8) Uani 1 1 d . . . F26 F 0.63218(13) 0.86063(18) 0.42626(11) 0.0817(9) Uani 1 1 d . . . C31 C 0.40171(18) 1.0305(2) 0.34359(10) 0.0301(7) Uani 1 1 d . . . C32 C 0.47148(18) 1.0600(2) 0.35543(10) 0.0321(7) Uani 1 1 d . . . H32 H 0.4867 1.0517 0.3821 0.039 Uiso 1 1 calc R . . C33 C 0.51950(18) 1.1011(2) 0.32981(10) 0.0320(7) Uani 1 1 d . . . C34 C 0.49977(19) 1.1151(2) 0.29071(10) 0.0362(8) Uani 1 1 d . . . H34 H 0.5327 1.1428 0.2731 0.043 Uiso 1 1 calc R . . C35 C 0.43012(19) 1.0875(2) 0.27799(10) 0.0348(8) Uani 1 1 d . . . C36 C 0.38231(19) 1.0475(2) 0.30415(10) 0.0331(8) Uani 1 1 d . . . H36 H 0.3345 1.0310 0.2949 0.040 Uiso 1 1 calc R . . C37 C 0.5919(2) 1.1305(2) 0.34593(11) 0.0388(8) Uani 1 1 d . . . C38 C 0.4059(2) 1.1029(3) 0.23634(11) 0.0419(9) Uani 1 1 d . . . F31 F 0.63167(12) 1.06998(15) 0.36322(8) 0.0568(6) Uani 1 1 d . . . F32 F 0.63720(12) 1.16435(16) 0.31876(7) 0.0580(7) Uani 1 1 d . . . F33 F 0.58280(12) 1.18812(14) 0.37424(7) 0.0500(6) Uani 1 1 d . . . F34 F 0.45985(15) 1.1232(2) 0.21230(7) 0.0871(10) Uani 1 1 d . . . F35 F 0.3758(2) 1.0370(2) 0.21969(8) 0.1124(14) Uani 1 1 d . . . F36 F 0.3555(2) 1.1602(3) 0.23311(8) 0.1092(14) Uani 1 1 d . . . C41 C 0.29626(18) 0.9105(2) 0.35312(9) 0.0291(7) Uani 1 1 d . . . C42 C 0.32155(18) 0.8668(2) 0.31989(9) 0.0303(7) Uani 1 1 d . . . H42 H 0.3690 0.8801 0.3090 0.036 Uiso 1 1 calc R . . C43 C 0.27932(19) 0.8047(2) 0.30230(10) 0.0325(8) Uani 1 1 d . . . C44 C 0.20946(19) 0.7840(2) 0.31677(10) 0.0341(8) Uani 1 1 d . . . H44 H 0.1801 0.7427 0.3043 0.041 Uiso 1 1 calc R . . C45 C 0.18378(18) 0.8254(2) 0.34994(10) 0.0325(7) Uani 1 1 d . . . C46 C 0.22732(18) 0.8859(2) 0.36799(10) 0.0306(7) Uani 1 1 d . . . H46 H 0.2092 0.9114 0.3914 0.037 Uiso 1 1 calc R . . C47 C 0.3079(2) 0.7620(2) 0.26591(11) 0.0405(9) Uani 1 1 d . . . C48 C 0.1073(2) 0.8086(2) 0.36594(12) 0.0409(9) Uani 1 1 d . . . F41 F 0.38206(12) 0.76717(14) 0.26173(6) 0.0490(6) Uani 1 1 d . . . F42 F 0.27774(14) 0.79255(16) 0.23252(6) 0.0611(7) Uani 1 1 d . . . F43 F 0.29140(14) 0.68134(14) 0.26573(7) 0.0549(6) Uani 1 1 d . . . F44 F 0.06717(15) 0.7601(2) 0.34282(10) 0.0916(11) Uani 1 1 d . . . F45 F 0.10658(14) 0.7791(2) 0.40195(9) 0.0959(12) Uani 1 1 d . . . F46 F 0.06673(12) 0.87791(15) 0.36849(8) 0.0568(6) Uani 1 1 d . . . Fe1 Fe 0.32366(3) 0.89867(3) 0.117051(15) 0.03649(16) Uani 1 1 d . . . O1 O 0.26261(16) 0.73562(19) 0.09844(9) 0.0553(7) Uani 1 1 d . . . O2 O 0.42308(15) 0.8455(2) 0.18102(8) 0.0548(7) Uani 1 1 d . . . N1 N 0.20386(18) 0.9219(2) 0.17848(9) 0.0429(7) Uani 1 1 d . . . C51 C 0.2943(3) 0.9530(3) 0.06306(13) 0.0581(12) Uani 1 1 d . . . H51 H 0.2480 0.9413 0.0475 0.070 Uiso 1 1 calc R . . C52 C 0.3622(3) 0.9124(3) 0.05919(13) 0.0615(12) Uani 1 1 d . . . H52 H 0.3728 0.8664 0.0403 0.074 Uiso 1 1 calc R . . C53 C 0.4125(2) 0.9470(3) 0.08469(14) 0.0633(13) Uani 1 1 d . . . H53 H 0.4661 0.9305 0.0875 0.076 Uiso 1 1 calc R . . C54 C 0.3766(3) 1.0112(3) 0.10618(14) 0.0683(14) Uani 1 1 d . . . H54 H 0.3998 1.0489 0.1262 0.082 Uiso 1 1 calc R . . C55 C 0.3024(3) 1.0143(3) 0.09142(15) 0.0652(14) Uani 1 1 d . . . H55 H 0.2629 1.0540 0.0999 0.078 Uiso 1 1 calc R . . C56 C 0.2873(2) 0.7982(3) 0.10547(11) 0.0399(9) Uani 1 1 d . . . C57 C 0.3844(2) 0.8644(3) 0.15601(12) 0.0430(9) Uani 1 1 d . . . C58 C 0.2487(2) 0.9154(2) 0.15397(11) 0.0398(8) Uani 1 1 d . . . C59 C 0.15522(19) 0.9309(2) 0.21067(11) 