# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Eur.J.Inorg.Chem. _journal_coden_cambridge 1290 _journal_year 2005 _journal_page_first 4255 _journal_volume ? _publ_contact_author_address # ; IEM-UMII, cc047, 34095 Montpellier Cedex 5, France ; _publ_contact_author_email barboiu@iemm.univ-montp2.fr _publ_contact_author_name 'M. Barboiu' loop_ _publ_author_name 'F. Dumitru' 'E. Petit' 'A.van der Lee' 'M. Barboiu' data_CRYSTALS_cif1 _database_code_depnum_ccdc_archive 'CCDC 266698' _audit_creation_date 04-08-19 _audit_creation_method CRYSTALS_ver_12.39 _oxford_structure_analysis_title vdlee21 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 8.2081(3) _cell_length_b 14.5003(5) _cell_length_c 18.7227(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2228.37(14) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 2 21 21 ' _symmetry_space_group_name_Hall 'P 2bc 2 ' 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 57.7997 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Zn 0.2220 1.4310 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097 1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 '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' 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' _cell_formula_units_Z 2 # Given Formula = C25 H3 F6 N3 O3 S1 Zn1 # Dc = 1.80 Fooo = 1040.00 Mu = 12.83 M = 604.75 # Found Formula = C22 H18 F3 N4 O3 S1 Zn0.50 # Dc = 1.51 FOOO = 1040.00 Mu = 7.28 M = 508.16 _chemical_formula_sum 'C44 H36 F6 N8 O6 S2 Zn ' _chemical_formula_moiety 'C38 H30 N6 Zn, 2(C F3 O3 S), 2(C2 H3 N)' _chemical_compound_source ? _chemical_formula_weight 1016.34 _cell_measurement_reflns_used 12480 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _cell_measurement_temperature 120 _exptl_crystal_description prism _exptl_crystal_colour 'translucent yellow' _exptl_crystal_size_min 0.17 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_max 0.38 _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 0.728 # Sheldrick geometric approximatio 0.83 0.88 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8336 _exptl_absorpt_correction_T_max 0.8836 _diffrn_measurement_device_type 'Oxford Diffraction XCALIBUR' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'Xcalibur, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis RED, (Oxford Diffraction, 2002)' _computing_cell_refinement 'CrysAlis RED, (Oxford Diffraction, 2002)' _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_number '4 frames' _diffrn_standards_interval_time 30 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 120 _diffrn_reflns_number 42552 _reflns_number_total 7222 _diffrn_reflns_av_R_equivalents 0.077 # Number of reflections with Friedels Law is 5195 # Number of reflections without Friedels Law is 7222 # Theoretical number of reflections is about 3992 _diffrn_reflns_theta_min 3.301 _diffrn_reflns_theta_max 32.375 _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 30.433 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 21 _reflns_limit_l_min 0 _reflns_limit_l_max 28 _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 -0.73 _refine_diff_density_max 0.57 _refine_ls_number_reflns 5195 _refine_ls_number_restraints 0 _refine_ls_number_parameters 304 #_refine_ls_R_factor_ref 0.0362 _refine_ls_wR_factor_ref 0.0363 _refine_ls_goodness_of_fit_ref 1.1160 #_reflns_number_all 7221 _refine_ls_R_factor_all 0.0506 _refine_ls_wR_factor_all 0.0387 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>2.00u(I) _reflns_number_gt 5195 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_gt 0.0363 _refine_ls_shift/su_max 0.001555 _refine_ls_abs_structure_Flack 0.015(9) _refine_ls_abs_structure_details 'Flack, 2027 Friedel-pairs' # 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 ad _refine_ls_structure_factor_coef F _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, 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: 17.9 -13.6 12.8 ; _refine_special_details ; All atoms, except hydrogens were refined anisotropically ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo G., Guagliardi A., Burla M.C., Polidori, G. & Camalli, M. (1994) SIR92 - a program for automatic solution of crystal structures by direct methods. J. Appl. Cryst. (27), 435-435 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Oxford Diffraction, (2002) CrysAlis RED. Oxford Diffraction, (2002) Xcalibur User Manual 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 atoms attached 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 _atom_site_attached_hydrogens Zn1 Zn -0.51494(4) 0.0000 -1.0000 0.0180 1.0000 Uani S T . . . . C2 C -0.1840(3) -0.01929(13) -1.12849(12) 0.0221 1.0000 Uani . . . . . . C3 C -0.0967(3) -0.04313(16) -1.18982(13) 0.0269 1.0000 Uani . . . . . . C4 C -0.0861(3) 0.01721(17) -1.24625(14) 0.0321 1.0000 Uani . . . . . . C5 C -0.1637(3) 0.10225(18) -1.24259(13) 0.0329 1.0000 Uani . . . . . . C6 C -0.2502(3) 0.12786(16) -1.18226(13) 0.0267 1.0000 Uani . . . . . . C7 C -0.2581(2) 0.06717(15) -1.12475(11) 0.0201 1.0000 Uani . . . . . . N8 N -0.3405(2) 0.08975(12) -1.06081(10) 0.0190 1.0000 Uani . . . . . . C9 C -0.3390(3) 0.17361(14) -1.03818(12) 0.0209 1.0000 Uani . . . . . . C10 C -0.4289(3) 0.19466(13) -0.97234(12) 0.0193 1.0000 Uani . . . . . . C11 C -0.4217(3) 0.27944(14) -0.93666(13) 0.0237 1.0000 Uani . . . . . . C12 C -0.5051(3) 0.28758(13) -0.87241(12) 0.0270 1.0000 Uani . . . . . . C13 C -0.5903(3) 0.21266(15) -0.84456(12) 0.0253 1.0000 Uani . . . . . . C14 C -0.5934(3) 0.13151(14) -0.88425(11) 0.0185 1.0000 Uani . . . . . . N15 N -0.5153(2) 0.12421(10) -0.94623(9) 0.0182 1.0000 Uani . . . . . . C16 C -0.6780(3) 0.04720(13) -0.86135(12) 0.0212 1.0000 Uani . . . . . . N17 N -0.6775(2) -0.02253(11) -0.90338(10) 0.0193 1.0000 Uani . . . . . . C18 C -0.7472(3) -0.10650(14) -0.87829(12) 0.0207 1.0000 Uani . . . . . . C19 C -0.7232(3) -0.13637(17) -0.80802(13) 0.0284 1.0000 Uani . . . . . . C20 C -0.7957(4) -0.21727(18) -0.78538(14) 0.0342 1.0000 Uani . . . . . . C21 C -0.8917(3) -0.26839(16) -0.83132(16) 0.0326 1.0000 Uani . . . . . . C22 C -0.9132(3) -0.23966(16) -0.90104(15) 0.0289 1.0000 Uani . . . . . . C23 C -0.8389(3) -0.15897(15) -0.92531(13) 0.0246 1.0000 Uani . . . . . . S24 S -0.29082(7) 0.43242(4) -1.13388(3) 0.0229 1.0000 Uani . . . . . . O25 O -0.2530(3) 0.38126(15) -1.19761(11) 0.0479 1.0000 Uani . . . . . . O26 O -0.2234(2) 0.39408(12) -1.06960(10) 0.0329 1.0000 Uani . . . . . . O27 O -0.2766(3) 0.53049(13) -1.14187(13) 0.0456 1.0000 Uani . . . . . . C28 C -0.5078(4) 0.4143(2) -1.1226(2) 0.0572 1.0000 Uani . . . . . . F29 F -0.5398(3) 0.32646(17) -1.11068(18) 0.0928 1.0000 Uani . . . . . . F30 F -0.5877(3) 0.4402(2) -1.18086(19) 0.1063 1.0000 Uani . . . . . . F31 F -0.5660(3) 0.4616(2) -1.0686(2) 0.1191 1.0000 Uani . . . . . . N32 N -1.0026(5) 0.2348(2) -0.90706(18) 0.0657 1.0000 Uani . . . . . . C33 C -0.9721(4) 0.3081(2) -0.92245(15) 0.0404 1.0000 Uani . . . . . . C34 C -0.9332(4) 0.4023(2) -0.94394(17) 0.0447 1.0000 Uani . . . . . . H35 H -0.0250 0.0006 -1.2873 0.0500 1.0000 Uiso . . . . . . H36 H -0.3608 0.3338 -0.9552 0.0500 1.0000 Uiso . . . . . . H37 H -0.1963 -0.0688 -1.0868 0.0500 1.0000 Uiso . . . . . . H38 H -0.4992 0.3431 -0.8462 0.0500 1.0000 Uiso . . . . . . H39 H -0.2775 0.2171 -1.0648 0.0500 1.0000 Uiso . . . . . . H40 H -0.9838 -0.2723 -0.9420 0.0500 1.0000 Uiso . . . . . . H41 H -0.7287 0.0477 -0.8130 0.0500 1.0000 Uiso . . . . . . H42 H -0.6475 -0.0958 -0.7765 0.0500 1.0000 Uiso . . . . . . H43 H -0.6417 0.2110 -0.7998 0.0500 1.0000 Uiso . . . . . . H44 H -0.0367 -0.1100 -1.1912 0.0500 1.0000 Uiso . . . . . . H45 H -0.3004 0.1854 -1.1800 0.0500 1.0000 Uiso . . . . . . H46 H -0.8708 -0.1421 -0.9702 0.0500 1.0000 Uiso . . . . . . H47 H -0.1425 0.1469 -1.2782 0.0500 1.0000 Uiso . . . . . . H48 H -0.9746 -0.3179 -0.8265 0.0500 1.0000 Uiso . . . . . . H49 H -0.8000 -0.2352 -0.7285 0.0500 1.0000 Uiso . . . . . . H50 H -0.9053 0.4409 -0.9011 0.0543 1.0000 Uiso . . . . . . H51 H -1.0285 0.4311 -0.9692 0.0543 1.0000 Uiso . . . . . . H52 H -0.8369 0.4025 -0.9774 0.0543 1.0000 Uiso . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02506(19) 0.01180(11) 0.01725(13) -0.00222(14) 0.0000 0.0000 C2 0.0247(10) 0.0185(9) 0.0232(9) -0.0020(7) 0.0041(8) -0.0012(7) C3 0.0268(11) 0.0254(11) 0.0286(12) -0.0056(9) 0.0043(9) 0.0020(8) C4 0.0304(11) 0.0354(14) 0.0304(11) -0.0013(9) 0.0098(9) 0.0021(10) C5 0.0436(15) 0.0320(12) 0.0231(11) 0.0051(9) 0.0095(10) 0.0028(10) C6 0.0350(12) 0.0217(10) 0.0235(11) 0.0022(8) 0.0044(9) 0.0034(8) C7 0.0227(9) 0.0184(8) 0.0192(9) -0.0030(8) 0.0011(7) -0.0029(7) N8 0.0215(8) 0.0183(8) 0.0171(8) -0.0006(6) 0.0025(6) -0.0003(6) C9 0.0237(10) 0.0157(8) 0.0234(10) -0.0001(7) 0.0034(8) -0.0023(7) C10 0.0227(10) 0.0135(8) 0.0218(9) 0.0006(7) -0.0011(8) -0.0004(7) C11 0.0323(11) 0.0133(8) 0.0254(10) -0.0014(7) 0.0016(9) -0.0032(8) C12 0.0381(12) 0.0163(8) 0.0265(9) -0.0074(7) 0.0012(11) -0.0019(9) C13 0.0349(12) 0.0190(9) 0.0220(10) -0.0046(8) 0.0048(9) -0.0026(8) C14 0.0212(9) 0.0166(8) 0.0176(9) -0.0013(7) 0.0022(7) -0.0010(7) N15 0.0218(8) 0.0154(6) 0.0173(7) -0.0003(5) 0.0005(7) -0.0013(6) C16 0.0250(10) 0.0180(9) 0.0206(9) -0.0003(7) 0.0043(8) -0.0020(7) N17 0.0206(8) 0.0141(7) 0.0231(8) 0.0002(6) 0.0020(7) -0.0023(5) C18 0.0202(9) 0.0169(9) 0.0250(10) 0.0003(8) 0.0040(7) -0.0024(7) C19 0.0335(13) 0.0261(10) 0.0256(11) 0.0034(9) 0.0009(10) -0.0042(9) C20 0.0384(14) 0.0318(12) 0.0323(13) 0.0093(10) 0.0045(11) -0.0045(11) C21 0.0317(12) 0.0229(11) 0.0432(15) 0.0051(10) 0.0087(11) -0.0052(9) C22 0.0231(11) 0.0222(10) 0.0414(14) -0.0043(9) 0.0022(10) -0.0049(8) C23 0.0267(11) 0.0209(10) 0.0262(11) -0.0039(8) 0.0012(9) -0.0027(8) S24 0.0252(3) 0.0196(2) 0.0239(2) 0.0016(2) -0.0006(2) 0.00295(19) O25 0.0671(15) 0.0474(12) 0.0291(10) -0.0104(9) -0.0010(10) 0.0124(11) O26 0.0343(10) 0.0342(9) 0.0302(9) 0.0060(7) -0.0086(7) 0.0000(7) O27 0.0541(12) 0.0223(8) 0.0604(14) 0.0110(9) 0.0040(11) -0.0005(8) C28 0.0270(13) 0.0545(17) 0.090(3) 0.0243(17) -0.0044(17) 0.0053(13) F29 0.0447(12) 0.0759(15) 0.158(3) 0.0591(17) -0.0349(14) -0.0322(11) F30 0.0498(14) 0.118(2) 0.151(3) 0.064(2) -0.0534(17) -0.0021(15) F31 0.0617(16) 0.139(3) 0.157(3) 0.002(2) 0.0639(19) 0.0295(16) N32 0.086(2) 0.0546(16) 0.0563(17) 0.0191(14) 0.004(2) -0.0071(19) C33 0.0423(15) 0.0498(15) 0.0289(12) 0.0013(11) -0.0017(11) 0.0005(13) C34 0.0588(19) 0.0394(14) 0.0359(15) -0.0017(12) -0.0041(13) -0.0016(13) _refine_ls_extinction_method None _oxford_refine_ls_scale 3.021(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 Zn1 . N17 2_553 2.2717(18) yes Zn1 . N8 2_553 2.2451(17) yes Zn1 . N15 2_553 2.0634(15) yes Zn1 . N8 . 2.2451(17) yes Zn1 . N15 . 2.0634(15) yes Zn1 . N17 . 2.2717(18) yes C2 . C3 . 1.397(3) yes C2 . C7 . 1.395(3) yes C2 . H37 . 1.064 no C3 . C4 . 1.375(4) yes C3 . H44 . 1.088 no C4 . C5 . 1.390(3) yes C4 . H35 . 0.949 no C5 . C6 . 1.385(3) yes C5 . H47 . 0.945 no C6 . C7 . 1.392(3) yes C6 . H45 . 0.932 no C7 . N8 . 1.413(3) yes N8 . C9 . 1.288(3) yes C9 . C10 . 1.469(3) yes C9 . H39 . 0.949 no C10 . C11 . 1.400(3) yes C10 . N15 . 1.336(3) yes C11 . C12 . 1.389(3) yes C11 . H36 . 0.995 no C12 . C13 . 1.393(3) yes C12 . H38 . 0.945 no C13 . C14 . 1.392(3) yes C13 . H43 . 0.938 no C14 . N15 . 1.330(3) yes C14 . C16 . 1.470(3) yes C16 . N17 . 1.281(3) yes C16 . H41 . 0.996 no N17 . C18 . 1.425(3) yes C18 . C19 . 1.399(3) yes C18 . C23 . 1.386(3) yes C19 . C20 . 1.382(3) yes C19 . H42 . 1.039 no C20 . C21 . 1.382(4) yes C20 . H49 . 1.097 no C21 . C22 . 1.382(4) yes C21 . H48 . 0.993 no C22 . C23 . 1.396(3) yes C22 . H40 . 1.071 no C23 . H46 . 0.913 no S24 . O25 . 1.439(2) yes S24 . O26 . 1.4367(18) yes S24 . O27 . 1.4348(19) yes S24 . C28 . 1.812(3) yes C28 . F29 . 1.320(4) yes C28 . F30 . 1.327(4) yes C28 . F31 . 1.311(5) yes N32 . C33 . 1.130(4) yes C33 . C34 . 1.460(4) yes C34 . H50 . 1.004 no C34 . H51 . 1.004 no C34 . H52 . 1.009 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 N17 2_553 Zn1 . N8 2_553 149.53(6) yes N17 2_553 Zn1 . N15 2_553 74.71(6) yes N8 2_553 Zn1 . N15 2_553 75.06(6) yes N17 2_553 Zn1 . N8 . 83.54(6) yes N8 2_553 Zn1 . N8 . 100.75(9) yes N15 2_553 Zn1 . N8 . 105.03(7) yes N17 2_553 Zn1 . N15 . 105.21(6) yes N8 2_553 Zn1 . N15 . 105.03(7) yes N15 2_553 Zn1 . N15 . 179.85(10) yes N8 . Zn1 . N15 . 75.06(6) yes N17 2_553 Zn1 . N17 . 108.04(9) yes N8 2_553 Zn1 . N17 . 83.54(6) yes N15 2_553 Zn1 . N17 . 105.21(6) yes N8 . Zn1 . N17 . 149.53(6) yes N15 . Zn1 . N17 . 74.71(6) yes C3 . C2 . C7 . 119.2(2) yes C3 . C2 . H37 . 118.938 no C7 . C2 . H37 . 121.855 no C2 . C3 . C4 . 120.4(2) yes C2 . C3 . H44 . 118.164 no C4 . C3 . H44 . 121.383 no C3 . C4 . C5 . 119.9(2) yes C3 . C4 . H35 . 119.677 no C5 . C4 . H35 . 120.464 no C4 . C5 . C6 . 120.9(2) yes C4 . C5 . H47 . 119.252 no C6 . C5 . H47 . 119.060 no C5 . C6 . C7 . 119.0(2) yes C5 . C6 . H45 . 120.272 no C7 . C6 . H45 . 120.682 no C2 . C7 . C6 . 120.59(19) yes C2 . C7 . N8 . 117.34(19) yes C6 . C7 . N8 . 122.07(19) yes Zn1 . N8 . C7 . 126.90(13) yes Zn1 . N8 . C9 . 112.73(14) yes C7 . N8 . C9 . 119.54(18) yes N8 . C9 . C10 . 117.89(18) yes N8 . C9 . H39 . 117.317 no C10 . C9 . H39 . 124.776 no C9 . C10 . C11 . 124.16(19) yes C9 . C10 . N15 . 114.50(17) yes C11 . C10 . N15 . 121.3(2) yes C10 . C11 . C12 . 117.8(2) yes C10 . C11 . H36 . 123.379 no C12 . C11 . H36 . 118.798 no C11 . C12 . C13 . 120.35(18) yes C11 . C12 . H38 . 119.834 no C13 . C12 . H38 . 119.730 no C12 . C13 . C14 . 117.9(2) yes C12 . C13 . H43 . 125.400 no C14 . C13 . H43 . 116.582 no C13 . C14 . N15 . 121.63(19) yes C13 . C14 . C16 . 123.77(19) yes N15 . C14 . C16 . 114.59(17) yes C10 . N15 . C14 . 120.94(17) yes C10 . N15 . Zn1 . 119.22(14) yes C14 . N15 . Zn1 . 119.72(13) yes C14 . C16 . N17 . 118.41(19) yes C14 . C16 . H41 . 117.149 no N17 . C16 . H41 . 124.407 no Zn1 . N17 . C16 . 112.17(13) yes Zn1 . N17 . C18 . 128.40(13) yes C16 . N17 . C18 . 118.08(18) yes N17 . C18 . C19 . 121.22(19) yes N17 . C18 . C23 . 118.52(19) yes C19 . C18 . C23 . 120.3(2) yes C18 . C19 . C20 . 119.4(2) yes C18 . C19 . H42 . 116.297 no C20 . C19 . H42 . 124.287 no C19 . C20 . C21 . 120.6(2) yes C19 . C20 . H49 . 120.865 no C21 . C20 . H49 . 117.303 no C20 . C21 . C22 . 119.9(2) yes C20 . C21 . H48 . 136.194 no C22 . C21 . H48 . 102.489 no C21 . C22 . C23 . 120.3(2) yes C21 . C22 . H40 . 127.766 no C23 . C22 . H40 . 111.935 no C22 . C23 . C18 . 119.4(2) yes C22 . C23 . H46 . 113.487 no C18 . C23 . H46 . 126.373 no O25 . S24 . O26 . 114.32(12) yes O25 . S24 . O27 . 114.01(14) yes O26 . S24 . O27 . 116.06(13) yes O25 . S24 . C28 . 103.56(17) yes O26 . S24 . C28 . 103.00(14) yes O27 . S24 . C28 . 103.63(14) yes S24 . C28 . F29 . 110.8(2) yes S24 . C28 . F30 . 110.4(3) yes F29 . C28 . F30 . 108.2(3) yes S24 . C28 . F31 . 111.9(3) yes F29 . C28 . F31 . 107.6(3) yes F30 . C28 . F31 . 107.8(3) yes N32 . C33 . C34 . 178.8(3) yes C33 . C34 . H50 . 110.523 no C33 . C34 . H51 . 110.386 no H50 . C34 . H51 . 108.833 no C33 . C34 . H52 . 110.169 no H50 . C34 . H52 . 108.427 no H51 . C34 . H52 . 108.445 no data_5 _database_code_depnum_ccdc_archive 'CCDC 695908' _montpellier_publication_code 32Zn2+ _montpellier_structure_analysis_code bar1 _montpellier_compound_description 'PDA-pF-Zn-Tf 2:1' _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; The maximum and minium densities relate to disorder in a triflate counterion which was not accounted for. No attempt was done to model the disorder since it appears to be less important than in 5Zn2+ (local code flo1). The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 10.09216(17) _cell_length_b 20.3191(4) _cell_length_c 22.3161(3) _cell_angle_alpha 114.4009(16) _cell_angle_beta 91.6422(13) _cell_angle_gamma 89.7369(12) _cell_volume 4165.62(13) _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' 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' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Zn 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097 1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C80 H51 F20 N12 O12 S4 Zn2 # Dc = 1.60 Fooo = 2030.00 Mu = 7.90 M = 2011.34 # Found Formula = C80 H51 F20 N12 O12 S4 Zn2 # Dc = 1.60 FOOO = 2030.00 Mu = 7.90 M = 2011.34 _chemical_formula_sum 'C80 H51 F20 N12 O12 S4 Zn2' _chemical_formula_moiety ; C38 H26 F4 N6 Zn, C38 H25 F4 N6 Zn, 4(C F3 O3 S) ; _chemical_compound_source ? _chemical_formula_weight 2011.34 _cell_measurement_reflns_used 58577 _cell_measurement_theta_min 3.8117 _cell_measurement_theta_max 34.6235 _cell_measurement_temperature 175 _exptl_crystal_description block _exptl_crystal_colour transparant _exptl_crystal_size_min 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_max 0.55 _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2030 _exptl_absorpt_coefficient_mu 0.790 _exptl_absorpt_correction_T_min 0.91005 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.0143 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_measurement_device 'Oxford Diffraction XCALIBUR' _diffrn_measurement_device_type Area _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _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_orient_matrix_UB_11 -0.0454013723 _diffrn_orient_matrix_UB_12 0.0150423011 _diffrn_orient_matrix_UB_13 -0.0156966556 _diffrn_orient_matrix_UB_21 0.0423328178 _diffrn_orient_matrix_UB_22 0.0304876954 _diffrn_orient_matrix_UB_23 0.0083613048 _diffrn_orient_matrix_UB_31 0.0330803893 _diffrn_orient_matrix_UB_32 -0.0177841765 _diffrn_orient_matrix_UB_33 -0.0300646466 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -0.27 50.73 1.0000 10.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 35.0000 80.0000 -90.0000 0.0000 0.0000 51 #__ type_ start__ end____ width___ exp.time_ 2 omega -38.00 70.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 35.0000 -80.0000 -120.0000 0.0000 0.0000 108 #__ type_ start__ end____ width___ exp.time_ 3 omega -24.65 10.35 1.0000 10.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -35.0000 -100.0000 -190.0000 0.0000 0.0000 35 #__ type_ start__ end____ width___ exp.time_ 4 phi -180.00 170.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames 20.0000 35.0000 50.0000 - 0.0000 0.0000 350 #__ type_ start__ end____ width___ exp.time_ 5 omega 6.00 106.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 35.0000 40.0000 90.0000 0.0000 0.0000 100 #__ type_ start__ end____ width___ exp.time_ 6 omega -10.93 24.07 1.0000 10.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 35.0000 100.0000 0.0000 0.0000 0.0000 35 #__ type_ start__ end____ width___ exp.time_ 7 omega -63.00 37.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -35.0000 40.0000 90.0000 0.0000 0.0000 100 #__ type_ start__ end____ width___ exp.time_ 8 omega -37.00 63.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 35.0000 -40.0000 90.0000 0.0000 0.0000 100 #__ type_ start__ end____ width___ exp.time_ 9 omega -36.00 63.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 35.0000 -40.0000 120.0000 0.0000 0.0000 99 #__ type_ start__ end____ width___ exp.time_ 10 omega -107.00 -6.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -35.0000 -40.0000 90.0000 0.0000 0.0000 101 #__ type_ start__ end____ width___ exp.time_ 11 omega -36.00 68.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 35.0000 -80.0000 0.0000 0.0000 0.0000 104 #__ type_ start__ end____ width___ exp.time_ 12 omega -36.00 68.00 1.0000 10.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 35.0000 -80.0000 120.0000 0.0000 0.0000 104 ; _diffrn_standards_interval_time ? _diffrn_standards_interval_count 'every 50 frames' _diffrn_standards_number '2 frames' _diffrn_standards_decay_% 0 _diffrn_ambient_temperature 173 _diffrn_reflns_number 124395 _reflns_number_total 31833 _diffrn_reflns_av_R_equivalents 0.023 # Number of reflections with Friedels Law is 31833 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 35783 _diffrn_reflns_theta_min 3.829 _diffrn_reflns_theta_max 34.729 _diffrn_measured_fraction_theta_max 0.886 _diffrn_reflns_theta_full 25.005 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _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 -32 _reflns_limit_k_max 29 _reflns_limit_l_min 0 _reflns_limit_l_max 35 _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 -1.21 _refine_diff_density_max 2.64 # 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 21186 _refine_ls_number_restraints 0 _refine_ls_number_parameters 1171 _oxford_refine_ls_R_factor_ref 0.0489 _refine_ls_wR_factor_ref 0.0485 _refine_ls_goodness_of_fit_ref 1.0902 _refine_ls_shift/su_max 0.001543 # The values computed from all data _oxford_reflns_number_all 31833 _refine_ls_R_factor_all 0.0792 _refine_ls_wR_factor_all 0.0583 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 21186 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_gt 0.0485 # 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: 10.4 -5.01 7.16 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Burla, M. C., Camalli, M. B., Carrozzini, G. L., Cascarano, R., Giacovazzo, C., Polidori, G. & Spagna, R., J. Appl. Crystallogr., 2003, 36, 1103. North, A.C.T., Phillips, D.C. & Mathews, F.S., (1968). Acta Cryst, A24, 351-359. Oxford Diffraction, (2002). CrysAlis RED. Oxford Diffraction, (2002). Xcalibur User Manual. 