# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_Publication _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_name 'Prof. Smail Triki' _publ_contact_author_address ;UMR CNRS 6521, Universit\'e de Bretagne Occidentale, BP 809, 29285 Brest Cedex (France) ; _publ_contact_author_email triki@univ-brest.fr _publ_contact_author_phone +33298016146 _publ_contact_author_fax +33298017001 loop_ _publ_author_name _publ_author_address S.Triki ;UMR CNRS 6521, Universit\'e de Bretagne Occidentale, BP 809, 29285 Brest Cedex (France) ; G.Dupouy ;UMR CNRS 6521, Universit\'e de Bretagne Occidentale, BP 809, 29285 Brest Cedex (France) ; C.J.Gomez-Garcia ;UMR CNRS 6521, Universit\'e de Bretagne Occidentale, BP 809, 29285 Brest Cedex (France) ; C.Lecomte ;UMR CNRS 6521, Universit\'e de Bretagne Occidentale, BP 809, 29285 Brest Cedex (France) ; J.-F.Letard ;Instituto de Ciencia Molecular, Univ. de Valencia, 46980 Paterna, (Spain). ; M.Marchivie ;LCM3B, (UMR UHP-CNRS 7036), Bld des aiguillettes, BP 239, 54506 Vandoeuvre-les-Nancy Cedex, (France).' ; S.Pillet ;LCM3B, (UMR UHP-CNRS 7036), Bld des aiguillettes, BP 239, 54506 Vandoeuvre-les-Nancy Cedex, (France).' ; J.Sala-Pala ;ICMCB-CNRS 87, Avenue du Docteur Albert Schweitzer 33608 PESSAC cedex (France) ; _publ_requested_category FM data_dc293 _database_code_depnum_ccdc_archive 'CCDC 705802' ####################################################################### # # # [Fe(abpt)2(tcpd)] at 293 K # # # ####################################################################### #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2008-09-25 at 16:47:30 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\program files\wingx\files\archive.dat # CIF files read : dc297 struct _audit_creation_date 2008-09-25T16:47:30-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C34 H20 Fe1 N18' _chemical_formula_sum 'C34 H20 Fe N18' _chemical_formula_weight 736.53 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.3762(3) _cell_length_b 12.4222(3) _cell_length_c 11.8683(3) _cell_angle_alpha 90 _cell_angle_beta 92.031(2) _cell_angle_gamma 90 _cell_volume 1676.14(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8664 _cell_measurement_theta_min 2.9319 _cell_measurement_theta_max 27.4247 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.507 _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 0.96419 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 8.3622 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_unetI/netI 0.0227 _diffrn_reflns_number 18122 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 23.25 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 2390 _reflns_number_gt 1858 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _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 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0286P)^2^+0.8533P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 2390 _refine_ls_number_parameters 332 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0791 _refine_ls_wR_factor_gt 0.0747 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.202 _refine_diff_density_min -0.137 _refine_diff_density_rms 0.039 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4497(3) 0.7504(3) 0.0250(3) 0.0534(8) Uani 1 1 d . A . C2 C 0.4350(3) 0.6453(3) -0.0103(3) 0.0643(9) Uani 1 1 d . . . C3 C 0.4592(3) 0.6203(3) -0.1196(3) 0.0682(9) Uani 1 1 d . . . C4 C 0.4984(3) 0.6991(3) -0.1902(3) 0.0571(8) Uani 1 1 d . . . C5 C 0.5108(2) 0.8027(2) -0.1494(2) 0.0430(7) Uani 1 1 d . A . C6 C 0.5465(2) 0.8962(2) -0.2136(2) 0.0396(7) Uani 1 1 d . A . C7 C 0.6089(2) 1.0094(2) -0.33845(19) 0.0384(6) Uani 1 1 d . A . C8 C 0.6526(2) 1.0542(2) -0.4425(2) 0.0440(7) Uani 1 1 d . . . C9 C 0.6911(3) 1.1594(3) -0.4475(3) 0.0641(9) Uani 1 1 d . . . C10 C 0.7302(3) 1.1970(4) -0.5481(4) 0.0786(11) Uani 1 1 d . . . C11 C 0.7296(3) 1.1311(4) -0.6390(3) 0.0759(12) Uani 1 1 d . . . C12 C 0.6912(3) 1.0285(4) -0.6277(3) 0.0667(10) Uani 1 1 d . . . C15 C 1.0912(3) 0.8471(3) -0.1001(2) 0.0435(7) Uani 1 1 d . . . C16 C 1.0000 1.0000 0.0000 0.0376(8) Uani 1 2 d S . . N3 N 0.6884(2) 0.9846(2) 0.03438(19) 0.0516(6) Uani 1 1 d . . . C131 C 0.7805(14) 0.9841(11) -0.0031(8) 0.038(3) Uani 0.50 1 d P A 1 C141 C 0.870(2) 0.935(3) -0.164(3) 0.047(5) Uani 0.50 1 d P A 1 N81 N 0.854(3) 0.911(3) -0.257(2) 0.071(4) Uani 0.50 1 d P A 1 N91 N 1.1568(6) 0.7832(9) -0.1152(7) 0.056(2) Uani 0.50 1 d P B 1 C17 C 0.8867(4) 0.9746(4) -0.0545(4) 0.0416(14) Uani 0.50 1 d P A 1 C132 C 0.7843(13) 1.0091(11) 0.0331(8) 0.030(2) Uani 0.50 1 d P A 2 C142 C 0.901(2) 0.915(3) -0.166(3) 0.042(4) Uani 0.50 1 d P B 2 N82 N 0.831(2) 0.893(3) -0.231(2) 0.070(4) Uani 0.50 1 d P B 2 N92 N 1.0998(8) 0.7674(9) -0.1428(8) 0.062(2) Uani 0.50 1 d P B 2 C18 C 0.8992(4) 1.0516(4) 0.0436(4) 0.0396(13) Uani 0.50 1 d P . 2 C19 C 0.9946(4) 0.9220(4) -0.0838(4) 0.0404(13) Uani 0.50 1 d P . 