0.0386(8) Uani 1 1 d . . . C60 C 0.1696(2) 0.9917(3) 0.23790(11) 0.0449(9) Uani 1 1 d . . . H60 H 0.2109 1.0279 0.2347 0.054 Uiso 1 1 calc R . . C61 C 0.1223(2) 0.9990(3) 0.27021(12) 0.0499(10) Uani 1 1 d . . . H61 H 0.1307 1.0412 0.2893 0.060 Uiso 1 1 calc R . . C62 C 0.0637(2) 0.9461(3) 0.27487(12) 0.0509(10) Uani 1 1 d . . . H62 H 0.0323 0.9512 0.2974 0.061 Uiso 1 1 calc R . . C63 C 0.0496(3) 0.8856(3) 0.24739(13) 0.0586(12) Uani 1 1 d . . . H63 H 0.0081 0.8498 0.2507 0.070 Uiso 1 1 calc R . . C64 C 0.0961(2) 0.8772(3) 0.21487(12) 0.0526(11) Uani 1 1 d . . . H64 H 0.0875 0.8351 0.1958 0.063 Uiso 1 1 calc R . . F1S F 0.3771(4) 1.4817(4) 0.46547(19) 0.0876(12) Uiso 0.50 1 d P . . C1S C 0.4502(4) 1.4931(6) 0.4858(3) 0.0876(12) Uiso 0.50 1 d PG . . C2S C 0.4962(5) 1.5621(4) 0.4861(2) 0.0876(12) Uiso 0.50 1 d PG . . H2S H 0.4823 1.6101 0.4718 0.105 Uiso 0.50 1 calc PR . . C3S C 0.5626(4) 1.5609(5) 0.5074(3) 0.0876(12) Uiso 0.50 1 d PG . . H3S H 0.5941 1.6081 0.5076 0.105 Uiso 0.50 1 calc PR . . C4S C 0.5831(3) 1.4907(6) 0.5284(2) 0.0876(12) Uiso 0.50 1 d PG . . H4S H 0.6285 1.4899 0.5429 0.105 Uiso 0.50 1 calc PR . . C5S C 0.5371(5) 1.4216(4) 0.5281(2) 0.0876(12) Uiso 0.50 1 d PG . . H5S H 0.5510 1.3736 0.5425 0.105 Uiso 0.50 1 calc PR . . C6S C 0.4706(4) 1.4228(5) 0.5068(3) 0.0876(12) Uiso 0.50 1 d PG . . H6S H 0.4392 1.3756 0.5066 0.105 Uiso 0.50 1 calc PR . . 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 B1 0.0254(18) 0.034(2) 0.031(2) -0.0032(16) 0.0011(14) -0.0036(16) C11 0.0290(17) 0.0339(19) 0.0308(17) 0.0001(14) 0.0018(13) -0.0021(14) C12 0.0319(17) 0.0320(18) 0.0344(18) -0.0033(14) 0.0048(14) -0.0029(15) C13 0.0314(17) 0.0314(18) 0.0324(17) 0.0020(14) 0.0014(14) -0.0005(15) C14 0.0353(19) 0.0342(19) 0.0344(18) -0.0035(15) 0.0068(15) 0.0038(15) C15 0.0385(19) 0.0313(18) 0.0320(17) -0.0011(14) 0.0024(14) -0.0045(15) C16 0.0300(17) 0.037(2) 0.0320(17) -0.0025(15) 0.0013(14) -0.0031(15) C17 0.039(2) 0.037(2) 0.041(2) -0.0055(17) -0.0036(16) 0.0047(17) C18 0.052(2) 0.042(2) 0.039(2) -0.0073(17) -0.0016(18) -0.0018(19) F11 0.0636(18) 0.143(3) 0.086(2) 0.066(2) -0.0295(16) -0.0297(19) F12 0.0605(18) 0.165(3) 0.135(3) -0.100(3) -0.0425(19) 0.065(2) F13 0.0418(14) 0.0589(16) 0.116(2) 0.0108(15) -0.0231(14) -0.0077(12) F14 0.0779(18) 0.0411(14) 0.0728(17) -0.0218(12) -0.0207(14) 0.0081(12) F15 0.104(2) 0.101(2) 0.0388(13) -0.0226(14) 0.0201(14) -0.0325(18) F16 0.0554(15) 0.0635(16) 0.0538(14) -0.0222(12) -0.0204(11) 0.0088(12) C21 0.0296(17) 0.0298(18) 0.0333(17) -0.0058(14) -0.0001(14) -0.0050(14) C22 0.0316(18) 0.039(2) 0.0347(18) -0.0027(15) 0.0048(14) -0.0004(15) C23 0.043(2) 0.042(2) 0.0318(18) -0.0010(16) 0.0022(15) -0.0009(17) C24 0.0362(19) 0.049(2) 0.0350(19) 0.0029(16) -0.0039(15) 0.0015(17) C25 0.0279(17) 0.0338(19) 0.0373(19) -0.0025(15) 0.0002(14) -0.0033(15) C26 0.0293(17) 0.0345(19) 0.0318(17) -0.0022(15) 0.0008(14) -0.0042(15) C27 0.059(3) 0.066(3) 0.034(2) 0.002(2) 0.0035(19) 0.009(2) C28 0.035(2) 0.049(2) 0.045(2) 0.0046(18) -0.0002(16) 0.0037(18) F21 0.143(3) 0.091(2) 0.0608(18) 0.0278(17) 0.0391(19) 0.010(2) F22 0.095(2) 0.169(3) 0.0416(15) 0.0129(18) 0.0285(15) 0.055(2) F23 0.160(4) 0.209(4) 0.0348(15) -0.036(2) 0.0184(19) -0.101(3) F24 0.0564(14) 0.0600(16) 0.0626(15) 0.0109(12) 0.0061(12) 0.0222(12) F25 0.0557(15) 0.100(2) 0.0431(13) 0.0069(13) 0.0118(11) 0.0345(14) F26 0.0315(13) 0.0717(18) 