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 Zn1 Zn 0.71933(2) 0.243002(12) 0.246840(9) 0.0196 1.0000 Uani . . . . . . . N2 N 0.72398(15) 0.29113(8) 0.34674(7) 0.0188 1.0000 Uani . . . . . . . C3 C 0.81903(17) 0.33915(10) 0.37919(8) 0.0207 1.0000 Uani . . . . . . . C4 C 0.91998(18) 0.34844(10) 0.33686(9) 0.0220 1.0000 Uani . . . . . . . N5 N 0.90395(15) 0.31424(8) 0.27443(7) 0.0196 1.0000 Uani . . . . . . . C6 C 1.00592(18) 0.31641(10) 0.23264(9) 0.0210 1.0000 Uani . . . . . . . C7 C 0.97155(19) 0.32695(11) 0.17659(9) 0.0246 1.0000 Uani . . . . . . . C8 C 1.0684(2) 0.32944(13) 0.13471(10) 0.0319 1.0000 Uani . . . . . . . C9 C 1.1975(2) 0.31878(15) 0.14935(11) 0.0373 1.0000 Uani . . . . . . . F10 F 1.29332(15) 0.31998(12) 0.10839(8) 0.0586 1.0000 Uani . . . . . . . C11 C 1.2339(2) 0.30616(18) 0.20329(13) 0.0452 1.0000 Uani . . . . . . . C12 C 1.1372(2) 0.30584(15) 0.24628(11) 0.0354 1.0000 Uani . . . . . . . H13 H 1.1615 0.2985 0.2840 0.0447 1.0000 Uiso R . . . . . . H14 H 1.3227 0.2974 0.2111 0.0584 1.0000 Uiso R . . . . . . H15 H 1.0454 0.3380 0.0967 0.0393 1.0000 Uiso R . . . . . . H16 H 0.8805 0.3329 0.1676 0.0292 1.0000 Uiso R . . . . . . H17 H 0.9938 0.3794 0.3564 0.0251 1.0000 Uiso R . . . . . . C18 C 0.8221(2) 0.37454(12) 0.44751(9) 0.0279 1.0000 Uani . . . . . . . C19 C 0.7239(2) 0.35806(14) 0.48168(9) 0.0339 1.0000 Uani . . . . . . . C20 C 0.6264(2) 0.30753(13) 0.44770(9) 0.0303 1.0000 Uani . . . . . . . C21 C 0.62999(18) 0.27467(10) 0.37930(8) 0.0217 1.0000 Uani . . . . . . . C22 C 0.53299(18) 0.22019(10) 0.33744(9) 0.0219 1.0000 Uani . . . . . . . N23 N 0.54101(15) 0.19634(8) 0.27464(7) 0.0204 1.0000 Uani . . . . . . . C24 C 0.44347(18) 0.14697(10) 0.23327(9) 0.0230 1.0000 Uani . . . . . . . C25 C 0.3137(2) 0.14717(13) 0.25293(11) 0.0368 1.0000 Uani . . . . . . . C26 C 0.2233(2) 0.09701(16) 0.21112(13) 0.0510 1.0000 Uani . . . . . . . C27 C 0.2634(2) 0.04849(15) 0.15058(12) 0.0437 1.0000 Uani . . . . . . . F28 F 0.17261(17) 0.00066(11) 0.11024(9) 0.0710 1.0000 Uani . . . . . . . C29 C 0.3899(2) 0.04686(14) 0.12944(11) 0.0397 1.0000 Uani . . . . . . . C30 C 0.4805(2) 0.09716(12) 0.17175(10) 0.0319 1.0000 Uani . . . . . . . H31 H 0.5673 0.0977 0.1582 0.0343 1.0000 Uiso R . . . . . . H32 H 0.4150 0.0136 0.0883 0.0407 1.0000 Uiso R . . . . . . H33 H 0.1364 0.0965 0.2242 0.0485 1.0000 Uiso R . . . . . . H34 H 0.2860 0.1810 0.2942 0.0366 1.0000 Uiso R . . . . . . H35 H 0.4673 0.2028 0.3559 0.0269 1.0000 Uiso R . . . . . . H36 H 0.5604 0.2956 0.4700 0.0355 1.0000 Uiso R . . . . . . H37 H 0.7227 0.3813 0.5276 0.0374 1.0000 Uiso R . . . . . . H38 H 0.8893 0.4081 0.4704 0.0295 1.0000 Uiso R . . . . . . N39 N 0.60884(15) 0.32314(8) 0.22008(7) 0.0209 1.0000 Uani . . . . . . . C40 C 0.57107(18) 0.39369(10) 0.26423(9) 0.0222 1.0000 Uani . . . . . . . C41 C 0.4935(2) 0.40168(12) 0.31722(10) 0.0306 1.0000 Uani . . . . . . . C42 C 0.4575(3) 0.47030(13) 0.36155(11) 0.0382 1.0000 Uani . . . . . . . C43 C 0.5042(3) 0.52895(12) 0.35280(11) 0.0373 1.0000 Uani . . . . . . . F44 F 0.4709(2) 0.59629(9) 0.39611(8) 0.0567 1.0000 Uani . . . . . . . C45 C 0.5861(3) 0.52280(12) 0.30256(12) 0.0380 1.0000 Uani . . . . . . . C46 C 0.6176(2) 0.45419(12) 0.25692(11) 0.0310 1.0000 Uani . . . . . . . H47 H 0.6703 0.4491 0.2216 0.0383 1.0000 Uiso R . . . . . . H48 H 0.6200 0.5644 0.2997 0.0468 1.0000 Uiso R . . . . . . H49 H 0.4021 0.4767 0.3970 0.0452 1.0000 Uiso R . . . . . . H50 H 0.4652 0.3607 0.3228 0.0376 1.0000 Uiso R . . . . . . C51 C 0.60495(18) 0.30566(11) 0.15784(9) 0.0231 1.0000 Uani . . . . . . . C52 C 0.66170(18) 0.23599(10) 0.11472(8) 0.0216 1.0000 Uani . . . . . . . N53 N 0.72280(15) 0.20115(8) 0.14668(7) 0.0193 1.0000 Uani . . . . . . . C54 C 0.78418(18) 0.13851(10) 0.11398(8) 0.0221 1.0000 Uani . . . . . . . C55 C 0.84663(18) 0.10725(10) 0.15680(9) 0.0229 1.0000 Uani . . . . . . . N56 N 0.83677(15) 0.14124(8) 0.21923(7) 0.0205 1.0000 Uani . . . . . . . C57 C 0.88731(18) 0.11028(10) 0.26176(9) 0.0221 1.0000 Uani . . . . . . . C58 C 0.8798(3) 0.03649(12) 0.24458(11) 0.0381 1.0000 Uani . . . . . . . C59 C 0.9289(4) 0.00901(13) 0.28783(14) 0.0526 1.0000 Uani . . . . . . . C60 C 0.9843(3) 0.05502(13) 0.34718(12) 0.0421 1.0000 Uani . . . . . . . F61 F 1.0310(2) 0.02672(9) 0.38899(9) 0.0665 1.0000 Uani . . . . . . . C62 C 0.9928(3) 0.12819(12) 0.36600(11) 0.0350 1.0000 Uani . . . . . . . C63 C 0.9430(2) 0.15597(10) 0.32264(10) 0.0274 1.0000 Uani . . . . . . . H64 H 0.9483 0.2067 0.3350 0.0311 1.0000 Uiso R . . . . . . H65 H 1.0306 0.1589 0.4067 0.0402 1.0000 Uiso R . . . . . . H66 H 0.9251 -0.0408 0.2765 0.0611 1.0000 Uiso R . . . . . . H67 H 0.8419 0.0045 0.2034 0.0447 1.0000 Uiso R . . . . . . H68 H 0.8926 0.0632 0.1381 0.0263 1.0000 Uiso R . . . . . . C69 C 0.7844(2) 0.10709(11) 0.04562(9) 0.0280 1.0000 Uani . . . . . . . C70 C 0.7191(2) 0.14261(12) 0.01190(9) 0.0327 1.0000 Uani . . . . . . . C71 C 0.6577(2) 0.20835(11) 0.04621(9) 0.0285 1.0000 Uani . . . . . . . H72 H 0.7162 0.1228 -0.0338 0.0362 1.0000 Uiso R . . . . . . H73 H 0.8271 0.0629 0.0233 0.0316 1.0000 Uiso R . . . . . . H74 H 0.5671 0.3362 0.1405 0.0282 1.0000 Uiso R . . . . . . Zn75 Zn 0.75013(2) 0.744534(12) 0.253738(10) 0.0211 1.0000 Uani . . . . . . . N76 N 0.58209(16) 0.70242(9) 0.28927(8) 0.0224 1.0000 Uani . . . . . . . C77 C 0.57679(19) 0.73100(11) 0.35219(9) 0.0246 1.0000 Uani . . . . . . . C78 C 0.67496(19) 0.78725(11) 0.38986(9) 0.0239 1.0000 Uani . . . . . . . N79 N 0.76450(16) 0.80016(8) 0.35340(7) 0.0212 1.0000 Uani . . . . . . . C80 C 0.86208(19) 0.84813(10) 0.38168(9) 0.0238 1.0000 Uani . . . . . . . C81 C 0.96027(19) 0.85141(10) 0.33544(9) 0.0251 1.0000 Uani . . . . . . . N82 N 0.93732(16) 0.81459(9) 0.27375(8) 0.0227 1.0000 Uani . . . . . . . C83 C 1.03773(19) 0.80893(11) 0.22851(9) 0.0247 1.0000 Uani . . . . . . . C84 C 1.1649(2) 0.78768(14) 0.23801(11) 0.0333 1.0000 Uani . . . . . . . C85 C 1.2602(2) 0.77866(17) 0.19152(12) 0.0415 1.0000 Uani . . . . . . . C86 C 1.2268(2) 0.79225(17) 0.13785(12) 0.0408 1.0000 Uani . . . . . . . F87 F 1.32170(16) 0.78529(13) 0.09402(8) 0.0615 1.0000 Uani . . . . . . . C88 C 1.1015(2) 0.81285(17) 0.12708(12) 0.0419 1.0000 Uani . . . . . . . C89 C 1.0052(2) 0.82051(14) 0.17254(11) 0.0332 1.0000 Uani . . . . . . . H90 H 0.9190 0.8337 0.1657 0.0423 1.0000 Uiso R . . . . . . H91 H 1.0823 0.8226 0.0904 0.0549 1.0000 Uiso R . . . . . . H92 H 1.3457 0.7629 0.1970 0.0512 1.0000 Uiso R . . . . . . H93 H 1.1865 0.7796 0.2751 0.0419 1.0000 Uiso R . . . . . . H94 H 1.0378 0.8796 0.3515 0.0293 1.0000 Uiso R . . . . . . C95 C 0.8712(2) 0.88711(13) 0.44947(10) 0.0337 1.0000 Uani . . . . . . . C96 C 0.7768(2) 0.87499(15) 0.48757(10) 0.0391 1.0000 Uani . . . . . . . C97 C 0.6776(2) 0.82373(13) 0.45818(10) 0.0328 1.0000 Uani . . . . . . . H98 H 0.6141 0.8133 0.4828 0.0387 1.0000 Uiso R . . . . . . H99 H 0.7796 0.9013 0.5335 0.0423 1.0000 Uiso R . . . . . . H100 H 0.9391 0.9214 0.4685 0.0357 1.0000 Uiso R . . . . . . H101 H 0.5110 0.7177 0.3735 0.0307 1.0000 Uiso R . . . . . . C102 C 0.48524(19) 0.65044(11) 0.25112(10) 0.0250 1.0000 Uani . . . . . . . C103 C 0.3585(2) 0.64860(14) 0.27377(12) 0.0372 1.0000 Uani . . . . . . . C104 C 0.2708(2) 0.59463(17) 0.23553(15) 0.0510 1.0000 Uani . . . . . . . C105 C 0.3095(2) 0.54427(16) 0.17582(13) 0.0452 1.0000 Uani . . . . . . . F106 F 0.22182(19) 0.49262(13) 0.13896(10) 0.0747 1.0000 Uani . . . . . . . C107 C 0.4334(2) 0.54458(15) 0.15183(12) 0.0401 1.0000 Uani . . . . . . . C108 C 0.5211(2) 0.59872(13) 0.19007(10) 0.0318 1.0000 Uani . . . . . . . H109 H 0.6066 0.6002 0.1744 0.0359 1.0000 Uiso R . . . . . . H110 H 0.4566 0.5089 0.1106 0.0440 1.0000 Uiso R . . . . . . H111 H 0.1849 0.5916 0.2497 0.0535 1.0000 Uiso R . . . . . . H112 H 0.3337 0.6828 0.3140 0.0416 1.0000 Uiso R . . . . . . N113 N 0.76537(16) 0.69839(8) 0.15395(7) 0.0205 1.0000 Uani . . . . . . . C114 C 0.70402(19) 0.72873(10) 0.11809(8) 0.0222 1.0000 Uani . . . . . . . C115 C 0.62456(18) 0.79277(10) 0.15655(9) 0.0231 1.0000 Uani . . . . . . . N116 N 0.62409(16) 0.81461(9) 0.21922(8) 0.0223 1.0000 Uani . . . . . . . C117 C 0.5576(2) 0.87992(11) 0.25724(10) 0.0255 1.0000 Uani . . . . . . . C118 C 0.4883(3) 0.88478(13) 0.31177(11) 0.0362 1.0000 Uani . . . . . . . C119 C 0.4222(3) 0.94765(15) 0.34947(12) 0.0463 1.0000 Uani . . . . . . . C120 C 0.4297(4) 1.00447(16) 0.33257(15) 0.0574 1.0000 Uani . . . . . . . F121 F 0.3669(3) 1.06647(12) 0.36962(11) 0.0962 1.0000 Uani . . . . . . . C122 C 0.4996(5) 1.00205(17) 0.28032(18) 0.0777 1.0000 Uani . . . . . . . C123 C 0.5637(3) 0.93916(14) 0.24210(14) 0.0519 1.0000 Uani . . . . . . . H124 H 0.6122 0.9366 0.2056 0.0650 1.0000 Uiso R . . . . . . H125 H 0.5068 1.0423 0.2706 0.0948 1.0000 Uiso R . . . . . . H126 H 0.3741 0.9506 0.3856 0.0552 1.0000 Uiso R . . . . . . H127 H 0.4864 0.8455 0.3229 0.0431 1.0000 Uiso R . . . . . . H128 H 0.5745 0.8172 0.1352 0.0283 1.0000 Uiso R . . . . . . C129 C 0.7192(2) 0.70251(11) 0.05062(9) 0.0292 1.0000 Uani . . . . . . . C130 C 0.8032(3) 0.64412(12) 0.02110(10) 0.0350 1.0000 Uani . . . . . . . C131 C 0.8685(2) 0.61348(11) 0.05883(10) 0.0308 1.0000 Uani . . . . . . . C132 C 0.84611(19) 0.64232(10) 0.12595(9) 0.0235 1.0000 Uani . . . . . . . C133 C 0.90602(19) 0.61419(10) 0.17113(9) 0.0230 1.0000 Uani . . . . . . . N134 N 0.88089(15) 0.64591(8) 0.23259(7) 0.0210 1.0000 Uani . . . . . . . C135 C 0.92995(17) 0.61567(10) 0.27594(9) 0.0215 1.0000 Uani . . . . . . . C136 C 0.9721(2) 0.66189(11) 0.33934(10) 0.0298 1.0000 Uani . . . . . . . C137 C 1.0228(3) 0.63415(12) 0.38253(11) 0.0355 1.0000 Uani . . . . . . . C138 C 1.0291(3) 0.56085(12) 0.36109(11) 0.0346 1.0000 Uani . . . . . . . F139 F 1.0783(2) 0.53252(9) 0.40260(8) 0.0558 1.0000 Uani . . . . . . . C140 C 0.9879(3) 0.51367(12) 0.29900(11) 0.0385 1.0000 Uani . . . . . . . C141 C 0.9367(2) 0.54128(11) 0.25595(10) 0.0296 1.0000 Uani . . . . . . . H142 H 0.9061 0.5098 0.2137 0.0361 1.0000 Uiso R . . . . . . H143 H 0.9937 0.4637 0.2860 0.0467 1.0000 Uiso R . . . . . . H144 H 1.0518 0.6655 0.4254 0.0407 1.0000 Uiso R . . . . . . H145 H 0.9680 0.7115 0.3527 0.0342 1.0000 Uiso R . . . . . . H146 H 0.9622 0.5743 0.1547 0.0286 1.0000 Uiso R . . . . . . H147 H 0.9258 0.5747 0.0400 0.0366 1.0000 Uiso R . . . . . . H148 H 0.8156 0.6259 -0.0241 0.0413 1.0000 Uiso R . . . . . . H149 H 0.6755 0.7232 0.0262 0.0340 1.0000 Uiso R . . . . . . S150 S 0.23541(5) 0.31340(3) 0.43591(3) 0.0302 1.0000 Uani . . . . . . . O151 O 0.2943(2) 0.31413(12) 0.37802(9) 0.0521 1.0000 Uani . . . . . . . O152 O 0.3102(2) 0.27467(13) 0.46549(13) 0.0560 1.0000 Uani . . . . . . . O153 O 0.09506(19) 0.30236(12) 0.43090(14) 0.0608 1.0000 Uani . . . . . . . C154 C 0.2526(3) 0.40809(15) 0.49315(13) 0.0445 1.0000 Uani . . . . . . . F155 F 0.3778(2) 0.43029(11) 0.49744(10) 0.0655 1.0000 Uani . . . . . . . F156 F 0.2177(3) 0.41986(15) 0.55296(10) 0.0913 1.0000 Uani . . . . . . . F157 F 0.1787(3) 0.44899(10) 0.47194(13) 0.0862 1.0000 Uani . . . . . . . S158 S 0.70544(6) 0.90318(3) 0.05887(3) 0.0329 1.0000 Uani . . . . . . . O159 O 0.6042(2) 0.84986(12) 0.03130(13) 0.0585 1.0000 Uani . . . . . . . O160 O 0.7726(2) 0.89909(13) 0.11522(9) 0.0573 1.0000 Uani . . . . . . . O161 O 0.6747(2) 0.97439(12) 0.06581(15) 0.0708 1.0000 Uani . . . . . . . C162 C 0.8355(4) 0.87599(18) -0.00075(15) 0.0558 1.0000 Uani . . . . . . . F163 F 0.8893(2) 0.81401(12) -0.00655(11) 0.0798 1.0000 Uani . . . . . . . F164 F 0.9322(3) 0.92588(16) 0.01904(17) 0.1133 1.0000 Uani . . . . . . . F165 F 0.7945(4) 0.8678(2) -0.05920(12) 0.1220 1.0000 Uani . . . . . . . S166 S 0.79688(6) 0.41985(4) 0.06593(3) 0.0389 1.0000 Uani . . . . . . . O167 O 0.92136(19) 0.44635(11) 0.05744(10) 0.0487 1.0000 Uani . . . . . . . O168 O 0.7305(3) 0.4718(2) 0.12142(12) 0.1068 1.0000 Uani . . . . . . . O169 O 0.7940(4) 0.34867(19) 0.0604(2) 0.1284 1.0000 Uani . . . . . . . C170 C 0.6930(4) 0.41648(17) -0.00262(14) 0.0542 1.0000 Uani . . . . . . . F171 F 0.6684(3) 0.48223(14) 0.00225(15) 0.1084 1.0000 Uani . . . . . . . F172 F 0.5776(3) 0.38708(17) -0.00405(15) 0.1049 1.0000 Uani . . . . . . . F173 F 0.7456(3) 0.37984(17) -0.05909(10) 0.1078 1.0000 Uani . . . . . . . S174 S 0.25187(8) 0.81607(4) 0.44977(3) 0.0465 1.0000 Uani . . . . . . . O175 O 0.3464(3) 0.76720(16) 0.45634(15) 0.0736 1.0000 Uani . . . . . . . O176 O 0.2693(6) 0.8253(2) 0.39167(16) 0.1364 1.0000 Uani . . . . . . . O177 O 0.1224(3) 0.80530(15) 0.46551(19) 0.0928 1.0000 Uani . . . . . . . C178 C 0.3006(4) 0.9010(2) 0.5140(2) 0.0844 1.0000 Uani . . . . . . . F179 F 0.4175(2) 0.92473(15) 0.50640(15) 0.0958 1.0000 Uani . . . . . . . F180 F 0.2971(5) 0.9038(3) 0.57118(14) 0.1939 1.0000 Uani . . . . . . . F181 F 0.2158(4) 0.95161(16) 0.5112(4) 0.2177 1.0000 Uani . . . . . . . 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 Zn1 0.02390(10) 0.01976(10) 0.01305(8) 0.00464(7) 0.00114(7) -0.00014(7) N2 0.0200(6) 0.0211(7) 0.0148(6) 0.0068(5) 0.0013(5) 0.0003(5) C3 0.0213(7) 0.0217(8) 0.0161(7) 0.0049(6) 0.0005(6) 0.0012(6) C4 0.0238(8) 0.0203(8) 0.0196(7) 0.0059(6) 0.0005(6) -0.0022(6) N5 0.0211(6) 0.0193(6) 0.0171(6) 0.0064(5) 0.0009(5) -0.0007(5) C6 0.0211(7) 0.0237(8) 0.0192(7) 0.0098(6) 0.0002(6) -0.0027(6) C7 0.0218(8) 0.0318(9) 0.0222(8) 0.0129(7) 0.0001(6) -0.0011(7) C8 0.0291(9) 0.0460(12) 0.0268(9) 0.0210(9) 0.0021(7) -0.0028(8) C9 0.0265(10) 0.0594(15) 0.0297(10) 0.0218(10) 0.0054(8) -0.0049(9) F10 0.0315(7) 0.1107(16) 0.0452(9) 0.0431(10) 0.0123(6) -0.0043(8) C11 0.0204(9) 0.086(2) 0.0388(12) 0.0355(13) 0.0025(8) 0.0020(11) C12 0.0221(9) 0.0625(15) 0.0298(10) 0.0272(10) 0.0001(7) 0.0006(9) C18 0.0252(8) 0.0331(10) 0.0168(7) 0.0019(7) -0.0005(6) 0.0005(7) C19 0.0289(9) 0.0517(13) 0.0137(7) 0.0062(8) 0.0015(6) 0.0026(9) C20 0.0249(9) 0.0488(12) 0.0172(7) 0.0135(8) 0.0037(6) 0.0015(8) C21 0.0214(7) 0.0272(8) 0.0173(7) 0.0099(6) 0.0010(6) 0.0013(6) C22 0.0201(7) 0.0257(8) 0.0223(7) 0.0124(6) 0.0025(6) -0.0002(6) N23 0.0202(6) 0.0205(7) 0.0202(6) 0.0081(5) 0.0012(5) -0.0009(5) C24 0.0210(8) 0.0208(8) 0.0247(8) 0.0067(6) 0.0018(6) -0.0003(6) C25 0.0218(9) 0.0373(11) 0.0330(10) -0.0043(9) 0.0050(7) 0.0009(8) C26 0.0220(10) 0.0562(16) 0.0431(13) -0.0117(11) 0.0067(9) -0.0070(10) C27 0.0279(10) 0.0441(13) 0.0365(11) -0.0063(10) 0.0023(8) -0.0110(9) F28 0.0378(8) 0.0738(12) 0.0530(10) -0.0231(9) 0.0064(7) -0.0261(8) C29 0.0328(11) 0.0389(12) 0.0293(10) -0.0046(9) 0.0071(8) -0.0087(9) C30 0.0274(9) 0.0339(10) 0.0260(9) 0.0034(8) 0.0064(7) -0.0063(8) N39 0.0208(7) 0.0226(7) 0.0188(6) 0.0081(5) 0.0012(5) -0.0006(5) C40 0.0247(8) 0.0236(8) 0.0187(7) 0.0090(6) 0.0022(6) 0.0039(6) C41 0.0388(11) 0.0301(10) 0.0254(9) 0.0134(8) 0.0102(8) 0.0027(8) C42 0.0518(14) 0.0359(11) 0.0276(10) 0.0128(9) 0.0180(9) 0.0113(10) C43 0.0558(14) 0.0270(10) 0.0290(10) 0.0111(8) 0.0123(9) 0.0159(9) F44 0.0948(14) 0.0315(7) 0.0422(8) 0.0120(6) 0.0301(9) 0.0245(8) C45 0.0566(14) 0.0243(10) 0.0366(11) 0.0152(9) 0.0154(10) 0.0093(9) C46 0.0393(11) 0.0267(9) 0.0306(9) 0.0149(8) 0.0128(8) 0.0068(8) C51 0.0215(8) 0.0279(9) 0.0213(7) 0.0116(7) -0.0009(6) 0.0003(6) C52 0.0222(8) 0.0252(8) 0.0172(7) 0.0087(6) -0.0017(6) -0.0043(6) N53 0.0201(6) 0.0208(7) 0.0152(6) 0.0055(5) 0.0005(5) -0.0009(5) C54 0.0236(8) 0.0233(8) 0.0167(7) 0.0054(6) 0.0044(6) -0.0019(6) C55 0.0242(8) 0.0213(8) 0.0208(7) 0.0062(6) 0.0045(6) 0.0022(6) N56 0.0196(6) 0.0201(7) 0.0203(6) 0.0070(5) 0.0003(5) -0.0007(5) C57 0.0228(8) 0.0195(8) 0.0223(7) 0.0070(6) -0.0009(6) -0.0003(6) C58 0.0599(15) 0.0221(9) 0.0312(10) 0.0108(8) -0.0156(10) -0.0092(9) C59 0.092(2) 0.0232(10) 0.0422(13) 0.0152(10) -0.0269(14) -0.0105(12) C60 0.0646(16) 0.0285(11) 0.0358(11) 0.0168(9) -0.0162(11) -0.0014(10) F61 0.1149(17) 0.0397(9) 0.0505(10) 0.0267(8) -0.0369(10) -0.0043(10) C62 0.0475(13) 0.0264(10) 0.0283(9) 0.0092(8) -0.0129(9) -0.0019(9) C63 0.0348(10) 0.0188(8) 0.0246(8) 0.0055(6) -0.0048(7) -0.0002(7) C69 0.0369(10) 0.0250(9) 0.0174(7) 0.0037(6) 0.0067(7) -0.0020(7) C70 0.0482(12) 0.0324(10) 0.0141(7) 0.0061(7) 0.0026(7) -0.0055(9) C71 0.0371(10) 0.0304(10) 0.0169(7) 0.0088(7) -0.0025(7) -0.0065(8) Zn75 0.02433(10) 0.02319(10) 0.01467(8) 0.00659(7) 0.00310(7) 0.00175(8) N76 0.0230(7) 0.0234(7) 0.0227(7) 0.0111(6) 0.0039(5) 0.0023(5) C77 0.0262(8) 0.0288(9) 0.0226(8) 0.0143(7) 0.0059(6) 0.0022(7) C78 0.0270(8) 0.0279(9) 0.0187(7) 0.0114(7) 0.0044(6) 0.0047(7) N79 0.0255(7) 0.0207(7) 0.0165(6) 0.0065(5) 0.0035(5) 0.0029(5) C80 0.0264(8) 0.0215(8) 0.0207(7) 0.0058(6) 0.0015(6) 0.0036(6) C81 0.0264(9) 0.0215(8) 0.0255(8) 0.0077(7) 0.0014(7) -0.0018(6) N82 0.0232(7) 0.0235(7) 0.0215(7) 0.0094(6) 0.0016(5) -0.0004(5) C83 0.0233(8) 0.0289(9) 0.0230(8) 0.0118(7) 0.0010(6) -0.0029(7) C84 0.0255(9) 0.0531(13) 0.0271(9) 0.0223(9) 0.0012(7) 0.0008(9) C85 0.0241(10) 0.0713(18) 0.0346(11) 0.0271(12) 0.0037(8) 0.0031(10) C86 0.0290(10) 0.0674(17) 0.0301(10) 0.0241(11) 0.0037(8) -0.0085(10) F87 0.0375(8) 0.1155(17) 0.0404(8) 0.0404(10) 0.0112(6) -0.0085(9) C88 0.0345(11) 0.0696(18) 0.0328(11) 0.0325(12) -0.0021(9) -0.0099(11) C89 0.0264(9) 0.0497(13) 0.0318(10) 0.0254(10) -0.0022(7) -0.0041(9) C95 0.0338(10) 0.0346(11) 0.0213(8) 0.0003(7) -0.0011(7) 0.0011(8) C96 0.0419(12) 0.0491(14) 0.0162(8) 0.0034(8) 0.0010(8) 0.0031(10) C97 0.0353(10) 0.0446(12) 0.0185(8) 0.0130(8) 0.0056(7) 0.0052(9) C102 0.0218(8) 0.0274(9) 0.0268(8) 0.0120(7) 0.0014(6) -0.0004(7) C103 0.0222(9) 0.0415(12) 0.0388(11) 0.0071(9) 0.0075(8) 0.0013(8) C104 0.0236(10) 0.0593(17) 0.0538(15) 0.0067(13) 0.0067(10) -0.0079(10) C105 0.0311(11) 0.0528(15) 0.0406(12) 0.0084(11) -0.0029(9) -0.0133(10) F106 0.0453(10) 0.0859(15) 0.0601(11) -0.0030(10) -0.0034(8) -0.0343(10) C107 0.0347(11) 0.0464(13) 0.0284(10) 0.0045(9) 0.0008(8) -0.0080(10) C108 0.0259(9) 0.0403(11) 0.0248(9) 0.0089(8) 0.0036(7) -0.0047(8) N113 0.0259(7) 0.0201(7) 0.0161(6) 0.0077(5) 0.0039(5) 0.0013(5) C114 0.0290(8) 0.0209(8) 0.0171(7) 0.0082(6) 0.0001(6) -0.0031(6) C115 0.0236(8) 0.0251(8) 0.0224(7) 0.0118(7) -0.0010(6) 0.0005(6) N116 0.0230(7) 0.0221(7) 0.0227(7) 0.0100(6) 0.0024(5) 0.0024(5) C117 0.0277(9) 0.0237(8) 0.0258(8) 0.0107(7) 0.0036(7) 0.0058(7) C118 0.0528(14) 0.0318(11) 0.0275(9) 0.0151(8) 0.0128(9) 0.0140(9) C119 0.0679(17) 0.0428(14) 0.0322(11) 0.0183(10) 0.0240(11) 0.0248(12) C120 0.094(2) 0.0387(14) 0.0446(14) 0.0203(12) 0.0344(15) 0.0376(15) F121 0.170(3) 0.0625(13) 0.0710(13) 0.0388(11) 0.0750(16) 0.0776(15) C122 0.144(4) 0.0369(15) 0.068(2) 0.0342(15) 0.063(2) 0.0445(19) C123 0.084(2) 0.0306(12) 0.0488(14) 0.0224(11) 0.0385(14) 0.0218(12) C129 0.0431(11) 0.0286(9) 0.0171(7) 0.0105(7) 0.0008(7) -0.0004(8) C130 0.0581(14) 0.0294(10) 0.0172(8) 0.0089(7) 0.0098(8) 0.0026(9) C131 0.0448(11) 0.0258(9) 0.0215(8) 0.0087(7) 0.0133(8) 0.0066(8) C132 0.0293(9) 0.0225(8) 0.0196(7) 0.0094(6) 0.0061(6) 0.0017(6) C133 0.0247(8) 0.0218(8) 0.0235(8) 0.0101(6) 0.0065(6) 0.0048(6) N134 0.0213(7) 0.0215(7) 0.0210(6) 0.0096(5) 0.0023(5) 0.0017(5) C135 0.0205(7) 0.0231(8) 0.0224(7) 0.0110(6) 0.0015(6) 0.0006(6) C136 0.0409(11) 0.0217(8) 0.0235(8) 0.0062(7) -0.0035(8) 0.0046(8) C137 0.0501(13) 0.0277(10) 0.0248(9) 0.0076(8) -0.0101(9) 0.0020(9) C138 0.0503(13) 0.0289(10) 0.0274(9) 0.0152(8) -0.0111(9) -0.0018(9) F139 0.0962(14) 0.0368(8) 0.0379(8) 0.0206(7) -0.0262(8) 0.0011(8) C140 0.0616(15) 0.0230(9) 0.0326(10) 0.0142(8) -0.0151(10) -0.0074(9) C141 0.0399(11) 0.0237(9) 0.0261(9) 0.0119(7) -0.0089(8) -0.0086(8) S150 0.0283(2) 0.0255(2) 0.0349(2) 0.01093(19) -0.00289(19) 0.00205(18) O151 0.0727(14) 0.0509(12) 0.0285(8) 0.0120(8) 0.0039(8) 0.0095(10) O152 0.0409(10) 0.0646(14) 0.0909(17) 0.0607(13) 0.0024(10) 0.0063(9) O153 0.0297(9) 0.0447(11) 0.0980(18) 0.0201(12) -0.0112(10) -0.0044(8) C154 0.0491(14) 0.0383(13) 0.0340(11) 0.0027(10) -0.0006(10) -0.0045(11) F155 0.0648(12) 0.0621(12) 0.0584(11) 0.0139(9) -0.0104(9) -0.0326(10) F156 0.0971(17) 0.1087(19) 0.0352(9) -0.0051(11) 0.0248(10) -0.0198(14) F157 0.1035(18) 0.0307(9) 0.1077(19) 0.0135(10) -0.0211(14) 0.0167(10) S158 0.0306(2) 0.0278(2) 0.0378(3) 0.0108(2) 0.0054(2) -0.00206(19) O159 0.0433(11) 0.0540(12) 0.0838(16) 0.0356(12) -0.0257(10) -0.0196(9) O160 0.0590(13) 0.0714(15) 0.0293(9) 0.0089(9) -0.0050(8) -0.0094(11) O161 0.0607(14) 0.0365(11) 0.119(2) 0.0336(13) 0.0390(14) 0.0152(10) C162 0.068(2) 0.0523(17) 0.0448(15) 0.0164(13) 0.0258(14) 0.0155(14) F163 0.0875(15) 0.0658(13) 0.0702(14) 0.0113(11) 0.0226(11) 0.0402(12) F164 0.0720(15) 0.0954(19) 0.159(3) 0.0344(19) 0.0692(17) -0.0091(14) F165 0.186(3) 0.146(3) 0.0521(13) 0.0579(17) 0.0414(17) 0.062(2) S166 0.0364(3) 0.0550(4) 0.0334(3) 0.0269(3) -0.0075(2) -0.0124(3) O167 0.0377(9) 0.0501(11) 0.0532(11) 0.0156(9) 0.0119(8) -0.0021(8) O168 0.0464(13) 0.206(4) 0.0351(11) 0.0166(17) 0.0093(10) -0.0049(18) O169 0.139(3) 0.096(2) 0.198(4) 0.116(3) -0.122(3) -0.074(2) C170 0.070(2) 0.0501(16) 0.0388(13) 0.0161(12) -0.0200(13) -0.0029(14) F171 0.141(2) 0.0663(15) 0.122(2) 0.0466(16) -0.065(2) 0.0022(15) F172 0.0751(16) 0.120(2) 0.117(2) 0.0497(18) -0.0609(16) -0.0366(15) F173 0.151(3) 0.122(2) 0.0291(9) 0.0109(12) -0.0082(13) 0.016(2) S174 0.0512(4) 0.0448(4) 0.0406(3) 0.0151(3) -0.0053(3) 0.0047(3) O175 0.0677(16) 0.0765(18) 0.096(2) 0.0537(16) 0.0262(14) 0.0266(13) O176 0.265(6) 0.098(3) 0.0606(18) 0.0490(19) -0.040(3) -0.039(3) O177 0.0452(13) 0.0528(15) 0.145(3) 0.0046(17) 0.0064(15) 0.0014(11) C178 0.067(2) 0.054(2) 0.089(3) -0.0154(19) 0.027(2) -0.0069(17) F179 0.0671(14) 0.0838(17) 0.117(2) 0.0210(16) 0.0040(14) -0.0242(13) F180 0.200(4) 0.257(6) 0.0429(14) -0.023(2) 0.025(2) -0.124(4) F181 0.099(2) 0.0416(15) 0.421(9) 0.003(3) 0.034(4) 0.0168(15) _refine_ls_extinction_method None _oxford_refine_ls_scale 2.6653(18) 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 Zn1 . N2 . 