#Copyright The Royal Society of Chemistry, 1998 data_1M-RT _publ_contact_autor ; Fausto Calderazzo Dipartimento di Chimica e Chimica Industriale Universita' di Pisa Via Risorgimento, 35 56126 Pisa Italy ; _publ_contact_author_phone '050 918218' _publ_contact_author_fax '050 20237' _publ_contact_author_email 'facal@dcci.unipi.it' _publ_requested_journal 'Journal of Chemical Society, Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis, crystal structure and polymorphism of a \m-oxo bridged binuclear iron(III) complex of 2,2': 6',2'': 6'',2'''-quaterpyridine. ; loop_ _publ_author_name _publ_author_address 'Fausto Calderazzo' ; Dipartimento di Chimica e Chimica Industriale Universita' di Pisa Via Risorgimento, 35 56126 Pisa Italy ; 'Luca Labella' ; Dipartimento di Chimica e Chimica Industriale Universita' di Pisa Via Risorgimento, 35 56126 Pisa Italy ; 'Marchetti, Fabio' ; Dipartimento di Chimica e Chimica Industriale Universita' di Pisa Via Risorgimento, 35 56126 Pisa Italy ; #============================================================================== _audit_creation_method SHELXL _chemical_name_systematic ; bis-2,2':6',2'':6'',2''-quaterpyridine-bis-aquo-\m-oxo-diiron(III) perchlorate dihydrate ; _chemical_name_common ? _chemical_formula_moiety '[(Fe(C20H14N4)(H2O))2(\m-O)](ClO4)4.2H2O' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C40 H36 Cl4 Fe2 N8 O21' _chemical_formula_weight 1218.27 _chemical_melting_point ? _chemical_compound_source ? 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' '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 13.080(3) _cell_length_b 14.045(3) _cell_length_c 13.778(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.52(3) _cell_angle_gamma 90.00 _cell_volume 2438.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature '296 K' _cell_measurement_reflns_used 17 _cell_measurement_theta_min 8.4 _cell_measurement_theta_max 10.1 _exptl_crystal_description 'prism' _exptl_crystal_colour 'ruby-red' _exptl_crystal_size_max '0.31 mm' _exptl_crystal_size_mid '0.20 mm' _exptl_crystal_size_min '0.14 mm' _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.659 _exptl_crystal_density_method ? _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.903 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.6136 _exptl_absorpt_correction_T_max 0.6546 _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 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.07 _diffrn_reflns_number 3472 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0837 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 21.25 _reflns_number_total 2703 _reflns_number_observed 1711 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'SIR92' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.1440P)^2^+14.0219P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2702 _refine_ls_number_parameters 320 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1383 _refine_ls_R_factor_obs 0.0868 _refine_ls_wR_factor_all 0.2740 _refine_ls_wR_factor_obs 0.2260 _refine_ls_goodness_of_fit_all 1.049 _refine_ls_goodness_of_fit_obs 1.120 _refine_ls_restrained_S_all 1.050 _refine_ls_restrained_S_obs 1.118 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe Fe 0.98192(13) 0.38254(12) 0.45129(12) 0.0379(6) Uani 1 d . . O1 O 1.0000 0.5000 0.5000 0.047(3) Uani 1 d S . OW1 O 0.9710(7) 0.2378(7) 0.4681(8) 0.067(3) Uani 1 d D . HW1A H 0.9163 0.2177 0.4324 0.080 Uiso 1 d D . HW1B H 1.0150 0.2006 0.4586 0.080 Uiso 1 d D . N1 N 1.1495(8) 0.3547(7) 0.5233(8) 0.045(3) Uani 1 d . . N2 N 1.0576(8) 0.3753(7) 0.3336(8) 0.045(3) Uani 1 d . . N3 N 0.8593(8) 0.3977(7) 0.3162(7) 0.040(3) Uani 1 d . . N4 N 0.8334(8) 0.3793(7) 0.4957(8) 0.043(3) Uani 1 d . . C1 C 1.1893(11) 0.3490(10) 0.6229(11) 0.057(4) Uani 1 d . . H1 H 1.1438(11) 0.3529(10) 0.6643(11) 0.068 Uiso 1 calc R . C2 C 1.2984(12) 0.3372(10) 0.6666(12) 0.065(4) Uani 1 d . . H2 H 1.3260(12) 0.3357(10) 0.7361(12) 0.078 Uiso 1 calc R . C3 C 1.3617(12) 0.3281(11) 0.6050(15) 0.072(5) Uani 1 d . . H3 H 