0.142(3) -0.0221(18) 0.0038(15) -0.0050(13) C31 0.0297(17) 0.0278(18) 0.0328(17) -0.0047(14) 0.0004(14) 0.0016(14) C32 0.0291(17) 0.0331(19) 0.0340(18) -0.0040(15) 0.0006(14) -0.0006(15) C33 0.0300(17) 0.0300(18) 0.0360(18) -0.0040(15) 0.0026(14) -0.0011(14) C34 0.0347(18) 0.036(2) 0.0381(19) -0.0002(15) 0.0081(15) 0.0004(15) C35 0.0343(18) 0.038(2) 0.0324(17) 0.0011(15) 0.0025(14) 0.0045(15) C36 0.0307(17) 0.035(2) 0.0331(18) -0.0006(15) 0.0016(14) 0.0021(15) C37 0.0323(18) 0.042(2) 0.042(2) 0.0009(17) 0.0062(16) -0.0037(16) C38 0.037(2) 0.051(2) 0.038(2) 0.0032(18) 0.0038(16) 0.0011(18) F31 0.0351(12) 0.0562(15) 0.0792(17) 0.0089(13) -0.0122(11) -0.0006(11) F32 0.0421(13) 0.0783(17) 0.0537(14) 0.0048(12) 0.0089(11) -0.0255(12) F33 0.0464(13) 0.0522(14) 0.0513(13) -0.0124(11) -0.0026(10) -0.0121(11) F34 0.0536(15) 0.168(3) 0.0393(14) 0.0338(17) 0.0060(12) -0.0031(18) F35 0.181(4) 0.112(3) 0.0441(16) 0.0085(16) -0.038(2) -0.061(3) F36 0.117(3) 0.164(3) 0.0465(16) 0.0118(18) -0.0028(16) 0.096(3) C41 0.0257(16) 0.0305(18) 0.0309(17) 0.0011(14) -0.0025(13) 0.0020(14) C42 0.0252(16) 0.0347(19) 0.0312(17) -0.0012(14) 0.0002(13) 0.0001(14) C43 0.0326(18) 0.0330(19) 0.0318(18) -0.0021(14) -0.0007(14) 0.0042(15) C44 0.0307(17) 0.0305(18) 0.0411(19) -0.0063(15) -0.0055(15) 0.0005(14) C45 0.0262(16) 0.0302(18) 0.0411(19) -0.0008(15) 0.0018(14) -0.0017(14) C46 0.0299(17) 0.0307(18) 0.0314(17) 0.0003(14) 0.0004(13) 0.0010(14) C47 0.038(2) 0.044(2) 0.039(2) -0.0083(17) -0.0043(16) 0.0029(17) C48 0.037(2) 0.038(2) 0.048(2) -0.0024(18) 0.0030(17) -0.0032(17) F41 0.0412(12) 0.0601(15) 0.0458(12) -0.0175(11) 0.0106(10) 0.0013(11) F42 0.0717(17) 0.0764(17) 0.0350(12) -0.0101(11) -0.0071(11) 0.0255(14) F43 0.0612(15) 0.0414(13) 0.0620(15) -0.0206(11) 0.0081(12) -0.0012(11) F44 0.0491(15) 0.096(2) 0.130(3) -0.064(2) 0.0272(16) -0.0360(15) F45 0.0425(15) 0.152(3) 0.093(2) 0.078(2) 0.0162(14) 0.0096(17) F46 0.0349(12) 0.0535(14) 0.0821(17) 0.0023(13) 0.0145(12) 0.0048(11) Fe1 0.0287(3) 0.0450(3) 0.0358(3) 0.0030(2) 0.0022(2) 0.0017(2) O1 0.0474(17) 0.0492(18) 0.069(2) -0.0078(15) -0.0074(14) 0.0037(14) O2 0.0409(15) 0.081(2) 0.0429(15) 0.0074(15) -0.0083(13) -0.0020(15) N1 0.0381(17) 0.0465(19) 0.0442(18) 0.0006(15) 0.0066(15) 0.0066(15) C51 0.056(3) 0.066(3) 0.053(3) 0.025(2) -0.007(2) -0.008(2) C52 0.065(3) 0.075(3) 0.044(2) 0.010(2) 0.012(2) 0.004(3) C53 0.038(2) 0.087(4) 0.065(3) 0.034(3) 0.011(2) -0.003(2) C54 0.082(4) 0.067(3) 0.055(3) 0.012(2) -0.002(3) -0.036(3) C55 0.069(3) 0.049(3) 0.077(3) 0.026(3) 0.026(3) 0.014(2) C56 0.0299(19) 0.050(2) 0.040(2) 0.0018(18) -0.0018(16) 0.0112(18) C57 0.036(2) 0.051(2) 0.042(2) -0.0011(18) 0.0090(18) -0.0034(18) C58 0.0384(19) 0.037(2) 0.044(2) 0.0029(16) -0.0010(18) 0.0010(16) C59 0.0335(19) 0.045(2) 0.0373(19) 0.0018(17) 0.0045(15) 0.0057(16) C60 0.040(2) 0.048(2) 0.047(2) 0.0002(18) -0.0009(17) -0.0024(18) C61 0.057(3) 0.052(3) 0.041(2) -0.0056(19) -0.0018(19) 0.004(2) C62 0.053(3) 0.060(3) 0.040(2) 0.003(2) 0.0074(18) 0.009(2) C63 0.051(2) 0.070(3) 0.055(3) -0.003(2) 0.015(2) -0.015(2) C64 0.055(3) 0.055(3) 0.048(2) -0.011(2) 0.008(2) -0.012(2) _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 B1 C11 1.644(5) . ? B1 C21 1.644(5) . ? B1 C41 1.646(5) . ? B1 C31 1.647(5) . ? C11 C12 1.401(5) . ? C11 C16 1.405(5) . ? C12 C13 1.389(5) . ? C12 H12 0.9500 . ? C13 C14 1.383(5) . ? C13 C17 1.498(5) . ? C14 