data_33_cryst_1 #local ID: mo33 _publ_requested_journal Inorg.Chem. _publ_contact_author_name 'Professor W. Robert Scheidt' _publ_contact_author_address ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; _publ_contact_author_email W.R.Scheidt.1@nd.edu _publ_contact_author_phone 1(574)6315939 _publ_contact_author_fax 1(574)6316652 loop_ _publ_author_name _publ_author_address 'Scheidt, W. Robert ' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Silvernail, Nathan J.' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Noll, Bruce C.' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Olmstead, Marilyn M.' ;University of California at Davis Department of Chemistry One Shields Avenue Davis, CA 95616 ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common [Fe(TPP)(NO] _chemical_melting_point ? _chemical_formula_moiety 'C44 H28 Fe N5 O' _chemical_formula_sum 'C44 H28 Fe N5 O' _chemical_formula_weight 698.56 _chemical_compound_source synthesized loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' .3463 .8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.745(2) _cell_length_b 9.867(2) _cell_length_c 10.375(3) _cell_angle_alpha 82.66(2) _cell_angle_beta 66.010(2) _cell_angle_gamma 70.05(2) _cell_volume 856.7(4) _cell_formula_units_Z 1 _cell_measurement_temperature 33(2) _cell_measurement_reflns_used 2647 _cell_measurement_theta_min 3.0978 _cell_measurement_theta_max 24.9878 _exptl_crystal_description 'square bipyramid' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 361 _exptl_absorpt_coefficient_mu 0.484 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9052 _exptl_absorpt_correction_T_max 0.9623 _exptl_absorpt_process_details 'Blessing, R.H. ACTA Cryst. (1995) A51, 33-38' _exptl_crystal_recrystallization_method 'liquid diffusion (chloroform/methanol)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 33(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4221 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1199 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4221 _reflns_number_gt 2476 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Platon (Spek, 2004)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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. The structures were solved by direct methods using SHELXS-97 and refined against F^2^ using SHELXL-97;subsequent difference Fourier syntheses led to the location of most of the remaining non-hydrogen atoms. For the structure refinement all data were used including negative intensities. All nonhydrogen atoms were refined anisotropically. Hydrogen atoms were idealized with the standard SHELXL-97 idealization methods. Hydrogen atoms were placed at calculated geometries and allowed to ride on the position of the parent atom. Hydrogen thermal parameters were set to 1.2\\times the equivalent isotropic U of the parent atom, 1.5\\times for methyl hydrogens. The program SADABS was applied for the absorption correction. The structure is a tetraphenyl porphyrin bound axially by a nitrosyl. Crystal twin not merged, so ratio of unique / expected reflections is greater than 1. Second component of twin is rotated from first domain by 179.9 degrees about reciprocal axis 1.000 0.499 0.498 and real axis 1.000 0.177 0.078 Twin law to convert hkl from first to 0.775 0.313 0.138 this domain (SHELXL TWIN matrix): 0.886 -0.844 0.068 0.884 0.158 -0.931 ; _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^)+(0.0648P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4221 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0940 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.0884 _refine_ls_wR_factor_gt 0.0806 _refine_ls_goodness_of_fit_ref 0.827 _refine_ls_restrained_S_all 0.827 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.4811(7) 0.4971(9) 0.4985(9) 0.0146(7) Uani 0.50 1 d P . . N1 N 0.4642(2) 0.6814(2) 0.3923(2) 0.0147(5) Uani 1 1 d . . . N2 N 0.3571(3) 0.6095(2) 0.67951(19) 0.0153(5) Uani 1 1 d . . . C(M1 C 0.6313(3) 0.5875(3) 0.1493(2) 0.0152(6) Uani 1 1 d . . . C(M2 C 0.2814(3) 0.8561(3) 0.5877(2) 0.0134(6) Uani 1 1 d . . . C(A1 C 0.5281(3) 0.6986(3) 0.2469(2) 0.0155(6) Uani 1 1 d . . . C(A2 C 0.3689(3) 0.8190(3) 0.4448(3) 0.0157(6) Uani 1 1 d . . . C(A3 C 0.2790(3) 0.7565(3) 0.6961(2) 0.0145(6) Uani 1 1 d . . . C(A4 C 0.3166(3) 0.5565(3) 0.8149(2) 0.0153(6) Uani 1 1 d . . . C(B1 C 0.4726(3) 0.8464(3) 0.2107(3) 0.0190(6) Uani 1 1 d . . . H(BA H 0.4997 0.8851 0.1184 0.023 Uiso 1 1 calc R . . C(B2 C 0.3742(3) 0.9206(3) 0.3330(2) 0.0176(6) Uani 1 1 d . . . H(BB H 0.3190 1.0213 0.3427 0.021 Uiso 1 1 calc R . . C(B3 C 0.1910(3) 0.7945(3) 0.8430(2) 0.0177(6) Uani 1 1 d . . . H(BC H 0.1283 0.8885 0.8816 0.021 Uiso 1 1 calc R . . C(B4 C 0.2145(3) 0.6707(3) 0.9159(2) 0.0183(6) Uani 1 1 d . . . H(BD H 0.1714 0.6614 1.0155 0.022 Uiso 1 1 calc R . . C10 C 0.6924(3) 0.6269(2) -0.0040(2) 0.0138(6) Uani 1 1 d . . . C11 C 0.8411(3) 0.6458(3) -0.0682(3) 0.0193(7) Uani 1 1 d . . . H11A H 0.9037 0.6342 -0.0148 0.023 Uiso 1 1 calc R . . C12 C 0.8985(3) 0.6816(3) -0.2106(3) 0.0196(7) Uani 1 1 d . . . H12A H 0.9997 0.6947 -0.2537 0.024 Uiso 1 1 calc R . . C13 C 0.8081(3) 0.6981(2) -0.2892(2) 0.0195(7) Uani 1 1 d . . . H13A H 0.8481 0.7203 -0.3866 0.023 Uiso 1 1 calc R . . C14 C 0.6593(3) 0.6821(3) -0.2252(3) 0.0227(7) Uani 1 1 d . . . H14A H 0.5962 0.6951 -0.2783 0.027 Uiso 1 1 calc R . . C15 C 0.6017(3) 0.6468(3) -0.0829(3) 0.0203(7) Uani 1 1 d . . . H15A H 0.4993 0.6364 -0.0397 0.024 Uiso 1 1 calc R . . C20 C 0.1827(3) 1.0105(3) 0.6267(2) 0.0133(6) Uani 1 1 d . . . C21 C 0.0223(3) 1.0567(3) 0.6517(3) 0.0217(7) Uani 1 1 d . . . H21A H -0.0250 0.9899 0.6442 0.026 Uiso 1 1 calc R . . C22 C -0.0695(3) 1.1995(3) 0.6876(3) 0.0231(7) Uani 1 1 d . . . H22A H -0.1789 1.2298 0.7043 0.028 Uiso 1 1 calc R . . C23 C -0.0021(3) 1.2979(3) 0.6993(2) 0.0205(7) Uani 1 1 d . . . H23A H -0.0649 1.3957 0.7234 0.025 Uiso 1 1 calc R . . C24 C 0.1566(3) 1.2531(3) 0.6756(3) 0.0273(7) Uani 1 1 d . . . H24A H 0.2032 1.3198 0.6845 0.033 Uiso 1 1 calc R . . C25 C 0.2482(3) 1.1104(3) 0.6389(3) 0.0253(7) Uani 1 1 d . . . H25A H 0.3577 1.0807 0.6217 0.030 Uiso 1 1 calc R . . N3 N 0.3092(5) 0.4894(4) 0.4901(4) 0.0166(10) Uani 0.50 1 d P . . O1 O 0.1804(4) 0.5563(4) 0.5027(4) 0.0214(9) Uani 0.50 1 d 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 Fe1 0.022(2) 0.0127(6) 0.0105(4) 0.0003(4) -0.0061(16) -0.0070(15) N1 0.0170(13) 0.0109(12) 0.0127(11) 0.0000(9) -0.0044(10) -0.0017(10) N2 0.0175(13) 0.0124(12) 0.0116(11) 0.0043(9) -0.0053(10) -0.0013(10) C(M1 0.0166(15) 0.0172(14) 0.0118(13) 0.0030(10) -0.0056(12) -0.0062(12) C(M2 0.0126(14) 0.0131(14) 0.0147(13) 0.0000(10) -0.0058(12) -0.0036(11) C(A1 0.0159(15) 0.0176(15) 0.0103(13) 0.0023(11) -0.0031(12) -0.0053(12) C(A2 0.0123(14) 0.0169(14) 0.0174(13) -0.0005(11) -0.0044(12) -0.0052(12) C(A3 0.0159(15) 0.0126(14) 0.0136(13) 0.0010(11) -0.0066(12) -0.0020(12) C(A4 0.0133(15) 0.0165(14) 0.0135(13) 0.0009(10) -0.0038(12) -0.0038(12) C(B1 0.0189(16) 0.0170(15) 0.0173(14) 0.0043(11) -0.0066(13) -0.0032(12) C(B2 0.0213(16) 0.0119(14) 0.0185(14) 0.0038(11) -0.0070(13) -0.0065(12) C(B3 0.0165(15) 0.0139(14) 0.0173(14) -0.0024(11) -0.0055(12) 0.0012(12) C(B4 0.0199(16) 0.0191(15) 0.0124(13) 0.0003(11) -0.0064(12) -0.0021(13) C10 0.0173(15) 0.0115(13) 0.0087(12) 0.0021(10) -0.0048(12) -0.0011(12) C11 0.0180(15) 0.0200(15) 0.0169(14) 0.0004(11) -0.0071(12) -0.0020(12) C12 0.0193(16) 0.0203(16) 0.0155(14) 0.0003(12) -0.0027(13) -0.0069(12) C13 0.0299(17) 0.0090(13) 0.0108(13) 0.0001(10) -0.0011(13) -0.0041(12) C14 0.0363(18) 0.0208(16) 0.0179(15) 0.0038(12) -0.0180(14) -0.0096(14) C15 0.0227(16) 0.0223(16) 0.0177(15) 0.0035(12) -0.0083(13) -0.0102(13) C20 0.0184(16) 0.0145(14) 0.0066(12) 0.0022(10) -0.0045(12) -0.0058(12) C21 0.0187(16) 0.0198(16) 0.0311(16) -0.0031(13) -0.0134(13) -0.0059(13) C22 0.0179(16) 0.0194(16) 0.0327(17) -0.0050(13) -0.0121(14) -0.0023(13) C23 0.0267(17) 0.0137(14) 0.0143(13) -0.0018(11) -0.0044(13) -0.0021(13) C24 0.0317(18) 0.0181(16) 0.0389(18) -0.0046(13) -0.0156(15) -0.0120(14) C25 0.0161(16) 0.0282(18) 0.0341(17) -0.0053(14) -0.0095(14) -0.0084(13) N3 0.015(2) 0.014(2) 0.016(2) -0.0016(18) -0.005(2) 0.0010(19) O1 0.024(2) 0.021(2) 0.018(2) 0.0010(16) -0.0085(18) -0.0052(17) _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 Fe1 Fe1 0.405(7) 2_666 ? Fe1 N3 1.739(6) . ? Fe1 N1 1.995(9) . ? Fe1 N2 1.997(9) . ? Fe1 N2 2.000(9) 2_666 ? Fe1 N1 2.004(9) 2_666 ? Fe1 N3 2.143(5) 2_666 ? N1 C(A2 1.385(3) . ? N1 C(A1 1.391(3) . ? N1 Fe1 2.003(9) 2_666 ? N2 C(A4 1.380(3) . ? N2 C(A3 1.385(3) . ? N2 Fe1 2.000(9) 2_666 ? C(M1 C(A1 1.393(3) . ? C(M1 C(A4 1.393(3) 2_666 ? C(M1 C10 1.505(3) . ? C(M2 C(A3 1.394(3) . ? C(M2 C(A2 1.400(3) . ? C(M2 C20 1.500(3) . ? C(A1 C(B1 1.431(3) . ? C(A2 C(B2 1.429(3) . ? C(A3 C(B3 1.436(3) . ? C(A4 C(M1 1.393(3) 2_666 ? C(A4 C(B4 1.430(3) . ? C(B1 C(B2 1.355(3) . ? C(B1 H(BA 0.9500 . ? C(B2 H(BB 0.9500 . ? C(B3 C(B4 1.353(3) . ? C(B3 H(BC 0.9500 . ? C(B4 H(BD 0.9500 . ? C10 C15 1.385(4) . ? C10 C11 1.394(3) . ? C11 C12 1.397(3) . ? C11 H11A 0.9500 . ? C12 C13 1.385(4) . ? C12 H12A 0.9500 . ? C13 C14 1.384(4) . ? C13 H13A 0.9500 . ? C14 C15 1.394(3) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C20 C25 1.386(4) . ? C20 C21 1.391(4) . ? C21 C22 1.388(3) . ? C21 H21A 0.9500 . ? C22 C23 1.385(4) . ? C22 H22A 0.9500 . ? C23 C24 1.378(4) . ? C23 H23A 0.9500 . ? C24 C25 1.388(3) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? N3 O1 1.163(5) . ? N3 Fe1 2.143(5) 2_666 ? 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 Fe1 Fe1 N3 175(3) 2_666 . ? Fe1 Fe1 N1 85(3) 2_666 . ? N3 Fe1 N1 90.9(4) . . ? Fe1 Fe1 N2 85(2) 2_666 . ? N3 Fe1 N2 91.5(3) . . ? N1 Fe1 N2 89.6(4) . . ? Fe1 Fe1 N2 84(2) 2_666 2_666 ? N3 Fe1 N2 100.1(4) . 2_666 ? N1 Fe1 N2 89.5(4) . 2_666 ? N2 Fe1 N2 168.4(2) . 2_666 ? Fe1 Fe1 N1 83(3) 2_666 2_666 ? N3 Fe1 N1 100.7(4) . 2_666 ? N1 Fe1 N1 168.4(2) . 2_666 ? N2 Fe1 N1 89.3(4) . 2_666 ? N2 Fe1 N1 89.3(3) 2_666 2_666 ? Fe1 Fe1 N3 4(2) 2_666 2_666 ? N3 Fe1 N3 179.0(5) . 2_666 ? N1 Fe1 N3 88.4(3) . 2_666 ? N2 Fe1 N3 87.7(3) . 2_666 ? N2 Fe1 N3 80.7(3) 2_666 2_666 ? N1 Fe1 N3 80.0(3) 2_666 2_666 ? C(A2 N1 C(A1 104.3(2) . . ? C(A2 N1 Fe1 127.6(3) . . ? C(A1 N1 Fe1 127.6(3) . . ? C(A2 N1 Fe1 127.8(3) . 2_666 ? C(A1 N1 Fe1 127.5(3) . 2_666 ? C(A4 N2 C(A3 104.8(2) . . ? C(A4 N2 Fe1 127.7(3) . . ? C(A3 N2 Fe1 127.2(3) . . ? C(A4 N2 Fe1 127.4(3) . 2_666 ? C(A3 N2 Fe1 127.2(3) . 2_666 ? C(A1 C(M1 C(A4 124.2(2) . 2_666 ? C(A1 C(M1 C10 117.6(2) . . ? C(A4 C(M1 C10 118.2(2) 2_666 . ? C(A3 C(M2 C(A2 123.4(2) . . ? C(A3 C(M2 C20 118.1(2) . . ? C(A2 C(M2 C20 118.5(2) . . ? N1 C(A1 C(M1 124.9(2) . . ? N1 C(A1 C(B1 110.7(2) . . ? C(M1 C(A1 C(B1 124.4(2) . . ? N1 C(A2 C(M2 125.3(2) . . ? N1 C(A2 C(B2 110.9(2) . . ? C(M2 C(A2 C(B2 123.8(2) . . ? N2 C(A3 C(M2 126.0(2) . . ? N2 C(A3 C(B3 110.50(19) . . ? C(M2 C(A3 C(B3 123.5(2) . . ? N2 C(A4 C(M1 125.4(2) . 2_666 ? N2 C(A4 C(B4 110.7(2) . . ? C(M1 C(A4 C(B4 123.9(2) 2_666 . ? C(B2 C(B1 C(A1 107.0(2) . . ? C(B2 C(B1 H(BA 126.5 . . ? C(A1 C(B1 H(BA 126.5 . . ? C(B1 C(B2 C(A2 107.1(2) . . ? C(B1 C(B2 H(BB 126.5 . . ? C(A2 C(B2 H(BB 126.5 . . ? C(B4 C(B3 C(A3 106.8(2) . . ? C(B4 C(B3 H(BC 126.6 . . ? C(A3 C(B3 H(BC 126.6 . . ? C(B3 C(B4 C(A4 107.2(2) . . ? C(B3 C(B4 H(BD 126.4 . . ? C(A4 C(B4 H(BD 126.4 . . ? C15 C10 C11 119.0(2) . . ? C15 C10 C(M1 120.8(2) . . ? C11 C10 C(M1 120.2(2) . . ? C10 C11 C12 120.4(3) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C13 C12 C11 120.1(3) . . ? C13 C12 H12A 119.9 . . ? C11 C12 H12A 119.9 . . ? C14 C13 C12 119.7(2) . . ? C14 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? C13 C14 C15 120.2(3) . . ? C13 C14 H14A 119.9 . . ? C15 C14 H14A 119.9 . . ? C10 C15 C14 120.6(3) . . ? C10 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? C25 C20 C21 118.3(2) . . ? C25 C20 C(M2 121.3(2) . . ? C21 C20 C(M2 120.4(2) . . ? C22 C21 C20 120.6(3) . . ? C22 C21 H21A 119.7 . . ? C20 C21 H21A 119.7 . . ? C23 C22 C21 120.3(3) . . ? C23 C22 H22A 119.9 . . ? C21 C22 H22A 119.9 . . ? C24 C23 C22 119.6(2) . . ? C24 C23 H23A 120.2 . . ? C22 C23 H23A 120.2 . . ? C23 C24 C25 120.0(3) . . ? C23 C24 H24A 120.0 . . ? C25 C24 H24A 120.0 . . ? C20 C25 C24 121.2(3) . . ? C20 C25 H25A 119.4 . . ? C24 C25 H25A 119.4 . . ? O1 N3 Fe1 144.4(5) . . ? O1 N3 Fe1 143.3(4) . 2_666 ? _diffrn_measured_fraction_theta_max .958 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full .958 _refine_diff_density_max .423 _refine_diff_density_min -.545 _refine_diff_density_rms .082 #===END data_90_cryst_1 #local ID: mo90 _publ_requested_journal Inorg.Chem. _publ_contact_author_name 'Professor W. Robert Scheidt' _publ_contact_author_address ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; _publ_contact_author_email W.R.Scheidt.1@nd.edu _publ_contact_author_phone 1(574)6315939 _publ_contact_author_fax 1(574)6316652 loop_ _publ_author_name _publ_author_address 'Scheidt, W. Robert ' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Silvernail, Nathan J.' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Noll, Bruce C.' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Olmstead, Marilyn M.' ;University of California at Davis Department of Chemistry One Shields Avenue Davis, CA 95616 ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common [Fe(TPP)(NO] _chemical_melting_point ? _chemical_formula_moiety 'C44 H28 Fe N5 O' _chemical_formula_sum 'C44 H28 Fe N5 O' _chemical_formula_weight 698.56 _chemical_compound_source synthesized loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' .3463 .8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.754(2) _cell_length_b 9.943(2) _cell_length_c 10.394(3) _cell_angle_alpha 82.25(2) _cell_angle_beta 65.78(2) _cell_angle_gamma 69.44(2) _cell_volume 860.7(4) _cell_formula_units_Z 1 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'square bipyramid' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 361 _exptl_absorpt_coefficient_mu 0.481 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9057 _exptl_absorpt_correction_T_max 0.9625 _exptl_absorpt_process_details 'Blessing, R.H. ACTA Cryst. (1995) A51, 33-38' _exptl_crystal_recrystallization_method 'liquid diffusion (chloroform/methanol)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4337 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0795 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.71 _reflns_number_total 4337 _reflns_number_gt 2843 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Platon (Spek, 2004)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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. The structures were solved by direct methods using SHELXS-97 and refined against F^2^ using SHELXL-97;subsequent difference Fourier syntheses led to the location of most of the remaining non-hydrogen atoms. For the structure refinement all data were used including negative intensities. All nonhydrogen atoms were refined anisotropically. Hydrogen atoms were idealized with the standard SHELXL-97 idealization methods. Hydrogen atoms were placed at calculated geometries and allowed to ride on the position of the parent atom. Hydrogen thermal parameters were set to 1.2\\times the equivalent isotropic U of the parent atom, 1.5\\times for methyl hydrogens. The program SADABS was applied for the absorption correction. The structure is a tetraphenyl porphyrin bound axially by a nitrosyl. ; _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^)+(0.0648P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4337 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0792 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1174 _refine_ls_wR_factor_gt 0.1084 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.4801(5) 0.4983(7) 0.4996(7) 0.0196(5) Uani 0.50 1 d P . . N1 N 0.4632(2) 0.68161(18) 0.39282(19) 0.0200(4) Uani 1 1 d . . . N2 N 0.3569(2) 0.60885(18) 0.67908(19) 0.0200(4) Uani 1 1 d . . . C(M1 C 0.6311(3) 0.5886(2) 0.1495(2) 0.0207(5) Uani 1 1 d . . . C(M2 C 0.2809(3) 0.8545(2) 0.5876(2) 0.0204(5) Uani 1 1 d . . . C(A1 C 0.5269(3) 0.6981(2) 0.2478(2) 0.0216(5) Uani 1 1 d . . . C(A2 C 0.3685(3) 0.8177(2) 0.4459(2) 0.0214(5) Uani 1 1 d . . . C(A3 C 0.2780(3) 0.7553(2) 0.6961(2) 0.0223(5) Uani 1 1 d . . . C(A4 C 0.3168(3) 0.5555(2) 0.8143(2) 0.0220(5) Uani 1 1 d . . . C(B1 C 0.4713(3) 0.8458(2) 0.2116(2) 0.0255(5) Uani 1 1 d . . . H(BA H 0.4984 0.8845 0.1192 0.031 Uiso 1 1 calc R . . C(B2 C 0.3731(3) 0.9198(2) 0.3333(2) 0.0239(5) Uani 1 1 d . . . H(BB H 0.3177 1.0202 0.3428 0.029 Uiso 1 1 calc R . . C(B3 C 0.1902(3) 0.7928(2) 0.8432(2) 0.0270(6) Uani 1 1 d . . . H(BC H 0.1281 0.8867 0.8818 0.032 Uiso 1 1 calc R . . C(B4 C 0.2127(3) 0.6696(2) 0.9164(2) 0.0253(5) Uani 1 1 d . . . H(BD H 0.1683 0.6600 1.0160 0.030 Uiso 1 1 calc R . . C10 C 0.6911(3) 0.6278(2) -0.0037(2) 0.0212(5) Uani 1 1 d . . . C11 C 0.8386(3) 0.6462(3) -0.0685(3) 0.0283(6) Uani 1 1 d . . . H11A H 0.9013 0.6346 -0.0153 0.034 Uiso 1 1 calc R . . C12 C 0.8962(3) 0.6813(2) -0.2102(3) 0.0296(6) Uani 1 1 d . . . H12A H 0.9976 0.6938 -0.2536 0.036 Uiso 1 1 calc R . . C13 C 0.8053(3) 0.6981(2) -0.2885(2) 0.0273(6) Uani 1 1 d . . . H13A H 0.8448 0.7207 -0.3858 0.033 Uiso 1 1 calc R . . C14 C 0.6577(3) 0.6817(3) -0.2243(3) 0.0334(6) Uani 1 1 d . . . H14A H 0.5945 0.6946 -0.2772 0.040 Uiso 1 1 calc R . . C15 C 0.6005(3) 0.6464(3) -0.0822(3) 0.0311(6) Uani 1 1 d . . . H15A H 0.4985 0.6350 -0.0387 0.037 Uiso 1 1 calc R . . C20 C 0.1829(3) 1.0092(2) 0.6270(2) 0.0205(5) Uani 1 1 d . . . C21 C 0.0226(3) 1.0579(2) 0.6517(3) 0.0303(6) Uani 1 1 d . . . H21A H -0.0258 0.9928 0.6447 0.036 Uiso 1 1 calc R . . C22 C -0.0682(3) 1.2007(3) 0.6866(3) 0.0338(6) Uani 1 1 d . . . H22A H -0.1777 1.2328 0.7021 0.041 Uiso 1 1 calc R . . C23 C 0.0000(3) 1.2964(2) 0.6988(2) 0.0283(6) Uani 1 1 d . . . H23A H -0.0619 1.3943 0.7226 0.034 Uiso 1 1 calc R . . C24 C 0.1592(3) 1.2479(3) 0.6761(3) 0.0369(7) Uani 1 1 d . . . H24A H 0.2068 1.3126 0.6853 0.044 Uiso 1 1 calc R . . C25 C 0.2502(3) 1.1054(3) 0.6397(3) 0.0340(6) Uani 1 1 d . . . H25A H 0.3600 1.0736 0.6234 0.041 Uiso 1 1 calc R . . N3 N 0.3085(5) 0.4907(4) 0.4910(4) 0.0198(8) Uani 0.50 1 d P . . O1 O 0.1798(4) 0.5546(4) 0.5029(4) 0.0336(8) Uani 0.50 1 d 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 Fe1 0.0213(19) 0.0187(4) 0.0143(3) 0.0007(2) -0.0038(13) -0.0052(12) N1 0.0198(11) 0.0192(9) 0.0158(10) -0.0001(7) -0.0051(8) -0.0027(8) N2 0.0189(11) 0.0185(9) 0.0167(10) 0.0013(7) -0.0056(9) -0.0016(8) C(M1 0.0214(13) 0.0236(11) 0.0150(11) 0.0030(8) -0.0069(10) -0.0061(10) C(M2 0.0186(13) 0.0208(11) 0.0191(12) -0.0030(9) -0.0066(10) -0.0033(9) C(A1 0.0234(14) 0.0255(12) 0.0144(11) 0.0034(9) -0.0070(10) -0.0078(10) C(A2 0.0188(13) 0.0214(11) 0.0208(12) -0.0007(8) -0.0062(10) -0.0045(10) C(A3 0.0212(14) 0.0224(12) 0.0196(12) -0.0014(9) -0.0074(10) -0.0029(10) C(A4 0.0213(14) 0.0248(12) 0.0171(11) 0.0005(9) -0.0069(10) -0.0052(10) C(B1 0.0288(15) 0.0244(12) 0.0171(12) 0.0037(9) -0.0067(11) -0.0054(10) C(B2 0.0261(14) 0.0204(11) 0.0208(12) 0.0016(9) -0.0085(11) -0.0040(10) C(B3 0.0289(15) 0.0241(12) 0.0191(12) -0.0029(9) -0.0063(11) -0.0009(10) C(B4 0.0262(15) 0.0271(13) 0.0140(11) -0.0007(9) -0.0049(10) -0.0021(11) C10 0.0261(14) 0.0157(11) 0.0165(11) 0.0001(8) -0.0062(10) -0.0032(10) C11 0.0256(15) 0.0341(14) 0.0229(13) 0.0019(10) -0.0098(11) -0.0076(11) C12 0.0288(15) 0.0298(13) 0.0236(13) 0.0023(10) -0.0043(11) -0.0097(11) C13 0.0400(17) 0.0184(11) 0.0151(11) 0.0032(9) -0.0064(11) -0.0063(11) C14 0.0448(18) 0.0363(15) 0.0238(14) 0.0067(11) -0.0201(13) -0.0130(13) C15 0.0312(15) 0.0402(15) 0.0240(14) 0.0057(11) -0.0112(12) -0.0157(12) C20 0.0256(14) 0.0187(11) 0.0133(11) 0.0002(8) -0.0062(10) -0.0045(10) C21 0.0247(15) 0.0241(13) 0.0450(16) -0.0056(11) -0.0159(13) -0.0063(11) C22 0.0249(15) 0.0285(14) 0.0452(17) -0.0070(11) -0.0153(13) -0.0009(11) C23 0.0367(17) 0.0202(11) 0.0182(12) -0.0030(9) -0.0055(11) -0.0032(11) C24 0.0444(19) 0.0263(14) 0.0446(17) -0.0064(11) -0.0173(14) -0.0145(12) C25 0.0266(15) 0.0303(14) 0.0478(17) -0.0057(12) -0.0147(13) -0.0100(11) N3 0.020(2) 0.0179(19) 0.0145(19) 0.0027(14) -0.0048(17) -0.0018(16) O1 0.023(2) 0.043(2) 0.031(2) 0.0001(16) -0.0105(17) -0.0073(17) _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 Fe1 Fe1 0.406(5) 2_666 ? Fe1 N3 1.740(5) . ? Fe1 N2 1.980(7) . ? Fe1 N1 1.994(7) . ? Fe1 N1 2.007(7) 2_666 ? Fe1 N2 2.008(7) 2_666 ? Fe1 N3 2.146(5) 2_666 ? N1 C(A2 1.376(3) . ? N1 C(A1 1.387(3) . ? N1 Fe1 2.007(7) 2_666 ? N2 C(A4 1.380(3) . ? N2 C(A3 1.384(3) . ? N2 Fe1 2.008(7) 2_666 ? C(M1 C(A1 1.390(3) . ? C(M1 C(A4 1.397(3) 2_666 ? C(M1 C10 1.503(3) . ? C(M2 C(A2 1.388(3) . ? C(M2 C(A3 1.393(3) . ? C(M2 C20 1.504(3) . ? C(A1 C(B1 1.433(3) . ? C(A2 C(B2 1.439(3) . ? C(A3 C(B3 1.437(3) . ? C(A4 C(M1 1.397(3) 2_666 ? C(A4 C(B4 1.441(3) . ? C(B1 C(B2 1.349(3) . ? C(B1 H(BA 0.9500 . ? C(B2 H(BB 0.9500 . ? C(B3 C(B4 1.351(3) . ? C(B3 H(BC 0.9500 . ? C(B4 H(BD 0.9500 . ? C10 C11 1.383(3) . ? C10 C15 1.385(3) . ? C11 C12 1.389(3) . ? C11 H11A 0.9500 . ? C12 C13 1.388(3) . ? C12 H12A 0.9500 . ? C13 C14 1.376(4) . ? C13 H13A 0.9500 . ? C14 C15 1.392(3) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C20 C25 1.383(3) . ? C20 C21 1.384(3) . ? C21 C22 1.386(3) . ? C21 H21A 0.9500 . ? C22 C23 1.383(4) . ? C22 H22A 0.9500 . ? C23 C24 1.379(4) . ? C23 H23A 0.9500 . ? C24 C25 1.387(3) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? N3 O1 1.153(4) . ? N3 Fe1 2.146(5) 2_666 ? 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 Fe1 Fe1 N3 177(2) 2_666 . ? Fe1 Fe1 N2 88.1(19) 2_666 . ? N3 Fe1 N2 92.0(3) . . ? Fe1 Fe1 N1 86.1(18) 2_666 . ? N3 Fe1 N1 91.2(3) . . ? N2 Fe1 N1 89.8(3) . . ? Fe1 Fe1 N1 82.3(18) 2_666 2_666 ? N3 Fe1 N1 100.5(3) . 2_666 ? N2 Fe1 N1 89.8(3) . 2_666 ? N1 Fe1 N1 168.35(16) . 2_666 ? Fe1 Fe1 N2 80.2(18) 2_666 2_666 ? N3 Fe1 N2 99.6(3) . 2_666 ? N2 Fe1 N2 168.33(16) . 2_666 ? N1 Fe1 N2 89.4(3) . 2_666 ? N1 Fe1 N2 88.6(3) 2_666 2_666 ? Fe1 Fe1 N3 2.2(17) 2_666 2_666 ? N3 Fe1 N3 179.5(4) . 2_666 ? N2 Fe1 N3 88.0(2) . 2_666 ? N1 Fe1 N3 88.3(2) . 2_666 ? N1 Fe1 N3 80.1(2) 2_666 2_666 ? N2 Fe1 N3 80.3(2) 2_666 2_666 ? C(A2 N1 C(A1 104.98(17) . . ? C(A2 N1 Fe1 127.1(2) . . ? C(A1 N1 Fe1 127.5(2) . . ? C(A2 N1 Fe1 127.9(2) . 2_666 ? C(A1 N1 Fe1 126.7(2) . 2_666 ? C(A4 N2 C(A3 104.82(17) . . ? C(A4 N2 Fe1 127.5(2) . . ? C(A3 N2 Fe1 127.3(2) . . ? C(A4 N2 Fe1 127.1(2) . 2_666 ? C(A3 N2 Fe1 127.5(2) . 2_666 ? C(A1 C(M1 C(A4 123.5(2) . 2_666 ? C(A1 C(M1 C10 118.05(18) . . ? C(A4 C(M1 C10 118.42(19) 2_666 . ? C(A2 C(M2 C(A3 123.4(2) . . ? C(A2 C(M2 C20 118.72(18) . . ? C(A3 C(M2 C20 117.90(19) . . ? N1 C(A1 C(M1 125.66(19) . . ? N1 C(A1 C(B1 110.39(18) . . ? C(M1 C(A1 C(B1 123.9(2) . . ? N1 C(A2 C(M2 125.8(2) . . ? N1 C(A2 C(B2 110.51(19) . . ? C(M2 C(A2 C(B2 123.7(2) . . ? N2 C(A3 C(M2 125.7(2) . . ? N2 C(A3 C(B3 110.57(18) . . ? C(M2 C(A3 C(B3 123.8(2) . . ? N2 C(A4 C(M1 125.74(19) . 2_666 ? N2 C(A4 C(B4 110.72(18) . . ? C(M1 C(A4 C(B4 123.5(2) 2_666 . ? C(B2 C(B1 C(A1 107.13(19) . . ? C(B2 C(B1 H(BA 126.4 . . ? C(A1 C(B1 H(BA 126.4 . . ? C(B1 C(B2 C(A2 106.99(19) . . ? C(B1 C(B2 H(BB 126.5 . . ? C(A2 C(B2 H(BB 126.5 . . ? C(B4 C(B3 C(A3 107.1(2) . . ? C(B4 C(B3 H(BC 126.5 . . ? C(A3 C(B3 H(BC 126.5 . . ? C(B3 C(B4 C(A4 106.8(2) . . ? C(B3 C(B4 H(BD 126.6 . . ? C(A4 C(B4 H(BD 126.6 . . ? C11 C10 C15 118.9(2) . . ? C11 C10 C(M1 120.2(2) . . ? C15 C10 C(M1 120.9(2) . . ? C10 C11 C12 120.8(2) . . ? C10 C11 H11A 119.6 . . ? C12 C11 H11A 119.6 . . ? C13 C12 C11 119.9(2) . . ? C13 C12 H12A 120.1 . . ? C11 C12 H12A 120.1 . . ? C14 C13 C12 119.6(2) . . ? C14 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? C13 C14 C15 120.3(2) . . ? C13 C14 H14A 119.8 . . ? C15 C14 H14A 119.8 . . ? C10 C15 C14 120.5(2) . . ? C10 C15 H15A 119.8 . . ? C14 C15 H15A 119.8 . . ? C25 C20 C21 118.6(2) . . ? C25 C20 C(M2 120.9(2) . . ? C21 C20 C(M2 120.4(2) . . ? C20 C21 C22 120.8(2) . . ? C20 C21 H21A 119.6 . . ? C22 C21 H21A 119.6 . . ? C23 C22 C21 120.3(2) . . ? C23 C22 H22A 119.8 . . ? C21 C22 H22A 119.8 . . ? C24 C23 C22 119.1(2) . . ? C24 C23 H23A 120.4 . . ? C22 C23 H23A 120.4 . . ? C23 C24 C25 120.5(2) . . ? C23 C24 H24A 119.7 . . ? C25 C24 H24A 119.7 . . ? C20 C25 C24 120.7(2) . . ? C20 C25 H25A 119.7 . . ? C24 C25 H25A 119.7 . . ? O1 N3 Fe1 145.6(4) . . ? O1 N3 Fe1 145.2(4) . 2_666 ? _diffrn_measured_fraction_theta_max .968 _diffrn_reflns_theta_full 27.71 _diffrn_measured_fraction_theta_full .968 _refine_diff_density_max .498 _refine_diff_density_min -.358 _refine_diff_density_rms .067 #===END data_100_cryst_2 #local ID: ns44 _publ_requested_journal Inorg.Chem. _publ_contact_author_name 'Professor W. Robert Scheidt' _publ_contact_author_address ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; _publ_contact_author_email W.R.Scheidt.1@nd.edu _publ_contact_author_phone 1(574)6315939 _publ_contact_author_fax 1(574)6316652 loop_ _publ_author_name _publ_author_address 'Scheidt, W. Robert ' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Silvernail, Nathan J.' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Noll, Bruce C.' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Olmstead, Marilyn M.' ;University of California at Davis Department of Chemistry One Shields Avenue Davis, CA 95616 ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common [Fe(TPP)(NO] _chemical_melting_point ? _chemical_formula_moiety 'C44 H28 Fe N5 O' _chemical_formula_sum 'C44 H28 Fe N5 O' _chemical_formula_weight 698.56 _chemical_compound_source synthesized loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' .3463 .8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7310(8) _cell_length_b 9.9238(8) _cell_length_c 10.3902(6) _cell_angle_alpha 82.195(1) _cell_angle_beta 65.693(4) _cell_angle_gamma 69.384(5) _cell_volume 855.81(11) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9991 _cell_measurement_theta_min 2.1928 _cell_measurement_theta_max 30.9699 _exptl_crystal_description 'square bipyramid' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 361 _exptl_absorpt_coefficient_mu 0.484 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9064 _exptl_absorpt_correction_T_max 0.9785 _exptl_absorpt_process_details 'Blessing, R.H. ACTA Cryst. (1995) A51, 33-38' _exptl_crystal_recrystallization_method 'liquid diffusion (chloroform/methanol)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker x8 APEX II CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6497 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 31.22 _reflns_number_total 6497 _reflns_number_gt 4766 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Platon (Spek, 2004)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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. The structures were solved by direct methods using SHELXS-97 and refined against F^2^ using SHELXL-97;subsequent difference Fourier syntheses led to the location of most of the remaining non-hydrogen atoms. For the structure refinement all data were used including negative intensities. All nonhydrogen atoms were refined anisotropically. Hydrogen atoms were idealized with the standard SHELXL-97 idealization methods. Hydrogen atoms were placed at calculated geometries and allowed to ride on the position of the parent atom. Hydrogen thermal parameters were set to 1.2\\times the equivalent isotropic U of the parent atom, 1.5\\times for methyl hydrogens. The program SADABS was applied for the absorption correction. The structure is a tetraphenyl porphyrin bound axially by a nitrosyl. ; _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^)+(0.0841P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6497 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0660 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1309 _refine_ls_wR_factor_gt 0.1213 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.4807(3) 0.4983(4) 0.4986(4) 0.0166(3) Uani 0.50 1 d P . . N1 N 0.46321(16) 0.68120(13) 0.39278(13) 0.0174(3) Uani 1 1 d . . . N2 N 0.35704(16) 0.60896(14) 0.67936(13) 0.0179(3) Uani 1 1 d . . . C(M1 C 0.6314(2) 0.58824(17) 0.14934(15) 0.0180(3) Uani 1 1 d . . . C(M2 C 0.28062(19) 0.85505(16) 0.58793(16) 0.0169(3) Uani 1 1 d . . . C(A1 C 0.52685(19) 0.69787(16) 0.24781(15) 0.0183(3) Uani 1 1 d . . . C(A2 C 0.3682(2) 0.81761(16) 0.44628(15) 0.0173(3) Uani 1 1 d . . . C(A3 C 0.2786(2) 0.75531(16) 0.69620(16) 0.0179(3) Uani 1 1 d . . . C(A4 C 0.31648(19) 0.55493(16) 0.81498(15) 0.0185(3) Uani 1 1 d . . . C(B1 C 0.4710(2) 0.84603(16) 0.21156(16) 0.0217(3) Uani 1 1 d . . . H(BA H 0.4980 0.8848 0.1191 0.026 Uiso 1 1 calc R . . C(B2 C 0.3725(2) 0.92018(16) 0.33371(16) 0.0207(3) Uani 1 1 d . . . H(BB H 0.3168 1.0208 0.3434 0.025 Uiso 1 1 calc R . . C(B3 C 0.1905(2) 0.79302(17) 0.84369(16) 0.0217(3) Uani 1 1 d . . . H(BC H 0.1281 0.8870 0.8824 0.026 Uiso 1 1 calc R . . C(B4 C 0.2132(2) 0.66964(17) 0.91643(16) 0.0223(3) Uani 1 1 d . . . H(BD H 0.1693 0.6602 1.0162 0.027 Uiso 1 1 calc R . . C10 C 0.6918(2) 0.62742(16) -0.00410(15) 0.0188(3) Uani 1 1 d . . . C11 C 0.8390(2) 0.64617(19) -0.06820(17) 0.0255(4) Uani 1 1 d . . . H11A H 0.9018 0.6348 -0.0151 0.031 Uiso 1 1 calc R . . C12 C 0.8963(2) 0.68176(19) -0.21056(17) 0.0268(4) Uani 1 1 d . . . H12A H 0.9976 0.6950 -0.2541 0.032 Uiso 1 1 calc R . . C13 C 0.8059(2) 0.69778(16) -0.28827(16) 0.0249(4) Uani 1 1 d . . . H13A H 0.8462 0.7195 -0.3859 0.030 Uiso 1 1 calc R . . C14 C 0.6569(2) 0.6822(2) -0.22403(18) 0.0301(4) Uani 1 1 d . . . H14A H 0.5934 0.6957 -0.2769 0.036 Uiso 1 1 calc R . . C15 C 0.5997(2) 0.64677(19) -0.08165(18) 0.0270(4) Uani 1 1 d . . . H15A H 0.4972 0.6358 -0.0376 0.032 Uiso 1 1 calc R . . C20 C 0.1832(2) 1.00909(16) 0.62716(15) 0.0176(3) Uani 1 1 d . . . C21 C 0.0225(2) 1.05790(19) 0.6516(2) 0.0276(4) Uani 1 1 d . . . H21A H -0.0258 0.9929 0.6438 0.033 Uiso 1 1 calc R . . C22 C -0.0683(2) 1.20081(19) 