############################################################################## # # # This CIF contains the data in a paper accepted for publication in # # Acta Crystallographica Section E. It conforms to the requirements of # # Notes for Authors for Acta Crystallographica Section E, and has been # # peer reviewed under the auspices of the IUCr Commission on Journals. # # # # Full details of the Crystallographic Information File format # # are given in the paper "The Crystallographic Information File (CIF): # # a New Standard Archive File for Crystallography" by S. R. Hall, F. H. # # Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. # # # # The current version of the core CIF dictionary is obtainable from # # ftp://ftp.iucr.org/pub/cif_core.dic. # # # # Software is freely available for graphical display of the structure(s) # # in this CIF. For information consult the CIF software page # # http://www.iucr.org/resources/cif/software. # # # # This file may be used for bona fide research purposes within the # # scientific community so long as proper attribution is given to the journal # # article from which it was obtained. # # # ############################################################################## data_I _audit_creation_method SHELXL-2013 _journal_date_recd_electronic 2015-12-02 _journal_date_accepted 2015-12-16 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2016 _journal_volume 72 _journal_issue 1 _journal_page_first 92 _journal_page_last 95 _journal_paper_category GM _journal_paper_doi 10.1107/S2056989015024214 _journal_coeditor_code WM5252 _publ_contact_author_name 'Heinrich Lang' _publ_contact_author_address ; Technische Universit\"at Chemnitz Fakult\"at f\"ur Naturwissenschaften Institut f\"ur Chemie Anorganische Chemie D-09107 Chemnitz Germany ; _publ_contact_author_email 'heinrich.lang@chemie.tu-chemnitz.de' _publ_contact_author_fax '+49 (0)371-531-21210' _publ_contact_author_phone '+49 (0)371-531-21219' _publ_section_title ; Crystal structure of 3-ferrocenyl-1-phenyl-1H-pyrrole [Fe(\h^5^-C~5~H~4~^c^C~4~H~3~NPh)(\h^5^-C~5~H~5~)] ; loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Pfaff, Ulrike' . ; Technische Universit\"at Chemnitz Fakult\"at f\"ur Naturwissenschaften Institut f\"ur Chemie Anorganische Chemie D-09107 Chemnitz Germany ; 'Korb, Marcus' . ; Technische Universit\"at Chemnitz Fakult\"at f\"ur Naturwissenschaften Institut f\"ur Chemie Anorganische Chemie D-09107 Chemnitz Germany ; 'Lang, Heinrich' . ; Technische Universit\"at Chemnitz Fakult\"at f\"ur Naturwissenschaften Institut f\"ur Chemie Anorganische Chemie D-09107 Chemnitz Germany ; _publ_section_synopsis ; The molecular structure of 3-ferrocenyl-N-phenylpyrrole, [Fe(\h^5^-C~5~H~4~^c^C~4~H~3~NPh)(\h^5^-C~5~H~5~)] has an L-type shape, with the N-phenylpyrrole moiety fused with the cyclapentadienyl ring being approximately coplanar. ; _chemical_name_systematic ; 3-Ferrocenyl-1-phenyl-1H-pyrrole ; _chemical_name_common ? _chemical_formula_moiety 'C20 H17 Fe N' _chemical_formula_sum 'C20 H17 Fe N' _chemical_formula_iupac '[Fe (C5 H5) (C15 H12 N)]' _chemical_formula_weight 327.19 _chemical_melting_point ? _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.9173(8) _cell_length_b 5.8011(6) _cell_length_c 23.085(2) _cell_angle_alpha 90 _cell_angle_beta 93.160(7) _cell_angle_gamma 90 _cell_volume 1459.8(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 1838 _cell_measurement_theta_min 3.962 _cell_measurement_theta_max 28.301 _cell_measurement_temperature 110(2) _exptl_crystal_description 'plate' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 1.028 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (CrysAlis RED; Oxford Diffraction, 2006) ; _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_T_min 0.19226 _exptl_absorpt_correction_T_max 1.00000 _exptl_special_details ? _diffrn_ambient_temperature 110(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Gemini S' _diffrn_measurement_method '/w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6054 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_theta_min 3.158 _diffrn_reflns_theta_max 25.997 _diffrn_reflns_theta_full 26.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 25 _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time 10 _diffrn_standards_decay_% 0 _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. ; _reflns_number_total 2858 _reflns_number_gt 2198 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0668 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_gt 0.1005 _refine_ls_wR_factor_ref 0.1102 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_number_reflns 2858 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0503P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.502 _refine_diff_density_min -0.751 _refine_ls_extinction_method none _refine_ls_extinction_coef . 