2 N1 N 0.48670(17) 0.82883(18) -0.04153(17) 0.0415(6) Uani 1 1 d . . . N2 N 0.54073(17) 0.99465(18) -0.17228(16) 0.0412(5) Uani 1 1 d . . . N4 N 0.57992(18) 1.06643(18) -0.25046(17) 0.0438(6) Uani 1 1 d . A . N5 N 0.58862(18) 0.90268(18) -0.31868(17) 0.0414(5) Uani 1 1 d . . . N6 N 0.6172(3) 0.8117(2) -0.3839(3) 0.0609(8) Uani 1 1 d . A . N7 N 0.65156(19) 0.9874(2) -0.53147(18) 0.0547(6) Uani 1 1 d . . . Fe01 Fe 0.5000 1.0000 0.0000 0.03932(19) Uani 1 2 d S . . H1 H 0.438(2) 0.770(2) 0.095(2) 0.052(9) Uiso 1 1 d . . . H1N H 0.614(3) 0.832(3) -0.447(3) 0.079(13) Uiso 1 1 d . . . H2 H 0.406(3) 0.591(3) 0.041(3) 0.079(10) Uiso 1 1 d . . . H2N H 0.701(3) 0.800(3) -0.355(3) 0.101(14) Uiso 1 1 d . . . H3 H 0.451(3) 0.547(3) -0.147(3) 0.077(10) Uiso 1 1 d . . . H4 H 0.512(2) 0.688(2) -0.265(2) 0.058(9) Uiso 1 1 d . . . H5 H 0.688(2) 0.976(2) -0.684(3) 0.063(10) Uiso 1 1 d . . . H6 H 0.762(3) 1.154(3) -0.695(3) 0.101(14) Uiso 1 1 d . . . H7 H 0.753(3) 1.264(3) -0.552(3) 0.082(12) Uiso 1 1 d . . . H8 H 0.691(3) 1.202(2) -0.390(3) 0.069(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0493(18) 0.065(2) 0.0467(19) 0.0085(18) 0.0110(15) -0.0037(16) C2 0.064(2) 0.057(2) 0.072(2) 0.0161(19) 0.0162(18) -0.0041(18) C3 0.077(2) 0.050(2) 0.079(3) -0.0006(19) 0.0138(19) -0.0065(18) C4 0.065(2) 0.054(2) 0.053(2) -0.0025(17) 0.0113(16) -0.0027(16) C5 0.0343(15) 0.0474(18) 0.0473(17) -0.0010(14) 0.0027(12) -0.0017(13) C6 0.0325(15) 0.0496(19) 0.0368(15) -0.0044(13) 0.0039(12) -0.0001(13) C7 0.0325(14) 0.0472(18) 0.0356(14) -0.0022(14) 0.0037(11) -0.0003(13) C8 0.0349(15) 0.0602(19) 0.0373(15) 0.0050(14) 0.0039(12) 0.0026(14) C9 0.071(2) 0.063(2) 0.060(2) 0.0061(19) 0.0147(18) -0.0074(19) C10 0.085(3) 0.078(3) 0.075(3) 0.023(2) 0.023(2) -0.012(2) C11 0.063(2) 0.112(4) 0.054(2) 0.031(3) 0.0176(19) 0.005(2) C12 0.058(2) 0.103(3) 0.0396(19) 0.007(2) 0.0088(15) 0.011(2) C15 0.042(2) 0.052(2) 0.0366(17) 0.0041(16) 0.0084(13) 0.002(2) C16 0.0262(19) 0.054(2) 0.0329(19) 0.007(2) 0.0054(15) -0.001(2) N3 0.0279(14) 0.0721(18) 0.0551(15) -0.0109(13) 0.0074(12) 0.0000(13) C131 0.039(5) 0.055(7) 0.019(6) -0.013(4) -0.001(5) 0.002(4) C141 0.025(11) 0.074(13) 0.044(7) -0.007(8) 0.015(8) 0.009(7) N81 0.066(10) 0.113(11) 0.034(9) 0.008(6) -0.003(5) -0.010(7) N91 0.057(5) 0.063(5) 0.049(4) 0.013(3) 0.011(4) 0.017(5) C17 0.025(3) 0.066(4) 0.033(3) -0.006(3) 0.006(2) 0.003(3) C132 0.025(5) 0.049(6) 0.017(6) -0.010(4) 0.003(4) 0.007(4) C142 0.025(11) 0.063(9) 0.039(7) -0.015(6) 0.005(8) 0.013(7) N82 0.061(10) 0.104(11) 0.042(11) -0.003(8) -0.014(7) -0.011(7) N92 0.061(6) 0.060(5) 0.067(5) -0.004(4) 0.008(4) -0.004(5) C18 0.027(4) 0.056(4) 0.036(3) -0.002(3) 0.005(2) 0.002(3) C19 0.034(3) 0.058(4) 0.029(3) -0.001(3) 0.000(3) 0.001(3) N1 0.0321(12) 0.0538(15) 0.0389(13) 0.0033(11) 0.0056(10) -0.0013(11) N2 0.0387(12) 0.0470(13) 0.0383(11) 0.0005(12) 0.0076(9) -0.0016(11) N4 0.0438(14) 0.0484(14) 0.0396(13) 0.0002(12) 0.0086(11) -0.0018(11) N5 0.0408(13) 0.0483(15) 0.0356(13) -0.0069(11) 0.0078(10) -0.0005(11) N6 0.083(2) 0.0548(17) 0.0464(18) -0.0118(15) 0.0186(16) -0.0024(15) N7 0.0527(15) 0.0746(17) 0.0373(13) -0.0046(13) 0.0077(11) 0.0010(13) Fe01 0.0264(3) 0.0536(4) 0.0384(3) -0.0012(3) 0.0075(2) -0.0019(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.332(3) . ? C1 C2 1.379(5) . ? C2 C3 1.372(5) . ? C3 C4 1.373(4) . ? C4 C5 1.380(4) . ? C5 N1 1.358(3) . ? C5 C6 1.455(4) . ? C6 N2 1.321(3) . ? C6 N5 1.354(3) . ? C7 N4 1.313(3) . ? C7 N5 1.368(3) . ? C7 C8 1.458(3) . ? C8 N7 1.343(3) . ? C8 C9 1.379(4) . ? C9 C10 1.371(5) . ? C10 C11 1.354(5) . ? C11 C12 1.355(5) . ? C12 N7 1.344(4) . ? C15 N91 1.108(10) . ? C15 N92 1.118(11) . ? C15 C18 1.427(6) 3_775 ? C15 C19 1.458(6) . ? C16 C19 1.388(5) 3_775 ? C16 C19 1.388(5) . ? C16 C18 1.427(5) 3_775 ? C16 C18 1.427(5) . ? C16 C17 1.456(5) . ? C16 C17 1.456(5) 3_775 ? N3 C132 1.133(15) . ? N3 C131 1.152(16) . ? N3 Fe01 2.176(2) . ? C131 C17 1.378(16) . ? C141 N81 1.16(5) . ? C141 C17 1.39(4) . ? C132 C18 1.411(15) . ? C142 N82 1.12(5) . ? C142 C19 1.42(3) . ? C18 C19 1.324(7) 3_775 ? C18 C15 1.427(6) 3_775 ? C19 C18 1.324(7) 3_775 ? N1 Fe01 2.187(2) . ? N2 N4 1.373(3) . ? N2 Fe01 2.1134(19) . ? N5 N6 1.414(3) . ? Fe01 N2 2.1134(19) 3_675 ? Fe01 N3 2.176(2) 3_675 ? Fe01 N1 2.187(2) 3_675 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.4(3) . . ? C3 C2 C1 118.4(3) . . ? C2 C3 C4 119.8(3) . . ? C3 C4 C5 118.8(3) . . ? N1 C5 C4 122.2(3) . . ? N1 C5 C6 111.8(2) . . ? C4 C5 C6 126.0(3) . . ? N2 C6 N5 108.1(2) . . ? N2 C6 C5 121.8(2) . . ? N5 C6 C5 130.1(2) . . ? N4 C7 N5 109.7(2) . . ? N4 C7 C8 124.8(3) . . ? N5 C7 C8 125.5(2) . . ? N7 C8 C9 123.1(3) . . ? N7 C8 C7 115.8(3) . . ? C9 C8 C7 121.1(3) . . ? C10 C9 C8 118.3(4) . . ? C11 C10 C9 119.7(4) . . ? C10 C11 C12 118.8(4) . . ? N7 C12 C11 124.1(4) . . ? N91 C15 N92 38.9(4) . . ? N91 C15 C18 131.8(7) . 3_775 ? N92 C15 C18 170.6(7) . 3_775 ? N91 C15 C19 173.3(7) . . ? N92 C15 C19 134.7(7) . . ? C18 C15 C19 54.6(3) 3_775 . ? C19 C16 C19 180.0(4) 3_775 . ? C19 C16 C18 123.9(3) 3_775 3_775 ? C19 C16 C18 56.1(3) . 3_775 ? C19 C16 C18 56.1(3) 3_775 . ? C19 C16 C18 123.9(3) . . ? C18 C16 C18 180.000(1) 3_775 . ? C19 C16 C17 119.1(3) 3_775 . ? C19 C16 C17 60.9(3) . . ? C18 C16 C17 116.8(3) 3_775 . ? C18 C16 C17 63.2(3) . . ? C19 C16 C17 60.9(3) 3_775 3_775 ? C19 C16 C17 119.1(3) . 3_775 ? C18 C16 C17 63.2(3) 3_775 3_775 ? C18 C16 C17 116.8(3) . 3_775 ? C17 C16 C17 180.000(1) . 3_775 ? C132 N3 C131 26.9(6) . . ? C132 N3 Fe01 156.4(7) . . ? C131 N3 Fe01 146.2(6) . . ? N3 C131 C17 174.1(10) . . ? N81 C141 C17 175(3) . . ? C131 C17 C141 110.7(12) . . ? C131 C17 C16 124.1(5) . . ? C141 C17 C16 125.2(11) . . ? N3 C132 C18 171.3(9) . . ? N82 C142 C19 169(3) . . ? C19 C18 C132 162.7(7) 3_775 . ? C19 C18 C16 60.5(3) 3_775 . ? C132 C18 C16 123.6(6) . . ? C19 C18 C15 63.9(4) 3_775 3_775 ? C132 C18 C15 115.2(6) . 3_775 ? C16 C18 C15 121.2(4) . 