2.0302(14) yes Zn1 . N5 . 2.2735(15) yes Zn1 . N23 . 2.2555(15) yes Zn1 . N39 . 2.2361(16) yes Zn1 . N53 . 2.0383(14) yes Zn1 . N56 . 2.2420(16) yes N2 . C3 . 1.335(2) yes N2 . C21 . 1.335(2) yes C3 . C4 . 1.473(2) yes C3 . C18 . 1.391(2) yes C4 . N5 . 1.280(2) yes C4 . H17 . 0.949 no N5 . C6 . 1.421(2) yes C6 . C7 . 1.388(3) yes C6 . C12 . 1.387(3) yes C7 . C8 . 1.387(3) yes C7 . H16 . 0.952 no C8 . C9 . 1.371(3) yes C8 . H15 . 0.957 no C9 . F10 . 1.357(2) yes C9 . C11 . 1.371(3) yes C11 . C12 . 1.390(3) yes C11 . H14 . 0.938 no C12 . H13 . 0.939 no C18 . C19 . 1.391(3) yes C18 . H38 . 0.939 no C19 . C20 . 1.386(3) yes C19 . H37 . 0.936 no C20 . C21 . 1.392(2) yes C20 . H36 . 0.933 no C21 . C22 . 1.470(3) yes C22 . N23 . 1.285(2) yes C22 . H35 . 0.934 no N23 . C24 . 1.421(2) yes C24 . C25 . 1.393(3) yes C24 . C30 . 1.388(3) yes C25 . C26 . 1.384(3) yes C25 . H34 . 0.942 no C26 . C27 . 1.374(3) yes C26 . H33 . 0.934 no C27 . F28 . 1.354(3) yes C27 . C29 . 1.369(3) yes C29 . C30 . 1.391(3) yes C29 . H32 . 0.929 no C30 . H31 . 0.937 no N39 . C40 . 1.421(2) yes N39 . C51 . 1.283(2) yes C40 . C41 . 1.390(3) yes C40 . C46 . 1.391(3) yes C41 . C42 . 1.390(3) yes C41 . H50 . 0.938 no C42 . C43 . 1.372(3) yes C42 . H49 . 0.947 no C43 . F44 . 1.357(3) yes C43 . C45 . 1.376(3) yes C45 . C46 . 1.387(3) yes C45 . H48 . 0.941 no C46 . H47 . 0.933 no C51 . C52 . 1.469(3) yes C51 . H74 . 0.932 no C52 . N53 . 1.333(2) yes C52 . C71 . 1.393(2) yes N53 . C54 . 1.337(2) yes C54 . C55 . 1.475(3) yes C54 . C69 . 1.389(2) yes C55 . N56 . 1.281(2) yes C55 . H68 . 0.943 no N56 . C57 . 1.421(2) yes C57 . C58 . 1.387(3) yes C57 . C63 . 1.394(3) yes C58 . C59 . 1.380(3) yes C58 . H67 . 0.950 no C59 . C60 . 1.371(3) yes C59 . H66 . 0.938 no C60 . F61 . 1.356(3) yes C60 . C62 . 1.370(3) yes C62 . C63 . 1.389(3) yes C62 . H65 . 0.935 no C63 . H64 . 0.953 no C69 . C70 . 1.392(3) yes C69 . H73 . 0.938 no C70 . C71 . 1.389(3) yes C70 . H72 . 0.929 no Zn75 . N76 . 2.2109(16) yes Zn75 . N79 . 2.0374(15) yes Zn75 . N82 . 2.2904(16) yes Zn75 . N113 . 2.0383(15) yes Zn75 . N116 . 2.2522(16) yes Zn75 . N134 . 2.2825(16) yes N76 . C77 . 1.281(2) yes N76 . C102 . 1.419(2) yes C77 . C78 . 1.471(3) yes C77 . H101 . 0.931 no C78 . N79 . 1.330(2) yes C78 . C97 . 1.392(3) yes N79 . C80 . 1.335(2) yes C80 . C81 . 1.472(3) yes C80 . C95 . 1.388(3) yes C81 . N82 . 1.281(2) yes C81 . H94 . 0.942 no N82 . C83 . 1.422(2) yes C83 . C84 . 1.390(3) yes C83 . C89 . 1.394(3) yes C84 . C85 . 1.390(3) yes C84 . H93 . 0.928 no C85 . C86 . 1.369(3) yes C85 . H92 . 0.941 no C86 . F87 . 1.354(3) yes C86 . C88 . 1.375(4) yes C88 . C89 . 1.387(3) yes C88 . H91 . 0.934 no C89 . H90 . 0.935 no C95 . C96 . 1.383(3) yes C95 . H100 . 0.938 no C96 . C97 . 1.388(3) yes C96 . H99 . 0.940 no C97 . H98 . 0.935 no C102 . C103 . 1.395(3) yes C102 . C108 . 1.391(3) yes C103 . C104 . 1.381(3) yes C103 . H112 . 0.921 no C104 . C105 . 1.369(4) yes C104 . H111 . 0.942 no C105 . F106 . 1.347(3) yes C105 . C107 . 1.375(3) yes C107 . C108 . 1.383(3) yes C107 . H110 . 0.942 no C108 . H109 . 0.945 no N113 . C114 . 1.334(2) yes N113 . C132 . 1.336(2) yes C114 . C115 . 1.477(3) yes C114 . C129 . 1.387(2) yes C115 . N116 . 1.281(2) yes C115 . H128 . 0.953 no N116 . C117 . 1.423(2) yes C117 . C118 . 1.389(3) yes C117 . C123 . 1.380(3) yes C118 . C119 . 1.386(3) yes C118 . H127 . 0.929 no C119 . C120 . 1.358(4) yes C119 . H126 . 0.933 no C120 . F121 . 1.354(3) yes C120 . C122 . 1.364(4) yes C122 . C123 . 1.379(4) yes C122 . H125 . 0.933 no C123 . H124 . 0.944 no C129 . C130 . 1.392(3) yes C129 . H149 . 0.918 no C130 . C131 . 1.389(3) yes C130 . H148 . 0.932 no C131 . C132 . 1.389(3) yes C131 . H147 . 0.932 no C132 . C133 . 1.465(3) yes C133 . N134 . 1.284(2) yes C133 . H146 . 0.936 no N134 . C135 . 1.421(2) yes C135 . C136 . 1.391(3) yes C135 . C141 . 1.390(3) yes C136 . C137 . 1.388(3) yes C136 . H145 . 0.927 no C137 . C138 . 1.365(3) yes C137 . H144 . 0.944 no C138 . F139 . 1.359(2) yes C138 . C140 . 1.373(3) yes C140 . C141 . 1.385(3) yes C140 . H143 . 0.937 no C141 . H142 . 0.938 no S150 . O151 . 1.443(2) yes S150 . O152 . 1.4213(19) yes S150 . O153 . 1.429(2) yes S150 . C154 . 1.823(3) yes C154 . F155 . 1.331(3) yes C154 . F156 . 1.314(3) yes C154 . F157 . 1.331(4) yes S158 . O159 . 1.421(2) yes S158 . O160 . 1.444(2) yes S158 . O161 . 1.424(2) yes S158 . C162 . 1.812(3) yes C162 . F163 . 1.327(4) yes C162 . F164 . 1.338(4) yes C162 . F165 . 1.300(4) yes S166 . O167 . 1.4170(19) yes S166 . O168 . 1.434(3) yes S166 . O169 . 1.400(3) yes S166 . C170 . 1.808(3) yes C170 . F171 . 1.318(4) yes C170 . F172 . 1.305(4) yes C170 . F173 . 1.298(4) yes S174 . O175 . 1.421(3) yes S174 . O176 . 1.401(3) yes S174 . O177 . 1.404(3) yes S174 . C178 . 1.788(4) yes C178 . F179 . 1.319(5) yes C178 . F180 . 1.254(6) yes C178 . F181 . 1.355(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 N2 . Zn1 . N5 . 75.16(6) yes N2 . Zn1 . N23 . 76.11(6) yes N5 . Zn1 . N23 . 151.23(5) yes N2 . Zn1 . N39 . 102.50(6) yes N5 . Zn1 . N39 . 90.98(6) yes N23 . Zn1 . N39 . 96.59(6) yes N2 . Zn1 . N53 . 175.66(6) yes N5 . Zn1 . N53 . 100.91(6) yes N23 . Zn1 . N53 . 107.86(6) yes N39 . Zn1 . N53 . 75.53(6) yes N2 . Zn1 . N56 . 106.03(6) yes N5 . Zn1 . N56 . 93.01(5) yes N23 . Zn1 . N56 . 93.48(6) yes N39 . Zn1 . N56 . 151.27(5) yes N53 . Zn1 . N56 . 75.78(6) yes Zn1 . N2 . C3 . 120.24(12) yes Zn1 . N2 . C21 . 119.09(12) yes C3 . N2 . C21 . 120.66(15) yes N2 . C3 . C4 . 114.38(15) yes N2 . C3 . C18 . 121.38(17) yes C4 . C3 . C18 . 124.19(17) yes C3 . C4 . N5 . 118.18(16) yes C3 . C4 . H17 . 119.5 no N5 . C4 . H17 . 122.3 no Zn1 . N5 . C4 . 111.89(12) yes Zn1 . N5 . C6 . 128.07(11) yes C4 . N5 . C6 . 119.40(15) yes N5 . C6 . C7 . 118.88(16) yes N5 . C6 . C12 . 120.75(16) yes C7 . C6 . C12 . 120.33(17) yes C6 . C7 . C8 . 120.47(18) yes C6 . C7 . H16 . 119.0 no C8 . C7 . H16 . 120.6 no C7 . C8 . C9 . 117.94(19) yes C7 . C8 . H15 . 120.7 no C9 . C8 . H15 . 121.4 no C8 . C9 . F10 . 118.7(2) yes C8 . C9 . C11 . 122.86(19) yes F10 . C9 . C11 . 118.4(2) yes C9 . C11 . C12 . 119.1(2) yes C9 . C11 . H14 . 120.8 no C12 . C11 . H14 . 120.1 no C11 . C12 . C6 . 119.21(19) yes C11 . C12 . H13 . 119.8 no C6 . C12 . H13 . 121.0 no C3 . C18 . C19 . 118.22(18) yes C3 . C18 . H38 . 121.4 no C19 . C18 . H38 . 120.3 no C18 . C19 . C20 . 120.07(17) yes C18 . C19 . H37 . 120.3 no C20 . C19 . H37 . 119.6 no C19 . C20 . C21 . 118.20(18) yes C19 . C20 . H36 . 121.0 no C21 . C20 . H36 . 120.8 no C20 . C21 . N2 . 121.45(17) yes C20 . C21 . C22 . 123.69(17) yes N2 . C21 . C22 . 114.85(15) yes C21 . C22 . N23 . 118.57(16) yes C21 . C22 . H35 . 120.9 no N23 . C22 . H35 . 120.5 no Zn1 . N23 . C22 . 111.26(12) yes Zn1 . N23 . C24 . 129.25(12) yes C22 . N23 . C24 . 119.49(15) yes N23 . C24 . C25 . 121.95(17) yes N23 . C24 . C30 . 118.27(16) yes C25 . C24 . C30 . 119.78(18) yes C24 . C25 . C26 . 119.53(19) yes C24 . C25 . H34 . 121.2 no C26 . C25 . H34 . 119.2 no C25 . C26 . C27 . 119.1(2) yes C25 . C26 . H33 . 119.9 no C27 . C26 . H33 . 121.0 no C26 . C27 . F28 . 117.9(2) yes C26 . C27 . C29 . 123.0(2) yes F28 . C27 . C29 . 119.0(2) yes C27 . C29 . C30 . 117.6(2) yes C27 . C29 . H32 . 121.7 no C30 . C29 . H32 . 120.7 no C29 . C30 . C24 . 120.91(19) yes C29 . C30 . H31 . 119.3 no C24 . C30 . H31 . 119.7 no Zn1 . N39 . C40 . 126.19(11) yes Zn1 . N39 . C51 . 112.50(13) yes C40 . N39 . C51 . 119.91(16) yes N39 . C40 . C41 . 119.06(17) yes N39 . C40 . C46 . 120.55(16) yes C41 . C40 . C46 . 120.28(18) yes C40 . C41 . C42 . 119.9(2) yes C40 . C41 . H50 . 119.9 no C42 . C41 . H50 . 120.2 no C41 . C42 . C43 . 118.5(2) yes C41 . C42 . H49 . 121.0 no C43 . C42 . H49 . 120.5 no C42 . C43 . F44 . 119.1(2) yes C42 . C43 . C45 . 122.9(2) yes F44 . C43 . C45 . 118.0(2) yes C43 . C45 . C46 . 118.5(2) yes C43 . C45 . H48 . 120.3 no C46 . C45 . H48 . 121.2 no C40 . C46 . C45 . 119.88(19) yes C40 . C46 . H47 . 120.6 no C45 . C46 . H47 . 119.5 no N39 . C51 . C52 . 118.01(17) yes N39 . C51 . H74 . 121.0 no C52 . C51 . H74 . 121.0 no C51 . C52 . N53 . 114.23(15) yes C51 . C52 . C71 . 124.15(18) yes N53 . C52 . C71 . 121.58(18) yes C52 . N53 . Zn1 . 119.48(12) yes C52 . N53 . C54 . 121.03(15) yes Zn1 . N53 . C54 . 119.48(12) yes N53 . C54 . C55 . 114.03(15) yes N53 . C54 . C69 . 121.04(18) yes C55 . C54 . C69 . 124.92(18) yes C54 . C55 . N56 . 118.54(17) yes C54 . C55 . H68 . 120.0 no N56 . C55 . H68 . 121.4 no Zn1 . N56 . C55 . 112.16(13) yes Zn1 . N56 . C57 . 127.50(12) yes C55 . N56 . C57 . 120.10(16) yes N56 . C57 . C58 . 121.61(17) yes N56 . C57 . C63 . 118.55(16) yes C58 . C57 . C63 . 119.82(18) yes C57 . C58 . C59 . 119.5(2) yes C57 . C58 . H67 . 121.1 no C59 . C58 . H67 . 119.4 no C58 . C59 . C60 . 119.5(2) yes C58 . C59 . H66 . 120.2 no C60 . C59 . H66 . 120.3 no C59 . C60 . F61 . 118.4(2) yes C59 . C60 . C62 . 122.6(2) yes F61 . C60 . C62 . 119.0(2) yes C60 . C62 . C63 . 117.93(19) yes C60 . C62 . H65 . 121.7 no C63 . C62 . H65 . 120.4 no C57 . C63 . C62 . 120.57(18) yes C57 . C63 . H64 . 120.5 no C62 . C63 . H64 . 118.9 no C54 . C69 . C70 . 118.25(19) yes C54 . C69 . H73 . 120.1 no C70 . C69 . H73 . 121.6 no C69 . C70 . C71 . 120.39(17) yes C69 . C70 . H72 . 120.5 no C71 . C70 . H72 . 119.1 no C52 . C71 . C70 . 117.70(19) yes N76 . Zn75 . N79 . 76.36(6) yes N76 . Zn75 . N82 . 150.70(6) yes N79 . Zn75 . N82 . 74.49(6) yes N76 . Zn75 . N113 . 113.67(6) yes N79 . Zn75 . N113 . 169.95(6) yes N82 . Zn75 . N113 . 95.46(6) yes N76 . Zn75 . N116 . 94.90(6) yes N79 . Zn75 . N116 . 104.62(6) yes N82 . Zn75 . N116 . 95.20(6) yes N113 . Zn75 . N116 . 75.82(6) yes N76 . Zn75 . N134 . 95.12(6) yes N79 . Zn75 . N134 . 104.17(6) yes N82 . Zn75 . N134 . 89.16(6) yes N113 . Zn75 . N134 . 75.24(6) yes N116 . Zn75 . N134 . 151.01(6) yes Zn75 . N76 . C77 . 112.37(13) yes Zn75 . N76 . C102 . 127.82(12) yes C77 . N76 . C102 . 119.81(16) yes N76 . C77 . C78 . 118.19(16) yes N76 . C77 . H101 . 121.0 no C78 . C77 . H101 . 120.8 no C77 . C78 . N79 . 114.52(16) yes C77 . C78 . C97 . 123.73(18) yes N79 . C78 . C97 . 121.74(19) yes C78 . N79 . Zn75 . 118.49(13) yes C78 . N79 . C80 . 120.58(16) yes Zn75 . N79 . C80 . 120.93(12) yes N79 . C80 . C81 . 114.13(16) yes N79 . C80 . C95 . 121.23(18) yes C81 . C80 . C95 . 124.52(18) yes C80 . C81 . N82 . 118.12(17) yes C80 . C81 . H94 . 120.0 no N82 . C81 . H94 . 121.9 no Zn75 . N82 . C81 . 112.02(13) yes Zn75 . N82 . C83 . 127.06(12) yes C81 . N82 . C83 . 119.39(16) yes N82 . C83 . C84 . 120.21(17) yes N82 . C83 . C89 . 119.24(18) yes C84 . C83 . C89 . 120.44(18) yes C83 . C84 . C85 . 119.6(2) yes C83 . C84 . H93 . 120.5 no C85 . C84 . H93 . 119.9 no C84 . C85 . C86 . 118.9(2) yes C84 . C85 . H92 . 120.0 no C86 . C85 . H92 . 121.1 no C85 . C86 . F87 . 118.2(2) yes C85 . C86 . C88 . 122.6(2) yes F87 . C86 . C88 . 119.1(2) yes C86 . C88 . C89 . 118.8(2) yes C86 . C88 . H91 . 120.6 no C89 . C88 . H91 . 120.6 no C83 . C89 . C88 . 119.6(2) yes C83 . C89 . H90 . 120.3 no C88 . C89 . H90 . 120.1 no C80 . C95 . C96 . 118.5(2) yes C80 . C95 . H100 . 120.2 no C96 . C95 . H100 . 121.3 no C95 . C96 . C97 . 120.15(19) yes C95 . C96 . H99 . 120.2 no C97 . C96 . H99 . 119.6 no C78 . C97 . C96 . 117.79(19) yes C78 . C97 . H98 . 120.1 no C96 . C97 . H98 . 122.1 no N76 . C102 . C103 . 122.23(18) yes N76 . C102 . C108 . 117.97(17) yes C103 . C102 . C108 . 119.77(19) yes C102 . C103 . C104 . 119.4(2) yes C102 . C103 . H112 . 120.4 no C104 . C103 . H112 . 120.2 no C103 . C104 . C105 . 119.3(2) yes C103 . C104 . H111 . 121.4 no C105 . C104 . H111 . 119.2 no C104 . C105 . F106 . 118.4(2) yes C104 . C105 . C107 . 122.8(2) yes F106 . C105 . C107 . 118.8(2) yes C105 . C107 . C108 . 117.8(2) yes C105 . C107 . H110 . 120.4 no C108 . C107 . H110 . 121.8 no C102 . C108 . C107 . 120.8(2) yes C102 . C108 . H109 . 119.9 no C107 . C108 . H109 . 119.2 no Zn75 . N113 . C114 . 119.36(12) yes Zn75 . N113 . C132 . 119.61(12) yes C114 . N113 . C132 . 120.74(15) yes N113 . C114 . C115 . 114.42(15) yes N113 . C114 . C129 . 121.53(18) yes C115 . C114 . C129 . 124.01(18) yes C114 . C115 . N116 . 118.52(17) yes C114 . C115 . H128 . 120.7 no N116 . C115 . H128 . 120.8 no Zn75 . N116 . C115 . 111.83(13) yes Zn75 . N116 . C117 . 129.00(12) yes C115 . N116 . C117 . 118.94(16) yes N116 . C117 . C118 . 119.29(18) yes N116 . C117 . C123 . 121.33(18) yes C118 . C117 . C123 . 119.4(2) yes C117 . C118 . C119 . 120.5(2) yes C117 . C118 . H127 . 119.6 no C119 . C118 . H127 . 120.0 no C118 . C119 . C120 . 118.3(2) yes C118 . C119 . H126 . 120.5 no C120 . C119 . H126 . 121.2 no C119 . C120 . F121 . 118.8(2) yes C119 . C120 . C122 . 122.6(2) yes F121 . C120 . C122 . 118.6(3) yes C120 . C122 . C123 . 119.1(3) yes C120 . C122 . H125 . 121.5 no C123 . C122 . H125 . 119.4 no C117 . C123 . C122 . 120.1(2) yes C117 . C123 . H124 . 119.8 no C122 . C123 . H124 . 120.1 no C114 . C129 . C130 . 118.04(19) yes C114 . C129 . H149 . 120.9 no C130 . C129 . H149 . 121.0 no C129 . C130 . C131 . 120.20(18) yes C129 . C130 . H148 . 119.5 no C131 . C130 . H148 . 120.3 no C130 . C131 . C132 . 118.07(19) yes C130 . C131 . H147 . 121.4 no C132 . C131 . H147 . 120.5 no C131 . C132 . N113 . 121.40(18) yes C131 . C132 . C133 . 123.75(18) yes N113 . C132 . C133 . 114.85(15) yes C132 . C133 . N134 . 118.67(16) yes C132 . C133 . H146 . 119.4 no N134 . C133 . H146 . 121.9 no Zn75 . N134 . C133 . 111.23(12) yes Zn75 . N134 . C135 . 129.69(12) yes C133 . N134 . C135 . 119.02(16) yes N134 . C135 . C136 . 118.88(17) yes N134 . C135 . C141 . 121.18(16) yes C136 . C135 . C141 . 119.94(17) yes C135 . C136 . C137 . 120.36(19) yes C135 . C136 . H145 . 120.1 no C137 . C136 . H145 . 119.5 no C136 . C137 . C138 . 118.16(19) yes C136 . C137 . H144 . 120.3 no C138 . C137 . H144 . 121.5 no C137 . C138 . F139 . 119.15(19) yes C137 . C138 . C140 . 123.0(2) yes F139 . C138 . C140 . 117.8(2) yes C138 . C140 . C141 . 118.9(2) yes C138 . C140 . H143 . 120.6 no C141 . C140 . H143 . 120.5 no C135 . C141 . C140 . 119.62(18) yes C135 . C141 . H142 . 120.4 no C140 . C141 . H142 . 119.9 no O151 . S150 . O152 . 113.72(13) yes O151 . S150 . O153 . 114.98(15) yes O152 . S150 . O153 . 116.57(14) yes O151 . S150 . C154 . 101.17(13) yes O152 . S150 . C154 . 105.07(15) yes O153 . S150 . C154 . 102.73(13) yes S150 . C154 . F155 . 110.8(2) yes S150 . C154 . F156 . 112.6(2) yes F155 . C154 . F156 . 107.1(2) yes S150 . C154 . F157 . 109.91(18) yes F155 . C154 . F157 . 107.6(3) yes F156 . C154 . F157 . 108.7(3) yes O159 . S158 . O160 . 112.59(14) yes O159 . S158 . O161 . 116.90(15) yes O160 . S158 . O161 . 115.01(17) yes O159 . S158 . C162 . 105.30(16) yes O160 . S158 . C162 . 101.48(15) yes O161 . S158 . C162 . 103.21(15) yes S158 . C162 . F163 . 111.4(2) yes S158 . C162 . F164 . 109.7(2) yes F163 . C162 . F164 . 107.2(3) yes S158 . C162 . F165 . 113.2(3) yes F163 . C162 . F165 . 107.3(3) yes F164 . C162 . F165 . 107.9(3) yes O167 . S166 . O168 . 111.51(17) yes O167 . S166 . O169 . 116.4(2) yes O168 . S166 . O169 . 115.4(3) yes O167 . S166 . C170 . 105.48(15) yes O168 . S166 . C170 . 102.46(17) yes O169 . S166 . C170 . 103.66(16) yes S166 . C170 . F171 . 110.5(2) yes S166 . C170 . F172 . 112.0(2) yes F171 . C170 . F172 . 105.9(3) yes S166 . C170 . F173 . 112.7(3) yes F171 . C170 . F173 . 108.4(3) yes F172 . C170 . F173 . 106.9(3) yes O175 . S174 . O176 . 111.1(3) yes O175 . S174 . O177 . 114.25(19) yes O176 . S174 . O177 . 117.9(3) yes O175 . S174 . C178 . 103.3(2) yes O176 . S174 . C178 . 104.4(2) yes O177 . S174 . C178 . 103.79(18) yes S174 . C178 . F179 . 114.2(3) yes S174 . C178 . F180 . 115.1(4) yes F179 . C178 . F180 . 108.5(4) yes S174 . C178 . F181 . 107.6(4) yes F179 . C178 . F181 . 103.4(4) yes F180 . C178 . F181 . 107.1(5) 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 C12 . H13 . O151 1_655 155 0.94 2.36 3.242(3) yes C25 . H34 . O151 . 146 0.94 2.58 3.397(3) yes C20 . H36 . O152 . 141 0.93 2.55 3.331(3) yes C46 . H47 . O168 . 154 0.93 2.55 3.415(3) yes C41 . H50 . O151 . 144 0.94 2.55 3.351(3) yes C58 . H67 . O160 1_545 161 0.95 2.32 3.239(3) yes C89 . H90 . O160 . 147 0.93 2.52 3.343(3) yes C84 . H93 . O176 1_655 150 0.93 2.49 3.330(3) yes C77 . H101 . O175 . 142 0.93 2.41 3.199(3) yes C123 . H124 . O160 . 162 0.94 2.49 3.398(3) yes C141 . H142 . O168 . 151 0.94 2.54 3.391(3) yes C131 . H147 . O167 2_765 126 0.93 2.59 3.224(3) yes #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 695909' _montpellier_publication_code 52Zn2+ _montpellier_structure_analysis_code flo1 _montpellier_compound_description 'PDA-OMe-Zn-Tf 2:1' _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; One triflate anion was found to be disordered within the oxygen and fluorine part, sharing the S-C skeletton. The two parts were regularized using the coordinates of the non-disordered triflate counter ion and refined using rigid body contraints and bond length restraints. The total occupancy of the two parts was fixed at 1.00. Equivalent isotropic temperature factors for the F and O atoms of each part were refined. Despite this modelling rather large residuals are still found in the oxygen and fluorine parts of the disordered triflate counter anion. All atoms,except H refined anisotropically. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 12.9994(3) _cell_length_b 13.0121(3) _cell_length_c 14.4037(3) _cell_angle_alpha 76.696(2) _cell_angle_beta 74.783(2) _cell_angle_gamma 88.9478(19) _cell_volume 2285.57(9) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall ? 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' 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' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Zn 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097 1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C44 H38 F6 N6 O10 S2 Zn1 # Dc = 1.53 Fooo = 1080.00 Mu = 7.18 M = 1054.32 # Found Formula = C44 H38 F6 N6 O10 S2 Zn1 # Dc = 1.53 FOOO = 1080.00 Mu = 7.18 M = 1054.32 _chemical_formula_sum 'C44 H38 F6 N6 O10 S2 Zn1' _chemical_formula_moiety 'C42 H38 N6 O4 Zn, 2(C F3 O3 S)' _chemical_compound_source ? _chemical_formula_weight 1054.32 _exptl_absorpt_correction_T_min 0.76674 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_measurement_device Gemini _diffrn_measurement_device_type Serial _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w/2\q _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_detector_area_resol_mean 16.0143 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_orient_matrix_UB_11 0.0513443261 _diffrn_orient_matrix_UB_12 0.0258672643 _diffrn_orient_matrix_UB_13 -0.0179349369 _diffrn_orient_matrix_UB_21 0.0160457152 _diffrn_orient_matrix_UB_22 -0.0342799027 _diffrn_orient_matrix_UB_23 -0.0324850074 _diffrn_orient_matrix_UB_31 -0.0176277178 _diffrn_orient_matrix_UB_32 0.0360041577 _diffrn_orient_matrix_UB_33 -0.0370710697 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -8.00 110.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 32.0000 79.0000 0.0000 0.0000 0.0000 118 #__ type_ start__ end____ width___ exp.time_ 2 omega -8.00 110.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 32.0000 79.0000 120.0000 0.0000 0.0000 118 #__ type_ start__ end____ width___ exp.time_ 3 omega -72.00 47.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -32.0000 80.0000 90.0000 0.0000 0.0000 119 #__ type_ start__ end____ width___ exp.time_ 4 phi -180.00 98.00 1.0000 20.