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ; CrysAlis CCD (Oxford Diffraction, 2006) ; _computing_cell_refinement ; CrysAlis RED (Oxford Diffraction, 2006) ; _computing_data_reduction ; CrysAlis RED (Oxford Diffraction, 2006) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick, 2015) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) and SHELXTL (Sheldrick, 2008) ; _computing_publication_material ; WinGX (Farrugia, 2012) and publCIF (Westrip, 2010) ; loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C C1 0.5499(3) 0.1196(5) 0.24155(12) 0.0173(6) Uani d 1 . . H H1 0.5176 0.2615 0.2298 0.021 Uiso calc 1 . . C C2 0.5435(3) 0.0236(5) 0.29591(12) 0.0165(6) Uani d 1 . . C C3 0.6066(3) -0.1911(5) 0.29421(13) 0.0201(7) Uani d 1 . . H H3 0.6183 -0.2940 0.3249 0.024 Uiso calc 1 . . C C4 0.6466(3) -0.2195(5) 0.24043(12) 0.0195(7) Uani d 1 . . H H4 0.6901 -0.3461 0.2278 0.023 Uiso calc 1 . . C C5 0.4917(3) 0.1248(5) 0.34651(13) 0.0165(6) Uani d 1 . . C C6 0.4859(3) 0.0136(5) 0.40182(12) 0.0186(7) Uani d 1 . . H H6 0.5099 -0.1371 0.4103 0.022 Uiso calc 1 . . C C7 0.4375(3) 0.1710(5) 0.44135(13) 0.0217(7) Uani d 1 . . H H7 0.4251 0.1424 0.4802 0.026 Uiso calc 1 . . C C8 0.4112(3) 0.3799(5) 0.41138(13) 0.0203(7) Uani d 1 . . H H8 0.3783 0.5122 0.4272 0.024 Uiso calc 1 . . C C9 0.4436(3) 0.3527(5) 0.35336(13) 0.0195(7) Uani d 1 . . H H9 0.4352 0.4640 0.3244 0.023 Uiso calc 1 . . C C10 0.2029(3) -0.0235(6) 0.30801(14) 0.0249(7) Uani d 1 . . H H10 0.2257 -0.0582 0.2708 0.030 Uiso calc 1 . . C C11 0.2121(3) -0.1733(5) 0.35651(15) 0.0281(8) Uani d 1 . . H H11 0.2417 -0.3236 0.3566 0.034 Uiso calc 1 . . C C12 0.1686(3) -0.0549(6) 0.40452(15) 0.0302(8) Uani d 1 . . H H12 0.1649 -0.1128 0.4419 0.036 Uiso calc 1 . . C C13 0.1314(3) 0.1681(5) 0.38567(14) 0.0258(8) Uani d 1 . . H H13 0.0985 0.2822 0.4085 0.031 Uiso calc 1 . . C C14 0.1533(3) 0.1862(5) 0.32592(13) 0.0241(7) Uani d 1 . . H H14 0.1375 0.3148 0.3026 0.029 Uiso calc 1 . . C C15 0.6417(3) 0.0084(5) 0.14879(13) 0.0183(7) Uani d 1 . . C C16 0.6046(3) 0.2088(5) 0.12047(13) 0.0259(7) Uani d 1 . . H H16 0.5595 0.3184 0.1396 0.031 Uiso calc 1 . . C C17 0.6347(3) 0.2466(6) 0.06357(14) 0.0332(8) Uani d 1 . . H H17 0.6088 0.3811 0.0447 0.040 Uiso calc 1 . . C C18 0.7025(3) 0.0869(6) 0.03478(15) 0.0315(8) Uani d 1 . . H H18 0.7229 0.1129 -0.0033 0.038 Uiso calc 1 . . C C19 0.7393(3) -0.1117(6) 0.06342(14) 0.0308(8) Uani d 1 . . H H19 0.7850 -0.2204 0.0443 0.037 Uiso calc 1 . . C C20 0.7101(3) -0.1529(5) 0.11972(13) 0.0254(8) Uani d 1 . . H H20 0.7359 -0.2881 0.1383 0.030 Uiso calc 1 . . N N1 0.6125(2) -0.0310(4) 0.20734(10) 0.0172(5) Uani d 1 . . Fe Fe1 0.31350(4) 0.11585(7) 0.37338(2) 0.01626(16) Uani d 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C1 0.0098(15) 0.0181(14) 0.0240(17) 0.0015(13) 0.0006(12) -0.0006(12) C2 0.0070(14) 0.0192(15) 0.0232(16) -0.0028(12) -0.0017(12) 0.0033(12) C3 0.0102(15) 0.0227(15) 0.0271(17) -0.0025(13) -0.0020(13) 0.0043(13) C4 0.0098(15) 0.0177(14) 0.0306(17) 0.0029(13) -0.0015(13) 0.0014(13) C5 0.0051(14) 0.0218(15) 0.0227(16) -0.0020(12) 0.0006(12) 0.0030(13) C6 0.0096(15) 0.0242(16) 0.0216(16) -0.0006(13) -0.0035(12) 0.0042(13) C7 0.0140(16) 0.0309(17) 0.0196(16) -0.0016(14) -0.0042(13) -0.0010(13) C8 0.0142(16) 0.0216(15) 0.0246(16) -0.0006(13) -0.0026(13) -0.0019(13) C9 0.0098(15) 0.0222(16) 0.0267(17) -0.0023(13) 0.0016(13) 0.0042(13) C10 0.0094(16) 0.0397(19) 0.0251(17) -0.0013(15) -0.0034(13) -0.0053(15) C11 0.0120(16) 0.0218(16) 0.050(2) -0.0024(14) -0.0049(16) -0.0019(15) C12 0.0154(17) 0.045(2) 0.0299(19) -0.0096(16) -0.0031(14) 0.0086(16) C13 0.0083(15) 0.0350(19) 0.0342(19) -0.0024(14) 0.0040(14) -0.0093(15) C14 0.0115(16) 0.0283(16) 0.0319(18) -0.0019(14) -0.0049(14) 0.0060(14) C15 0.0052(14) 0.0260(16) 0.0236(16) -0.0037(13) -0.0008(12) -0.0020(13) C16 0.0182(17) 0.0286(17) 0.0312(18) 0.0062(15) 0.0040(14) 0.0016(15) C17 0.027(2) 0.041(2) 0.0320(19) 0.0071(17) 0.0014(16) 0.0096(17) C18 0.0201(18) 0.049(2) 0.0258(18) 0.0030(17) 0.0049(15) 0.0022(16) C19 0.0221(18) 0.040(2) 0.0308(19) 0.0060(17) 0.0055(15) -0.0011(16) C20 0.0193(18) 0.0292(18) 0.0274(18) 0.0049(14) 0.0001(14) 0.0019(14) N1 0.0068(12) 0.0208(12) 0.0237(14) 0.0003(11) -0.0009(10) 0.0003(11) Fe1 0.0085(2) 0.0199(2) 0.0202(3) -0.00065(19) -0.00110(17) 0.00174(18) _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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 C2 . 1.378(4) ? C1 N1 . 1.384(3) ? C1 H1 . 0.9300 ? C2 C3 . 1.425(4) ? C2 C5 . 1.449(4) ? C3 C4 . 1.349(4) ? C3 H3 . 0.9300 ? C4 N1 . 1.373(4) ? C4 H4 . 0.9300 ? C5 C9 . 1.435(4) ? C5 C6 . 1.435(4) ? C5 Fe1 . 2.075(3) ? C6 C7 . 1.414(4) ? C6 Fe1 . 2.046(3) ? C6 H6 . 0.9300 ? C7 C8 . 1.417(4) ? C7 Fe1 . 2.040(3) ? C7 H7 . 0.9300 ? C8 C9 . 1.413(4) ? C8 Fe1 . 2.038(3) ? C8 H8 . 0.9300 ? C9 Fe1 . 2.047(3) ? C9 H9 . 0.9300 ? C10 C14 . 1.403(4) ? C10 C11 . 1.417(4) ? C10 Fe1 . 2.047(3) ? C10 H10 . 0.9300 ? C11 C12 . 1.409(5) ? C11 Fe1 . 2.036(3) ? C11 H11 . 0.9300 ? C12 C13 . 1.417(4) ? C12 Fe1 . 2.032(3) ? C12 H12 . 0.9300 ? C13 C14 . 1.417(4) ? C13 Fe1 . 2.046(3) ? C13 H13 . 0.9300 ? C14 Fe1 . 2.053(3) ? C14 H14 . 0.9300 ? C15 C16 . 1.384(4) ? C15 C20 . 1.392(4) ? C15 N1 . 1.424(4) ? C16 C17 . 1.389(4) ? C16 H16 . 0.9300 ? C17 C18 . 1.379(4) ? C17 H17 . 0.9300 ? C18 C19 . 1.378(4) ? C18 H18 . 0.9300 ? C19 C20 . 1.376(4) ? C19 H19 . 0.9300 ? C20 H20 . 