3_775 ? C18 C19 C16 63.4(3) 3_775 . ? C18 C19 C142 156.0(15) 3_775 . ? C16 C19 C142 123.0(10) . . ? C18 C19 C15 61.5(4) 3_775 . ? C16 C19 C15 121.7(4) . . ? C142 C19 C15 115.0(10) . . ? C1 N1 C5 117.5(3) . . ? C1 N1 Fe01 126.8(2) . . ? C5 N1 Fe01 115.50(17) . . ? C6 N2 N4 109.2(2) . . ? C6 N2 Fe01 113.83(17) . . ? N4 N2 Fe01 136.15(17) . . ? C7 N4 N2 106.5(2) . . ? C6 N5 C7 106.4(2) . . ? C6 N5 N6 123.5(2) . . ? C7 N5 N6 129.6(2) . . ? C8 N7 C12 116.0(3) . . ? N2 Fe01 N2 180.0 . 3_675 ? N2 Fe01 N3 93.99(8) . 3_675 ? N2 Fe01 N3 86.01(8) 3_675 3_675 ? N2 Fe01 N3 86.01(8) . . ? N2 Fe01 N3 93.99(8) 3_675 . ? N3 Fe01 N3 180.0 3_675 . ? N2 Fe01 N1 103.47(8) . 3_675 ? N2 Fe01 N1 76.53(8) 3_675 3_675 ? N3 Fe01 N1 90.96(8) 3_675 3_675 ? N3 Fe01 N1 89.04(8) . 3_675 ? N2 Fe01 N1 76.53(8) . . ? N2 Fe01 N1 103.47(8) 3_675 . ? N3 Fe01 N1 89.04(8) 3_675 . ? N3 Fe01 N1 90.96(8) . . ? N1 Fe01 N1 180.0 3_675 . ? #===END data_dc100 _database_code_depnum_ccdc_archive 'CCDC 705803' ###################################################################### # # # [Fe(abpt)2(tcpd)] at 100 K # # # ###################################################################### #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2008-09-25 at 17:00:40 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\program files\wingx\files\archive.dat # CIF files read : dc90 struct _audit_creation_date 2008-09-25T17:00:40-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C34 H20 Fe1 N18' _chemical_formula_sum 'C34 H20 Fe N18' _chemical_formula_weight 736.53 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.2359(3) _cell_length_b 12.2079(2) _cell_length_c 11.8655(2) _cell_angle_alpha 90 _cell_angle_beta 91.703(2) _cell_angle_gamma 90 _cell_volume 1626.83(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10058 _cell_measurement_theta_min 2.5293 _cell_measurement_theta_max 27.375 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.522 _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 0.96164 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 8.3622 _diffrn_orient_matrix_ub_11 -0.0023615143 _diffrn_orient_matrix_ub_12 0.0478319269 _diffrn_orient_matrix_ub_13 0.0338721149 _diffrn_orient_matrix_ub_21 0.0133179744 _diffrn_orient_matrix_ub_22 0.0326651915 _diffrn_orient_matrix_ub_23 -0.0474935019 _diffrn_orient_matrix_ub_31 -0.0617441291 _diffrn_orient_matrix_ub_32 0.0052344172 _diffrn_orient_matrix_ub_33 -0.0133629364 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_unetI/netI 0.0389 _diffrn_reflns_number 21459 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.972 _diffrn_measured_fraction_theta_max 0.972 _reflns_number_total 3234 _reflns_number_gt 2353 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _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 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+1.4140P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 3234 _refine_ls_number_parameters 322 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.0884 _refine_ls_wR_factor_gt 0.0839 _refine_ls_goodness_of_fit_ref 1.11 _refine_ls_restrained_S_all 1.11 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.285 _refine_diff_density_min -0.25 _refine_diff_density_rms 0.052 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4495(2) 0.7521(2) 0.0318(2) 0.0333(6) Uani 1 1 d . A . C2 C 0.4327(2) 0.6450(2) -0.0030(3) 0.0407(7) Uani 1 1 d . . . C3 C 0.4558(3) 0.6175(2) -0.1126(3) 0.0396(7) Uani 1 1 d . . . C4 C 0.4957(2) 0.6965(2) -0.1856(2) 0.0331(6) Uani 1 1 d . . . C5 C 0.5095(2) 0.8023(2) -0.1448(2) 0.0281(6) Uani 1 1 d . A . C6 C 0.5454(2) 0.8967(2) -0.2107(2) 0.0266(6) Uani 1 1 d . A . C7 C 0.6083(2) 1.0116(2) -0.33547(19) 0.0268(5) Uani 1 1 d . A . C8 C 0.6524(2) 1.0567(2) -0.4408(2) 0.0284(6) Uani 1 1 d . . . C9 C 0.6949(2) 1.1631(2) -0.4462(2) 0.0338(6) Uani 1 1 d . . . C10 C 0.7336(3) 1.2006(2) -0.5480(2) 0.0379(7) Uani 1 1 d . . . C11 C 0.7302(2) 1.1322(2) -0.6404(2) 0.0376(7) Uani 1 1 d . . . C12 C 0.6869(2) 1.0276(2) -0.6272(2) 0.0357(7) Uani 1 1 d . . . C15 C 1.0920(2) 0.8434(2) -0.10019(19) 0.0261(6) Uani 1 1 d . . . C16 C 1.0000 1.0000 0.0000 0.0228(7) Uani 1 2 d S . . N3 N 0.6821(2) 0.98781(18) 0.03217(17) 0.0322(5) Uani 1 1 d . . . C131 C 0.7793(13) 0.9867(10) -0.0010(8) 0.022(2) Uani 0.50 1 d P A 1 C141 C 0.8780(7) 0.9357(6) -0.1657(6) 0.027(2) Uiso 0.50 1 d P A 1 N81 N 0.8576(9) 0.9011(13) -0.2548(10) 0.032(2) Uani 0.50 1 d P A 1 N91 N 1.1568(5) 0.7768(6) -0.1151(5) 0.0304(15) Uani 0.50 1 d P B 1 C17 C 0.8892(4) 0.9769(4) -0.0535(4) 0.0241(11) Uani 0.50 1 d P A 1 C132 C 0.7789(12) 1.0114(9) 0.0303(8) 0.0159(19) Uani 0.50 1 d P A 2 C142 C 0.8920(6) 0.9106(6) -0.1645(6) 0.023(2) Uiso 0.50 1 d P B 2 N82 N 0.8219(10) 0.8993(13) -0.2322(11) 0.034(2) Uani 0.50 1 d P B 2 N92 N 1.1033(6) 0.7632(6) -0.1423(5) 0.0292(14) Uani 0.50 1 d P B 2 C18 C 0.8943(4) 1.0502(4) 0.0425(4) 0.0213(10) Uani 0.50 1 d P . 2 C19 C 0.9914(4) 0.9185(4) -0.0847(4) 0.0228(10) Uani 0.50 1 d P . 