1.4340(12) 0.3185(11) 0.6326(15) 0.086 Uiso 1 calc R . C4 C 1.3215(12) 0.3326(10) 0.4998(15) 0.068(5) Uani 1 d . . H4 H 1.3654(12) 0.3258(10) 0.4571(15) 0.082 Uiso 1 calc R . C5 C 1.2149(10) 0.3474(9) 0.4633(11) 0.053(4) Uani 1 d . . C6 C 1.1623(11) 0.3594(9) 0.3550(10) 0.049(4) Uani 1 d . . C7 C 1.2111(13) 0.3538(11) 0.2794(13) 0.071(5) Uani 1 d . . H7 H 1.2835(13) 0.3417(11) 0.2931(13) 0.085 Uiso 1 calc R . C8 C 1.1500(16) 0.3666(13) 0.1817(13) 0.079(5) Uani 1 d . . H8 H 1.1826(16) 0.3651(13) 0.1294(13) 0.095 Uiso 1 calc R . C9 C 1.0467(14) 0.3810(11) 0.1604(11) 0.062(4) Uani 1 d . . H9 H 1.0068(14) 0.3871(11) 0.0939(11) 0.075 Uiso 1 calc R . C10 C 0.9994(12) 0.3867(9) 0.2367(10) 0.051(4) Uani 1 d . . C11 C 0.8856(11) 0.4026(8) 0.2268(9) 0.044(3) Uani 1 d . . C12 C 0.8059(14) 0.4133(10) 0.1375(10) 0.061(4) Uani 1 d . . H12 H 0.8221(14) 0.4151(10) 0.0758(10) 0.073 Uiso 1 calc R . C13 C 0.7003(13) 0.4212(11) 0.1429(11) 0.068(4) Uani 1 d . . H13 H 0.6464(13) 0.4301(11) 0.0839(11) 0.082 Uiso 1 calc R . C14 C 0.6757(11) 0.4161(10) 0.2314(10) 0.056(4) Uani 1 d . . H14 H 0.6054(11) 0.4195(10) 0.2337(10) 0.067 Uiso 1 calc R . C15 C 0.7566(10) 0.4057(9) 0.3191(9) 0.044(3) Uani 1 d . . C16 C 0.7451(10) 0.4005(9) 0.4237(10) 0.044(3) Uani 1 d . . C17 C 0.6489(11) 0.4171(10) 0.4480(12) 0.060(4) Uani 1 d . . H17 H 0.5874(11) 0.4309(10) 0.3978(12) 0.072 Uiso 1 calc R . C18 C 0.6473(12) 0.4128(11) 0.5461(12) 0.066(4) Uani 1 d . . H18 H 0.5849(12) 0.4260(11) 0.5636(12) 0.079 Uiso 1 calc R . C19 C 0.7347(13) 0.3899(12) 0.6172(12) 0.070(4) Uani 1 d . . H19 H 0.7331(13) 0.3852(12) 0.6841(12) 0.084 Uiso 1 calc R . C20 C 0.8286(12) 0.3730(11) 0.5904(10) 0.059(4) Uani 1 d . . H20 H 0.8895(12) 0.3569(11) 0.6403(10) 0.071 Uiso 1 calc R . OW2 O 0.8087(11) 0.1454(10) 0.4892(14) 0.142(6) Uani 1 d D . HW2A H 0.8322 0.1002 0.5207 0.170 Uiso 1 d D . HW2B H 0.7553 0.1321 0.4444 0.170 Uiso 1 d D . Cl1 Cl 1.0985(3) 0.0594(3) 0.3381(2) 0.0548(10) Uani 1 d . . O2 O 1.0859(18) 0.1549(11) 0.3249(15) 0.171(8) Uani 1 d . . O3 O 1.0645(10) 0.0144(11) 0.2429(9) 0.107(4) Uani 1 d . . O4 O 1.2040(11) 0.0375(17) 0.3828(12) 0.170(8) Uani 1 d . . O5 O 1.0344(12) 0.0297(13) 0.3999(9) 0.136(6) Uani 1 d . . Cl2 Cl 0.5215(4) 0.1781(3) 0.3541(3) 0.0824(14) Uani 1 d . . O9 O 0.4725(17) 0.2623(16) 0.3038(16) 0.174(7) Uiso 1 d . . O8 O 0.4409(36) 0.1183(31) 0.3697(30) 0.338(20) Uiso 1 d . . O7 O 0.5360(21) 0.1119(19) 0.2889(21) 0.217(10) Uiso 1 d . . O6 O 0.5713(23) 0.1963(21) 0.4472(22) 0.239(11) Uiso 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 Fe 0.0393(11) 0.0409(11) 0.0364(10) -0.0049(8) 0.0150(8) 0.0011(9) O1 0.055(8) 0.043(8) 0.047(7) -0.011(6) 0.022(6) 0.005(6) OW1 0.057(6) 0.045(6) 0.104(8) 0.003(5) 0.030(6) 0.001(5) N1 0.047(6) 0.035(6) 0.052(7) -0.012(5) 0.015(6) 0.005(5) N2 0.053(7) 0.039(6) 0.057(7) -0.011(5) 0.037(6) -0.001(5) N3 0.055(7) 0.034(6) 0.031(6) 0.000(4) 0.012(5) 0.000(5) N4 0.034(6) 0.051(7) 0.048(7) -0.004(5) 0.017(5) 0.010(5) C1 0.054(9) 0.052(9) 0.061(10) -0.005(7) 0.009(8) 0.004(7) C2 0.049(9) 0.058(10) 0.074(10) 0.008(8) -0.006(9) 0.008(8) C3 0.032(8) 0.069(11) 0.111(15) 0.005(10) 0.013(10) 0.008(8) C4 0.047(10) 0.047(9) 0.116(15) -0.008(9) 0.033(10) 0.003(7) C5 0.040(8) 0.040(8) 0.087(11) -0.015(7) 0.034(8) -0.005(6) C6 0.057(9) 0.041(8) 0.061(9) -0.022(7) 0.037(8) -0.004(7) C7 0.069(10) 0.077(11) 0.086(12) -0.023(9) 0.053(10) -0.013(9) C8 0.098(15) 0.087(13) 0.069(12) -0.001(9) 0.049(11) -0.027(11) C9 0.078(12) 0.063(10) 0.054(9) -0.007(8) 0.032(9) 0.000(9) C10 0.085(11) 0.043(8) 0.037(8) -0.013(6) 0.036(8) 0.004(8) C11 0.059(9) 0.035(7) 0.037(8) -0.002(6) 0.007(7) 0.002(6) C12 0.100(13) 0.046(9) 0.037(8) -0.002(6) 0.018(8) -0.008(8) C13 0.064(11) 0.077(11) 0.050(10) -0.006(8) -0.007(8) 0.012(8) C14 0.047(9) 0.059(9) 0.054(9) 0.005(7) 0.001(7) 0.003(7) C15 0.043(8) 0.040(8) 0.048(8) -0.005(6) 0.009(7) 0.003(6) C16 0.043(8) 0.034(7) 0.062(9) -0.008(6) 0.025(7) 0.003(6) C17 0.050(9) 0.044(9) 0.080(11) -0.006(7) 0.011(8) 0.007(7) C18 0.052(10) 0.085(12) 