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames 11.0000 32.0000 60.0000 - 0.0000 0.0000 278 ; _cell_measurement_reflns_used 16476 _cell_measurement_temperature 173 _exptl_crystal_description prism _exptl_crystal_colour 'light red' _exptl_crystal_size_min 0.3 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_max 0.5 _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 0.718 # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _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 'every 50 frames' _diffrn_standards_number '2 frames' _diffrn_standards_decay_% 0 _diffrn_ambient_temperature 173 _diffrn_reflns_number 23919 _reflns_number_total 12517 _diffrn_reflns_av_R_equivalents 0.011 # Number of reflections with Friedels Law is 12517 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 14532 _diffrn_reflns_theta_min 3.693 _diffrn_reflns_theta_max 31.110 _diffrn_measured_fraction_theta_max 0.852 _diffrn_reflns_theta_full 25.199 _diffrn_measured_fraction_theta_full 0.963 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min -17 _reflns_limit_h_max 18 _reflns_limit_k_min -17 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _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 -1.57 _refine_diff_density_max 2.47 # 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 10261 _refine_ls_number_restraints 828 _refine_ls_number_parameters 583 _oxford_refine_ls_R_factor_ref 0.0789 _refine_ls_wR_factor_ref 0.0998 _refine_ls_goodness_of_fit_ref 1.0773 _refine_ls_shift/su_max 0.009108 # The values computed from all data _oxford_reflns_number_all 12517 _refine_ls_R_factor_all 0.0910 _refine_ls_wR_factor_all 0.1088 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 10261 _refine_ls_R_factor_gt 0.0789 _refine_ls_wR_factor_gt 0.0998 # 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: 21.7 -3.39 16.2 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined structure solution reference User-defined data collection reference User defined data reduction User defined cell refinement Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 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 Zn1 Zn 0.44138(3) 0.35381(3) 0.29159(3) 0.0186 1.0000 Uani . . . . . . . N2 N 0.4721(2) 0.4889(2) 0.1474(2) 0.0212 1.0000 Uani . . . . . . . C3 C 0.3954(3) 0.5637(3) 0.1272(2) 0.0215 1.0000 Uani . . . . . . . C4 C 0.2960(3) 0.5268(3) 0.1234(3) 0.0251 1.0000 Uani . . . . . . . C5 C 0.2138(3) 0.5960(3) 0.1197(3) 0.0271 1.0000 Uani . . . . . . . C6 C 0.2287(3) 0.7015(3) 0.1213(3) 0.0274 1.0000 Uani . . . . . . . O7 O 0.1410(3) 0.7605(3) 0.1246(3) 0.0378 1.0000 Uani . . . . . . . C8 C 0.1518(4) 0.8685(4) 0.1278(5) 0.0504 1.0000 Uani . . . . . . . H9 H 0.0842 0.8986 0.1304 0.0645 1.0000 Uiso R . . . . . . H10 H 0.1739 0.8741 0.1842 0.0645 1.0000 Uiso R . . . . . . H11 H 0.2018 0.9063 0.0686 0.0645 1.0000 Uiso R . . . . . . C12 C 0.3284(3) 0.7397(3) 0.1214(3) 0.0269 1.0000 Uani . . . . . . . C13 C 0.4118(3) 0.6702(3) 0.1240(3) 0.0242 1.0000 Uani . . . . . . . H14 H 0.4778 0.6954 0.1248 0.0296 1.0000 Uiso R . . . . . . H15 H 0.3402 0.8101 0.1194 0.0329 1.0000 Uiso R . . . . . . H16 H 0.1482 0.5729 0.1160 0.0345 1.0000 Uiso R . . . . . . H17 H 0.2851 0.4562 0.1236 0.0316 1.0000 Uiso R . . . . . . C18 C 0.5729(3) 0.5104(3) 0.1100(2) 0.0243 1.0000 Uani . . . . . . . C19 C 0.6475(3) 0.4380(3) 0.1494(2) 0.0226 1.0000 Uani . . . . . . . N20 N 0.6015(2) 0.3602(2) 0.2281(2) 0.0201 1.0000 Uani . . . . . . . C21 C 0.6606(3) 0.2936(3) 0.2749(3) 0.0232 1.0000 Uani . . . . . . . C22 C 0.7720(3) 0.3008(3) 0.2435(3) 0.0300 1.0000 Uani . . . . . . . C23 C 0.8203(3) 0.3806(4) 0.1613(3) 0.0334 1.0000 Uani . . . . . . . C24 C 0.7578(3) 0.4508(3) 0.1134(3) 0.0301 1.0000 Uani . . . . . . . H25 H 0.7883 0.5046 0.0599 0.0361 1.0000 Uiso R . . . . . . H26 H 0.8936 0.3872 0.1387 0.0392 1.0000 Uiso R . . . . . . H27 H 0.8123 0.2533 0.2773 0.0375 1.0000 Uiso R . . . . . . C28 C 0.6006(3) 0.2197(3) 0.3657(3) 0.0238 1.0000 Uani . . . . . . . N29 N 0.4992(2) 0.2299(2) 0.3972(2) 0.0208 1.0000 Uani . . . . . . . C30 C 0.4375(3) 0.1626(3) 0.4858(2) 0.0205 1.0000 Uani . . . . . . . C31 C 0.3270(3) 0.1648(3) 0.5031(3) 0.0261 1.0000 Uani . . . . . . . C32 C 0.2589(3) 0.0995(3) 0.5857(3) 0.0292 1.0000 Uani . . . . . . . C33 C 0.3026(3) 0.0322(3) 0.6539(3) 0.0282 1.0000 Uani . . . . . . . O34 O 0.2443(3) -0.0341(3) 0.7377(3) 0.0436 1.0000 Uani . . . . . . . C35 C 0.1304(5) -0.0296(6) 0.7584(5) 0.0679 1.0000 Uani . . . . . . . H36 H 0.0985 -0.0784 0.8196 0.0727 1.0000 Uiso R . . . . . . H37 H 0.1101 0.0405 0.7623 0.0727 1.0000 Uiso R . . . . . . H38 H 0.1057 -0.0481 0.7066 0.0727 1.0000 Uiso R . . . . . . C39 C 0.4133(3) 0.0310(3) 0.6384(3) 0.0269 1.0000 Uani . . . . . . . C40 C 0.4806(3) 0.0957(3) 0.5555(3) 0.0232 1.0000 Uani . . . . . . . H41 H 0.5540 0.0943 0.5472 0.0300 1.0000 Uiso R . . . . . . H42 H 0.4418 -0.0135 0.6853 0.0326 1.0000 Uiso R . . . . . . H43 H 0.1858 0.1011 0.5944 0.0352 1.0000 Uiso R . . . . . . H44 H 0.2982 0.2110 0.4578 0.0319 1.0000 Uiso R . . . . . . H45 H 0.6354 0.1678 0.3997 0.0293 1.0000 Uiso R . . . . . . H46 H 0.5973 0.5717 0.0602 0.0290 1.0000 Uiso R . . . . . . N47 N 0.4418(2) 0.4954(2) 0.3610(2) 0.0209 1.0000 Uani . . . . . . . C48 C 0.3500(3) 0.5352(3) 0.3800(3) 0.0237 1.0000 Uani . . . . . . . C49 C 0.2589(3) 0.4754(3) 0.3718(2) 0.0226 1.0000 Uani . . . . . . . N50 N 0.2843(2) 0.3893(2) 0.3371(2) 0.0194 1.0000 Uani . . . . . . . C51 C 0.2100(3) 0.3303(3) 0.3209(2) 0.0205 1.0000 Uani . . . . . . . C52 C 0.2525(3) 0.2412(3) 0.2779(2) 0.0209 1.0000 Uani . . . . . . . N53 N 0.3545(2) 0.2348(2) 0.2502(2) 0.0196 1.0000 Uani . . . . . . . C54 C 0.3995(3) 0.1461(3) 0.2160(2) 0.0203 1.0000 Uani . . . . . . . C55 C 0.4959(3) 0.1614(3) 0.1431(3) 0.0229 1.0000 Uani . . . . . . . C56 C 0.5447(3) 0.0757(3) 0.1088(3) 0.0253 1.0000 Uani . . . . . . . C57 C 0.4979(3) -0.0257(3) 0.1497(3) 0.0238 1.0000 Uani . . . . . . . O58 O 0.5397(2) -0.1150(2) 0.1243(2) 0.0318 1.0000 Uani . . . . . . . C59 C 0.6410(4) -0.1046(3) 0.0526(4) 0.0372 1.0000 Uani . . . . . . . H60 H 0.6611 -0.1743 0.0443 0.0470 1.0000 Uiso R . . . . . . H61 H 0.6929 -0.0756 0.0765 0.0470 1.0000 Uiso R . . . . . . H62 H 0.6373 -0.0601 -0.0093 0.0470 1.0000 Uiso R . . . . . . C63 C 0.4012(3) -0.0410(3) 0.2243(3) 0.0257 1.0000 Uani . . . . . . . C64 C 0.3529(3) 0.0441(3) 0.2572(3) 0.0236 1.0000 Uani . . . . . . . H65 H 0.2889 0.0346 0.3079 0.0288 1.0000 Uiso R . . . . . . H66 H 0.3701 -0.1086 0.2519 0.0314 1.0000 Uiso R . . . . . . H67 H 0.6081 0.0858 0.0594 0.0308 1.0000 Uiso R . . . . . . H68 H 0.5285 0.2288 0.1171 0.0274 1.0000 Uiso R . . . . . . H69 H 0.2063 0.1901 0.2720 0.0262 1.0000 Uiso R . . . . . . C70 C 0.1031(3) 0.3555(3) 0.3429(3) 0.0261 1.0000 Uani . . . . . . . C71 C 0.0754(3) 0.4431(3) 0.3824(3) 0.0305 1.0000 Uani . . . . . . . C72 C 0.1536(3) 0.5059(3) 0.3952(3) 0.0289 1.0000 Uani . . . . . . . H73 H 0.1363 0.5664 0.4186 0.0341 1.0000 Uiso R . . . . . . H74 H 0.0043 0.4602 0.4002 0.0366 1.0000 Uiso R . . . . . . H75 H 0.0522 0.3137 0.3309 0.0317 1.0000 Uiso R . . . . . . H76 H 0.3397 0.6003 0.3978 0.0302 1.0000 Uiso R . . . . . . C77 C 0.5355(3) 0.5531(3) 0.3556(2) 0.0218 1.0000 Uani . . . . . . . C78 C 0.6207(3) 0.4976(3) 0.3810(3) 0.0235 1.0000 Uani . . . . . . . C79 C 0.7188(3) 0.5484(3) 0.3661(3) 0.0250 1.0000 Uani . . . . . . . C80 C 0.7328(3) 0.6563(3) 0.3238(3) 0.0270 1.0000 Uani . . . . . . . O81 O 0.8260(3) 0.7135(3) 0.3017(3) 0.0375 1.0000 Uani . . . . . . . C82 C 0.9178(4) 0.6558(5) 0.3116(4) 0.0449 1.0000 Uani . . . . . . . H83 H 0.9792 0.7039 0.2881 0.0535 1.0000 Uiso R . . . . . . H84 H 0.9102 0.6216 0.3792 0.0535 1.0000 Uiso R . . . . . . H85 H 0.9288 0.6033 0.2729 0.0535 1.0000 Uiso R . . . . . . C86 C 0.6467(3) 0.7138(3) 0.3000(3) 0.0305 1.0000 Uani . . . . . . . C87 C 0.5494(3) 0.6630(3) 0.3165(3) 0.0271 1.0000 Uani . . . . . . . H88 H 0.4933 0.7015 0.3003 0.0354 1.0000 Uiso R . . . . . . H89 H 0.6561 0.7857 0.2736 0.0395 1.0000 Uiso R . . . . . . H90 H 0.7743 0.5093 0.3842 0.0328 1.0000 Uiso R . . . . . . H91 H 0.6120 0.4249 0.4082 0.0313 1.0000 Uiso R . . . . . . S92 S 0.81202(8) 0.21787(8) 0.52949(9) 0.0346 1.0000 Uani . . . . . . . O93 O 0.8510(3) 0.3133(3) 0.4548(3) 0.0413 1.0000 Uani . . . . . . . O94 O 0.7521(5) 0.1425(4) 0.5055(5) 0.0848 1.0000 Uani . . . . . . . O95 O 0.7710(5) 0.2357(4) 0.6277(4) 0.0790 1.0000 Uani . . . . . . . C96 C 0.9310(4) 0.1470(5) 0.5419(5) 0.0532 1.0000 Uani . . . . . . . F97 F 0.9060(4) 0.0582(3) 0.6134(3) 0.0757 1.0000 Uani . . . . . . . F98 F 0.9836(4) 0.1232(4) 0.4596(4) 0.0998 1.0000 Uani . . . . . . . F99 F 1.0009(4) 0.2041(4) 0.5610(4) 0.0983 1.0000 Uani . . . . . . . S100 S 1.13071(11) 0.26798(16) 0.08749(9) 0.0660 1.0000 Uani D . . . . . . C104 C 1.0676(3) 0.2560(3) -0.0088(3) 0.0486 1.0000 Uani D . . . . . . F105 F 1.1273(3) 0.2163(4) -0.0784(3) 0.0649(8) 0.594(3) Uiso DG . P . . . . F106 F 0.9732(3) 0.2097(4) 0.0268(3) 0.0649(8) 0.594(3) Uiso DG . P . . . . F107 F 1.0450(4) 0.3559(3) -0.0487(3) 0.0649(8) 0.594(3) Uiso DG . P . . . . O108 O 1.0623(3) 0.3138(4) 0.1560(3) 0.0649(8) 0.594(3) Uiso DG . P . . . . O109 O 1.1438(4) 0.1488(3) 0.1240(3) 0.0649(8) 0.594(3) Uiso DG . P . . . . O110 O 1.2310(3) 0.3196(4) 0.0332(3) 0.0649(8) 0.594(3) Uiso DG . P . . . . O111 O 1.0861(6) 0.3714(5) 0.1157(6) 0.0867(14) 0.406(3) Uiso DG . P . . . . O112 O 1.2461(3) 0.2768(7) 0.0378(5) 0.0867(14) 0.406(3) Uiso DG . P . . . . O113 O 1.0913(6) 0.1754(5) 0.1680(4) 0.0867(14) 0.406(3) Uiso DG . P . . . . F114 F 1.1004(6) 0.1634(5) -0.0330(5) 0.0867(14) 0.406(3) Uiso DG . P . . . . F115 F 1.0940(6) 0.3377(5) -0.0853(4) 0.0867(14) 0.406(3) Uiso DG . P . . . . F116 F 0.9614(3) 0.2544(6) 0.0254(5) 0.0867(14) 0.406(3) Uiso DG . P . . . . 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 Zn1 0.01550(17) 0.01848(17) 0.02079(18) -0.00483(13) -0.00296(13) 0.00094(12) N2 0.0225(13) 0.0217(12) 0.0191(12) -0.0056(10) -0.0041(10) -0.0003(10) C3 0.0246(15) 0.0225(14) 0.0160(12) -0.0022(11) -0.0048(11) -0.0014(12) C4 0.0268(16) 0.0261(15) 0.0217(14) -0.0040(12) -0.0062(12) -0.0048(13) C5 0.0238(15) 0.0338(17) 0.0250(15) -0.0065(13) -0.0090(13) -0.0021(13) C6 0.0278(17) 0.0321(17) 0.0224(15) -0.0044(13) -0.0086(13) 0.0032(14) O7 0.0296(14) 0.0384(16) 0.0461(17) -0.0086(13) -0.0129(13) 0.0082(12) C8 0.039(2) 0.042(2) 0.070(3) -0.017(2) -0.012(2) 0.015(2) C12 0.0308(17) 0.0236(15) 0.0262(16) -0.0045(12) -0.0085(13) 0.0010(13) C13 0.0240(15) 0.0236(15) 0.0238(14) -0.0039(12) -0.0056(12) -0.0022(12) C18 0.0252(15) 0.0266(15) 0.0177(13) -0.0041(11) -0.0007(12) -0.0010(12) C19 0.0215(15) 0.0234(14) 0.0205(14) -0.0069(12) 0.0001(11) -0.0020(12) N20 0.0195(12) 0.0207(12) 0.0193(12) -0.0056(10) -0.0026(10) 0.0001(10) C21 0.0193(14) 0.0227(14) 0.0266(15) -0.0066(12) -0.0033(12) 0.0010(11) C22 0.0198(15) 0.0327(18) 0.0354(18) -0.0083(15) -0.0036(14) 0.0039(13) C23 0.0179(15) 0.040(2) 0.0376(19) -0.0080(16) 0.0006(14) -0.0025(14) C24 0.0215(16) 0.0349(18) 0.0278(16) -0.0054(14) 0.0026(13) -0.0057(14) C28 0.0207(14) 0.0218(14) 0.0270(15) -0.0041(12) -0.0047(12) 0.0040(11) N29 0.0183(12) 0.0212(12) 0.0218(12) -0.0048(10) -0.0035(10) 0.0013(10) C30 0.0209(14) 0.0193(13) 0.0200(13) -0.0036(11) -0.0043(11) 0.0017(11) C31 0.0196(14) 0.0310(17) 0.0233(15) -0.0002(13) -0.0036(12) 0.0034(12) C32 0.0221(15) 0.0317(17) 0.0290(17) -0.0008(14) -0.0038(13) -0.0003(13) C33 0.0332(18) 0.0226(15) 0.0246(15) -0.0016(12) -0.0032(13) -0.0032(13) O34 0.0376(16) 0.0396(17) 0.0375(16) 0.0125(13) -0.0002(13) -0.0058(13) C35 0.041(3) 0.060(3) 0.068(4) 0.022(3) 0.012(3) -0.005(2) C39 0.0314(17) 0.0252(15) 0.0232(15) -0.0006(12) -0.0104(13) 0.0014(13) C40 0.0234(15) 0.0232(14) 0.0237(14) -0.0039(12) -0.0086(12) 0.0016(12) N47 0.0228(13) 0.0207(12) 0.0194(12) -0.0057(10) -0.0051(10) 0.0007(10) C48 0.0257(15) 0.0248(15) 0.0220(14) -0.0097(12) -0.0050(12) 0.0039(12) C49 0.0224(14) 0.0242(14) 0.0197(13) -0.0049(11) -0.0035(11) 0.0017(12) N50 0.0172(12) 0.0224(12) 0.0182(11) -0.0044(10) -0.0043(9) 0.0021(9) C51 0.0188(14) 0.0215(14) 0.0194(13) -0.0030(11) -0.0035(11) -0.0002(11) C52 0.0201(14) 0.0207(14) 0.0215(13) -0.0028(11) -0.0063(11) -0.0014(11) N53 0.0206(12) 0.0190(12) 0.0191(11) -0.0049(9) -0.0046(10) 0.0014(9) C54 0.0200(14) 0.0204(13) 0.0202(13) -0.0055(11) -0.0042(11) 0.0001(11) C55 0.0240(15) 0.0181(13) 0.0240(14) -0.0036(11) -0.0028(12) -0.0012(11) C56 0.0258(16) 0.0229(15) 0.0242(15) -0.0049(12) -0.0019(12) 0.0010(12) C57 0.0278(16) 0.0203(14) 0.0251(15) -0.0072(12) -0.0086(13) 0.0026(12) O58 0.0320(14) 0.0203(11) 0.0410(15) -0.0114(11) -0.0028(12) 0.0043(10) C59 0.034(2) 0.0304(18) 0.045(2) -0.0158(17) -0.0025(17) 0.0078(15) C63 0.0276(16) 0.0172(13) 0.0303(16) -0.0041(12) -0.0054(13) -0.0016(12) C64 0.0213(14) 0.0221(14) 0.0246(14) -0.0048(12) -0.0017(12) -0.0020(12) C70 0.0177(14) 0.0295(16) 0.0277(16) -0.0023(13) -0.0040(12) -0.0010(12) C71 0.0189(15) 0.0339(18) 0.0359(18) -0.0085(15) -0.0026(13) 0.0049(13) C72 0.0235(16) 0.0300(17) 0.0317(17) -0.0106(14) -0.0025(13) 0.0069(13) C77 0.0244(15) 0.0213(14) 0.0217(14) -0.0098(11) -0.0056(12) 0.0027(12) C78 0.0275(16) 0.0203(14) 0.0241(14) -0.0074(12) -0.0077(12) 0.0037(12) C79 0.0229(15) 0.0301(16) 0.0240(15) -0.0096(13) -0.0070(12) 0.0048(13) C80 0.0250(16) 0.0288(16) 0.0289(16) -0.0107(13) -0.0064(13) -0.0008(13) O81 0.0284(14) 0.0350(15) 0.0469(17) -0.0062(13) -0.0090(12) -0.0048(12) C82 0.0264(19) 0.055(3) 0.047(2) -0.006(2) -0.0058(17) -0.0025(18) C86 0.0311(18) 0.0218(15) 0.042(2) -0.0090(14) -0.0139(15) 0.0008(13) C87 0.0279(17) 0.0217(15) 0.0359(18) -0.0100(13) -0.0131(14) 0.0047(13) S92 0.0198(4) 0.0290(4) 0.0501(6) -0.0050(4) -0.0042(4) 0.0009(3) O93 0.0337(15) 0.0378(16) 0.0439(17) 0.0026(13) -0.0063(13) 0.0025(13) O94 0.075(3) 0.066(3) 0.124(4) 0.003(3) -0.067(3) -0.024(2) O95 0.101(4) 0.043(2) 0.059(2) -0.0058(19) 0.030(2) 0.014(2) C96 0.036(2) 0.045(3) 0.069(3) 0.006(2) -0.014(2) 0.002(2) F97 0.064(2) 0.053(2) 0.088(3) 0.0237(19) -0.019(2) 0.0049(17) F98 0.079(3) 0.062(2) 0.114(4) -0.005(2) 0.037(3) 0.029(2) F99 0.057(2) 0.098(3) 0.133(4) 0.028(3) -0.060(3) -0.023(2) S100 0.0365(6) 0.1274(15) 0.0291(5) 0.0000(7) -0.0138(5) -0.0302(8) C104 0.048(3) 0.065(3) 0.033(2) -0.012(2) -0.0093(19) -0.016(2) _refine_ls_extinction_method None _oxford_refine_ls_scale 4.264(10) 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 Zn1 . N2 . 2.339(3) yes Zn1 . N20 . 2.036(3) yes Zn1 . N29 . 2.215(3) yes Zn1 . N47 . 2.290(3) yes Zn1 . N50 . 2.053(3) yes Zn1 . N53 . 2.207(3) yes N2 . C3 . 1.419(5) yes N2 . C18 . 1.288(5) yes C3 . C4 . 1.405(5) yes C3 . C13 . 1.396(5) yes C4 . C5 . 1.389(5) yes C4 . H17 . 0.930 no C5 . C6 . 1.397(6) yes C5 . H16 . 0.927 no C6 . O7 . 1.359(5) yes C6 . C12 . 1.397(5) yes O7 . C8 . 1.428(6) yes C8 . H9 . 0.951 no C8 . H10 . 0.948 no C8 . H11 . 0.958 no C12 . C13 . 1.401(5) yes C12 . H15 . 0.924 no C13 . H14 . 0.927 no C18 . C19 . 1.470(5) yes C18 . H46 . 0.936 no C19 . N20 . 1.344(4) yes C19 . C24 . 1.390(5) yes N20 . C21 . 1.333(5) yes C21 . C22 . 1.397(5) yes C21 . C28 . 1.469(5) yes C22 . C23 . 1.393(6) yes C22 . H27 . 0.936 no C23 . C24 . 1.396(6) yes C23 . H26 . 0.921 no C24 . H25 . 0.918 no C28 . N29 . 1.291(4) yes C28 . H45 . 0.924 no N29 . C30 . 1.419(4) yes C30 . C31 . 1.392(5) yes C30 . C40 . 1.397(4) yes C31 . C32 . 1.389(5) yes C31 . H44 . 0.932 no C32 . C33 . 1.392(5) yes C32 . H43 . 0.926 no C33 . O34 . 1.356(4) yes C33 . C39 . 1.397(6) yes O34 . C35 . 1.434(7) yes C35 . H36 . 0.956 no C35 . H37 . 0.956 no C35 . H38 . 0.964 no C39 . C40 . 1.385(5) yes C39 . H42 . 0.933 no C40 . H41 . 0.930 no N47 . C48 . 1.280(5) yes N47 . C77 . 1.418(4) yes C48 . C49 . 1.474(5) yes C48 . H76 . 0.938 no C49 . N50 . 1.331(5) yes C49 . C72 . 1.394(5) yes N50 . C51 . 1.343(4) yes C51 . C52 . 1.470(5) yes C51 . C70 . 1.392(5) yes C52 . N53 . 1.287(4) yes C52 . H69 . 0.938 no N53 . C54 . 1.415(4) yes C54 . C55 . 1.391(5) yes C54 . C64 . 1.400(5) yes C55 . C56 . 1.396(5) yes C55 . H68 . 0.932 no C56 . C57 . 1.394(5) yes C56 . H67 . 0.926 no C57 . O58 . 1.359(4) yes C57 . C63 . 1.406(5) yes O58 . C59 . 1.431(5) yes C59 . H60 . 0.965 no C59 . H61 . 0.952 no C59 . H62 . 0.957 no C63 . C64 . 1.380(5) yes C63 . H66 . 0.929 no C64 . H65 . 0.940 no C70 . C71 . 1.389(6) yes C70 . H75 . 0.939 no C71 . C72 . 1.390(6) yes C71 . H74 . 0.930 no C72 . H73 . 0.928 no C77 . C78 . 1.394(5) yes C77 . C87 . 1.408(5) yes C78 . C79 . 1.390(5) yes C78 . H91 . 0.934 no C79 . C80 . 1.390(5) yes C79 . H90 . 0.933 no C80 . O81 . 1.358(5) yes C80 . C86 . 1.408(6) yes O81 . C82 . 1.419(6) yes C82 . H83 . 0.961 no C82 . H84 . 0.953 no C82 . H85 . 0.963 no C86 . C87 . 1.376(5) yes C86 . H89 . 0.923 no C87 . H88 . 0.926 no S92 . O93 . 1.441(3) yes S92 . O94 . 1.418(5) yes S92 . O95 . 1.445(5) yes S92 . C96 . 1.814(6) yes C96 . F97 . 1.339(6) yes C96 . F98 . 1.306(9) yes C96 . F99 . 1.305(8) yes S100 . C104 . 1.822(4) yes S100 . O108 . 1.383(3) yes S100 . O109 . 1.540(3) yes S100 . O110 . 1.420(3) yes S100 . O111 . 1.554(4) yes S100 . O112 . 1.477(4) yes S100 . O113 . 1.458(4) yes C104 . F105 . 1.300(4) yes C104 . F106 . 1.299(4) yes C104 . F107 . 1.355(4) yes C104 . F114 . 1.361(4) yes C104 . F115 . 1.319(4) yes C104 . F116 . 1.338(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 N2 . Zn1 . N20 . 74.09(11) yes N2 . Zn1 . N29 . 151.29(11) yes N20 . Zn1 . N29 . 77.22(11) yes N2 . Zn1 . N47 . 81.37(10) yes N20 . Zn1 . N47 . 96.21(11) yes N29 . Zn1 . N47 . 100.73(10) yes N2 . Zn1 . N50 . 92.41(11) yes N20 . Zn1 . N50 . 164.71(11) yes N29 . Zn1 . N50 . 115.87(11) yes N47 . Zn1 . N50 . 74.26(11) yes N2 . Zn1 . N53 . 100.40(10) yes N20 . Zn1 . N53 . 112.70(11) yes N29 . Zn1 . N53 . 91.63(10) yes N47 . Zn1 . N53 . 150.50(11) yes N50 . Zn1 . N53 . 76.24(11) yes Zn1 . N2 . C3 . 123.3(2) yes Zn1 . N2 . C18 . 110.6(2) yes C3 . N2 . C18 . 121.6(3) yes N2 . C3 . C4 . 118.7(3) yes N2 . C3 . C13 . 121.0(3) yes C4 . C3 . C13 . 119.8(3) yes C3 . C4 . C5 . 119.7(3) yes C3 . C4 . H17 . 120.3 no C5 . C4 . H17 . 120.0 no C4 . C5 . C6 . 120.5(3) yes C4 . C5 . H16 . 120.6 no C6 . C5 . H16 . 118.9 no C5 . C6 . O7 . 115.7(4) yes C5 . C6 . C12 . 120.1(4) yes O7 . C6 . C12 . 124.2(4) yes C6 . O7 . C8 . 117.8(4) yes O7 . C8 . H9 . 107.8 no O7 . C8 . H10 . 111.0 no H9 . C8 . H10 . 109.6 no O7 . C8 . H11 . 110.0 no H9 . C8 . H11 . 108.1 no H10 . C8 . H11 . 110.3 no C6 . C12 . C13 . 119.4(3) yes C6 . C12 . H15 . 120.9 no C13 . C12 . H15 . 119.6 no C12 . C13 . C3 . 120.3(3) yes C12 . C13 . H14 . 119.4 no C3 . C13 . H14 . 120.2 no N2 . C18 . C19 . 118.1(3) yes N2 . C18 . H46 . 120.4 no C19 . C18 . H46 . 121.5 no C18 . C19 . N20 . 114.9(3) yes C18 . C19 . C24 . 123.7(3) yes N20 . C19 . C24 . 121.3(3) yes C19 . N20 . Zn1 . 121.0(2) yes C19 . N20 . C21 . 120.8(3) yes Zn1 . N20 . C21 . 117.6(2) yes N20 . C21 . C22 . 121.6(3) yes N20 . C21 . C28 . 115.1(3) yes C22 . C21 . C28 . 123.1(3) yes C21 . C22 . C23 . 118.0(4) yes C21 . C22 . H27 . 120.5 no C23 . C22 . H27 . 121.6 no C22 . C23 . C24 . 120.1(3) yes C22 . C23 . H26 . 120.0 no C24 . C23 . H26 . 120.0 no C23 . C24 . C19 . 118.3(3) yes C23 . C24 . H25 . 121.3 no C19 . C24 . H25 . 120.4 no C21 . C28 . N29 . 118.7(3) yes C21 . C28 . H45 . 120.1 no N29 . C28 . H45 . 121.2 no Zn1 . N29 . C28 . 111.2(2) yes Zn1 . N29 . C30 . 127.5(2) yes C28 . N29 . C30 . 121.2(3) yes N29 . C30 . C31 . 116.8(3) yes N29 . C30 . C40 . 124.2(3) yes C31 . C30 . C40 . 118.9(3) yes C30 . C31 . C32 . 121.8(3) yes C30 . C31 . H44 . 118.9 no C32 . C31 . H44 . 119.2 no C31 . C32 . C33 . 118.8(4) yes C31 . C32 . H43 . 120.0 no C33 . C32 . H43 . 121.2 no C32 . C33 . O34 . 124.1(4) yes C32 . C33 . C39 . 119.9(3) yes O34 . C33 . C39 . 116.0(3) yes C33 . O34 . C35 . 117.0(4) yes O34 . C35 . H36 . 109.2 no O34 . C35 . H37 . 109.4 no H36 . C35 . H37 . 110.1 no O34 . C35 . H38 . 110.5 no H36 . C35 . H38 . 109.0 no H37 . C35 . H38 . 108.7 no C33 . C39 . C40 . 120.9(3) yes C33 . C39 . H42 . 119.2 no C40 . C39 . H42 . 119.9 no C30 . C40 . C39 . 119.7(3) yes C30 . C40 . H41 . 121.0 no C39 . C40 . H41 . 119.4 no Zn1 . N47 . C48 . 112.1(2) yes Zn1 . N47 . C77 . 123.9(2) yes C48 . N47 . C77 . 121.2(3) yes N47 . C48 . C49 . 117.5(3) yes N47 . C48 . H76 . 122.4 no C49 . C48 . H76 . 120.0 no C48 . C49 . N50 . 114.8(3) yes C48 . C49 . C72 . 124.0(3) yes N50 . C49 . C72 . 121.1(3) yes C49 . N50 . Zn1 . 120.2(2) yes C49 . N50 . C51 . 121.2(3) yes Zn1 . N50 . C51 . 118.2(2) yes N50 . C51 . C52 . 114.2(3) yes N50 . C51 . C70 . 121.0(3) yes C52 . C51 . C70 . 124.9(3) yes C51 . C52 . N53 . 118.1(3) yes C51 . C52 . H69 . 120.6 no N53 . C52 . H69 . 121.3 no Zn1 . N53 . C52 . 112.8(2) yes Zn1 . N53 . C54 . 125.5(2) yes C52 . N53 . C54 . 120.4(3) yes N53 . C54 . C55 . 118.2(3) yes N53 . C54 . C64 . 121.9(3) yes C55 . C54 . C64 . 119.8(3) yes C54 . C55 . C56 . 120.2(3) yes C54 . C55 . H68 . 120.1 no C56 . C55 . H68 . 119.6 no C55 . C56 . C57 . 119.8(3) yes C55 . C56 . H67 . 120.4 no C57 . C56 . H67 . 119.8 no C56 . C57 . O58 . 124.9(3) yes C56 . C57 . C63 . 119.8(3) yes O58 . C57 . C63 . 115.3(3) yes C57 . O58 . C59 . 117.6(3) yes O58 . C59 . H60 . 107.8 no O58 . C59 . H61 . 