C15 1.394(5) . ? C14 H14 0.9500 . ? C15 C16 1.382(5) . ? C15 C18 1.498(5) . ? C16 H16 0.9500 . ? C17 F12 1.296(4) . ? C17 F11 1.315(5) . ? C17 F13 1.330(4) . ? C18 F14 1.331(5) . ? C18 F15 1.336(5) . ? C18 F16 1.337(5) . ? C21 C22 1.396(5) . ? C21 C26 1.402(5) . ? C22 C23 1.392(5) . ? C22 H22 0.9500 . ? C23 C24 1.376(5) . ? C23 C27 1.501(5) . ? C24 C25 1.389(5) . ? C24 H24 0.9500 . ? C25 C26 1.388(5) . ? C25 C28 1.494(5) . ? C26 H26 0.9500 . ? C27 F23 1.284(5) . ? C27 F22 1.316(5) . ? C27 F21 1.330(5) . ? C28 F24 1.320(4) . ? C28 F25 1.333(4) . ? C28 F26 1.336(5) . ? C31 C32 1.397(5) . ? C31 C36 1.403(5) . ? C32 C33 1.390(5) . ? C32 H32 0.9500 . ? C33 C34 1.384(5) . ? C33 C37 1.485(5) . ? C34 C35 1.393(5) . ? C34 H34 0.9500 . ? C35 C36 1.390(5) . ? C35 C38 1.491(5) . ? C36 H36 0.9500 . ? C37 F32 1.342(4) . ? C37 F31 1.345(4) . ? C37 F33 1.346(4) . ? C38 F36 1.301(5) . ? C38 F34 1.304(4) . ? C38 F35 1.321(5) . ? C41 C46 1.392(5) . ? C41 C42 1.401(5) . ? C42 C43 1.393(5) . ? C42 H42 0.9500 . ? C43 C44 1.384(5) . ? C43 C47 1.499(5) . ? C44 C45 1.383(5) . ? C44 H44 0.9500 . ? C45 C46 1.393(5) . ? C45 C48 1.497(5) . ? C46 H46 0.9500 . ? C47 F41 1.339(4) . ? C47 F43 1.341(4) . ? C47 F42 1.344(4) . ? C48 F45 1.306(5) . ? C48 F44 1.321(4) . ? C48 F46 1.341(4) . ? Fe1 C57 1.794(4) . ? Fe1 C56 1.796(5) . ? Fe1 C58 1.851(4) . ? Fe1 C52 2.082(4) . ? Fe1 C53 2.084(4) . ? Fe1 C54 2.088(5) . ? Fe1 C51 2.091(4) . ? Fe1 C55 2.098(4) . ? O1 C56 1.132(5) . ? O2 C57 1.134(5) . ? N1 C58 1.158(5) . ? N1 C59 1.400(5) . ? C51 C55 1.386(7) . ? C51 C52 1.388(7) . ? C51 H51 1.0000 . ? C52 C53 1.367(7) . ? C52 H52 1.0000 . ? C53 C54 1.422(7) . ? C53 H53 1.0000 . ? C54 C55 1.420(7) . ? C54 H54 1.0000 . ? C55 H55 1.0000 . ? C59 C60 1.372(5) . ? C59 C64 1.378(6) . ? C60 C61 1.386(5) . ? C60 H60 0.9500 . ? C61 C62 1.364(6) . ? C61 H61 0.9500 . ? C62 C63 1.373(6) . ? C62 H62 0.9500 . ? C63 C64 1.384(6) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? F1S C1S 1.490(9) . ? C1S C2S 1.3900 . ? C1S C6S 1.3900 . ? C2S C3S 1.3900 . ? C2S H2S 0.9500 . ? C3S C4S 1.3900 . ? C3S H3S 0.9500 . ? C4S C5S 1.3900 . ? C4S H4S 0.9500 . ? C5S C6S 1.3900 . ? C5S H5S 0.9500 . ? C6S H6S 0.9500 . ? 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 C11 B1 C21 113.3(3) . . ? C11 B1 C41 110.8(3) . . ? C21 B1 C41 105.2(3) . . ? C11 B1 C31 105.4(3) . . ? C21 B1 C31 110.3(3) . . ? C41 B1 C31 112.0(3) . . ? C12 C11 C16 114.8(3) . . ? C12 C11 B1 122.4(3) . . ? C16 C11 B1 122.7(3) . . ? C13 C12 C11 123.0(3) . . ? C13 C12 H12 118.5 . . ? C11 C12 H12 118.5 . . ? C14 C13 C12 120.9(3) . . ? C14 C13 C17 120.1(3) . . ? C12 C13 C17 119.0(3) . . ? C13 C14 C15 117.5(3) . . ? C13 C14 H14 121.2 . . ? C15 C14 H14 121.2 . . ? C16 C15 C14 121.2(3) . . ? C16 C15 C18 120.7(3) . . ? C14 C15 C18 118.0(3) . . ? C15 C16 C11 122.6(3) . . ? C15 C16 H16 118.7 . . ? C11 C16 H16 118.7 . . ? F12 C17 F11 108.2(4) . . ? F12 C17 F13 105.3(4) . . ? F11 C17 F13 102.5(3) . . ? F12 C17 C13 114.0(3) . . ? F11 C17 C13 113.4(3) . . ? F13 C17 C13 112.6(3) . . ? F14 C18 F15 105.8(3) . . ? F14 C18 F16 105.9(3) . . ? F15 C18 F16 106.6(3) . . ? F14 C18 C15 113.0(3) . . ? F15 C18 C15 111.8(3) . . ? F16 C18 C15 113.2(3) . . ? C22 C21 C26 115.4(3) . . ? C22 C21 B1 124.5(3) . . ? C26 C21 B1 119.9(3) . . ? C23 C22 C21 122.1(3) . . ? C23 C22 H22 118.9 . . ? C21 C22 H22 118.9 . . ? C24 C23 C22 121.2(3) . . ? C24 