0.9300 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 C1 N1 . . 108.4(2) ? C2 C1 H1 . . 125.8 ? N1 C1 H1 . . 125.8 ? C1 C2 C3 . . 106.2(2) ? C1 C2 C5 . . 127.7(3) ? C3 C2 C5 . . 125.9(3) ? C4 C3 C2 . . 108.3(3) ? C4 C3 H3 . . 125.9 ? C2 C3 H3 . . 125.9 ? C3 C4 N1 . . 108.9(3) ? C3 C4 H4 . . 125.6 ? N1 C4 H4 . . 125.6 ? C9 C5 C6 . . 106.4(3) ? C9 C5 C2 . . 128.5(3) ? C6 C5 C2 . . 125.0(3) ? C9 C5 Fe1 . . 68.60(16) ? C6 C5 Fe1 . . 68.56(16) ? C2 C5 Fe1 . . 130.1(2) ? C7 C6 C5 . . 108.7(3) ? C7 C6 Fe1 . . 69.53(17) ? C5 C6 Fe1 . . 70.70(16) ? C7 C6 H6 . . 125.7 ? C5 C6 H6 . . 125.7 ? Fe1 C6 H6 . . 125.7 ? C6 C7 C8 . . 108.1(3) ? C6 C7 Fe1 . . 69.99(17) ? C8 C7 Fe1 . . 69.56(17) ? C6 C7 H7 . . 126.0 ? C8 C7 H7 . . 126.0 ? Fe1 C7 H7 . . 126.1 ? C9 C8 C7 . . 108.2(3) ? C9 C8 Fe1 . . 70.14(16) ? C7 C8 Fe1 . . 69.77(17) ? C9 C8 H8 . . 125.9 ? C7 C8 H8 . . 125.9 ? Fe1 C8 H8 . . 125.8 ? C8 C9 C5 . . 108.6(3) ? C8 C9 Fe1 . . 69.40(17) ? C5 C9 Fe1 . . 70.67(16) ? C8 C9 H9 . . 125.7 ? C5 C9 H9 . . 125.7 ? Fe1 C9 H9 . . 125.8 ? C14 C10 C11 . . 108.1(3) ? C14 C10 Fe1 . . 70.23(18) ? C11 C10 Fe1 . . 69.28(18) ? C14 C10 H10 . . 125.9 ? C11 C10 H10 . . 125.9 ? Fe1 C10 H10 . . 126.1 ? C12 C11 C10 . . 108.1(3) ? C12 C11 Fe1 . . 69.58(18) ? C10 C11 Fe1 . . 70.12(17) ? C12 C11 H11 . . 126.0 ? C10 C11 H11 . . 126.0 ? Fe1 C11 H11 . . 125.9 ? C11 C12 C13 . . 107.9(3) ? C11 C12 Fe1 . . 69.89(19) ? C13 C12 Fe1 . . 70.22(18) ? C11 C12 H12 . . 126.1 ? C13 C12 H12 . . 126.1 ? Fe1 C12 H12 . . 125.4 ? C14 C13 C12 . . 107.8(3) ? C14 C13 Fe1 . . 70.06(18) ? C12 C13 Fe1 . . 69.12(18) ? C14 C13 H13 . . 126.1 ? C12 C13 H13 . . 126.1 ? Fe1 C13 H13 . . 126.3 ? C10 C14 C13 . . 108.1(3) ? C10 C14 Fe1 . . 69.73(18) ? C13 C14 Fe1 . . 69.51(18) ? C10 C14 H14 . . 125.9 ? C13 C14 H14 . . 125.9 ? Fe1 C14 H14 . . 126.4 ? C16 C15 C20 . . 119.2(3) ? C16 C15 N1 . . 120.6(3) ? C20 C15 N1 . . 120.2(3) ? C15 C16 C17 . . 120.1(3) ? C15 C16 H16 . . 120.0 ? C17 C16 H16 . . 120.0 ? C18 C17 C16 . . 120.7(3) ? C18 C17 H17 . . 119.6 ? C16 C17 H17 . . 119.6 ? C19 C18 C17 . . 118.7(3) ? C19 C18 H18 . . 120.6 ? C17 C18 H18 . . 120.6 ? C20 C19 C18 . . 121.4(3) ? C20 C19 H19 . . 119.3 ? C18 C19 H19 . . 119.3 ? C19 C20 C15 . . 119.8(3) ? C19 C20 H20 . . 120.1 ? C15 C20 H20 . . 120.1 ? C4 N1 C1 . . 108.2(2) ? C4 N1 C15 . . 126.0(2) ? C1 N1 C15 . . 125.7(2) ? C12 Fe1 C11 . . 40.53(13) ? C12 Fe1 C8 . . 127.87(13) ? C11 Fe1 C8 . . 165.53(13) ? C12 Fe1 C7 . . 107.52(13) ? C11 Fe1 C7 . . 127.38(13) ? C8 Fe1 C7 . . 40.67(12) ? C12 Fe1 C13 . . 40.66(13) ? C11 Fe1 C13 . . 68.05(13) ? C8 Fe1 C13 . . 108.58(12) ? C7 Fe1 C13 . . 118.60(13) ? C12 Fe1 C6 . . 117.74(13) ? C11 Fe1 C6 . . 107.65(12) ? C8 Fe1 C6 . . 68.25(12) ? C7 Fe1 C6 . . 40.48(11) ? C13 Fe1 C6 . . 151.85(13) ? C12 Fe1 C10 . . 68.21(13) ? C11 Fe1 C10 . . 40.61(13) ? C8 Fe1 C10 . . 152.65(13) ? C7 Fe1 C10 . . 165.59(12) ? C13 Fe1 C10 . . 67.81(13) ? C6 Fe1 C10 . . 128.09(12) ? C12 Fe1 C9 . . 166.10(13) ? C11 Fe1 C9 . . 152.46(13) ? C8 Fe1 C9 . . 40.47(11) ? C7 Fe1 C9 . . 68.23(12) ? C13 Fe1 C9 . . 128.57(12) ? C6 Fe1 C9 . . 68.27(12) ? C10 Fe1 C9 . . 119.17(13) ? C12 Fe1 C14 . . 68.19(13) ? C11 Fe1 C14 . . 67.88(13) ? C8 Fe1 C14 . . 119.39(12) ? C7 Fe1 C14 . . 152.72(13) ? C13 Fe1 C14 . . 40.43(12) ? C6 Fe1 C14 . . 165.97(12) ? C10 Fe1 C14 . . 40.03(12) ? C9 Fe1 C14 . . 109.11(12) ? C12 Fe1 C5 . . 151.56(12) ? C11 Fe1 C5 . . 118.19(12) ? C8 Fe1 C5 . . 68.44(12) ? C7 Fe1 C5 . . 68.45(12) ? C13 Fe1 C5 . . 166.39(12) ? C6 Fe1 C5 . . 40.74(11) ? C10 Fe1 C5 . . 108.33(12) ? C9 Fe1 C5 . . 40.73(11) ? C14 Fe1 C5 . . 128.38(12) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag N1 C1 C2 C3 . . . . 0.9(3) ? N1 C1 C2 C5 . . . . 176.7(3) ? C1 C2 C3 C4 . . . . -0.8(3) ? C5 C2 C3 C4 . . . . -176.7(3) ? C2 C3 C4 N1 . . . . 0.4(3) ? C1 C2 C5 C9 . . . . -5.1(5) ? C3 C2 C5 C9 . . . . 169.9(3) ? C1 C2 C5 C6 . . . . 178.8(3) ? C3 C2 C5 C6 . . . . -6.2(5) ? C1 C2 C5 Fe1 . . . . 88.4(4) ? C3 C2 C5 Fe1 . . . . -96.6(3) ? C9 C5 C6 C7 . . . . -1.0(3) ? C2 C5 C6 C7 . . . . 175.9(3) ? Fe1 C5 C6 C7 . . . . -59.4(2) ? C9 C5 C6 Fe1 . . . . 58.4(2) ? C2 C5 C6 Fe1 . . . . -124.8(3) ? C5 C6 C7 C8 . . . . 0.7(3) ? Fe1 C6 C7 C8 . . . . -59.4(2) ? C5 C6 C7 Fe1 . . . . 60.1(2) ? C6 C7 C8 C9 . . . . -0.2(3) ? Fe1 C7 C8 C9 . . . . -59.8(2) ? C6 C7 C8 Fe1 . . . . 59.6(2) ? C7 C8 C9 C5 . . . . -0.4(3) ? Fe1 C8 C9 C5 . . . . -60.0(2) ? C7 C8 C9 Fe1 . . . . 59.6(2) ? C6 C5 C9 C8 . . . . 0.8(3) ? C2 C5 C9 C8 . . . . -175.8(3) ? Fe1 C5 C9 C8 . . . . 59.2(2) ? C6 C5 C9 Fe1 . . . . -58.38(19) ? C2 C5 C9 Fe1 . . . . 125.0(3) ? C14 C10 C11 C12 . . . . -0.3(4) ? Fe1 C10 C11 C12 . . . . 59.5(2) ? C14 C10 C11 Fe1 . . . . -59.7(2) ? C10 C11 C12 C13 . . . . 0.4(4) ? Fe1 C11 C12 C13 . . . . 60.2(2) ? C10 C11 C12 Fe1 . . . . -59.8(2) ? C11 C12 C13 C14 . . . . -0.4(4) ? Fe1 C12 C13 C14 . . . . 59.6(2) ? C11 C12 C13 Fe1 . . . . -60.0(2) ? C11 C10 C14 C13 . . . . 0.0(3) ? Fe1 C10 C14 C13 . . . . -59.1(2) ? C11 C10 C14 Fe1 . . . . 59.1(2) ? C12 C13 C14 C10 . . . . 0.3(3) ? Fe1 C13 C14 C10 . . . . 59.3(2) ? C12 C13 C14 Fe1 . . . . -59.0(2) ? C20 C15 C16 C17 . . . . 0.6(5) ? N1 C15 C16 C17 . . . . 