109.5 no H60 . C59 . H61 . 108.8 no O58 . C59 . H62 . 110.9 no H60 . C59 . H62 . 110.1 no H61 . C59 . H62 . 109.7 no C57 . C63 . C64 . 120.2(3) yes C57 . C63 . H66 . 119.8 no C64 . C63 . H66 . 120.0 no C54 . C64 . C63 . 120.2(3) yes C54 . C64 . H65 . 119.0 no C63 . C64 . H65 . 120.8 no C51 . C70 . C71 . 118.1(3) yes C51 . C70 . H75 . 120.0 no C71 . C70 . H75 . 121.9 no C70 . C71 . C72 . 120.4(3) yes C70 . C71 . H74 . 120.0 no C72 . C71 . H74 . 119.6 no C49 . C72 . C71 . 118.1(4) yes C49 . C72 . H73 . 120.9 no C71 . C72 . H73 . 121.0 no N47 . C77 . C78 . 118.7(3) yes N47 . C77 . C87 . 122.3(3) yes C78 . C77 . C87 . 118.7(3) yes C77 . C78 . C79 . 121.3(3) yes C77 . C78 . H91 . 119.5 no C79 . C78 . H91 . 119.2 no C78 . C79 . C80 . 119.4(3) yes C78 . C79 . H90 . 119.4 no C80 . C79 . H90 . 121.2 no C79 . C80 . O81 . 124.8(4) yes C79 . C80 . C86 . 119.9(3) yes O81 . C80 . C86 . 115.3(3) yes C80 . O81 . C82 . 116.7(4) yes O81 . C82 . H83 . 108.9 no O81 . C82 . H84 . 110.2 no H83 . C82 . H84 . 109.5 no O81 . C82 . H85 . 111.1 no H83 . C82 . H85 . 108.2 no H84 . C82 . H85 . 108.9 no C80 . C86 . C87 . 120.2(3) yes C80 . C86 . H89 . 119.5 no C87 . C86 . H89 . 120.4 no C77 . C87 . C86 . 120.4(3) yes C77 . C87 . H88 . 120.1 no C86 . C87 . H88 . 119.5 no O93 . S92 . O94 . 117.7(3) yes O93 . S92 . O95 . 113.4(3) yes O94 . S92 . O95 . 115.2(4) yes O93 . S92 . C96 . 104.6(2) yes O94 . S92 . C96 . 101.7(3) yes O95 . S92 . C96 . 101.2(3) yes S92 . C96 . F97 . 110.7(4) yes S92 . C96 . F98 . 112.3(5) yes F97 . C96 . F98 . 109.0(6) yes S92 . C96 . F99 . 112.4(5) yes F97 . C96 . F99 . 109.0(5) yes F98 . C96 . F99 . 103.0(6) yes C104 . S100 . O108 . 109.8(2) yes C104 . S100 . O109 . 96.18(19) yes O108 . S100 . O109 . 114.7(2) yes C104 . S100 . O110 . 103.29(19) yes O108 . S100 . O110 . 119.3(2) yes O109 . S100 . O110 . 110.4(2) yes C104 . S100 . O111 . 103.0(3) yes C104 . S100 . O112 . 104.3(3) yes O111 . S100 . O112 . 113.5(3) yes C104 . S100 . O113 . 105.3(3) yes O111 . S100 . O113 . 111.7(2) yes O112 . S100 . O113 . 117.4(3) yes S100 . C104 . F105 . 114.3(3) yes S100 . C104 . F106 . 112.7(3) yes F105 . C104 . F106 . 112.5(3) yes S100 . C104 . F107 . 105.3(3) yes F105 . C104 . F107 . 109.0(3) yes F106 . C104 . F107 . 102.0(3) yes S100 . C104 . F114 . 105.3(3) yes S100 . C104 . F115 . 111.4(3) yes F114 . C104 . F115 . 112.5(3) yes S100 . C104 . F116 . 110.2(3) yes F114 . C104 . F116 . 111.2(3) yes F115 . C104 . F116 . 106.3(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 C24 . H25 . O110 2_765 146 0.92 2.42 3.218(6) yes C23 . H26 . O108 . 147 0.92 2.43 3.234(6) yes C23 . H26 . O111 . 166 0.92 2.45 3.349(6) yes C40 . H41 . O94 . 165 0.93 2.54 3.448(6) yes C31 . H44 . N50 . 155 0.93 2.59 3.463(6) yes C28 . H45 . O94 . 142 0.92 2.39 3.166(6) yes C18 . H46 . O110 2_765 140 0.94 2.54 3.315(6) yes C59 . H60 . O112 2_755 151 0.96 2.13 3.014(6) yes C63 . H66 . O95 2_656 152 0.93 2.50 3.346(6) yes C52 . H69 . O113 1_455 138 0.94 2.42 3.173(6) yes C48 . H76 . O95 2_666 140 0.94 2.56 3.338(6) yes #===END #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 695910' _montpellier_publication_code 12Fe2+ _montpellier_structure_analysis_code flo6 _montpellier_compound_description 'PDA-H-Fe-BF4 2:1' _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; Weak data, because of rather small crystal and rather large mosaicity. Only Fe atoms refined anisotropically The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # # End of 'script/refcif-b.dat' #end of refcif _cell_length_a 8.1717(5) _cell_length_b 46.7421(2) _cell_length_c 19.9558(4) _cell_angle_alpha 90 _cell_angle_beta 101.11(2) _cell_angle_gamma 90 _cell_volume 7479.5(7) _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' 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' 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' 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' 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' _cell_formula_units_Z 4 _chemical_formula_sum 'C78 H65 B4 F16 Fe2 N13 O1' _chemical_formula_moiety '2(C38 H30 Fe N6), C2 H3 N, 4(B F4), H2 O' _chemical_compound_source ? _chemical_formula_weight 1659.37 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 175 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_min 0.09 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_max 0.19 _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 3392 _exptl_absorpt_coefficient_mu 0.484 # Sheldrick geometric approximatio 0.95 0.96 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.95 _exptl_absorpt_correction_T_max 0.96 _diffrn_measurement_device 'Oxford Diffraction XCALIBUR' _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 'Xcalibur, (Oxford Diffraction, 2002)' _computing_cell_refinement 'CrysAlis RED, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis RED, (Oxford Diffraction, 2002)' _computing_structure_solution 'Sir2004 (Burla et al., 2005)' _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 173 _diffrn_reflns_number 46072 _reflns_number_total 19550 _diffrn_reflns_av_R_equivalents 0.061 # Number of reflections with Friedels Law is 19550 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 23800 _diffrn_reflns_theta_min 3.646 _diffrn_reflns_theta_max 31.334 _diffrn_measured_fraction_theta_max 0.798 _diffrn_reflns_theta_full 25.068 _diffrn_measured_fraction_theta_full 0.942 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -65 _diffrn_reflns_limit_k_max 65 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 28 _reflns_limit_h_min -11 _reflns_limit_h_max 11 _reflns_limit_k_min 0 _reflns_limit_k_max 65 _reflns_limit_l_min 0 _reflns_limit_l_max 28 _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 -0.88 _refine_diff_density_max 1.03 # 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 3803 _refine_ls_number_restraints 0 _refine_ls_number_parameters 467 _oxford_refine_ls_R_factor_ref 0.0963 _refine_ls_wR_factor_ref 0.0666 _refine_ls_goodness_of_fit_ref 1.0469 _refine_ls_shift/su_max 0.000316 # The values computed from all data _oxford_reflns_number_all 19537 _refine_ls_R_factor_all 0.3169 _refine_ls_wR_factor_all 0.0959 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3803 _refine_ls_R_factor_gt 0.0963 _refine_ls_wR_factor_gt 0.0666 # 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: 35.5 -11.2 17.4 16.4 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Burla, M. C. , Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G. L., D Caro, L. , Giacovazzo, C., Polidori, G., & Spagna R. J. Appl. Cryst. (2005). 381-388. 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. Oxford Diffraction, (2002). CrysAlis RED. Oxford Diffraction, (2002). Xcalibur User Manual. 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 0.5198(2) 0.43038(3) 0.78757(10) 0.0272 1.0000 Uani . . . . . . . N2 N 0.6899(11) 0.43615(19) 0.8711(4) 0.024(2) 1.0000 Uiso . . . . . . . C3 C 0.7452(14) 0.4634(2) 0.8996(6) 0.028(3) 1.0000 Uiso . . . . . . . C4 C 0.6991(16) 0.4732(3) 0.9588(6) 0.044(4) 1.0000 Uiso . . . . . . . C5 C 0.7349(17) 0.5010(3) 0.9810(8) 0.058(4) 1.0000 Uiso . . . . . . . C6 C 0.8279(17) 0.5183(3) 0.9457(7) 0.059(4) 1.0000 Uiso . . . . . . . C7 C 0.8779(17) 0.5086(3) 0.8870(7) 0.050(4) 1.0000 Uiso . . . . . . . C8 C 0.8371(15) 0.4813(3) 0.8643(7) 0.039(3) 1.0000 Uiso . . . . . . . H9 H 0.8740 0.4744 0.8260 0.0504 1.0000 Uiso R . . . . . . H10 H 0.9386 0.5204 0.8629 0.0650 1.0000 Uiso R . . . . . . H11 H 0.8548 0.5368 0.9613 0.0770 1.0000 Uiso R . . . . . . H12 H 0.7040 0.5074 1.0210 0.0625 1.0000 Uiso R . . . . . . H13 H 0.6366 0.4616 0.9822 0.0437 1.0000 Uiso R . . . . . . C14 C 0.7269(15) 0.4128(3) 0.9078(6) 0.033(3) 1.0000 Uiso . . . . . . . C15 C 0.6596(16) 0.3873(3) 0.8779(6) 0.039(3) 1.0000 Uiso . . . . . . . N16 N 0.5614(11) 0.39261(19) 0.8162(5) 0.027(2) 1.0000 Uiso . . . . . . . C17 C 0.4800(14) 0.3714(2) 0.7776(6) 0.029(3) 1.0000 Uiso . . . . . . . C18 C 0.4969(16) 0.3431(3) 0.7989(6) 0.042(4) 1.0000 Uiso . . . . . . . C19 C 0.5924(16) 0.3378(3) 0.8636(7) 0.046(4) 1.0000 Uiso . . . . . . . C20 C 0.6730(14) 0.3592(3) 0.9033(6) 0.035(3) 1.0000 Uiso . . . . . . . H21 H 0.7361 0.3553 0.9461 0.0468 1.0000 Uiso R . . . . . . H22 H 0.6010 0.3191 0.8804 0.0487 1.0000 Uiso R . . . . . . H23 H 0.4413 0.3285 0.7717 0.0498 1.0000 Uiso R . . . . . . C24 C 0.3786(15) 0.3826(2) 0.7154(6) 0.032(3) 1.0000 Uiso . . . . . . . N25 N 0.3701(11) 0.4103(2) 0.7122(5) 0.027(2) 1.0000 Uiso . . . . . . . C26 C 0.2704(14) 0.4235(2) 0.6509(6) 0.029(3) 1.0000 Uiso . . . . . . . C27 C 0.2891(15) 0.4148(3) 0.5861(6) 0.032(3) 1.0000 Uiso . . . . . . . C28 C 0.1956(16) 0.4282(3) 0.5304(7) 0.048(4) 1.0000 Uiso . . . . . . . C29 C 0.0892(19) 0.4499(3) 0.5379(8) 0.061(4) 1.0000 Uiso . . . . . . . C30 C 0.0721(17) 0.4584(3) 0.6034(7) 0.053(4) 1.0000 Uiso . . . . . . . C31 C 0.1622(15) 0.4452(3) 0.6616(7) 0.038(3) 1.0000 Uiso . . . . . . . H32 H 0.1520 0.4509 0.7054 0.0393 1.0000 Uiso R . . . . . . H33 H -0.0022 0.4730 0.6082 0.0677 1.0000 Uiso R . . . . . . H34 H 0.0281 0.4590 0.4998 0.0612 1.0000 Uiso R . . . . . . H35 H 0.2071 0.4226 0.4868 0.0531 1.0000 Uiso R . . . . . . H36 H 0.3632 0.4002 0.5803 0.0399 1.0000 Uiso R . . . . . . H37 H 0.3255 0.3709 0.6800 0.0361 1.0000 Uiso R . . . . . . H38 H 0.7922 0.4134 0.9515 0.0425 1.0000 Uiso R . . . . . . N39 N 0.3481(12) 0.4384(2) 0.8428(5) 0.031(3) 1.0000 Uiso . . . . . . . C40 C 0.2808(15) 0.4171(3) 0.8850(6) 0.033(3) 1.0000 Uiso . . . . . . . C41 C 0.3239(15) 0.4190(3) 0.9545(6) 0.037(3) 1.0000 Uiso . . . . . . . C42 C 0.2694(17) 0.3980(3) 0.9943(8) 0.051(4) 1.0000 Uiso . . . . . . . C43 C 0.1715(16) 0.3757(3) 0.9623(7) 0.045(4) 1.0000 Uiso . . . . . . . C44 C 0.1284(16) 0.3751(3) 0.8918(7) 0.043(4) 1.0000 Uiso . . . . . . . C45 C 0.1855(15) 0.3957(2) 0.8515(7) 0.034(3) 1.0000 Uiso . . . . . . . H46 H 0.1609 0.3948 0.8040 0.0312 1.0000 Uiso R . . . . . . H47 H 0.0593 0.3606 0.8703 0.0522 1.0000 Uiso R . . . . . . H48 H 0.1281 0.3620 0.9883 0.0455 1.0000 Uiso R . . . . . . H49 H 0.3020 0.3982 1.0414 0.0555 1.0000 Uiso R . . . . . . H50 H 0.3892 0.4342 0.9751 0.0449 1.0000 Uiso R . . . . . . C51 C 0.3118(15) 0.4652(3) 0.8461(6) 0.035(3) 1.0000 Uiso . . . . . . . C52 C 0.3877(14) 0.4841(2) 0.8051(6) 0.026(3) 1.0000 Uiso . . . . . . . N53 N 0.4821(11) 0.46957(19) 0.7668(5) 0.031(3) 1.0000 Uiso . . . . . . . C54 C 0.5625(14) 0.4826(2) 0.7248(6) 0.029(3) 1.0000 Uiso . . . . . . . C55 C 0.6615(15) 0.4622(3) 0.6943(6) 0.035(3) 1.0000 Uiso . . . . . . . N56 N 0.6658(11) 0.4365(2) 0.7181(5) 0.027(2) 1.0000 Uiso . . . . . . . C57 C 0.7458(14) 0.4147(2) 0.6864(6) 0.029(3) 1.0000 Uiso . . . . . . . C58 C 0.7266(16) 0.4134(3) 0.6147(7) 0.041(4) 1.0000 Uiso . . . . . . . C59 C 0.8025(16) 0.3917(3) 0.5832(7) 0.047(4) 1.0000 Uiso . . . . . . . C60 C 0.8948(16) 0.3717(3) 0.6230(7) 0.043(4) 1.0000 Uiso . . . . . . . C61 C 0.9179(15) 0.3719(3) 0.6947(6) 0.034(3) 1.0000 Uiso . . . . . . . C62 C 0.8389(14) 0.3935(2) 0.7240(6) 0.028(3) 1.0000 Uiso . . . . . . . H63 H 0.8513 0.3939 0.7714 0.0286 1.0000 Uiso R . . . . . . H64 H 0.9831 0.3582 0.7210 0.0328 1.0000 Uiso R . . . . . . H65 H 0.9401 0.3566 0.6021 0.0355 1.0000 Uiso R . . . . . . H66 H 0.7926 0.3914 0.5362 0.0484 1.0000 Uiso R . . . . . . H67 H 0.6620 0.4271 0.5879 0.0533 1.0000 Uiso R . . . . . . H68 H 0.7185 0.4674 0.6603 0.0419 1.0000 Uiso R . . . . . . C69 C 0.5506(15) 0.5126(3) 0.7150(6) 0.035(3) 1.0000 Uiso . . . . . . . C70 C 0.4600(15) 0.5283(3) 0.7533(6) 0.042(3) 1.0000 Uiso . . . . . . . C71 C 0.3780(15) 0.5137(2) 0.7994(6) 0.034(3) 1.0000 Uiso . . . . . . . H72 H 0.3133 0.5237 0.8246 0.0290 1.0000 Uiso R . . . . . . H73 H 0.4502 0.5480 0.7478 0.0501 1.0000 Uiso R . . . . . . H74 H 0.6069 0.5215 0.6846 0.0522 1.0000 Uiso R . . . . . . H75 H 0.2422 0.4717 0.8747 0.0315 1.0000 Uiso R . . . . . . Fe76 Fe 0.5359(2) 0.30557(3) 0.28262(9) 0.0251 1.0000 Uani . . . . . . . N77 N 0.5665(10) 0.30598(19) 0.3784(4) 0.021(2) 1.0000 Uiso . . . . . . . C78 C 0.6555(15) 0.2852(2) 0.4157(6) 0.028(3) 1.0000 Uiso . . . . . . . C79 C 0.6752(16) 0.2855(3) 0.4860(7) 0.042(4) 1.0000 Uiso . . . . . . . C80 C 0.6085(15) 0.3075(3) 0.5188(7) 0.045(3) 1.0000 Uiso . . . . . . . C81 C 0.5198(14) 0.3293(3) 0.4785(6) 0.031(3) 1.0000 Uiso . . . . . . . C82 C 0.5015(15) 0.3278(3) 0.4080(6) 0.031(3) 1.0000 Uiso . . . . . . . C83 C 0.4055(14) 0.3470(3) 0.3582(6) 0.029(3) 1.0000 Uiso . . . . . . . N84 N 0.3963(12) 0.3392(2) 0.2962(5) 0.035(3) 1.0000 Uiso . . . . . . . C85 C 0.3030(14) 0.3573(3) 0.2447(6) 0.028(3) 1.0000 Uiso . . . . . . . C86 C 0.1744(15) 0.3461(3) 0.1965(6) 0.033(3) 1.0000 Uiso . . . . . . . C87 C 0.0823(16) 0.3629(3) 0.1472(6) 0.037(3) 1.0000 Uiso . . . . . . . C88 C 0.1205(16) 0.3912(3) 0.1449(6) 0.040(3) 1.0000 Uiso . . . . . . . C89 C 0.2508(16) 0.4039(3) 0.1919(7) 0.048(4) 1.0000 Uiso . . . . . . . C90 C 0.3400(15) 0.3861(3) 0.2417(6) 0.033(3) 1.0000 Uiso . . . . . . . H91 H 0.4298 0.3935 0.2725 0.0339 1.0000 Uiso R . . . . . . H92 H 0.2779 0.4233 0.1896 0.0507 1.0000 Uiso R . . . . . . H93 H 0.0563 0.4028 0.1120 0.0388 1.0000 Uiso R . . . . . . H94 H -0.0051 0.3550 0.1158 0.0414 1.0000 Uiso R . . . . . . H95 H 0.1527 0.3264 0.1970 0.0500 1.0000 Uiso R . . . . . . H96 H 0.3561 0.3638 0.3701 0.0299 1.0000 Uiso R . . . . . . H97 H 0.4774 0.3450 0.4987 0.0331 1.0000 Uiso R . . . . . . H98 H 0.6203 0.3078 0.5662 0.0522 1.0000 Uiso R . . . . . . H99 H 0.7312 0.2705 0.5112 0.0349 1.0000 Uiso R . . . . . . C100 C 0.7170(14) 0.2651(3) 0.3723(6) 0.028(3) 1.0000 Uiso . . . . . . . N101 N 0.6842(12) 0.27132(19) 0.3066(5) 0.029(2) 1.0000 Uiso . . . . . . . C102 C 0.7405(14) 0.2516(2) 0.2607(6) 0.025(3) 1.0000 Uiso . . . . . . . C103 C 0.8120(14) 0.2619(2) 0.2084(6) 0.027(3) 1.0000 Uiso . . . . . . . C104 C 0.8692(14) 0.2428(2) 0.1635(6) 0.032(3) 1.0000 Uiso . . . . . . . C105 C 0.8539(15) 0.2133(3) 0.1756(6) 0.040(3) 1.0000 Uiso . . . . . . . C106 C 0.7766(15) 0.2035(3) 0.2265(6) 0.043(4) 1.0000 Uiso . . . . . . . C107 C 0.7211(15) 0.2225(3) 0.2694(6) 0.039(3) 1.0000 Uiso . . . . . . . H108 H 0.6684 0.2160 0.3037 0.0500 1.0000 Uiso R . . . . . . H109 H 0.7583 0.1841 0.2310 0.0347 1.0000 Uiso R . . . . . . H110 H 0.8984 0.2000 0.1492 0.0459 1.0000 Uiso R . . . . . . H111 H 0.9202 0.2493 0.1287 0.0509 1.0000 Uiso R . . . . . . H112 H 0.8092 0.2815 0.1996 0.0600 1.0000 Uiso R . . . . . . H113 H 0.7765 0.2489 0.3896 0.0344 1.0000 Uiso R . . . . . . N114 N 0.5032(10) 0.3087(2) 0.1880(4) 0.025(2) 1.0000 Uiso . . . . . . . C115 C 0.3874(14) 0.2918(2) 0.1487(6) 0.027(3) 1.0000 Uiso . . . . . . . C116 C 0.3508(15) 0.2952(2) 0.0785(6) 0.030(3) 1.0000 Uiso . . . . . . . C117 C 0.4293(14) 0.3178(3) 0.0484(6) 0.037(3) 1.0000 Uiso . . . . . . . C118 C 0.5445(15) 0.3349(3) 0.0892(6) 0.039(3) 1.0000 Uiso . . . . . . . C119 C 0.5820(14) 0.3291(2) 0.1600(6) 0.023(3) 1.0000 Uiso . . . . . . . C120 C 0.7025(14) 0.3427(2) 0.2112(6) 0.029(3) 1.0000 Uiso . . . . . . . N121 N 0.7120(11) 0.33376(19) 0.2721(5) 0.026(2) 1.0000 Uiso . . . . . . . C122 C 0.8309(14) 0.3447(2) 0.3279(6) 0.023(3) 1.0000 Uiso . . . . . . . C123 C 0.9413(14) 0.3258(3) 0.3664(6) 0.036(3) 1.0000 Uiso . . . . . . . C124 C 1.0445(15) 0.3354(3) 0.4257(6) 0.036(3) 1.0000 Uiso . . . . . . . C125 C 1.0415(16) 0.3641(3) 0.4460(7) 0.038(3) 1.0000 Uiso . . . . . . . C126 C 0.9314(15) 0.3821(3) 0.4067(6) 0.039(3) 1.0000 Uiso . . . . . . . C127 C 0.8254(15) 0.3731(3) 0.3491(6) 0.033(3) 1.0000 Uiso . . . . . . . H128 H 0.7457 0.3854 0.3249 0.0419 1.0000 Uiso R . . . . . . H129 H 0.9273 0.4012 0.4197 0.0364 1.0000 Uiso R . . . . . . H130 H 1.1126 0.3707 0.4852 0.0360 1.0000 Uiso R . . . . . . H131 H 1.1139 0.3224 0.4531 0.0368 1.0000 Uiso R . . . . . . H132 H 0.9501 0.3072 0.3509 0.0407 1.0000 Uiso R . . . . . . H133 H 0.7699 0.3572 0.1998 0.0325 1.0000 Uiso R . . . . . . H134 H 0.5964 0.3499 0.0705 0.0394 1.0000 Uiso R . . . . . . H135 H 0.4031 0.3207 0.0012 0.0325 1.0000 Uiso R . . . . . . H136 H 0.2759 0.2831 0.0514 0.0283 1.0000 Uiso R . . . . . . C137 C 0.3111(15) 0.2732(2) 0.1912(6) 0.030(3) 1.0000 Uiso . . . . . . . N138 N 0.3515(11) 0.2770(2) 0.2565(5) 0.027(3) 1.0000 Uiso . . . . . . . C139 C 0.2866(13) 0.2582(2) 0.2996(6) 0.024(3) 1.0000 Uiso . . . . . . . C140 C 0.2384(14) 0.2699(3) 0.3570(6) 0.032(3) 1.0000 Uiso . . . . . . . C141 C 0.1720(14) 0.2521(2) 0.4027(6) 0.032(3) 1.0000 Uiso . . . . . . . C142 C 0.1562(16) 0.2232(3) 0.3894(7) 0.045(4) 1.0000 Uiso . . . . . . . C143 C 0.1993(15) 0.2114(3) 0.3317(6) 0.036(3) 1.0000 Uiso . . . . . . . C144 C 0.2690(14) 0.2291(3) 0.2867(6) 0.035(3) 1.0000 Uiso . . . . . . . H145 H 0.3029 0.2214 0.2484 0.0315 1.0000 Uiso R . . . . . . H146 H 0.1849 0.1918 0.3228 0.0400 1.0000 Uiso R . . . . . . H147 H 0.1096 0.2116 0.4189 0.0546 1.0000 Uiso R . . . . . . H148 H 0.1394 0.2597 0.4412 0.0374 1.0000 Uiso R . . . . . . H149 H 0.2517 0.2894 0.3655 0.0347 1.0000 Uiso R . . . . . . H150 H 0.2369 0.2589 0.1729 0.0283 1.0000 Uiso R . . . . . . F151 F 0.9575(8) 0.31762(15) 0.9886(3) 0.051(2) 1.0000 Uiso . . . . . . . B152 B 0.8787(18) 0.2955(3) 1.0194(8) 0.033(4) 1.0000 Uiso . . . . . . . F153 F 0.9715(8) 0.27095(14) 1.0168(3) 0.0431(19) 1.0000 Uiso . . . . . . . F154 F 0.7205(10) 0.29159(16) 0.9835(4) 0.060(2) 1.0000 Uiso . . . . . . . F155 F 0.8809(9) 0.30312(15) 1.0860(4) 0.056(2) 1.0000 Uiso . . . . . . . F156 F 0.5707(15) 0.4462(3) 0.4699(6) 0.123(4) 1.0000 Uiso . . . . . . . B157 B 0.519(2) 0.4266(4) 0.4181(10) 0.064(5) 1.0000 Uiso . . . . . . . F158 F 0.5057(11) 0.40065(19) 0.4450(5) 0.078(3) 1.0000 Uiso . . . . . . . F159 F 0.3661(13) 0.4371(2) 0.3847(5) 0.095(3) 1.0000 Uiso . . . . . . . F160 F 0.6172(12) 0.4281(2) 0.3710(5) 0.091(3) 1.0000 Uiso . . . . . . . F161 F -0.2835(9) 0.39983(16) 0.0651(4) 0.060(2) 1.0000 Uiso . . . . . . . B162 B -0.3009(18) 0.4211(3) 0.1123(8) 0.034(4) 1.0000 Uiso . . . . . . . F163 F -0.4507(9) 0.43488(15) 0.0920(4) 0.050(2) 1.0000 Uiso . . . . . . . F164 F -0.1714(10) 0.44085(17) 0.1140(4) 0.059(2) 1.0000 Uiso . . . . . . . F165 F -0.2927(10) 0.40946(17) 0.1756(4) 0.063(2) 1.0000 Uiso . . . . . . . F166 F 1.1343(14) 0.3006(2) 0.5763(6) 0.117(4) 1.0000 Uiso . . . . . . . B167 B 1.2537(18) 0.3134(4) 0.6208(7) 0.036(4) 1.0000 Uiso . . . . . . . F168 F 1.3051(10) 0.33685(19) 0.5881(4) 0.075(3) 1.0000 Uiso . . . . . . . F169 F 1.3837(13) 0.2958(2) 0.6413(5) 0.105(3) 1.0000 Uiso . . . . . . . F170 F 1.1943(8) 0.32296(13) 0.6779(3) 0.0394(18) 1.0000 Uiso . . . . . . . O171 O 0.280(2) 0.5007(3) 0.4443(8) 0.157(6) 1.0000 Uiso . . . . . . . H172 H 0.3333 0.4983 0.4847 0.2000 1.0000 Uiso R . . . . . . H173 H 0.1881 0.4937 0.4255 0.2000 1.0000 Uiso R . . . . . . N174 N 0.0155(15) 0.4973(3) 0.2694(6) 0.059(3) 1.0000 Uiso . . . . . . . C175 C 0.0042(18) 0.4748(3) 0.2884(8) 0.055(4) 1.0000 Uiso . . . . . . . C176 C -0.0194(19) 0.4456(3) 0.3081(7) 0.064(4) 1.0000 Uiso . . . . . . . H177 H 0.0231 0.4433 0.3556 0.0711 1.0000 Uiso R . . . . . . H178 H -0.1348 0.4410 0.2986 0.0711 1.0000 Uiso R . . . . . . H179 H 0.0387 0.4332 0.2830 0.0711 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 0.0312(11) 0.0205(9) 0.0303(11) -0.0008(10) 0.0069(8) -0.0003(10) Fe76 0.0253(9) 0.0228(11) 0.0267(10) -0.0019(9) 0.0041(7) -0.0004(9) _refine_ls_extinction_method None _oxford_refine_ls_scale 1.139(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 . N2 . 1.973(9) yes Fe1 . N16 . 1.866(9) yes Fe1 . N25 . 1.984(9) yes Fe1 . N39 . 1.980(10) yes Fe1 . N53 . 1.890(9) yes Fe1 . N56 . 2.016(9) yes N2 . C3 . 1.431(13) yes N2 . C14 . 1.315(14) yes C3 . C4 . 1.386(16) yes C3 . C8 . 1.400(16) yes C4 . C5 . 1.387(18) yes C4 . H13 . 0.930 no C5 . C6 . 1.389(18) yes C5 . H12 . 0.932 no C6 . C7 . 1.389(17) yes C6 . H11 . 0.932 no C7 . C8 . 1.376(17) yes C7 . H10 . 0.934 no C8 . H9 . 0.933 no C14 . C15 . 1.400(16) yes C14 . H38 . 0.931 no C15 . N16 . 1.356(14) yes C15 . C20 . 1.404(16) yes N16 . C17 . 1.350(13) yes C17 . C18 . 1.389(16) yes C17 . C24 . 1.451(15) yes C18 . C19 . 1.396(16) yes C18 . H23 . 0.933 no C19 . C20 . 1.365(16) yes C19 . H22 . 0.931 no C20 . H21 . 0.927 no C24 . N25 . 1.297(14) yes C24 . H37 . 0.931 no N25 . C26 . 1.471(14) yes C26 . C27 . 1.393(15) yes C26 . C31 . 1.386(15) yes C27 . C28 . 1.373(16) yes C27 . H36 . 0.934 no C28 . C29 . 1.366(18) yes C28 . H35 . 0.930 no C29 . C30 . 1.398(18) yes C29 . H34 . 0.928 no C30 . C31 . 1.394(17) yes C30 . H33 . 0.930 no C31 . H32 . 0.933 no N39 . C40 . 1.477(14) yes N39 . C51 . 1.293(14) yes C40 . C41 . 1.366(16) yes C40 . C45 . 1.361(16) yes C41 . C42 . 1.391(17) yes C41 . H50 . 0.934 no C42 . C43 . 1.394(17) yes C42 . H49 . 0.925 no C43 . C44 . 1.383(16) yes C43 . H48 . 0.935 no C44 . C45 . 1.393(16) yes C44 . H47 . 0.932 no C45 . H46 . 0.930 no C51 . C52 . 1.426(16) yes C51 . H75 . 0.931 no C52 . N53 . 1.367(13) yes C52 . C71 . 1.389(15) yes N53 . C54 . 1.312(13) yes C54 . C55 . 1.458(15) yes C54 . C69 . 1.413(16) yes C55 . N56 . 