# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 #=================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Jun Tao' _publ_contact_author_address ; Department of Chemistry Xiamen University Xiamen 361005 P. R. China ; _publ_contact_author_email taojun@xmu.edu.cn _publ_contact_author_Phone 86-592-2185191 _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for publication as a Communnication paper in Chemical Communications ; # TITLE AND AUTHOR LIST _publ_section_title ; Pressure effects and M\"ossbauer spectroscopic studies on a 3D mixed-valence iron spin-crossover complex with NiAs topology ; loop_ _publ_author_name _publ_author_address 'Yue-Ling Bai.' ; Department of Chemistry Xiamen University Xiamen 361005 P. R. China ; 'Jun Tao.' ; Department of Chemistry Xiamen University Xiamen 361005 P. R. China ; 'Rong-Bin Huang.' ; Department of Chemistry Xiamen University Xiamen 361005 P. R. China ; 'Lan-Sun Zheng.' ; Department of Chemistry Xiamen University Xiamen 361005 P. R. China ; ; Shao-Liang Zheng ; ; Department of Chemistry University at Buffalo the State University of New York Buffalo New York ; K.Oshida ; Department of Chemistry Faculty of Science and Technology Keio University Yokohama 223-8522 Japan ; Y.Einaga ; Department of Chemistry Faculty of Science and Technology Keio University Yokohama 223-8522 Japan ; #====================================================================== data_90K _database_code_depnum_ccdc_archive 'CCDC 668963' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H17 Cl Fe2 N12.5 O15' _chemical_formula_weight 699.47 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 Hexagonal _symmetry_space_group_name_H-M P63/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 10.7052(2) _cell_length_b 10.7052(2) _cell_length_c 22.9656(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2279.28(9) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 442 _cell_measurement_theta_min 4 _cell_measurement_theta_max 25 _exptl_crystal_description needle _exptl_crystal_colour 'orange red' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.913 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 1.484 _exptl_absorpt_correction_type 'empirical SADABS' _exptl_absorpt_correction_T_min 0.8122 _exptl_absorpt_correction_T_max 0.9150 _exptl_absorpt_process_details 'Blessing, R. (1995) Acta Crystallogr., A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13958 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0170 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 28.99 _reflns_number_total 2082 _reflns_number_gt 1826 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution SHELXS-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _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. Because of the disorder of water molecules and the Fe2 atom, restraints were used when refine. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0642P)^2^+4.9263P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2082 _refine_ls_number_parameters 140 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0526 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1333 _refine_ls_wR_factor_gt 0.1274 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.0000 1.0000 0.5000 0.0163(2) Uani 1 6 d S . . Fe2 Fe 0.73872(6) 1.53481(7) 0.2500 0.01573(19) Uani 0.8817(16) 2 d SP . 1 Fe2B Fe 0.7674(5) 1.6169(6) 0.2500 0.01573(19) Uani 0.1183(16) 2 d SP . 2 O1 O 0.4174(2) 1.3051(2) 0.31327(9) 0.0279(5) Uani 1 1 d . . . O2 O 0.6067(3) 1.5306(2) 0.31297(10) 0.0315(5) Uani 1 1 d . . . O1H O 0.6667 1.3333 0.2500 0.0210(9) Uani 1 6 d S . . O1W O 0.8135(5) 1.7561(4) 0.2500 0.0530(11) Uani 1 2 d S . . H1WA H 0.7770 1.7911 0.2732 0.064 Uiso 0.50 1 d PR . . H1WB H 0.8803 1.8113 0.2268 0.064 Uiso 0.50 1 d PR . . N1 N 0.1267(2) 1.1728(2) 0.45054(10) 0.0199(5) Uani 1 1 d . . . N2 N 0.0743(3) 1.2492(3) 0.42253(13) 0.0309(6) Uani 1 1 d . . . N3 N 0.1788(3) 1.3596(3) 0.39682(13) 0.0316(6) Uani 1 1 d . . . N4 N 0.3004(3) 1.3562(3) 0.40815(10) 0.0213(5) Uani 1 1 d . . . C1 C 0.2671(3) 1.2415(3) 0.44091(12) 0.0212(5) Uani 1 1 d . . . H1A H 0.3330 1.2137 0.4550 0.025 Uiso 1 1 calc R . . C2 C 0.4395(3) 1.4703(3) 0.38768(13) 0.0246(6) Uani 1 1 d . . . H2A H 0.5119 1.4946 0.4189 0.030 Uiso 1 1 calc R . . H2B H 0.4326 1.5575 0.3796 0.030 Uiso 1 1 calc R . . C3 C 0.4909(3) 1.4298(3) 0.33321(12) 0.0221(5) Uani 1 1 d . . . Cl1 Cl 0.3333 0.6667 0.52853(6) 0.0267(3) Uani 1 3 d S . . O11 O 0.3333 0.6667 0.5917(2) 0.0440(11) Uani 1 3 d S . . O12 O 0.2045(3) 0.6622(3) 0.50993(13) 0.0402(6) Uani 1 1 d . . . O2W O 0.0000 1.0000 0.3212(4) 0.047(2) Uani 0.50 3 d SP . . O3W O -0.6667 0.6667 0.2995(6) 0.087(6) Uani 0.40 3 d SPU A 1 O4W O -0.678(6) 0.707(3) 0.2500 0.15(3) Uani 0.33 2 d SPU . 