179.3(3) ? C15 C16 C17 C18 . . . . -0.6(5) ? C16 C17 C18 C19 . . . . 0.4(5) ? C17 C18 C19 C20 . . . . -0.1(5) ? C18 C19 C20 C15 . . . . 0.0(5) ? C16 C15 C20 C19 . . . . -0.3(5) ? N1 C15 C20 C19 . . . . -179.0(3) ? C3 C4 N1 C1 . . . . 0.2(3) ? C3 C4 N1 C15 . . . . 177.4(3) ? C2 C1 N1 C4 . . . . -0.7(3) ? C2 C1 N1 C15 . . . . -177.9(3) ? C16 C15 N1 C4 . . . . -178.3(3) ? C20 C15 N1 C4 . . . . 0.5(4) ? C16 C15 N1 C1 . . . . -1.6(4) ? C20 C15 N1 C1 . . . . 177.2(3) ? _shelx_hkl_file ; 0 0 -4 375688. 6736.99 3 0 0 -5 27.6328 86.5779 3 0 0 -5-40.6548 74.2707 2 0 0 5-77.9465 90.4105 2 0 0 -6 14827.7 513.981 2 0 0 6 13337.1 501.976 2 0 0 -6 13829.6 576.664 3 0 0 -7 136.306 115.576 3 0 0 7-103.060 116.594 2 0 0 8 51438.1 1310.97 2 0 0 -8 51220.9 1460.68 3 0 0 -9 160.610 127.995 3 0 0 9 424.452 200.528 3 0 0 -10 3298.97 341.677 3 0 0 10 2859.30 372.717 3 0 0 -11 31.5180 117.682 3 0 0 -11 54.7542 56.3434 4 0 0 11-222.483 185.347 3 0 0 -12 79920.5 2191.64 3 0 0 -12 68422.7 1472.62 4 0 0 -13 355.079 179.078 3 0 0 -13 344.261 84.7058 4 0 0 -14 5870.36 544.195 3 0 0 -14 4450.49 230.592 4 0 0 -15-40.5222 153.920 3 0 0 -16 30069.8 1437.42 3 0 0 -17 89.7627 166.194 3 0 0 -18 2255.03 449.681 3 0 0 -19-85.0876 236.285 3 0 0 -20 701.893 287.093 3 0 0 -21-397.213 261.503 3 0 0 -22 960.668 411.687 3 0 0 -23-105.856 341.395 3 0 0 -24 7681.48 944.855 3 0 0 -25-429.459 408.349 3 0 0 -26 1774.05 525.758 3 0 0 -27 342.065 296.997 3 0 0 -28 7910.74 1089.95 3 0 0 -29 380.734 380.587 3 0 0 -30 852.110 446.162 3 0 -1 0 82.1282 99.2471 2 0 -1 1 28441.1 848.947 2 0 -1 -1 27229.3 754.116 2 0 -1 -2 116610. 2247.06 2 0 -1 -2 117004. 2394.87 3 0 -1 2 114267. 2482.47 2 0 -1 -3 72628.1 1713.06 3 0 -1 -3 72851.3 1452.49 2 0 -1 3 73525.0 1772.14 2 0 -1 4 79.6055 153.953 2 0 -1 -4-45.3927 121.917 3 0 1 -5 21619.5 591.073 3 0 -1 5 22412.4 579.860 3 0 -1 -5 19953.8 822.658 3 0 -1 5 22108.8 862.492 2 0 -1 -6 54784.7 1585.49 3 0 -1 6 54995.4 1592.07 2 0 -1 6 57455.7 1259.59 3 0 -1 6 54561.1 1193.41 1 0 1 6 55794.1 1382.72 4 0 1 -6 55817.2 1261.30 3 0 -1 -7 8013.41 543.266 3 0 -1 7 8388.16 390.710 3 0 -1 7 8711.42 567.097 2 0 1 -7 8746.19 554.923 2 0 1 7 8172.21 445.136 4 0 1 -7 8373.23 399.236 3 0 -1 8 1178.47 252.757 2 0 1 8 878.426 152.571 4 0 -1 8 697.884 129.382 3 0 1 -8 946.589 155.944 3 0 -1 -8 769.464 188.791 3 0 1 -8 896.822 169.985 2 0 -1 9 22482.0 825.919 3 0 1 -9 23003.3 829.114 3 0 -1 9 22687.0 1014.90 2 0 -1 -9 23722.9 1056.35 3 0 -1 10 9416.18 550.631 3 0 -1 10 10266.9 687.992 2 0 -1 -10 9637.07 678.814 3 0 1 -10 9160.91 537.982 3 0 -1 -11-101.381 153.364 3 0 -1 11 16.0622 108.916 3 0 1 -11 48.5037 120.052 3 0 -1 11-204.197 235.283 2 0 -1 12 712.081 189.615 3 0 1 -12 714.848 184.118 3 0 -1 12 779.057 275.008 2 0 -1 -12 650.178 176.923 3 0 -1 13 21508.8 1031.41 3 0 -1 -13 21732.1 1175.98 3 0 1 -13 21329.9 994.140 3 0 1 -14 7676.03 599.244 3 0 -1 -14 6946.28 669.856 3 0 -1 -15 8092.49 753.934 3 0 1 -15 8551.09 673.168 3 0 -1 -16 437.377 247.399 3 0 1 -16 221.003 179.174 3 0 -1 -17 4177.78 574.260 3 0 1 -17 5088.23 551.191 3 0 1 -18 13421.0 957.210 3 0 -1 -18 12726.0 1038.87 3 0 1 -19 3205.13 517.354 3 0 -1 -19 2981.86 551.305 3 0 -1 -20-24.0823 198.374 3 0 1 -20 263.839 242.153 3 0 -1 -21 178.982 212.682 3 0 1 -21 142.232 192.938 3 0 1 -22 3948.58 605.991 3 0 -1 -22 3487.65 610.900 3 0 -1 -23 3814.84 684.621 3 0 1 -23 4969.13 703.558 3 0 1 -24 535.356 386.896 3 0 -1 -24 291.461 339.074 3 0 1 -25-338.466 285.416 3 0 -1 -25 7.71942 228.987 3 0 1 -26 3772.16 732.095 3 0 -1 -26 2439.60 754.258 3 0 -1 -27 5350.00 986.800 3 0 -1 -28 145.673 401.080 3 0 -1 -29 260.535 335.028 3 0 -1 -30 1833.00 563.137 3 0 -2 0-3.32262 96.6622 3 0 2 0-18.5353 100.764 3 0 -2 0 108.507 135.006 2 0 -2 1 21002.2 675.748 3 0 -2 -1 20669.9 764.362 3 0 2 1 17795.1 834.418 3 0 -2 1 19931.6 888.084 2 0 -2 -1 20442.0 838.656 2 0 -2 2 1195.02 227.406 2 0 -2 -2 1085.19 202.651 3 0 2 2 937.836 214.592 3 0 -2 -2 1095.05 191.993 2 0 -2 2 1108.43 124.100 3 0 2 3 12103.9 710.250 3 0 -2 3 12203.1 712.831 2 0 -2 -3 11672.9 625.624 3 0 -2 -3 12105.3 575.948 2 0 -2 3 11442.8 396.708 3 0 -2 -4 355.022 174.359 3 0 2 4 23.2837 132.213 3 0 -2 -4-24.7187 103.002 2 0 -2 4 414.917 214.333 2 0 2 5 25302.6 1132.77 3 0 -2 -5 24992.5 1037.98 3 0 -2 5 25419.5 1138.33 2 0 -2 -6 1148.77 242.356 3 0 2 6 995.368 235.809 4 0 -2 6 1336.62 300.529 2 0 -2 7 9073.93 681.684 2 0 2 7 9433.44 600.275 4 0 -2 -7 9317.79 671.340 3 0 -2 8 3775.48 204.531 3 0 -2 8 3781.05 459.754 2 0 2 -8 2393.26 214.981 3 0 2 8 4154.68 395.033 4 0 -2 -8 4210.31 470.450 3 0 2 9 70774.4 1952.20 4 0 2 -9 64789.1 1605.30 3 0 -2 9 72736.3 2288.37 2 0 -2 -9 68332.7 2193.80 3 0 -2 9 67760.3 1500.40 3 0 -2 10 22556.5 1205.28 2 0 2 -10 21107.4 732.397 3 0 -2 10 20593.0 697.385 3 0 -2 -10 19452.5 1094.96 3 0 2 10 21451.7 966.709 4 0 2 11 9316.25 640.499 4 0 -2 11 8756.26 473.081 3 0 2 -11 10121.1 496.660 3 0 -2 11 9816.06 809.810 2 0 -2 -11 9751.82 792.568 3 0 -2 -12 840.741 264.142 3 0 2 -12 854.140 178.423 3 0 -2 12 1035.16 322.945 2 0 -2 12 789.134 173.143 3 0 -2 12 568.331 92.6852 1 0 -2 -13 7412.56 732.449 3 0 2 -13 7308.63 481.932 3 0 -2 13 7062.54 496.252 3 0 -2 