0.074(11) -0.013(9) 0.041(9) -0.007(8) C19 0.070(11) 0.086(12) 0.064(10) 0.005(9) 0.038(10) -0.002(9) C20 0.061(9) 0.077(11) 0.045(9) 0.002(8) 0.023(7) 0.007(8) OW2 0.089(9) 0.094(10) 0.248(19) 0.061(11) 0.056(11) -0.012(8) Cl1 0.056(2) 0.062(2) 0.048(2) -0.007(2) 0.016(2) -0.001(2) O2 0.239(22) 0.061(10) 0.212(19) 0.000(11) 0.058(17) -0.004(11) O3 0.107(10) 0.139(12) 0.080(8) -0.025(8) 0.036(7) -0.026(9) O4 0.062(9) 0.314(26) 0.117(11) -0.036(14) -0.004(8) 0.044(12) O5 0.127(12) 0.222(18) 0.076(8) -0.014(10) 0.055(8) -0.078(12) Cl2 0.100(3) 0.078(3) 0.058(2) -0.013(2) 0.002(2) -0.004(3) _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 Fe O1 1.773(2) . ? Fe OW1 2.056(9) . ? Fe N2 2.117(9) . ? Fe N3 2.117(9) . ? Fe N1 2.186(10) . ? Fe N4 2.188(9) . ? O1 Fe 1.773(2) 3_766 ? N1 C1 1.33(2) . ? N1 C5 1.34(2) . ? N2 C6 1.34(2) . ? N2 C10 1.36(2) . ? N3 C15 1.36(2) . ? N3 C11 1.37(2) . ? N4 C20 1.33(2) . ? N4 C16 1.34(2) . ? C1 C2 1.40(2) . ? C2 C3 1.34(2) . ? C3 C4 1.40(2) . ? C4 C5 1.37(2) . ? C5 C6 1.48(2) . ? C6 C7 1.36(2) . ? C7 C8 1.38(2) . ? C8 C9 1.32(2) . ? C9 C10 1.36(2) . ? C10 C11 1.47(2) . ? C11 C12 1.39(2) . ? C12 C13 1.41(2) . ? C13 C14 1.34(2) . ? C14 C15 1.38(2) . ? C15 C16 1.49(2) . ? C16 C17 1.40(2) . ? C17 C18 1.36(2) . ? C18 C19 1.33(2) . ? C19 C20 1.39(2) . ? Cl1 O2 1.36(2) . ? Cl1 O4 1.387(14) . ? Cl1 O5 1.408(12) . ? Cl1 O3 1.417(12) . ? Cl2 O6 1.30(3) . ? Cl2 O7 1.34(3) . ? Cl2 O8 1.41(5) . ? Cl2 O9 1.43(2) . ? 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 O1 Fe OW1 152.1(3) . . ? O1 Fe N2 107.0(3) . . ? OW1 Fe N2 95.7(4) . . ? O1 Fe N3 103.4(3) . . ? OW1 Fe N3 98.0(4) . . ? N2 Fe N3 74.4(4) . . ? O1 Fe N1 88.8(3) . . ? OW1 Fe N1 82.1(4) . . ? N2 Fe N1 73.8(4) . . ? N3 Fe N1 148.1(4) . . ? O1 Fe N4 87.2(3) . . ? OW1 Fe N4 81.6(4) . . ? N2 Fe N4 147.8(4) . . ? N3 Fe N4 74.2(4) . . ? N1 Fe N4 136.6(4) . . ? Fe O1 Fe 180.0 . 3_766 ? C1 N1 C5 119.5(12) . . ? C1 N1 Fe 123.1(9) . . ? C5 N1 Fe 117.4(9) . . ? C6 N2 C10 120.6(10) . . ? C6 N2 Fe 119.9(9) . . ? C10 N2 Fe 119.5(8) . . ? C15 N3 C11 120.7(10) . . ? C15 N3 Fe 120.3(8) . . ? C11 N3 Fe 118.9(8) . . ? C20 N4 C16 119.1(11) . . ? C20 N4 Fe 123.8(9) . . ? C16 N4 Fe 116.2(8) . . ? N1 C1 C2 121.4(14) . . ? C3 C2 C1 118.0(15) . . ? C2 C3 C4 121.7(14) . . ? C5 C4 C3 116.7(15) . . ? N1 C5 C4 122.7(14) . . ? N1 C5 C6 114.4(11) . . ? C4 C5 C6 122.9(13) . . ? N2 C6 C7 120.1(14) . . ? N2 C6 C5 114.5(10) . . ? C7 C6 C5 125.4(14) . . ? C6 C7 C8 118.1(15) . . ? C9 C8 C7 121.8(15) . . ? C8 C9 C10 119.3(15) . . ? N2 C10 C9 120.1(14) . . ? N2 C10 C11 113.3(10) . . ? C9 C10 C11 126.5(14) . . ? N3 C11 C12 119.6(12) . . ? N3 C11 C10 113.6(11) . . ? C12 C11 C10 126.6(12) . . ? C11 C12 C13 118.4(13) . . ? C14 C13 C12 121.3(13) . . ? C13 C14 C15 119.0(14) . . ? N3 C15 C14 120.9(12) . . ? N3 C15 C16 112.4(10) . . ? C14 C15 C16 126.7(12) . . ? N4 C16 C17 120.6(12) . . ? N4 C16 C15 115.9(10) . . ? C17 C16 C15 123.5(12) . . ? C18 C17 C16 118.9(13) . . ? C19 C18 C17 120.3(13) . . ? C18 C19 C20 119.3(14) . . ? N4 C20 C19 121.7(14) . . ? O2 Cl1 O4 110.4(13) . . ? O2 Cl1 O5 107.7(12) . . ? O4 Cl1 O5 110.4(11) . . ? O2 Cl1 O3 108.6(11) . . ? O4 Cl1 O3 109.9(9) . . ? O5 Cl1 O3 109.7(8) . . ? O6 Cl2 O7 132.4(18) . . ? O6 Cl2 O8 99.5(20) . . ? O7 Cl2 O8 86.2(20) . . ? O6 Cl2 O9 110.9(16) . . ? O7 Cl2 O9 111.9(14) . . ? O8 Cl2 O9 108.0(19) . . ? _refine_diff_density_max 1.683 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.117 #=END data_1M-LT _audit_creation_method SHELXL _chemical_name_systematic ; bis-2,2':6',2'':6'',2''-quaterpyridine-bis-aquo-\m-oxo-diiron(III) perchlorate dihydrate ; _chemical_name_common ? _chemical_formula_moiety '[(Fe(C20H14N4)(H2O))2(\m-O)](ClO4)4.2H2O' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C40 H36 Cl4 Fe2 N8 O21' _chemical_formula_weight 1218.27 _chemical_melting_point ? _chemical_compound_source ? 