2 O5W O -0.823(2) 0.791(2) 0.2500 0.087(8) Uani 0.30 2 d SPU B 3 O6W O -0.810(4) 0.691(10) 0.2500 0.09(2) Uani 0.10 2 d SPU C 4 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 0.0140(3) 0.0140(3) 0.0208(4) 0.000 0.000 0.00701(14) Fe2 0.0177(3) 0.0185(4) 0.0113(3) 0.000 0.000 0.0093(3) Fe2B 0.0177(3) 0.0185(4) 0.0113(3) 0.000 0.000 0.0093(3) O1 0.0284(11) 0.0318(11) 0.0228(10) -0.0049(9) 0.0023(8) 0.0144(9) O2 0.0321(12) 0.0291(11) 0.0333(12) 0.0015(9) 0.0125(10) 0.0153(10) O1H 0.0245(15) 0.0245(15) 0.014(2) 0.000 0.000 0.0122(7) O1W 0.070(3) 0.0252(18) 0.049(2) 0.000 0.000 0.0126(19) N1 0.0194(10) 0.0192(11) 0.0228(11) -0.0006(9) -0.0009(9) 0.0110(9) N2 0.0262(13) 0.0306(13) 0.0403(15) 0.0105(12) 0.0031(11) 0.0174(11) N3 0.0269(13) 0.0328(14) 0.0390(15) 0.0117(12) 0.0041(11) 0.0178(12) N4 0.0240(11) 0.0206(11) 0.0221(11) 0.0000(9) 0.0031(9) 0.0133(10) C1 0.0203(12) 0.0203(12) 0.0235(13) -0.0001(10) 0.0010(10) 0.0105(10) C2 0.0266(14) 0.0209(13) 0.0247(13) 0.0000(11) 0.0069(11) 0.0106(11) C3 0.0272(13) 0.0259(13) 0.0182(12) 0.0031(10) 0.0023(10) 0.0170(12) Cl1 0.0247(4) 0.0247(4) 0.0308(6) 0.000 0.000 0.01235(18) O11 0.0504(17) 0.0504(17) 0.031(2) 0.000 0.000 0.0252(9) O12 0.0312(12) 0.0431(15) 0.0490(16) -0.0004(12) -0.0082(11) 0.0207(11) O2W 0.057(4) 0.057(4) 0.026(4) 0.000 0.000 0.0285(18) O3W 0.121(10) 0.121(10) 0.020(6) 0.000 0.000 0.060(5) O4W 0.20(5) 0.066(12) 0.016(4) 0.000 0.000 -0.06(2) O5W 0.061(12) 0.056(11) 0.067(12) 0.000 0.000 -0.029(9) O6W 0.014(16) 0.22(7) 0.011(15) 0.000 0.000 0.05(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 Fe1 N1 2.011(2) 8_456 ? Fe1 N1 2.011(2) 2_675 ? Fe1 N1 2.011(2) 3_465 ? Fe1 N1 2.011(2) 9_666 ? Fe1 N1 2.011(2) 7_576 ? Fe1 N1 2.011(2) . ? Fe2 O1H 1.8930(7) . ? Fe2 O2 2.007(2) 10_556 ? Fe2 O2 2.007(2) . ? Fe2 O1 2.026(2) 3_575 ? Fe2 O1 2.026(2) 12_576 ? Fe2 O1W 2.088(4) . ? Fe2B O1W 1.316(7) . ? Fe2B O2 2.078(4) 10_556 ? Fe2B O2 2.078(4) . ? Fe2B O1 2.092(4) 3_575 ? Fe2B O1 2.092(4) 12_576 ? O1 C3 1.249(4) . ? O1 Fe2 2.026(2) 2_775 ? O1 Fe2B 2.092(4) 2_775 ? O2 C3 1.256(4) . ? O1H Fe2 1.8930(7) 3_575 ? O1H Fe2 1.8930(7) 2_775 ? N1 C1 1.320(4) . ? N1 N2 1.363(3) . ? N2 N3 1.294(4) . ? N3 N4 1.346(3) . ? N4 C1 1.327(4) . ? N4 C2 1.453(4) . ? C2 C3 1.514(4) . ? Cl1 O12 1.422(3) . ? Cl1 O12 1.422(3) 3_565 ? Cl1 O12 1.422(3) 2_665 ? Cl1 O11 1.450(5) . ? O4W O4W 0.87(11) 2_575 ? O4W O4W 0.87(11) 3_355 ? 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 N1 180.000(1) 8_456 2_675 ? N1 Fe1 N1 88.78(9) 8_456 3_465 ? N1 Fe1 N1 91.22(9) 2_675 3_465 ? N1 Fe1 N1 91.22(9) 8_456 9_666 ? N1 Fe1 N1 88.78(9) 2_675 9_666 ? N1 Fe1 N1 180.00(11) 3_465 9_666 ? N1 Fe1 N1 91.22(9) 8_456 7_576 ? N1 Fe1 N1 88.78(9) 2_675 7_576 ? N1 Fe1 N1 88.78(9) 3_465 7_576 ? N1 Fe1 N1 91.22(9) 9_666 7_576 ? N1 Fe1 N1 88.78(9) 8_456 . ? N1 Fe1 N1 91.22(9) 2_675 . ? N1 Fe1 N1 91.22(9) 3_465 . ? N1 Fe1 N1 88.78(9) 9_666 . ? N1 Fe1 N1 180.0 7_576 . ? O1H Fe2 O2 95.34(7) . 10_556 ? O1H Fe2 O2 95.34(7) . . ? O2 Fe2 O2 92.20(15) 10_556 . ? O1H Fe2 O1 96.24(7) . 3_575 ? O2 Fe2 O1 168.42(10) 10_556 3_575 ? O2 Fe2 O1 86.89(10) . 3_575 ? O1H Fe2 O1 96.24(7) . 12_576 ? O2 Fe2 O1 86.89(10) 10_556 12_576 ? O2 Fe2 O1 168.42(10) . 12_576 ? O1 Fe2 O1 91.68(13) 3_575 12_576 ? O1H Fe2 O1W 178.72(15) . . ? O2 Fe2 O1W 83.78(12) 10_556 . ? O2 Fe2 O1W 83.78(12) . . ? O1 Fe2 O1W 84.64(12) 3_575 . ? O1 Fe2 O1W 84.64(12) 12_576 . ? O1W Fe2B O2 105.2(3) . 10_556 ? O1W Fe2B O2 105.2(3) . . ? O2 Fe2B O2 88.2(2) 10_556 . ? O1W Fe2B O1 106.5(3) . 3_575 ? O2 Fe2B O1 148.3(3) 10_556 3_575 ? O2 Fe2B O1 83.36(12) . 3_575 ? O1W Fe2B O1 106.5(3) . 12_576 ? O2 Fe2B O1 83.36(12) 10_556 12_576 ? O2 Fe2B O1 148.3(3) . 12_576 ? O1 Fe2B O1 88.0(2) 3_575 12_576 ? C3 O1 Fe2 129.9(2) . 2_775 ? C3 O1 Fe2B 150.2(2) . 2_775 ? Fe2 O1 Fe2B 21.54(15) 2_775 2_775 ? C3 O2 Fe2 131.9(2) . . ? C3 O2 Fe2B 151.8(3) . . ? Fe2 O2 Fe2B 21.71(15) . . ? Fe2 O1H Fe2 120.0 3_575 2_775 ? Fe2 O1H Fe2 120.0 3_575 . ? Fe2 O1H Fe2 120.0 2_775 . ? Fe2B O1W Fe2 0.4(2) . . ? C1 N1 N2 106.4(2) . . ? C1 N1 Fe1 131.61(19) . . ? N2 N1 Fe1 121.87(18) . . ? N3 N2 N1 109.7(2) . . ? N2 N3 N4 107.1(2) . . ? C1 N4 N3 108.5(2) . . ? C1 N4 C2 130.5(3) . . ? N3 N4 C2 120.9(2) . . ? N1 C1 N4 108.4(2) . . ? N4 C2 C3 113.1(2) . . ? O1 C3 O2 127.3(3) . . ? O1 C3 C2 118.9(3) . . ? O2 C3 C2 113.8(3) . . ? O12 Cl1 O12 111.39(12) . 3_565 ? O12 Cl1 O12 111.39(12) . 2_665 ? O12 Cl1 O12 111.39(12) 3_565 2_665 ? O12 Cl1 O11 107.48(13) . . ? O12 Cl1 O11 107.48(13) 3_565 . ? O12 Cl1 O11 107.48(13) 2_665 . ? O4W O4W O4W 60.000(10) 2_575 3_355 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.122 _refine_diff_density_min -1.423 _refine_diff_density_rms 0.119 #====================================================================== data_150K _database_code_depnum_ccdc_archive 'CCDC 668964' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H17 Cl Fe2 N12.5 O15' _chemical_formula_weight 699.47 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 Hexagonal _symmetry_space_group_name_H-M P63/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 10.7401(3) _cell_length_b 10.740 _cell_length_c 23.0238(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2299.98(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 442 _cell_measurement_theta_min 4 _cell_measurement_theta_max 25 _exptl_crystal_description needle _exptl_crystal_colour 'orange red' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.896 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 1.471 _exptl_absorpt_correction_type 'empirical SADABS' _exptl_absorpt_correction_T_min 0.8142 _exptl_absorpt_correction_T_max 0.9158 _exptl_absorpt_process_details 'Blessing, R. (1995) Acta Crystallogr., A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 37641 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0145 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 29.00 _reflns_number_total 2102 _reflns_number_gt 1818 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution SHELXS-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _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. Because of the disorder of water molecules and the Fe2 atom, restraints were used when refine. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0840P)^2^+4.3767P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2102 _refine_ls_number_parameters 140 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1623 _refine_ls_wR_factor_gt 0.1539 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.139 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.0000 1.0000 0.5000 0.0211(2) Uani 1 6 d S . . Fe2 Fe 0.73926(7) 1.53427(8) 0.2500 0.0219(2) Uani 0.8793(17) 2 d SP . 1 Fe2B Fe 0.7667(6) 1.6161(7) 0.2500 0.0219(2) Uani 0.1207(17) 2 d SP . 2 O1 O 0.4187(3) 1.3066(3) 0.31323(10) 0.0350(5) Uani 1 1 d . . . O2 O 0.6079(3) 1.5309(3) 0.31303(12) 0.0394(6) Uani 1 1 d . . . O1H O 0.6667 1.3333 0.2500 0.0269(11) Uani 1 6 d S . . O1W O 0.8151(6) 1.7545(5) 0.2500 0.0633(14) Uani 1 2 d S . . H1WA H 0.7794 1.7898 0.2732 0.076 Uiso 0.50 1 d PR . . H1WB H 0.8819 1.8091 0.2268 0.076 Uiso 0.50 1 d PR . . N1 N 0.1294(3) 1.1753(3) 0.44970(12) 0.0268(5) Uani 1 1 d . . . N2 N 0.0770(3) 1.2508(4) 0.42178(15) 0.0424(8) Uani 1 1 d . . . N3 N 0.1806(4) 1.3604(4) 0.39608(16) 0.0443(8) Uani 1 1 d . . . N4 N 0.3024(3) 1.3583(3) 0.40744(12) 0.0285(6) Uani 1 1 d . . . C1 C 0.2690(3) 1.2440(3) 0.44041(14) 0.0284(6) Uani 1 1 d . . . H1A H 0.3348 1.2167 0.4548 0.034 Uiso 1 1 calc R . . C2 C 0.4407(4) 1.4716(4) 0.38692(15) 0.0329(7) Uani 1 1 d . . . H2A H 0.5128 1.4962 0.4181 0.040 Uiso 1 1 calc R . . H2B H 0.4338 1.5583 0.3787 0.040 Uiso 1 1 calc R . . C3 C 0.4923(4) 1.4311(4) 0.33288(13) 0.0294(6) Uani 1 1 d . . . Cl1 Cl 0.3333 0.6667 0.52748(7) 0.0363(3) Uani 1 3 d S . . O11 O 0.3333 0.6667 0.5902(3) 0.0670(17) Uani 1 3 d S . . O12 O 0.2049(4) 0.6616(4) 0.51030(17) 0.0611(9) Uani 1 1 d . . . O2W O 0.0000 1.0000 0.3208(5) 0.060(3) Uani 0.50 3 d SP . . O3W O -0.6667 0.6667 0.2996(7) 0.120(8) Uani 0.50 3 d SPU A 1 O4W O -0.670(11) 0.7049(16) 0.2500 0.05(2) Uani 0.20 2 d SPU . 2 O5W O -0.819(3) 0.790(3) 0.2500 0.125(12) Uani 0.33 2 d SPU B 3 O6W O -0.806(8) 0.682(11) 0.2500 0.13(2) Uani 0.13 2 d SPU C 4 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 0.0194(3) 0.0194(3) 0.0245(5) 0.000 0.000 0.00969(16) Fe2 0.0253(4) 0.0258(4) 0.0150(3) 0.000 0.000 0.0129(3) Fe2B 0.0253(4) 0.0258(4) 0.0150(3) 0.000 0.000 0.0129(3) O1 0.0377(13) 0.0396(13) 0.0279(11) -0.0052(10) 0.0027(10) 0.0195(11) O2 0.0426(14) 0.0373(13) 0.0388(14) 0.0019(11) 0.0144(11) 0.0204(11) O1H 0.0310(17) 0.0310(17) 0.019(2) 0.000 0.000 0.0155(8) O1W 0.082(4) 0.034(2) 0.056(3) 0.000 0.000 0.016(2) N1 0.0275(12) 0.0264(12) 0.0287(12) -0.0004(10) -0.0007(10) 0.0152(10) N2 0.0370(16) 0.0445(17) 0.0524(19) 0.0158(15) 0.0041(14) 0.0255(14) N3 0.0403(17) 0.0484(18) 0.0527(19) 0.0174(16) 0.0048(15) 0.0285(15) N4 0.0332(14) 0.0295(13) 0.0274(12) -0.0002(10) 0.0040(11) 0.0191(11) C1 0.0300(15) 0.0292(15) 0.0292(15) 0.0000(12) 0.0005(12) 0.0172(12) C2 0.0374(17) 0.0305(15) 0.0310(16) 0.0003(13) 0.0084(13) 0.0171(13) C3 0.0377(17) 0.0348(16) 0.0220(13) 0.0033(11) 0.0027(12) 0.0230(14) Cl1 0.0346(5) 0.0346(5) 0.0395(8) 0.000 0.000 0.0173(2) O11 0.079(3) 0.079(3) 0.043(3) 0.000 0.000 0.0394(14) O12 0.0466(18) 0.070(2) 0.070(2) 0.0008(18) -0.0114(16) 0.0315(17) O2W 0.071(5) 0.071(5) 0.038(5) 0.000 0.000 0.036(2) O3W 0.156(12) 0.156(12) 0.048(8) 0.000 0.000 0.078(6) O4W 0.08(4) 0.021(9) 0.002(4) 0.000 0.000 -0.01(2) O5W 0.091(15) 0.089(15) 0.067(12) 0.000 0.000 -0.051(13) O6W 0.13(5) 0.23(7) 0.020(17) 0.000 0.000 0.09(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 2.050(3) 8_456 ? Fe1 N1 2.050(3) 3_465 ? Fe1 N1 2.050(3) 9_666 ? Fe1 N1 2.050(3) 2_675 ? Fe1 N1 2.050(3) 7_576 ? Fe1 N1 2.050(3) . ? Fe2 O1H 1.8928(8) . ? Fe2 O2 2.011(3) 10_556 ? Fe2 O2 2.011(3) . ? Fe2 O1 2.029(2) 3_575 ? Fe2 O1 2.029(2) 12_576 ? Fe2 O1W 2.081(5) . ? Fe2B O1W 1.306(8) . ? Fe2B O2 2.071(5) 10_556 ? Fe2B O2 2.071(5) . ? Fe2B O1 2.107(5) 3_575 ? Fe2B O1 2.107(5) 12_576 ? O1 C3 1.249(4) . ? O1 Fe2 2.029(2) 2_775 ? O1 Fe2B 2.107(5) 2_775 ? O2 C3 1.253(4) . ? O1H Fe2 1.8928(8) 3_575 ? O1H Fe2 1.8928(8) 2_775 ? N1 C1 1.317(4) . ? N1 N2 1.357(4) . ? N2 N3 1.290(5) . ? N3 N4 1.345(4) . ? N4 C1 1.331(4) . ? N4 C2 1.450(4) . ? C2 C3 1.511(4) . ? Cl1 O12 1.409(3) . ? Cl1 O12 1.409(3) 3_565 ? Cl1 O12 1.409(3) 2_665 ? Cl1 O11 1.443(6) . ? O4W O4W 0.74(11) 3_355 ? O4W O4W 0.74(11) 2_575 ? 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 N1 88.79(10) 8_456 3_465 ? N1 Fe1 N1 91.21(10) 8_456 9_666 ? N1 Fe1 N1 180.00(12) 3_465 9_666 ? N1 Fe1 N1 180.000(1) 8_456 2_675 ? N1 Fe1 N1 91.21(10) 3_465 2_675 ? N1 Fe1 N1 88.79(10) 9_666 2_675 ? N1 Fe1 N1 91.21(10) 8_456 7_576 ? N1 Fe1 N1 88.79(10) 3_465 7_576 ? N1 Fe1 N1 91.21(10) 9_666 7_576 ? N1 Fe1 N1 88.79(10) 2_675 7_576 ? N1 Fe1 N1 88.79(10) 8_456 . ? N1 Fe1 N1 91.21(10) 3_465 . ? N1 Fe1 N1 88.79(10) 9_666 . ? N1 Fe1 N1 91.21(10) 2_675 . ? N1 Fe1 N1 180.00(14) 7_576 . ? O1H Fe2 O2 95.40(8) . 10_556 ? O1H Fe2 O2 95.40(8) . . ? O2 Fe2 O2 92.36(17) 10_556 . ? O1H Fe2 O1 96.22(8) . 