# Copyright The Royal Society of Chemistry, 1999 # CCDC Number:440/117 data_global _submitted_journal 'New Journal of Chemistry' _publ_section_title ; Influence of the anion of FeIII salts on the product distribution in the oxidative degradation of a tetrapyridyl ligand ; loop_ _publ_author_name 'Michael Renz' 'Catherine Hemmert' 'Heinz Gornitzka' 'Bernard Meunier' data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H11 Cl3 Fe N3' _chemical_formula_weight 347.43 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' 'Cl' 'Cl' 0.1484 0.1585 '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 monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 11.257(2) _cell_length_b 8.6710(10) _cell_length_c 14.644(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.33(2) _cell_angle_gamma 90.00 _cell_volume 1364.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 24.09 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 1.676 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 'STOE-IPDS' _diffrn_measurement_method 'phi-rotation' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10040 _diffrn_reflns_av_R_equivalents 0.0553 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 24.09 _reflns_number_total 2097 _reflns_number_gt 1985 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE-IPDS' _computing_cell_refinement 'STOE-IPDS' _computing_data_reduction 'STOE-IPDS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP (Zsolnai, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+0.8864P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2097 _refine_ls_number_parameters 175 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0318 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0830 _refine_ls_wR_factor_gt 0.0819 _refine_ls_goodness_of_fit_ref 1.114 _refine_ls_restrained_S_all 1.114 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.35379(3) 0.17284(4) 0.64216(2) 0.02225(15) Uani 1 d . . . Cl1 Cl 0.42355(6) 0.24774(8) 0.51940(4) 0.0360(2) Uani 1 d . . . Cl2 Cl 0.16686(5) 0.30550(7) 0.60116(4) 0.02783(18) Uani 1 d . . . Cl3 Cl 0.27999(6) -0.07240(8) 0.59775(4) 0.03323(19) Uani 1 d . . . N1 N 0.34568(19) 0.1356(3) 0.78736(14) 0.0224(4) Uani 1 d . . . H1N H 0.294(3) 0.198(4) 0.799(2) 0.027(8) Uiso 1 d . . . H2N H 0.328(2) 0.041(4) 0.8003(18) 0.022(7) Uiso 1 d . . . C1 C 0.4706(2) 0.1804(3) 0.84702(17) 0.0221(5) Uani 1 d . . . H1 H 0.481(2) 0.167(3) 0.912(2) 0.025(7) Uiso 1 d . . . N2 N 0.53391(18) 0.0728(2) 0.71967(14) 0.0239(4) Uani 1 d . . . C2 C 0.6111(2) -0.0038(3) 0.68180(19) 0.0304(6) Uani 1 d . . . H2 H 0.5915 -0.0108 0.6142 0.036 Uiso 1 calc R . . C3 C 0.7180(2) -0.0726(3) 0.7379(2) 0.0353(7) Uani 1 d . . . H3 H 0.7705 -0.1280 0.7094 0.042 Uiso 1 calc R . . C4 C 0.7481(2) -0.0605(3) 0.8358(2) 0.0355(6) Uani 1 d . . . H4 H 0.8222 -0.1063 0.8755 0.043 Uiso 1 calc R . . C5 C 0.6691(2) 0.0194(3) 0.87588(18) 0.0304(6) Uani 1 d . . . H5 H 0.6880 0.0294 0.9433 0.036 Uiso 1 calc R . . C6 C 0.5630(2) 0.0836(3) 0.81557(17) 0.0237(5) Uani 1 d . . . N3 N 0.44112(18) 0.3748(3) 0.72792(14) 0.0236(4) Uani 1 d . . . C7 C 0.4508(2) 0.5176(3) 0.69652(19) 0.0296(6) Uani 1 d . . . H7 H 0.4182 0.5388 0.6301 0.036 Uiso 1 calc R . . C8 C 0.5064(2) 0.6345(3) 0.7574(2) 0.0343(6) Uani 1 d . . . H8 H 0.5103 0.7357 