1.291(14) yes C55 . H68 . 0.927 no N56 . C57 . 1.423(14) yes C57 . C58 . 1.411(16) yes C57 . C62 . 1.380(15) yes C58 . C59 . 1.399(17) yes C58 . H67 . 0.932 no C59 . C60 . 1.358(17) yes C59 . H66 . 0.926 no C60 . C61 . 1.407(16) yes C60 . H65 . 0.932 no C61 . C62 . 1.385(15) yes C61 . H64 . 0.930 no C62 . H63 . 0.932 no C69 . C70 . 1.374(16) yes C69 . H74 . 0.928 no C70 . C71 . 1.413(16) yes C70 . H73 . 0.932 no C71 . H72 . 0.924 no Fe76 . N77 . 1.878(8) yes Fe76 . N84 . 1.989(10) yes Fe76 . N101 . 2.010(9) yes Fe76 . N114 . 1.861(9) yes Fe76 . N121 . 1.992(9) yes Fe76 . N138 . 2.007(9) yes N77 . C78 . 1.348(13) yes N77 . C82 . 1.340(13) yes C78 . C79 . 1.380(16) yes C78 . C100 . 1.434(16) yes C79 . C80 . 1.387(17) yes C79 . H99 . 0.931 no C80 . C81 . 1.408(16) yes C80 . H98 . 0.933 no C81 . C82 . 1.389(15) yes C81 . H97 . 0.932 no C82 . C83 . 1.451(15) yes C83 . N84 . 1.278(13) yes C83 . H96 . 0.933 no N84 . C85 . 1.432(14) yes C85 . C86 . 1.383(15) yes C85 . C90 . 1.383(15) yes C86 . C87 . 1.365(16) yes C86 . H95 . 0.937 no C87 . C88 . 1.362(16) yes C87 . H94 . 0.931 no C88 . C89 . 1.407(17) yes C88 . H93 . 0.932 no C89 . C90 . 1.389(16) yes C89 . H92 . 0.936 no C90 . H91 . 0.929 no C100 . N101 . 1.318(13) yes C100 . H113 . 0.931 no N101 . C102 . 1.436(14) yes C102 . C103 . 1.377(15) yes C102 . C107 . 1.384(16) yes C103 . C104 . 1.410(15) yes C103 . H112 . 0.931 no C104 . C105 . 1.409(16) yes C104 . H111 . 0.926 no C105 . C106 . 1.374(16) yes C105 . H110 . 0.933 no C106 . C107 . 1.372(16) yes C106 . H109 . 0.926 no C107 . H108 . 0.929 no N114 . C115 . 1.359(13) yes N114 . C119 . 1.333(13) yes C115 . C116 . 1.385(15) yes C115 . C137 . 1.437(15) yes C116 . C117 . 1.429(16) yes C116 . H136 . 0.925 no C117 . C118 . 1.375(16) yes C117 . H135 . 0.934 no C118 . C119 . 1.413(16) yes C118 . H134 . 0.933 no C119 . C120 . 1.426(15) yes C120 . N121 . 1.273(13) yes C120 . H133 . 0.930 no N121 . C122 . 1.425(14) yes C122 . C123 . 1.384(15) yes C122 . C127 . 1.393(15) yes C123 . C124 . 1.389(16) yes C123 . H132 . 0.931 no C124 . C125 . 1.401(16) yes C124 . H131 . 0.932 no C125 . C126 . 1.363(16) yes C125 . H130 . 0.933 no C126 . C127 . 1.366(16) yes C126 . H129 . 0.934 no C127 . H128 . 0.931 no C137 . N138 . 1.292(13) yes C137 . H150 . 0.929 no N138 . C139 . 1.403(13) yes C139 . C140 . 1.395(15) yes C139 . C144 . 1.384(16) yes C140 . C141 . 1.417(16) yes C140 . H149 . 0.930 no C141 . C142 . 1.378(16) yes C141 . H148 . 0.932 no C142 . C143 . 1.383(16) yes C142 . H147 . 0.934 no C143 . C144 . 1.419(16) yes C143 . H146 . 0.933 no C144 . H145 . 0.935 no F151 . B152 . 1.418(15) yes B152 . F153 . 1.382(15) yes B152 . F154 . 1.364(16) yes B152 . F155 . 1.373(15) yes F156 . B157 . 1.38(2) yes B157 . F158 . 1.338(19) yes B157 . F159 . 1.390(19) yes B157 . F160 . 1.349(19) yes F161 . B162 . 1.395(15) yes B162 . F163 . 1.373(15) yes B162 . F164 . 1.399(15) yes B162 . F165 . 1.365(15) yes F166 . B167 . 1.329(16) yes B167 . F168 . 1.380(16) yes B167 . F169 . 1.343(16) yes B167 . F170 . 1.396(14) yes O171 . H172 . 0.848 no O171 . H173 . 0.837 no N174 . C175 . 1.128(15) yes C175 . C176 . 1.446(18) yes C176 . H177 . 0.950 no C176 . H178 . 0.950 no C176 . H179 . 0.950 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 N2 . Fe1 . N16 . 79.3(4) yes N2 . Fe1 . N25 . 159.5(4) yes N16 . Fe1 . N25 . 80.4(4) yes N2 . Fe1 . N39 . 87.9(4) yes N16 . Fe1 . N39 . 96.6(4) yes N25 . Fe1 . N39 . 96.4(4) yes N2 . Fe1 . N53 . 96.4(4) yes N16 . Fe1 . N53 . 174.9(4) yes N25 . Fe1 . N53 . 104.0(4) yes N39 . Fe1 . N53 . 80.6(4) yes N2 . Fe1 . N56 . 98.5(4) yes N16 . Fe1 . N56 . 104.3(4) yes N25 . Fe1 . N56 . 84.6(4) yes N39 . Fe1 . N56 . 158.9(4) yes N53 . Fe1 . N56 . 78.8(4) yes Fe1 . N2 . C3 . 125.0(7) yes Fe1 . N2 . C14 . 114.0(8) yes C3 . N2 . C14 . 119.7(10) yes N2 . C3 . C4 . 121.0(11) yes N2 . C3 . C8 . 119.4(10) yes C4 . C3 . C8 . 119.4(12) yes C3 . C4 . C5 . 120.5(13) yes C3 . C4 . H13 . 120.1 no C5 . C4 . H13 . 119.3 no C4 . C5 . C6 . 119.1(14) yes C4 . C5 . H12 . 119.8 no C6 . C5 . H12 . 120.9 no C5 . C6 . C7 . 121.1(14) yes C5 . C6 . H11 . 119.2 no C7 . C6 . H11 . 119.7 no C6 . C7 . C8 . 119.2(14) yes C6 . C7 . H10 . 121.0 no C8 . C7 . H10 . 119.8 no C3 . C8 . C7 . 120.6(13) yes C3 . C8 . H9 . 119.7 no C7 . C8 . H9 . 119.7 no N2 . C14 . C15 . 116.1(11) yes N2 . C14 . H38 . 121.7 no C15 . C14 . H38 . 122.1 no C14 . C15 . N16 . 110.2(11) yes C14 . C15 . C20 . 130.3(12) yes N16 . C15 . C20 . 119.4(11) yes C15 . N16 . Fe1 . 119.5(8) yes C15 . N16 . C17 . 121.5(10) yes Fe1 . N16 . C17 . 118.7(8) yes N16 . C17 . C18 . 121.1(11) yes N16 . C17 . C24 . 111.2(10) yes C18 . C17 . C24 . 127.7(11) yes C17 . C18 . C19 . 117.2(12) yes C17 . C18 . H23 . 120.6 no C19 . C18 . H23 . 122.1 no C18 . C19 . C20 . 121.9(13) yes C18 . C19 . H22 . 119.3 no C20 . C19 . H22 . 118.9 no C15 . C20 . C19 . 118.7(12) yes C15 . C20 . H21 . 120.6 no C19 . C20 . H21 . 120.7 no C17 . C24 . N25 . 114.7(11) yes C17 . C24 . H37 . 122.9 no N25 . C24 . H37 . 122.4 no Fe1 . N25 . C24 . 114.6(8) yes Fe1 . N25 . C26 . 126.3(7) yes C24 . N25 . C26 . 118.5(10) yes N25 . C26 . C27 . 120.4(10) yes N25 . C26 . C31 . 116.5(10) yes C27 . C26 . C31 . 123.0(11) yes C26 . C27 . C28 . 118.3(12) yes C26 . C27 . H36 . 121.2 no C28 . C27 . H36 . 120.4 no C27 . C28 . C29 . 121.2(14) yes C27 . C28 . H35 . 119.2 no C29 . C28 . H35 . 119.6 no C28 . C29 . C30 . 119.6(14) yes C28 . C29 . H34 . 120.2 no C30 . C29 . H34 . 120.2 no C29 . C30 . C31 . 121.3(14) yes C29 . C30 . H33 . 119.3 no C31 . C30 . H33 . 119.4 no C30 . C31 . C26 . 116.5(12) yes C30 . C31 . H32 . 121.6 no C26 . C31 . H32 . 121.9 no Fe1 . N39 . C40 . 124.9(7) yes Fe1 . N39 . C51 . 113.9(8) yes C40 . N39 . C51 . 120.6(10) yes N39 . C40 . C41 . 118.8(11) yes N39 . C40 . C45 . 117.1(11) yes C41 . C40 . C45 . 124.0(12) yes C40 . C41 . C42 . 119.0(13) yes C40 . C41 . H50 . 120.8 no C42 . C41 . H50 . 120.2 no C41 . C42 . C43 . 119.1(14) yes C41 . C42 . H49 . 121.0 no C43 . C42 . H49 . 119.9 no C42 . C43 . C44 . 119.5(13) yes C42 . C43 . H48 . 120.2 no C44 . C43 . H48 . 120.0 no C43 . C44 . C45 . 121.7(13) yes C43 . C44 . H47 . 119.7 no C45 . C44 . H47 . 118.5 no C44 . C45 . C40 . 116.6(12) yes C44 . C45 . H46 . 121.9 no C40 . C45 . H46 . 121.5 no N39 . C51 . C52 . 116.3(11) yes N39 . C51 . H75 . 121.5 no C52 . C51 . H75 . 122.2 no C51 . C52 . N53 . 111.5(10) yes C51 . C52 . C71 . 129.8(11) yes N53 . C52 . C71 . 118.7(10) yes C52 . N53 . Fe1 . 116.5(8) yes C52 . N53 . C54 . 122.1(9) yes Fe1 . N53 . C54 . 120.7(8) yes N53 . C54 . C55 . 110.4(10) yes N53 . C54 . C69 . 121.3(11) yes C55 . C54 . C69 . 128.3(11) yes C54 . C55 . N56 . 115.8(11) yes C54 . C55 . H68 . 122.1 no N56 . C55 . H68 . 122.1 no Fe1 . N56 . C55 . 114.0(8) yes Fe1 . N56 . C57 . 126.0(7) yes C55 . N56 . C57 . 119.1(10) yes N56 . C57 . C58 . 120.7(11) yes N56 . C57 . C62 . 121.7(11) yes C58 . C57 . C62 . 117.5(11) yes C57 . C58 . C59 . 121.0(13) yes C57 . C58 . H67 . 119.5 no C59 . C58 . H67 . 119.4 no C58 . C59 . C60 . 118.7(13) yes C58 . C59 . H66 . 120.4 no C60 . C59 . H66 . 120.9 no C59 . C60 . C61 . 122.7(13) yes C59 . C60 . H65 . 119.0 no C61 . C60 . H65 . 118.3 no C60 . C61 . C62 . 117.0(12) yes C60 . C61 . H64 . 121.3 no C62 . C61 . H64 . 121.7 no C61 . C62 . C57 . 123.1(12) yes C61 . C62 . H63 . 118.3 no C57 . C62 . H63 . 118.5 no C54 . C69 . C70 . 118.8(12) yes C54 . C69 . H74 . 120.5 no C70 . C69 . H74 . 120.7 no C69 . C70 . C71 . 118.7(12) yes C69 . C70 . H73 . 120.4 no C71 . C70 . H73 . 120.8 no C70 . C71 . C52 . 120.3(12) yes C70 . C71 . H72 . 120.3 no C52 . C71 . H72 . 119.3 no N77 . Fe76 . N84 . 79.7(4) yes N77 . Fe76 . N101 . 79.0(4) yes N84 . Fe76 . N101 . 158.7(4) yes N77 . Fe76 . N114 . 174.9(4) yes N84 . Fe76 . N114 . 95.9(4) yes N101 . Fe76 . N114 . 105.4(4) yes N77 . Fe76 . N121 . 98.2(4) yes N84 . Fe76 . N121 . 86.4(4) yes N101 . Fe76 . N121 . 97.9(4) yes N114 . Fe76 . N121 . 78.9(4) yes N77 . Fe76 . N138 . 102.6(4) yes N84 . Fe76 . N138 . 98.0(4) yes N101 . Fe76 . N138 . 85.3(4) yes N114 . Fe76 . N138 . 80.4(4) yes N121 . Fe76 . N138 . 159.2(4) yes Fe76 . N77 . C78 . 120.5(8) yes Fe76 . N77 . C82 . 118.0(7) yes C78 . N77 . C82 . 121.5(10) yes N77 . C78 . C79 . 119.9(11) yes N77 . C78 . C100 . 110.6(10) yes C79 . C78 . C100 . 129.4(12) yes C78 . C79 . C80 . 120.5(12) yes C78 . C79 . H99 . 119.3 no C80 . C79 . H99 . 120.2 no C79 . C80 . C81 . 118.3(12) yes C79 . C80 . H98 . 121.0 no C81 . C80 . H98 . 120.8 no C80 . C81 . C82 . 119.0(12) yes C80 . C81 . H97 . 120.9 no C82 . C81 . H97 . 120.0 no C81 . C82 . N77 . 120.7(11) yes C81 . C82 . C83 . 127.0(11) yes N77 . C82 . C83 . 112.1(10) yes C82 . C83 . N84 . 114.1(11) yes C82 . C83 . H96 . 123.2 no N84 . C83 . H96 . 122.7 no Fe76 . N84 . C83 . 115.4(8) yes Fe76 . N84 . C85 . 127.5(8) yes C83 . N84 . C85 . 116.6(10) yes N84 . C85 . C86 . 120.2(11) yes N84 . C85 . C90 . 121.1(11) yes C86 . C85 . C90 . 118.7(11) yes C85 . C86 . C87 . 121.6(12) yes C85 . C86 . H95 . 118.9 no C87 . C86 . H95 . 119.5 no C86 . C87 . C88 . 119.0(12) yes C86 . C87 . H94 . 120.2 no C88 . C87 . H94 . 120.9 no C87 . C88 . C89 . 122.4(13) yes C87 . C88 . H93 . 119.1 no C89 . C88 . H93 . 118.5 no C88 . C89 . C90 . 116.7(13) yes C88 . C89 . H92 . 122.0 no C90 . C89 . H92 . 121.3 no C89 . C90 . C85 . 121.7(12) yes C89 . C90 . H91 . 119.2 no C85 . C90 . H91 . 119.1 no C78 . C100 . N101 . 115.4(11) yes C78 . C100 . H113 . 121.9 no N101 . C100 . H113 . 122.7 no Fe76 . N101 . C100 . 114.2(8) yes Fe76 . N101 . C102 . 127.7(7) yes C100 . N101 . C102 . 117.7(10) yes N101 . C102 . C103 . 119.7(10) yes N101 . C102 . C107 . 119.4(10) yes C103 . C102 . C107 . 120.9(11) yes C102 . C103 . C104 . 120.1(11) yes C102 . C103 . H112 . 119.2 no C104 . C103 . H112 . 120.2 no C103 . C104 . C105 . 117.4(11) yes C103 . C104 . H111 . 121.3 no C105 . C104 . H111 . 121.2 no C104 . C105 . C106 . 121.6(12) yes C104 . C105 . H110 . 119.8 no C106 . C105 . H110 . 118.6 no C105 . C106 . C107 . 119.8(13) yes C105 . C106 . H109 . 120.3 no C107 . C106 . H109 . 119.8 no C102 . C107 . C106 . 120.1(12) yes C102 . C107 . H108 . 119.7 no C106 . C107 . H108 . 120.2 no Fe76 . N114 . C115 . 119.2(7) yes Fe76 . N114 . C119 . 119.6(7) yes C115 . N114 . C119 . 120.9(9) yes N114 . C115 . C116 . 120.5(10) yes N114 . C115 . C137 . 110.1(10) yes C116 . C115 . C137 . 129.3(11) yes C115 . C116 . C117 . 118.9(11) yes C115 . C116 . H136 . 120.7 no C117 . C116 . H136 . 120.4 no C116 . C117 . C118 . 119.5(12) yes C116 . C117 . H135 . 119.7 no C118 . C117 . H135 . 120.7 no C117 . C118 . C119 . 118.1(12) yes C117 . C118 . H134 . 120.7 no C119 . C118 . H134 . 121.1 no C118 . C119 . N114 . 121.9(11) yes C118 . C119 . C120 . 128.1(11) yes N114 . C119 . C120 . 110.0(10) yes C119 . C120 . N121 . 116.4(11) yes C119 . C120 . H133 . 120.7 no N121 . C120 . H133 . 122.9 no Fe76 . N121 . C120 . 113.9(8) yes Fe76 . N121 . C122 . 123.6(7) yes C120 . N121 . C122 . 122.4(10) yes N121 . C122 . C123 . 118.5(10) yes N121 . C122 . C127 . 121.5(10) yes C123 . C122 . C127 . 119.6(11) yes C122 . C123 . C124 . 119.4(11) yes C122 . C123 . H132 . 119.8 no C124 . C123 . H132 . 120.8 no C123 . C124 . C125 . 120.9(12) yes C123 . C124 . H131 . 119.4 no C125 . C124 . H131 . 119.7 no C124 . C125 . C126 . 118.0(12) yes C124 . C125 . H130 . 121.2 no C126 . C125 . H130 . 120.8 no C125 . C126 . C127 . 122.4(12) yes C125 . C126 . H129 . 119.1 no C127 . C126 . H129 . 118.5 no C122 . C127 . C126 . 119.7(12) yes C122 . C127 . H128 . 119.3 no C126 . C127 . H128 . 120.9 no C115 . C137 . N138 . 117.2(11) yes C115 . C137 . H150 . 121.8 no N138 . C137 . H150 . 121.0 no Fe76 . N138 . C137 . 112.7(8) yes Fe76 . N138 . C139 . 127.7(8) yes C137 . N138 . C139 . 118.6(10) yes N138 . C139 . C140 . 117.2(10) yes N138 . C139 . C144 . 122.6(10) yes C140 . C139 . C144 . 120.2(11) yes C139 . C140 . C141 . 120.1(11) yes C139 . C140 . H149 . 119.6 no C141 . C140 . H149 . 120.3 no C140 . C141 . C142 . 119.0(12) yes C140 . C141 . H148 . 120.8 no C142 . C141 . H148 . 120.2 no C141 . C142 . C143 . 121.5(13) yes C141 . C142 . H147 . 118.9 no C143 . C142 . H147 . 119.5 no C142 . C143 . C144 . 119.4(12) yes C142 . C143 . H146 . 120.4 no C144 . C143 . H146 . 120.1 no C143 . C144 . C139 . 119.7(11) yes C143 . C144 . H145 . 120.7 no C139 . C144 . H145 . 119.7 no F151 . B152 . F153 . 106.9(10) yes F151 . B152 . F154 . 109.5(11) yes F153 . B152 . F154 . 109.9(11) yes F151 . B152 . F155 . 107.9(11) yes F153 . B152 . F155 . 110.3(11) yes F154 . B152 . F155 . 112.2(12) yes F156 . B157 . F158 . 109.7(15) yes F156 . B157 . F159 . 103.8(15) yes F158 . B157 . F159 . 112.2(15) yes F156 . B157 . F160 . 110.4(15) yes F158 . B157 . F160 . 115.7(16) yes F159 . B157 . F160 . 104.3(15) yes F161 . B162 . F163 . 109.7(11) yes F161 . B162 . F164 . 108.2(11) yes F163 . B162 . F164 . 109.0(11) yes F161 . B162 . F165 . 110.2(11) yes F163 . B162 . F165 . 110.0(11) yes F164 . B162 . F165 . 109.8(11) yes F166 . B167 . F168 . 107.0(12) yes F166 . B167 . F169 . 111.3(14) yes F168 . B167 . F169 . 109.5(11) yes F166 . B167 . F170 . 111.3(12) yes F168 . B167 . F170 . 108.5(12) yes F169 . B167 . F170 . 109.0(11) yes H172 . O171 . H173 . 128.8 no N174 . C175 . C176 . 175.7(17) yes C175 . C176 . H177 . 109.5 no C175 . C176 . H178 . 109.8 no H177 . C176 . H178 . 109.5 no C175 . C176 . H179 . 109.0 no H177 . C176 . H179 . 109.5 no H178 . C176 . H179 . 109.5 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 C55 . H68 . O171 2_666 146 0.93 2.57 3.375(18) yes #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 695911' _montpellier_publication_code 42Zn2+ _montpellier_structure_analysis_code flo39 _montpellier_compound_description 'PDA-mF-Zn-Tf 2:1' _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; correct absolute structure assigned The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _cell_length_a 8.09170(10) _cell_length_b 14.7056(2) _cell_length_c 19.4187(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2310.70(6) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 2 21 21 ' _symmetry_space_group_name_Hall ? 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' 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' 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' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Zn 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097 1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 _chemical_formula_sum 'C44 H32 F10 N8 O6 S2 Zn ' _chemical_formula_moiety 'C38 H26 F4 N6 Zn, 2(C F3 O3 S), 2(C2 H3 N)' _chemical_compound_source ? _chemical_formula_weight 1088.31 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 175 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_max 0.25 _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.720 # Sheldrick geometric approximatio 0.90 0.93 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 0.93 _diffrn_measurement_device 'Oxford Diffraction XCALIBUR' _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 'Xcalibur, (Oxford Diffraction, 2002)' _computing_cell_refinement 'CrysAlis RED, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis RED, (Oxford Diffraction, 2002)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2006)' _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 173 _diffrn_reflns_number 23066 _reflns_number_total 5334 _diffrn_reflns_av_R_equivalents 0.031 # Number of reflections with Friedels Law is 3129 # Number of reflections without Friedels Law is 5334 # Theoretical number of reflections is about 2961 _diffrn_reflns_theta_min 3.744 _diffrn_reflns_theta_max 28.613 _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 26.038 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _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 -0.79 _refine_diff_density_max 0.67 # 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 4113 _refine_ls_number_restraints 0 _refine_ls_number_parameters 322 _oxford_refine_ls_R_factor_ref 0.0288 _refine_ls_wR_factor_ref 0.0350 _refine_ls_goodness_of_fit_ref 0.9201 _refine_ls_shift/su_max 0.000313 # The values computed from all data _oxford_reflns_number_all 5334 _refine_ls_R_factor_all 0.0401 _refine_ls_wR_factor_all 0.0387 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4113 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_gt 0.0350 _refine_ls_abs_structure_Flack 0.019(10) _refine_ls_abs_structure_details 'Flack (1983), 2205 Friedel-pairs' # 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 ad _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: 21.4 -16.6 16.8 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Palatinus, L. & Chapuis, G. (2006). Superflip - a computer program for solution of crystal structures by charge flipping in arbitrary dimensions. EPFL Lausanne, http://superspace.epfl.ch/superflip Flack, H. D. (1983). Acta Cryst. A39, 876-881. 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. Oxford Diffraction, (2002). CrysAlis RED. Oxford Diffraction, (2002). Xcalibur User Manual. 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 Zn1 Zn 0.49500(5) 0.5000 0.5000 0.0218 1.0000 Uani S T . . . . . N2 N 0.4981(3) 0.62482(10) 0.45278(8) 0.0223 1.0000 Uani . . . . . . . C3 C 0.4210(3) 0.63651(14) 0.39323(11) 0.0238 1.0000 Uani . . . . . . . C4 C 0.3328(3) 0.55563(15) 0.36750(11) 0.0262 1.0000 Uani . . . . . . . N5 N 0.3304(2) 0.48469(11) 0.40495(9) 0.0240 1.0000 Uani . . . . . . . C6 C 0.2548(3) 0.40446(15) 0.37857(12) 0.0249 1.0000 Uani . . . . . . . C7 C 0.1715(3) 0.34822(15) 0.42410(12) 0.0285 1.0000 Uani . . . . . . . C8 C 0.0911(3) 0.27134(17) 0.39995(14) 0.0336 1.0000 Uani . . . . . . . C9 C 0.0967(3) 0.24943(18) 0.33063(14) 0.0370 1.0000 Uani . . . . . . . C10 C 0.1851(4) 0.30467(18) 0.28747(13) 0.0394 1.0000 Uani . . . . . . . C11 C 0.2652(3) 0.38204(18) 0.30912(13) 0.0331 1.0000 Uani . . . . . . . C12 C 0.4262(3) 0.71905(16) 0.35762(13) 0.0314 1.0000 Uani . . . . . . . C13 C 0.5128(4) 0.79045(14) 0.38733(12) 0.0333 1.0000 Uani . . . . . . . C14 C 0.5926(3) 0.77793(15) 0.44994(13) 0.0304 1.0000 Uani . . . . . . . C15 C 0.5843(3) 0.69257(14) 0.48081(11) 0.0239 1.0000 Uani . . . . . . . C16 C 0.6727(3) 0.66745(14) 0.54451(11) 0.0260 1.0000 Uani . . . . . . . N17 N 0.6713(2) 0.58391(12) 0.56234(9) 0.0239 1.0000 Uani . . . . . . . C18 C 0.7491(3) 0.55679(15) 0.62437(12) 0.0244 1.0000 Uani . . . . . . . C19 C 0.8301(3) 0.47321(15) 0.62528(12) 0.0274 1.0000 Uani . . . . . . . C20 C 0.9081(3) 0.44445(16) 0.68547(13) 0.0316 1.0000 Uani . . . . . . . C21 C 0.9027(3) 0.4965(2) 0.74404(11) 0.0349 1.0000 Uani . . . . . . . C22 C 0.8179(4) 0.57772(18) 0.74155(12) 0.0381 1.0000 Uani . . . . . . . C23 C 0.7415(3) 0.61040(18) 0.68353(13) 0.0320 1.0000 Uani . . . . . . . C24 C 0.4842(5) 0.8980(3) 0.6281(3) 0.0940 1.0000 Uani . . . . . . . S25 S 0.69861(8) 0.91712(4) 0.64598(3) 0.0333 1.0000 Uani . . . . . . . O26 O 0.7804(3) 0.88424(14) 0.58564(10) 0.0418 1.0000 Uani . . . . . . . O27 O 0.7056(3) 1.01218(16) 0.65779(15) 0.0674 1.0000 Uani . . . . . . . O28 O 0.7350(4) 0.8663(2) 0.70647(13) 0.0818 1.0000 Uani . . . . . . . F29 F 0.3916(4) 0.9207(3) 0.6807(3) 0.1733 1.0000 Uani . . . . . . . F30 F 0.4343(5) 0.9412(4) 0.5754(3) 0.1841 1.0000 Uani . . . . . . . F31 F 0.4600(3) 0.8092(2) 0.6155(2) 0.1494 1.0000 Uani . . . . . . . C32 C 0.0244(4) 0.2010(2) 0.57053(14) 0.0432 1.0000 Uani . . . . . . . N33 N 0.0274(4) 0.27668(19) 0.57701(14) 0.0575 1.0000 Uani . . . . . . . C34 C 0.0156(6) 0.1033(2) 0.56107(18) 0.0672 1.0000 Uani . . . . . . . H41 H 0.2739 0.5580 0.3264 0.0323 1.0000 Uiso R . . . . . . H71 H 0.1656 0.3618 0.4718 0.0342 1.0000 Uiso R . . . . . . H91 H 0.0447 0.1967 0.3152 0.0450 1.0000 Uiso R . . . . . . H111 H 0.3214 0.4186 0.2774 0.0527 1.0000 Uiso R . . . . . . H121 H 0.3739 0.7253 0.3163 0.0414 1.0000 Uiso R . . . . . . H131 H 0.5232 0.8475 0.3651 0.0421 1.0000 Uiso R . . . . . . H141 H 0.6540 0.8237 0.4712 0.0375 1.0000 Uiso R . . . . . . H161 H 0.7270 0.7108 0.5704 0.0341 1.0000 Uiso R . . . . . . H191 H 0.8362 0.4388 0.5851 0.0372 1.0000 Uiso R . . . . . . H211 H 0.9487 0.4769 0.7854 0.0488 1.0000 Uiso R . . . . . . H231 H 0.6840 0.6671 0.6840 0.0345 1.0000 Uiso R . . . . . . H341 H 0.0853 0.0693 0.5918 0.0717 1.0000 Uiso R . . . . . . H342 H -0.0944 0.0842 0.5688 0.0717 1.0000 Uiso R . . . . . . H343 H 0.0448 0.0872 0.5153 0.0717 1.0000 Uiso R . . . . . . F1 F 0.1926(3) 0.28247(13) 0.22013(9) 0.0652 1.0000 Uani . . . . . . . F2 F 0.8090(3) 0.62891(14) 0.79937(9) 0.0662 1.0000 Uani . . . . . . . H81 H 0.0303 0.2355 0.4303 0.0410 1.0000 Uiso R . . . . . . H201 H 0.9636 0.3880 0.6854 0.0381 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 Zn1 0.03040(16) 0.01557(12) 0.01934(13) 0.00198(13) 0.0000 0.0000 N2 0.0274(8) 0.0179(7) 0.0217(7) 0.0021(6) 0.0010(9) -0.0001(9) C3 0.0292(10) 0.0215(10) 0.0208(10) 0.0038(8) -0.0005(8) 0.0007(8) C4 0.0319(12) 0.0257(11) 0.0209(10) 0.0006(8) -0.0060(8) -0.0002(8) N5 0.0272(8) 0.0232(10) 0.0216(8) 0.0023(7) -0.0032(7) -0.0012(7) C6 0.0254(10) 0.0202(10) 0.0290(11) 0.0007(8) -0.0047(8) 0.0014(8) C7 0.0310(12) 0.0252(10) 0.0292(11) 0.0032(9) -0.0012(9) -0.0026(9) C8 0.0311(12) 0.0275(11) 0.0423(14) 0.0053(10) -0.0020(11) -0.0053(10) C9 0.0389(14) 0.0279(12) 0.0441(15) -0.0018(10) -0.0098(11) -0.0074(10) C10 0.0554(16) 0.0349(13) 0.0281(12) -0.0066(10) -0.0072(12) -0.0056(12) C11 0.0432(14) 0.0294(12) 0.0267(12) 0.0008(10) -0.0027(10) -0.0043(10) C12 0.0424(13) 0.0244(11) 0.0275(11) 0.0067(9) -0.0053(10) 0.0018(10) C13 0.0466(14) 0.0169(9) 0.0363(11) 0.0081(8) 0.0039(12) -0.0019(11) C14 0.0359(12) 0.0189(10) 0.0364(12) -0.0010(9) 0.0016(10) -0.0043(9) C15 0.0299(11) 0.0185(9) 0.0232(10) -0.0013(7) 0.0008(8) -0.0003(8) C16 0.0321(12) 0.0205(9) 0.0253(10) -0.0031(8) -0.0015(9) -0.0034(8) N17 0.0284(9) 0.0215(8) 0.0218(8) -0.0021(7) -0.0010(7) 0.0001(8) C18 0.0254(10) 0.0224(11) 0.0254(10) 0.0017(8) -0.0017(8) -0.0020(8) C19 0.0315(12) 0.0228(10) 0.0277(10) -0.0009(8) -0.0031(9) -0.0017(8) C20 0.0290(12) 0.0276(12) 0.0381(13) 0.0014(9) -0.0039(10) 0.0015(9) C21 0.0369(12) 0.0388(12) 0.0292(10) 0.0059(13) -0.0095(9) 0.0015(13) C22 0.0500(14) 0.0370(13) 0.0274(11) -0.0067(10) -0.0104(11) 0.0062(12) C23 0.0394(14) 0.0280(12) 0.0286(13) -0.0030(9) -0.0071(10) 0.0056(10) C24 0.0333(17) 0.106(3) 0.143(4) -0.078(3) 0.013(3) 0.000(2) S25 0.0392(3) 0.0307(3) 0.0300(3) -0.0049(2) 0.0013(2) 0.0055(3) O26 0.0449(11) 0.0454(10) 0.0351(10) -0.0060(8) 0.0088(8) -0.0035(9) O27 0.0717(15) 0.0406(13) 0.0899(18) -0.0251(12) -0.0006(14) -0.0036(12) O28 0.115(3) 0.088(2) 0.0426(13) 0.0155(13) 0.0100(14) 0.0340(18) F29 0.0602(16) 0.212(4) 0.247(5) -0.150(4) 0.075(2) -0.021(2) F30 0.102(3) 0.262(6) 0.188(4) -0.073(4) -0.093(3) 0.090(3) F31 0.0723(19) 0.129(3) 0.247(5) -0.125(3) 0.073(2) -0.0596(18) C32 0.0482(17) 0.0514(16) 0.0301(11) 0.0035(11) -0.0008(11) -0.0024(13) N33 0.082(2) 0.0475(14) 0.0432(14) -0.0031(11) 0.0140(15) -0.0014(15) C34 0.102(3) 0.0450(16) 0.0550(18) 0.0062(13) -0.034(2) -0.010(2) F1 0.1094(16) 0.0548(11) 0.0314(9) -0.0142(8) -0.0039(10) -0.0287(12) F2 0.1035(16) 0.0630(11) 0.0323(9) -0.0198(8) -0.0243(10) 0.0333(12) _refine_ls_extinction_method None _oxford_refine_ls_scale 3.994(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 Zn1 . N5 2_566 2.2870(17) yes Zn1 . N17 2_566 2.2414(18) yes Zn1 . N2 2_566 2.0520(15) yes Zn1 . N2 . 