3_575 ? O2 Fe2 O1 168.38(12) 10_556 3_575 ? O2 Fe2 O1 86.79(11) . 3_575 ? O1H Fe2 O1 96.22(8) . 12_576 ? O2 Fe2 O1 86.79(11) 10_556 12_576 ? O2 Fe2 O1 168.38(12) . 12_576 ? O1 Fe2 O1 91.70(15) 3_575 12_576 ? O1H Fe2 O1W 178.93(18) . . ? O2 Fe2 O1W 83.87(14) 10_556 . ? O2 Fe2 O1W 83.87(14) . . ? O1 Fe2 O1W 84.52(14) 3_575 . ? O1 Fe2 O1W 84.52(14) 12_576 . ? O1W Fe2B O2 105.9(3) . 10_556 ? O1W Fe2B O2 105.9(3) . . ? O2 Fe2B O2 88.9(3) 10_556 . ? O1W Fe2B O1 105.8(3) . 3_575 ? O2 Fe2B O1 148.3(4) 10_556 3_575 ? O2 Fe2B O1 83.26(14) . 3_575 ? O1W Fe2B O1 105.8(3) . 12_576 ? O2 Fe2B O1 83.26(14) 10_556 12_576 ? O2 Fe2B O1 148.3(4) . 12_576 ? O1 Fe2B O1 87.4(2) 3_575 12_576 ? C3 O1 Fe2 129.9(2) . 2_775 ? C3 O1 Fe2B 150.1(3) . 2_775 ? Fe2 O1 Fe2B 21.50(17) 2_775 2_775 ? C3 O2 Fe2 131.7(2) . . ? C3 O2 Fe2B 151.5(3) . . ? Fe2 O2 Fe2B 21.82(17) . . ? Fe2 O1H Fe2 120.000(1) 3_575 2_775 ? Fe2 O1H Fe2 120.000(1) 3_575 . ? Fe2 O1H Fe2 120.000(1) 2_775 . ? Fe2B O1W Fe2 0.4(2) . . ? C1 N1 N2 106.5(3) . . ? C1 N1 Fe1 131.7(2) . . ? N2 N1 Fe1 121.6(2) . . ? N3 N2 N1 109.7(3) . . ? N2 N3 N4 107.3(3) . . ? C1 N4 N3 108.1(3) . . ? C1 N4 C2 130.5(3) . . ? N3 N4 C2 121.3(3) . . ? N1 C1 N4 108.4(3) . . ? N4 C2 C3 113.3(3) . . ? O1 C3 O2 127.6(3) . . ? O1 C3 C2 118.6(3) . . ? O2 C3 C2 113.8(3) . . ? O12 Cl1 O12 112.45(16) . 3_565 ? O12 Cl1 O12 112.45(16) . 2_665 ? O12 Cl1 O12 112.45(16) 3_565 2_665 ? O12 Cl1 O11 106.30(18) . . ? O12 Cl1 O11 106.30(18) 3_565 . ? O12 Cl1 O11 106.30(18) 2_665 . ? O4W O4W O4W 60.00(6) 3_355 2_575 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.994 _refine_diff_density_min -1.445 _refine_diff_density_rms 0.124 #====================================================================== data_210K _database_code_depnum_ccdc_archive 'CCDC 668965' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H17 Cl Fe2 N12.5 O15' _chemical_formula_weight 699.47 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 Hexagonal _symmetry_space_group_name_H-M P63/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 10.8575(2) _cell_length_b 10.858 _cell_length_c 23.1037(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2358.69(6) _cell_formula_units_Z 4 _cell_measurement_temperature 210(2) _cell_measurement_reflns_used 442 _cell_measurement_theta_min 4 _cell_measurement_theta_max 25 _exptl_crystal_description needle _exptl_crystal_colour 'orange red' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.849 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 1.434 _exptl_absorpt_correction_type 'empirical SADABS' _exptl_absorpt_correction_T_min 0.8180 _exptl_absorpt_correction_T_max 0.9178 _exptl_absorpt_process_details 'Blessing, R. (1995) Acta Crystallogr., A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 210(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 19907 _diffrn_reflns_av_R_equivalents 0.0261 _diffrn_reflns_av_sigmaI/netI 0.0147 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 29.00 _reflns_number_total 2155 _reflns_number_gt 1856 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution SHELXS-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _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. Because of the disorder of water molecules and the Fe2 atom, restraints were used when refine. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1012P)^2^+2.4955P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2155 _refine_ls_number_parameters 146 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0587 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1829 _refine_ls_wR_factor_gt 0.1762 _refine_ls_goodness_of_fit_ref 1.206 _refine_ls_restrained_S_all 1.198 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.0000 1.0000 0.5000 0.0288(3) Uani 1 6 d S . . Fe2 Fe 0.74268(7) 1.53281(7) 0.2500 0.0250(2) Uani 0.8773(16) 2 d SP . 1 Fe2B Fe 0.7720(5) 1.6201(6) 0.2500 0.0250(2) Uani 0.1227(16) 2 d SP . 2 O1 O 0.4254(3) 1.3137(3) 0.31278(11) 0.0405(6) Uani 1 1 d . . . O2 O 0.6151(3) 1.5341(3) 0.31294(12) 0.0433(6) Uani 1 1 d . . . O1H O 0.6667 1.3333 0.2500 0.0311(11) Uani 1 6 d S . . O1W O 0.8276(6) 1.7506(5) 0.2500 0.0729(15) Uani 1 2 d S . . H1WA H 0.7954 1.7887 0.2731 0.087 Uiso 0.50 1 d PR . . H1WB H 0.8949 1.8021 0.2269 0.087 Uiso 0.50 1 d PR . . N1 N 0.1388(3) 1.1834(3) 0.44713(13) 0.0344(6) Uani 1 1 d . . . N2 N 0.0885(4) 1.2573(4) 0.41880(19) 0.0596(11) Uani 1 1 d . . . N3 N 0.1916(4) 1.3675(4) 0.3939(2) 0.0590(10) Uani 1 1 d . . . N4 N 0.3105(3) 1.3650(3) 0.40601(12) 0.0330(6) Uani 1 1 d . . . C1 C 0.2766(4) 1.2519(3) 0.43879(16) 0.0368(7) Uani 1 1 d . . . H1A H 0.3408 1.2255 0.4535 0.044 Uiso 1 1 calc R . . C2 C 0.4483(4) 1.4778(3) 0.38585(16) 0.0378(7) Uani 1 1 d . . . H2A H 0.5183 1.5025 0.4169 0.045 Uiso 1 1 calc R . . H2B H 0.4414 1.5625 0.3772 0.045 Uiso 1 1 calc R . . C3 C 0.4998(4) 1.4366(3) 0.33265(13) 0.0325(6) Uani 1 1 d . . . Cl1 Cl 0.3333 0.6667 0.52585(8) 0.0468(4) Uani 1 3 d S . . O11 O 0.3333 0.6667 0.5883(3) 0.094(2) Uani 1 3 d S . . O12 O 0.2056(5) 0.6581(6) 0.5109(2) 0.0956(15) Uani 1 1 d . . . O2W O 0.0000 1.0000 0.3194(7) 0.111(6) Uani 0.50 3 d SP . . O3W O -0.6667 0.6667 0.2993(9) 0.124(9) Uani 0.40 3 d SPU A 1 O4W O -0.669(9) 0.7030(13) 0.2500 0.051(19) Uani 0.23 2 d SPU . 