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' '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 12.912(2) _cell_length_b 13.913(4) _cell_length_c 13.545(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.360(10) _cell_angle_gamma 90.00 _cell_volume 2346.4(8) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 21 _cell_measurement_theta_min 9.62 _cell_measurement_theta_max 9.96 _exptl_crystal_description 'prism' _exptl_crystal_colour 'ruby-red' _exptl_crystal_size_max '0.31 mm' _exptl_crystal_size_mid '0.20 mm' _exptl_crystal_size_min '0.14 mm' _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.724 _exptl_crystal_density_method ? _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.939 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.6871 _exptl_absorpt_correction_T_max 0.7076 _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.1 _diffrn_reflns_number 5145 _diffrn_reflns_av_R_equivalents 0.0522 _diffrn_reflns_av_sigmaI/netI 0.1217 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4129 _reflns_number_observed 2551 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution ? _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0469P)^2^+2.4163P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4129 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1263 _refine_ls_R_factor_obs 0.0634 _refine_ls_wR_factor_all 0.1436 _refine_ls_wR_factor_obs 0.1166 _refine_ls_goodness_of_fit_all 1.034 _refine_ls_goodness_of_fit_obs 1.095 _refine_ls_restrained_S_all 1.034 _refine_ls_restrained_S_obs 1.095 _refine_ls_shift/esd_max -0.008 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe Fe 0.98745(8) 0.37955(7) 0.45501(6) 0.0138(2) Uani 1 d . . O1 O 1.0000 0.5000 0.5000 0.021(2) Uani 1 d S . OW1 O 0.9841(5) 0.2323(4) 0.4714(4) 0.0222(12) Uani 1 d . . HW1A H 0.9329(61) 0.2159(55) 0.4573(55) 0.017(25) Uiso 1 d . . HW1B H 1.0324(95) 0.1887(85) 0.4337(81) 0.109(43) Uiso 1 d . . N1 N 1.1583(4) 0.3572(4) 0.5308(4) 0.0180(13) Uani 1 d . . N2 N 1.0656(4) 0.3718(4) 0.3360(4) 0.0148(11) Uani 1 d . . N3 N 0.8646(4) 0.3890(4) 0.3166(3) 0.0122(11) Uani 1 d . . N4 N 0.8359(4) 0.3734(4) 0.4987(4) 0.0159(12) Uani 1 d . . C1 C 1.1995(6) 0.3579(5) 0.6335(5) 0.022(2) Uani 1 d . . H1 H 1.1534(6) 0.3652(5) 0.6753(5) 0.027 Uiso 1 calc R . C2 C 1.3084(6) 0.3479(5) 0.6781(5) 0.021(2) Uani 1 d . . H2 H 1.3352(6) 0.3489(5) 0.7490(5) 0.025 Uiso 1 calc R . C3 C 1.3768(6) 0.3366(5) 0.6163(5) 0.023(2) Uani 1 d . . H3 H 1.4501(6) 0.3288(5) 0.6451(5) 0.028 Uiso 1 calc R . C4 C 1.3358(5) 0.3370(5) 0.5110(5) 0.0185(15) Uani 1 d . . H4 H 1.3808(5) 0.3292(5) 0.4681(5) 0.022 Uiso 1 calc R . C5 C 1.2252(5) 0.3493(4) 0.4705(5) 0.0177(15) Uani 1 d . . C6 C 1.1724(5) 0.3568(4) 0.3593(5) 0.0169(15) Uani 1 d . . C7 C 1.2251(6) 0.3503(5) 0.2826(5) 0.023(2) Uani 1 d . . H7 H 1.2988(6) 0.3397(5) 0.2986(5) 0.027 Uiso 1 calc R . C8 C 1.1661(6) 0.3598(5) 0.1820(5) 0.026(2) Uani 1 d . . H8 H 1.2003(6) 0.3556(5) 0.1298(5) 0.031 Uiso 1 calc R . C9 C 1.0565(5) 0.3754(5) 0.1582(5) 0.0198(15) Uani 1 d . . H9 H 1.0163(5) 0.3823(5) 0.0906(5) 0.024 Uiso 1 calc R . C10 C 1.0082(5) 0.3806(5) 0.2385(4) 0.0147(13) Uani 1 d . . C11 C 0.8904(5) 0.3921(5) 0.2268(4) 0.0162(14) Uani 1 d . . C12 C 0.8127(5) 0.4021(4) 0.1345(5) 0.0191(15) Uani 1 d . . H12 H 0.8313(5) 0.4063(4) 0.0728(5) 0.023 Uiso 1 calc R . C13 C 0.7065(6) 0.4055(5) 0.1377(5) 0.022(2) Uani 1 d . . H13 H 0.6527(6) 0.4106(5) 0.0768(5) 0.026 Uiso 1 calc R . C14 C 0.6788(5) 0.4015(5) 0.2288(5) 0.0197(15) Uani 1 d . . H14 H 0.6072(5) 0.4033(5) 0.2302(5) 0.024 Uiso 1 calc R . C15 C 0.7611(5) 0.3947(4) 0.3190(4) 0.0152(14) Uani 1 d . . C16 C 0.7459(5) 0.3936(5) 0.4235(5) 0.0160(14) Uani 1 d . . C17 C 0.6506(6) 0.4136(5) 0.4469(5) 0.020(2) Uani 1 d . . H17 H 0.5891(6) 0.4270(5) 0.3949(5) 0.024 Uiso 1 calc R . C18 C 0.6464(6) 0.4135(5) 0.5482(5) 0.022(2) Uani 1 d . . H18 H 0.5829(6) 0.4289(5) 0.5647(5) 0.026 Uiso 1 calc R . C19 C 0.7376(6) 0.3905(5) 0.6241(5) 0.027(2) Uani 1 d . . H19 H 0.7362(6) 0.3886(5) 0.6924(5) 0.033 Uiso 1 calc R . C20 C 0.8310(6) 0.3702(5) 0.5965(5) 0.025(2) Uani 1 d . . H20 H 0.8925(6) 0.3539(5) 0.6472(5) 0.030 Uiso 1 calc R . OW2 O 0.8090(6) 0.1331(4) 