2 N1 N 0.48688(16) 0.83104(17) -0.03733(16) 0.0265(5) Uani 1 1 d . . . N2 N 0.54063(16) 0.99690(17) -0.16813(15) 0.0262(4) Uani 1 1 d . . . N4 N 0.57970(18) 1.07010(16) -0.24649(16) 0.0279(5) Uani 1 1 d . A . N5 N 0.58722(18) 0.90303(16) -0.31613(17) 0.0283(5) Uani 1 1 d . . . N6 N 0.6161(2) 0.81001(18) -0.3815(2) 0.0357(6) Uani 1 1 d . A . N7 N 0.64725(18) 0.98843(18) -0.53007(16) 0.0323(5) Uani 1 1 d . . . Fe Fe 0.5000 1.0000 0.0000 0.02325(15) Uani 1 2 d S . . H1 H 0.435(2) 0.774(2) 0.106(2) 0.036(7) Uiso 1 1 d . . . H1N H 0.612(2) 0.831(2) -0.451(3) 0.047(9) Uiso 1 1 d . . . H2 H 0.407(2) 0.593(2) 0.051(2) 0.049(8) Uiso 1 1 d . . . H2N H 0.701(3) 0.800(2) -0.361(2) 0.050(9) Uiso 1 1 d . . . H3 H 0.446(2) 0.544(2) -0.140(2) 0.040(8) Uiso 1 1 d . . . H4 H 0.510(2) 0.683(2) -0.263(2) 0.034(7) Uiso 1 1 d . . . H5 H 0.683(2) 0.976(2) -0.686(2) 0.027(7) Uiso 1 1 d . . . H6 H 0.755(3) 1.155(2) -0.707(3) 0.055(9) Uiso 1 1 d . . . H7 H 0.763(2) 1.267(2) -0.559(2) 0.039(8) Uiso 1 1 d . . . H8 H 0.696(2) 1.206(2) -0.389(2) 0.036(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0247(14) 0.0392(16) 0.0366(16) 0.0119(13) 0.0076(12) 0.0037(12) C2 0.0323(17) 0.0391(17) 0.0512(19) 0.0221(15) 0.0107(13) 0.0044(13) C3 0.0351(17) 0.0278(15) 0.0561(19) 0.0072(14) 0.0043(14) 0.0026(13) C4 0.0312(15) 0.0321(15) 0.0360(16) 0.0039(12) 0.0003(12) 0.0041(12) C5 0.0203(13) 0.0304(14) 0.0336(14) 0.0029(11) 0.0013(11) 0.0016(11) C6 0.0239(14) 0.0304(15) 0.0255(13) -0.0003(11) 0.0012(10) 0.0009(11) C7 0.0270(13) 0.0286(14) 0.0246(12) 0.0025(11) -0.0012(10) -0.0026(12) C8 0.0262(14) 0.0332(15) 0.0258(13) 0.0041(11) -0.0029(11) -0.0006(11) C9 0.0352(16) 0.0319(15) 0.0340(15) 0.0029(13) -0.0019(13) -0.0025(13) C10 0.0374(17) 0.0346(16) 0.0419(17) 0.0113(14) 0.0049(13) -0.0062(14) C11 0.0316(16) 0.0515(18) 0.0298(15) 0.0160(14) 0.0040(12) 0.0011(14) C12 0.0326(15) 0.0485(19) 0.0262(14) 0.0030(13) 0.0019(12) 0.0003(13) C15 0.0320(16) 0.0294(15) 0.0171(12) 0.0050(11) 0.0057(10) 0.0060(13) C16 0.0253(18) 0.0266(17) 0.0167(15) 0.0075(16) 0.0033(13) 0.0047(17) N3 0.0320(13) 0.0327(13) 0.0326(12) -0.0058(10) 0.0135(10) 0.0005(11) C131 0.038(4) 0.018(5) 0.009(5) -0.005(3) 0.000(4) 0.003(4) N81 0.024(6) 0.054(4) 0.018(5) -0.003(3) 0.002(3) 0.001(5) N91 0.036(4) 0.037(3) 0.019(3) 0.005(2) 0.002(3) 0.011(3) C17 0.022(3) 0.029(3) 0.021(2) -0.0002(19) 0.005(2) 0.004(2) C132 0.024(4) 0.018(5) 0.006(5) -0.007(3) 0.001(4) 0.001(3) N82 0.027(6) 0.049(4) 0.027(5) -0.005(4) 0.007(3) 0.002(5) N92 0.031(4) 0.029(3) 0.028(3) -0.002(2) 0.000(3) 0.001(3) C18 0.023(3) 0.027(2) 0.015(2) -0.0008(19) 0.0045(19) 0.001(2) C19 0.024(3) 0.028(3) 0.016(2) 0.004(2) 0.002(2) 0.003(2) N1 0.0164(10) 0.0358(12) 0.0275(11) 0.0080(9) 0.0021(9) 0.0026(9) N2 0.0248(11) 0.0264(10) 0.0274(10) 0.0034(10) 0.0003(8) 0.0006(10) N4 0.0284(12) 0.0280(11) 0.0271(12) 0.0041(9) 0.0000(9) -0.0013(9) N5 0.0326(12) 0.0262(12) 0.0262(11) -0.0008(9) 0.0032(9) -0.0023(9) N6 0.0521(18) 0.0292(12) 0.0260(13) -0.0040(10) 0.0079(11) -0.0024(11) N7 0.0335(12) 0.0366(13) 0.0267(11) 0.0007(10) 0.0014(9) -0.0023(11) Fe 0.0162(3) 0.0291(3) 0.0247(3) 0.0017(2) 0.00520(18) 0.0020(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.342(3) . ? C1 C2 1.382(4) . ? C2 C3 1.375(4) . ? C3 C4 1.381(4) . ? C4 C5 1.386(4) . ? C5 N1 1.354(3) . ? C5 C6 1.456(3) . ? C6 N2 1.325(3) . ? C6 N5 1.352(3) . ? C7 N4 1.322(3) . ? C7 N5 1.367(3) . ? C7 C8 1.465(3) . ? C8 N7 1.348(3) . ? C8 C9 1.386(4) . ? C9 C10 1.374(4) . ? C10 C11 1.378(4) . ? C11 C12 1.377(4) . ? C12 N7 1.337(3) . ? C15 N91 1.108(7) . ? C15 N92 1.108(7) . ? C15 C19 1.471(5) . ? C15 C18 1.474(5) 3_775 ? C16 C17 1.409(5) . ? C16 C17 1.409(5) 3_775 ? C16 C19 1.415(5) 3_775 ? C16 C19 1.415(5) . ? C16 C18 1.441(4) . ? C16 C18 1.441(4) 3_775 ? N3 C132 1.126(14) . ? N3 C131 1.172(14) . ? N3 Fe 2.075(2) . ? C131 C17 1.405(14) . ? C141 N81 1.154(16) . ? C141 C17 1.426(9) . ? C132 C18 1.384(14) . ? C142 N82 1.117(17) . ? C142 C19 1.447(9) . ? C18 C19 1.417(6) 3_775 ? C18 C15 1.474(5) 3_775 ? C19 C18 1.417(6) 3_775 ? N1 Fe 2.114(2) . ? N2 N4 1.371(3) . ? N2 Fe 2.0600(18) . ? N5 N6 1.418(3) . ? Fe N2 2.0600(18) 3_675 ? Fe N3 2.075(2) 3_675 ? Fe N1 2.114(2) 3_675 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 122.6(3) . . ? C3 C2 C1 119.1(3) . . ? C2 C3 C4 119.8(3) . . ? C3 C4 C5 117.8(3) . . ? N1 C5 C4 123.2(2) . . ? N1 C5 C6 111.3(2) . . ? C4 C5 C6 125.4(2) . . ? N2 C6 N5 108.6(2) . . ? N2 C6 C5 120.7(2) . . ? N5 C6 C5 130.6(2) . . ? N4 C7 N5 110.0(2) . . ? N4 C7 C8 125.0(2) . . ? N5 C7 C8 124.9(2) . . ? N7 C8 C9 123.4(2) . . ? N7 C8 C7 115.5(2) . . ? C9 C8 C7 121.2(2) . . ? C10 C9 C8 118.1(3) . . ? C9 C10 C11 119.8(3) . . ? C12 C11 C10 118.2(3) . . ? N7 C12 C11 123.9(3) . . ? N91 C15 N92 36.4(3) . . ? N91 C15 C19 170.7(5) . . ? N92 C15 C19 134.8(5) . . ? N91 C15 C18 131.4(5) . 3_775 ? N92 C15 C18 167.5(5) . 3_775 ? C19 C15 C18 57.5(3) . 3_775 ? C17 C16 C17 180.0000(10) . 3_775 ? C17 C16 C19 120.1(3) . 3_775 ? C17 C16 C19 59.9(3) 3_775 3_775 ? C17 C16 C19 59.9(3) . . ? C17 C16 C19 120.1(3) 3_775 . ? C19 C16 C19 180.0(4) 3_775 . ? C17 C16 C18 61.1(3) . . ? C17 C16 C18 118.9(3) 3_775 . ? C19 C16 C18 59.4(3) 3_775 . ? C19 C16 C18 120.6(3) . . ? C17 C16 C18 118.9(3) . 3_775 ? C17 C16 C18 61.1(3) 3_775 3_775 ? C19 C16 C18 120.6(3) 3_775 3_775 ? C19 C16 C18 59.4(3) . 3_775 ? C18 C16 C18 180.0000(10) . 3_775 ? C132 N3 C131 23.9(5) . . ? C132 N3 Fe 157.7(7) . . ? C131 N3 Fe 149.7(6) . . ? N3 C131 C17 171.7(9) . . ? N81 C141 C17 173.4(8) . . ? C131 C17 C16 123.9(5) . . ? C131 C17 C141 113.1(6) . . ? C16 C17 C141 122.9(4) . . ? N3 C132 C18 171.4(8) . . ? N82 C142 C19 173.8(9) . . ? C132 C18 C19 164.9(6) . 3_775 ? C132 C18 C16 126.8(5) . . ? C19 C18 C16 59.4(3) 3_775 . ? C132 C18 C15 115.7(5) . 3_775 ? C19 C18 C15 61.1(3) 3_775 3_775 ? C16 C18 C15 117.5(3) . 3_775 ? C16 C19 C18 61.2(3) . 