0.7335 0.041 Uiso 1 calc R . . C9 C 0.5568(2) 0.6038(3) 0.8536(2) 0.0341(6) Uani 1 d . . . H9 H 0.5975 0.6829 0.8965 0.041 Uiso 1 calc R . . C10 C 0.5473(2) 0.4566(3) 0.88677(19) 0.0281(6) Uani 1 d . . . H10 H 0.5814 0.4323 0.9527 0.034 Uiso 1 calc R . . C11 C 0.4876(2) 0.3463(3) 0.82226(17) 0.0227(5) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0258(2) 0.0212(2) 0.0188(2) -0.00032(13) 0.00530(15) -0.00037(13) Cl1 0.0469(4) 0.0396(5) 0.0255(3) 0.0029(3) 0.0170(3) 0.0026(3) Cl2 0.0277(3) 0.0275(4) 0.0256(3) -0.0014(2) 0.0038(2) 0.0025(2) Cl3 0.0363(4) 0.0248(4) 0.0332(3) -0.0034(3) 0.0021(3) -0.0024(3) N1 0.0247(11) 0.0189(12) 0.0245(11) 0.0015(9) 0.0086(9) -0.0009(10) C1 0.0262(12) 0.0227(14) 0.0175(12) -0.0002(9) 0.0067(10) -0.0003(10) N2 0.0263(10) 0.0210(11) 0.0253(10) -0.0007(8) 0.0092(8) -0.0017(8) C2 0.0342(14) 0.0269(15) 0.0344(14) -0.0050(11) 0.0168(11) -0.0019(11) C3 0.0295(13) 0.0326(17) 0.0491(16) -0.0034(13) 0.0201(12) 0.0019(11) C4 0.0231(12) 0.0347(17) 0.0459(16) 0.0010(13) 0.0059(11) 0.0022(11) C5 0.0297(13) 0.0281(15) 0.0297(13) -0.0008(11) 0.0032(11) 0.0010(11) C6 0.0269(12) 0.0191(13) 0.0250(12) -0.0014(10) 0.0073(10) -0.0040(10) N3 0.0241(10) 0.0224(12) 0.0249(10) 0.0010(9) 0.0080(8) -0.0009(9) C7 0.0279(13) 0.0269(15) 0.0340(14) 0.0070(11) 0.0091(10) 0.0017(11) C8 0.0318(14) 0.0204(14) 0.0508(17) 0.0013(12) 0.0123(12) -0.0022(11) C9 0.0306(13) 0.0255(15) 0.0448(15) -0.0102(12) 0.0092(12) -0.0041(11) C10 0.0251(12) 0.0272(15) 0.0315(13) -0.0063(11) 0.0076(10) 0.0009(11) C11 0.0210(11) 0.0236(14) 0.0248(12) -0.0025(10) 0.0088(10) 0.0022(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 N1 2.179(2) . ? Fe1 N2 2.186(2) . ? Fe1 N3 2.208(2) . ? Fe1 Cl1 2.2608(8) . ? Fe1 Cl3 2.3050(8) . ? Fe1 Cl2 2.3150(8) . ? N1 C1 1.469(3) . ? C1 C11 1.510(4) . ? C1 C6 1.512(3) . ? N2 C2 1.338(3) . ? N2 C6 1.347(3) . ? C2 C3 1.375(4) . ? C3 C4 1.375(4) . ? C4 C5 1.387(4) . ? C5 C6 1.374(4) . ? N3 C7 1.337(4) . ? N3 C11 1.347(3) . ? C7 C8 1.372(4) . ? C8 C9 1.379(4) . ? C9 C10 1.382(4) . ? C10 C11 1.371(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N2 74.73(8) . . ? N1 Fe1 N3 72.75(8) . . ? N2 Fe1 N3 80.36(8) . . ? N1 Fe1 Cl1 160.70(6) . . ? N2 Fe1 Cl1 92.22(6) . . ? N3 Fe1 Cl1 91.33(6) . . ? N1 Fe1 Cl3 91.28(7) . . ? N2 Fe1 Cl3 88.92(6) . . ? N3 Fe1 Cl3 162.59(6) . . ? Cl1 Fe1 Cl3 102.83(3) . . ? N1 Fe1 Cl2 91.58(6) . . ? N2 Fe1 Cl2 164.26(6) . . ? N3 Fe1 Cl2 88.26(6) . . ? Cl1 Fe1 Cl2 98.93(3) . . ? Cl3 Fe1 Cl2 99.31(3) . . ? C1 N1 Fe1 103.31(15) . . ? N1 C1 C11 106.1(2) . . ? N1 C1 C6 107.2(2) . . ? C11 C1 C6 107.9(2) . . ? C2 N2 C6 118.7(2) . . ? C2 N2 Fe1 126.73(17) . . ? C6 N2 Fe1 114.45(16) . . ? N2 C2 C3 121.9(2) . . ? C2 C3 C4 119.4(2) . . ? C3 C4 C5 119.3(2) . . ? C6 C5 C4 118.3(2) . . ? N2 C6 C5 122.5(2) . . ? N2 C6 C1 112.3(2) . . ? C5 C6 C1 125.1(2) . . ? C7 N3 C11 118.5(2) . . ? C7 N3 Fe1 127.39(17) . . ? C11 N3 Fe1 114.14(17) . . ? N3 C7 C8 122.0(2) . . ? C7 C8 C9 119.4(3) . . ? C8 C9 C10 119.1(3) . . ? C11 C10 C9 118.4(2) . . ? N3 C11 C10 122.7(2) . . ? N3 C11 C1 112.5(2) . . ? C10 C11 C1 124.8(2) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 24.09 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.337 _refine_diff_density_min -0.580 _refine_diff_density_rms 0.069 #===END