0.6872(2) 0.0312(4) Uani 1 1 d . . . H22A H -0.1784 1.2330 0.7038 0.037 Uiso 1 1 calc R . . C23 C -0.0002(2) 1.29624(17) 0.69867(16) 0.0246(4) Uani 1 1 d . . . H23A H -0.0623 1.3945 0.7216 0.030 Uiso 1 1 calc R . . C24 C 0.1591(2) 1.2478(2) 0.6765(2) 0.0334(4) Uani 1 1 d . . . H24A H 0.2068 1.3125 0.6861 0.040 Uiso 1 1 calc R . . C25 C 0.2498(2) 1.1053(2) 0.6402(2) 0.0313(4) Uani 1 1 d . . . H25A H 0.3599 1.0734 0.6240 0.038 Uiso 1 1 calc R . . N3 N 0.3097(3) 0.4904(3) 0.4908(3) 0.0165(5) Uani 0.50 1 d P . . O1 O 0.1797(3) 0.5554(3) 0.5026(3) 0.0287(5) Uani 0.50 1 d 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 Fe1 0.0188(10) 0.0152(2) 0.0106(2) 0.00131(16) -0.0028(7) -0.0038(7) N1 0.0180(7) 0.0159(6) 0.0124(6) -0.0006(5) -0.0027(5) -0.0024(5) N2 0.0174(7) 0.0181(6) 0.0132(6) 0.0021(5) -0.0042(5) -0.0030(5) C(M1 0.0170(8) 0.0223(8) 0.0133(7) 0.0031(6) -0.0054(6) -0.0067(6) C(M2 0.0144(8) 0.0172(7) 0.0182(7) 0.0013(6) -0.0066(6) -0.0042(6) C(A1 0.0200(8) 0.0178(7) 0.0143(7) 0.0025(5) -0.0056(7) -0.0052(6) C(A2 0.0166(8) 0.0160(7) 0.0168(7) 0.0025(5) -0.0061(6) -0.0038(6) C(A3 0.0167(8) 0.0176(7) 0.0147(7) -0.0009(5) -0.0044(6) -0.0022(6) C(A4 0.0196(8) 0.0198(7) 0.0111(7) -0.0009(5) -0.0036(6) -0.0034(6) C(B1 0.0256(9) 0.0192(7) 0.0154(7) 0.0051(6) -0.0066(7) -0.0053(7) C(B2 0.0221(8) 0.0165(7) 0.0173(7) 0.0021(6) -0.0053(7) -0.0030(6) C(B3 0.0234(9) 0.0206(8) 0.0138(7) -0.0009(6) -0.0034(7) -0.0031(7) C(B4 0.0252(9) 0.0215(8) 0.0119(7) -0.0008(6) -0.0037(7) -0.0021(7) C10 0.0221(8) 0.0146(7) 0.0128(7) 0.0015(5) -0.0038(6) -0.0025(6) C11 0.0238(9) 0.0320(9) 0.0175(8) 0.0031(7) -0.0075(7) -0.0071(7) C12 0.0257(9) 0.0274(9) 0.0188(8) 0.0029(7) -0.0014(7) -0.0087(7) C13 0.0357(10) 0.0150(7) 0.0137(7) 0.0020(6) -0.0039(7) -0.0041(7) C14 0.0422(11) 0.0315(10) 0.0215(9) 0.0059(7) -0.0184(8) -0.0130(8) C15 0.0293(10) 0.0349(10) 0.0209(8) 0.0070(7) -0.0108(8) -0.0164(8) C20 0.0207(8) 0.0177(7) 0.0128(7) 0.0000(5) -0.0054(6) -0.0056(6) C21 0.0229(9) 0.0205(8) 0.0412(11) -0.0052(7) -0.0140(8) -0.0056(7) C22 0.0235(10) 0.0238(9) 0.0415(11) -0.0075(8) -0.0126(8) 0.0004(7) C23 0.0334(10) 0.0173(7) 0.0155(7) -0.0033(6) -0.0052(7) -0.0037(7) C24 0.0394(12) 0.0237(9) 0.0402(11) -0.0066(8) -0.0131(9) -0.0147(8) C25 0.0213(9) 0.0283(10) 0.0450(11) -0.0052(8) -0.0111(9) -0.0091(8) N3 0.0207(13) 0.0162(12) 0.0084(11) 0.0013(9) -0.0030(11) -0.0047(10) O1 0.0218(13) 0.0335(14) 0.0276(13) 0.0021(11) -0.0111(11) -0.0043(10) _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 Fe1 Fe1 0.402(3) 2_666 ? Fe1 N3 1.728(3) . ? Fe1 N1 1.981(4) . ? Fe1 N2 1.988(4) . ? Fe1 N2 1.998(4) 2_666 ? Fe1 N1 2.006(4) 2_666 ? Fe1 N3 2.129(3) 2_666 ? N1 C(A2 1.3772(19) . ? N1 C(A1 1.3843(18) . ? N1 Fe1 2.006(4) 2_666 ? N2 C(A3 1.3787(19) . ? N2 C(A4 1.3838(18) . ? N2 Fe1 1.998(4) 2_666 ? C(M1 C(A4 1.385(2) 2_666 ? C(M1 C(A1 1.390(2) . ? C(M1 C10 1.503(2) . ? C(M2 C(A2 1.387(2) . ? C(M2 C(A3 1.392(2) . ? C(M2 C20 1.494(2) . ? C(A1 C(B1 1.433(2) . ? C(A2 C(B2 1.439(2) . ? C(A3 C(B3 1.439(2) . ? C(A4 C(M1 1.385(2) 2_666 ? C(A4 C(B4 1.437(2) . ? C(B1 C(B2 1.351(2) . ? C(B1 H(BA 0.9500 . ? C(B2 H(BB 0.9500 . ? C(B3 C(B4 1.347(2) . ? C(B3 H(BC 0.9500 . ? C(B4 H(BD 0.9500 . ? C10 C11 1.378(2) . ? C10 C15 1.386(2) . ? C11 C12 1.393(2) . ? C11 H11A 0.9500 . ? C12 C13 1.379(3) . ? C12 H12A 0.9500 . ? C13 C14 1.380(3) . ? C13 H13A 0.9500 . ? C14 C15 1.393(2) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C20 C25 1.376(2) . ? C20 C21 1.385(2) . ? C21 C22 1.386(2) . ? C21 H21A 0.9500 . ? C22 C23 1.374(3) . ? C22 H22A 0.9500 . ? C23 C24 1.378(3) . ? C23 H23A 0.9500 . ? C24 C25 1.383(3) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? N3 O1 1.163(3) . ? N3 Fe1 2.129(3) 2_666 ? 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 Fe1 Fe1 N3 177.6(12) 2_666 . ? Fe1 Fe1 N1 87.7(11) 2_666 . ? N3 Fe1 N1 91.34(16) . . ? Fe1 Fe1 N2 85.7(11) 2_666 . ? N3 Fe1 N2 92.10(16) . . ? N1 Fe1 N2 89.86(16) . . ? Fe1 Fe1 N2 82.7(11) 2_666 2_666 ? N3 Fe1 N2 99.48(17) . 2_666 ? N1 Fe1 N2 89.67(17) . 2_666 ? N2 Fe1 N2 168.42(8) . 2_666 ? Fe1 Fe1 N1 80.8(11) 2_666 2_666 ? N3 Fe1 N1 100.21(17) . 2_666 ? N1 Fe1 N1 168.44(8) . 2_666 ? N2 Fe1 N1 89.28(16) . 2_666 ? N2 Fe1 N1 88.87(15) 2_666 2_666 ? Fe1 Fe1 N3 1.9(10) 2_666 2_666 ? N3 Fe1 N3 179.5(2) . 2_666 ? N1 Fe1 N3 88.48(13) . 2_666 ? N2 Fe1 N3 87.49(13) . 2_666 ? N2 Fe1 N3 80.93(12) 2_666 2_666 ? N1 Fe1 N3 79.98(12) 2_666 2_666 ? C(A2 N1 C(A1 105.02(12) . . ? C(A2 N1 Fe1 127.09(15) . . ? C(A1 N1 Fe1 127.40(15) . . ? C(A2 N1 Fe1 127.48(15) . 2_666 ? C(A1 N1 Fe1 127.09(15) . 2_666 ? Fe1 N1 Fe1 11.56(8) . 2_666 ? C(A3 N2 C(A4 105.02(12) . . ? C(A3 N2 Fe1 127.05(15) . . ? C(A4 N2 Fe1 127.59(15) . . ? C(A3 N2 Fe1 127.49(15) . 2_666 ? C(A4 N2 Fe1 126.91(15) . 2_666 ? Fe1 N2 Fe1 11.58(8) . 2_666 ? C(A4 C(M1 C(A1 123.55(14) 2_666 . ? C(A4 C(M1 C10 118.27(13) 2_666 . ? C(A1 C(M1 C10 118.18(13) . . ? C(A2 C(M2 C(A3 122.99(14) . . ? C(A2 C(M2 C20 118.91(13) . . ? C(A3 C(M2 C20 118.10(14) . . ? N1 C(A1 C(M1 125.65(14) . . ? N1 C(A1 C(B1 110.49(13) . . ? C(M1 C(A1 C(B1 123.86(14) . . ? N1 C(A2 C(M2 126.10(13) . . ? N1 C(A2 C(B2 110.50(13) . . ? C(M2 C(A2 C(B2 123.40(14) . . ? N2 C(A3 C(M2 125.92(14) . . ? N2 C(A3 C(B3 110.50(13) . . ? C(M2 C(A3 C(B3 123.57(14) . . ? N2 C(A4 C(M1 125.79(14) . 2_666 ? N2 C(A4 C(B4 110.31(13) . . ? C(M1 C(A4 C(B4 123.89(14) 2_666 . ? C(B2 C(B1 C(A1 107.06(13) . . ? C(B2 C(B1 H(BA 126.5 . . ? C(A1 C(B1 H(BA 126.5 . . ? C(B1 C(B2 C(A2 106.93(13) . . ? C(B1 C(B2 H(BB 126.5 . . ? C(A2 C(B2 H(BB 126.5 . . ? C(B4 C(B3 C(A3 106.96(13) . . ? C(B4 C(B3 H(BC 126.5 . . ? C(A3 C(B3 H(BC 126.5 . . ? C(B3 C(B4 C(A4 107.20(13) . . ? C(B3 C(B4 H(BD 126.4 . . ? C(A4 C(B4 H(BD 126.4 . . ? C11 C10 C15 119.51(14) . . ? C11 C10 C(M1 119.94(15) . . ? C15 C10 C(M1 120.54(15) . . ? C10 C11 C12 120.32(16) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C13 C12 C11 120.05(17) . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C12 C13 C14 119.93(15) . . ? C12 C13 H13A 120.0 . . ? C14 C13 H13A 120.0 . . ? C13 C14 C15 119.98(17) . . ? C13 C14 H14A 120.0 . . ? C15 C14 H14A 120.0 . . ? C10 C15 C14 120.17(17) . . ? C10 C15 H15A 119.9 . . ? C14 C15 H15A 119.9 . . ? C25 C20 C21 118.51(15) . . ? C25 C20 C(M2 121.29(15) . . ? C21 C20 C(M2 120.21(15) . . ? C20 C21 C22 120.50(16) . . ? C20 C21 H21A 119.8 . . ? C22 C21 H21A 119.8 . . ? C23 C22 C21 120.51(17) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C22 C23 C24 119.24(15) . . ? C22 C23 H23A 120.4 . . ? C24 C23 H23A 120.4 . . ? C23 C24 C25 120.20(17) . . ? C23 C24 H24A 119.9 . . ? C25 C24 H24A 119.9 . . ? C20 C25 C24 121.04(17) . . ? C20 C25 H25A 119.5 . . ? C24 C25 H25A 119.5 . . ? O1 N3 Fe1 145.3(3) . . ? O1 N3 Fe1 144.9(2) . 2_666 ? Fe1 N3 Fe1 0.5(2) . 2_666 ? _diffrn_measured_fraction_theta_max .921 _diffrn_reflns_theta_full 31.22 _diffrn_measured_fraction_theta_full .921 _refine_diff_density_max .519 _refine_diff_density_min -.608 _refine_diff_density_rms .068 #===END data_100_cryst_3 # local ID: ns43_0m _publ_requested_journal Inorg.Chem. _publ_contact_author_name 'Professor W. Robert Scheidt' _publ_contact_author_address ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; _publ_contact_author_email W.R.Scheidt.1@nd.edu _publ_contact_author_phone 1(574)6315939 _publ_contact_author_fax 1(574)6316652 loop_ _publ_author_name _publ_author_address 'Scheidt, W. Robert ' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Silvernail, Nathan J.' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Noll, Bruce C.' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Olmstead, Marilyn M.' ;University of California at Davis Department of Chemistry One Shields Avenue Davis, CA 95616 ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common [Fe(TPP)(NO] _chemical_melting_point ? _chemical_formula_moiety 'C44 H28 Fe N5 O' _chemical_formula_sum 'C44 H28 Fe N5 O' _chemical_formula_weight 698.56 _chemical_compound_source synthesized loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.734(3) _cell_length_b 9.960(3) _cell_length_c 10.391(3) _cell_angle_alpha 82.100(3) _cell_angle_beta 65.63(2) _cell_angle_gamma 69.249(19) _cell_volume 858.0(4) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'square bipyramid' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 361 _exptl_absorpt_coefficient_mu 0.483 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8013 _exptl_absorpt_correction_T_max 0.8888 _exptl_absorpt_process_details 'Blessing, R.H. ACTA Cryst. (1995) A51, 33-38' _exptl_crystal_recrystallization_method 'liquid diffusion (chloroform/methanol)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker x8 APEX II CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5092 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5092 _reflns_number_gt 4085 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Platon (Spek, 2004)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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. The structures were solved by direct methods using SHELXS-97 and refined against F^2^ using SHELXL-97;subsequent difference Fourier syntheses led to the location of most of the remaining non-hydrogen atoms. For the structure refinement all data were used including negative intensities. All nonhydrogen atoms were refined anisotropically. Hydrogen atoms were idealized with the standard SHELXL-97 idealization methods. Hydrogen atoms were placed at calculated geometries and allowed to ride on the position of the parent atom. Hydrogen thermal parameters were set to 1.2\\times the equivalent isotropic U of the parent atom, 1.5\\times for methyl hydrogens. The program SADABS was applied for the absorption correction. The structure is a tetraphenyl porphyrin bound axially by a nitrosyl. ; _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^)+(0.0648P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5092 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0999 _refine_ls_R_factor_gt 0.0788 _refine_ls_wR_factor_ref 0.2225 _refine_ls_wR_factor_gt 0.1979 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.4836(12) 0.4969(15) 0.4979(15) 0.0219(11) Uani 0.50 1 d P . . N1 N 0.4626(3) 0.6827(3) 0.3929(3) 0.0178(6) Uani 1 1 d . . . N2 N 0.3564(3) 0.6086(3) 0.6810(3) 0.0185(6) Uani 1 1 d . . . C(M1 C 0.6315(4) 0.5878(3) 0.1505(3) 0.0189(7) Uani 1 1 d . . . C(M2 C 0.2818(4) 0.8529(3) 0.5878(3) 0.0180(6) Uani 1 1 d . . . C(A1 C 0.5263(4) 0.6986(3) 0.2480(3) 0.0189(7) Uani 1 1 d . . . C(A2 C 0.3691(4) 0.8172(3) 0.4461(3) 0.0199(7) Uani 1 1 d . . . C(A3 C 0.2775(4) 0.7554(3) 0.6976(3) 0.0190(7) Uani 1 1 d . . . C(A4 C 0.3168(4) 0.5560(3) 0.8149(3) 0.0195(7) Uani 1 1 d . . . C(B1 C 0.4715(4) 0.8448(3) 0.2121(3) 0.0232(7) Uani 1 1 d . . . H(BA H 0.4986 0.8831 0.1195 0.028 Uiso 1 1 calc R . . C(B2 C 0.3742(4) 0.9190(3) 0.3329(3) 0.0215(7) Uani 1 1 d . . . H(BB H 0.3192 1.0195 0.3421 0.026 Uiso 1 1 calc R . . C(B3 C 0.1901(4) 0.7931(3) 0.8433(3) 0.0237(7) Uani 1 1 d . . . H(BC H 0.1281 0.8869 0.8819 0.028 Uiso 1 1 calc R . . C(B4 C 0.2123(4) 0.6698(3) 0.9160(3) 0.0207(7) Uani 1 1 d . . . H(BD H 0.1671 0.6601 1.0157 0.025 Uiso 1 1 calc R . . C10 C 0.6911(4) 0.6275(3) -0.0034(3) 0.0191(7) Uani 1 1 d . . . C11 C 0.8373(4) 0.6468(4) -0.0676(4) 0.0301(9) Uani 1 1 d . . . H11A H 0.9001 0.6360 -0.0147 0.036 Uiso 1 1 calc R . . C12 C 0.8941(5) 0.6824(4) -0.2102(4) 0.0302(9) Uani 1 1 d . . . H12A H 0.9952 0.6961 -0.2537 0.036 Uiso 1 1 calc R . . C13 C 0.8047(5) 0.6977(3) -0.2883(3) 0.0267(8) Uani 1 1 d . . . H13A H 0.8447 0.7196 -0.3860 0.032 Uiso 1 1 calc R . . C14 C 0.6562(5) 0.6809(4) -0.2231(4) 0.0336(9) Uani 1 1 d . . . H14A H 0.5923 0.6937 -0.2754 0.040 Uiso 1 1 calc R . . C15 C 0.6001(5) 0.6454(4) -0.0809(4) 0.0310(9) Uani 1 1 d . . . H15A H 0.4982 0.6333 -0.0368 0.037 Uiso 1 1 calc R . . C20 C 0.1830(4) 1.0077(3) 0.6274(3) 0.0196(7) Uani 1 1 d . . . C21 C 0.0221(5) 1.0590(4) 0.6511(4) 0.0327(9) Uani 1 1 d . . . H21A H -0.0270 0.9952 0.6431 0.039 Uiso 1 1 calc R . . C22 C -0.0680(5) 1.2014(4) 0.6862(4) 0.0349(9) Uani 1 1 d . . . H22A H -0.1780 1.2344 0.7016 0.042 Uiso 1 1 calc R . . C23 C 0.0000(5) 1.2953(3) 0.6990(3) 0.0279(8) Uani 1 1 d . . . H23A H -0.0616 1.3934 0.7222 0.033 Uiso 1 1 calc R . . C24 C 0.1591(5) 1.2452(4) 0.6777(4) 0.0374(10) Uani 1 1 d . . . H24A H 0.2069 1.3091 0.6878 0.045 Uiso 1 1 calc R . . C25 C 0.2505(5) 1.1025(4) 0.6417(4) 0.0349(9) Uani 1 1 d . . . H25A H 0.3603 1.0699 0.6268 0.042 Uiso 1 1 calc R . . N3 N 0.3115(6) 0.4892(6) 0.4913(6) 0.0186(11) Uani 0.50 1 d P . . O1 O 0.1803(6) 0.5545(6) 0.5033(6) 0.0338(12) Uani 0.50 1 d 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 Fe1 0.029(3) 0.0168(10) 0.0125(7) 0.0027(6) -0.005(2) -0.004(2) N1 0.0186(15) 0.0208(14) 0.0120(12) 0.0039(10) -0.0053(11) -0.0063(12) N2 0.0164(15) 0.0178(13) 0.0173(13) 0.0024(10) -0.0060(12) -0.0025(11) C(M1 0.0159(17) 0.0253(17) 0.0134(15) 0.0014(12) -0.0055(13) -0.0051(14) C(M2 0.0202(18) 0.0175(15) 0.0201(16) 0.0047(12) -0.0105(14) -0.0091(13) C(A1 0.0189(18) 0.0212(16) 0.0133(15) 0.0011(12) -0.0054(14) -0.0042(14) C(A2 0.0188(18) 0.0173(16) 0.0230(17) 0.0070(12) -0.0092(14) -0.0068(14) C(A3 0.0186(18) 0.0189(16) 0.0205(16) 0.0063(12) -0.0103(14) -0.0064(14) C(A4 0.0177(17) 0.0259(17) 0.0103(14) -0.0037(12) -0.0011(13) -0.0058(14) C(B1 0.028(2) 0.0207(16) 0.0153(15) 0.0050(12) -0.0070(15) -0.0051(15) C(B2 0.029(2) 0.0153(15) 0.0173(16) 0.0056(12) -0.0089(15) -0.0061(14) C(B3 0.0252(19) 0.0218(17) 0.0195(16) 0.0002(13) -0.0066(15) -0.0051(15) C(B4 0.0235(18) 0.0220(16) 0.0089(14) -0.0020(12) -0.0040(13) -0.0011(14) C10 0.0231(18) 0.0136(15) 0.0162(15) 0.0009(11) -0.0066(14) -0.0027(13) C11 0.028(2) 0.040(2) 0.0216(19) 0.0030(16) -0.0097(16) -0.0115(17) C12 0.028(2) 0.034(2) 0.0220(19) 0.0037(16) -0.0011(15) -0.0140(16) C13 0.039(2) 0.0154(16) 0.0155(16) -0.0016(12) -0.0042(16) -0.0043(15) C14 0.046(2) 0.035(2) 0.026(2) 0.0081(17) -0.0210(19) -0.0149(19) C15 0.034(2) 0.041(2) 0.023(2) 0.0091(16) -0.0135(17) -0.0191(18) C20 0.0228(19) 0.0233(16) 0.0103(14) 0.0036(12) -0.0047(14) -0.0083(14) C21 0.027(2) 0.0252(19) 0.049(2) -0.0033(17) -0.0192(19) -0.0060(16) C22 0.026(2) 0.030(2) 0.044(2) -0.0053(18) -0.0145(19) -0.0008(17) C23 0.041(2) 0.0190(16) 0.0133(16) 0.0027(13) -0.0061(16) -0.0047(16) C24 0.043(3) 0.028(2) 0.043(2) -0.0045(18) -0.014(2) -0.0155(18) C25 0.026(2) 0.030(2) 0.049(3) -0.0026(18) -0.0137(19) -0.0094(17) N3 0.018(3) 0.023(3) 0.010(2) 0.006(2) -0.004(2) -0.006(2) O1 0.026(3) 0.039(3) 0.035(3) 0.004(2) -0.015(2) -0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 Fe1 0.365(13) 2_666 ? Fe1 N3 1.734(8) . ? Fe1 N2 1.994(14) 2_666 ? Fe1 N1 2.004(14) . ? Fe1 N1 2.008(14) 2_666 ? Fe1 N2 2.013(14) . ? Fe1 N3 2.096(9) 2_666 ? N1 C(A2 1.361(4) . ? N1 C(A1 1.382(4) . ? N1 Fe1 2.008(14) 2_666 ? N2 C(A4 1.363(4) . ? N2 C(A3 1.386(4) . ? N2 Fe1 1.993(14) 2_666 ? C(M1 C(A4 1.390(4) 2_666 ? C(M1 C(A1 1.394(4) . ? C(M1 C10 1.508(4) . ? C(M2 C(A2 1.383(5) . ? C(M2 C(A3 1.390(4) . ? C(M2 C20 1.506(5) . ? C(A1 C(B1 1.417(4) . ? C(A2 C(B2 1.440(4) . ? C(A3 C(B3 1.423(4) . ? C(A4 C(M1 1.390(4) 2_666 ? C(A4 C(B4 1.432(4) . ? C(B1 C(B2 1.341(4) . ? C(B1 H(BA 0.9500 . ? C(B2 H(BB 0.9500 . ? C(B3 C(B4 1.348(5) . ? C(B3 H(BC 0.9500 . ? C(B4 H(BD 0.9500 . ? C10 C11 1.372(5) . ? C10 C15 1.379(5) . ? C11 C12 1.394(5) . ? C11 H11A 0.9500 . ? C12 C13 1.376(5) . ? C12 H12A 0.9500 . ? C13 C14 1.382(6) . ? C13 H13A 0.9500 . ? C14 C15 1.390(5) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C20 C25 1.380(5) . ? C20 C21 1.387(5) . ? C21 C22 1.382(5) . ? C21 H21A 0.9500 . ? C22 C23 1.370(6) . ? C22 H22A 0.9500 . ? C23 C24 1.377(6) . ? C23 H23A 0.9500 . ? C24 C25 1.388(6) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? N3 O1 1.171(7) . ? N3 Fe1 2.096(9) 2_666 ? 