3_775 ? C16 C19 C142 123.2(4) . . ? C18 C19 C142 157.5(5) 3_775 . ? C16 C19 C15 119.4(3) . . ? C18 C19 C15 61.4(3) 3_775 . ? C142 C19 C15 117.2(5) . . ? C1 N1 C5 117.4(2) . . ? C1 N1 Fe 126.45(18) . . ? C5 N1 Fe 115.87(16) . . ? C6 N2 N4 109.01(19) . . ? C6 N2 Fe 113.49(16) . . ? N4 N2 Fe 136.83(16) . . ? C7 N4 N2 106.24(19) . . ? C6 N5 C7 106.1(2) . . ? C6 N5 N6 123.5(2) . . ? C7 N5 N6 129.9(2) . . ? C12 N7 C8 116.7(2) . . ? N2 Fe N2 180.00(12) . 3_675 ? N2 Fe N3 93.95(7) . 3_675 ? N2 Fe N3 86.05(7) 3_675 3_675 ? N2 Fe N3 86.05(7) . . ? N2 Fe N3 93.95(7) 3_675 . ? N3 Fe N3 180.00(12) 3_675 . ? N2 Fe N1 101.82(8) . 3_675 ? N2 Fe N1 78.18(8) 3_675 3_675 ? N3 Fe N1 91.77(8) 3_675 3_675 ? N3 Fe N1 88.23(8) . 3_675 ? N2 Fe N1 78.18(8) . . ? N2 Fe N1 101.82(8) 3_675 . ? N3 Fe N1 88.23(8) 3_675 . ? N3 Fe N1 91.77(8) . . ? N1 Fe N1 180.00(10) 3_675 . ? #===END data_10K _database_code_depnum_ccdc_archive 'CCDC 705804' ###################################################################### # # # [Fe(abpt)2(tcpd)] at 10 K # # # ###################################################################### #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2008-10-17 at 10:30:09 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\program files\wingx\files\archive.dat # CIF files read : collect struct _audit_creation_date 2008-10-17T10:30:09-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C34 H20 Fe1 N18' _chemical_formula_sum 'C34 H20 Fe N18' _chemical_formula_weight 736.53 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.2071(8) _cell_length_b 12.1518(6) _cell_length_c 11.8916(5) _cell_angle_alpha 90 _cell_angle_beta 91.495(5) _cell_angle_gamma 90 _cell_volume 1618.92(16) _cell_formula_units_Z 2 _cell_measurement_temperature 10(2) _cell_measurement_reflns_used 3462 _cell_measurement_theta_min 2.9378 _cell_measurement_theta_max 26.3064 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.525 _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 0.90858 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 10(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 8.4221 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_unetI/netI 0.1045 _diffrn_reflns_number 7010 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 26.48 _diffrn_reflns_theta_full 26.48 _diffrn_measured_fraction_theta_full 0.739 _diffrn_measured_fraction_theta_max 0.739 _reflns_number_total 2474 _reflns_number_gt 1514 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _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 'SIR97 (Giacovazzo et al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0203P)^2^+1.4342P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 2474 _refine_ls_number_parameters 297 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0965 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.0865 _refine_ls_wR_factor_gt 0.081 _refine_ls_goodness_of_fit_ref 1.04 _refine_ls_restrained_S_all 1.04 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.333 _refine_diff_density_min -0.296 _refine_diff_density_rms 0.059 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4493(4) 0.7527(4) 0.0324(4) 0.0254(10) Uani 1 1 d . A . C2 C 0.4321(4) 0.6448(4) -0.0015(4) 0.0304(11) Uani 1 1 d . . . C3 C 0.4547(4) 0.6169(4) -0.1113(4) 0.0287(11) Uani 1 1 d . . . C4 C 0.4950(4) 0.6963(3) -0.1844(3) 0.0251(10) Uani 1 1 d . . . C5 C 0.5098(3) 0.8025(3) -0.1441(3) 0.0219(10) Uani 1 1 d . A . C6 C 0.5453(3) 0.8972(3) -0.2090(3) 0.0197(10) Uani 1 1 d . A . C7 C 0.6077(3) 1.0126(3) -0.3347(3) 0.0198(9) Uani 1 1 d . A . C8 C 0.6514(3) 1.0576(3) -0.4398(3) 0.0196(10) Uani 1 1 d . . . C9 C 0.6946(4) 1.1639(3) -0.4462(3) 0.0245(10) Uani 1 1 d . . . C10 C 0.7343(3) 1.2015(3) -0.5475(3) 0.0227(10) Uani 1 1 d . . . C11 C 0.7298(4) 1.1330(3) -0.6405(3) 0.0250(11) Uani 1 1 d . . . C12 C 0.6862(4) 1.0282(3) -0.6265(3) 0.0263(11) Uani 1 1 d . . . C15 C 1.0923(4) 0.8426(3) -0.1002(3) 0.0194(10) Uani 1 1 d . . . C16 C 1.0000 1.0000 0.0000 0.0168(12) Uani 1 2 d S . . N3 N 0.6809(3) 0.9885(3) 0.0310(2) 0.0244(8) Uani 1 1 d . . . C131 C 0.7786(10) 0.9870(8) 0.0005(7) 0.018(3) Uiso 0.50 1 d P A 1 C141 C 0.8773(11) 0.9364(10) -0.1650(9) 0.023(4) Uiso 0.50 1 d P A 1 N81 N 0.8582(8) 0.9018(7) -0.2533(7) 0.026(3) Uiso 0.50 1 d P A 1 N91 N 1.1567(8) 0.7743(9) -0.1150(8) 0.018(3) Uani 0.50 1 d P B 1 C17 C 0.8891(7) 0.9774(5) -0.0538(5) 0.0164(19) Uani 0.50 1 d P A 1 C132 C 0.7783(10) 1.0120(7) 0.0272(7) 0.012(2) Uiso 0.50 1 d P A 2 C142 C 0.8921(10) 0.9118(9) -0.1649(8) 0.010(3) Uiso 0.50 1 d P B 2 N82 N 0.8228(7) 0.8990(6) -0.2349(7) 0.021(2) Uiso 0.50 1 d P B 2 N92 N 1.1016(9) 0.7624(9) -0.1431(8) 0.019(3) Uani 0.50 1 d P B 2 C18 C 0.8938(7) 1.0499(5) 0.0418(5) 0.0119(16) Uiso 0.50 1 d P . 2 C19 C 0.9926(7) 0.9175(6) -0.0850(5) 0.0178(18) Uani 0.50 1 d P . 