13 4528.53 299.954 1 0 -2 13 8380.56 774.581 2 0 -2 -14-30.4981 231.092 3 0 -2 14 161.384 84.5603 1 0 2 -14 121.578 98.2043 3 0 -2 14 162.943 96.4253 3 0 -2 15 24998.7 1114.73 3 0 2 -15 27015.7 1052.88 3 0 -2 -15 26491.3 1479.38 3 0 -2 15 21322.8 875.268 1 0 -2 -16 6873.41 773.230 3 0 -2 16 4796.25 518.128 3 0 2 -16 6781.50 529.455 3 0 -2 -17 7841.20 848.245 3 0 2 -17 7340.63 575.248 3 0 2 -18 4971.62 504.842 3 0 -2 -18 4658.71 664.805 3 0 2 -19 12274.5 819.405 3 0 -2 -19 13030.2 1148.34 3 0 -2 -20 2379.30 531.163 3 0 2 -20 3016.64 419.327 3 0 -2 -21 9420.18 1027.92 3 0 2 -21 7604.20 682.009 3 0 2 -22 577.752 209.135 3 0 -2 -22 683.825 360.422 3 0 -2 -23 5441.45 840.605 3 0 -2 -24 107.689 239.588 3 0 -2 -25 2649.21 747.325 3 0 -2 -26-165.591 284.783 3 0 -2 -27 1867.45 611.665 3 0 -2 -28-149.734 380.383 3 0 -3 0-50.5565 146.921 2 0 -3 0 34.1777 116.308 3 0 -3 1 7073.35 627.148 2 0 3 1 7285.84 573.408 3 0 -3 -1 6932.53 488.791 3 0 -3 1 7206.39 444.212 3 0 -3 -1 6981.29 593.598 2 0 -3 -2 71994.4 2049.87 3 0 -3 -2 74442.9 2183.44 2 0 3 2 73331.5 2273.82 3 0 -3 2 75052.9 1780.43 3 0 -3 2 75436.4 2366.69 2 0 -3 3 16690.8 610.094 3 0 -3 3 16953.3 1005.83 2 0 -3 -3 17128.6 869.370 2 0 3 3 15098.4 964.810 3 0 -3 -3 16904.7 859.539 3 0 -3 -4 240.529 126.265 3 0 -3 4 173.180 68.6333 3 0 -3 -4 186.217 168.506 2 0 -3 4 109.731 181.882 2 0 -3 5 35.1183 37.9537 3 0 -3 -5 57.0394 121.052 3 0 -3 6 33809.2 1566.19 2 0 -3 -6 32703.1 1399.92 3 0 3 6 35403.7 1451.49 4 0 -3 -7 17277.7 1017.79 3 0 -3 7 18539.6 1172.85 2 0 3 7 18727.7 1018.53 4 0 3 8 293.284 195.162 4 0 -3 8 263.151 222.495 2 0 -3 -8 549.377 244.895 3 0 -3 -9 474.213 228.950 3 0 3 9 874.956 249.524 4 0 -3 9 778.041 338.571 2 0 -3 -10 12354.6 940.487 3 0 3 10 13201.2 861.394 4 0 -3 10 11386.5 967.177 2 0 -3 11 18256.7 1246.93 2 0 3 11 17437.5 1014.01 4 0 -3 -11 16347.7 1136.70 3 0 -3 -12 2936.26 486.962 3 0 -3 12 2387.96 498.648 2 0 3 12 2882.79 421.736 4 0 3 13 578.431 259.569 4 0 -3 13 323.638 252.995 2 0 -3 -13 482.836 266.194 3 0 3 14 32149.6 1480.42 4 0 -3 -14 29856.5 1650.34 3 0 -3 -15 9507.56 941.853 3 0 -3 -16 7714.45 877.968 3 0 -3 -17 576.647 287.090 3 0 -3 -18 6752.16 873.860 3 0 -3 -19-168.859 237.122 3 0 -3 -20 1807.55 498.525 3 0 -3 -21 5213.90 877.796 3 0 -3 -22 7453.81 998.928 3 0 -3 -23 1809.92 524.835 3 0 -3 -24 583.255 449.253 3 0 -3 -25-238.715 420.995 3 0 -3 -26 3478.74 873.799 3 0 -4 0 32976.4 1598.77 2 0 -4 0 33597.2 1272.81 3 0 4 0 34818.6 1648.04 4 0 -4 -1 1010.47 237.187 3 0 -4 1 1222.94 214.210 3 0 -4 -1 650.461 276.326 2 0 4 1 994.596 330.012 4 0 -4 1 1374.21 349.941 2 0 -4 2 3664.03 339.854 3 0 -4 2 3130.28 502.783 2 0 -4 -2 3587.55 411.236 3 0 -4 3 560.184 236.205 2 0 -4 -3 465.132 188.031 3 0 4 3 750.753 260.889 4 0 -4 3 558.156 145.683 3 0 -4 4 39911.6 1142.51 3 0 -4 4 42309.6 1961.57 2 0 -4 -4 41908.3 1660.73 3 0 4 4 41654.5 1820.35 4 0 -4 -5 751.675 248.093 3 0 4 5 807.561 260.400 4 0 -4 5 1310.83 404.965 2 0 -4 5 494.609 95.5422 3 0 4 6 498.803 253.237 4 0 -4 6 242.270 270.478 2 0 -4 -6 260.892 200.671 3 0 -4 -7 1057.17 318.881 3 0 4 -7 585.034 101.232 1 0 4 7 1297.55 378.113 4 0 -4 7 1667.43 442.256 2 0 -4 8 39770.7 2038.01 2 0 4 8 40287.2 1790.88 4 0 -4 -8 39011.9 1807.63 3 0 -4 -9 8031.76 793.166 3 0 4 9 7562.86 745.657 4 0 -4 9 8299.74 910.984 2 0 -4 10 9032.15 966.237 2 0 4 10 8044.39 776.326 4 0 -4 -10 9371.16 869.174 3 0 -4 -11 390.849 270.656 3 0 4 11 321.781 192.612 4 0 4 12 9076.97 846.837 4 0 -4 -12 8981.66 911.634 3 0 4 13 1376.36 340.532 4 0 -4 -13 2071.65 452.091 3 0 4 14-95.9053 197.822 4 0 -4 -14-9.29362 189.663 3 0 -4 -15 1394.76 423.077 3 0 4 15 1770.89 456.689 4 0 -4 -16 13193.6 1186.44 3 0 4 -16 12671.8 922.516 4 0 4 -17 1542.82 329.195 4 0 -4 -17 811.536 388.428 3 0 -4 -18 129.616 266.053 3 0 -4 -19 1729.03 495.341 3 0 -4 -20 10436.8 1220.15 3 0 -4 -21-192.349 343.116 3 0 -4 -22-189.493 261.125 3 0 -4 -23 233.190 260.508 3 0 5 0-8.20217 200.589 4 0 -5 0 165.321 152.109 3 0 5 -1 656.410 238.669 4 0 5 1 1161.81 347.813 4 0 -5 1 1319.57 277.726 3 0 -5 -1 1554.00 310.626 3 0 5 2 21749.6 1442.17 4 0 5 -2 21283.4 1393.58 4 0 -5 -2 20788.5 1145.22 3 0 -5 2 19208.5 929.018 3 0 -5 -3 6629.62 686.295 3 0 -5 3 6649.64 480.682 3 0 5 -3 7146.36 799.842 4 0 5 3 7825.42 860.560 4 0 -5 -4 3040.91 495.752 3 0 5 4 3659.36 624.404 4 0 5 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6605.47 659.842 4 -2 -4 15 5061.18 773.504 2 -2 4 15 5501.44 640.470 4 2 -4 -15 5653.14 796.114 3 2 -4 -14 4964.74 759.781 3 -2 -4 14 5084.16 824.055 2 2 4 -14 5188.08 589.091 4 -2 4 14 4773.46 609.680 4 2 -4 -13 824.174 393.670 3 -2 4 13 1487.13 363.330 4 -2 -4 13 1401.43 474.383 2 2 4 -13 1184.00 343.979 4 2 -4 -12 22039.9 1534.04 3 -2 -4 12 24104.1 1633.45 2 2 4 -12 24688.3 1284.44 4 -2 4 12 22969.0 1345.33 4 2 -4 -11-201.618 281.654 3 -2 4 11 18.9835 200.780 4 2 4 -11 302.320 248.113 4 -2 -4 11-496.002 335.491 2 2 -4 -10 1846.87 402.232 3 -2 4 10 1225.34 324.568 4 2 4 -10 784.037 205.431 4 -2 -4 10 1812.41 507.067 2 2 -4 -9 4627.41 653.146 3 2 4 -9 4802.05 573.172 4 -2 -4 9 4254.91 663.300 2 2 4 -8 6857.73 686.109 4 2 -4 -8 5989.12 753.135 3 -2 -4 8 7339.52 