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 Fe1 Fe1 N3 172(5) 2_666 . ? Fe1 Fe1 N2 88(4) 2_666 2_666 ? N3 Fe1 N2 99.1(6) . 2_666 ? Fe1 Fe1 N1 85(4) 2_666 . ? N3 Fe1 N1 91.0(6) . . ? N2 Fe1 N1 90.0(6) 2_666 . ? Fe1 Fe1 N1 84(4) 2_666 2_666 ? N3 Fe1 N1 99.3(6) . 2_666 ? N2 Fe1 N1 89.6(6) 2_666 2_666 ? N1 Fe1 N1 169.6(4) . 2_666 ? Fe1 Fe1 N2 82(4) 2_666 . ? N3 Fe1 N2 91.3(6) . . ? N2 Fe1 N2 169.6(4) 2_666 . ? N1 Fe1 N2 89.2(6) . . ? N1 Fe1 N2 89.3(6) 2_666 . ? N3 Fe1 N3 178.6(9) . 2_666 ? N2 Fe1 N3 82.1(4) 2_666 2_666 ? N1 Fe1 N3 88.3(4) . 2_666 ? N1 Fe1 N3 81.3(4) 2_666 2_666 ? N2 Fe1 N3 87.5(4) . 2_666 ? C(A2 N1 C(A1 105.4(2) . . ? C(A2 N1 Fe1 127.7(5) . . ? C(A1 N1 Fe1 126.4(4) . . ? C(A2 N1 Fe1 127.2(5) . 2_666 ? C(A1 N1 Fe1 127.0(5) . 2_666 ? C(A4 N2 C(A3 105.0(2) . . ? C(A4 N2 Fe1 127.6(4) . 2_666 ? C(A3 N2 Fe1 126.9(5) . 2_666 ? C(A4 N2 Fe1 127.8(5) . . ? C(A3 N2 Fe1 127.0(4) . . ? C(A4 C(M1 C(A1 124.7(3) 2_666 . ? C(A4 C(M1 C10 118.0(3) 2_666 . ? C(A1 C(M1 C10 117.3(3) . . ? C(A2 C(M2 C(A3 124.5(3) . . ? C(A2 C(M2 C20 118.4(3) . . ? C(A3 C(M2 C20 117.1(3) . . ? N1 C(A1 C(M1 125.2(3) . . ? N1 C(A1 C(B1 110.3(3) . . ? C(M1 C(A1 C(B1 124.5(3) . . ? N1 C(A2 C(M2 125.7(3) . . ? N1 C(A2 C(B2 110.1(3) . . ? C(M2 C(A2 C(B2 124.2(3) . . ? N2 C(A3 C(M2 125.1(3) . . ? N2 C(A3 C(B3 110.6(3) . . ? C(M2 C(A3 C(B3 124.4(3) . . ? N2 C(A4 C(M1 125.1(3) . 2_666 ? N2 C(A4 C(B4 110.5(3) . . ? C(M1 C(A4 C(B4 124.4(3) 2_666 . ? C(B2 C(B1 C(A1 107.4(3) . . ? C(B2 C(B1 H(BA 126.3 . . ? C(A1 C(B1 H(BA 126.3 . . ? C(B1 C(B2 C(A2 106.9(3) . . ? C(B1 C(B2 H(BB 126.6 . . ? C(A2 C(B2 H(BB 126.6 . . ? C(B4 C(B3 C(A3 106.7(3) . . ? C(B4 C(B3 H(BC 126.7 . . ? C(A3 C(B3 H(BC 126.7 . . ? C(B3 C(B4 C(A4 107.3(3) . . ? C(B3 C(B4 H(BD 126.4 . . ? C(A4 C(B4 H(BD 126.4 . . ? C11 C10 C15 119.3(3) . . ? C11 C10 C(M1 119.9(3) . . ? C15 C10 C(M1 120.8(3) . . ? C10 C11 C12 120.3(3) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C13 C12 C11 120.4(3) . . ? C13 C12 H12A 119.8 . . ? C11 C12 H12A 119.8 . . ? C12 C13 C14 119.3(3) . . ? C12 C13 H13A 120.4 . . ? C14 C13 H13A 120.4 . . ? C13 C14 C15 120.1(4) . . ? C13 C14 H14A 120.0 . . ? C15 C14 H14A 120.0 . . ? C10 C15 C14 120.6(4) . . ? C10 C15 H15A 119.7 . . ? C14 C15 H15A 119.7 . . ? C25 C20 C21 118.1(3) . . ? C25 C20 C(M2 120.6(3) . . ? C21 C20 C(M2 121.3(3) . . ? C22 C21 C20 121.2(3) . . ? C22 C21 H21A 119.4 . . ? C20 C21 H21A 119.4 . . ? C23 C22 C21 120.5(4) . . ? C23 C22 H22A 119.8 . . ? C21 C22 H22A 119.8 . . ? C22 C23 C24 118.9(3) . . ? C22 C23 H23A 120.5 . . ? C24 C23 H23A 120.5 . . ? C23 C24 C25 120.9(4) . . ? C23 C24 H24A 119.5 . . ? C25 C24 H24A 119.5 . . ? C20 C25 C24 120.4(4) . . ? C20 C25 H25A 119.8 . . ? C24 C25 H25A 119.8 . . ? O1 N3 Fe1 145.4(7) . . ? O1 N3 Fe1 144.1(6) . 2_666 ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 1.849 _refine_diff_density_min -0.659 _refine_diff_density_rms 0.125 #===END data_100_cryst_4 # local ID: bcn350_100t5 _publ_requested_journal Inorg.Chem. _publ_contact_author_name 'Professor W. Robert Scheidt' _publ_contact_author_address ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; _publ_contact_author_email W.R.Scheidt.1@nd.edu _publ_contact_author_phone 1(574)6315939 _publ_contact_author_fax 1(574)6316652 loop_ _publ_author_name _publ_author_address 'Scheidt, W. Robert ' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Silvernail, Nathan J.' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Noll, Bruce C.' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Olmstead, Marilyn M.' ;University of California at Davis Department of Chemistry One Shields Avenue Davis, CA 95616 ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common [Fe(TPP)(NO)] _chemical_melting_point ? _chemical_formula_moiety 'C44 H28 Fe N5 O' _chemical_formula_sum 'C44 H28 Fe N5 O' _chemical_formula_weight 698.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7201(7) _cell_length_b 9.9105(6) _cell_length_c 10.3715(6) _cell_angle_alpha 82.304(4) _cell_angle_beta 65.802(4) _cell_angle_gamma 69.546(4) _cell_volume 853.81(9) _cell_formula_units_Z 1 _cell_measurement_temperature 128(2) _cell_measurement_reflns_used 9963 _cell_measurement_theta_min 2.4311 _cell_measurement_theta_max 34.1300 _exptl_crystal_description octahedron _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.359 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 361 _exptl_absorpt_coefficient_mu 0.485 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.90 _exptl_absorpt_process_details 'Sheldrick, G. M. (2007) SADABS. University of G\"ottingen, Germany.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Siemens KFFMO2K-90' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker x8-Apex II CCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6741 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 34.57 _reflns_number_total 6741 _reflns_number_gt 4480 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Bruker-Nonius AXS. (2007). APEX2 and SAINT. Bruker-Nonius AXS, Madison, Wisconsin, USA. CCDC. (2005). enCIFer. The Cambridge Crystallographic Data Centre, Cambridge, UK. Sheldrick, G. M. (2007). SADABS. University of G\"ottingen, Germany. Sheldrick, G. M. (2001). XCIF, XL, and XS. Bruker-Nonius AXS, Madison, Wisconsin, USA. Sheldrick, G. M. (2003). XPREP. Bruker-Nonius AXS, Madison, Wisconsin, USA. ; _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2007; Sheldrick, 2003)' _computing_structure_solution 'XS (Sheldrick, 2001)' _computing_structure_refinement 'XL (Sheldrick, 2001)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XCIF (Sheldrick, 2001)/enCIFer (CCDC, 2005)' _refine_special_details ; Crystal was modeled as 4-component nonmerohedral twin. Scale factors, relative to the first component, refined to 0.304(2), 0.187(2), and 0.174(2). Twin laws for each component follow. Domain 2: Rotated from first domain by 180.0 degrees about reciprocal axis 1.000 0.501 0.503 and real axis 1.000 0.175 0.073 Twin law to convert hkl from first to 0.779 0.312 0.130 this domain (SHELXL TWIN matrix): 0.891 -0.844 0.065 0.894 0.157 -0.935 Domain 3: Rotated from first domain by 89.7 degrees about reciprocal axis 1.000 0.499 0.505 and real axis 1.000 0.174 0.075 Twin law to convert hkl from first to 0.847 0.086 0.219 this domain (SHELXL TWIN matrix): 0.916 0.052 -0.878 -0.079 1.056 0.112 Domain 4: Rotated from first domain by 90.4 degrees about reciprocal axis 1.000 0.499 0.504 and real axis 1.000 0.174 0.074 Twin law to convert hkl from first to 0.932 0.223 -0.087 this domain (SHELXL TWIN matrix): -0.027 0.101 0.944 0.977 -0.900 -0.046 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^)+(0.0930P)^2^+0.2239P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6741 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1118 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1806 _refine_ls_wR_factor_gt 0.1543 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe -0.0205(2) 0.4985(3) 0.9982(3) 0.0166(2) Uani 0.50 1 d P . . N1 N 0.0362(3) 0.3189(2) 1.10761(19) 0.0176(3) Uani 1 1 d . . . N2 N 0.1431(2) 0.3907(2) 0.82052(19) 0.0186(4) Uani 1 1 d . . . N3 N -0.1906(4) 0.4897(4) 0.9906(4) 0.0208(7) Uani 0.50 1 d P . . O1 O -0.3201(4) 0.5556(5) 1.0025(5) 0.0332(9) Uani 0.50 1 d P . . C(A1 C -0.0271(3) 0.3022(2) 1.2526(2) 0.0191(4) Uani 1 1 d . . . C(B1 C 0.0289(3) 0.1535(2) 1.2885(2) 0.0232(4) Uani 1 1 d . . . H(B1 H 0.0019 0.1144 1.3809 0.028 Uiso 1 1 calc R . . C(B2 C 0.1267(3) 0.0802(3) 1.1669(2) 0.0224(4) Uani 1 1 d . . . H(B2 H 0.1828 -0.0203 1.1571 0.027 Uiso 1 1 calc R . . C(A2 C 0.1307(3) 0.1824(2) 1.0541(2) 0.0183(4) Uani 1 1 d . . . C(M1 C 0.2192(3) 0.1448(2) 0.9121(2) 0.0188(4) Uani 1 1 d . . . C(A3 C 0.2215(3) 0.2451(3) 0.8039(2) 0.0198(4) Uani 1 1 d . . . C(B3 C 0.3103(3) 0.2059(3) 0.6561(2) 0.0227(4) Uani 1 1 d . . . H(B3 H 0.3723 0.1118 0.6177 0.027 Uiso 1 1 calc R . . C(B4 C 0.2872(3) 0.3305(3) 0.5833(2) 0.0235(5) Uani 1 1 d . . . H(B4 H 0.3312 0.3402 0.4835 0.028 Uiso 1 1 calc R . . C(A4 C 0.1841(3) 0.4445(2) 0.6848(2) 0.0193(4) Uani 1 1 d . . . C(M2 C 0.1308(3) 0.5888(2) 0.6495(2) 0.0186(4) Uani 1 1 d . . . C10 C 0.3166(3) -0.0085(2) 0.8726(2) 0.0187(4) Uani 1 1 d . . . C11 C 0.4770(3) -0.0572(3) 0.8489(3) 0.0297(6) Uani 1 1 d . . . H11 H 0.5252 0.0079 0.8569 0.036 Uiso 1 1 calc R . . C12 C 0.5680(3) -0.2003(3) 0.8133(3) 0.0325(6) Uani 1 1 d . . . H12 H 0.6779 -0.2324 0.7978 0.039 Uiso 1 1 calc R . . C13 C 0.5005(4) -0.2961(2) 0.8005(2) 0.0259(5) Uani 1 1 d . . . H13 H 0.5629 -0.3941 0.7762 0.031 Uiso 1 1 calc R . . C14 C 0.3407(4) -0.2480(3) 0.8234(4) 0.0360(6) Uani 1 1 d . . . H14 H 0.2931 -0.3131 0.8139 0.043 Uiso 1 1 calc R . . C15 C 0.2493(4) -0.1054(3) 0.8601(4) 0.0335(6) Uani 1 1 d . . . H15 H 0.1392 -0.0739 0.8768 0.040 Uiso 1 1 calc R . . C20 C 0.1917(3) 0.6275(2) 0.4957(2) 0.0199(4) Uani 1 1 d . . . C21 C 0.3392(3) 0.6466(3) 0.4317(3) 0.0276(5) Uani 1 1 d . . . H21 H 0.4019 0.6356 0.4849 0.033 Uiso 1 1 calc R . . C22 C 0.3961(3) 0.6821(3) 0.2892(3) 0.0294(6) Uani 1 1 d . . . H22 H 0.4975 0.6953 0.2456 0.035 Uiso 1 1 calc R . . C23 C 0.3062(3) 0.6979(3) 0.2114(2) 0.0264(5) Uani 1 1 d . . . H23 H 0.3464 0.7202 0.1138 0.032 Uiso 1 1 calc R . . C24 C 0.1577(4) 0.6816(3) 0.2752(3) 0.0330(6) Uani 1 1 d . . . H24 H 0.0944 0.6945 0.2220 0.040 Uiso 1 1 calc R . . C25 C 0.1006(3) 0.6461(3) 0.4176(3) 0.0295(6) Uani 1 1 d . . . H25 H -0.0017 0.6345 0.4614 0.035 Uiso 1 1 calc 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 0.0193(9) 0.0174(3) 0.0122(3) 0.0030(2) -0.0065(6) -0.0054(7) N1 0.0192(9) 0.0171(8) 0.0128(7) 0.0025(6) -0.0053(7) -0.0036(7) N2 0.0201(10) 0.0194(8) 0.0123(8) 0.0040(6) -0.0051(7) -0.0046(8) N3 0.0226(17) 0.024(2) 0.0151(16) 0.0040(14) -0.0070(15) -0.0086(15) O1 0.0235(18) 0.039(2) 0.035(2) 0.0023(17) -0.0148(17) -0.0041(16) C(A1 0.0220(11) 0.0197(10) 0.0143(9) 0.0042(7) -0.0071(9) -0.0067(9) C(B1 0.0263(12) 0.0198(10) 0.0179(10) 0.0050(8) -0.0073(9) -0.0045(9) C(B2 0.0249(12) 0.0197(10) 0.0180(10) 0.0029(8) -0.0077(9) -0.0038(9) C(A2 0.0189(11) 0.0178(9) 0.0151(9) 0.0028(7) -0.0065(8) -0.0034(8) C(M1 0.0187(10) 0.0189(9) 0.0181(9) 0.0035(7) -0.0088(9) -0.0047(8) C(A3 0.0201(11) 0.0206(10) 0.0170(9) 0.0018(8) -0.0075(9) -0.0050(9) C(B3 0.0257(12) 0.0202(10) 0.0170(9) 0.0018(8) -0.0063(9) -0.0044(9) C(B4 0.0258(12) 0.0234(11) 0.0146(9) 0.0007(8) -0.0062(9) -0.0025(10) C(A4 0.0213(11) 0.0222(10) 0.0130(9) 0.0023(7) -0.0067(8) -0.0063(9) C(M2 0.0193(10) 0.0216(10) 0.0133(8) 0.0045(7) -0.0068(8) -0.0059(8) C10 0.0207(11) 0.0171(9) 0.0167(9) 0.0012(7) -0.0065(8) -0.0056(8) C11 0.0249(12) 0.0195(11) 0.0469(16) -0.0062(11) -0.0165(12) -0.0043(10) C12 0.0257(13) 0.0228(12) 0.0456(17) -0.0056(11) -0.0152(12) -0.0003(10) C13 0.0361(14) 0.0175(9) 0.0176(9) -0.0022(7) -0.0068(10) -0.0049(10) C14 0.0407(16) 0.0270(14) 0.0459(17) -0.0054(12) -0.0170(14) -0.0154(12) C15 0.0231(12) 0.0305(14) 0.0485(17) -0.0055(12) -0.0125(12) -0.0103(11) C20 0.0258(12) 0.0179(9) 0.0131(8) 0.0023(7) -0.0070(8) -0.0054(9) C21 0.0245(12) 0.0397(15) 0.0186(11) 0.0054(10) -0.0084(9) -0.0124(11) C22 0.0282(12) 0.0347(14) 0.0208(11) 0.0046(10) -0.0043(10) -0.0130(11) C23 0.0387(14) 0.0190(10) 0.0134(9) 0.0043(7) -0.0054(10) -0.0073(10) C24 0.0445(16) 0.0391(15) 0.0231(12) 0.0084(11) -0.0210(12) -0.0161(13) C25 0.0316(13) 0.0408(15) 0.0238(12) 0.0106(11) -0.0154(11) -0.0190(12) _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 Fe1 Fe1 0.4272(16) 2_567 ? Fe1 N3 1.720(4) . ? Fe1 N1 1.979(3) 2_567 ? Fe1 N2 1.990(3) 2_567 ? Fe1 N2 2.001(3) . ? Fe1 N1 2.011(3) . ? Fe1 N3 2.146(4) 2_567 ? N1 C(A2 1.377(3) . ? N1 C(A1 1.384(3) . ? N1 Fe1 1.979(3) 2_567 ? N2 C(A3 1.372(3) . ? N2 C(A4 1.383(3) . ? N2 Fe1 1.990(3) 2_567 ? N3 O1 1.160(5) . ? N3 Fe1 2.146(4) 2_567 ? C(A1 C(M2 1.381(3) 2_567 ? C(A1 C(B1 1.437(3) . ? C(B1 C(B2 1.343(3) . ? C(B1 H(B1 0.9500 . ? C(B2 C(A2 1.439(3) . ? C(B2 H(B2 0.9500 . ? C(A2 C(M1 1.389(3) . ? C(M1 C(A3 1.395(3) . ? C(M1 C10 1.489(3) . ? C(A3 C(B3 1.444(3) . ? C(B3 C(B4 1.357(3) . ? C(B3 H(B3 0.9500 . ? C(B4 C(A4 1.433(3) . ? C(B4 H(B4 0.9500 . ? C(A4 C(M2 1.394(3) . ? C(M2 C(A1 1.381(3) 2_567 ? C(M2 C20 1.504(3) . ? C10 C15 1.381(4) . ? C10 C11 1.383(4) . ? C11 C12 1.388(4) . ? C11 H11 0.9500 . ? C12 C13 1.376(4) . ? C12 H12 0.9500 . ? C13 C14 1.381(4) . ? C13 H13 0.9500 . ? C14 C15 1.386(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C20 C25 1.381(4) . ? C20 C21 1.382(4) . ? C21 C22 1.393(4) . ? C21 H21 0.9500 . ? C22 C23 1.373(4) . ? C22 H22 0.9500 . ? C23 C24 1.379(4) . ? C23 H23 0.9500 . ? C24 C25 1.393(4) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Fe1 Fe1 N3 177.7(9) 2_567 . ? Fe1 Fe1 N1 88.2(8) 2_567 2_567 ? N3 Fe1 N1 91.98(18) . 2_567 ? Fe1 Fe1 N2 85.3(8) 2_567 2_567 ? N3 Fe1 N2 92.37(19) . 2_567 ? N1 Fe1 N2 89.91(15) 2_567 2_567 ? Fe1 Fe1 N2 82.4(7) 2_567 . ? N3 Fe1 N2 99.92(19) . . ? N1 Fe1 N2 89.70(15) 2_567 . ? N2 Fe1 N2 167.72(5) 2_567 . ? Fe1 Fe1 N1 79.6(8) 2_567 . ? N3 Fe1 N1 100.27(19) . . ? N1 Fe1 N1 167.74(5) 2_567 . ? N2 Fe1 N1 89.10(14) 2_567 . ? N2 Fe1 N1 88.69(14) . . ? Fe1 Fe1 N3 1.9(7) 2_567 2_567 ? N3 Fe1 N3 179.54(18) . 2_567 ? N1 Fe1 N3 88.05(15) 2_567 2_567 ? N2 Fe1 N3 87.17(15) 2_567 2_567 ? N2 Fe1 N3 80.55(14) . 2_567 ? N1 Fe1 N3 79.70(14) . 2_567 ? C(A2 N1 C(A1 104.99(18) . . ? C(A2 N1 Fe1 126.99(17) . 2_567 ? C(A1 N1 Fe1 127.47(18) . 2_567 ? C(A2 N1 Fe1 127.35(17) . . ? C(A1 N1 Fe1 127.21(17) . . ? Fe1 N1 Fe1 12.26(5) 2_567 . ? C(A3 N2 C(A4 105.00(18) . . ? C(A3 N2 Fe1 126.90(16) . 2_567 ? C(A4 N2 Fe1 127.68(18) . 2_567 ? C(A3 N2 Fe1 127.63(16) . . ? C(A4 N2 Fe1 126.79(18) . . ? Fe1 N2 Fe1 12.28(5) 2_567 . ? O1 N3 Fe1 144.5(4) . . ? O1 N3 Fe1 144.2(4) . 2_567 ? Fe1 N3 Fe1 0.46(18) . 