C23 C27 117.8(3) . . ? C22 C23 C27 121.0(3) . . ? C23 C24 C25 118.2(3) . . ? C23 C24 H24 120.9 . . ? C25 C24 H24 120.9 . . ? C26 C25 C24 120.4(3) . . ? C26 C25 C28 121.0(3) . . ? C24 C25 C28 118.6(3) . . ? C25 C26 C21 122.7(3) . . ? C25 C26 H26 118.7 . . ? C21 C26 H26 118.7 . . ? F23 C27 F22 110.2(4) . . ? F23 C27 F21 104.7(4) . . ? F22 C27 F21 101.8(4) . . ? F23 C27 C23 112.9(4) . . ? F22 C27 C23 114.0(3) . . ? F21 C27 C23 112.4(4) . . ? F24 C28 F25 105.9(3) . . ? F24 C28 F26 105.1(3) . . ? F25 C28 F26 105.9(3) . . ? F24 C28 C25 114.1(3) . . ? F25 C28 C25 113.7(3) . . ? F26 C28 C25 111.5(3) . . ? C32 C31 C36 115.2(3) . . ? C32 C31 B1 121.7(3) . . ? C36 C31 B1 123.0(3) . . ? C33 C32 C31 122.7(3) . . ? C33 C32 H32 118.6 . . ? C31 C32 H32 118.6 . . ? C34 C33 C32 120.9(3) . . ? C34 C33 C37 121.3(3) . . ? C32 C33 C37 117.8(3) . . ? C33 C34 C35 118.0(3) . . ? C33 C34 H34 121.0 . . ? C35 C34 H34 121.0 . . ? C36 C35 C34 120.4(3) . . ? C36 C35 C38 119.8(3) . . ? C34 C35 C38 119.8(3) . . ? C35 C36 C31 122.8(3) . . ? C35 C36 H36 118.6 . . ? C31 C36 H36 118.6 . . ? F32 C37 F31 105.9(3) . . ? F32 C37 F33 105.9(3) . . ? F31 C37 F33 105.2(3) . . ? F32 C37 C33 114.2(3) . . ? F31 C37 C33 112.9(3) . . ? F33 C37 C33 112.1(3) . . ? F36 C38 F34 106.4(4) . . ? F36 C38 F35 104.9(4) . . ? F34 C38 F35 104.0(3) . . ? F36 C38 C35 113.6(3) . . ? F34 C38 C35 114.4(3) . . ? F35 C38 C35 112.6(3) . . ? C46 C41 C42 115.5(3) . . ? C46 C41 B1 121.2(3) . . ? C42 C41 B1 123.3(3) . . ? C43 C42 C41 122.1(3) . . ? C43 C42 H42 119.0 . . ? C41 C42 H42 119.0 . . ? C44 C43 C42 121.0(3) . . ? C44 C43 C47 119.1(3) . . ? C42 C43 C47 119.8(3) . . ? C45 C44 C43 118.0(3) . . ? C45 C44 H44 121.0 . . ? C43 C44 H44 121.0 . . ? C44 C45 C46 120.6(3) . . ? C44 C45 C48 120.5(3) . . ? C46 C45 C48 118.8(3) . . ? C41 C46 C45 122.8(3) . . ? C41 C46 H46 118.6 . . ? C45 C46 H46 118.6 . . ? F41 C47 F43 106.2(3) . . ? F41 C47 F42 106.7(3) . . ? F43 C47 F42 105.5(3) . . ? F41 C47 C43 113.4(3) . . ? F43 C47 C43 112.2(3) . . ? F42 C47 C43 112.3(3) . . ? F45 C48 F44 109.0(4) . . ? F45 C48 F46 104.0(3) . . ? F44 C48 F46 104.0(3) . . ? F45 C48 C45 114.3(3) . . ? F44 C48 C45 113.2(3) . . ? F46 C48 C45 111.6(3) . . ? C57 Fe1 C56 95.68(17) . . ? C57 Fe1 C58 89.56(16) . . ? C56 Fe1 C58 90.94(16) . . ? C57 Fe1 C52 121.27(18) . . ? C56 Fe1 C52 90.77(19) . . ? C58 Fe1 C52 148.77(18) . . ? C57 Fe1 C53 92.10(18) . . ? C56 Fe1 C53 120.3(2) . . ? C58 Fe1 C53 148.4(2) . . ? C52 Fe1 C53 38.32(19) . . ? C57 Fe1 C54 97.1(2) . . ? C56 Fe1 C54 156.63(19) . . ? C58 Fe1 C54 108.6(2) . . ? C52 Fe1 C54 65.9(2) . . ? C53 Fe1 C54 39.8(2) . . ? C57 Fe1 C51 157.08(17) . . ? C56 Fe1 C51 95.82(18) . . ? C58 Fe1 C51 109.99(18) . . ? C52 Fe1 C51 38.86(18) . . ? C53 Fe1 C51 64.99(18) . . ? C54 Fe1 C51 65.99(19) . . ? C57 Fe1 C55 133.5(2) . . ? C56 Fe1 C55 130.8(2) . . ? C58 Fe1 C55 90.84(17) . . ? C52 Fe1 C55 65.04(19) . . ? C53 Fe1 C55 65.60(19) . . ? C54 Fe1 C55 39.7(2) . . ? C51 Fe1 C55 38.65(19) . . ? C58 N1 C59 174.5(4) . . ? C55 C51 C52 108.2(4) . . ? C55 C51 Fe1 71.0(3) . . ? C52 C51 Fe1 70.2(2) . . ? C55 C51 H51 125.9 . . ? C52 C51 H51 125.9 . . ? Fe1 C51 H51 125.9 . . ? C53 C52 C51 108.9(5) . . ? C53 C52 Fe1 70.9(3) . . ? C51 C52 Fe1 70.9(3) . . ? C53 C52 H52 125.5 . . ? C51 C52 H52 125.5 . . ? Fe1 C52 H52 125.5 . . ? C52 C53 C54 108.8(4) . . ? C52 C53 Fe1 70.8(3) . . ? C54 C53 Fe1 70.3(2) . . ? C52 C53 H53 