0.4502(5) 0.040(2) Uani 1 d . . HW2A H 0.7471(71) 0.1367(63) 0.4365(61) 0.037(28) Uiso 1 d . . HW2B H 0.8314(74) 0.0857(69) 0.4922(66) 0.055(30) Uiso 1 d . . Cl1 Cl 1.09673(13) 0.04716(11) 0.34095(11) 0.0185(4) Uani 1 d . . O2 O 1.0865(5) 0.1502(3) 0.3311(4) 0.0373(14) Uani 1 d . . O3 O 1.0660(4) 0.0041(4) 0.2414(3) 0.0272(12) Uani 1 d . . O4 O 1.0286(5) 0.0131(4) 0.4019(4) 0.045(2) Uani 1 d . . O5 O 1.2050(4) 0.0231(4) 0.3922(4) 0.045(2) Uani 1 d . . Cl2 Cl 0.51199(14) 0.17285(12) 0.36028(12) 0.0228(4) Uani 1 d . . O6 O 0.6014(4) 0.1920(4) 0.4482(3) 0.0334(13) Uani 1 d . . O7 O 0.5439(4) 0.1046(4) 0.2942(3) 0.0351(13) Uani 1 d . . O8 O 0.4244(5) 0.1338(5) 0.3958(4) 0.056(2) Uani 1 d . . O9 O 0.4787(5) 0.2602(4) 0.3047(4) 0.044(2) 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 Fe 0.0131(5) 0.0158(5) 0.0126(4) -0.0023(4) 0.0035(4) 0.0018(4) O1 0.024(4) 0.020(4) 0.021(3) -0.003(3) 0.008(3) 0.003(3) OW1 0.016(3) 0.019(3) 0.030(3) -0.002(2) 0.004(3) 0.000(3) N1 0.024(3) 0.014(3) 0.017(3) -0.003(2) 0.008(2) 0.001(3) N2 0.013(3) 0.011(3) 0.022(3) -0.001(2) 0.008(2) -0.001(2) N3 0.010(3) 0.014(3) 0.012(2) 0.001(2) 0.002(2) 0.003(2) N4 0.017(3) 0.013(3) 0.018(3) -0.002(2) 0.006(2) -0.001(3) C1 0.027(4) 0.018(4) 0.021(3) 0.005(3) 0.004(3) 0.000(3) C2 0.024(4) 0.020(4) 0.016(3) 0.001(3) -0.002(3) 0.000(3) C3 0.015(4) 0.020(4) 0.032(4) 0.003(3) 0.002(3) 0.001(3) C4 0.017(4) 0.014(3) 0.027(3) -0.006(3) 0.010(3) -0.001(3) C5 0.020(4) 0.014(3) 0.019(3) -0.001(3) 0.006(3) -0.003(3) C6 0.014(3) 0.015(3) 0.022(3) 0.001(3) 0.005(3) -0.004(3) C7 0.017(4) 0.025(4) 0.026(4) -0.006(3) 0.006(3) 0.003(3) C8 0.027(4) 0.031(4) 0.024(3) -0.001(3) 0.015(3) -0.002(4) C9 0.026(4) 0.021(3) 0.015(3) -0.003(3) 0.009(3) -0.004(3) C10 0.018(3) 0.015(3) 0.011(3) -0.001(3) 0.004(3) -0.006(3) C11 0.022(4) 0.012(3) 0.013(3) 0.000(3) 0.004(3) -0.004(3) C12 0.027(4) 0.015(3) 0.018(3) 0.004(3) 0.011(3) 0.000(3) C13 0.024(4) 0.018(4) 0.021(3) 0.000(3) 0.001(3) 0.001(3) C14 0.014(3) 0.026(4) 0.021(3) 0.001(3) 0.008(3) 0.002(3) C15 0.016(3) 0.011(3) 0.018(3) 0.001(3) 0.004(3) 0.000(3) C16 0.016(4) 0.013(3) 0.019(3) -0.002(3) 0.006(3) -0.003(3) C17 0.017(4) 0.023(4) 0.020(3) 0.001(3) 0.002(3) -0.009(3) C18 0.016(4) 0.025(4) 0.027(4) -0.002(3) 0.012(3) 0.003(3) C19 0.032(4) 0.029(4) 0.025(3) -0.001(3) 0.013(3) 0.000(4) C20 0.027(4) 0.034(4) 0.013(3) -0.002(3) 0.004(3) 0.002(4) OW2 0.028(4) 0.030(3) 0.058(4) 0.015(3) 0.005(3) -0.005(3) Cl1 0.0181(9) 0.0205(8) 0.0175(8) -0.0016(7) 0.0060(7) -0.0009(7) O2 0.053(4) 0.016(3) 0.042(3) 0.000(2) 0.010(3) 0.001(3) O3 0.029(3) 0.035(3) 0.018(2) -0.009(2) 0.006(2) -0.002(3) O4 0.060(4) 0.057(4) 0.029(3) -0.010(3) 0.029(3) -0.030(3) O5 0.025(3) 0.060(4) 0.041(3) -0.012(3) -0.009(3) 0.011(3) Cl2 0.0220(9) 0.0255(9) 0.0202(8) -0.0044(7) 0.0043(7) 0.0009(8) O6 0.032(3) 0.042(3) 0.023(2) 0.000(2) 0.003(2) -0.003(3) O7 0.042(3) 0.039(3) 0.027(2) -0.006(2) 0.013(2) 0.010(3) O8 0.039(4) 0.084(5) 0.053(4) -0.010(4) 0.026(3) -0.024(4) O9 0.043(4) 0.033(3) 0.047(3) 0.006(3) -0.005(3) 0.004(3) _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 Fe O1 1.7758(10) . ? Fe OW1 2.063(5) . ? Fe N3 2.115(5) . ? Fe N2 2.118(5) . ? Fe N4 2.191(5) . ? Fe N1 2.194(6) . ? O1 Fe 1.7758(10) 3_766 ? N1 C5 1.342(8) . ? N1 C1 1.351(8) . ? N2 C10 1.338(7) . ? N2 C6 1.347(8) . ? N3 C11 1.344(7) . ? N3 C15 1.348(8) . ? N4 C20 1.343(8) . ? N4 C16 1.356(8) . ? C1 C2 1.383(10) . ? C2 C3 1.377(10) . ? C3 C4 1.384(9) . ? C4 C5 1.399(9) . ? C5 C6 1.484(8) . ? C6 C7 1.389(9) . ? C7 C8 1.380(9) . ? C8 C9 1.383(10) . ? C9 C10 1.392(8) . ? C10 C11 1.496(9) . ? C11 C12 1.387(9) . ? C12 C13 1.384(10) . ? C13 C14 1.374(9) . ? C14 C15 1.394(8) . ? C15 C16 1.480(8) . ? C16 C17 1.379(9) . ? C17 C18 1.387(9) . ? C18 C19 1.380(9) . ? C19 C20 1.384(10) . ? Cl1 O5 1.426(5) . ? Cl1 O3 1.432(4) . ? Cl1 O4 1.437(5) . ? Cl1 O2 1.443(5) . ? Cl2 O9 1.434(5) . ? Cl2 O7 1.438(5) . ? Cl2 O8 1.447(6) . ? Cl2 O6 1.447(5) . ? 