2.0520(15) yes Zn1 . N5 . 2.2870(17) yes Zn1 . N17 . 2.2414(18) yes N2 . C3 . 1.325(3) yes N2 . C15 . 1.333(3) yes C3 . C4 . 1.474(3) yes C3 . C12 . 1.397(3) yes C4 . N5 . 1.272(3) yes C4 . H41 . 0.931 no N5 . C6 . 1.425(3) yes C6 . C7 . 1.385(3) yes C6 . C11 . 1.391(3) yes C7 . C8 . 1.386(3) yes C7 . H71 . 0.949 no C8 . C9 . 1.385(4) yes C8 . H81 . 0.931 no C9 . C10 . 1.369(4) yes C9 . H91 . 0.931 no C10 . C11 . 1.375(4) yes C10 . F1 . 1.349(3) yes C11 . H111 . 0.937 no C12 . C13 . 1.388(4) yes C12 . H121 . 0.912 no C13 . C14 . 1.389(4) yes C13 . H131 . 0.946 no C14 . C15 . 1.393(3) yes C14 . H141 . 0.933 no C15 . C16 . 1.476(3) yes C16 . N17 . 1.276(3) yes C16 . H161 . 0.922 no N17 . C18 . 1.416(3) yes C18 . C19 . 1.393(3) yes C18 . C23 . 1.395(3) yes C19 . C20 . 1.394(3) yes C19 . H191 . 0.931 no C20 . C21 . 1.372(4) yes C20 . H201 . 0.944 no C21 . C22 . 1.378(4) yes C21 . H211 . 0.930 no C22 . C23 . 1.372(4) yes C22 . F2 . 1.354(3) yes C23 . H231 . 0.955 no C24 . S25 . 1.792(4) yes C24 . F29 . 1.310(5) yes C24 . F30 . 1.269(8) yes C24 . F31 . 1.343(5) yes S25 . O26 . 1.4298(19) yes S25 . O27 . 1.418(2) yes S25 . O28 . 1.423(3) yes C32 . N33 . 1.120(4) yes C32 . C34 . 1.450(4) yes C34 . H341 . 0.961 no C34 . H342 . 0.945 no C34 . H343 . 0.951 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 N5 2_566 Zn1 . N17 2_566 149.40(6) yes N5 2_566 Zn1 . N2 2_566 74.60(7) yes N17 2_566 Zn1 . N2 2_566 75.00(7) yes N5 2_566 Zn1 . N2 . 106.24(7) yes N17 2_566 Zn1 . N2 . 104.08(7) yes N2 2_566 Zn1 . N2 . 178.61(12) yes N5 2_566 Zn1 . N5 . 108.79(9) yes N17 2_566 Zn1 . N5 . 83.14(6) yes N2 2_566 Zn1 . N5 . 106.24(7) yes N2 . Zn1 . N5 . 74.60(7) yes N5 2_566 Zn1 . N17 . 83.14(6) yes N17 2_566 Zn1 . N17 . 100.92(9) yes N2 2_566 Zn1 . N17 . 104.08(7) yes N2 . Zn1 . N17 . 75.00(7) yes N5 . Zn1 . N17 . 149.40(6) yes Zn1 . N2 . C3 . 120.02(14) yes Zn1 . N2 . C15 . 119.51(14) yes C3 . N2 . C15 . 120.40(17) yes N2 . C3 . C4 . 114.76(18) yes N2 . C3 . C12 . 122.0(2) yes C4 . C3 . C12 . 123.2(2) yes C3 . C4 . N5 . 118.39(19) yes C3 . C4 . H41 . 120.6 no N5 . C4 . H41 . 120.9 no Zn1 . N5 . C4 . 111.83(14) yes Zn1 . N5 . C6 . 128.47(14) yes C4 . N5 . C6 . 118.70(18) yes N5 . C6 . C7 . 118.3(2) yes N5 . C6 . C11 . 121.3(2) yes C7 . C6 . C11 . 120.5(2) yes C6 . C7 . C8 . 119.9(2) yes C6 . C7 . H71 . 121.4 no C8 . C7 . H71 . 118.6 no C7 . C8 . C9 . 120.2(2) yes C7 . C8 . H81 . 119.7 no C9 . C8 . H81 . 120.1 no C8 . C9 . C10 . 118.3(2) yes C8 . C9 . H91 . 119.4 no C10 . C9 . H91 . 122.3 no C9 . C10 . C11 . 123.4(2) yes C9 . C10 . F1 . 118.3(2) yes C11 . C10 . F1 . 118.4(3) yes C6 . C11 . C10 . 117.6(2) yes C6 . C11 . H111 . 122.1 no C10 . C11 . H111 . 120.2 no C3 . C12 . C13 . 117.8(2) yes C3 . C12 . H121 . 120.6 no C13 . C12 . H121 . 121.6 no C12 . C13 . C14 . 119.9(2) yes C12 . C13 . H131 . 121.7 no C14 . C13 . H131 . 118.4 no C13 . C14 . C15 . 118.3(2) yes C13 . C14 . H141 . 122.7 no C15 . C14 . H141 . 119.0 no C14 . C15 . N2 . 121.5(2) yes C14 . C15 . C16 . 124.3(2) yes N2 . C15 . C16 . 114.14(18) yes C15 . C16 . N17 . 117.66(19) yes C15 . C16 . H161 . 120.9 no N17 . C16 . H161 . 121.4 no Zn1 . N17 . C16 . 112.87(15) yes Zn1 . N17 . C18 . 125.95(14) yes C16 . N17 . C18 . 119.87(19) yes N17 . C18 . C19 . 117.9(2) yes N17 . C18 . C23 . 121.5(2) yes C19 . C18 . C23 . 120.6(2) yes C18 . C19 . C20 . 119.4(2) yes C18 . C19 . H191 . 119.6 no C20 . C19 . H191 . 120.9 no C19 . C20 . C21 . 120.8(2) yes C19 . C20 . H201 . 118.8 no C21 . C20 . H201 . 120.5 no C20 . C21 . C22 . 118.1(2) yes C20 . C21 . H211 . 121.9 no C22 . C21 . H211 . 119.9 no C21 . C22 . C23 . 123.8(2) yes C21 . C22 . F2 . 118.6(2) yes C23 . C22 . F2 . 117.5(2) yes C18 . C23 . C22 . 117.3(2) yes C18 . C23 . H231 . 121.6 no C22 . C23 . H231 . 121.1 no S25 . C24 . F29 . 111.3(3) yes S25 . C24 . F30 . 112.7(4) yes F29 . C24 . F30 . 108.6(5) yes S25 . C24 . F31 . 109.2(3) yes F29 . C24 . F31 . 107.8(5) yes F30 . C24 . F31 . 107.1(5) yes C24 . S25 . O26 . 103.64(17) yes C24 . S25 . O27 . 102.99(19) yes O26 . S25 . O27 . 116.58(15) yes C24 . S25 . O28 . 106.2(3) yes O26 . S25 . O28 . 113.77(15) yes O27 . S25 . O28 . 112.09(18) yes N33 . C32 . C34 . 178.2(4) yes C32 . C34 . H341 . 114.1 no C32 . C34 . H342 . 108.7 no H341 . C34 . H342 . 107.4 no C32 . C34 . H343 . 110.7 no H341 . C34 . H343 . 107.7 no H342 . C34 . H343 . 108.0 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 C4 . H41 . O28 4_664 143 0.93 2.58 3.376(4) yes C11 . H111 . O27 4_664 142 0.94 2.54 3.333(4) yes C13 . H131 . O27 2_576 147 0.95 2.58 3.410(4) yes C34 . H342 . O27 1_445 145 0.94 2.59 3.408(4) yes #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 695912' _montpellier_publication_code 12Co2+ _montpellier_structure_analysis_code vdlee29 _montpellier_compound_description 'PDA-H-Co-BF4 2:1' _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; good data The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _cell_length_a 12.4612(5) _cell_length_b 15.4657(7) _cell_length_c 21.0453(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4055.9(3) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcb _symmetry_space_group_name_Hall '-P 2bc 2b' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,z x,-y+1/2,-z x,-y,z+1/2 -x,y,-z+1/2 -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 57.7997 0.0030 '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' F 0.0140 0.0100 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0000 0.0010 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Co 0.2990 0.9730 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692 1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C38 H30 B2 Co1 F8 N6 # Dc = 1.32 Fooo = 1804.00 Mu = 4.94 M = 401.62 # Found Formula = C44 H36 B2 Co1 F8 N6 # Dc = 1.44 FOOO = 1804.00 Mu = 5.01 M = 440.67 _chemical_formula_sum 'C44 H36 B2 Co1 F8 N6' _chemical_formula_moiety 'C38 H30 Co N6, C6 H6, 2(BF4)' _chemical_compound_source ? _chemical_formula_weight 881.35 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 175 _exptl_crystal_description prism _exptl_crystal_colour white _exptl_crystal_size_min 0.15 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_max 0.27 _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): 1806.33 _exptl_crystal_F_000 1804 _exptl_absorpt_coefficient_mu 0.501 # Sheldrick geometric approximatio 0.90 0.93 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 0.93 _diffrn_measurement_device 'Oxford Diffraction XCALIBUR' _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 'Xcalibur, (Oxford Diffraction, 2002)' _computing_cell_refinement 'CrysAlis RED, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis RED, (Oxford Diffraction, 2002)' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _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 173 _diffrn_reflns_number 78751 _reflns_number_total 6892 _diffrn_reflns_av_R_equivalents 0.051 # Number of reflections with Friedels Law is 6892 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 7221 _diffrn_reflns_theta_min 3.248 _diffrn_reflns_theta_max 32.409 _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 30.789 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _reflns_limit_h_min 0 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 31 _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 -0.44 _refine_diff_density_max 0.54 # 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>1.0\s(I) _refine_ls_number_reflns 3048 _refine_ls_number_restraints 8 _refine_ls_number_parameters 281 _oxford_refine_ls_R_factor_ref 0.0493 _refine_ls_wR_factor_ref 0.0417 _refine_ls_goodness_of_fit_ref 1.1007 _refine_ls_shift/su_max 0.000348 # The values computed from all data _oxford_reflns_number_all 6892 _refine_ls_R_factor_all 0.1626 _refine_ls_wR_factor_all 0.0506 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 1859 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_gt 0.0352 # 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: 5.58 -7.44 2.26 -0.311 -1.74 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 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. Oxford Diffraction, (2002). CrysAlis RED. Oxford Diffraction, (2002). Xcalibur User Manual. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Sheldrick, G. M. (2008). Acta Cryst A64, 112-122. 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 Co1 Co 0.16710(4) 0.7500 0.5000 0.0185 1.0000 Uani S T . . . . . N2 N 0.16507(17) 0.74270(16) 0.58910(8) 0.0212 1.0000 Uani . . . . . . . C3 C 0.0915(2) 0.69291(17) 0.61792(12) 0.0240 1.0000 Uani . . . . . . . C4 C 0.0881(3) 0.6855(2) 0.68356(13) 0.0339 1.0000 Uani . . . . . . . C5 C 0.1607(3) 0.73194(19) 0.71933(12) 0.0372 1.0000 Uani . . . . . . . C6 C 0.2352(2) 0.7845(2) 0.68972(13) 0.0346 1.0000 Uani . . . . . . . C7 C 0.2362(2) 0.78810(18) 0.62362(12) 0.0249 1.0000 Uani . . . . . . . C8 C 0.31078(19) 0.83730(17) 0.58421(11) 0.0234 1.0000 Uani . . . . . . . N9 N 0.29504(18) 0.83470(14) 0.52423(10) 0.0231 1.0000 Uani . . . . . . . C10 C 0.3705(2) 0.87304(17) 0.48180(12) 0.0260 1.0000 Uani . . . . . . . C11 C 0.4801(2) 0.8694(2) 0.49309(16) 0.0349 1.0000 Uani . . . . . . . C12 C 0.5511(2) 0.9040(2) 0.44946(16) 0.0428 1.0000 Uani . . . . . . . C13 C 0.5136(3) 0.9406(2) 0.39401(15) 0.0400 1.0000 Uani . . . . . . . C14 C 0.4048(3) 0.9435(2) 0.38217(15) 0.0409 1.0000 Uani . . . . . . . C15 C 0.3338(3) 0.90994(18) 0.42601(13) 0.0335 1.0000 Uani . . . . . . . H16 H 0.2605 0.9113 0.4183 0.0275 1.0000 Uiso R . . . . . . H17 H 0.3795 0.9669 0.3450 0.0382 1.0000 Uiso R . . . . . . H18 H 0.5630 0.9629 0.3636 0.0368 1.0000 Uiso R . . . . . . H19 H 0.6237 0.9021 0.4571 0.0401 1.0000 Uiso R . . . . . . H20 H 0.5067 0.8426 0.5299 0.0301 1.0000 Uiso R . . . . . . H21 H 0.3675 0.8682 0.6025 0.0331 1.0000 Uiso R . . . . . . H22 H 0.2828 0.8168 0.7128 0.0312 1.0000 Uiso R . . . . . . H23 H 0.1582 0.7272 0.7638 0.0337 1.0000 Uiso R . . . . . . H24 H 0.0402 0.6481 0.7026 0.0331 1.0000 Uiso R . . . . . . C25 C 0.0206(2) 0.64910(17) 0.57295(12) 0.0260 1.0000 Uani . . . . . . . N26 N 0.04225(18) 0.66028(15) 0.51370(9) 0.0244 1.0000 Uani . . . . . . . C27 C -0.0304(2) 0.62914(19) 0.46628(12) 0.0279 1.0000 Uani . . . . . . . C28 C 0.0114(2) 0.59242(17) 0.41119(12) 0.0290 1.0000 Uani . . . . . . . C29 C -0.0573(3) 0.5685(2) 0.36261(14) 0.0383 1.0000 Uani . . . . . . . C30 C -0.1659(3) 0.5824(3) 0.36806(18) 0.0574 1.0000 Uani . . . . . . . C31 C -0.2070(3) 0.6177(4) 0.4223(2) 0.0757 1.0000 Uani . . . . . . . C32 C -0.1410(3) 0.6407(3) 0.47265(18) 0.0571 1.0000 Uani . . . . . . . H33 H -0.1695 0.6645 0.5099 0.0509 1.0000 Uiso R . . . . . . H34 H -0.2814 0.6265 0.4258 0.0695 1.0000 Uiso R . . . . . . H35 H -0.2117 0.5676 0.3350 0.0569 1.0000 Uiso R . . . . . . H36 H -0.0290 0.5420 0.3257 0.0558 1.0000 Uiso R . . . . . . H37 H 0.0854 0.5857 0.4071 0.0462 1.0000 Uiso R . . . . . . H38 H -0.0363 0.6145 0.5860 0.0534 1.0000 Uiso R . . . . . . F39 F 0.70355(19) 0.5577(2) 0.72750(12) 0.0760 1.0000 Uani . . . . . . . B40 B 0.7818(3) 0.5527(3) 0.6832(2) 0.0421 1.0000 Uani . . . . . . . F41 F 0.88141(18) 0.54772(19) 0.70845(14) 0.0848 1.0000 Uani . . . . . . . F42 F 0.76225(19) 0.48909(18) 0.63982(16) 0.0925 1.0000 Uani . . . . . . . F43 F 0.7786(3) 0.63098(19) 0.64968(14) 0.0921 1.0000 Uani . . . . . . . C44 C 0.500000(7) 0.6076(3) 0.250000(7) 0.0385 1.0000 Uani S T . . . . . C45 C 0.5431(2) 0.6522(2) 0.30092(15) 0.0388 1.0000 Uani . . . . . . . C46 C 0.5435(3) 0.7418(2) 0.30059(16) 0.0460 1.0000 Uani . . . . . . . C47 C 0.500000(7) 0.7865(3) 0.250000(7) 0.0534 1.0000 Uani S T . . . . . H49 H 0.5737 0.7720 0.3348 0.0548 1.0000 Uiso R . . . . . . H50 H 0.5742 0.6231 0.3353 0.0463 1.0000 Uiso R . . . . . . H471 H 0.5000 0.8460 0.2500 0.0636 1.0000 Uiso RS . . . . . . H441 H 0.5000 0.5482 0.2500 0.0461 1.0000 Uiso RS . . . . . . 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 Co1 0.01600(16) 0.02122(18) 0.01841(17) 0.0019(3) 0.0000 0.0000 N2 0.0199(7) 0.0229(10) 0.0206(7) 0.0018(9) -0.0005(8) 0.0017(11) C3 0.0261(12) 0.0251(12) 0.0208(11) 0.0020(9) 0.0022(9) 0.0011(10) C4 0.0379(16) 0.0390(16) 0.0248(13) 0.0071(11) 0.0077(12) -0.0037(13) C5 0.0463(16) 0.048(2) 0.0170(10) 0.0057(10) 0.0010(12) -0.0026(15) C6 0.0359(15) 0.0448(16) 0.0231(13) -0.0005(12) -0.0071(11) -0.0001(13) C7 0.0220(12) 0.0293(13) 0.0234(12) -0.0002(10) -0.0028(9) 0.0019(11) C8 0.0217(13) 0.0270(12) 0.0214(11) -0.0037(10) -0.0040(9) 0.0014(9) N9 0.0249(10) 0.0237(11) 0.0207(9) 0.0009(8) 0.0003(8) 0.0017(9) C10 0.0293(12) 0.0211(12) 0.0275(12) -0.0045(9) 0.0033(10) -0.0044(11) C11 0.0279(13) 0.0437(15) 0.0332(16) 0.0033(14) 0.0033(13) 0.0025(11) C12 0.0280(14) 0.0504(19) 0.0501(19) 0.0024(16) 0.0135(14) 0.0039(14) C13 0.0443(18) 0.0342(15) 0.0415(17) 0.0010(13) 0.0153(14) -0.0082(14) C14 0.057(2) 0.0336(16) 0.0318(15) 0.0071(12) -0.0015(14) -0.0157(15) C15 0.0381(14) 0.0314(14) 0.0310(13) 0.0045(11) -0.0047(14) -0.0097(14) C25 0.0246(13) 0.0249(13) 0.0285(12) 0.0025(10) 0.0069(10) -0.0015(10) N26 0.0238(10) 0.0260(11) 0.0236(12) 0.0007(8) 0.0032(7) 0.0012(9) C27 0.0247(13) 0.0313(14) 0.0276(14) -0.0042(10) 0.0004(10) -0.0009(11) C28 0.0311(14) 0.0271(14) 0.0289(13) -0.0018(11) 0.0057(11) -0.0046(11) C29 0.0450(17) 0.0374(16) 0.0326(15) -0.0073(12) 0.0022(13) -0.0100(14) C30 0.0448(18) 0.078(3) 0.0491(19) -0.0244(19) -0.0151(18) -0.003(2) C31 0.0262(16) 0.129(5) 0.072(3) -0.044(3) -0.0126(18) 0.007(2) C32 0.0302(16) 0.093(3) 0.0482(19) -0.036(2) -0.0062(14) 0.0108(19) F39 0.0495(12) 0.115(2) 0.0630(14) 0.0008(14) 0.0170(11) -0.0125(14) B40 0.0297(17) 0.044(2) 0.052(2) -0.0151(17) 0.0015(15) -0.0040(15) F41 0.0372(12) 0.103(2) 0.115(2) -0.0579(17) -0.0185(13) 0.0111(13) F42 0.0562(14) 0.0795(18) 0.142(3) -0.0766(19) -0.0258(15) 0.0127(13) F43 0.131(3) 0.0729(18) 0.0728(17) 0.0017(15) 0.0039(18) -0.0284(18) C44 0.040(2) 0.0237(19) 0.052(2) 0.0000 0.005(2) 0.0000 C45 0.0371(15) 0.0407(17) 0.0386(16) 0.0019(13) 0.0033(13) 0.0036(14) C46 0.0583(19) 0.0347(18) 0.0451(16) -0.0091(15) 0.0039(14) -0.0071(17) C47 0.071(4) 0.027(2) 0.062(3) 0.0000 0.012(3) 0.0000 _refine_ls_extinction_method None _oxford_refine_ls_scale 0.9913(15) 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 Co1 . N9 4_566 2.125(2) yes Co1 . N26 4_566 2.105(2) yes Co1 . N2 4_566 1.8787(17) yes Co1 . N2 . 1.8787(17) yes Co1 . N9 . 2.125(2) yes Co1 . N26 . 2.105(2) yes N2 . C3 . 1.342(3) yes N2 . C7 . 1.344(3) yes C3 . C4 . 1.387(4) yes C3 . C25 . 1.462(4) yes C4 . C5 . 1.379(4) yes C4 . H24 . 0.922 no C5 . C6 . 1.383(4) yes C5 . H23 . 0.939 no C6 . C7 . 1.392(3) yes C6 . H22 . 0.914 no C7 . C8 . 1.460(4) yes C8 . N9 . 1.278(3) yes C8 . H21 . 0.937 no N9 . C10 . 1.426(3) yes C10 . C11 . 1.388(4) yes C10 . C15 . 1.383(4) yes C11 . C12 . 1.382(4) yes C11 . H20 . 0.939 no C12 . C13 . 1.379(5) yes C12 . H19 . 0.919 no C13 . C14 . 1.379(5) yes C13 . H18 . 0.953 no C14 . C15 . 1.380(4) yes C14 . H17 . 0.917 no C15 . H16 . 0.928 no C25 . N26 . 1.288(3) yes C25 . H38 . 0.930 no N26 . C27 . 1.431(3) yes C27 . C28 . 1.392(4) yes C27 . C32 . 1.396(4) yes C28 . C29 . 1.384(4) yes C28 . H37 . 0.931 no C29 . C30 . 1.375(5) yes C29 . H36 . 0.946 no C30 . C31 . 1.365(5) yes C30 . H35 . 0.928 no C31 . C32 . 1.387(5) yes C31 . H34 . 0.941 no C32 . H33 . 0.936 no F39 . B40 . 1.351(4) yes B40 . F41 . 1.352(4) yes B40 . F42 . 1.364(4) yes B40 . F43 . 1.402(5) yes C44 . C45 6_655 1.383(4) yes C44 . C45 . 1.383(4) yes C44 . H441 . 0.918 no C45 . C46 . 1.387(5) yes C45 . H50 . 0.935 no C46 . C47 . 1.380(4) yes C46 . H49 . 0.936 no C47 . H471 . 0.921 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 N9 4_566 Co1 . N26 4_566 158.12(8) yes N9 4_566 Co1 . N2 4_566 78.91(9) yes N26 4_566 Co1 . N2 4_566 79.26(9) yes N9 4_566 Co1 . N2 . 102.27(9) yes N26 4_566 Co1 . N2 . 99.58(9) yes N2 4_566 Co1 . N2 . 178.45(13) yes N9 4_566 Co1 . N9 . 82.80(12) yes N26 4_566 Co1 . N9 . 100.43(8) yes N2 4_566 Co1 . N9 . 102.27(9) yes N2 . Co1 . N9 . 78.91(9) yes N9 4_566 Co1 . N26 . 100.43(8) yes N26 4_566 Co1 . N26 . 84.66(12) yes N2 4_566 Co1 . N26 . 99.58(9) yes N2 . Co1 . N26 . 79.26(9) yes N9 . Co1 . N26 . 158.12(8) yes Co1 . N2 . C3 . 119.65(17) yes Co1 . N2 . C7 . 119.95(18) yes C3 . N2 . C7 . 120.4(2) yes N2 . C3 . C4 . 121.3(3) yes N2 . C3 . C25 . 112.7(2) yes C4 . C3 . C25 . 126.0(3) yes C3 . C4 . C5 . 118.7(3) yes C3 . C4 . H24 . 120.4 no C5 . C4 . H24 . 120.9 no C4 . C5 . C6 . 120.1(2) yes C4 . C5 . H23 . 118.8 no C6 . C5 . H23 . 121.1 no C5 . C6 . C7 . 118.7(3) yes C5 . C6 . H22 . 121.1 no C7 . C6 . H22 . 120.2 no C6 . C7 . N2 . 120.9(3) yes C6 . C7 . C8 . 126.5(3) yes N2 . C7 . C8 . 112.6(2) yes C7 . C8 . N9 . 116.6(2) yes C7 . C8 . H21 . 120.9 no N9 . C8 . H21 . 122.6 no Co1 . N9 . C8 . 111.80(18) yes Co1 . N9 . C10 . 126.91(17) yes C8 . N9 . C10 . 120.3(2) yes N9 . C10 . C11 . 121.7(3) yes N9 . C10 . C15 . 119.1(3) yes C11 . C10 . C15 . 119.2(3) yes C10 . C11 . C12 . 120.0(3) yes C10 . C11 . H20 . 120.4 no C12 . C11 . H20 . 119.5 no C11 . C12 . C13 . 120.3(3) yes C11 . C12 . H19 . 120.0 no C13 . C12 . H19 . 119.7 no C12 . C13 . C14 . 120.0(3) yes C12 . C13 . H18 . 119.9 no C14 . C13 . H18 . 120.1 no C13 . C14 . C15 . 119.8(3) yes C13 . C14 . H17 . 120.3 no C15 . C14 . H17 . 119.9 no C10 . C15 . C14 . 120.7(3) yes C10 . C15 . H16 . 118.9 no C14 . C15 . H16 . 120.4 no C3 . C25 . N26 . 116.0(2) yes C3 . C25 . H38 . 122.5 no N26 . C25 . H38 . 121.6 no Co1 . N26 . C25 . 112.12(18) yes Co1 . N26 . C27 . 126.45(17) yes C25 . N26 . C27 . 119.8(2) yes N26 . C27 . C28 . 118.8(2) yes N26 . C27 . C32 . 121.0(3) yes C28 . C27 . C32 . 120.1(3) yes C27 . C28 . C29 . 119.5(3) yes C27 . C28 . H37 . 119.5 no C29 . C28 . H37 . 121.0 no C28 . C29 . C30 . 120.4(3) yes C28 . C29 . H36 . 119.5 no C30 . C29 . H36 . 120.2 no C29 . C30 . C31 . 120.1(3) yes C29 . C30 . H35 . 120.2 no C31 . C30 . H35 . 119.7 no C30 . C31 . C32 . 121.3(3) yes C30 . C31 . H34 . 119.5 no C32 . C31 . H34 . 119.2 no C27 . C32 . C31 . 118.6(3) yes C27 . C32 . H33 . 120.3 no C31 . C32 . H33 . 121.1 no F39 . B40 . F41 . 113.2(3) yes F39 . B40 . F42 . 112.0(3) yes F41 . B40 . F42 . 112.7(3) yes F39 . B40 . F43 . 106.1(3) yes F41 . B40 . F43 . 105.8(3) yes F42 . B40 . F43 . 106.3(3) yes C45 6_655 C44 . C45 . 120.2(4) yes C45 6_655 C44 . H441 . 119.9 no C45 . C44 . H441 . 119.9 no C44 . C45 . C46 . 119.7(3) yes C44 . C45 . H50 . 121.4 no C46 . C45 . H50 . 118.9 no C45 . C46 . C47 . 120.2(3) yes C45 . C46 . H49 . 