868.657 2 -2 -4 7 2790.70 348.117 3 2 4 -7 3136.50 490.311 4 -2 -4 7 2079.08 305.431 3 -2 -4 7 3413.47 585.834 2 2 4 -7 2003.85 222.370 1 2 -4 -7 3981.54 538.984 3 2 4 -6 5484.75 423.089 1 2 4 -6 6756.53 691.921 4 -2 -4 6 5985.03 733.725 2 -2 -4 6 7229.20 546.008 3 2 -4 -6 5138.56 662.094 3 -2 -4 5 4623.70 669.058 2 2 4 -5 4325.86 546.914 4 -2 -4 5 4548.69 457.204 3 2 -4 -5 4455.03 529.975 3 2 4 -5 4296.51 416.738 1 2 4 -4 16724.5 916.832 1 2 -4 -4 16469.1 1019.14 3 -2 -4 4 18337.0 945.968 3 -2 -4 4 16875.8 1234.03 2 2 4 -4 16104.5 1079.01 4 -2 -4 3 396.540 334.634 2 2 4 -3 277.322 128.139 1 2 4 -3 168.090 168.810 4 -2 -4 3 509.120 180.710 3 2 -4 -3 290.709 215.788 3 2 4 -2 5304.58 587.319 4 -2 -4 2 5354.03 514.668 3 2 -4 -2 5287.21 519.957 3 -2 -4 2 5040.44 654.932 2 -2 -4 1 437.258 177.363 3 2 4 -1 915.804 300.899 4 -2 -4 1 252.669 216.153 2 2 -4 -1 718.961 224.624 3 2 -4 0 13156.5 739.013 3 2 4 0 12304.6 944.795 4 -2 -4 0 13449.0 892.594 3 -2 4 0 9142.40 770.226 3 -2 -4 0 12423.2 964.263 2 -2 4 -1 1105.60 266.129 3 -2 -4 -1 963.748 216.717 3 2 4 1 974.570 285.543 4 -2 -4 -1 1455.49 344.895 2 2 -4 1 947.120 199.030 3 -2 -4 -2 21180.3 1230.42 2 2 4 2 20030.8 1233.65 4 -2 -4 -2 23141.4 1241.29 3 2 -4 2 20417.8 834.042 3 -2 4 -2 19965.5 947.936 3 2 -4 3 3969.71 317.529 3 -2 -4 -3 4856.36 566.274 3 2 4 3 4908.85 604.218 4 -2 4 -3 3575.41 369.742 3 -2 -4 -3 4532.60 570.825 2 2 4 4 12223.2 951.881 4 -2 -4 -4 12279.2 917.238 3 -2 -4 -4 11590.2 867.194 2 2 4 5 2120.75 418.833 4 -2 -4 -5 1745.47 351.763 2 -2 -4 -5 2091.59 392.820 3 -2 -4 -6 13616.2 1014.01 3 2 4 6 14186.8 1061.59 4 -2 4 -6 16349.6 819.525 1 -2 -4 -6 14290.7 927.841 2 -2 4 -7 7586.36 522.371 1 -2 -4 -7 6508.39 723.796 3 -2 -4 -7 6948.17 602.337 2 2 4 7 6092.74 706.698 4 2 4 8 8364.95 822.883 4 -2 4 -8 8030.22 503.860 1 -2 -4 -8 9467.78 688.115 2 -2 -4 -8 7760.26 781.667 3 -2 4 -9 3423.74 281.754 1 -2 -4 -9 4707.53 476.211 2 -2 -4 -9 4623.53 651.365 3 -2 -4 -10 17367.6 1256.45 3 -2 -4 -10 18405.1 909.856 2 -2 -4 -11 82.1623 184.679 3 -2 -4 -11 245.180 164.301 2 -2 -4 -12 16076.0 1251.17 3 -2 -4 -13 1394.81 384.365 3 -2 -4 -14 5507.31 761.502 3 -2 -4 -15 514.150 239.582 3 -2 -4 -16 8344.94 1006.66 3 -2 -4 -17 646.858 390.839 3 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54068.0 1676.36 3 -3 0 4 37.0942 133.442 1 3 0 -4 28.5601 136.664 3 -3 0 3 31953.5 1183.28 1 3 0 -3 30495.9 1164.14 3 -3 0 2 21.9961 132.904 1 -3 0 1 2156.40 279.518 1 -3 0 0 37.1640 119.835 1 -3 0 -1 297232. 5856.51 1 -3 0 -2-37.2395 126.423 1 -3 0 -3 191082. 4102.65 1 -3 0 -4 217.696 149.645 1 -3 0 -5 269.714 135.623 1 -3 0 -6 23.7101 115.965 1 -3 0 -7 53504.1 1801.16 1 3 0 8 99.3291 169.438 1 -3 0 -8 324.103 186.052 3 -3 0 -9 9644.01 704.468 3 -3 0 -10-241.029 212.168 3 -3 0 -11 83330.2 2571.69 3 -3 0 -12-54.4694 162.311 3 -3 0 -13 679.546 298.309 3 -3 0 -14 74.5759 147.385 3 -3 0 -15 28679.5 1444.76 3 -3 0 -16 29.4930 193.350 3 -3 0 -17 459.375 246.943 3 -3 0 -18-374.308 232.905 3 -3 0 -19 18501.6 1231.21 3 -3 0 -20 79.7287 230.065 3 -3 0 -21 8054.20 868.301 3 -3 0 -22-243.072 227.920 3 -3 0 -23 40316.2 2112.40 3 -3 0 -24 123.504 286.099 3 -3 0 -25-71.9220 259.963 3 -3 0 -26-91.7615 259.167 3 -3 0 -27 8014.24 1050.58 3 -3 0 -28 389.232 400.763 3 3 -1 -29 3030.10 775.512 3 3 1 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405.954 666.112 1 -12 1 15 2992.26 901.522 1 -12 -1 15 4579.02 1056.99 1 -12 1 14-477.782 605.425 1 -12 -1 14 195.721 413.150 1 -12 1 13 1241.87 582.338 1 -12 -1 13-198.064 407.570 1 -12 1 12 437.071 437.187 1 -12 -1 12 1048.69 515.738 1 -12 1 11 301.304 485.602 1 -12 -1 11 530.937 433.341 1 -12 1 10 3376.91 833.466 1 -12 -1 10 3787.11 842.439 1 -12 -1 9 12745.4 1516.62 1 -12 1 9 11171.3 1482.06 1 -12 1 8-508.507 414.050 1 -12 -1 8 48.6888 373.298 1 -12 -1 7 1145.30 452.795 1 -12 1 7 1589.75 634.697 1 -12 -1 6 210.445 315.892 1 -12 1 6 158.689 397.613 1 -12 -1 5 12761.9 1414.56 1 -12 1 5 14437.7 1570.53 1 -12 -1 4 5242.19 930.906 1 -12 1 4 6615.99 1098.74 1 -12 -1 3 6131.40 968.905 1 -12 1 3 6044.71 1037.82 1 -12 -1 2 1640.23 535.576 1 -12 1 2 1699.75 560.627 1 -12 -1 1 13032.2 1422.62 1 -12 1 1 12508.6 1447.86 1 -12 -1 0 6283.70 983.628 1 -12 1 0 5519.40 980.559 1 -12 -1 -1 4586.22 851.762 1 -12 1 -1 4452.49 861.781 1 -12 -1 -2-405.303 396.433 1 -12 1 -2-102.228 401.500 1 -12 1 -3 6292.79 988.199 1 -12 -1 -3 7235.77 1073.79 1 -12 1 -4 7715.02 1116.61 1 -12 -1 -4 5831.79 978.901 1 -12 1 -5 5790.98 987.203 1 -12 -1 -5 5447.76 933.783 1 -12 1 -6 1647.24 597.017 1 -12 -1 -6 2450.47 683.863 1 -12 -1 -7 11308.4 1399.12 1 -12 1 -7 10592.7 1311.52 1 -12 -1 -8 6266.83 1034.53 1 -12 1 -8 6253.94 1024.70 1 -12 -1 -9 8519.83 1256.42 1 -12 1 -9 8520.12 1214.55 1 -12 -1 -10 373.641 506.223 1 -12 1 -10 828.899 534.153 1 -12 -1 -11 361.924 360.157 1 -12 1 -11 683.723 433.735 1 -12 1 -12 8569.06 1275.16 1 -12 1 -13 2181.96 757.295 1 -12 1 -14 763.728 544.409 1 -12 -2 14 3.27368 293.945 1 -12 -2 13 929.828 449.266 1 -12 -2 12 31.8007 324.051 1 -12 2 12 241.142 323.511 1 -12 -2 11 5260.21 967.899 1 -12 2 11 4163.29 1056.71 1 -12 -2 10 200.648 343.265 1 -12 2 10 153.931 373.695 1 -12 -2 9 