2 N1 N 0.4867(3) 0.8320(2) -0.0365(2) 0.0182(8) Uani 1 1 d . . . N2 N 0.5403(2) 0.9979(3) -0.1669(2) 0.0198(7) Uani 1 1 d . . . N4 N 0.5793(3) 1.0717(2) -0.2453(2) 0.0213(8) Uani 1 1 d . A . N5 N 0.5872(3) 0.9037(2) -0.3149(2) 0.0220(8) Uani 1 1 d . . . N6 N 0.6160(4) 0.8103(3) -0.3809(3) 0.0286(9) Uani 1 1 d . A . N7 N 0.6464(3) 0.9887(3) -0.5292(2) 0.0237(8) Uani 1 1 d . . . Fe Fe 0.5000 1.0000 0.0000 0.0194(2) Uani 1 2 d S . . H1 H 0.437(3) 0.774(3) 0.105(3) 0.024(11) Uiso 1 1 d . . . H1N H 0.616(5) 0.836(4) -0.452(4) 0.10(2) Uiso 1 1 d . . . H2 H 0.405(3) 0.591(3) 0.053(3) 0.040(12) Uiso 1 1 d . . . H2N H 0.699(4) 0.795(3) -0.357(3) 0.045(15) Uiso 1 1 d . . . H3 H 0.446(3) 0.544(3) -0.139(3) 0.023(11) Uiso 1 1 d . . . H4 H 0.509(3) 0.682(3) -0.269(3) 0.029(10) Uiso 1 1 d . . . H5 H 0.685(3) 0.977(3) -0.687(2) 0.018(10) Uiso 1 1 d . . . H6 H 0.761(3) 1.155(3) -0.710(3) 0.036(11) Uiso 1 1 d . . . H7 H 0.761(3) 1.270(3) -0.560(3) 0.020(11) Uiso 1 1 d . . . H8 H 0.700(3) 1.208(3) -0.391(3) 0.014(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.017(3) 0.029(3) 0.030(2) 0.007(2) 0.0022(19) 0.002(2) C2 0.022(3) 0.028(3) 0.041(3) 0.020(2) 0.008(2) 0.005(2) C3 0.021(3) 0.020(3) 0.046(3) 0.006(2) -0.001(2) 0.003(2) C4 0.019(3) 0.028(3) 0.028(2) 0.006(2) -0.0010(19) 0.006(2) C5 0.016(3) 0.021(3) 0.028(2) 0.0010(19) -0.0006(19) 0.002(2) C6 0.012(3) 0.026(3) 0.021(2) -0.0012(18) 0.0003(18) -0.0031(19) C7 0.017(2) 0.021(3) 0.022(2) 0.0044(19) -0.0023(16) -0.004(2) C8 0.018(3) 0.021(2) 0.019(2) 0.0029(17) -0.0087(18) -0.0004(19) C9 0.025(3) 0.024(3) 0.025(2) 0.000(2) 0.000(2) -0.001(2) C10 0.018(3) 0.022(3) 0.028(2) 0.006(2) 0.000(2) -0.004(2) C11 0.022(3) 0.031(3) 0.022(2) 0.010(2) 0.000(2) 0.001(2) C12 0.028(3) 0.030(3) 0.021(2) 0.0011(19) 0.0023(19) -0.004(2) C15 0.028(3) 0.019(3) 0.012(2) 0.0027(19) 0.0047(19) 0.006(3) C16 0.018(4) 0.018(3) 0.014(2) 0.008(3) 0.007(3) 0.005(3) N3 0.023(2) 0.023(2) 0.0278(16) -0.0059(15) 0.0131(16) 0.0029(18) N91 0.023(8) 0.022(5) 0.007(5) 0.000(3) -0.009(5) 0.009(5) C17 0.014(5) 0.018(5) 0.017(4) -0.002(3) 0.005(4) 0.000(4) N92 0.014(8) 0.025(6) 0.016(5) 0.004(4) -0.009(5) 0.000(5) C19 0.028(5) 0.016(4) 0.009(4) 0.003(3) 0.002(4) 0.005(4) N1 0.007(2) 0.028(2) 0.0198(18) 0.0085(14) -0.0032(15) 0.0018(15) N2 0.0173(19) 0.0178(17) 0.0241(15) 0.0023(17) -0.0025(13) -0.0027(18) N4 0.024(2) 0.022(2) 0.0188(18) 0.0041(15) 0.0026(15) -0.0024(16) N5 0.026(2) 0.017(2) 0.0232(18) -0.0012(15) 0.0028(15) -0.0011(16) N6 0.039(3) 0.021(2) 0.025(2) -0.0020(16) 0.003(2) 0.0005(19) N7 0.025(2) 0.0240(19) 0.0223(16) -0.0020(16) 0.0024(14) -0.0028(18) Fe 0.0150(5) 0.0215(5) 0.0219(4) 0.0021(4) 0.0041(3) 0.0024(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.339(4) . ? C1 C2 1.383(5) . ? C2 C3 1.378(5) . ? C3 C4 1.383(5) . ? C4 C5 1.386(5) . ? C5 N1 1.361(4) . ? C5 C6 1.446(5) . ? C6 N2 1.325(4) . ? C6 N5 1.358(4) . ? C7 N4 1.328(4) . ? C7 N5 1.364(4) . ? C7 C8 1.461(5) . ? C8 N7 1.353(4) . ? C8 C9 1.382(5) . ? C9 C10 1.373(5) . ? C10 C11 1.384(5) . ? C11 C12 1.375(5) . ? C12 N7 1.339(4) . ? C15 N92 1.109(11) . ? C15 N91 1.114(12) . ? C15 C19 1.454(8) . ? C15 C18 1.486(8) 3_775 ? C16 C17 1.408(8) . ? C16 C17 1.408(8) 3_775 ? C16 C19 1.424(7) 3_775 ? C16 C19 1.424(7) . ? C16 C18 1.439(8) . ? C16 C18 1.439(8) 3_775 ? N3 C132 1.133(11) . ? N3 C131 1.159(11) . ? N3 Fe 2.056(3) . ? C131 C17 1.421(12) . ? C141 N81 1.143(14) . ? C141 C17 1.420(13) . ? C132 C18 1.374(12) . ? C142 N82 1.135(14) . ? C142 C19 1.458(13) . ? C18 C19 1.417(10) 3_775 ? C18 C15 1.486(8) 3_775 ? C19 C18 1.417(10) 3_775 ? N1 Fe 2.091(3) . ? N2 N4 1.372(4) . ? N2 Fe 2.047(3) . ? N5 N6 1.422(4) . ? Fe N2 2.047(3) 3_675 ? Fe N3 2.056(3) 3_675 ? Fe N1 2.091(3) 3_675 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.2(4) . . ? C3 C2 C1 118.8(4) . . ? C2 C3 C4 119.7(4) . . ? C3 C4 C5 118.0(4) . . ? N1 C5 C4 123.2(3) . . ? N1 C5 C6 110.7(3) . . ? C4 C5 C6 126.0(3) . . ? N2 C6 N5 108.4(3) . . ? N2 C6 C5 121.2(3) . . ? N5 C6 C5 130.4(3) . . ? N4 C7 N5 109.9(3) . . ? N4 C7 C8 125.1(3) . . ? N5 C7 C8 124.9(3) . . ? N7 C8 C9 122.8(3) . . ? N7 C8 C7 115.7(3) . . ? C9 C8 C7 121.5(3) . . ? C10 C9 C8 118.8(4) . . ? C9 C10 C11 119.7(4) . . ? C12 C11 C10 117.8(4) . . ? N7 C12 C11 124.3(4) . . ? N92 C15 N91 37.2(5) . . ? N92 C15 C19 133.3(8) . . ? N91 C15 C19 169.9(8) . . ? N92 C15 C18 168.8(8) . 3_775 ? N91 C15 C18 132.0(8) . 3_775 ? C19 C15 C18 57.6(4) . 3_775 ? C17 C16 C17 180.0000(10) . 3_775 ? C17 C16 C19 119.4(4) . 3_775 ? C17 C16 C19 60.6(4) 3_775 3_775 ? C17 C16 C19 60.6(4) . . ? C17 C16 C19 119.4(4) 3_775 . ? C19 C16 C19 180.0(5) 3_775 . ? C17 C16 C18 60.6(4) . . ? C17 C16 C18 119.4(4) 3_775 . ? C19 C16 C18 59.3(4) 3_775 . ? C19 C16 C18 120.7(4) . . ? C17 C16 C18 119.4(4) . 3_775 ? C17 C16 C18 60.6(4) 3_775 3_775 ? C19 C16 C18 120.7(4) 3_775 3_775 ? C19 C16 C18 59.3(4) . 3_775 ? C18 C16 C18 180.0000(10) . 3_775 ? C132 N3 C131 22.1(7) . . ? C132 N3 Fe 157.6(5) . . ? C131 N3 Fe 151.5(5) . . ? N3 C131 C17 169.9(10) . . ? N81 C141 C17 174.2(13) . . ? C16 C17 C141 123.4(7) . . ? C16 C17 C131 123.2(6) . . ? C141 C17 C131 113.2(9) . . ? N3 C132 C18 169.7(10) . . ? N82 C142 C19 171.7(12) . . ? C132 C18 C19 165.7(7) . 3_775 ? C132 C18 C16 127.0(7) . . ? C19 C18 C16 59.8(4) 3_775 . ? C132 C18 C15 116.0(7) . 3_775 ? C19 C18 C15 60.1(4) 3_775 3_775 ? C16 C18 C15 116.9(6) . 3_775 ? C18 C19 C16 60.8(4) 3_775 . ? C18 C19 C15 62.3(5) 3_775 . ? C16 C19 C15 120.0(6) . . ? C18 C19 C142 157.3(7) 3_775 . ? C16 C19 C142 121.8(7) . . ? C15 C19 C142 118.0(7) . . ? C1 N1 C5 117.1(3) . . ? C1 N1 Fe 126.7(3) . . ? C5 N1 Fe 116.0(2) . . ? C6 N2 N4 109.2(3) . . ? C6 N2 Fe 113.0(2) . . ? N4 N2 Fe 137.1(2) . . ? C7 N4 N2 106.1(3) . . ? C6 N5 C7 106.3(3) . . ? C6 N5 N6 123.7(3) . . ? C7 N5 N6 129.6(3) . . ? C12 N7 C8 116.7(3) . . ? N2 Fe N2 180.00(19) 3_675 . ? N2 Fe N3 86.08(10) 3_675 3_675 ? N2 Fe N3 93.92(10) . 3_675 ? N2 Fe N3 93.92(10) 3_675 . ? N2 Fe N3 86.08(10) . . ? N3 Fe N3 180.00(18) 3_675 . ? N2 Fe N1 78.65(12) 3_675 3_675 ? N2 Fe N1 101.35(12) . 