2 O5W O -0.8460(19) 0.8209(17) 0.2500 0.090(6) Uani 0.33 2 d SPU B 3 O6W O -0.826(4) 0.636(5) 0.2500 0.052(11) Uani 0.10 2 d SPU C 4 O7W O -0.788(5) 0.748(7) 0.2500 0.037(12) Uani 0.07 2 d SPU D 5 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 0.0235(3) 0.0235(3) 0.0393(6) 0.000 0.000 0.01176(17) Fe2 0.0265(4) 0.0264(4) 0.0228(4) 0.000 0.000 0.0137(3) Fe2B 0.0265(4) 0.0264(4) 0.0228(4) 0.000 0.000 0.0137(3) O1 0.0392(12) 0.0423(13) 0.0391(13) -0.0053(10) 0.0049(10) 0.0197(11) O2 0.0431(13) 0.0387(13) 0.0470(15) 0.0011(11) 0.0147(11) 0.0196(11) O1H 0.0337(16) 0.0337(16) 0.026(2) 0.000 0.000 0.0169(8) O1W 0.086(4) 0.034(2) 0.082(4) 0.000 0.000 0.018(2) N1 0.0326(13) 0.0307(13) 0.0416(15) 0.0028(11) 0.0029(11) 0.0171(11) N2 0.0408(17) 0.058(2) 0.085(3) 0.030(2) 0.0083(17) 0.0287(16) N3 0.0408(17) 0.058(2) 0.084(3) 0.033(2) 0.0121(17) 0.0289(16) N4 0.0350(13) 0.0292(12) 0.0373(14) 0.0011(10) 0.0067(11) 0.0179(11) C1 0.0352(16) 0.0343(15) 0.0419(18) 0.0059(13) 0.0037(13) 0.0181(13) C2 0.0406(17) 0.0300(14) 0.0398(18) 0.0017(13) 0.0123(14) 0.0154(13) C3 0.0376(15) 0.0356(15) 0.0306(15) 0.0031(12) 0.0036(12) 0.0230(13) Cl1 0.0428(5) 0.0428(5) 0.0550(9) 0.000 0.000 0.0214(3) O11 0.111(4) 0.111(4) 0.060(4) 0.000 0.000 0.056(2) O12 0.062(2) 0.120(4) 0.107(4) 0.010(3) -0.014(2) 0.047(3) O2W 0.127(9) 0.127(9) 0.078(11) 0.000 0.000 0.064(5) O3W 0.158(15) 0.158(15) 0.057(11) 0.000 0.000 0.079(7) O4W 0.07(3) 0.021(8) 0.017(5) 0.000 0.000 -0.008(17) O5W 0.060(10) 0.048(8) 0.134(17) 0.000 0.000 0.006(7) O6W 0.025(16) 0.06(3) 0.031(17) 0.000 0.000 -0.009(15) O7W 0.04(2) 0.06(4) 0.003(16) 0.000 0.000 0.02(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 2.174(3) 2_675 ? Fe1 N1 2.174(3) 9_666 ? Fe1 N1 2.174(3) 7_576 ? Fe1 N1 2.174(3) . ? Fe1 N1 2.174(3) 8_456 ? Fe1 N1 2.174(3) 3_465 ? Fe2 O1H 1.8933(7) . ? Fe2 O2 2.013(3) 10_556 ? Fe2 O2 2.013(3) . ? Fe2 O1 2.023(2) 3_575 ? Fe2 O1 2.023(2) 12_576 ? Fe2 O1W 2.064(4) . ? Fe2B O1W 1.231(7) . ? Fe2B O2 2.074(4) 10_556 ? Fe2B O2 2.074(4) . ? Fe2B O1 2.136(4) 3_575 ? Fe2B O1 2.136(4) 12_576 ? O1 C3 1.251(4) . ? O1 Fe2 2.023(2) 2_775 ? O1 Fe2B 2.136(4) 2_775 ? O2 C3 1.253(4) . ? O1H Fe2 1.8933(7) 3_575 ? O1H Fe2 1.8933(7) 2_775 ? N1 C1 1.310(4) . ? N1 N2 1.345(4) . ? N2 N3 1.295(5) . ? N3 N4 1.334(4) . ? N4 C1 1.329(4) . ? N4 C2 1.457(4) . ? C2 C3 1.508(4) . ? Cl1 O12 1.387(4) . ? Cl1 O12 1.387(4) 3_565 ? Cl1 O12 1.387(4) 2_665 ? Cl1 O11 1.442(8) . ? O4W O4W 0.71(10) 2_575 ? O4W O4W 0.71(10) 3_355 ? 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 N1 88.48(11) 2_675 9_666 ? N1 Fe1 N1 88.48(11) 2_675 7_576 ? N1 Fe1 N1 91.52(11) 9_666 7_576 ? N1 Fe1 N1 91.52(11) 2_675 . ? N1 Fe1 N1 88.48(11) 9_666 . ? N1 Fe1 N1 180.000(1) 7_576 . ? N1 Fe1 N1 180.000(1) 2_675 8_456 ? N1 Fe1 N1 91.52(11) 9_666 8_456 ? N1 Fe1 N1 91.52(11) 7_576 8_456 ? N1 Fe1 N1 88.48(11) . 8_456 ? N1 Fe1 N1 91.52(11) 2_675 3_465 ? N1 Fe1 N1 180.00(13) 9_666 3_465 ? N1 Fe1 N1 88.48(11) 7_576 3_465 ? N1 Fe1 N1 91.52(11) . 3_465 ? N1 Fe1 N1 88.48(11) 8_456 3_465 ? O1H Fe2 O2 95.75(8) . 10_556 ? O1H Fe2 O2 95.75(8) . . ? O2 Fe2 O2 92.48(17) 10_556 . ? O1H Fe2 O1 95.82(7) . 3_575 ? O2 Fe2 O1 168.42(11) 10_556 3_575 ? O2 Fe2 O1 86.78(11) . 3_575 ? O1H Fe2 O1 95.82(7) . 12_576 ? O2 Fe2 O1 86.78(11) 10_556 12_576 ? O2 Fe2 O1 168.42(11) . 12_576 ? O1 Fe2 O1 91.62(16) 3_575 12_576 ? O1H Fe2 O1W 179.42(18) . . ? O2 Fe2 O1W 84.65(14) 10_556 . ? O2 Fe2 O1W 84.65(14) . . ? O1 Fe2 O1W 83.78(15) 3_575 . ? O1 Fe2 O1W 83.78(15) 12_576 . ? O1W Fe2B O2 109.7(3) . 10_556 ? O1W Fe2B O2 109.7(3) . . ? O2 Fe2B O2 89.1(3) 10_556 . ? O1W Fe2B O1 105.1(3) . 3_575 ? O2 Fe2B O1 145.1(3) 10_556 3_575 ? O2 Fe2B O1 82.38(14) . 3_575 ? O1W Fe2B O1 105.1(3) . 12_576 ? O2 Fe2B O1 82.38(14) 10_556 12_576 ? O2 Fe2B O1 145.1(3) . 12_576 ? O1 Fe2B O1 85.5(2) 3_575 12_576 ? C3 O1 Fe2 130.7(2) . 2_775 ? C3 O1 Fe2B 152.4(3) . 2_775 ? Fe2 O1 Fe2B 22.96(14) 2_775 2_775 ? C3 O2 Fe2 131.0(2) . . ? C3 O2 Fe2B 152.1(3) . . ? Fe2 O2 Fe2B 23.52(15) . . ? Fe2 O1H Fe2 120.000(1) 3_575 2_775 ? Fe2 O1H Fe2 120.000(1) 3_575 . ? Fe2 O1H Fe2 120.0 2_775 . ? Fe2B O1W Fe2 2.3(3) . . ? C1 N1 N2 106.2(3) . . ? C1 N1 Fe1 132.4(2) . . ? N2 N1 Fe1 121.1(2) . . ? N3 N2 N1 110.2(3) . . ? N2 N3 N4 106.7(3) . . ? C1 N4 N3 108.3(3) . . ? C1 N4 C2 130.7(3) . . ? N3 N4 C2 120.9(3) . . ? N1 C1 N4 108.6(3) . . ? N4 C2 C3 112.9(3) . . ? O1 C3 O2 127.4(3) . . ? O1 C3 C2 118.5(3) . . ? O2 C3 C2 114.0(3) . . ? O12 Cl1 O12 114.0(2) . 3_565 ? O12 Cl1 O12 114.0(2) . 2_665 ? O12 Cl1 O12 114.0(2) 3_565 2_665 ? O12 Cl1 O11 104.4(2) . . ? O12 Cl1 O11 104.4(3) 3_565 . ? O12 Cl1 O11 104.4(2) 2_665 . ? O4W O4W O4W 60.000(3) 2_575 3_355 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.891 _refine_diff_density_min -1.329 _refine_diff_density_rms 0.118 #====================================================================== data_270K _database_code_depnum_ccdc_archive 'CCDC 668966' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H17 Cl Fe2 N12.5 O15' _chemical_formula_weight 699.47 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 Hexagonal _symmetry_space_group_name_H-M P63/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 10.8858(2) _cell_length_b 10.886 _cell_length_c 23.1388(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2374.61(7) _cell_formula_units_Z 