1597.36 560.083 1 -12 2 9 1081.78 550.888 1 -12 -2 8-298.659 408.366 1 -12 2 8-433.837 376.633 1 -12 -2 7 5779.54 999.633 1 -12 2 7 5678.91 1088.29 1 -12 2 6-137.967 373.375 1 -12 -2 6 198.374 280.219 1 -12 2 5 437.647 306.354 1 -12 -2 5-66.9569 279.703 1 -12 -2 4-144.219 337.089 1 -12 2 4 1501.42 648.879 1 -12 -2 3 13929.1 1465.54 1 -12 2 3 13832.9 1599.08 1 -12 2 2 3336.62 789.049 1 -12 -2 2 2763.55 677.649 1 -12 2 1 7904.48 1186.43 1 -12 -2 1 7994.16 1112.86 1 -12 2 0 451.354 366.866 1 -12 -2 0-351.453 372.228 1 -12 -2 -1 12290.9 1430.35 1 -12 2 -1 10728.3 1341.87 1 -12 2 -2 1298.98 551.521 1 -12 -2 -2 416.921 286.410 1 -12 -2 -3 14743.7 1579.10 1 -12 2 -3 17230.5 1694.80 1 -12 2 -4 3859.23 810.709 1 -12 -2 -4 4590.28 828.808 1 -12 2 -5 18750.2 1756.30 1 -12 -2 -5 21314.3 1914.19 1 -12 2 -6 5782.00 975.096 1 -12 -2 -6 4200.42 856.422 1 -12 2 -7 15590.0 1625.94 1 -12 -2 -7 15829.1 1659.08 1 -12 2 -8 8774.22 1205.56 1 -12 -2 -8 7288.62 1148.89 1 -12 2 -9 7294.99 1130.56 1 -12 -2 -9 8955.20 1263.28 1 -12 2 -10 1380.05 587.844 1 -12 2 -11 6049.45 1106.08 1 -12 2 -12 755.668 570.191 1 -12 2 -13 7512.26 1248.40 1 -12 2 -14-586.074 604.785 1 -12 2 -15 5202.38 1094.26 1 -12 -3 10 4.67851 356.344 1 -12 -3 9 1887.74 614.434 1 -12 -3 8 7829.29 1119.72 1 -12 3 7-23.5087 372.950 1 -12 -3 7 980.203 438.824 1 -12 3 6-258.095 493.582 1 -12 -3 6-287.332 413.806 1 -12 3 5 26.3507 600.293 1 -12 -3 5 538.321 317.103 1 -12 3 4 8023.07 1306.30 1 -12 -3 4 7742.17 1095.97 1 -12 3 3 989.793 479.300 1 -12 -3 3 238.183 360.006 1 -12 -3 2 793.100 450.517 1 -12 3 2 2012.28 651.099 1 -12 -3 1 2080.21 589.575 1 -12 3 1 2353.72 720.945 1 -12 3 0 10739.7 1382.04 1 -12 -3 0 11456.4 1398.62 1 -12 -3 -1 3387.84 655.024 1 -12 3 -1 5707.91 1048.57 1 -12 3 -2 86.7755 328.351 1 -12 -3 -2-208.195 462.983 1 -12 3 -3 99.1641 480.252 1 -12 -3 -3 40.7650 291.538 1 -12 3 -4 5063.61 980.174 1 -12 -3 -4 4139.21 926.193 1 -12 3 -5 9481.04 1303.57 1 -12 3 -6 809.856 507.532 1 -12 3 -7 771.910 522.978 1 -12 3 -8 13893.9 1595.17 1 -12 3 -9 5029.67 878.947 1 -12 3 -10-299.999 458.538 1 -12 3 -11-271.805 455.344 1 -12 3 -12 3791.10 898.918 1 -12 -4 5 1808.47 640.470 1 -12 -4 4 1111.15 580.368 1 -12 -4 3 1127.80 365.076 1 -12 4 0 910.117 441.268 1 -12 4 -1 100.237 352.276 1 -12 4 -2 5251.34 1076.05 1 -12 4 -3 238.112 503.510 1 -12 4 -4 968.907 627.498 1 -12 4 -5 1561.22 642.534 1 -12 4 -6 7671.03 1189.20 1 -12 4 -7 16.7314 437.361 1 -13 0 12-215.850 335.884 1 -13 0 11 3752.35 1017.51 1 -13 0 10 380.062 321.604 1 -13 0 9 248.046 363.815 1 -13 0 8-594.830 602.855 1 -13 0 7 16034.4 1809.42 1 -13 0 6 125.424 375.040 1 -13 0 5 1813.76 506.613 1 -13 0 4 472.013 455.807 1 -13 0 3 14485.1 1680.23 1 -13 0 2 104.461 410.523 1 -13 0 1 444.802 525.191 1 -13 0 0 224.483 410.646 1 -13 0 -1 7733.43 1201.69 1 -13 0 -2-572.756 467.416 1 -13 0 -3 1224.89 642.771 1 -13 0 -4 624.960 544.786 1 -13 0 -5 2459.26 689.296 1 -13 0 -6-110.948 430.775 1 -13 0 -7-613.984 441.554 1 -13 -1 13 1764.09 804.562 1 -13 -1 12 7306.51 1257.38 1 -13 -1 11 1131.69 614.532 1 -13 -1 10-284.092 386.708 1 -13 -1 9 13262.5 1628.49 1 -13 1 9 13712.7 1785.86 1 -13 -1 8 4429.01 940.143 1 -13 1 8 3405.34 906.538 1 -13 -1 7 108.319 399.967 1 -13 1 7 223.254 384.049 1 -13 -1 6 816.842 529.622 1 -13 1 6 857.328 477.643 1 -13 -1 5 2267.74 698.522 1 -13 1 5 1547.14 605.470 1 -13 -1 4 2426.48 704.634 1 -13 1 4 2131.24 662.768 1 -13 -1 3 282.369 400.851 1 -13 1 3 502.226 467.715 1 -13 -1 2 2775.52 757.223 1 -13 1 2 3284.58 860.005 1 -13 -1 1 4946.79 978.892 1 -13 1 1 5473.25 1098.58 1 -13 -1 0 8205.97 1232.60 1 -13 1 0 7281.55 1223.92 1 -13 -1 -1 2261.26 761.575 1 -13 1 -1 2551.52 785.601 1 -13 1 -2 492.955 586.093 1 -13 -1 -2 533.802 365.814 1 -13 1 -3 6287.01 1101.38 1 -13 -1 -3 7191.50 1121.90 1 -13 1 -4 1081.19 595.969 1 -13 -1 -4 442.020 468.344 1 -13 1 -5 382.406 496.253 1 -13 -1 -5 58.6768 401.875 1 -13 1 -6 3095.03 826.956 1 -13 1 -7 5634.02 1075.88 1 -13 1 -8 804.469 527.880 1 -13 -2 14 671.857 522.329 1 -13 -2 13 672.035 573.088 1 -13 -2 12 461.083 600.742 1 -13 -2 11 1707.06 702.383 1 -13 -2 10 87.1446 379.705 1 -13 -2 9-334.795 322.040 1 -13 -2 8 924.787 433.863 1 -13 -2 7 2730.96 730.467 1 -13 -2 6 1147.99 483.861 1 -13 -2 5-191.314 493.708 1 -13 -2 4 1451.06 525.088 1 -13 2 4 2474.89 764.787 1 -13 2 3 1040.06 614.281 1 -13 -2 3 974.299 508.608 1 -13 2 2 728.918 353.025 1 -13 -2 2 1254.22 570.757 1 -13 2 1 788.464 480.032 1 -13 -2 1 1018.55 553.888 1 -13 2 0 3611.02 924.270 1 -13 -2 0 3831.56 794.553 1 -13 2 -1 2035.94 683.317 1 -13 -2 -1 1239.11 634.408 1 -13 -2 -2 11836.8 1414.74 1 -13 2 -2 11509.4 1491.43 1 -13 2 -3 2091.85 632.153 1 -13 2 -4-107.818 371.207 1 -13 2 -5 3915.27 822.124 1 -13 2 -6 15863.0 1709.59 1 -13 -3 9 3324.80 848.904 1 -13 -3 8 210.078 382.456 1 -13 -3 7 386.744 349.323 1 -13 -3 6 2600.65 728.063 1 -13 -3 5 1987.17 642.949 1 -13 -3 4 1777.47 711.072 1 -13 -3 3 10.6795 456.191 1 0 0 0 0.00 0.00 0 TITL UP-3FcPhPy in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 0.71073 10.917331 5.801106 23.085213 90.0000 93.1598 90.0000 ZERR 4.00 0.000772 0.000579 0.002298 0.0000 0.0073 