2_567 ? C(M2 C(A1 N1 125.6(2) 2_567 . ? C(M2 C(A1 C(B1 124.1(2) 2_567 . ? N1 C(A1 C(B1 110.3(2) . . ? C(B2 C(B1 C(A1 107.09(19) . . ? C(B2 C(B1 H(B1 126.5 . . ? C(A1 C(B1 H(B1 126.5 . . ? C(B1 C(B2 C(A2 107.2(2) . . ? C(B1 C(B2 H(B2 126.4 . . ? C(A2 C(B2 H(B2 126.4 . . ? N1 C(A2 C(M1 126.2(2) . . ? N1 C(A2 C(B2 110.40(19) . . ? C(M1 C(A2 C(B2 123.4(2) . . ? C(A2 C(M1 C(A3 122.7(2) . . ? C(A2 C(M1 C10 119.18(19) . . ? C(A3 C(M1 C10 118.1(2) . . ? N2 C(A3 C(M1 126.2(2) . . ? N2 C(A3 C(B3 110.95(18) . . ? C(M1 C(A3 C(B3 122.9(2) . . ? C(B4 C(B3 C(A3 106.2(2) . . ? C(B4 C(B3 H(B3 126.9 . . ? C(A3 C(B3 H(B3 126.9 . . ? C(B3 C(B4 C(A4 107.2(2) . . ? C(B3 C(B4 H(B4 126.4 . . ? C(A4 C(B4 H(B4 126.4 . . ? N2 C(A4 C(M2 125.4(2) . . ? N2 C(A4 C(B4 110.55(19) . . ? C(M2 C(A4 C(B4 124.0(2) . . ? C(A1 C(M2 C(A4 123.9(2) 2_567 . ? C(A1 C(M2 C20 118.3(2) 2_567 . ? C(A4 C(M2 C20 117.8(2) . . ? C15 C10 C11 118.6(2) . . ? C15 C10 C(M1 121.0(2) . . ? C11 C10 C(M1 120.4(2) . . ? C10 C11 C12 120.6(2) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C11 120.5(3) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C14 119.1(2) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? C13 C14 C15 120.4(3) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C10 C15 C14 120.7(3) . . ? C10 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C25 C20 C21 119.3(2) . . ? C25 C20 C(M2 120.7(2) . . ? C21 C20 C(M2 120.0(2) . . ? C20 C21 C22 120.1(3) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 C21 120.3(3) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 119.9(2) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C25 119.9(3) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C20 C25 C24 120.4(3) . . ? C20 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? _diffrn_measured_fraction_theta_max 0.890 _diffrn_reflns_theta_full 34.57 _diffrn_measured_fraction_theta_full 0.890 _refine_diff_density_max 0.972 _refine_diff_density_min -0.458 _refine_diff_density_rms 0.110 _chemical_compound_source synthesized #===END data_130_cryst_4 # local ID: bcn350_130w5 _publ_requested_journal Inorg.Chem. _publ_contact_author_name 'Professor W. Robert Scheidt' _publ_contact_author_address ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; _publ_contact_author_email W.R.Scheidt.1@nd.edu _publ_contact_author_phone 1(574)6315939 _publ_contact_author_fax 1(574)6316652 loop_ _publ_author_name _publ_author_address 'Scheidt, W. Robert ' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Silvernail, Nathan J.' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Noll, Bruce C.' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Olmstead, Marilyn M.' ;University of California at Davis Department of Chemistry One Shields Avenue Davis, CA 95616 ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common [Fe(TPP)(NO)] _chemical_melting_point ? _chemical_formula_moiety 'C44 H28 Fe N5 O' _chemical_formula_sum 'C44 H28 Fe N5 O' _chemical_formula_weight 698.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7394(10) _cell_length_b 9.9634(10) _cell_length_c 10.3998(10) _cell_angle_alpha 82.078(4) _cell_angle_beta 65.661(4) _cell_angle_gamma 69.225(4) _cell_volume 859.65(15) _cell_formula_units_Z 1 _cell_measurement_temperature 128(2) _cell_measurement_reflns_used 8201 _cell_measurement_theta_min 2.432 _cell_measurement_theta_max 27.940 _exptl_crystal_description octahedron _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 361 _exptl_absorpt_coefficient_mu 0.482 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 0.90 _exptl_absorpt_process_details 'Sheldrick, G. M. (2007) SADABS. University of G\"ottingen, Germany.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 128(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Siemens KFFMO2K-90' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker x8-Apex II CCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4103 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 28.22 _reflns_number_total 4103 _reflns_number_gt 3204 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Bruker-Nonius AXS. (2007). APEX2 and SAINT. Bruker-Nonius AXS, Madison, Wisconsin, USA. CCDC. (2005). enCIFer. The Cambridge Crystallographic Data Centre, Cambridge, UK. Sheldrick, G. M. (2007). SADABS. University of G\"ottingen, Germany. Sheldrick, G. M. (2001). XCIF, XL, and XS. Bruker-Nonius AXS, Madison, Wisconsin, USA. Sheldrick, G. M. (2003). XPREP. Bruker-Nonius AXS, Madison, Wisconsin, USA. ; _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2007; Sheldrick, 2003)' _computing_structure_solution 'XS (Sheldrick, 2001)' _computing_structure_refinement 'XL (Sheldrick, 2001)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XCIF (Sheldrick, 2001)/enCIFer (CCDC, 2005)' _refine_special_details ; Crystal was modeled as 4-component nonmerohedral twin. Scale factors, relative to the first component, refined to 0.307(3), 0.175(3), and 0.189(3). Twin laws for each component follow. Domain 2: Rotated from first domain by 179.9 degrees about reciprocal axis 1.000 0.507 0.503 and real axis 1.000 0.149 0.062 Twin law to convert hkl from first to 0.808 0.269 0.111 this domain (SHELXL TWIN matrix): 0.917 -0.864 0.054 0.909 0.137 -0.944 Domain 3: Rotated from first domain by 90.2 degrees about reciprocal axis 1.000 0.509 0.515 and real axis 1.000 0.152 0.075 Twin law to convert hkl from first to 0.930 0.206 -0.068 this domain (SHELXL TWIN matrix): -0.029 0.094 0.953 0.992 -0.907 -0.031 Domain 4: Rotated from first domain by 90.4 degrees about reciprocal axis 1.000 0.510 0.501 and real axis 1.000 0.153 0.060 Twin law to convert hkl from first to 0.860 0.080 0.196 this domain (SHELXL TWIN matrix): 0.940 0.038 -0.888 -0.074 1.052 0.083 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^)+(0.0800P)^2^+0.3133P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4103 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1517 _refine_ls_wR_factor_gt 0.1354 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe -0.0198(4) 0.4980(5) 0.9983(6) 0.0221(4) Uani 0.50 1 d P . . N1 N 0.0363(3) 0.3191(2) 1.1076(2) 0.0222(5) Uani 1 1 d . . . N2 N 0.1434(3) 0.3910(3) 0.8208(2) 0.0237(5) Uani 1 1 d . . . N3 N -0.1910(5) 0.4905(5) 0.9910(5) 0.0237(9) Uani 0.50 1 d P . . O1 O -0.3205(5) 0.5546(5) 1.0025(6) 0.0425(11) Uani 0.50 1 d P . . C(A1 C -0.0268(3) 0.3024(3) 1.2526(3) 0.0235(6) Uani 1 1 d . . . C(B1 C 0.0296(4) 0.1543(3) 1.2878(3) 0.0282(6) Uani 1 1 d . . . H(B1 H 0.0030 0.1155 1.3801 0.034 Uiso 1 1 calc R . . C(B2 C 0.1271(4) 0.0804(3) 1.1666(3) 0.0280(6) Uani 1 1 d . . . H(B2 H 0.1824 -0.0201 1.1570 0.034 Uiso 1 1 calc R . . C(A2 C 0.1315(4) 0.1830(3) 1.0536(3) 0.0239(6) Uani 1 1 d . . . C(M1 C 0.2198(3) 0.1448(3) 0.9122(3) 0.0233(5) Uani 1 1 d . . . C(A3 C 0.2214(4) 0.2459(3) 0.8038(3) 0.0244(6) Uani 1 1 d . . . C(B3 C 0.3108(4) 0.2071(3) 0.6561(3) 0.0280(6) Uani 1 1 d . . . H(B3 H 0.3734 0.1133 0.6177 0.034 Uiso 1 1 calc R . . C(B4 C 0.2874(4) 0.3310(3) 0.5836(3) 0.0289(6) Uani 1 1 d . . . H(B4 H 0.3316 0.3408 0.4840 0.035 Uiso 1 1 calc R . . C(A4 C 0.1836(3) 0.4448(3) 0.6849(3) 0.0236(5) Uani 1 1 d . . . C(M2 C 0.1306(3) 0.5885(3) 0.6504(3) 0.0228(5) Uani 1 1 d . . . C10 C 0.3165(3) -0.0083(3) 0.8728(3) 0.0236(5) Uani 1 1 d . . . C11 C 0.4771(4) -0.0585(4) 0.8487(4) 0.0360(7) Uani 1 1 d . . . H11 H 0.5261 0.0056 0.8563 0.043 Uiso 1 1 calc R . . C12 C 0.5668(4) -0.2008(4) 0.8138(4) 0.0394(8) Uani 1 1 d . . . H12 H 0.6766 -0.2340 0.7989 0.047 Uiso 1 1 calc R . . C13 C 0.4986(4) -0.2948(3) 0.8004(3) 0.0326(6) Uani 1 1 d . . . H13 H 0.5606 -0.3926 0.7757 0.039 Uiso 1 1 calc R . . C14 C 0.3393(4) -0.2451(4) 0.8232(4) 0.0411(8) Uani 1 1 d . . . H14 H 0.2909 -0.3090 0.8142 0.049 Uiso 1 1 calc R . . C15 C 0.2490(4) -0.1031(4) 0.8592(4) 0.0397(8) Uani 1 1 d . . . H15 H 0.1391 -0.0705 0.8747 0.048 Uiso 1 1 calc R . . C20 C 0.1908(4) 0.6278(3) 0.4964(3) 0.0242(5) Uani 1 1 d . . . C21 C 0.3376(4) 0.6468(4) 0.4317(3) 0.0337(7) Uani 1 1 d . . . H21 H 0.4004 0.6359 0.4847 0.040 Uiso 1 1 calc R . . C22 C 0.3948(4) 0.6820(4) 0.2893(3) 0.0366(7) Uani 1 1 d . . . H22 H 0.4964 0.6945 0.2455 0.044 Uiso 1 1 calc R . . C23 C 0.3042(4) 0.6985(3) 0.2121(3) 0.0323(6) Uani 1 1 d . . . H23 H 0.3436 0.7216 0.1148 0.039 Uiso 1 1 calc R . . C24 C 0.1569(4) 0.6816(4) 0.2760(3) 0.0396(8) Uani 1 1 d . . . H24 H 0.0939 0.6938 0.2231 0.047 Uiso 1 1 calc R . . C25 C 0.0995(4) 0.6464(4) 0.4189(3) 0.0360(7) Uani 1 1 d . . . H25 H -0.0028 0.6352 0.4628 0.043 Uiso 1 1 calc 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 0.0255(15) 0.0228(4) 0.0155(4) 0.0036(3) -0.0069(11) -0.0077(11) N1 0.0218(12) 0.0232(12) 0.0147(10) 0.0021(8) -0.0042(9) -0.0037(9) N2 0.0245(12) 0.0275(13) 0.0168(10) 0.0038(9) -0.0082(10) -0.0073(10) N3 0.027(2) 0.025(2) 0.017(2) 0.0034(17) -0.0082(19) -0.0080(18) O1 0.028(2) 0.051(3) 0.047(3) 0.001(2) -0.019(2) -0.006(2) C(A1 0.0241(14) 0.0262(14) 0.0181(13) 0.0046(10) -0.0081(11) -0.0077(11) C(B1 0.0301(15) 0.0254(14) 0.0222(13) 0.0064(11) -0.0075(12) -0.0071(12) C(B2 0.0311(15) 0.0243(14) 0.0225(13) 0.0046(11) -0.0084(12) -0.0063(12) C(A2 0.0238(14) 0.0255(14) 0.0208(13) 0.0076(10) -0.0098(11) -0.0077(11) C(M1 0.0215(13) 0.0261(14) 0.0221(13) 0.0047(10) -0.0099(11) -0.0078(11) C(A3 0.0254(14) 0.0274(15) 0.0203(12) 0.0031(11) -0.0109(12) -0.0073(12) C(B3 0.0302(15) 0.0266(14) 0.0218(13) 0.0004(11) -0.0090(12) -0.0048(12) C(B4 0.0307(16) 0.0322(16) 0.0172(12) 0.0008(11) -0.0076(12) -0.0051(13) C(A4 0.0257(14) 0.0263(14) 0.0162(12) 0.0038(10) -0.0082(11) -0.0071(11) C(M2 0.0224(13) 0.0282(14) 0.0154(11) 0.0070(10) -0.0068(10) -0.0089(11) C10 0.0254(14) 0.0236(13) 0.0183(12) 0.0027(10) -0.0071(11) -0.0066(11) C11 0.0299(16) 0.0300(16) 0.052(2) -0.0038(14) -0.0191(15) -0.0085(13) C12 0.0303(17) 0.0345(18) 0.051(2) -0.0050(15) -0.0177(15) -0.0035(14) C13 0.0448(19) 0.0243(14) 0.0189(12) -0.0018(10) -0.0064(13) -0.0068(13) C14 0.0444(19) 0.0336(18) 0.049(2) -0.0068(15) -0.0159(16) -0.0168(15) C15 0.0290(16) 0.0401(19) 0.055(2) -0.0035(16) -0.0169(15) -0.0148(14) C20 0.0289(14) 0.0239(13) 0.0151(11) 0.0028(9) -0.0071(11) -0.0064(11) C21 0.0313(15) 0.0468(19) 0.0230(14) 0.0075(13) -0.0106(12) -0.0154(14) C22 0.0358(16) 0.0429(19) 0.0246(14) 0.0067(13) -0.0049(13) -0.0161(14) C23 0.0451(18) 0.0255(14) 0.0179(12) 0.0060(10) -0.0072(13) -0.0106(13) C24 0.053(2) 0.047(2) 0.0253(15) 0.0075(14) -0.0234(15) -0.0158(16) C25 0.0372(17) 0.050(2) 0.0280(16) 0.0108(14) -0.0159(14) -0.0226(15) _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 Fe1 Fe1 0.418(4) 2_567 ? Fe1 N3 1.728(5) . ? Fe1 N1 1.986(6) 2_567 ? Fe1 N2 1.993(6) 2_567 ? Fe1 N2 1.999(6) . ? Fe1 N1 2.008(6) . ? Fe1 N3 2.145(5) 2_567 ? N1 C(A2 1.379(4) . ? N1 C(A1 1.385(3) . ? N1 Fe1 1.986(6) 2_567 ? N2 C(A3 1.371(4) . ? N2 C(A4 1.386(3) . ? N2 Fe1 1.993(6) 2_567 ? N3 O1 1.156(6) . ? N3 Fe1 2.145(5) 2_567 ? C(A1 C(M2 1.379(4) 2_567 ? C(A1 C(B1 1.434(4) . ? C(B1 C(B2 1.344(4) . ? C(B1 H(B1 0.9500 . ? C(B2 C(A2 1.445(4) . ? C(B2 H(B2 0.9500 . ? C(A2 C(M1 1.388(4) . ? C(M1 C(A3 1.403(4) . ? C(M1 C10 1.488(4) . ? C(A3 C(B3 1.445(4) . ? C(B3 C(B4 1.353(4) . ? C(B3 H(B3 0.9500 . ? C(B4 C(A4 1.434(4) . ? C(B4 H(B4 0.9500 . ? C(A4 C(M2 1.390(4) . ? C(M2 C(A1 1.379(4) 2_567 ? C(M2 C20 1.510(3) . ? C10 C15 1.378(5) . ? C10 C11 1.384(4) . ? C11 C12 1.380(4) . ? C11 H11 0.9500 . ? C12 C13 1.376(5) . ? C12 H12 0.9500 . ? C13 C14 1.376(5) . ? C13 H13 0.9500 . ? C14 C15 1.381(5) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C20 C21 1.377(4) . ? C20 C25 1.382(4) . ? C21 C22 1.394(4) . ? C21 H21 0.9500 . ? C22 C23 1.376(5) . ? C22 H22 0.9500 . ? C23 C24 1.372(5) . ? C23 H23 0.9500 . ? C24 C25 1.398(4) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Fe1 Fe1 N3 176.6(16) 2_567 . ? Fe1 Fe1 N1 86.9(15) 2_567 2_567 ? N3 Fe1 N1 91.7(3) . 2_567 ? Fe1 Fe1 N2 84.7(14) 2_567 2_567 ? N3 Fe1 N2 92.1(3) . 2_567 ? N1 Fe1 N2 89.7(2) 2_567 2_567 ? Fe1 Fe1 N2 83.3(14) 2_567 . ? N3 Fe1 N2 99.9(3) . . ? N1 Fe1 N2 89.6(2) 2_567 . ? N2 Fe1 N2 167.99(10) 2_567 . ? Fe1 Fe1 N1 81.1(15) 2_567 . ? N3 Fe1 N1 100.2(3) . . ? N1 Fe1 N1 168.01(10) 2_567 . ? N2 Fe1 N1 89.2(2) 2_567 . ? N2 Fe1 N1 88.9(2) . . ? Fe1 Fe1 N3 2.8(13) 2_567 2_567 ? N3 Fe1 N3 179.3(3) . 2_567 ? N1 Fe1 N3 88.0(2) 2_567 2_567 ? N2 Fe1 N3 87.3(2) 2_567 2_567 ? N2 Fe1 N3 80.73(19) . 2_567 ? N1 Fe1 N3 80.0(2) . 2_567 ? C(A2 N1 C(A1 105.2(2) . . ? C(A2 N1 Fe1 126.8(2) . 2_567 ? C(A1 N1 Fe1 127.4(2) . 2_567 ? C(A2 N1 Fe1 127.1(2) . . ? C(A1 N1 Fe1 127.3(2) . . ? Fe1 N1 Fe1 11.99(10) 2_567 . ? C(A3 N2 C(A4 104.9(2) . . ? C(A3 N2 Fe1 127.3(2) . 2_567 ? C(A4 N2 Fe1 127.6(3) . 2_567 ? C(A3 N2 Fe1 127.6(2) . . ? C(A4 N2 Fe1 126.9(2) . . ? Fe1 N2 Fe1 12.01(10) 2_567 . ? O1 N3 Fe1 145.7(5) . . ? O1 N3 Fe1 145.1(4) . 2_567 ? Fe1 N3 Fe1 0.7(3) . 2_567 ? C(M2 C(A1 N1 125.3(3) 2_567 . ? C(M2 C(A1 C(B1 124.6(2) 2_567 . ? N1 C(A1 C(B1 110.1(2) . . ? C(B2 C(B1 C(A1 107.6(2) . . ? C(B2 C(B1 H(B1 126.2 . . ? C(A1 C(B1 H(B1 126.2 . . ? C(B1 C(B2 C(A2 106.8(2) . . ? C(B1 C(B2 H(B2 126.6 . . ? C(A2 C(B2 H(B2 126.6 . . ? N1 C(A2 C(M1 126.7(2) . . ? N1 C(A2 C(B2 110.2(2) . . ? C(M1 C(A2 C(B2 123.0(2) . . ? C(A2 C(M1 C(A3 122.2(2) . . ? C(A2 C(M1 C10 119.4(2) . . ? C(A3 C(M1 C10 118.4(2) . . ? N2 C(A3 C(M1 126.2(3) . . ? N2 C(A3 C(B3 111.1(2) . . ? C(M1 C(A3 C(B3 122.7(3) . . ? C(B4 C(B3 C(A3 106.3(2) . . ? C(B4 C(B3 H(B3 126.9 . . ? C(A3 C(B3 H(B3 126.9 . . ? C(B3 C(B4 C(A4 107.3(2) . . ? C(B3 C(B4 H(B4 126.3 . . ? C(A4 C(B4 H(B4 126.3 . . ? N2 C(A4 C(M2 125.2(2) . . ? N2 C(A4 C(B4 110.5(2) . . ? C(M2 C(A4 C(B4 124.3(2) . . ? C(A1 C(M2 C(A4 124.4(2) 2_567 . ? C(A1 C(M2 C20 117.8(2) 2_567 . ? C(A4 C(M2 C20 117.7(2) . . ? C15 C10 C11 118.4(3) . . ? C15 C10 C(M1 121.1(3) . . ? C11 C10 C(M1 120.5(3) . . ? C12 C11 C10 120.7(3) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C13 C12 C11 120.5(3) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 C12 118.9(3) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? C13 C14 C15 120.7(3) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C10 C15 C14 120.7(3) . . ? C10 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C21 C20 C25 119.2(2) . . ? C21 C20 C(M2 120.1(3) . . ? C25 C20 C(M2 120.7(3) . . ? C20 C21 C22 120.5(3) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C23 C22 C21 120.0(3) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C24 C23 C22 119.8(3) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C25 120.2(3) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C20 C25 C24 120.2(3) . . ? C20 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 28.22 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.776 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.086 _chemical_compound_source synthesized #===END data_180_cryst_1 # local ID: mo180 _publ_requested_journal Inorg.Chem. _publ_contact_author_name 'Professor W. Robert Scheidt' _publ_contact_author_address ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; _publ_contact_author_email W.R.Scheidt.1@nd.edu _publ_contact_author_phone 1(574)6315939 _publ_contact_author_fax 1(574)6316652 loop_ _publ_author_name _publ_author_address 'Scheidt, W. Robert ' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Silvernail, Nathan J.' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Noll, Bruce C.' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Olmstead, Marilyn M.' ;University of California at Davis Department of Chemistry One Shields Avenue Davis, CA 95616 ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common [Fe(TPP)(NO] _chemical_melting_point ? _chemical_formula_moiety 'C44 H28 Fe N5 O' _chemical_formula_sum 'C44 H28 Fe N5 O' _chemical_formula_weight 698.56 _chemical_compound_source synthesized loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' .3463 .8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.765(2) _cell_length_b 10.120(2) _cell_length_c 10.466(2) _cell_angle_alpha 81.35(2) _cell_angle_beta 65.23(2) _cell_angle_gamma 68.12(2) _cell_volume 871.4(4) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'square bipyramid' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 361 _exptl_absorpt_coefficient_mu 0.476 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9067 _exptl_absorpt_correction_T_max 0.9629 _exptl_absorpt_process_details 'Blessing, R.H. ACTA Cryst. (1995) A51, 33-38' _exptl_crystal_recrystallization_method 'liquid diffusion (chloroform/methanol)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4628 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0964 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 28.37 _reflns_number_total 4628 _reflns_number_gt 2579 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Platon (Spek, 2004)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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. The structures were solved by direct methods using SHELXS-97 and refined against F^2^ using SHELXL-97;subsequent difference Fourier syntheses led to the location of most of the remaining non-hydrogen atoms. For the structure refinement all data were used including negative intensities. All nonhydrogen atoms were refined anisotropically. Hydrogen atoms were idealized with the standard SHELXL-97 idealization methods. Hydrogen atoms were placed at calculated geometries and allowed to ride on the position of the parent atom. Hydrogen thermal parameters were set to 1.2\\times the equivalent isotropic U of the parent atom, 1.5\\times for methyl hydrogens. The program SADABS was applied for the absorption correction. The structure is a tetraphenyl porphyrin bound axially by a nitrosyl. ; _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^)+(0.0648P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4628 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1034 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1102 _refine_ls_wR_factor_gt 0.0981 _refine_ls_goodness_of_fit_ref 0.893 _refine_ls_restrained_S_all 0.893 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.4794(5) 0.4972(7) 0.5008(8) 0.0274(6) Uani 0.50 1 d P . . N1 N 0.4619(2) 0.68075(18) 0.39300(19) 0.0291(5) Uani 1 1 d . . . N2 N 0.3566(2) 0.60801(19) 0.67935(18) 0.0286(5) Uani 1 1 d . . . C(M1 C 0.6301(3) 0.5889(2) 0.1504(2) 0.0296(5) Uani 1 1 d . . . C(M2 C 0.2801(3) 0.8529(2) 0.5884(2) 0.0282(5) Uani 1 1 d . . . C(A1 C 0.5255(3) 0.6974(2) 0.2482(2) 0.0300(6) Uani 1 1 d . . . C(A2 C 0.3673(3) 0.8151(2) 0.4472(2) 0.0287(5) Uani 1 1 d . . . C(A3 C 0.2773(3) 0.7531(2) 0.6972(2) 0.0310(6) Uani 1 1 d . . . C(A4 C 0.3170(3) 0.5539(2) 0.8147(2) 0.0315(6) Uani 1 1 d . . . C(B1 C 0.4694(3) 0.8445(2) 0.2135(2) 0.0370(6) Uani 1 1 d . . . H(BA H 0.4962 0.8835 0.1215 0.044 Uiso 1 1 calc R . . C(B2 C 0.3717(3) 0.9179(2) 0.3350(2) 0.0346(6) Uani 1 1 d . . . H(BB H 0.3165 1.0178 0.3449 0.042 Uiso 1 1 calc R . . C(B3 C 0.1897(3) 0.7896(2) 0.8428(2) 0.0381(6) Uani 1 1 d . . . H(BC H 0.1264 0.8825 0.8816 0.046 Uiso 1 1 calc R . . C(B4 C 0.2138(3) 0.6672(2) 0.9150(2) 0.0369(6) Uani 1 1 d . . . H(BD H 0.1702 0.6578 1.0144 0.044 Uiso 1 1 calc R . . C10 C 0.6892(3) 0.6280(2) -0.0032(2) 0.0311(6) Uani 1 1 d . . . C11 C 0.8357(3) 0.6466(3) -0.0691(3) 0.0430(7) Uani 1 1 d . . . H11A H 0.8990 0.6354 -0.0171 0.052 Uiso 1 1 calc R . . C12 C 0.8920(3) 0.6813(3) -0.2102(3) 0.0457(7) Uani 1 1 d . . . H12A H 0.9934 0.6938 -0.2544 0.055 Uiso 1 1 calc R . . C13 C 0.8018(3) 0.6979(2) -0.2867(3) 0.0427(7) Uani 1 1 d . . . H13A H 0.8411 0.7203 -0.3839 0.051 Uiso 1 1 calc R . . C14 C 0.6541(4) 0.6817(3) -0.2212(3) 0.0521(8) Uani 1 1 d . . . H14A H 0.5902 0.6940 -0.2730 0.063 Uiso 1 1 calc R . . C15 C 0.5982(3) 0.6473(3) -0.0792(3) 0.0460(7) Uani 1 1 d . . . H15A H 0.4957 0.6372 -0.0343 0.055 Uiso 1 1 calc R . . C20 C 0.1843(3) 1.0063(2) 0.6278(2) 0.0291(5) Uani 1 1 d . . . C21 C 0.0231(3) 1.0604(3) 0.6514(3) 0.0436(7) Uani 1 1 d . . . H21A H -0.0274 0.9996 0.6437 0.052 Uiso 1 1 calc R . . C22 C -0.0651(3) 1.2025(3) 0.6861(3) 0.0514(8) Uani 1 1 d . . . H22A H -0.1756 1.2385 0.7013 0.062 Uiso 1 1 calc R . . C23 C 0.0043(4) 1.2918(3) 0.6988(2) 0.0427(7) Uani 1 1 d . . . H23A H -0.0567 1.3894 0.7224 0.051 Uiso 1 1 calc R . . C24 C 0.1638(4) 1.2381(3) 0.6768(3) 0.0510(8) Uani 1 1 d . . . H24A H 0.2135 1.2988 0.6862 0.061 Uiso 1 1 calc R . . C25 C 0.2525(3) 1.0969(3) 0.6411(3) 0.0470(7) Uani 1 1 d . . . H25A H 0.3631 1.0618 0.6254 0.056 Uiso 1 1 calc R . . N3 N 0.3085(4) 0.4909(4) 0.4914(4) 0.0293(9) Uani 0.50 1 d P . . O1 O 0.1806(4) 0.5506(4) 0.5019(4) 0.0590(11) Uani 0.50 1 d 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 Fe1 0.0263(19) 0.0261(5) 0.0208(3) 0.0031(3) -0.0021(15) -0.0088(13) N1 0.0277(11) 0.0279(10) 0.0237(11) 0.0030(8) -0.0083(9) -0.0045(9) N2 0.0291(11) 0.0276(10) 0.0229(10) 0.0035(8) -0.0089(9) -0.0062(9) C(M1 0.0278(13) 0.0349(13) 0.0223(12) 0.0056(9) -0.0090(10) -0.0097(11) C(M2 0.0264(13) 0.0261(12) 0.0285(13) 0.0005(9) -0.0102(11) -0.0060(10) C(A1 0.0292(13) 0.0325(13) 0.0252(13) 0.0045(10) -0.0099(11) -0.0098(11) C(A2 0.0265(13) 0.0297(12) 0.0279(13) 0.0034(9) -0.0107(11) -0.0088(11) C(A3 0.0280(14) 0.0308(13) 0.0282(13) -0.0008(10) -0.0091(11) -0.0058(11) C(A4 0.0292(14) 0.0342(13) 0.0251(13) 0.0032(10) -0.0096(11) -0.0071(11) C(B1 0.0395(15) 0.0307(13) 0.0327(14) 0.0078(10) -0.0122(12) -0.0088(11) C(B2 0.0388(15) 0.0263(12) 0.0309(14) 0.0035(10) -0.0117(12) -0.0065(11) C(B3 0.0376(15) 0.0333(13) 0.0334(14) -0.0025(10) -0.0097(12) -0.0056(12) C(B4 0.0417(15) 0.0378(14) 0.0202(12) -0.0011(10) -0.0063(11) -0.0083(12) C10 0.0367(15) 0.0263(12) 0.0230(12) 0.0041(9) -0.0092(11) -0.0075(11) C11 0.0386(15) 0.0575(17) 0.0333(15) 0.0095(12) -0.0145(13) -0.0203(14) C12 0.0446(17) 0.0527(17) 0.0338(16) 0.0052(12) -0.0063(13) -0.0230(14) C13 0.0597(19) 0.0292(13) 0.0234(13) 0.0046(10) -0.0073(13) -0.0108(13) C14 0.067(2) 0.0599(19) 0.0353(17) 0.0122(13) -0.0296(15) -0.0214(16) C15 0.0430(16) 0.0623(18) 0.0386(17) 0.0121(13) -0.0192(13) -0.0254(14) C20 0.0320(14) 0.0284(12) 0.0218(12) 0.0007(9) -0.0072(11) -0.0091(11) C21 0.0335(15) 0.0347(15) 0.0643(19) -0.0080(12) -0.0199(14) -0.0098(12) C22 0.0367(17) 0.0414(17) 0.068(2) -0.0085(14) -0.0202(15) -0.0016(14) C23 0.059(2) 0.0263(13) 0.0293(14) -0.0017(10) -0.0107(13) -0.0077(14) C24 0.064(2) 0.0374(16) 0.060(2) -0.0034(13) -0.0260(16) -0.0229(15) C25 0.0378(16) 0.0440(17) 0.063(2) -0.0056(13) -0.0210(14) -0.0144(14) N3 0.028(2) 0.032(2) 0.022(2) 0.0044(16) -0.0101(18) -0.0070(18) O1 0.040(2) 0.069(3) 0.071(3) 0.004(2) -0.028(2) -0.017(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 Fe1 0.421(6) 2_666 ? Fe1 N3 1.736(5) . ? Fe1 N2 1.984(7) . ? Fe1 N1 1.993(7) 2_666 ? Fe1 N1 2.012(7) . ? Fe1 N2 2.014(7) 2_666 ? Fe1 N3 2.154(5) 2_666 ? N1 C(A2 1.371(3) . ? N1 C(A1 1.387(3) . ? N1 Fe1 1.993(7) 2_666 ? N2 C(A3 1.380(3) . ? N2 C(A4 1.386(3) . ? N2 Fe1 2.014(7) 2_666 ? C(M1 C(A1 1.386(3) . ? C(M1 C(A4 1.390(3) 2_666 ? C(M1 C10 1.508(3) . ? C(M2 C(A2 1.389(3) . ? C(M2 C(A3 1.402(3) . ? C(M2 C20 1.497(3) . ? C(A1 C(B1 1.431(3) . ? C(A2 C(B2 1.444(3) . ? C(A3 C(B3 1.426(3) . ? C(A4 C(M1 1.390(3) 2_666 ? C(A4 C(B4 1.431(3) . ? C(B1 C(B2 1.348(3) . ? C(B1 H(BA 0.9500 . ? C(B2 H(BB 0.9500 . ? C(B3 C(B4 1.345(3) . ? C(B3 H(BC 0.9500 . ? C(B4 H(BD 0.9500 . ? C10 C15 1.370(3) . ? C10 C11 1.376(3) . ? C11 C12 1.384(3) . ? C11 H11A 0.9500 . ? C12 C13 1.372(4) . ? C12 H12A 0.9500 . ? C13 C14 1.376(4) . ? C13 H13A 0.9500 . ? C14 C15 1.390(3) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C20 C25 1.369(4) . ? C20 C21 1.383(4) . ? C21 C22 1.384(3) . ? C21 H21A 0.9500 . ? C22 C23 1.364(4) . ? C22 H22A 0.9500 . ? C23 C24 1.371(4) . ? C23 H23A 0.9500 . ? C24 C25 1.378(3) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? N3 O1 1.131(4) . ? N3 Fe1 2.154(5) 2_666 ? 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 Fe1 Fe1 N3 173(2) 2_666 . ? Fe1 Fe1 N2 88(2) 2_666 . ? N3 Fe1 N2 93.6(3) . . ? Fe1 Fe1 N1 87(2) 2_666 2_666 ? N3 Fe1 N1 100.5(3) . 2_666 ? N2 Fe1 N1 90.2(3) . 2_666 ? Fe1 Fe1 N1 81.4(19) 2_666 . ? N3 Fe1 N1 91.5(3) . . ? N2 Fe1 N1 89.4(3) . . ? N1 Fe1 N1 167.95(17) 2_666 . ? Fe1 Fe1 N2 79.9(19) 2_666 2_666 ? N3 Fe1 N2 98.4(3) . 2_666 ? N2 Fe1 N2 167.96(18) . 2_666 ? N1 Fe1 N2 89.1(3) 2_666 2_666 ? N1 Fe1 N2 88.8(3) . 2_666 ? Fe1 Fe1 N3 5.8(18) 2_666 2_666 ? N3 Fe1 N3 178.6(4) . 2_666 ? N2 Fe1 N3 86.7(2) . 2_666 ? N1 Fe1 N3 80.9(2) 2_666 2_666 ? N1 Fe1 N3 87.1(2) . 2_666 ? N2 Fe1 N3 81.3(2) 2_666 2_666 ? C(A2 N1 C(A1 105.52(18) . . ? C(A2 N1 Fe1 127.4(3) . 2_666 ? C(A1 N1 Fe1 126.6(2) . 2_666 ? C(A2 N1 Fe1 126.5(3) . . ? C(A1 N1 Fe1 127.5(3) . . ? C(A3 N2 C(A4 104.73(18) . . ? C(A3 N2 Fe1 128.1(3) . . ? C(A4 N2 Fe1 126.9(3) . . ? C(A3 N2 Fe1 127.2(2) . 2_666 ? C(A4 N2 Fe1 127.4(3) . 2_666 ? C(A1 C(M1 C(A4 123.9(2) . 2_666 ? C(A1 C(M1 C10 118.13(19) . . ? C(A4 C(M1 C10 117.97(19) 2_666 . ? C(A2 C(M2 C(A3 122.8(2) . . ? C(A2 C(M2 C20 119.25(19) . . ? C(A3 C(M2 C20 118.0(2) . . ? C(M1 C(A1 N1 125.7(2) . . ? C(M1 C(A1 C(B1 124.4(2) . . ? N1 C(A1 C(B1 109.93(18) . . ? N1 C(A2 C(M2 126.8(2) . . ? N1 C(A2 C(B2 110.3(2) . . ? C(M2 C(A2 C(B2 122.9(2) . . ? N2 C(A3 C(M2 125.4(2) . . ? N2 C(A3 C(B3 110.81(19) . . ? C(M2 C(A3 C(B3 123.8(2) . . ? N2 C(A4 C(M1 125.6(2) . 2_666 ? N2 C(A4 C(B4 110.01(19) . . ? C(M1 C(A4 C(B4 124.4(2) 2_666 . ? C(B2 C(B1 C(A1 107.6(2) . . ? C(B2 C(B1 H(BA 126.2 . . ? C(A1 C(B1 H(BA 126.2 . . ? C(B1 C(B2 C(A2 106.71(19) . . ? C(B1 C(B2 H(BB 126.6 . . ? C(A2 C(B2 H(BB 126.6 . . ? C(B4 C(B3 C(A3 106.9(2) . . ? C(B4 C(B3 H(BC 126.5 . . ? C(A3 C(B3 H(BC 126.5 . . ? C(B3 C(B4 C(A4 107.5(2) . . ? C(B3 C(B4 H(BD 126.2 . . ? C(A4 C(B4 H(BD 126.2 . . ? C15 C10 C11 118.8(2) . . ? C15 C10 C(M1 121.1(2) . . ? C11 C10 C(M1 120.2(2) . . ? C10 C11 C12 120.8(3) . . ? C10 C11 H11A 119.6 . . ? C12 C11 H11A 119.6 . . ? C13 C12 C11 120.3(3) . . ? C13 C12 H12A 119.9 . . ? C11 C12 H12A 119.9 . . ? C12 C13 C14 119.4(2) . . ? C12 C13 H13A 120.3 . . ? C14 C13 H13A 120.3 . . ? C13 C14 C15 119.9(3) . . ? C13 C14 H14A 120.0 . . ? C15 C14 H14A 120.0 . . ? C10 C15 C14 120.9(3) . . ? C10 C15 H15A 119.6 . . ? C14 C15 H15A 119.6 . . ? C25 C20 C21 118.1(2) . . ? C25 C20 C(M2 121.5(2) . . ? C21 C20 C(M2 120.3(2) . . ? C20 C21 C22 120.4(3) . . ? C20 C21 H21A 119.8 . . ? C22 C21 H21A 119.8 . . ? C23 C22 C21 121.0(3) . . ? C23 C22 H22A 119.5 . . ? C21 C22 H22A 119.5 . . ? C22 C23 C24 118.8(2) . . ? C22 C23 H23A 120.6 . . ? C24 C23 H23A 120.6 . . ? C23 C24 C25 120.5(3) . . ? C23 C24 H24A 119.7 . . ? C25 C24 H24A 119.7 . . ? C20 C25 C24 121.3(2) . . ? C20 C25 H25A 119.4 . . ? C24 C25 H25A 119.4 . . ? O1 N3 Fe1 147.3(4) . . ? O1 N3 Fe1 146.5(4) . 2_666 ? _diffrn_measured_fraction_theta_max .963 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full .963 _refine_diff_density_max .430 _refine_diff_density_min -.433 _refine_diff_density_rms .066 #===END data_273_cryst_4 # locla ID: bcn350_273_0m _publ_requested_journal Inorg.Chem. _publ_contact_author_name 'Professor W. Robert Scheidt' _publ_contact_author_address ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; _publ_contact_author_email W.R.Scheidt.1@nd.edu _publ_contact_author_phone 1(574)6315939 _publ_contact_author_fax 1(574)6316652 loop_ _publ_author_name _publ_author_address 'Scheidt, W. Robert ' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Silvernail, Nathan J.' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Noll, Bruce C.' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Olmstead, Marilyn M.' ;University of California at Davis Department of Chemistry One Shields Avenue Davis, CA 95616 ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common [Fe(TPP)(NO)] _chemical_melting_point ? _chemical_formula_moiety 'C44 H28 Fe N5 O' _chemical_formula_sum 'C44 H28 Fe N5 O' _chemical_formula_weight 698.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 4/m' _symmetry_int_tables_number 87 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 13.4152(2) _cell_length_b 13.4152(2) _cell_length_c 9.7151(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1748.40(7) _cell_formula_units_Z 2 _cell_measurement_temperature 272(2) _cell_measurement_reflns_used 4123 _cell_measurement_theta_min 2.5885 _cell_measurement_theta_max 26.4586 _exptl_crystal_description octahedron _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 722 _exptl_absorpt_coefficient_mu 0.474 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8783 _exptl_absorpt_correction_T_max 0.8783 _exptl_absorpt_process_details 'Sheldrick, G. M. (2007). SADABS. University of G\"ottingen. Germany.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 272(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Siemens KFFMO2K-90' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8-Apex II CCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11545 _diffrn_reflns_av_R_equivalents 0.0238 _diffrn_reflns_av_sigmaI/netI 0.0112 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 27.87 _reflns_number_total 1101 _reflns_number_gt 918 _reflns_threshold_expression >2sigma(I) # References and fields for routine structure determination _publ_section_references ; Bruker-Nonius AXS. (2004). APEX2 and SAINT. Bruker-Nonius AXS, Madison, Wisconsin, USA. CCDC. (2004). enCIFer. The Cambridge Crystallographic Data Centre, Cambridge, UK. Sheldrick, G. M. (2001). XCIF, XL, and XS. Bruker-Nonius AXS, Madison, Wisconsin, USA. Sheldrick, G. M. (2003). XPREP. Bruker-Nonius AXS, Madison, Wisconsin, USA. ; _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'APEX2/SAINT (Bruker, 2007)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2007; Sheldrick, 2003)' _computing_structure_solution 'XS (Sheldrick, 2001)' _computing_structure_refinement 'XL (Sheldrick, 2001)' _computing_molecular_graphics 'XP (Sheldrick, 1998)' _computing_publication_material 'XCIF (Sheldrick, 2001)/enCIFer (CCDC, 2005)' _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^)+(0.0698P)^2^+0.5801P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1101 _refine_ls_number_parameters 82 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.1239 _refine_ls_wR_factor_gt 0.1132 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.5000 0.5000 0.02458(14) 0.0458(5) Uani 0.50 4 d SP . . N1 N 0.35686(13) 0.53668(13) 0.0000 0.0489(4) Uani 1 2 d S . . N2 N 0.5000 0.5000 0.1998(6) 0.0494(11) Uani 0.50 4 d SP . . O1 O 0.516(6) 0.4625(10) 0.2967(10) 0.095(15) Uani 0.13 1 d P . . C(A1 C 0.27652(16) 0.47339(17) 0.0000 0.0513(5) Uani 1 2 d S . . C(B1 C 0.18567(18) 0.52908(18) 0.0000 0.0617(6) Uani 1 2 d S . . H(B1 H 0.1214 0.5030 0.0000 0.074 Uiso 1 2 calc SR . . C(B2 C 0.21027(17) 0.62567(19) 0.0000 0.0610(6) Uani 1 2 d S . . H(B2 H 0.1664 0.6793 0.0000 0.073 Uiso 1 2 calc SR . . C(A2 C 0.31728(16) 0.63098(17) 0.0000 0.0520(5) Uani 1 2 d S . . C(M1 C 0.37002(17) 0.71920(16) 0.0000 0.0511(5) Uani 1 2 d S . . C10 C 0.31341(16) 0.81527(16) 0.0000 0.0535(5) Uani 1 2 d S . . C11 C 0.28725(18) 0.86012(15) 0.1208(2) 0.0770(6) Uani 1 1 d . . . H11 H 0.3056 0.8312 0.2040 0.092 Uiso 1 1 calc R . . C12 C 0.2335(2) 0.94844(16) 0.1204(3) 0.0857(7) Uani 1 1 d . . . H12 H 0.2158 0.9782 0.2033 0.103 Uiso 1 1 calc R . . C13 C 0.2066(2) 0.99164(18) 0.0000 0.0730(7) Uani 1 2 d S . . H13 H 0.1699 1.0505 0.0000 0.088 Uiso 1 2 calc SR . . 