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 O1 Fe OW1 154.6(2) . . ? O1 Fe N3 102.98(15) . . ? OW1 Fe N3 97.1(2) . . ? O1 Fe N2 106.91(15) . . ? OW1 Fe N2 93.4(2) . . ? N3 Fe N2 74.0(2) . . ? O1 Fe N4 87.19(14) . . ? OW1 Fe N4 83.5(2) . . ? N3 Fe N4 74.2(2) . . ? N2 Fe N4 147.4(2) . . ? O1 Fe N1 89.07(14) . . ? OW1 Fe N1 81.8(2) . . ? N3 Fe N1 148.0(2) . . ? N2 Fe N1 74.1(2) . . ? N4 Fe N1 136.6(2) . . ? Fe O1 Fe 180.0 . 3_766 ? C5 N1 C1 119.0(6) . . ? C5 N1 Fe 117.1(4) . . ? C1 N1 Fe 123.7(5) . . ? C10 N2 C6 120.7(5) . . ? C10 N2 Fe 119.7(4) . . ? C6 N2 Fe 119.6(4) . . ? C11 N3 C15 120.3(5) . . ? C11 N3 Fe 119.8(4) . . ? C15 N3 Fe 119.9(4) . . ? C20 N4 C16 119.5(6) . . ? C20 N4 Fe 123.1(4) . . ? C16 N4 Fe 116.0(4) . . ? N1 C1 C2 121.8(6) . . ? C3 C2 C1 119.1(6) . . ? C2 C3 C4 119.7(6) . . ? C3 C4 C5 118.4(6) . . ? N1 C5 C4 121.8(6) . . ? N1 C5 C6 114.5(6) . . ? C4 C5 C6 123.6(6) . . ? N2 C6 C7 120.7(6) . . ? N2 C6 C5 114.5(6) . . ? C7 C6 C5 124.8(6) . . ? C8 C7 C6 118.7(6) . . ? C7 C8 C9 120.6(6) . . ? C8 C9 C10 117.9(6) . . ? N2 C10 C9 121.4(6) . . ? N2 C10 C11 113.4(5) . . ? C9 C10 C11 125.1(5) . . ? N3 C11 C12 121.7(6) . . ? N3 C11 C10 112.9(5) . . ? C12 C11 C10 125.4(6) . . ? C13 C12 C11 117.5(6) . . ? C14 C13 C12 121.5(6) . . ? C13 C14 C15 118.0(6) . . ? N3 C15 C14 120.9(6) . . ? N3 C15 C16 113.9(5) . . ? C14 C15 C16 125.1(6) . . ? N4 C16 C17 120.6(6) . . ? N4 C16 C15 114.6(5) . . ? C17 C16 C15 124.8(6) . . ? C16 C17 C18 119.9(6) . . ? C19 C18 C17 119.2(6) . . ? C18 C19 C20 118.6(6) . . ? N4 C20 C19 122.1(6) . . ? O5 Cl1 O3 110.6(3) . . ? O5 Cl1 O4 108.3(3) . . ? O3 Cl1 O4 110.1(3) . . ? O5 Cl1 O2 109.4(4) . . ? O3 Cl1 O2 109.4(3) . . ? O4 Cl1 O2 109.0(4) . . ? O9 Cl2 O7 109.1(3) . . ? O9 Cl2 O8 110.0(4) . . ? O7 Cl2 O8 109.7(4) . . ? O9 Cl2 O6 109.8(3) . . ? O7 Cl2 O6 109.6(3) . . ? O8 Cl2 O6 108.6(3) . . ? _refine_diff_density_max 0.541 _refine_diff_density_min -0.502 _refine_diff_density_rms 0.108 #=END data_1O-RT _audit_creation_method SHELXL _chemical_name_systematic ; bis-2,2':6',2'':6'',2''-quaterpyridine-bis-aquo-\m-oxo-diiron(III) perchlorate dihydrate ; _chemical_name_common ? _chemical_formula_moiety '[(Fe(C20H14N4)(H2O))2(\m-O)](ClO4)4.2H2O' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C40 H36 Cl4 Fe2 N8 O21' _chemical_formula_weight 1218.27 _chemical_melting_point ? _chemical_compound_source ? 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' '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 'Orthorhombic' _symmetry_space_group_name_H-M 'Pbca ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.175(2) _cell_length_b 16.4630(10) _cell_length_c 20.949(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4888.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 31 _cell_measurement_theta_min 5.00 _cell_measurement_theta_max 12.28 _exptl_crystal_description 'prism' _exptl_crystal_colour 'ruby-red' _exptl_crystal_size_max '0.44 mm' _exptl_crystal_size_mid '0.32 mm' _exptl_crystal_size_min '0.12 mm' _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.655 _exptl_crystal_density_method ? _exptl_crystal_F_000 2480 _exptl_absorpt_coefficient_mu 0.901 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.8078 _exptl_absorpt_correction_T_max 0.8346 _exptl_crystal_face_index_h ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.1 _diffrn_reflns_number 3995 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0782 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 22.50 _reflns_number_total 3189 _reflns_number_observed 1673 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.2489P)^2^+4.9688P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3189 _refine_ls_number_parameters 297 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1770 _refine_ls_R_factor_obs 0.1069 _refine_ls_wR_factor_all 0.3759 _refine_ls_wR_factor_obs 0.2976 _refine_ls_goodness_of_fit_all 1.010 _refine_ls_goodness_of_fit_obs 1.120 _refine_ls_restrained_S_all 1.010 _refine_ls_restrained_S_obs 1.120 _refine_ls_shift/esd_max -0.012 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe Fe 