125.6 . . ? C54 C53 H53 125.6 . . ? Fe1 C53 H53 125.6 . . ? C55 C54 C53 105.7(4) . . ? C55 C54 Fe1 70.5(3) . . ? C53 C54 Fe1 69.9(3) . . ? C55 C54 H54 127.1 . . ? C53 C54 H54 127.1 . . ? Fe1 C54 H54 127.1 . . ? C51 C55 C54 108.4(4) . . ? C51 C55 Fe1 70.4(3) . . ? C54 C55 Fe1 69.8(3) . . ? C51 C55 H55 125.8 . . ? C54 C55 H55 125.8 . . ? Fe1 C55 H55 125.8 . . ? O1 C56 Fe1 178.2(3) . . ? O2 C57 Fe1 177.7(4) . . ? N1 C58 Fe1 175.6(3) . . ? C60 C59 C64 122.0(4) . . ? C60 C59 N1 118.5(3) . . ? C64 C59 N1 119.5(4) . . ? C59 C60 C61 118.2(4) . . ? C59 C60 H60 120.9 . . ? C61 C60 H60 120.9 . . ? C62 C61 C60 120.5(4) . . ? C62 C61 H61 119.8 . . ? C60 C61 H61 119.8 . . ? C61 C62 C63 120.8(4) . . ? C61 C62 H62 119.6 . . ? C63 C62 H62 119.6 . . ? C62 C63 C64 119.7(4) . . ? C62 C63 H63 120.2 . . ? C64 C63 H63 120.2 . . ? C59 C64 C63 118.8(4) . . ? C59 C64 H64 120.6 . . ? C63 C64 H64 120.6 . . ? C2S C1S C6S 120.0 . . ? C2S C1S F1S 128.6(7) . . ? C6S C1S F1S 111.4(7) . . ? C3S C2S C1S 120.0 . . ? C3S C2S H2S 120.0 . . ? C1S C2S H2S 120.0 . . ? C2S C3S C4S 120.0 . . ? C2S C3S H3S 120.0 . . ? C4S C3S H3S 120.0 . . ? C5S C4S C3S 120.0 . . ? C5S C4S H4S 120.0 . . ? C3S C4S H4S 120.0 . . ? C4S C5S C6S 120.0 . . ? C4S C5S H5S 120.0 . . ? C6S C5S H5S 120.0 . . ? C5S C6S C1S 120.0 . . ? C5S C6S H6S 120.0 . . ? C1S C6S H6S 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 B1 C11 C12 -146.4(3) . . . . ? C41 B1 C11 C12 -28.4(4) . . . . ? C31 B1 C11 C12 92.9(4) . . . . ? C21 B1 C11 C16 37.9(4) . . . . ? C41 B1 C11 C16 155.8(3) . . . . ? C31 B1 C11 C16 -82.8(4) . . . . ? C16 C11 C12 C13 -2.3(5) . . . . ? B1 C11 C12 C13 -178.4(3) . . . . ? C11 C12 C13 C14 2.2(5) . . . . ? C11 C12 C13 C17 -175.3(3) . . . . ? C12 C13 C14 C15 -0.9(5) . . . . ? C17 C13 C14 C15 176.5(3) . . . . ? C13 C14 C15 C16 0.0(5) . . . . ? C13 C14 C15 C18 -177.1(3) . . . . ? C14 C15 C16 C11 -0.3(5) . . . . ? C18 C15 C16 C11 176.7(3) . . . . ? C12 C11 C16 C15 1.4(5) . . . . ? B1 C11 C16 C15 177.5(3) . . . . ? C14 C13 C17 F12 -12.9(5) . . . . ? C12 C13 C17 F12 164.6(4) . . . . ? C14 C13 C17 F11 111.5(4) . . . . ? C12 C13 C17 F11 -71.0(5) . . . . ? C14 C13 C17 F13 -132.7(4) . . . . ? C12 C13 C17 F13 44.8(5) . . . . ? C16 C15 C18 F14 138.0(4) . . . . ? C14 C15 C18 F14 -44.8(5) . . . . ? C16 C15 C18 F15 -102.7(4) . . . . ? C14 C15 C18 F15 74.4(4) . . . . ? C16 C15 C18 F16 17.7(5) . . . . ? C14 C15 C18 F16 -165.2(3) . . . . ? C11 B1 C21 C22 25.1(5) . . . . ? C41 B1 C21 C22 -96.1(4) . . . . ? C31 B1 C21 C22 143.0(3) . . . . ? C11 B1 C21 C26 -158.3(3) . . . . ? C41 B1 C21 C26 80.5(4) . . . . ? C31 B1 C21 C26 -40.5(4) . . . . ? C26 C21 C22 C23 1.8(5) . . . . ? B1 C21 C22 C23 178.5(3) . . . . ? C21 C22 C23 C24 0.0(6) . . . . ? C21 C22 C23 C27 177.7(4) . . . . ? C22 C23 C24 C25 -1.3(6) . . . . ? C27 C23 C24 C25 -179.0(4) . . . . ? C23 C24 C25 C26 0.6(5) . . . . ? C23 C24 C25 C28 178.5(3) . . . . ? C24 C25 C26 C21 1.3(5) . . . . ? C28 C25 C26 C21 -176.6(3) . . . . ? C22 C21 C26 C25 -2.4(5) . . . . ? B1 C21 C26 C25 -179.3(3) . . . . ? C24 C23 C27 F23 66.1(6) . . . . ? C22 C23 C27 F23 -111.7(5) . . . . ? C24 C23 C27 F22 -167.3(4) . . . . ? C22 C23 C27 F22 14.9(6) . . . . ? C24 C23 C27 F21 -52.1(5) . . . . ? C22 C23 C27 F21 130.1(4) . . . . ? C26 C25 C28 F24 -142.1(3) . . . . ? C24 C25 C28 F24 40.0(5) . . . . ? C26 C25 C28 F25 -20.5(5) . . . . ? C24 C25 C28 F25 161.6(3) . . . . ? C26 C25 C28 