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 0.0429(3) 0.0429(3) 0.0515(13) 0.000 0.000 0.000 N1 0.0471(9) 0.0464(9) 0.0532(9) 0.000 0.000 0.0005(6) N2 0.0456(15) 0.0456(15) 0.057(3) 0.000 0.000 0.000 O1 0.15(4) 0.077(7) 0.061(4) 0.025(8) -0.036(17) -0.023(18) C(A1 0.0461(10) 0.0535(11) 0.0544(11) 0.000 0.000 -0.0002(8) C(B1 0.0462(11) 0.0591(13) 0.0799(15) 0.000 0.000 0.0009(9) C(B2 0.0476(11) 0.0556(12) 0.0798(15) 0.000 0.000 0.0054(9) C(A2 0.0479(11) 0.0524(11) 0.0557(11) 0.000 0.000 0.0040(9) C(M1 0.0532(11) 0.0486(11) 0.0515(10) 0.000 0.000 0.0058(9) C10 0.0500(11) 0.0455(10) 0.0649(12) 0.000 0.000 0.0025(8) C11 0.0974(15) 0.0696(11) 0.0640(10) -0.0043(9) -0.0019(10) 0.0239(10) C12 0.0977(16) 0.0686(12) 0.0909(15) -0.0196(10) 0.0041(12) 0.0212(11) C13 0.0612(14) 0.0450(12) 0.113(2) 0.000 0.000 0.0051(10) _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 Fe1 Fe1 0.478(3) 9_665 ? Fe1 N2 1.702(5) . ? Fe1 N1 1.9966(18) 11_565 ? Fe1 N1 1.9966(18) . ? Fe1 N1 1.9966(18) 9_665 ? Fe1 N1 1.9966(18) 3_655 ? Fe1 N2 2.180(6) 9_665 ? N1 C(A2 1.372(3) . ? N1 C(A1 1.372(3) . ? N1 Fe1 1.9966(18) 9_665 ? N2 O1 1.088(18) 3_655 ? N2 O1 1.088(18) 2_665 ? N2 O1 1.088(18) . ? N2 O1 1.088(18) 4_565 ? N2 Fe1 2.180(6) 9_665 ? O1 O1 0.77(4) 3_655 ? O1 O1 0.77(4) 4_565 ? O1 O1 1.09(6) 2_665 ? C(A1 C(M1 1.388(3) 3_655 ? C(A1 C(B1 1.430(3) . ? C(B1 C(B2 1.337(4) . ? C(B1 H(B1 0.9300 . ? C(B2 C(A2 1.437(3) . ? C(B2 H(B2 0.9300 . ? C(A2 C(M1 1.379(3) . ? C(M1 C(A1 1.388(3) 11_565 ? C(M1 C10 1.496(3) . ? C10 C11 1.364(2) 10 ? C10 C11 1.364(2) . ? C11 C12 1.387(3) . ? C11 H11 0.9300 . ? C12 C13 1.354(3) . ? C12 H12 0.9300 . ? C13 C12 1.354(3) 10 ? C13 H13 0.9300 . ? 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 Fe1 Fe1 N2 180.000(2) 9_665 . ? Fe1 Fe1 N1 83.13(4) 9_665 11_565 ? N2 Fe1 N1 96.87(4) . 11_565 ? Fe1 Fe1 N1 83.13(4) 9_665 . ? N2 Fe1 N1 96.87(4) . . ? N1 Fe1 N1 89.180(10) 11_565 . ? Fe1 Fe1 N1 83.13(4) 9_665 9_665 ? N2 Fe1 N1 96.87(4) . 9_665 ? N1 Fe1 N1 89.180(10) 11_565 9_665 ? N1 Fe1 N1 166.26(8) . 9_665 ? Fe1 Fe1 N1 83.13(4) 9_665 3_655 ? N2 Fe1 N1 96.87(4) . 3_655 ? N1 Fe1 N1 166.26(8) 11_565 3_655 ? N1 Fe1 N1 89.180(10) . 3_655 ? N1 Fe1 N1 89.180(10) 9_665 3_655 ? Fe1 Fe1 N2 0.000(1) 9_665 9_665 ? N2 Fe1 N2 180.000(1) . 9_665 ? N1 Fe1 N2 83.13(4) 11_565 9_665 ? N1 Fe1 N2 83.13(4) . 9_665 ? N1 Fe1 N2 83.13(4) 9_665 9_665 ? N1 Fe1 N2 83.13(4) 3_655 9_665 ? C(A2 N1 C(A1 105.46(17) . . ? C(A2 N1 Fe1 126.83(14) . . ? C(A1 N1 Fe1 127.08(14) . . ? C(A2 N1 Fe1 126.83(14) . 9_665 ? C(A1 N1 Fe1 127.08(14) . 9_665 ? Fe1 N1 Fe1 13.74(8) . 9_665 ? O1 N2 O1 41.5(17) 3_655 2_665 ? O1 N2 O1 41.5(17) 3_655 . ? O1 N2 O1 60(3) 2_665 . ? O1 N2 O1 60(3) 3_655 4_565 ? O1 N2 O1 41.5(17) 2_665 4_565 ? O1 N2 O1 41.5(17) . 4_565 ? O1 N2 Fe1 149.9(13) 3_655 . ? O1 N2 Fe1 149.9(13) 2_665 . ? O1 N2 Fe1 149.9(13) . . ? O1 N2 Fe1 149.9(13) 4_565 . ? O1 N2 Fe1 149.9(13) 3_655 9_665 ? O1 N2 Fe1 149.9(13) 2_665 9_665 ? O1 N2 Fe1 149.9(13) . 9_665 ? O1 N2 Fe1 149.9(13) 4_565 9_665 ? Fe1 N2 Fe1 0.0 . 9_665 ? O1 O1 O1 90.00(3) 3_655 4_565 ? O1 O1 N2 69.3(9) 3_655 . ? O1 O1 N2 69.3(8) 4_565 . ? O1 O1 O1 45.00(3) 3_655 2_665 ? O1 O1 O1 45.000(12) 4_565 2_665 ? N2 O1 O1 59.9(13) . 2_665 ? N1 C(A1 C(M1 125.86(19) . 3_655 ? N1 C(A1 C(B1 110.3(2) . . ? C(M1 C(A1 C(B1 123.9(2) 3_655 . ? C(B2 C(B1 C(A1 107.2(2) . . ? C(B2 C(B1 H(B1 126.4 . . ? C(A1 C(B1 H(B1 126.4 . . ? C(B1 C(B2 C(A2 107.1(2) . . ? C(B1 C(B2 H(B2 126.4 . . ? C(A2 C(B2 H(B2 126.4 . . ? N1 C(A2 C(M1 126.4(2) . . ? N1 C(A2 C(B2 109.9(2) . . ? C(M1 C(A2 C(B2 123.7(2) . . ? C(A2 C(M1 C(A1 123.2(2) . 11_565 ? C(A2 C(M1 C10 118.6(2) . . ? C(A1 C(M1 C10 118.13(19) 11_565 . ? C11 C10 C11 118.6(2) 10 . ? C11 C10 C(M1 120.70(11) 10 . ? C11 C10 C(M1 120.70(11) . . ? C10 C11 C12 120.53(19) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C11 120.4(2) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C12 119.4(2) 10 . ? C12 C13 H13 120.3 10 . ? C12 C13 H13 120.3 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.287 _refine_diff_density_min -0.141 _refine_diff_density_rms 0.041 _chemical_compound_source synthesized #===END data_290_cryst_2 # local ID: ns44_290_0m _publ_requested_journal Inorg.Chem. _publ_contact_author_name 'Professor W. Robert Scheidt' _publ_contact_author_address ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; _publ_contact_author_email W.R.Scheidt.1@nd.edu _publ_contact_author_phone 1(574)6315939 _publ_contact_author_fax 1(574)6316652 loop_ _publ_author_name _publ_author_address 'Scheidt, W. Robert ' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Silvernail, Nathan J.' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Noll, Bruce C.' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Olmstead, Marilyn M.' ;University of California at Davis Department of Chemistry One Shields Avenue Davis, CA 95616 ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common [Fe(TPP)(NO] _chemical_melting_point ? _chemical_formula_moiety 'C44 H28 Fe N5 O' _chemical_formula_sum 'C44 H28 Fe N5 O' _chemical_formula_weight 698.56 _chemical_compound_source synthesized loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Tetragonal' _symmetry_space_group_name_H-M 'I 4/m ' _symmetry_space_group_name_Hall '-I 4 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 13.4466(3) _cell_length_b 13.4466(3) _cell_length_c 9.7498(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1762.87(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7738 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 25.12 _exptl_crystal_description 'square bipyramid' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 722.6 _exptl_absorpt_coefficient_mu 0.470 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9090 _exptl_absorpt_correction_T_max 0.9792 _exptl_absorpt_process_details 'Blessing, R.H. ACTA Cryst. (1995) A51, 33-38' _exptl_crystal_recrystallization_method 'liquid diffusion (chloroform/methanol)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33834 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0090 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 28.23 _reflns_number_total 1155 _reflns_number_gt 973 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Platon (Spek, 2004)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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. The structures were solved by direct methods using SHELXS-97 and refined against F^2^ using SHELXL-97;subsequent difference Fourier syntheses led to the location of most of the remaining non-hydrogen atoms. For the structure refinement all data were used including negative intensities. All nonhydrogen atoms were refined anisotropically. Hydrogen atoms were idealized with the standard SHELXL-97 idealization methods. Hydrogen atoms were placed at calculated geometries and allowed to ride on the position of the parent atom. Hydrogen thermal parameters were set to 1.2\\times the equivalent isotropic U of the parent atom, 1.5\\times for methyl hydrogens. The program SADABS was applied for the absorption correction. The structure is a tetraphenyl porphyrin bound axially by a nitrosyl. ; _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^)+(0.0648P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0069(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1155 _refine_ls_number_parameters 83 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.1077 _refine_ls_wR_factor_gt 0.0996 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.5000 0.5000 0.02351(16) 0.0457(5) Uani 0.50 4 d SP . . N1 N 0.46314(11) 0.35716(12) 0.0000 0.0499(4) Uani 1 2 d S . . C(M1 C 0.28062(14) 0.37030(15) 0.0000 0.0522(4) Uani 1 2 d S . . C(A1 C 0.52642(15) 0.27656(14) 0.0000 0.0524(4) Uani 1 2 d S . . C(A2 C 0.36874(14) 0.31738(14) 0.0000 0.0527(4) Uani 1 2 d S . . C(B1 C 0.47062(16) 0.18593(15) 0.0000 0.0632(5) Uani 1 2 d S . . H(B1 H 0.4965 0.1218 0.0000 0.076 Uiso 1 2 calc SR . . C(B2 C 0.37407(16) 0.21065(15) 0.0000 0.0625(5) Uani 1 2 d S . . H(B2 H 0.3205 0.1669 0.0000 0.075 Uiso 1 2 calc SR . . C10 C 0.18473(14) 0.31364(14) 0.0000 0.0547(5) Uani 1 2 d S . . C11 C 0.13974(14) 0.28742(16) -0.12077(19) 0.0791(5) Uani 1 1 d . . . H11 H 0.1684 0.3058 -0.2038 0.095 Uiso 1 1 calc R . . C12 C 0.05158(14) 0.23357(17) -0.1201(2) 0.0877(6) Uani 1 1 d . . . H12 H 0.0218 0.2160 -0.2027 0.105 Uiso 1 1 calc R . . C13 C 0.00852(16) 0.20639(18) 0.0000 0.0755(7) Uani 1 2 d S . . H13 H -0.0500 0.1695 0.0000 0.091 Uiso 1 2 calc SR . . N2 N 0.5000 0.5000 0.2004(5) 0.0470(9) Uani 0.50 4 d SP . . O1 O 0.512(9) 0.4626(13) 0.2978(9) 0.10(2) Uani 0.13 1 d 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 Fe1 0.0421(2) 0.0421(2) 0.0530(13) 0.000 0.000 0.000 N1 0.0457(8) 0.0464(8) 0.0575(9) 0.000 0.000 -0.0007(6) C(M1 0.0473(9) 0.0529(10) 0.0564(10) 0.000 0.000 -0.0048(7) C(A1 0.0531(10) 0.0449(9) 0.0592(10) 0.000 0.000 0.0009(7) C(A2 0.0503(10) 0.0478(9) 0.0599(11) 0.000 0.000 -0.0050(7) C(B1 0.0591(11) 0.0448(10) 0.0858(14) 0.000 0.000 -0.0006(8) C(B2 0.0555(11) 0.0473(10) 0.0847(14) 0.000 0.000 -0.0059(8) C10 0.0448(9) 0.0505(10) 0.0688(12) 0.000 0.000 -0.0018(7) C11 0.0688(10) 0.0979(13) 0.0706(10) 0.0022(9) -0.0051(8) -0.0238(9) C12 0.0678(10) 0.0978(14) 0.0975(14) -0.0039(11) -0.0207(10) -0.0216(9) C13 0.0447(10) 0.0603(12) 0.121(2) 0.000 0.000 -0.0060(9) N2 0.0422(12) 0.0422(12) 0.057(3) 0.000 0.000 0.000 O1 0.17(6) 0.071(6) 0.062(4) 0.022(9) -0.031(17) -0.03(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 1.725(5) . ? Fe1 N1 1.9968(16) . ? Fe1 N2 2.183(5) 9_665 ? N1 C(A2 1.378(2) . ? N1 C(A1 1.378(2) . ? N1 Fe1 1.9969(16) 9_665 ? C(M1 C(A2 1.382(3) . ? C(M1 C(A1 1.390(3) 11_565 ? C(M1 C10 1.498(3) . ? C(A1 C(M1 1.390(3) 3_655 ? C(A1 C(B1 1.431(3) . ? C(A2 C(B2 1.437(3) . ? C(B1 C(B2 1.340(3) . ? C(B1 H(B1 0.9300 . ? C(B2 H(B2 0.9300 . ? C10 C11 1.370(2) . ? C10 C11 1.370(2) 10 ? C11 C12 1.389(2) . ? C11 H11 0.9300 . ? C12 C13 1.356(3) . ? C12 H12 0.9300 . ? C13 C12 1.356(3) 10 ? C13 H13 0.9300 . ? N2 O1 1.09(3) . ? N2 Fe1 2.183(5) 9_665 ? 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 Fe1 Fe1 N2 179.997(1) 9_665 . ? Fe1 Fe1 N1 83.41(5) 9_665 11_565 ? N2 Fe1 N1 96.59(4) . 11_565 ? Fe1 Fe1 N1 83.41(4) 9_665 3_655 ? N2 Fe1 N1 96.59(4) . 3_655 ? N1 Fe1 N1 166.82(9) 11_565 3_655 ? Fe1 Fe1 N1 83.41(4) 9_665 9_665 ? N2 Fe1 N1 96.59(4) . 9_665 ? N1 Fe1 N1 89.244(10) 11_565 9_665 ? N1 Fe1 N1 89.244(10) 3_655 9_665 ? Fe1 Fe1 N1 83.41(4) 9_665 . ? N2 Fe1 N1 96.59(4) . . ? N1 Fe1 N1 89.246(10) 11_565 . ? N1 Fe1 N1 89.245(10) 3_655 . ? N1 Fe1 N1 166.82(9) 9_665 . ? N2 Fe1 N2 180.0 . 9_665 ? N1 Fe1 N2 83.41(4) 11_565 9_665 ? N1 Fe1 N2 83.41(4) 3_655 9_665 ? N1 Fe1 N2 83.41(4) 9_665 9_665 ? N1 Fe1 N2 83.41(4) . 9_665 ? C(A2 N1 C(A1 105.29(15) . . ? C(A2 N1 Fe1 127.03(13) . . ? C(A1 N1 Fe1 127.11(13) . . ? C(A2 N1 Fe1 127.03(13) . 9_665 ? C(A1 N1 Fe1 127.11(13) . 9_665 ? C(A2 C(M1 C(A1 123.24(18) . 11_565 ? C(A2 C(M1 C10 118.43(17) . . ? C(A1 C(M1 C10 118.33(17) 11_565 . ? N1 C(A1 C(M1 125.88(17) . 3_655 ? N1 C(A1 C(B1 110.24(18) . . ? C(M1 C(A1 C(B1 123.87(18) 3_655 . ? N1 C(A2 C(M1 126.17(17) . . ? N1 C(A2 C(B2 109.98(18) . . ? C(M1 C(A2 C(B2 123.85(19) . . ? C(B2 C(B1 C(A1 107.26(18) . . ? C(B2 C(B1 H(B1 126.4 . . ? C(A1 C(B1 H(B1 126.4 . . ? C(B1 C(B2 C(A2 107.22(18) . . ? C(B1 C(B2 H(B2 126.4 . . ? C(A2 C(B2 H(B2 126.4 . . ? C11 C10 C11 118.5(2) . 10 ? C11 C10 C(M1 120.74(10) . . ? C11 C10 C(M1 120.74(10) 10 . ? C10 C11 C12 120.45(18) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C13 C12 C11 120.60(19) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C12 119.4(2) 10 . ? C12 C13 H13 120.3 10 . ? C12 C13 H13 120.3 . . ? O1 N2 O1 58(4) 4_565 3_655 ? O1 N2 O1 58(4) . 2_665 ? O1 N2 Fe1 151(2) . . ? O1 N2 Fe1 151(2) 4_565 . ? O1 N2 Fe1 151(2) 3_655 . ? O1 N2 Fe1 151(2) 2_665 . ? O1 N2 Fe1 151(2) . 9_665 ? O1 N2 Fe1 151(2) 4_565 9_665 ? O1 N2 Fe1 151(2) 3_655 9_665 ? O1 N2 Fe1 151(2) 2_665 9_665 ? O1 O1 N2 69.9(15) 4_565 . ? O1 O1 N2 69.9(14) 3_655 . ? O1 O1 N2 61(2) 2_665 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.23 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.220 _refine_diff_density_min -0.193 _refine_diff_density_rms 0.037 #===END data_293_cryst_1 #local ID: mo293 _publ_requested_journal Inorg.Chem. _publ_contact_author_name 'Professor W. Robert Scheidt' _publ_contact_author_address ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; _publ_contact_author_email W.R.Scheidt.1@nd.edu _publ_contact_author_phone 1(574)6315939 _publ_contact_author_fax 1(574)6316652 loop_ _publ_author_name _publ_author_address 'Scheidt, W. Robert ' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Silvernail, Nathan J.' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Noll, Bruce C.' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Olmstead, Marilyn M.' ;University of California at Davis Department of Chemistry One Shields Avenue Davis, CA 95616 ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common [Fe(TPP)(NO] _chemical_melting_point ? _chemical_formula_moiety 'C44 H28 Fe N5 O' _chemical_formula_sum 'C44 H28 Fe N5 O' _chemical_formula_weight 698.560 _chemical_compound_source synthesized loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' .3463 .8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Tetragonal' _symmetry_space_group_name_H-M 'I 4/m ' _symmetry_space_group_name_Hall '-I 4 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 13.4748(12) _cell_length_b 13.4748(12) _cell_length_c 9.7686(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1773.