0.38033(12) 0.02908(11) 0.50768(8) 0.0429(7) Uani 1 d . . O1 O 0.5000 0.0000 0.5000 0.049(3) Uani 1 d S . OW1 O 0.2379(7) 0.0190(8) 0.4848(5) 0.076(3) Uani 1 d . . HW1A H 0.2095 0.0238 0.4511 0.091 Uiso 1 d . . HW1B H 0.2143 0.0504 0.5139 0.091 Uiso 1 d . . N1 N 0.3844(8) 0.0686(8) 0.4088(5) 0.058(3) Uani 1 d . . N2 N 0.3906(7) 0.1568(7) 0.5104(5) 0.050(3) Uani 1 d . . N3 N 0.3667(8) 0.0607(7) 0.6053(5) 0.051(3) Uani 1 d . . N4 N 0.3529(7) -0.0845(7) 0.5589(5) 0.052(3) Uani 1 d . . C1 C 0.3842(12) 0.0176(11) 0.3587(7) 0.070(4) Uani 1 d . . H1 H 0.3718(12) -0.0370(11) 0.3662(7) 0.084 Uiso 1 calc R . C2 C 0.4010(15) 0.0418(14) 0.2975(9) 0.089(6) Uani 1 d . . H2 H 0.4010(15) 0.0049(14) 0.2638(9) 0.107 Uiso 1 calc R . C3 C 0.4173(16) 0.1204(16) 0.2880(9) 0.101(6) Uani 1 d . . H3 H 0.4275(16) 0.1389(16) 0.2466(9) 0.122 Uiso 1 calc R . C4 C 0.4197(12) 0.1755(12) 0.3381(8) 0.084(5) Uani 1 d . . H4 H 0.4322(12) 0.2301(12) 0.3304(8) 0.101 Uiso 1 calc R . C5 C 0.4034(9) 0.1489(9) 0.3980(7) 0.055(4) Uani 1 d . . C6 C 0.4035(10) 0.1985(9) 0.4557(8) 0.060(4) Uani 1 d . . C7 C 0.4149(11) 0.2818(11) 0.4577(9) 0.074(5) Uani 1 d . . H7 H 0.4203(11) 0.3113(11) 0.4201(9) 0.089 Uiso 1 calc R . C8 C 0.4183(12) 0.3214(11) 0.5167(11) 0.085(5) Uani 1 d . . H8 H 0.4305(12) 0.3768(11) 0.5188(11) 0.102 Uiso 1 calc R . C9 C 0.4036(13) 0.2778(11) 0.5711(11) 0.092(6) Uani 1 d . . H9 H 0.4014(13) 0.3043(11) 0.6103(11) 0.110 Uiso 1 calc R . C10 C 0.3918(10) 0.1944(10) 0.5686(8) 0.065(4) Uani 1 d . . C11 C 0.3761(11) 0.1408(12) 0.6222(7) 0.069(5) Uani 1 d . . C12 C 0.3690(12) 0.1614(13) 0.6859(9) 0.085(5) Uani 1 d . . H12 H 0.3739(12) 0.2154(13) 0.6985(9) 0.102 Uiso 1 calc R . C13 C 0.3544(14) 0.1005(16) 0.7312(9) 0.098(7) Uani 1 d . . H13 H 0.3492(14) 0.1143(16) 0.7741(9) 0.118 Uiso 1 calc R . C14 C 0.3478(13) 0.0208(15) 0.7133(8) 0.090(6) Uani 1 d . . H14 H 0.3400(13) -0.0197(15) 0.7439(8) 0.108 Uiso 1 calc R . C15 C 0.3530(9) 0.0010(10) 0.6482(7) 0.056(4) Uani 1 d . . C16 C 0.3462(9) -0.0795(10) 0.6210(7) 0.059(4) Uani 1 d . . C17 C 0.3377(11) -0.1501(13) 0.6604(8) 0.076(5) Uani 1 d . . H17 H 0.3325(11) -0.1455(13) 0.7045(8) 0.091 Uiso 1 calc R . C18 C 0.3376(13) -0.2238(13) 0.6318(12) 0.090(6) Uani 1 d . . H18 H 0.3342(13) -0.2711(13) 0.6559(12) 0.108 Uiso 1 calc R . C19 C 0.3425(12) -0.2275(10) 0.5653(10) 0.076(5) Uani 1 d . . H19 H 0.3413(12) -0.2771(10) 0.5441(10) 0.092 Uiso 1 calc R . C20 C 0.3493(7) -0.1554(7) 0.5321(5) 0.067(4) Uani 1 d . . H20 H 0.3514(7) -0.1579(7) 0.4877(5) 0.081 Uiso 1 calc R . OW2 O 0.1665(7) 0.0507(7) 0.3745(5) 0.103(4) Uani 1 d R . HW2A H 0.1673 0.1008 0.3811 0.123 Uiso 1 d . . HW2B H 0.1088 0.0367 0.3721 0.123 Uiso 1 d . . Cl1 Cl 0.0718(3) 0.0359(3) 0.6206(2) 0.0734(13) Uani 1 d . . O2 O 0.0645(20) 0.0392(17) 0.5544(14) 0.210(10) Uiso 1 d . . O3 O 0.0081(17) 0.0815(14) 0.6494(11) 0.188(9) Uiso 1 d . . O4 O 0.1523(24) 0.0706(21) 0.6363(17) 0.255(13) Uiso 1 d . . O5 O 0.0773(17) -0.0448(14) 0.6402(11) 0.182(8) Uiso 1 d . . Cl2 Cl 0.1495(4) 0.2689(4) 0.3342(3) 0.104(2) Uani 1 d . . O6 O 0.1739(21) 0.2228(19) 0.3973(15) 0.236(12) Uiso 1 d . . O7 O 0.0807(21) 0.2128(17) 0.3111(13) 0.224(10) Uiso 1 d . . O8 O 0.0996(18) 0.3180(17) 0.3689(13) 0.202(9) Uiso 1 d . . O9 O 0.2161(26) 0.2593(20) 0.2989(19) 0.293(17) Uiso 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 Fe 0.0406(12) 0.0510(12) 0.0372(11) 0.0008(9) 0.0031(8) 0.0035(9) O1 0.044(8) 0.059(8) 0.043(7) 0.013(6) 0.005(6) -0.001(6) OW1 0.053(6) 0.113(9) 0.062(6) 0.009(6) -0.010(5) -0.002(6) N1 0.054(7) 0.080(9) 0.040(6) 0.012(6) 0.002(5) 0.003(7) N2 0.043(6) 0.047(6) 0.061(7) 0.000(6) 0.004(5) 0.003(5) N3 0.051(7) 0.057(7) 0.046(6) -0.007(6) -0.002(5) 0.007(6) N4 0.038(6) 0.065(8) 0.053(7) 0.010(6) 0.006(5) -0.005(6) C1 0.082(11) 0.080(11) 0.048(9) -0.008(8) 0.013(8) 0.000(9) C2 0.101(15) 0.107(15) 0.059(11) -0.021(11) 0.000(9) 0.031(13) C3 0.112(16) 0.134(20) 0.059(11) 0.001(13) 0.000(10) 0.012(15) C4 0.083(12) 0.091(13) 0.077(12) 0.048(11) 0.004(9) 0.019(11) C5 0.042(8) 0.066(10) 