3_675 ? N3 Fe N1 92.04(12) 3_675 3_675 ? N3 Fe N1 87.96(12) . 3_675 ? N2 Fe N1 101.35(12) 3_675 . ? N2 Fe N1 78.65(12) . . ? N3 Fe N1 87.96(12) 3_675 . ? N3 Fe N1 92.04(12) . . ? N1 Fe N1 180 3_675 . ? #===END data_10K_irr _database_code_depnum_ccdc_archive 'CCDC 705805' ###################################################################### # # # [Fe(abpt)2(tcpd)] at 10 K after irradiation at 534 nm # # # ###################################################################### #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2008-09-15 at 08:17:40 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.3 # Request file : c:\program files\wingx\files\archive.dat # CIF files read : collect struct _audit_creation_date 2008-09-15T08:17:40-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C34 H20 Fe1 N18' _chemical_formula_sum 'C34 H20 Fe N18' _chemical_formula_weight 736.53 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.3894(8) _cell_length_b 12.1165(4) _cell_length_c 11.8384(4) _cell_angle_alpha 90 _cell_angle_beta 92.832(4) _cell_angle_gamma 90 _cell_volume 1631.70(14) _cell_formula_units_Z 2 _cell_measurement_temperature 10(2) _cell_measurement_reflns_used 3462 _cell_measurement_theta_min 2.9378 _cell_measurement_theta_max 26.3064 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.52 _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 0.90858 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 10(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 8.4221 _diffrn_orient_matrix_ub_11 0.0158039796 _diffrn_orient_matrix_ub_12 -0.0565078239 _diffrn_orient_matrix_ub_13 -0.0012570447 _diffrn_orient_matrix_ub_21 0.008405415 _diffrn_orient_matrix_ub_22 0.0000342591 _diffrn_orient_matrix_ub_23 0.0596667705 _diffrn_orient_matrix_ub_31 -0.0596262315 _diffrn_orient_matrix_ub_32 -0.0149877477 _diffrn_orient_matrix_ub_33 0.0049928758 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_unetI/netI 0.0585 _diffrn_reflns_number 6258 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 26.36 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.703 _diffrn_measured_fraction_theta_max 0.703 _reflns_number_total 2337 _reflns_number_gt 1747 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _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 'SIR97 (Giacovazzo et al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0176P)^2^+3.1516P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 2337 _refine_ls_number_parameters 288 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0729 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.0935 _refine_ls_wR_factor_gt 0.0892 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.144 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.423 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.06 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4457(3) 0.7452(3) 0.0255(3) 0.0161(10) Uani 1 1 d . A . C2 C 0.4280(3) 0.6375(3) -0.0112(3) 0.0186(10) Uani 1 1 d . . . C3 C 0.4524(4) 0.6117(3) -0.1206(3) 0.0201(10) Uani 1 1 d . . . C4 C 0.4935(3) 0.6918(3) -0.1915(3) 0.0164(9) Uani 1 1 d . . . C5 C 0.5081(3) 0.7979(3) -0.1490(3) 0.0152(9) Uani 1 1 d . A . C6 C 0.5456(3) 0.8936(3) -0.2136(3) 0.0140(9) Uani 1 1 d . A . C7 C 0.6093(3) 1.0086(3) -0.3380(3) 0.0124(9) Uani 1 1 d . A . C8 C 0.6532(3) 1.0529(3) -0.4430(3) 0.0129(9) Uani 1 1 d . . . C9 C 0.6984(3) 1.1591(3) -0.4484(3) 0.0157(10) Uani 1 1 d . . . H9 H 0.7025 1.2055 -0.3836 0.019 Uiso 1 1 calc R . . C10 C 0.7368(4) 1.1953(3) -0.5502(3) 0.0160(10) Uani 1 1 d . . . C11 C 0.7295(4) 1.1259(3) -0.6431(3) 0.0177(10) Uani 1 1 d . . . C12 C 0.6842(3) 1.0215(3) -0.6297(3) 0.0174(10) Uani 1 1 d . . . C15 C 1.0913(3) 0.8443(3) -0.1025(3) 0.0102(9) Uani 1 1 d . . . C16 C 1.0000 1.0000 0.0000 0.0117(14) Uani 1 2 d S . . N3 N 0.6882(3) 0.9826(2) 0.0361(2) 0.0155(8) Uani 1 1 d . . . C131 C 0.7790(9) 0.9837(7) 0.0011(7) 0.013(2) Uiso 0.50 1 d P A 1 C141 C 0.8695(10) 0.9328(8) -0.1668(9) 0.015(3) Uiso 0.50 1 d P A 1 N81 N 0.8520(8) 0.8993(6) -0.2555(7) 0.019(2) Uiso 0.50 1 d P A 1 N91 N 1.1593(7) 0.7790(5) -0.1180(5) 0.0149(16) Uiso 0.50 1 d P B 1 C17 C 0.8854(8) 0.9746(5) -0.0540(6) 0.0108(18) Uani 0.50 1 d P A 1 C132 C 0.7859(9) 1.0072(7) 0.0317(7) 0.008(2) Uiso 0.50 1 d P A 2 C142 C 0.8957(10) 0.9106(7) -0.1646(8) 0.008(3) Uiso 0.50 1 d P B 2 N82 N 0.8236(8) 0.8960(6) -0.2354(8) 0.016(2) Uiso 0.50 1 d P B 2 N92 N 1.0991(7) 0.7633(5) -0.1472(5) 0.0146(16) Uiso 0.50 1 d P B 2 C18 C 0.9004(8) 1.0498(5) 0.0441(6) 0.011(2) Uani 0.50 1 d P . 2 C19 C 0.9940(7) 0.9193(6) -0.0854(6) 0.011(2) Uani 0.50 1 d P . 