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'square bipyramid' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 722.6 _exptl_absorpt_coefficient_mu 0.467 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9082 _exptl_absorpt_correction_T_max 0.9636 _exptl_absorpt_process_details 'Blessing, R.H. ACTA Cryst. (1995) A51, 33-38' _exptl_crystal_recrystallization_method 'liquid diffusion (chloroform/methanol)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9839 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0151 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1081 _reflns_number_gt 842 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Platon (Spek, 2004)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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. The structures were solved by direct methods using SHELXS-97 and refined against F^2^ using SHELXL-97;subsequent difference Fourier syntheses led to the location of most of the remaining non-hydrogen atoms. For the structure refinement all data were used including negative intensities. All nonhydrogen atoms were refined anisotropically. Hydrogen atoms were idealized with the standard SHELXL-97 idealization methods. Hydrogen atoms were placed at calculated geometries and allowed to ride on the position of the parent atom. Hydrogen thermal parameters were set to 1.2\\times the equivalent isotropic U of the parent atom, 1.5\\times for methyl hydrogens. The program SADABS was applied for the absorption correction. The structure is a tetraphenyl porphyrin bound axially by a nitrosyl. ; _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^)+(0.0648P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1081 _refine_ls_number_parameters 82 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.1069 _refine_ls_wR_factor_gt 0.0989 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.5000 0.5000 0.0235(3) 0.0542(7) Uani 0.50 4 d SP . . N1 N 0.35716(13) 0.46326(12) 0.0000 0.0573(4) Uani 1 2 d S . . C(M1 C 0.37029(16) 0.28062(15) 0.0000 0.0596(5) Uani 1 2 d S . . C(A1 C 0.27646(15) 0.52653(16) 0.0000 0.0609(5) Uani 1 2 d S . . C(A2 C 0.31742(15) 0.36876(16) 0.0000 0.0603(5) Uani 1 2 d S . . C(B1 C 0.18617(17) 0.47046(18) 0.0000 0.0716(6) Uani 1 2 d S . . H(B1 H 0.1221 0.4962 0.0000 0.086 Uiso 1 2 calc SR . . C(B2 C 0.21081(17) 0.37432(18) 0.0000 0.0711(6) Uani 1 2 d S . . H(B2 H 0.1671 0.3209 0.0000 0.085 Uiso 1 2 calc SR . . C10 C 0.31374(16) 0.18469(16) 0.0000 0.0627(5) Uani 1 2 d S . . C11 C 0.28741(17) 0.13999(15) 0.1203(2) 0.0872(6) Uani 1 1 d . . . H11 H 0.3055 0.1688 0.2031 0.105 Uiso 1 1 calc R . . C12 C 0.23382(18) 0.05178(15) 0.1197(3) 0.0956(7) Uani 1 1 d . . . H12 H 0.2165 0.0220 0.2022 0.115 Uiso 1 1 calc R . . C13 C 0.2067(2) 0.00887(18) 0.0000 0.0845(8) Uani 1 2 d S . . H13 H 0.1697 -0.0495 0.0000 0.101 Uiso 1 2 calc SR . . N2 N 0.5000 0.5000 0.1995(6) 0.0568(11) Uani 0.50 4 d SP . . O1 O 0.472(4) 0.469(4) 0.2972(10) 0.090(7) Uani 0.13 1 d 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 Fe1 0.0475(3) 0.0475(3) 0.068(2) 0.000 0.000 0.000 N1 0.0521(9) 0.0511(9) 0.0688(11) 0.000 0.000 -0.0002(7) C(M1 0.0586(11) 0.0541(11) 0.0661(12) 0.000 0.000 -0.0053(9) C(A1 0.0497(11) 0.0601(12) 0.0728(14) 0.000 0.000 0.0017(8) C(A2 0.0538(11) 0.0555(11) 0.0717(13) 0.000 0.000 -0.0049(9) C(B1 0.0508(11) 0.0660(13) 0.0978(17) 0.000 0.000 -0.0006(9) C(B2 0.0529(11) 0.0614(13) 0.0991(17) 0.000 0.000 -0.0067(9) C10 0.0569(11) 0.0509(11) 0.0803(15) 0.000 0.000 -0.0015(8) C11 0.1044(14) 0.0754(11) 0.0818(12) 0.0060(10) -0.0015(11) -0.0238(10) C12 0.1048(15) 0.0740(12) 0.1081(17) 0.0216(11) 0.0035(12) -0.0227(10) C13 0.0670(14) 0.0514(12) 0.135(3) 0.000 0.000 -0.0063(10) N2 0.0496(15) 0.0496(15) 0.071(3) 0.000 0.000 0.000 O1 0.080(17) 0.11(3) 0.080(5) 0.025(12) 0.003(9) 0.000(5) _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 Fe1 Fe1 0.459(5) 9_665 ? Fe1 N2 1.720(6) . ? Fe1 N1 2.0005(17) 9_665 ? Fe1 N2 2.179(7) 9_665 ? N1 C(A2 1.381(3) . ? N1 C(A1 1.382(3) . ? N1 Fe1 2.0005(17) 9_665 ? C(M1 C(A2 1.385(3) . ? C(M1 C(A1 1.391(3) 3_655 ? C(M1 C10 1.500(3) . ? C(A1 C(M1 1.391(3) 11_565 ? C(A1 C(B1 1.432(3) . ? C(A2 C(B2 1.438(3) . ? C(B1 C(B2 1.337(3) . ? C(B1 H(B1 0.9300 . ? C(B2 H(B2 0.9300 . ? C10 C11 1.367(2) 10 ? C10 C11 1.367(2) . ? C11 C12 1.391(3) . ? C11 H11 0.9300 . ? C12 C13 1.355(3) . ? C12 H12 0.9300 . ? C13 C12 1.355(3) 10 ? C13 H13 0.9300 . ? N2 O1 1.107(11) . ? N2 Fe1 2.179(7) 9_665 ? O1 O1 0.795(19) 4_565 ? 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 Fe1 Fe1 N2 179.999(2) 9_665 . ? Fe1 Fe1 N1 83.42(8) 9_665 . ? N2 Fe1 N1 96.58(8) . . ? Fe1 Fe1 N1 83.42(8) 9_665 3_655 ? N2 Fe1 N1 96.58(8) . 3_655 ? N1 Fe1 N1 89.247(18) . 3_655 ? Fe1 Fe1 N1 83.42(8) 9_665 11_565 ? N2 Fe1 N1 96.58(8) . 11_565 ? N1 Fe1 N1 89.248(18) . 11_565 ? N1 Fe1 N1 166.84(16) 3_655 11_565 ? Fe1 Fe1 N1 83.42(8) 9_665 9_665 ? N2 Fe1 N1 96.58(8) . 9_665 ? N1 Fe1 N1 166.84(16) . 9_665 ? N1 Fe1 N1 89.247(18) 3_655 9_665 ? N1 Fe1 N1 89.247(18) 11_565 9_665 ? Fe1 Fe1 N2 0.001(1) 9_665 9_665 ? N2 Fe1 N2 180.0 . 9_665 ? N1 Fe1 N2 83.42(8) . 9_665 ? N1 Fe1 N2 83.42(8) 3_655 9_665 ? N1 Fe1 N2 83.42(8) 11_565 9_665 ? N1 Fe1 N2 83.42(8) 9_665 9_665 ? C(A2 N1 C(A1 105.29(17) . . ? C(A2 N1 Fe1 126.95(14) . . ? C(A1 N1 Fe1 127.19(14) . . ? C(A2 N1 Fe1 126.95(14) . 9_665 ? C(A1 N1 Fe1 127.19(14) . 9_665 ? C(A2 C(M1 C(A1 123.3(2) . 3_655 ? C(A2 C(M1 C10 118.53(19) . . ? C(A1 C(M1 C10 118.21(19) 3_655 . ? N1 C(A1 C(M1 125.79(19) . 11_565 ? N1 C(A1 C(B1 110.07(19) . . ? C(M1 C(A1 C(B1 124.1(2) 11_565 . ? N1 C(A2 C(M1 126.24(19) . . ? N1 C(A2 C(B2 109.83(19) . . ? C(M1 C(A2 C(B2 123.9(2) . . ? C(B2 C(B1 C(A1 107.46(19) . . ? C(B2 C(B1 H(B1 126.3 . . ? C(A1 C(B1 H(B1 126.3 . . ? C(B1 C(B2 C(A2 107.36(19) . . ? C(B1 C(B2 H(B2 126.3 . . ? C(A2 C(B2 H(B2 126.3 . . ? C11 C10 C11 118.5(2) 10 . ? C11 C10 C(M1 120.76(11) 10 . ? C11 C10 C(M1 120.76(11) . . ? C10 C11 C12 120.5(2) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C11 120.6(2) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C12 119.3(2) . 10 ? C12 C13 H13 120.3 . . ? C12 C13 H13 120.3 10 . ? O1 N2 O1 61.0(14) 4_565 3_655 ? O1 N2 O1 61.0(14) . 2_665 ? O1 N2 Fe1 149.5(7) . . ? O1 N2 Fe1 149.5(7) 4_565 . ? O1 N2 Fe1 149.5(7) 3_655 . ? O1 N2 Fe1 149.5(7) 2_665 . ? O1 N2 Fe1 149.5(7) . 9_665 ? O1 N2 Fe1 149.5(7) 4_565 9_665 ? O1 N2 Fe1 149.5(7) 3_655 9_665 ? O1 N2 Fe1 149.5(7) 2_665 9_665 ? O1 O1 O1 90.01(2) 4_565 3_655 ? O1 O1 N2 69.0(4) 4_565 . ? O1 O1 N2 69.0(5) 3_655 . ? O1 O1 O1 45.003(8) 4_565 2_665 ? O1 O1 O1 45.003(14) 3_655 2_665 ? N2 O1 O1 59.5(7) . 2_665 ? _diffrn_measured_fraction_theta_max .997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full .997 _refine_diff_density_max .193 _refine_diff_density_min -.276 _refine_diff_density_rms .029 #===END data_293_cryst_2 #local ID: ns44i4m _publ_requested_journal Inorg.Chem. _publ_contact_author_name 'Professor W. Robert Scheidt' _publ_contact_author_address ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; _publ_contact_author_email W.R.Scheidt.1@nd.edu _publ_contact_author_phone 1(574)6315939 _publ_contact_author_fax 1(574)6316652 loop_ _publ_author_name _publ_author_address 'Scheidt, W. Robert ' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Silvernail, Nathan J.' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Noll, Bruce C.' ;University of Notre Dame Department of Chemistry and Biochemistry 251 Nieuwland Science Hall Notre Dame, IN 46556-5670 ; 'Olmstead, Marilyn M.' ;University of California at Davis Department of Chemistry One Shields Avenue Davis, CA 95616 ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common [Fe(TPP)(NO] _chemical_melting_point ? _chemical_formula_moiety 'C44 H28 Fe N5 O1' _chemical_formula_sum 'C44 H28 Fe N5 O1.04' _chemical_formula_weight 698.56 _chemical_compound_source synthesized loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Tetragonal' _symmetry_space_group_name_H-M 'I 4/m ' _symmetry_space_group_name_Hall '-I 4 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x, z' '-x, -y, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x, -y, -z' 'y, -x, -z' 'x, y, -z' '-y, x, -z' '-x+1/2, -y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 13.4502(3) _cell_length_b 13.4502(3) _cell_length_c 9.7533(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1764.45(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3281 _cell_measurement_theta_min 2.1413 _cell_measurement_theta_max 23.3164 _exptl_crystal_description 'square bipyramid' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 722.6 _exptl_absorpt_coefficient_mu 0.470 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8491 _exptl_absorpt_correction_T_max 0.9320 _exptl_absorpt_process_details 'Blessing, R.H. ACTA Cryst. (1995) A51, 33-38' _exptl_crystal_recrystallization_method 'liquid diffusion (chloroform/methanol)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9687 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0173 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.85 _reflns_number_total 1108 _reflns_number_gt 881 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2/SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2004; Sheldrick, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Platon (Spek, 2004)' _computing_publication_material 'XCIF (Sheldrick, 2001)' _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. The structures were solved by direct methods using SHELXS-97 and refined against F^2^ using SHELXL-97;subsequent difference Fourier syntheses led to the location of most of the remaining non-hydrogen atoms. For the structure refinement all data were used including negative intensities. All nonhydrogen atoms were refined anisotropically. Hydrogen atoms were idealized with the standard SHELXL-97 idealization methods. Hydrogen atoms were placed at calculated geometries and allowed to ride on the position of the parent atom. Hydrogen thermal parameters were set to 1.2\\times the equivalent isotropic U of the parent atom, 1.5\\times for methyl hydrogens. The program SADABS was applied for the absorption correction. The structure is a tetraphenyl porphyrin bound axially by a nitrosyl. ; _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^)+(0.0648P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0109(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1108 _refine_ls_number_parameters 83 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.1115 _refine_ls_wR_factor_gt 0.1024 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.5000 0.5000 0.0231(3) 0.0481(7) Uani 0.50 4 d SP . . N1 N 0.35723(13) 0.46306(13) 0.0000 0.0510(4) Uani 1 2 d S . . C(M1 C 0.37032(16) 0.28065(15) 0.0000 0.0532(5) Uani 1 2 d S . . C(A1 C 0.27654(15) 0.52632(17) 0.0000 0.0540(5) Uani 1 2 d S . . C(A2 C 0.31748(15) 0.36872(16) 0.0000 0.0538(5) Uani 1 2 d S . . C(B1 C 0.18608(17) 0.47042(18) 0.0000 0.0648(6) Uani 1 2 d S . . H(B1 H 0.1219 0.4963 0.0000 0.078 Uiso 1 2 calc SR . . C(B2 C 0.21075(17) 0.37414(18) 0.0000 0.0640(6) Uani 1 2 d S . . H(B2 H 0.1670 0.3206 0.0000 0.077 Uiso 1 2 calc SR . . C10 C 0.31372(16) 0.18460(16) 0.0000 0.0559(5) Uani 1 2 d S . . C11 C 0.28751(17) 0.13973(15) 0.1203(2) 0.0802(6) Uani 1 1 d . . . H11 H 0.3058 0.1685 0.2033 0.096 Uiso 1 1 calc R . . C12 C 0.23390(19) 0.05176(16) 0.1200(3) 0.0894(7) Uani 1 1 d . . . H12 H 0.2165 0.0220 0.2027 0.107 Uiso 1 1 calc R . . C13 C 0.2065(2) 0.00859(18) 0.0000 0.0778(8) Uani 1 2 d S . . H13 H 0.1694 -0.0498 0.0000 0.093 Uiso 1 2 calc SR . . N2 N 0.5000 0.5000 0.1998(6) 0.0481(11) Uani 0.50 4 d SP . . O1 O 0.478(5) 0.464(3) 0.2972(10) 0.084(6) Uani 0.13 1 d 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 Fe1 0.0433(3) 0.0433(3) 0.058(2) 0.000 0.000 0.000 N1 0.0473(9) 0.0467(9) 0.0591(11) 0.000 0.000 -0.0006(7) C(M1 0.0542(11) 0.0485(11) 0.0568(12) 0.000 0.000 -0.0053(9) C(A1 0.0465(10) 0.0550(11) 0.0604(13) 0.000 0.000 0.0007(9) C(A2 0.0475(10) 0.0515(11) 0.0624(13) 0.000 0.000 -0.0052(9) C(B1 0.0457(11) 0.0615(13) 0.0871(17) 0.000 0.000 -0.0006(9) C(B2 0.0486(11) 0.0563(12) 0.0872(17) 0.000 0.000 -0.0056(9) C10 0.0512(11) 0.0464(10) 0.0700(14) 0.000 0.000 -0.0014(8) C11 0.0982(14) 0.0701(11) 0.0722(12) 0.0051(9) -0.0032(10) -0.0238(10) C12 0.1003(16) 0.0699(12) 0.0982(16) 0.0208(11) 0.0038(12) -0.0216(11) C13 0.0610(14) 0.0453(12) 0.127(3) 0.000 0.000 -0.0055(10) N2 0.0427(14) 0.0427(14) 0.059(3) 0.000 0.000 0.000 O1 0.10(3) 0.079(16) 0.070(5) 0.015(7) 0.021(13) 0.005(11) _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 Fe1 Fe1 0.450(5) 9_665 ? Fe1 N2 1.724(6) . ? Fe1 N1 1.9962(17) 10_565 ? Fe1 N1 1.9962(17) 2_655 ? Fe1 N1 1.9963(17) . ? Fe1 N1 1.9963(17) 9_665 ? Fe1 N2 2.174(6) 9_665 ? N1 C(A2 1.377(3) . ? N1 C(A1 1.379(3) . ? N1 Fe1 1.9963(17) 9_665 ? C(M1 C(A2 1.381(3) . ? C(M1 C(A1 1.391(3) 2_655 ? C(M1 C10 1.499(3) . ? C(A1 C(M1 1.391(3) 10_565 ? C(A1 C(B1 1.430(3) . ? C(A2 C(B2 1.437(3) . ? C(B1 C(B2 1.337(3) . ? C(B1 H(B1 0.9300 . ? C(B2 H(B2 0.9300 . ? C10 C11 1.366(2) 11 ? C10 C11 1.366(2) . ? C11 C12 1.386(3) . ? C11 H11 0.9300 . ? C12 C13 1.357(3) . ? C12 H12 0.9300 . ? C13 C12 1.357(3) 11 ? C13 H13 0.9300 . ? N2 O1 1.108(11) 2_655 ? N2 O1 1.108(11) 4_565 ? N2 O1 1.108(11) 3_665 ? N2 O1 1.108(11) . ? N2 Fe1 2.174(6) 9_665 ? 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 Fe1 Fe1 N2 179.995(2) 9_665 . ? Fe1 Fe1 N1 83.53(7) 9_665 10_565 ? N2 Fe1 N1 96.47(7) . 10_565 ? Fe1 Fe1 N1 83.52(7) 9_665 2_655 ? N2 Fe1 N1 96.47(7) . 2_655 ? N1 Fe1 N1 167.05(15) 10_565 2_655 ? Fe1 Fe1 N1 83.53(8) 9_665 . ? N2 Fe1 N1 96.47(7) . . ? N1 Fe1 N1 89.272(17) 10_565 . ? N1 Fe1 N1 89.271(17) 2_655 . ? Fe1 Fe1 N1 83.52(7) 9_665 9_665 ? N2 Fe1 N1 96.47(7) . 9_665 ? N1 Fe1 N1 89.271(17) 10_565 9_665 ? N1 Fe1 N1 89.273(17) 2_655 9_665 ? N1 Fe1 N1 167.05(15) . 9_665 ? Fe1 Fe1 N2 0.004(2) 9_665 9_665 ? N2 Fe1 N2 180.0 . 9_665 ? N1 Fe1 N2 83.53(7) 10_565 9_665 ? N1 Fe1 N2 83.53(7) 2_655 9_665 ? N1 Fe1 N2 83.53(7) . 9_665 ? N1 Fe1 N2 83.53(7) 9_665 9_665 ? C(A2 N1 C(A1 105.25(17) . . ? C(A2 N1 Fe1 127.08(14) . . ? C(A1 N1 Fe1 127.12(14) . . ? C(A2 N1 Fe1 127.08(14) . 9_665 ? C(A1 N1 Fe1 127.12(14) . 9_665 ? C(A2 C(M1 C(A1 123.2(2) . 2_655 ? C(A2 C(M1 C10 118.53(19) . . ? C(A1 C(M1 C10 118.23(19) 2_655 . ? N1 C(A1 C(M1 125.82(19) . 10_565 ? N1 C(A1 C(B1 110.2(2) . . ? C(M1 C(A1 C(B1 124.0(2) 10_565 . ? N1 C(A2 C(M1 126.19(19) . . ? N1 C(A2 C(B2 109.94(19) . . ? C(M1 C(A2 C(B2 123.9(2) . . ? C(B2 C(B1 C(A1 107.34(19) . . ? C(B2 C(B1 H(B1 126.3 . . ? C(A1 C(B1 H(B1 126.3 . . ? C(B1 C(B2 C(A2 107.3(2) . . ? C(B1 C(B2 H(B2 126.4 . . ? C(A2 C(B2 H(B2 126.4 . . ? C11 C10 C11 118.5(2) 11 . ? C11 C10 C(M1 120.77(11) 11 . ? C11 C10 C(M1 120.77(11) . . ? C10 C11 C12 120.6(2) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C11 120.6(2) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C12 119.1(2) . 11 ? C12 C13 H13 120.4 . . ? C12 C13 H13 120.4 11 . ? O1 N2 O1 62.1(13) 2_655 4_565 ? O1 N2 O1 62.1(13) 3_665 . ? O1 N2 Fe1 149.0(6) 2_655 . ? O1 N2 Fe1 149.0(6) 4_565 . ? O1 N2 Fe1 149.0(7) 3_665 . ? O1 N2 Fe1 149.0(6) . . ? O1 N2 Fe1 149.0(6) 2_655 9_665 ? O1 N2 Fe1 149.0(6) 4_565 9_665 ? O1 N2 Fe1 149.0(7) 3_665 9_665 ? O1 N2 Fe1 149.0(6) . 9_665 ? O1 O1 O1 90.00(2) 4_565 2_655 ? O1 O1 N2 68.6(4) 4_565 . ? O1 O1 N2 68.6(4) 2_655 . ? N2 O1 O1 59.0(6) . 3_665 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.85 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.236 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.040 #===END