119.7 no C47 . C46 . H49 . 120.1 no C46 . C47 . C46 6_655 119.9(5) yes C46 . C47 . H471 . 120.0 no C46 6_655 C47 . H471 . 120.0 no #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 695913' _audit_creation_date 04-08-19 _audit_creation_method CRYSTALS_ver_12.39 _montpellier_publication_code 22Zn2+ _montpellier_structure_analysis_code vdlee46 _montpellier_compound_description 'PDA-OH-Zn-Tf 2:1' _oxford_structure_analysis_title vdlee46 _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 25.526(2) _cell_length_b 8.2795(5) _cell_length_c 23.826(2) _cell_angle_alpha 90 _cell_angle_beta 113.137(6) _cell_angle_gamma 90 _cell_volume 4630.4(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' 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' 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' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Zn 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097 1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C40 H30 F6 N6 O10 S2 Zn1 # Dc = 1.43 Fooo = 2204.00 Mu = 7.04 M = 998.21 # Found Formula = C44 H35 F6 N8 O10 S2 Zn1 # Dc = 1.55 FOOO = 2204.00 Mu = 7.12 M = 1079.31 _chemical_formula_sum 'C44 H36 F6 N8 O10 S2 Zn1' _chemical_formula_moiety 'C38 H30 N6 O4 Zn, 2(C F3 O3 S), 2(C2 H3 N)' _chemical_compound_source ? _chemical_formula_weight 1080.34 _cell_measurement_reflns_used 5087 _cell_measurement_theta_min 2 _cell_measurement_theta_max 20 _cell_measurement_temperature 120 _exptl_crystal_description prism _exptl_crystal_colour 'translucent light yellow' _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.48 _exptl_crystal_density_diffrn 1.548 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 2204 _exptl_absorpt_coefficient_mu 0.712 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.849 _exptl_absorpt_correction_T_max 0.961 _exptl_absorpt_process_details ; Absorption ans scaling correction was done using the abspack option in Crysalis RED (Oxford Diffraction, 2002) ; _diffrn_measurement_device_type 'Oxford Diffraction XCALIBUR' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'Xcalibur, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis RED, (Oxford Diffraction, 2002)' _computing_cell_refinement 'CrysAlis RED, (Oxford Diffraction, 2002)' _computing_structure_solution 'SIR2002 (Burla 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_number '4 frames' _diffrn_standards_interval_time 30 _diffrn_standards_decay_% 0.00 _diffrn_ambient_temperature 173 _diffrn_reflns_number 87879 _reflns_number_total 15280 _diffrn_reflns_av_R_equivalents 0.097 # Number of reflections with Friedels Law is 15280 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 12673 _diffrn_reflns_theta_min 2.536 _diffrn_reflns_theta_max 32.424 _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 30.479 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 34 _reflns_limit_h_min -38 _reflns_limit_h_max 35 _reflns_limit_k_min 0 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 35 _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 -0.45 _refine_diff_density_max 0.77 _refine_ls_number_reflns 2117 _refine_ls_number_restraints 0 _refine_ls_number_parameters 290 #_refine_ls_R_factor_ref 0.0486 _refine_ls_wR_factor_ref 0.0554 _refine_ls_goodness_of_fit_ref 1.1693 #_reflns_number_all 15252 _refine_ls_R_factor_all 0.2709 _refine_ls_wR_factor_all 0.0630 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>2.00u(I) _reflns_number_gt 2117 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_gt 0.0554 _refine_ls_shift/su_max 0.000125 # 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 noref # 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: 7.67 -6.62 5.36 ; _refine_special_details ; All atoms, except hydrogens, were refined isotropically in order to keep the data to parameter ratio reasonable. Not much data because of the crystal shape (thin platelet). Zn, however, was refined anisotropically. ; _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. M.C. Burla, M. Camalli, B. Carrozzini, G.L. Cascarano, C. Giacovazzo, G.Polidori, R.Spagna. J. Appl. Cryst. (2003). 36, 1103 Oxford Diffraction, (2002) CrysAlis RED. Oxford Diffraction, (2002) Xcalibur User Manual 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 atoms attached 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 _atom_site_attached_hydrogens Zn1 Zn 0.22187(5) 0.45246(17) 0.42611(6) 0.0220 1.0000 Uani . . . . . . N2 N 0.1714(3) 0.6495(10) 0.4488(4) 0.020(2) 1.0000 Uiso . . . . . . C3 C 0.1256(4) 0.7445(13) 0.4085(4) 0.021(2) 1.0000 Uiso . . . . . . C4 C 0.1287(4) 0.7976(14) 0.3552(5) 0.030(3) 1.0000 Uiso . . . . . . C5 C 0.0867(4) 0.8988(13) 0.3148(5) 0.028(3) 1.0000 Uiso . . . . . . C6 C 0.0411(4) 0.9413(15) 0.3297(5) 0.027(3) 1.0000 Uiso . . . . . . O7 O 0.0018(3) 1.0429(10) 0.2884(3) 0.0358(18) 1.0000 Uiso . . . . . . C8 C 0.0355(4) 0.8816(13) 0.3813(4) 0.021(2) 1.0000 Uiso . . . . . . C9 C 0.0775(4) 0.7842(13) 0.4201(4) 0.025(3) 1.0000 Uiso . . . . . . C10 C 0.1833(4) 0.6537(12) 0.5066(4) 0.021(2) 1.0000 Uiso . . . . . . C11 C 0.2289(4) 0.5476(14) 0.5471(4) 0.021(2) 1.0000 Uiso . . . . . . C12 C 0.2454(4) 0.5419(15) 0.6102(4) 0.025(2) 1.0000 Uiso . . . . . . C13 C 0.2871(4) 0.4354(16) 0.6436(5) 0.035(3) 1.0000 Uiso . . . . . . C14 C 0.3122(5) 0.3382(14) 0.6136(5) 0.032(3) 1.0000 Uiso . . . . . . C15 C 0.2939(4) 0.3505(13) 0.5511(5) 0.023(3) 1.0000 Uiso . . . . . . N16 N 0.2531(3) 0.4519(11) 0.5191(3) 0.0213(19) 1.0000 Uiso . . . . . . C17 C 0.3148(4) 0.2478(13) 0.5128(5) 0.022(2) 1.0000 Uiso . . . . . . N18 N 0.2868(3) 0.2478(10) 0.4552(4) 0.022(2) 1.0000 Uiso . . . . . . C19 C 0.3052(4) 0.1536(13) 0.4170(4) 0.020(2) 1.0000 Uiso . . . . . . C20 C 0.2629(4) 0.0871(13) 0.3645(5) 0.023(3) 1.0000 Uiso . . . . . . C21 C 0.2775(4) -0.0121(13) 0.3274(5) 0.026(3) 1.0000 Uiso . . . . . . C22 C 0.3350(4) -0.0394(14) 0.3402(4) 0.023(2) 1.0000 Uiso . . . . . . C23 C 0.3766(4) 0.0286(13) 0.3901(4) 0.021(2) 1.0000 Uiso . . . . . . C24 C 0.3626(4) 0.1254(13) 0.4288(5) 0.022(3) 1.0000 Uiso . . . . . . O25 O 0.3466(3) -0.1391(9) 0.2997(3) 0.0316(19) 1.0000 Uiso . . . . . . O26 O 0.4906(3) 0.8445(9) 0.5521(3) 0.036(2) 1.0000 Uiso . . . . . . C27 C 0.4391(4) 0.7739(13) 0.5159(5) 0.025(3) 1.0000 Uiso . . . . . . C28 C 0.4397(4) 0.6674(14) 0.4733(5) 0.029(3) 1.0000 Uiso . . . . . . C29 C 0.3887(4) 0.5991(13) 0.4341(5) 0.024(3) 1.0000 Uiso . . . . . . C30 C 0.3381(4) 0.6392(13) 0.4389(4) 0.019(2) 1.0000 Uiso . . . . . . C31 C 0.3385(4) 0.7421(13) 0.4850(4) 0.024(3) 1.0000 Uiso . . . . . . C32 C 0.3897(4) 0.8137(13) 0.5238(4) 0.022(2) 1.0000 Uiso . . . . . . N33 N 0.2841(3) 0.5769(10) 0.3984(4) 0.022(2) 1.0000 Uiso . . . . . . C34 C 0.2741(4) 0.5596(15) 0.3423(4) 0.024(2) 1.0000 Uiso . . . . . . C35 C 0.2206(4) 0.4846(13) 0.3031(5) 0.025(3) 1.0000 Uiso . . . . . . C36 C 0.2033(4) 0.4515(16) 0.2410(5) 0.029(3) 1.0000 Uiso . . . . . . C37 C 0.1512(5) 0.3788(15) 0.2104(6) 0.040(3) 1.0000 Uiso . . . . . . C38 C 0.1186(4) 0.3297(14) 0.2427(5) 0.028(3) 1.0000 Uiso . . . . . . C39 C 0.1390(4) 0.3628(13) 0.3047(5) 0.022(3) 1.0000 Uiso . . . . . . N40 N 0.1886(3) 0.4382(11) 0.3334(3) 0.023(2) 1.0000 Uiso . . . . . . C41 C 0.1128(4) 0.3041(14) 0.3456(5) 0.025(3) 1.0000 Uiso . . . . . . N42 N 0.1435(3) 0.3031(10) 0.4022(4) 0.021(2) 1.0000 Uiso . . . . . . C43 C 0.1238(4) 0.2385(15) 0.4456(5) 0.032(3) 1.0000 Uiso . . . . . . C44 C 0.1615(4) 0.1478(12) 0.4916(4) 0.020(2) 1.0000 Uiso . . . . . . C45 C 0.1440(4) 0.0770(13) 0.5352(4) 0.021(2) 1.0000 Uiso . . . . . . C46 C 0.0879(4) 0.0994(13) 0.5293(5) 0.025(3) 1.0000 Uiso . . . . . . O47 O 0.0676(3) 0.0288(10) 0.5686(3) 0.0355(19) 1.0000 Uiso . . . . . . C48 C 0.0519(4) 0.1951(14) 0.4847(5) 0.027(3) 1.0000 Uiso . . . . . . C49 C 0.0680(4) 0.2648(13) 0.4418(5) 0.025(3) 1.0000 Uiso . . . . . . S50 S 0.48327(11) 0.3028(4) 0.14592(13) 0.0281(7) 1.0000 Uiso . . . . . . O51 O 0.4743(3) 0.3512(11) 0.0841(4) 0.052(2) 1.0000 Uiso . . . . . . O52 O 0.5402(3) 0.3223(11) 0.1885(4) 0.047(2) 1.0000 Uiso . . . . . . O53 O 0.4399(3) 0.3568(10) 0.1644(3) 0.040(2) 1.0000 Uiso . . . . . . C54 C 0.4736(5) 0.0862(16) 0.1375(6) 0.043(3) 1.0000 Uiso . . . . . . F55 F 0.5139(3) 0.0150(8) 0.1242(3) 0.0476(19) 1.0000 Uiso . . . . . . F56 F 0.4238(3) 0.0480(12) 0.0960(4) 0.080(2) 1.0000 Uiso . . . . . . F57 F 0.4763(3) 0.0237(11) 0.1909(4) 0.083(3) 1.0000 Uiso . . . . . . S58 S 0.11486(11) 0.8087(4) 0.16252(12) 0.0278(7) 1.0000 Uiso . . . . . . O59 O 0.1418(3) 0.7186(10) 0.1297(3) 0.038(2) 1.0000 Uiso . . . . . . O60 O 0.0650(3) 0.7287(10) 0.1647(3) 0.036(2) 1.0000 Uiso . . . . . . O61 O 0.1533(4) 0.8783(11) 0.2186(4) 0.052(2) 1.0000 Uiso . . . . . . C62 C 0.0862(5) 0.9798(16) 0.1141(6) 0.045(3) 1.0000 Uiso . . . . . . F63 F 0.0542(3) 1.0727(11) 0.1323(3) 0.073(2) 1.0000 Uiso . . . . . . F64 F 0.1277(3) 1.0735(9) 0.1111(3) 0.059(2) 1.0000 Uiso . . . . . . F65 F 0.0553(3) 0.9371(10) 0.0567(3) 0.058(2) 1.0000 Uiso . . . . . . N66 N 0.2859(4) 0.5645(14) 0.0859(5) 0.051(3) 1.0000 Uiso . . . . . . C67 C 0.3224(5) 0.6141(15) 0.1278(6) 0.041(3) 1.0000 Uiso . . . . . . C68 C 0.3700(5) 0.6861(17) 0.1782(6) 0.049(3) 1.0000 Uiso . . . . . . N69 N 0.3415(5) 0.3885(16) 0.2646(5) 0.070(4) 1.0000 Uiso . . . . . . C70 C 0.3799(6) 0.3110(17) 0.2751(6) 0.047(3) 1.0000 Uiso . . . . . . C71 C 0.4307(5) 0.2146(18) 0.2900(6) 0.052(4) 1.0000 Uiso . . . . . . H72 H -0.0185 1.0993 0.3024 0.0430 1.0000 Uiso . . . . . . H73 H 0.0889 0.9359 0.2749 0.0336 1.0000 Uiso . . . . . . H74 H 0.1623 0.7598 0.3447 0.0348 1.0000 Uiso . . . . . . H75 H 0.0727 0.7381 0.4574 0.0300 1.0000 Uiso . . . . . . H76 H 0.0014 0.9119 0.3913 0.0240 1.0000 Uiso . . . . . . H77 H 0.1616 0.7287 0.5230 0.0264 1.0000 Uiso . . . . . . H78 H 0.2264 0.6191 0.6306 0.0300 1.0000 Uiso . . . . . . H79 H 0.2989 0.4265 0.6894 0.0420 1.0000 Uiso . . . . . . H80 H 0.3435 0.2612 0.6375 0.0384 1.0000 Uiso . . . . . . H81 H 0.3501 0.1782 0.5325 0.0276 1.0000 Uiso . . . . . . H82 H 0.3937 0.1766 0.4657 0.0264 1.0000 Uiso . . . . . . H83 H 0.4185 0.0030 0.3991 0.0264 1.0000 Uiso . . . . . . H84 H 0.3027 0.5998 0.3253 0.0300 1.0000 Uiso . . . . . . H85 H 0.3810 -0.1508 0.3033 0.0384 1.0000 Uiso . . . . . . H86 H 0.2464 -0.0641 0.2905 0.0312 1.0000 Uiso . . . . . . H87 H 0.2211 0.1127 0.3543 0.0276 1.0000 Uiso . . . . . . H88 H 0.0903 -0.0469 0.5871 0.0418 1.0000 Uiso . . . . . . H89 H 0.0116 0.2149 0.4816 0.0324 1.0000 Uiso . . . . . . H90 H 0.0415 0.3351 0.4088 0.0312 1.0000 Uiso . . . . . . H91 H 0.2023 0.1316 0.4951 0.0240 1.0000 Uiso . . . . . . H92 H 0.1719 0.0116 0.5701 0.0252 1.0000 Uiso . . . . . . H93 H 0.0716 0.2652 0.3286 0.0312 1.0000 Uiso . . . . . . H94 H 0.0808 0.2692 0.2217 0.0348 1.0000 Uiso . . . . . . H95 H 0.1364 0.3595 0.1643 0.0480 1.0000 Uiso . . . . . . H96 H 0.2295 0.4761 0.2195 0.0360 1.0000 Uiso . . . . . . H97 H 0.3886 0.5203 0.4011 0.0300 1.0000 Uiso . . . . . . H98 H 0.4770 0.6396 0.4689 0.0348 1.0000 Uiso . . . . . . H99 H 0.4799 0.9500 0.5634 0.0432 1.0000 Uiso . . . . . . H100 H 0.3915 0.8950 0.5574 0.0276 1.0000 Uiso . . . . . . H101 H 0.3623 0.8040 0.1823 0.0735 1.0000 Uiso . . . . . . H102 H 0.3757 0.6308 0.2179 0.0735 1.0000 Uiso . . . . . . H103 H 0.4059 0.6763 0.1709 0.0735 1.0000 Uiso . . . . . . H104 H 0.4628 0.2544 0.3285 0.0780 1.0000 Uiso . . . . . . H105 H 0.4456 0.2221 0.2558 0.0780 1.0000 Uiso . . . . . . H106 H 0.4237 0.0984 0.2954 0.0780 1.0000 Uiso . . . . . . H107 H 0.3019 0.7663 0.4905 0.0300 1.0000 Uiso . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0154(5) 0.0252(7) 0.0262(6) 0.0003(8) 0.0089(4) -0.0009(7) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.4486(12) 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 Zn1 . N2 . 2.271(8) yes Zn1 . N16 . 2.039(8) yes Zn1 . N18 . 2.279(8) yes Zn1 . N33 . 2.202(8) yes Zn1 . N40 . 2.035(8) yes Zn1 . N42 . 2.227(8) yes N2 . C3 . 1.423(12) yes N2 . C10 . 1.289(12) yes C3 . C4 . 1.375(13) yes C3 . C9 . 1.399(13) yes C4 . C5 . 1.401(15) yes C4 . H74 . 1.033 no C5 . C6 . 1.389(14) yes C5 . H73 . 1.021 no C6 . O7 . 1.381(13) yes C6 . C8 . 1.384(14) yes O7 . H72 . 0.858 no C8 . C9 . 1.370(14) yes C8 . H76 . 1.020 no C9 . H75 . 1.019 no C10 . C11 . 1.475(14) yes C10 . H77 . 1.008 no C11 . C12 . 1.393(12) yes C11 . N16 . 1.334(12) yes C12 . C13 . 1.371(15) yes C12 . H78 . 1.032 no C13 . C14 . 1.389(15) yes C13 . H79 . 1.014 no C14 . C15 . 1.376(14) yes C14 . H80 . 1.006 no C15 . N16 . 1.321(13) yes C15 . C17 . 1.491(14) yes C17 . N18 . 1.276(11) yes C17 . H81 . 1.016 no N18 . C19 . 1.412(12) yes C19 . C20 . 1.403(13) yes C19 . C24 . 1.399(13) yes C20 . C21 . 1.362(14) yes C20 . H87 . 1.019 no C21 . C22 . 1.395(13) yes C21 . H86 . 1.020 no C22 . C23 . 1.367(13) yes C22 . O25 . 1.386(12) yes C23 . C24 . 1.371(14) yes C23 . H83 . 1.026 no C24 . H82 . 1.018 no O25 . H85 . 0.854 no O26 . C27 . 1.387(12) yes O26 . H99 . 0.985 no C27 . C28 . 1.349(14) yes C27 . C32 . 1.386(13) yes C28 . C29 . 1.391(14) yes C28 . H98 . 1.024 no C29 . C30 . 1.383(13) yes C29 . H97 . 1.020 no C30 . C31 . 1.386(14) yes C30 . N33 . 1.431(12) yes C31 . C32 . 1.402(14) yes C31 . H107 . 1.012 no C32 . H100 . 1.033 no N33 . C34 . 1.267(11) yes C34 . C35 . 1.458(14) yes C34 . H84 . 1.019 no C35 . C36 . 1.395(14) yes C35 . N40 . 1.342(12) yes C36 . C37 . 1.379(15) yes C36 . H96 . 1.010 no C37 . C38 . 1.398(15) yes C37 . H95 . 1.024 no C38 . C39 . 1.387(14) yes C38 . H94 . 1.026 no C39 . N40 . 1.333(12) yes C39 . C41 . 1.465(14) yes C41 . N42 . 1.265(12) yes C41 . H93 . 1.020 no N42 . C43 . 1.420(13) yes C43 . C44 . 1.364(14) yes C43 . C49 . 1.408(14) yes C44 . C45 . 1.410(13) yes C44 . H91 . 1.022 no C45 . C46 . 1.395(13) yes C45 . H92 . 1.013 no C46 . O47 . 1.366(12) yes C46 . C48 . 1.354(14) yes O47 . H88 . 0.849 no C48 . C49 . 1.369(14) yes C48 . H89 . 1.016 no C49 . H90 . 0.998 no S50 . O51 . 1.456(9) yes S50 . O52 . 1.417(8) yes S50 . O53 . 1.416(8) yes S50 . C54 . 1.811(13) yes C54 . F55 . 1.327(13) yes C54 . F56 . 1.305(13) yes C54 . F57 . 1.349(14) yes S58 . O59 . 1.436(8) yes S58 . O60 . 1.453(7) yes S58 . O61 . 1.431(9) yes S58 . C62 . 1.791(13) yes C62 . F63 . 1.313(13) yes C62 . F64 . 1.338(13) yes C62 . F65 . 1.331(13) yes N66 . C67 . 1.141(14) yes C67 . C68 . 1.459(17) yes C68 . H101 . 1.009 no C68 . H102 . 1.009 no C68 . H103 . 1.000 no N69 . C70 . 1.113(15) yes C70 . C71 . 1.445(18) yes C71 . H104 . 1.015 no C71 . H105 . 1.027 no C71 . H106 . 0.996 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 N2 . Zn1 . N16 . 76.1(3) yes N2 . Zn1 . N18 . 151.0(3) yes N16 . Zn1 . N18 . 75.0(3) yes N2 . Zn1 . N33 . 106.2(3) yes N16 . Zn1 . N33 . 107.8(3) yes N18 . Zn1 . N33 . 85.1(3) yes N2 . Zn1 . N40 . 105.4(3) yes N16 . Zn1 . N40 . 176.2(4) yes N18 . Zn1 . N40 . 103.3(3) yes N33 . Zn1 . N40 . 75.2(3) yes N2 . Zn1 . N42 . 85.6(3) yes N16 . Zn1 . N42 . 101.8(3) yes N18 . Zn1 . N42 . 97.9(3) yes N33 . Zn1 . N42 . 149.9(3) yes N40 . Zn1 . N42 . 75.0(3) yes Zn1 . N2 . C3 . 129.0(6) yes Zn1 . N2 . C10 . 110.9(6) yes C3 . N2 . C10 . 119.4(8) yes N2 . C3 . C4 . 118.1(9) yes N2 . C3 . C9 . 123.3(9) yes C4 . C3 . C9 . 118.6(9) yes C3 . C4 . C5 . 121.4(9) yes C3 . C4 . H74 . 118.7 no C5 . C4 . H74 . 119.9 no C4 . C5 . C6 . 117.8(10) yes C4 . C5 . H73 . 120.9 no C6 . C5 . H73 . 121.3 no C5 . C6 . O7 . 114.8(9) yes C5 . C6 . C8 . 121.8(10) yes O7 . C6 . C8 . 123.4(9) yes C6 . O7 . H72 . 115.8 no C6 . C8 . C9 . 118.8(9) yes C6 . C8 . H76 . 121.1 no C9 . C8 . H76 . 120.1 no C3 . C9 . C8 . 121.4(10) yes C3 . C9 . H75 . 120.1 no C8 . C9 . H75 . 118.5 no N2 . C10 . C11 . 118.5(9) yes N2 . C10 . H77 . 119.9 no C11 . C10 . H77 . 121.6 no C10 . C11 . C12 . 123.6(9) yes C10 . C11 . N16 . 115.3(8) yes C12 . C11 . N16 . 121.0(10) yes C11 . C12 . C13 . 119.0(10) yes C11 . C12 . H78 . 119.2 no C13 . C12 . H78 . 121.7 no C12 . C13 . C14 . 118.9(10) yes C12 . C13 . H79 . 120.4 no C14 . C13 . H79 . 120.7 no C13 . C14 . C15 . 119.0(10) yes C13 . C14 . H80 . 119.9 no C15 . C14 . H80 . 121.1 no C14 . C15 . N16 . 121.8(10) yes C14 . C15 . C17 . 124.6(10) yes N16 . C15 . C17 . 113.5(9) yes C11 . N16 . C15 . 120.2(9) yes C11 . N16 . Zn1 . 118.8(7) yes C15 . N16 . Zn1 . 120.8(7) yes C15 . C17 . N18 . 118.4(9) yes C15 . C17 . H81 . 120.5 no N18 . C17 . H81 . 121.1 no Zn1 . N18 . C17 . 111.1(7) yes Zn1 . N18 . C19 . 127.0(6) yes C17 . N18 . C19 . 120.5(9) yes N18 . C19 . C20 . 117.2(8) yes N18 . C19 . C24 . 123.3(9) yes C20 . C19 . C24 . 119.5(9) yes C19 . C20 . C21 . 120.3(9) yes C19 . C20 . H87 . 119.9 no C21 . C20 . H87 . 119.9 no C20 . C21 . C22 . 119.3(9) yes C20 . C21 . H86 . 119.7 no C22 . C21 . H86 . 121.0 no C21 . C22 . C23 . 120.9(10) yes C21 . C22 . O25 . 115.9(9) yes C23 . C22 . O25 . 123.1(9) yes C22 . C23 . C24 . 120.5(9) yes C22 . C23 . H83 . 119.0 no C24 . C23 . H83 . 120.5 no C19 . C24 . C23 . 119.5(9) yes C19 . C24 . H82 . 120.3 no C23 . C24 . H82 . 120.2 no C22 . O25 . H85 . 119.2 no C27 . O26 . H99 . 104.2 no O26 . C27 . C28 . 117.0(9) yes O26 . C27 . C32 . 120.5(9) yes C28 . C27 . C32 . 122.5(10) yes C27 . C28 . C29 . 119.2(10) yes C27 . C28 . H98 . 120.7 no C29 . C28 . H98 . 120.1 no C28 . C29 . C30 . 120.3(10) yes C28 . C29 . H97 . 119.8 no C30 . C29 . H97 . 119.9 no C29 . C30 . C31 . 119.8(9) yes C29 . C30 . N33 . 122.7(9) yes C31 . C30 . N33 . 117.5(8) yes C30 . C31 . C32 . 119.8(9) yes C30 . C31 . H107 . 120.3 no C32 . C31 . H107 . 119.9 no C31 . C32 . C27 . 118.2(9) yes C31 . C32 . H100 . 122.2 no C27 . C32 . H100 . 119.6 no Zn1 . N33 . C30 . 125.7(6) yes Zn1 . N33 . C34 . 113.2(7) yes C30 . N33 . C34 . 119.6(8) yes N33 . C34 . C35 . 118.3(9) yes N33 . C34 . H84 . 120.2 no C35 . C34 . H84 . 121.5 no C34 . C35 . C36 . 126.1(9) yes C34 . C35 . N40 . 113.1(9) yes C36 . C35 . N40 . 120.7(9) yes C35 . C36 . C37 . 118.9(10) yes C35 . C36 . H96 . 120.1 no C37 . C36 . H96 . 121.0 no C36 . C37 . C38 . 119.7(11) yes C36 . C37 . H95 . 120.4 no C38 . C37 . H95 . 119.9 no C37 . C38 . C39 . 118.2(10) yes C37 . C38 . H94 . 121.4 no C39 . C38 . H94 . 120.3 no C38 . C39 . N40 . 121.5(9) yes C38 . C39 . C41 . 124.3(9) yes N40 . C39 . C41 . 113.8(9) yes C35 . N40 . C39 . 120.9(8) yes C35 . N40 . Zn1 . 119.0(6) yes C39 . N40 . Zn1 . 119.4(7) yes C39 . C41 . N42 . 117.3(9) yes C39 . C41 . H93 . 120.6 no N42 . C41 . H93 . 122.1 no Zn1 . N42 . C41 . 112.7(7) yes Zn1 . N42 . C43 . 124.3(6) yes C41 . N42 . C43 . 122.0(9) yes N42 . C43 . C44 . 116.9(9) yes N42 . C43 . C49 . 122.3(10) yes C44 . C43 . C49 . 120.8(10) yes C43 . C44 . C45 . 119.6(9) yes C43 . C44 . H91 . 120.8 no C45 . C44 . H91 . 119.6 no C44 . C45 . C46 . 118.7(9) yes C44 . C45 . H92 . 120.2 no C46 . C45 . H92 . 121.2 no C45 . C46 . O47 . 121.6(9) yes C45 . C46 . C48 . 120.6(10) yes O47 . C46 . C48 . 117.8(9) yes C46 . O47 . H88 . 107.9 no C46 . C48 . C49 . 121.6(10) yes C46 . C48 . H89 . 120.4 no C49 . C48 . H89 . 118.0 no C43 . C49 . C48 . 118.6(10) yes C43 . C49 . H90 . 119.7 no C48 . C49 . H90 . 121.7 no O51 . S50 . O52 . 113.8(5) yes O51 . S50 . O53 . 113.4(5) yes O52 . S50 . O53 . 116.6(5) yes O51 . S50 . C54 . 101.6(6) yes O52 . S50 . C54 . 104.4(6) yes O53 . S50 . C54 . 104.9(6) yes S50 . C54 . F55 . 112.4(8) yes S50 . C54 . F56 . 112.0(9) yes F55 . C54 . F56 . 109.1(10) yes S50 . C54 . F57 . 108.8(9) yes F55 . C54 . F57 . 107.3(10) yes F56 . C54 . F57 . 107.1(10) yes O59 . S58 . O60 . 113.3(5) yes O59 . S58 . O61 . 114.7(5) yes O60 . S58 . O61 . 116.1(5) yes O59 . S58 . C62 . 102.8(5) yes O60 . S58 . C62 . 104.0(5) yes O61 . S58 . C62 . 103.8(6) yes S58 . C62 . F63 . 113.6(9) yes S58 . C62 . F64 . 111.2(8) yes F63 . C62 . F64 . 106.7(10) yes S58 . C62 . F65 . 112.3(9) yes F63 . C62 . F65 . 107.4(10) yes F64 . C62 . F65 . 105.2(10) yes N66 . C67 . C68 . 175.6(14) yes C67 . C68 . H101 . 110.1 no C67 . C68 . H102 . 110.7 no H101 . C68 . H102 . 108.0 no C67 . C68 . H103 . 110.4 no H101 . C68 . H103 . 108.8 no H102 . C68 . H103 . 108.8 no N69 . C70 . C71 . 178.2(15) yes C70 . C71 . H104 . 111.7 no C70 . C71 . H105 . 110.4 no H104 . C71 . H105 . 106.2 no C70 . C71 . H106 . 112.0 no H104 . C71 . H106 . 108.6 no H105 . C71 . H106 . 107.6 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 O7 . H72 . O60 3_555 179.6 0.858 1.977 2.834 yes O25 . H85 . O52 3_645 179.9 0.854 1.956 2.811 yes O47 . H88 . O59 4_555 179.6 0.849 1.932 2.782 yes O26 . H99 . O51 4_565 168.5 0.985 1.740 2.712 yes _vrf_PLAT026_CRYSTALS_cif ; PROBLEM: Ratio Observed / Unique Reflections too Low .... 14 Perc. RESPONSE: All crystals were thin platelets and in addition a weak scatterer: inspection of the diffraction images shows a rather high mosaicity. This leads to the overall low intensity and the low number of observed reflections ; _vrf_PLAT201_CRYSTALS_cif ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 48 RESPONSE: In order to keep the number of observed reflections to number of parmaters ratio reasonable it was decided to refine only the heaviest atom (i.e. Zn) anisotropically ;