4 _cell_measurement_temperature 270(2) _cell_measurement_reflns_used 442 _cell_measurement_theta_min 4 _cell_measurement_theta_max 25 _exptl_crystal_description needle _exptl_crystal_colour 'orange red' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.836 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 1.425 _exptl_absorpt_correction_type 'empirical SADABS' _exptl_absorpt_correction_T_min 0.8188 _exptl_absorpt_correction_T_max 0.9180 _exptl_absorpt_process_details 'Blessing, R. (1995) Acta Crystallogr., A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 270(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 20067 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0150 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 29.00 _reflns_number_total 2163 _reflns_number_gt 1835 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution SHELXS-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _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. Because of the disorder of water molecules and the Fe2 atom, restraints were used when refine. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0815P)^2^+2.6628P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2163 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1561 _refine_ls_wR_factor_gt 0.1489 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.138 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.0000 1.0000 0.5000 0.0317(3) Uani 1 6 d S . . Fe2 Fe 0.74172(6) 1.53223(7) 0.2500 0.0266(2) Uani 0.8778(14) 2 d SP . 1 Fe2B Fe 0.7726(5) 1.6202(5) 0.2500 0.0266(2) Uani 0.1222(14) 2 d SP . 2 O1 O 0.4256(2) 1.3129(2) 0.31276(10) 0.0434(5) Uani 1 1 d . . . O2 O 0.6140(3) 1.5327(2) 0.31289(11) 0.0469(6) Uani 1 1 d . . . O1H O 0.6667 1.3333 0.2500 0.0318(10) Uani 1 6 d S . . O1W O 0.8254(6) 1.7492(4) 0.2500 0.0783(14) Uani 1 2 d S . . H1WA H 0.7929 1.7868 0.2731 0.094 Uiso 0.50 1 d PR . . H1WB H 0.8923 1.8010 0.2269 0.094 Uiso 0.50 1 d PR . . N1 N 0.1388(3) 1.1839(3) 0.44693(12) 0.0376(6) Uani 1 1 d . . . N2 N 0.0888(4) 1.2572(4) 0.41824(18) 0.0689(11) Uani 1 1 d . . . N3 N 0.1907(3) 1.3653(4) 0.39281(19) 0.0671(11) Uani 1 1 d . . . N4 N 0.3097(3) 1.3645(3) 0.40550(11) 0.0364(6) Uani 1 1 d . . . C1 C 0.2757(3) 1.2529(3) 0.43841(15) 0.0413(7) Uani 1 1 d . . . H1A H 0.3393 1.2275 0.4532 0.050 Uiso 1 1 calc R . . C2 C 0.4469(4) 1.4767(3) 0.38503(15) 0.0423(7) Uani 1 1 d . . . H2A H 0.5161 1.5019 0.4157 0.051 Uiso 1 1 calc R . . H2B H 0.4398 1.5599 0.3761 0.051 Uiso 1 1 calc R . . C3 C 0.4987(3) 1.4353(3) 0.33239(13) 0.0349(6) Uani 1 1 d . . . Cl1 Cl 0.3333 0.6667 0.52429(8) 0.0560(4) Uani 1 3 d S . . O11 O 0.3333 0.6667 0.5870(4) 0.136(4) Uani 1 3 d S . . O12 O 0.2057(5) 0.6565(7) 0.5118(3) 0.132(2) Uani 1 1 d . . . O2W O 0.0000 1.0000 0.3172(8) 0.146(8) Uani 0.50 3 d SP . . O3W O -0.6667 0.6667 0.2981(10) 0.136(9) Uani 0.40 3 d SP A 1 O4W O -0.666(19) 0.702(2) 0.2500 0.06(4) Uani 0.23 2 d SP . 2 O5W O -0.849(2) 0.8219(16) 0.2500 0.101(6) Uani 0.33 2 d SP B 3 O6W O -0.818(3) 0.629(5) 0.2500 0.057(10) Uani 0.10 2 d SP C 4 O7W O -0.768(9) 0.760(8) 0.2500 0.07(2) Uani 0.07 2 d SP D 5 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 0.0267(3) 0.0267(3) 0.0416(6) 0.000 0.000 0.01336(16) Fe2 0.0270(3) 0.0273(3) 0.0259(3) 0.000 0.000 0.0139(3) Fe2B 0.0270(3) 0.0273(3) 0.0259(3) 0.000 0.000 0.0139(3) O1 0.0411(12) 0.0422(12) 0.0443(12) -0.0070(10) 0.0052(10) 0.0189(10) O2 0.0465(13) 0.0407(12) 0.0518(14) 0.0012(10) 0.0167(11) 0.0205(10) O1H 0.0317(14) 0.0317(14) 0.032(2) 0.000 0.000 0.0159(7) O1W 0.093(3) 0.0352(19) 0.089(3) 0.000 0.000 0.019(2) N1 0.0357(12) 0.0333(12) 0.0450(14) 0.0062(10) 0.0049(11) 0.0181(10) N2 0.0438(17) 0.068(2) 0.101(3) 0.039(2) 0.0120(18) 0.0325(16) N3 0.0458(17) 0.064(2) 0.099(3) 0.040(2) 0.0158(18) 0.0325(16) N4 0.0382(13) 0.0310(12) 0.0417(13) 0.0018(10) 0.0087(10) 0.0185(10) C1 0.0385(15) 0.0384(15) 0.0486(18) 0.0092(13) 0.0058(13) 0.0204(13) C2 0.0431(16) 0.0320(14) 0.0460(17) 0.0016(12) 0.0146(14) 0.0143(12) C3 0.0387(14) 0.0383(14) 0.0335(14) 0.0033(11) 0.0034(11) 0.0236(12) Cl1 0.0511(5) 0.0511(5) 0.0656(10) 0.000 0.000 0.0256(3) O11 0.167(6) 0.167(6) 0.073(5) 0.000 0.000 0.084(3) O12 0.079(3) 0.176(6) 0.147(5) 0.020(4) -0.022(3) 0.069(3) O2W 0.167(12) 0.167(12) 0.104(14) 0.000 0.000 0.084(6) O3W 0.169(15) 0.169(15) 0.069(12) 0.000 0.000 0.085(8) O4W 0.09(6) 0.030(9) 0.023(5) 0.000 0.000 -0.01(3) O5W 0.084(11) 0.050(8) 0.132(16) 0.000 0.000 0.005(8) O6W 0.026(16) 0.07(3) 0.037(17) 0.000 0.000 -0.002(15) O7W 0.09(5) 0.08(5) 0.02(2) 0.000 0.000 0.03(4) _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 2.185(3) 2_675 ? Fe1 N1 2.185(3) 8_456 ? Fe1 N1 2.185(2) 9_666 ? Fe1 N1 2.185(2) 3_465 ? Fe1 N1 2.185(3) . ? Fe1 N1 2.185(3) 7_576 ? Fe2 O1H 1.8938(6) . ? Fe2 O2 2.014(2) . ? Fe2 O2 2.014(2) 10_556 ? Fe2 O1 2.026(2) 3_575 ? Fe2 O1 2.026(2) 12_576 ? Fe2 O1W 2.063(4) . ? Fe2B O1W 1.223(6) . ? Fe2B O2 2.088(4) 10_556 ? Fe2B O2 2.088(4) . ? Fe2B O1 2.130(4) 3_575 ? Fe2B O1 2.130(4) 12_576 ? O1 C3 1.247(4) . ? O1 Fe2 2.026(2) 2_775 ? O1 Fe2B 2.130(4) 2_775 ? O2 C3 1.254(4) . ? O1H Fe2 1.8938(6) 3_575 ? O1H Fe2 1.8938(6) 2_775 ? N1 C1 1.306(4) . ? N1 N2 1.344(4) . ? N2 N3 1.287(5) . ? N3 N4 1.333(4) . ? N4 C1 1.320(4) . ? N4 C2 1.457(4) . ? C2 C3 1.502(4) . ? Cl1 O12 1.369(5) . ? Cl1 O12 1.369(5) 3_565 ? Cl1 O12 1.369(4) 2_665 ? Cl1 O11 1.451(9) . ? O4W O4W 0.7(2) 3_355 ? O4W O4W 0.7(2) 2_575 ? 