0.056(9) 0.010(8) -0.001(6) 0.017(7) C6 0.052(9) 0.046(9) 0.083(11) 0.017(8) 0.004(7) 0.004(7) C7 0.062(10) 0.072(12) 0.089(12) 0.006(10) -0.009(9) 0.007(9) C8 0.070(11) 0.044(9) 0.140(18) -0.008(11) 0.003(12) 0.000(8) C9 0.085(13) 0.058(11) 0.133(18) -0.026(12) 0.020(12) -0.004(10) C10 0.047(9) 0.070(11) 0.079(11) -0.027(9) 0.001(8) -0.005(8) C11 0.061(10) 0.104(14) 0.042(8) -0.014(9) -0.008(7) 0.002(9) C12 0.076(12) 0.093(13) 0.086(13) -0.016(12) 0.004(10) 0.012(11) C13 0.087(14) 0.152(22) 0.055(10) -0.028(13) -0.013(9) 0.022(14) C14 0.072(11) 0.148(20) 0.050(10) 0.010(12) 0.009(8) -0.004(13) C15 0.036(8) 0.090(11) 0.042(8) 0.008(8) 0.002(6) 0.004(7) C16 0.033(7) 0.086(11) 0.058(9) 0.020(9) 0.013(6) 0.007(7) C17 0.048(9) 0.117(16) 0.064(10) 0.039(11) 0.006(8) 0.006(10) C18 0.065(11) 0.082(14) 0.125(18) 0.038(14) 0.003(12) -0.001(10) C19 0.067(10) 0.057(10) 0.105(14) 0.010(10) 0.006(10) -0.001(9) C20 0.047(9) 0.072(11) 0.083(11) 0.029(10) 0.010(8) -0.006(8) OW2 0.084(9) 0.116(11) 0.108(10) 0.015(9) -0.020(8) -0.007(8) Cl1 0.087(3) 0.072(3) 0.062(2) 0.003(2) 0.009(2) 0.006(2) Cl2 0.096(4) 0.095(4) 0.122(4) -0.019(3) 0.034(3) -0.006(3) _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 Fe O1 1.770(2) . ? Fe OW1 2.082(10) . ? Fe N2 2.109(11) . ? Fe N3 2.119(11) . ? Fe N1 2.172(11) . ? Fe N4 2.190(11) . ? O1 Fe 1.770(2) 5_656 ? N1 C1 1.34(2) . ? N1 C5 1.37(2) . ? N2 C6 1.35(2) . ? N2 C10 1.37(2) . ? N3 C15 1.35(2) . ? N3 C11 1.37(2) . ? N4 C20 1.30(2) . ? N4 C16 1.31(2) . ? C1 C2 1.36(3) . ? C2 C3 1.33(3) . ? C3 C4 1.39(3) . ? C4 C5 1.35(2) . ? C5 C6 1.46(2) . ? C6 C7 1.38(2) . ? C7 C8 1.40(2) . ? C8 C9 1.36(3) . ? C9 C10 1.38(2) . ? C10 C11 1.44(2) . ? C11 C12 1.38(2) . ? C12 C13 1.40(3) . ? C13 C14 1.37(3) . ? C14 C15 1.40(2) . ? C15 C16 1.44(2) . ? C16 C17 1.43(2) . ? C17 C18 1.35(3) . ? C18 C19 1.40(3) . ? C19 C20 1.38(2) . ? Cl1 O4 1.32(3) . ? Cl1 O3 1.32(2) . ? Cl1 O2 1.39(3) . ? Cl1 O5 1.39(2) . ? Cl2 O9 1.21(4) . ? Cl2 O8 1.30(3) . ? Cl2 O7 1.43(3) . ? Cl2 O6 1.56(3) . ? 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 O1 Fe OW1 152.5(4) . . ? O1 Fe N2 101.9(3) . . ? OW1 Fe N2 98.8(5) . . ? O1 Fe N3 104.0(3) . . ? OW1 Fe N3 98.8(4) . . ? N2 Fe N3 74.6(4) . . ? O1 Fe N1 88.2(3) . . ? OW1 Fe N1 80.2(4) . . ? N2 Fe N1 74.0(5) . . ? N3 Fe N1 148.1(5) . . ? O1 Fe N4 89.1(3) . . ? OW1 Fe N4 82.7(4) . . ? N2 Fe N4 148.2(4) . . ? N3 Fe N4 73.8(5) . . ? N1 Fe N4 136.7(5) . . ? Fe O1 Fe 180.0 5_656 . ? C1 N1 C5 118.4(12) . . ? C1 N1 Fe 123.9(11) . . ? C5 N1 Fe 116.9(10) . . ? C6 N2 C10 121.8(12) . . ? C6 N2 Fe 119.6(9) . . ? C10 N2 Fe 118.4(10) . . ? C15 N3 C11 122.9(12) . . ? C15 N3 Fe 118.6(10) . . ? C11 N3 Fe 118.5(10) . . ? C20 N4 C16 119.0(12) . . ? C20 N4 Fe 124.3(8) . . ? C16 N4 Fe 116.6(11) . . ? N1 C1 C2 123.5(17) . . ? C3 C2 C1 117.0(18) . . ? C2 C3 C4 121.9(19) . . ? C5 C4 C3 119.2(18) . . ? C4 C5 N1 120.1(15) . . ? C4 C5 C6 126.2(16) . . ? N1 C5 C6 113.8(12) . . ? N2 C6 C7 119.6(15) . . ? N2 C6 C5 114.9(12) . . ? C7 C6 C5 125.5(15) . . ? C6 C7 C8 119.6(17) . . ? C9 C8 C7 119.2(16) . . ? C8 C9 C10 120.6(19) . . ? N2 C10 C9 118.9(17) . . ? N2 C10 C11 114.5(13) . . ? C9 C10 C11 126.6(17) . . ? N3 C11 C12 118.6(17) . . ? N3 C11 C10 113.7(12) . . ? C12 C11 C10 127.7(18) . . ? C11 C12 C13 119.4(19) . . ? C14 C13 C12 120.9(17) . . ? C13 C14 C15 119.0(19) . . ? N3 C15 C14 119.1(17) . . ? N3 C15 C16 114.6(12) . . ? C14 C15 C16 126.3(16) . . ? N4 C16 C17 122.0(17) . . ? N4 C16 C15 116.4(14) . . ? C17 C16 C15 121.6(15) . . ? C18 C17 C16 118.2(16) . . ? C17 C18 C19 118.7(17) . . ? C20 C19 C18 118.1(17) . . ? N4 C20 C19 124.0(13) . . ? O4 Cl1 O3 103.4(18) . . ? O4 Cl1 O2 107.2(19) . . ? O3 Cl1 O2 112.5(16) . . ? O4 Cl1 O5 107.0(18) . . ? O3 Cl1 O5 116.6(15) . . ? O2 Cl1 O5 109.5(16) . . ? O9 Cl2 O8 148.2(21) . . ? O9 Cl2 O7 104.0(20) . . ? O8 Cl2 O7 102.8(17) . . ? O9 Cl2 O6 106.2(21) . . ? O8 Cl2 O6 87.1(16) . . ? O7 Cl2 O6 97.1(16) . . ? _refine_diff_density_max 1.199 _refine_diff_density_min -0.609 _refine_diff_density_rms 0.149 #=END