2 N1 N 0.4845(3) 0.8252(2) -0.0415(2) 0.0120(8) Uani 1 1 d . . . N2 N 0.5412(2) 0.9951(2) -0.1720(2) 0.0134(7) Uani 1 1 d . . . N4 N 0.5815(3) 1.0682(2) -0.2499(2) 0.0141(8) Uani 1 1 d . A . N5 N 0.5876(3) 0.8994(2) -0.3181(2) 0.0131(8) Uani 1 1 d . . . N6 N 0.6166(4) 0.8050(2) -0.3825(3) 0.0174(9) Uani 1 1 d . A . N7 N 0.6450(3) 0.9837(2) -0.5325(2) 0.0153(8) Uani 1 1 d . . . Fe Fe 0.5000 1.0000 0.0000 0.0143(2) Uani 1 2 d S . . H1 H 0.430(3) 0.766(3) 0.095(3) 0.016(10) Uiso 1 1 d . . . H1N H 0.614(4) 0.827(3) -0.450(4) 0.032(14) Uiso 1 1 d . . . H2 H 0.398(3) 0.581(3) 0.041(3) 0.025(10) Uiso 1 1 d . . . H2N H 0.708(4) 0.797(3) -0.360(3) 0.033(13) Uiso 1 1 d . . . H3 H 0.441(3) 0.538(3) -0.150(3) 0.015(10) Uiso 1 1 d . . . H4 H 0.508(3) 0.681(3) -0.269(3) 0.015(9) Uiso 1 1 d . . . H5 H 0.681(3) 0.968(3) -0.689(3) 0.010(9) Uiso 1 1 d . . . H6 H 0.761(4) 1.144(3) -0.707(3) 0.038(13) Uiso 1 1 d . . . H7 H 0.768(3) 1.263(3) -0.560(3) 0.010(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.008(3) 0.024(2) 0.016(2) 0.0023(18) -0.0007(19) -0.0011(18) C2 0.009(3) 0.020(2) 0.026(2) 0.0081(18) 0.000(2) 0.0005(18) C3 0.012(3) 0.016(2) 0.031(2) 0.0005(18) -0.003(2) 0.0001(17) C4 0.010(3) 0.020(2) 0.019(2) 0.0007(17) -0.0007(19) 0.0037(17) C5 0.007(3) 0.0189(19) 0.020(2) -0.0007(16) -0.0017(19) 0.0011(17) C6 0.007(3) 0.016(2) 0.018(2) -0.0024(16) 0.0006(19) -0.0017(17) C7 0.005(2) 0.0148(18) 0.0172(19) -0.0009(17) -0.0008(17) -0.0008(18) C8 0.007(3) 0.0169(18) 0.0142(19) 0.0000(15) -0.0049(18) 0.0035(17) C9 0.011(3) 0.0158(19) 0.020(2) -0.0001(16) 0.0001(19) 0.0050(17) C10 0.012(3) 0.0154(19) 0.020(2) 0.0034(17) 0.0006(19) -0.0009(18) C11 0.014(3) 0.025(2) 0.015(2) 0.0049(18) 0.002(2) 0.0060(18) C12 0.015(3) 0.020(2) 0.017(2) 0.0010(17) 0.0031(19) 0.0030(17) C15 0.011(3) 0.0146(18) 0.0052(17) 0.0022(15) -0.0012(17) -0.0014(17) C16 0.017(4) 0.009(2) 0.010(2) 0.004(2) 0.004(3) 0.001(3) N3 0.014(2) 0.0167(16) 0.0153(16) -0.0013(13) -0.0005(17) 0.0004(15) C17 0.009(6) 0.010(4) 0.013(4) -0.006(3) -0.005(4) 0.000(3) C18 0.017(6) 0.013(3) 0.005(4) -0.003(3) 0.004(4) -0.003(4) C19 0.013(6) 0.015(4) 0.006(4) 0.000(3) 0.004(4) -0.005(4) N1 0.002(2) 0.0189(16) 0.0147(16) 0.0031(13) -0.0036(15) 0.0010(14) N2 0.008(2) 0.0154(14) 0.0169(15) 0.0033(15) 0.0008(14) -0.0019(15) N4 0.011(2) 0.0169(16) 0.0147(17) 0.0026(13) 0.0024(16) 0.0000(14) N5 0.008(2) 0.0148(16) 0.0163(17) -0.0026(13) 0.0024(15) -0.0011(14) N6 0.021(3) 0.0148(16) 0.017(2) -0.0052(15) 0.0035(18) -0.0001(15) N7 0.013(2) 0.0154(16) 0.0183(16) -0.0036(13) 0.0033(15) 0.0004(14) Fe 0.0097(6) 0.0164(4) 0.0169(4) 0.0031(4) 0.0019(4) -0.0012(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.341(4) . ? C1 C2 1.387(5) . ? C2 C3 1.375(5) . ? C3 C4 1.380(5) . ? C4 C5 1.388(5) . ? C5 N1 1.355(4) . ? C5 C6 1.465(5) . ? C6 N2 1.326(4) . ? C6 N5 1.350(4) . ? C7 N4 1.320(4) . ? C7 N5 1.368(4) . ? C7 C8 1.464(5) . ? C8 N7 1.350(4) . ? C8 C9 1.389(5) . ? C9 C10 1.374(5) . ? C10 C11 1.384(5) . ? C11 C12 1.378(5) . ? C12 N7 1.336(4) . ? C15 N92 1.120(7) . ? C15 N91 1.131(7) . ? C15 C19 1.455(8) . ? C15 C18 1.457(8) 3_775 ? C16 C18 1.407(7) . ? C16 C18 1.407(7) 3_775 ? C16 C19 1.407(7) . ? C16 C19 1.407(7) 3_775 ? C16 C17 1.457(9) . ? C16 C17 1.457(9) 3_775 ? N3 C131 1.134(10) . ? N3 C132 1.155(10) . ? N3 Fe 2.175(3) . ? C131 C17 1.407(12) . ? C141 N81 1.135(15) . ? C141 C17 1.431(13) . ? C132 C18 1.407(13) . ? C142 N82 1.157(14) . ? C142 C19 1.427(13) . ? C18 C19 1.330(11) 3_775 ? C18 C15 1.457(8) 3_775 ? C19 C18 1.330(11) 3_775 ? N1 Fe 2.179(3) . ? N2 N4 1.374(4) . ? N2 Fe 2.113(3) . ? N5 N6 1.423(4) . ? Fe N2 2.113(3) 3_675 ? Fe N3 2.175(3) 3_675 ? Fe N1 2.179(3) 3_675 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 122.9(3) . . ? C3 C2 C1 118.4(3) . . ? C2 C3 C4 120.2(4) . . ? C3 C4 C5 118.0(3) . . ? N1 C5 C4 122.7(3) . . ? N1 C5 C6 112.0(3) . . ? C4 C5 C6 125.2(3) . . ? N2 C6 N5 108.3(3) . . ? N2 C6 C5 121.5(3) . . ? N5 C6 C5 130.2(3) . . ? N4 C7 N5 109.9(3) . . ? N4 C7 C8 125.1(3) . . ? N5 C7 C8 124.9(3) . . ? N7 C8 C9 123.4(3) . . ? N7 C8 C7 115.2(3) . . ? C9 C8 C7 121.4(3) . . ? C10 C9 C8 118.1(3) . . ? C9 C10 C11 119.6(4) . . ? C12 C11 C10 118.3(3) . . ? N7 C12 C11 123.8(3) . . ? N92 C15 N91 40.3(4) . . ? N92 C15 C19 133.8(7) . . ? N91 C15 C19 173.8(6) . . ? N92 C15 C18 171.7(7) . 3_775 ? N91 C15 C18 131.6(7) . 3_775 ? C19 C15 C18 54.3(4) . 3_775 ? C18 C16 C18 180.0000(10) . 3_775 ? C18 C16 C19 123.6(4) . . ? C18 C16 C19 56.4(4) 3_775 . ? C18 C16 C19 56.4(4) . 3_775 ? C18 C16 C19 123.6(4) 3_775 3_775 ? C19 C16 C19 180.0(6) . 3_775 ? C18 C16 C17 62.2(4) . . ? C18 C16 C17 117.8(4) 3_775 . ? C19 C16 C17 61.7(4) . . ? C19 C16 C17 118.3(4) 3_775 . ? C18 C16 C17 117.8(4) . 3_775 ? C18 C16 C17 62.2(4) 3_775 3_775 ? C19 C16 C17 118.3(4) . 3_775 ? C19 C16 C17 61.7(4) 3_775 3_775 ? C17 C16 C17 180.0000(10) . 3_775 ? C131 N3 C132 23.4(6) . . ? C131 N3 Fe 146.6(5) . . ? C132 N3 Fe 155.2(4) . . ? N3 C131 C17 172.2(11) . . ? N81 C141 C17 177.4(12) . . ? C131 C17 C141 112.6(9) . . ? C131 C17 C16 123.6(7) . . ? C141 C17 C16 123.7(7) . . ? N3 C132 C18 168.9(9) . . ? N82 C142 C19 172.3(11) . . ? C19 C18 C16 61.8(5) 3_775 . ? C19 C18 C132 164.0(7) 3_775 . ? C16 C18 C132 124.3(6) . . ? C19 C18 C15 62.8(5) 3_775 3_775 ? C16 C18 C15 121.3(6) . 3_775 ? C132 C18 C15 114.3(6) . 3_775 ? C18 C19 C16 61.8(5) 3_775 . ? C18 C19 C142 158.0(7) 3_775 . ? C16 C19 C142 122.1(7) . . ? C18 C19 C15 62.9(5) 3_775 . ? C16 C19 C15 121.5(7) . . ? C142 C19 C15 116.3(7) . . ? C1 N1 C5 117.7(3) . . ? C1 N1 Fe 126.5(2) . . ? C5 N1 Fe 115.5(2) . . ? C6 N2 N4 109.2(3) . . ? C6 N2 Fe 113.4(2) . . ? N4 N2 Fe 136.6(2) . . ? C7 N4 N2 106.2(3) . . ? C6 N5 C7 106.5(3) . . ? C6 N5 N6 123.5(3) . . ? C7 N5 N6 129.5(3) . . ? C12 N7 C8 116.7(3) . . ? N2 Fe N2 180.0000(10) . 3_675 ? N2 Fe N3 94.41(11) . 3_675 ? N2 Fe N3 85.59(11) 3_675 3_675 ? N2 Fe N3 85.59(11) . . ? N2 Fe N3 94.41(11) 3_675 . ? N3 Fe N3 180 3_675 . ? N2 Fe N1 77.00(10) . . ? N2 Fe N1 103.00(10) 3_675 . ? N3 Fe N1 88.98(11) 3_675 . ? N3 Fe N1 91.02(11) . . ? N2 Fe N1 103.00(10) . 3_675 ? N2 Fe N1 77.00(10) 3_675 3_675 ? N3 Fe N1 91.02(11) 3_675 3_675 ? N3 Fe N1 88.98(11) . 3_675 ? N1 Fe N1 180.00(14) . 3_675 ? #===END