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 N1 180.000(1) 2_675 8_456 ? N1 Fe1 N1 88.51(10) 2_675 9_666 ? N1 Fe1 N1 91.49(10) 8_456 9_666 ? N1 Fe1 N1 91.49(10) 2_675 3_465 ? N1 Fe1 N1 88.51(10) 8_456 3_465 ? N1 Fe1 N1 180.00(12) 9_666 3_465 ? N1 Fe1 N1 91.49(10) 2_675 . ? N1 Fe1 N1 88.51(10) 8_456 . ? N1 Fe1 N1 88.51(10) 9_666 . ? N1 Fe1 N1 91.49(10) 3_465 . ? N1 Fe1 N1 88.51(10) 2_675 7_576 ? N1 Fe1 N1 91.49(10) 8_456 7_576 ? N1 Fe1 N1 91.49(10) 9_666 7_576 ? N1 Fe1 N1 88.51(10) 3_465 7_576 ? N1 Fe1 N1 180.0 . 7_576 ? O1H Fe2 O2 95.70(7) . . ? O1H Fe2 O2 95.70(7) . 10_556 ? O2 Fe2 O2 92.51(16) . 10_556 ? O1H Fe2 O1 95.77(7) . 3_575 ? O2 Fe2 O1 86.80(11) . 3_575 ? O2 Fe2 O1 168.51(10) 10_556 3_575 ? O1H Fe2 O1 95.77(7) . 12_576 ? O2 Fe2 O1 168.51(10) . 12_576 ? O2 Fe2 O1 86.80(11) 10_556 12_576 ? O1 Fe2 O1 91.60(14) 3_575 12_576 ? O1H Fe2 O1W 179.47(17) . . ? O2 Fe2 O1W 84.66(13) . . ? O2 Fe2 O1W 84.66(13) 10_556 . ? O1 Fe2 O1W 83.86(13) 3_575 . ? O1 Fe2 O1W 83.86(13) 12_576 . ? O1W Fe2B O2 109.3(3) . 10_556 ? O1W Fe2B O2 109.3(3) . . ? O2 Fe2B O2 88.4(2) 10_556 . ? O1W Fe2B O1 105.9(3) . 3_575 ? O2 Fe2B O1 144.7(3) 10_556 3_575 ? O2 Fe2B O1 82.30(13) . 3_575 ? O1W Fe2B O1 105.9(3) . 12_576 ? O2 Fe2B O1 82.30(13) 10_556 12_576 ? O2 Fe2B O1 144.7(3) . 12_576 ? O1 Fe2B O1 86.0(2) 3_575 12_576 ? C3 O1 Fe2 130.8(2) . 2_775 ? C3 O1 Fe2B 152.5(2) . 2_775 ? Fe2 O1 Fe2B 23.17(13) 2_775 2_775 ? C3 O2 Fe2 131.1(2) . . ? C3 O2 Fe2B 152.4(3) . . ? Fe2 O2 Fe2B 23.57(13) . . ? Fe2 O1H Fe2 120.000(1) 3_575 2_775 ? Fe2 O1H Fe2 120.000(1) 3_575 . ? Fe2 O1H Fe2 120.0 2_775 . ? Fe2B O1W Fe2 1.5(2) . . ? C1 N1 N2 105.5(3) . . ? C1 N1 Fe1 132.8(2) . . ? N2 N1 Fe1 121.4(2) . . ? N3 N2 N1 110.4(3) . . ? N2 N3 N4 106.8(3) . . ? C1 N4 N3 107.9(3) . . ? C1 N4 C2 131.1(3) . . ? N3 N4 C2 121.0(3) . . ? N1 C1 N4 109.3(3) . . ? N4 C2 C3 113.2(3) . . ? O1 C3 O2 127.4(3) . . ? O1 C3 C2 118.7(3) . . ? O2 C3 C2 113.9(3) . . ? O12 Cl1 O12 115.6(2) . 3_565 ? O12 Cl1 O12 115.6(2) . 2_665 ? O12 Cl1 O12 115.6(2) 3_565 2_665 ? O12 Cl1 O11 102.2(3) . . ? O12 Cl1 O11 102.2(3) 3_565 . ? O12 Cl1 O11 102.2(3) 2_665 . ? O4W O4W O4W 60.00(10) 3_355 2_575 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.041 _refine_diff_density_min -1.211 _refine_diff_density_rms 0.116 #====================================================================== data_330K _database_code_depnum_ccdc_archive 'CCDC 668967' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H17 Cl Fe2 N12.5 O15' _chemical_formula_weight 699.47 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 Hexagonal _symmetry_space_group_name_H-M P63/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 11.036(6) _cell_length_b 11.036 _cell_length_c 22.991(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2425.2(19) _cell_formula_units_Z 4 _cell_measurement_temperature 330(2) _cell_measurement_reflns_used 442 _cell_measurement_theta_min 4 _cell_measurement_theta_max 25 _exptl_crystal_description needle _exptl_crystal_colour 'orange red' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.798 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 1.395 _exptl_absorpt_correction_type 'empirical SADABS' _exptl_absorpt_correction_T_min 0.8232 _exptl_absorpt_correction_T_max 0.9200 _exptl_absorpt_process_details 'Blessing, R. (1995) Acta Crystallogr., A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 330(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX area-detector diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 19820 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0182 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 28.92 _reflns_number_total 2178 _reflns_number_gt 1799 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution SHELXS-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _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. Because of the disorder of water molecules and the Fe2 atom, restraints were used when refine. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0953P)^2^+2.8492P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2178 _refine_ls_number_parameters 130 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1799 _refine_ls_wR_factor_gt 0.1713 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.127 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.0000 1.0000 0.5000 0.0357(3) Uani 1 6 d S . . Fe2 Fe -0.25990(7) 1.20842(7) 0.2500 0.0306(2) Uani 0.8801(16) 2 d SP . 1 Fe2B Fe -0.2283(5) 1.1524(6) 0.2500 0.0306(2) Uani 0.1199(16) 2 d SP . 