F26 99.1(4) . . . . ? C24 C25 C28 F26 -78.8(4) . . . . ? C11 B1 C31 C32 93.6(4) . . . . ? C21 B1 C31 C32 -29.0(4) . . . . ? C41 B1 C31 C32 -145.9(3) . . . . ? C11 B1 C31 C36 -82.8(4) . . . . ? C21 B1 C31 C36 154.5(3) . . . . ? C41 B1 C31 C36 37.7(4) . . . . ? C36 C31 C32 C33 -1.9(5) . . . . ? B1 C31 C32 C33 -178.6(3) . . . . ? C31 C32 C33 C34 0.3(5) . . . . ? C31 C32 C33 C37 179.4(3) . . . . ? C32 C33 C34 C35 0.6(5) . . . . ? C37 C33 C34 C35 -178.4(3) . . . . ? C33 C34 C35 C36 0.3(5) . . . . ? C33 C34 C35 C38 178.7(3) . . . . ? C34 C35 C36 C31 -2.2(5) . . . . ? C38 C35 C36 C31 179.4(3) . . . . ? C32 C31 C36 C35 2.9(5) . . . . ? B1 C31 C36 C35 179.5(3) . . . . ? C34 C33 C37 F32 -5.3(5) . . . . ? C32 C33 C37 F32 175.6(3) . . . . ? C34 C33 C37 F31 -126.3(4) . . . . ? C32 C33 C37 F31 54.6(4) . . . . ? C34 C33 C37 F33 115.1(4) . . . . ? C32 C33 C37 F33 -64.0(4) . . . . ? C36 C35 C38 F36 72.4(5) . . . . ? C34 C35 C38 F36 -106.0(4) . . . . ? C36 C35 C38 F34 -165.2(4) . . . . ? C34 C35 C38 F34 16.4(5) . . . . ? C36 C35 C38 F35 -46.7(5) . . . . ? C34 C35 C38 F35 134.9(4) . . . . ? C11 B1 C41 C46 -37.0(4) . . . . ? C21 B1 C41 C46 85.8(4) . . . . ? C31 B1 C41 C46 -154.4(3) . . . . ? C11 B1 C41 C42 145.5(3) . . . . ? C21 B1 C41 C42 -91.7(4) . . . . ? C31 B1 C41 C42 28.1(4) . . . . ? C46 C41 C42 C43 1.8(5) . . . . ? B1 C41 C42 C43 179.5(3) . . . . ? C41 C42 C43 C44 0.9(5) . . . . ? C41 C42 C43 C47 177.8(3) . . . . ? C42 C43 C44 C45 -1.9(5) . . . . ? C47 C43 C44 C45 -178.8(3) . . . . ? C43 C44 C45 C46 0.0(5) . . . . ? C43 C44 C45 C48 177.2(3) . . . . ? C42 C41 C46 C45 -3.7(5) . . . . ? B1 C41 C46 C45 178.6(3) . . . . ? C44 C45 C46 C41 2.9(5) . . . . ? C48 C45 C46 C41 -174.3(3) . . . . ? C44 C43 C47 F41 -160.6(3) . . . . ? C42 C43 C47 F41 22.5(5) . . . . ? C44 C43 C47 F43 -40.3(4) . . . . ? C42 C43 C47 F43 142.8(3) . . . . ? C44 C43 C47 F42 78.3(4) . . . . ? C42 C43 C47 F42 -98.6(4) . . . . ? C44 C45 C48 F45 118.1(4) . . . . ? C46 C45 C48 F45 -64.7(5) . . . . ? C44 C45 C48 F44 -7.5(5) . . . . ? C46 C45 C48 F44 169.7(3) . . . . ? C44 C45 C48 F46 -124.3(4) . . . . ? C46 C45 C48 F46 52.9(4) . . . . ? C57 Fe1 C51 C55 -82.6(6) . . . . ? C56 Fe1 C51 C55 157.7(3) . . . . ? C58 Fe1 C51 C55 64.5(3) . . . . ? C52 Fe1 C51 C55 -118.4(4) . . . . ? C53 Fe1 C51 C55 -81.6(3) . . . . ? C54 Fe1 C51 C55 -37.6(3) . . . . ? C57 Fe1 C51 C52 35.8(6) . . . . ? C56 Fe1 C51 C52 -84.0(3) . . . . ? C58 Fe1 C51 C52 -177.1(3) . . . . ? C53 Fe1 C51 C52 36.8(3) . . . . ? C54 Fe1 C51 C52 80.8(3) . . . . ? C55 Fe1 C51 C52 118.4(4) . . . . ? C55 C51 C52 C53 0.2(5) . . . . ? Fe1 C51 C52 C53 -61.0(3) . . . . ? C55 C51 C52 Fe1 61.1(3) . . . . ? C57 Fe1 C52 C53 -45.6(4) . . . . ? C56 Fe1 C52 C53 -142.7(3) . . . . ? C58 Fe1 C52 C53 124.2(4) . . . . ? C54 Fe1 C52 C53 37.8(3) . . . . ? C51 Fe1 C52 C53 118.9(4) . . . . ? C55 Fe1 C52 C53 81.6(3) . . . . ? C57 Fe1 C52 C51 -164.5(3) . . . . ? C56 Fe1 C52 C51 98.3(3) . . . . ? C58 Fe1 C52 C51 5.2(5) . . . . ? C53 Fe1 C52 C51 -118.9(4) . . . . ? C54 Fe1 C52 C51 -81.1(3) . . . . ? C55 Fe1 C52 C51 -37.3(3) . . . . ? C51 C52 C53 C54 0.7(5) . . . . ? Fe1 C52 C53 C54 -60.2(3) . . . . ? C51 C52 C53 Fe1 61.0(3) . . . . ? C57 Fe1 C53 C52 142.3(3) . . . . ? C56 Fe1 C53 C52 44.5(4) . . . . ? C58 Fe1 C53 C52 -125.1(4) . . . . ? C54 Fe1 C53 C52 -119.2(4) . . . . ? C51 Fe1 C53 C52 -37.3(3) . . . . ? C55 Fe1 C53 C52 -80.0(3) . . . . ? C57 Fe1 