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C N Fe UNIT 80.00 4.00 4.00 TREF HKLF 4 END ; _shelx_hkl_checksum 11623 _shelx_res_file ; TITL UP-3FcPhPy in P2(1)/n CELL 0.71073 10.9173 5.8011 23.0852 90.000 93.160 90.000 ZERR 4.00 0.0008 0.0006 0.0023 0.000 0.007 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C N FE H UNIT 80 4 4 68 MERG 2 OMIT 0.00 52.00 OMIT 4 5 10 OMIT -1 0 13 OMIT -11 3 12 OMIT -2 1 11 OMIT -2 6 14 FMAP 2 PLAN 25 ACTA 52.00 BOND $H CONF L.S. 14 WGHT 0.050300 FVAR 3.40023 C1 1 0.549892 0.119583 0.241549 11.00000 0.00983 0.01805 = 0.02402 -0.00063 0.00056 0.00150 AFIX 43 H1 4 0.517579 0.261516 0.229843 11.00000 -1.20000 AFIX 0 C2 1 0.543498 0.023649 0.295914 11.00000 0.00702 0.01916 = 0.02316 0.00325 -0.00168 -0.00284 C3 1 0.606628 -0.191115 0.294215 11.00000 0.01022 0.02274 = 0.02711 0.00434 -0.00199 -0.00248 AFIX 43 H3 4 0.618263 -0.293989 0.324923 11.00000 -1.20000 AFIX 0 C4 1 0.646590 -0.219521 0.240429 11.00000 0.00982 0.01768 = 0.03059 0.00137 -0.00147 0.00293 AFIX 43 H4 4 0.690108 -0.346083 0.227810 11.00000 -1.20000 AFIX 0 C5 1 0.491718 0.124759 0.346513 11.00000 0.00515 0.02177 = 0.02268 0.00297 0.00060 -0.00195 C6 1 0.485870 0.013583 0.401817 11.00000 0.00956 0.02416 = 0.02158 0.00423 -0.00352 -0.00058 AFIX 43 H6 4 0.509908 -0.137061 0.410256 11.00000 -1.20000 AFIX 0 C7 1 0.437507 0.171008 0.441352 11.00000 0.01403 0.03090 = 0.01963 -0.00102 -0.00425 -0.00164 AFIX 43 H7 4 0.425105 0.142441 0.480234 11.00000 -1.20000 AFIX 0 C8 1 0.411232 0.379943 0.411376 11.00000 0.01416 0.02165 = 0.02463 -0.00189 -0.00262 -0.00061 AFIX 43 H8 4 0.378344 0.512190 0.427173 11.00000 -1.20000 AFIX 0 C9 1 0.443614 0.352702 0.353358 11.00000 0.00976 0.02216 = 0.02665 0.00420 0.00159 -0.00233 AFIX 43 H9 4 0.435155 0.464002 0.324419 11.00000 -1.20000 AFIX 0 C10 1 0.202854 -0.023537 0.308009 11.00000 0.00939 0.03970 = 0.02509 -0.00533 -0.00337 -0.00126 AFIX 43 H10 4 0.225677 -0.058165 0.270775 11.00000 -1.20000 AFIX 0 C11 1 0.212098 -0.173340 0.356513 11.00000 0.01199 0.02181 = 0.04982 -0.00194 -0.00488 -0.00240 AFIX 43 H11 4 0.241738 -0.323646 0.356640 11.00000 -1.20000 AFIX 0 C12 1 0.168559 -0.054902 0.404517 11.00000 0.01539 0.04483 = 0.02990 0.00856 -0.00308 -0.00964 AFIX 43 H12 4 0.164857 -0.112798 0.441947 11.00000 -1.20000 AFIX 0 C13 1 0.131407 0.168069 0.385670 11.00000 0.00833 0.03501 = 0.03423 -0.00925 0.00397 -0.00243 AFIX 43 H13 4 0.098526 0.282191 0.408466 11.00000 -1.20000 AFIX 0 C14 1 0.153260 0.186224 0.325923 11.00000 0.01149 0.02825 = 0.03188 0.00600 -0.00485 -0.00193 AFIX 43 H14 4 0.137487 0.314777 0.302623 11.00000 -1.20000 AFIX 0 C15 1 0.641667 0.008380 0.148787 11.00000 0.00521 0.02599 = 0.02362 -0.00195 -0.00075 -0.00369 C16 1 0.604597 0.208842 0.120470 11.00000 0.01824 0.02859 = 0.03121 0.00161 0.00399 0.00617 AFIX 43 H16 4 0.559480 0.318418 0.139564 11.00000 -1.20000 AFIX 0 C17 1 0.634673 0.246649 0.063569 11.00000 0.02657 0.04089 = 0.03198 0.00960 0.00136 0.00714 AFIX 43 H17 4 0.608810 0.381119 0.044675 11.00000 -1.20000 AFIX 0 C18 1 0.702482 0.086938 0.034775 11.00000 0.02012 0.04881 = 0.02583 0.00223 0.00487 0.00298 AFIX 43 H18 4 0.722937 0.112871 -0.003255 11.00000 -1.20000 AFIX 0 C19 1 0.739337 -0.111742 0.063422 11.00000 0.02214 0.03987 = 0.03077 -0.00115 0.00549 0.00603 AFIX 43 H19 4 0.784994 -0.220393 0.044297 11.00000 -1.20000 AFIX 0 C20 1 0.710060 -0.152933 0.119724 11.00000 0.01934 0.02916 = 0.02744 0.00191 0.00011 0.00488 AFIX 43 H20 4 0.735883 -0.288106 0.138298 11.00000 -1.20000 AFIX 0 N1 2 0.612526 -0.031030 0.207336 11.00000 0.00681 0.02083 = 0.02375 0.00025 -0.00087 0.00028 FE1 3 0.313501 0.115849 0.373377 11.00000 0.00849 0.01993 = 0.02015 0.00174 -0.00110 -0.00065 HKLF 4 REM UP-3FcPhPy in P2(1)/n REM R1 = 0.0450 for 2198 Fo > 4sig(Fo) and 0.0668 for all 2858 data REM 199 parameters refined using 0 restraints END WGHT 0.0503 0.0000 REM Highest difference peak 0.502, deepest hole -0.751, 1-sigma level 0.088 Q1 1 0.2339 -0.0529 0.3795 11.00000 0.05 0.50 Q2 1 0.2449 0.0882 0.3280 11.00000 0.05 0.41 Q3 1 0.3979 -0.0368 0.3645 11.00000 0.05 0.40 Q4 1 0.5833 -0.2057 0.2621 11.00000 0.05 0.38 Q5 1 0.6823 -0.1321 0.2622 11.00000 0.05 0.35 Q6 1 0.3010 -0.3510 0.3725 11.00000 0.05 0.35 Q7 1 0.3064 -0.0475 0.4145 11.00000 0.05 0.34 Q8 1 0.1459 -0.1092 0.3694 11.00000 0.05 0.34 Q9 1 0.6672 0.2235 0.0953 11.00000 0.05 0.33 Q10 1 0.4062 0.2407 0.3452 11.00000 0.05 0.33 Q11 1 0.5832 -0.0756 0.2958 11.00000 0.05 0.31 Q12 1 0.4128 0.0788 0.5000 11.00000 0.05 0.31 Q13 1 0.4016 0.4077 0.3220 11.00000 0.05 0.31 Q14 1 0.5502 0.3953 0.3806 11.00000 0.05 0.30 Q15 1 0.4014 0.2140 0.4110 11.00000 0.05 0.30 Q16 1 0.6160 0.0948 0.1208 11.00000 0.05 0.30 Q17 1 0.5630 0.0917 0.2822 11.00000 0.05 0.28 Q18 1 0.5382 0.0882 0.3160 11.00000 0.05 0.28 Q19 1 0.1206 0.2261 0.2737 11.00000 0.05 0.28 Q20 1 0.3782 0.1001 0.4187 11.00000 0.05 0.28 Q21 1 0.5054 0.5183 0.4672 11.00000 0.05 0.27 Q22 1 0.3158 0.2197 0.3167 11.00000 0.05 0.27 Q23 1 0.5776 0.2203 0.0861 11.00000 0.05 0.27 Q24 1 0.5005 0.2369 0.2178 11.00000 0.05 0.26 Q25 1 0.8220 0.2243 0.0543 11.00000 0.05 0.26 ; _shelx_res_checksum 82994 _shelxl_version_number .2013