2 O1 O -0.0813(3) 1.5298(3) 0.31268(13) 0.0531(7) Uani 1 1 d . . . O2 O -0.1138(3) 1.3110(3) 0.31271(12) 0.0499(6) Uani 1 1 d . . . O1H O -0.3333 1.3333 0.2500 0.0374(11) Uani 1 6 d S . . O1W O -0.1818(7) 1.0705(7) 0.2500 0.0895(18) Uani 1 2 d S . . H1WA H -0.1154 1.0845 0.2728 0.107 Uiso 0.50 1 d PR . . H1WB H -0.2163 1.0006 0.2272 0.107 Uiso 0.50 1 d PR . . N1 N 0.0463(3) 1.1837(3) 0.44674(14) 0.0430(7) Uani 1 1 d . . . N2 N 0.1686(4) 1.2562(5) 0.4175(2) 0.0809(14) Uani 1 1 d . . . N3 N 0.1739(4) 1.3623(5) 0.3913(2) 0.0815(14) Uani 1 1 d . . . N4 N 0.0558(3) 1.3630(3) 0.40469(13) 0.0424(7) Uani 1 1 d . . . C1 C -0.0198(4) 1.2539(4) 0.43851(17) 0.0486(8) Uani 1 1 d . . . H1A H -0.1065 1.2303 0.4541 0.058 Uiso 1 1 calc R . . C2 C 0.0303(4) 1.4747(4) 0.38420(18) 0.0490(9) Uani 1 1 d . . . H2A H 0.1191 1.5565 0.3745 0.059 Uiso 1 1 calc R . . H2B H -0.0113 1.5005 0.4155 0.059 Uiso 1 1 calc R . . C3 C -0.0638(3) 1.4333(4) 0.33227(15) 0.0399(7) Uani 1 1 d . . . Cl1 Cl -0.3333 1.3333 0.47736(10) 0.0681(5) Uani 1 3 d S . . O11 O -0.3333 1.3333 0.4141(5) 0.193(6) Uani 1 3 d S . . O12 O -0.3437(10) 1.2049(7) 0.4864(4) 0.181(3) Uani 1 1 d . . . O2W O -0.6667 0.6667 0.2500 0.246(15) Uani 1 6 d SU A 1 O3W O -0.6667 0.6667 0.2972(13) 0.235(14) Uani 0.60 3 d SPU B 2 O4W O 0.0000 1.0000 0.305(2) 0.242(16) Uani 0.50 3 d SPU C 3 O5W O -0.330(4) 0.824(2) 0.2500 0.131(11) Uani 0.27 2 d SPU . . 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 0.0325(4) 0.0325(4) 0.0423(6) 0.000 0.000 0.01623(19) Fe2 0.0309(4) 0.0309(4) 0.0298(4) 0.000 0.000 0.0152(3) Fe2B 0.0309(4) 0.0309(4) 0.0298(4) 0.000 0.000 0.0152(3) O1 0.0541(15) 0.0474(14) 0.0575(17) 0.0008(12) -0.0169(13) 0.0252(12) O2 0.0537(15) 0.0480(14) 0.0496(14) -0.0073(11) -0.0152(12) 0.0267(12) O1H 0.0368(17) 0.0368(17) 0.039(3) 0.000 0.000 0.0184(8) O1W 0.113(5) 0.102(4) 0.099(4) 0.000 0.000 0.087(4) N1 0.0408(14) 0.0393(14) 0.0478(16) 0.0075(12) 0.0011(12) 0.0192(12) N2 0.055(2) 0.086(3) 0.114(4) 0.047(3) 0.030(2) 0.045(2) N3 0.057(2) 0.082(3) 0.114(4) 0.052(3) 0.030(2) 0.041(2) N4 0.0374(14) 0.0382(14) 0.0456(15) 0.0022(12) -0.0079(12) 0.0143(11) C1 0.0479(19) 0.0473(19) 0.051(2) 0.0121(16) 0.0051(16) 0.0242(16) C2 0.055(2) 0.0384(17) 0.050(2) 0.0001(15) -0.0162(17) 0.0204(16) C3 0.0366(16) 0.0425(17) 0.0380(16) 0.0037(13) -0.0013(13) 0.0179(13) Cl1 0.0638(7) 0.0638(7) 0.0765(13) 0.000 0.000 0.0319(4) O11 0.248(10) 0.248(10) 0.085(7) 0.000 0.000 0.124(5) O12 0.260(10) 0.106(4) 0.183(7) 0.026(4) -0.037(7) 0.097(6) O2W 0.35(2) 0.35(2) 0.034(6) 0.000 0.000 0.176(12) O3W 0.29(2) 0.29(2) 0.133(19) 0.000 0.000 0.143(12) O4W 0.216(19) 0.216(19) 0.30(4) 0.000 0.000 0.108(10) O5W 0.21(3) 0.066(14) 0.11(2) 0.000 0.000 0.063(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_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 2.198(3) 2_675 ? Fe1 N1 2.198(3) 8_456 ? Fe1 N1 2.198(3) 9_666 ? Fe1 N1 2.198(3) 3_465 ? Fe1 N1 2.198(3) . ? Fe1 N1 2.198(3) 7_576 ? Fe2 O1H 1.9169(8) . ? Fe2 O1 2.019(3) 12_366 ? Fe2 O1 2.019(3) 3_365 ? Fe2 O2 2.034(3) . ? Fe2 O2 2.034(3) 10_556 ? Fe2 O1W 2.091(5) . ? Fe2B O1W 1.243(7) . ? Fe2B O1 2.108(5) 12_366 ? Fe2B O1 2.108(5) 3_365 ? Fe2B O2 2.128(5) . ? Fe2B O2 2.128(5) 10_556 ? O1 C3 1.257(4) . ? O1 Fe2 2.019(3) 2_685 ? O1 Fe2B 2.108(5) 2_685 ? O2 C3 1.258(4) . ? O1H Fe2 1.9169(7) 2_685 ? O1H Fe2 1.9169(12) 3_365 ? N1 C1 1.317(5) . ? N1 N2 1.355(5) . ? N2 N3 1.292(5) . ? N3 N4 1.343(5) . ? N4 C1 1.321(5) . ? N4 C2 1.473(4) . ? C2 C3 1.496(5) . ? Cl1 O12 1.379(6) . ? Cl1 O12 1.379(7) 2_685 ? Cl1 O12 1.379(6) 3_365 ? Cl1 O11 1.455(12) . ? 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 N1 180.000(1) 2_675 8_456 ? N1 Fe1 N1 88.02(12) 2_675 9_666 ? N1 Fe1 N1 91.98(12) 8_456 9_666 ? N1 Fe1 N1 91.98(12) 2_675 3_465 ? N1 Fe1 N1 88.02(12) 8_456 3_465 ? N1 Fe1 N1 180.00(13) 9_666 3_465 ? N1 Fe1 N1 91.98(12) 2_675 . ? N1 Fe1 N1 88.02(12) 8_456 . ? N1 Fe1 N1 88.02(12) 9_666 . ? N1 Fe1 N1 91.98(12) 3_465 . ? N1 Fe1 N1 88.02(12) 2_675 7_576 ? N1 Fe1 N1 91.98(12) 8_456 7_576 ? N1 Fe1 N1 91.98(12) 9_666 7_576 ? N1 Fe1 N1 88.02(12) 3_465 7_576 ? N1 Fe1 N1 180.000(1) . 7_576 ? O1H Fe2 O1 95.45(8) . 12_366 ? O1H Fe2 O1 95.45(8) . 3_365 ? O1 Fe2 O1 91.11(19) 12_366 3_365 ? O1H Fe2 O2 95.87(8) . . ? O1 Fe2 O2 168.67(12) 12_366 . ? O1 Fe2 O2 88.18(13) 3_365 . ? O1H Fe2 O2 95.87(8) . 10_556 ? O1 Fe2 O2 88.18(13) 12_366 10_556 ? O1 Fe2 O2 168.67(12) 3_365 10_556 ? O2 Fe2 O2 90.30(17) . 10_556 ? O1H Fe2 O1W 179.5(2) . . ? O1 Fe2 O1W 84.16(16) 12_366 . ? O1 Fe2 O1W 84.16(16) 3_365 . ? O2 Fe2 O1W 84.52(16) . . ? O2 Fe2 O1W 84.52(16) 10_556 . ? O1W Fe2B O1 107.8(3) . 12_366 ? O1W Fe2B O1 107.8(3) . 3_365 ? O1 Fe2B O1 86.3(3) 12_366 3_365 ? O1W Fe2B O2 107.9(3) . . ? O1 Fe2B O2 144.3(3) 12_366 . ? O1 Fe2B O2 83.46(15) 3_365 . ? O1W Fe2B O2 107.9(3) . 10_556 ? O1 Fe2B O2 83.46(15) 12_366 10_556 ? O1 Fe2B O2 144.3(3) 3_365 10_556 ? O2 Fe2B O2 85.3(2) . 10_556 ? C3 O1 Fe2 131.8(2) . 2_685 ? C3 O1 Fe2B 153.2(3) . 2_685 ? Fe2 O1 Fe2B 23.60(15) 2_685 2_685 ? C3 O2 Fe2 130.6(2) . . ? C3 O2 Fe2B 152.4(3) . . ? Fe2 O2 Fe2B 23.38(15) . . ? Fe2 O1H Fe2 120.00(3) . 2_685 ? Fe2 O1H Fe2 120.00(2) . 3_365 ? Fe2 O1H Fe2 120.000(8) 2_685 3_365 ? Fe2B O1W Fe2 0.0(3) . . ? C1 N1 N2 105.2(3) . . ? C1 N1 Fe1 132.9(3) . . ? N2 N1 Fe1 121.7(2) . . ? N3 N2 N1 110.3(3) . . ? N2 N3 N4 107.1(3) . . ? C1 N4 N3 107.6(3) . . ? C1 N4 C2 130.8(3) . . ? N3 N4 C2 121.6(3) . . ? N1 C1 N4 109.8(3) . . ? N4 C2 C3 113.2(3) . . ? O1 C3 O2 127.6(3) . . ? O1 C3 C2 113.9(3) . . ? O2 C3 C2 118.6(3) . . ? O12 Cl1 O12 117.8(2) . 2_685 ? O12 Cl1 O12 117.8(2) . 3_365 ? O12 Cl1 O12 117.8(2) 2_685 3_365 ? O12 Cl1 O11 98.6(4) . . ? O12 Cl1 O11 98.6(4) 2_685 . ? O12 Cl1 O11 98.6(4) 3_365 . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.92 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.081 _refine_diff_density_min -1.007 _refine_diff_density_rms 0.110 #_eof #End of Crystallographic Information File