C53 C54 -98.5(3) . . . . ? C56 Fe1 C53 C54 163.7(3) . . . . ? C58 Fe1 C53 C54 -6.0(5) . . . . ? C52 Fe1 C53 C54 119.2(4) . . . . ? C51 Fe1 C53 C54 81.9(3) . . . . ? C55 Fe1 C53 C54 39.1(3) . . . . ? C52 C53 C54 C55 -1.3(5) . . . . ? Fe1 C53 C54 C55 -61.9(3) . . . . ? C52 C53 C54 Fe1 60.6(3) . . . . ? C57 Fe1 C54 C55 -159.4(3) . . . . ? C56 Fe1 C54 C55 78.0(6) . . . . ? C58 Fe1 C54 C55 -67.5(3) . . . . ? C52 Fe1 C54 C55 79.4(3) . . . . ? C53 Fe1 C54 C55 115.8(4) . . . . ? C51 Fe1 C54 C55 36.7(3) . . . . ? C57 Fe1 C54 C53 84.8(3) . . . . ? C56 Fe1 C54 C53 -37.8(6) . . . . ? C58 Fe1 C54 C53 176.7(3) . . . . ? C52 Fe1 C54 C53 -36.4(3) . . . . ? C51 Fe1 C54 C53 -79.1(3) . . . . ? C55 Fe1 C54 C53 -115.8(4) . . . . ? C52 C51 C55 C54 -1.0(5) . . . . ? Fe1 C51 C55 C54 59.7(3) . . . . ? C52 C51 C55 Fe1 -60.7(3) . . . . ? C53 C54 C55 C51 1.4(5) . . . . ? Fe1 C54 C55 C51 -60.0(3) . . . . ? C53 C54 C55 Fe1 61.5(3) . . . . ? C57 Fe1 C55 C51 147.9(3) . . . . ? C56 Fe1 C55 C51 -30.0(4) . . . . ? C58 Fe1 C55 C51 -122.0(3) . . . . ? C52 Fe1 C55 C51 37.5(3) . . . . ? C53 Fe1 C55 C51 79.9(3) . . . . ? C54 Fe1 C55 C51 119.2(4) . . . . ? C57 Fe1 C55 C54 28.7(4) . . . . ? C56 Fe1 C55 C54 -149.2(3) . . . . ? C58 Fe1 C55 C54 118.9(3) . . . . ? C52 Fe1 C55 C54 -81.7(3) . . . . ? C53 Fe1 C55 C54 -39.3(3) . . . . ? C51 Fe1 C55 C54 -119.2(4) . . . . ? C64 C59 C60 C61 -0.7(6) . . . . ? N1 C59 C60 C61 -178.4(3) . . . . ? C59 C60 C61 C62 0.9(6) . . . . ? C60 C61 C62 C63 -1.2(7) . . . . ? C61 C62 C63 C64 1.1(7) . . . . ? C60 C59 C64 C63 0.7(6) . . . . ? N1 C59 C64 C63 178.4(4) . . . . ? C62 C63 C64 C59 -0.9(7) . . . . ? C6S C1S C2S C3S 0.0 . . . . ? F1S C1S C2S C3S 179.4(8) . . . . ? C1S C2S C3S C4S 0.0 . . . . ? C2S C3S C4S C5S 0.0 . . . . ? C3S C4S C5S C6S 0.0 . . . . ? C4S C5S C6S C1S 0.0 . . . . ? C2S C1S C6S C5S 0.0 . . . . ? F1S C1S C6S C5S -179.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.001 _refine_diff_density_min -1.233 _refine_diff_density_rms 0.077 #============================================================================== # start Validation Reply Form _vrf_PLAT242_4 ; PROBLEM: Check Low Ueq as Compared to Neighbors for C53 RESPONSE: The strucure includes serverely librating CF~3~ groups. Although the worst of the disorder has been modelled using parts, some of the ellipses are still quite large compared to their parent carbon. ; _vrf_PLAT220_9 ; PROBLEM: Large Non-Solvent F Ueq(max)/Ueq(min) ... 5.01 Ratio RESPONSE: The strucure includes serverely librating CF~3~ groups. Although the worst of the disorder has been modelled using parts, some of the ellipses are still quite large and prolate. ; _vrf_PLAT213_11 ; PROBLEM: Atom F148 has ADP max/min Ratio ............. 5.20 prola RESPONSE: The strucure includes serverely librating CF~3~ groups. Although the worst of the disorder has been modelled using parts, some of the ellipses are still quite large and prolate. ; _vrf_PLAT220_11 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.65 Ratio RESPONSE: The structure contains a lot of cyclohexyl groups that exhibit a lot of thermal motion. ; _vrf_PLAT242_11 ; PROBLEM: Check Low Ueq as Compared to Neighbors for C106 RESPONSE: The strucure includes serverely librating CF~3~ groups. Although the worst of the disorder has been modelled using parts, some of the ellipses are still quite large and prolate. ; # end Validation Reply Form