# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1920 data_fecanbombabs97 _audit_creation_method SHELXL-97 _chemical_name_systematic ; catena-diaqua-\M(O,O',O'',O'''chloranilato)iron(II) hydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H24 Cl8 Fe4 O28' _chemical_formula_weight 316.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 4.9199(2) _cell_length_b 14.255(1) _cell_length_c 14.011(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.980(7) _cell_angle_gamma 90.00 _cell_volume 978.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.9 _cell_measurement_theta_max 56.6 _exptl_crystal_description 'trapezoidal prism' _exptl_crystal_colour black _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.150 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 17.632 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5237 _exptl_absorpt_correction_T_max 0.2480 _exptl_absorpt_process_details 'SHELX-76 (Sheldrick, 1976)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method \w:2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 'no observable decay' _diffrn_reflns_number 1230 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 6.21 _diffrn_reflns_theta_max 74.86 _reflns_number_total 1007 _reflns_number_gt 909 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD-4 Software' _computing_cell_refinement 'CAD-4 Software' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0524P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1007 _refine_ls_number_parameters 87 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0802 _refine_ls_wR_factor_gt 0.0778 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.043 _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 0.12185(4) 0.2500 0.02104(18) Uani 1 2 d S . . Cl1 Cl 0.21915(13) 0.40236(5) 0.03710(5) 0.02744(19) Uani 1 1 d . . . O1 O -0.3162(4) 0.12201(13) 0.13688(14) 0.0253(4) Uani 1 1 d . . . O2 O 0.1003(4) 0.23501(13) 0.15694(12) 0.0239(4) Uani 1 1 d . . . C1 C -0.2937(5) 0.17766(18) 0.06835(18) 0.0192(5) Uani 1 1 d . . . C2 C -0.0596(5) 0.24828(17) 0.08303(17) 0.0197(5) Uani 1 1 d . . . C3 C -0.0369(5) 0.32037(17) 0.01688(17) 0.0199(5) Uani 1 1 d . . . O3 O 0.2139(5) 0.01588(16) 0.18507(17) 0.0346(5) Uani 1 1 d D . . H1 H 0.182(9) -0.038(2) 0.197(3) 0.050(12) Uiso 1 1 d D . . H2 H 0.354(7) 0.031(4) 0.166(4) 0.077(17) Uiso 1 1 d D . . O4 O 0.5000 0.3515(2) 0.2500 0.0415(8) Uani 1 2 d SD . . H3 H 0.388(8) 0.320(3) 0.221(3) 0.070(15) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0248(3) 0.0210(3) 0.0161(3) 0.000 -0.0052(2) 0.000 Cl1 0.0272(3) 0.0264(3) 0.0272(3) 0.0018(2) -0.0064(2) -0.0071(2) O1 0.0246(9) 0.0280(9) 0.0219(9) 0.0069(7) -0.0055(7) -0.0058(7) O2 0.0255(9) 0.0276(9) 0.0168(9) 0.0029(7) -0.0086(7) -0.0046(7) C1 0.0189(10) 0.0212(11) 0.0170(11) 0.0007(9) -0.0015(9) -0.0002(9) C2 0.0198(11) 0.0219(11) 0.0167(11) -0.0010(9) -0.0016(9) -0.0009(9) C3 0.0184(11) 0.0211(11) 0.0194(12) -0.0010(9) -0.0028(9) -0.0010(9) O3 0.0340(11) 0.0299(10) 0.0413(13) -0.0053(9) 0.0115(10) -0.0008(9) O4 0.0459(19) 0.0278(15) 0.046(2) 0.000 -0.0247(16) 0.000 _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 O3 2.094(2) . ? Fe1 O3 2.094(2) 2 ? Fe1 O1 2.1222(19) . ? Fe1 O1 2.1223(19) 2 ? Fe1 O2 2.1580(18) . ? Fe1 O2 2.1581(18) 2 ? Cl1 C3 1.724(3) . ? O1 C1 1.258(3) . ? O2 C2 1.259(3) . ? C1 C3 1.396(3) 7_455 ? C1 C2 1.530(3) . ? C2 C3 1.395(3) . ? C3 C1 1.396(3) 7_455 ? 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 O3 Fe1 O3 87.64(13) . 2 ? O3 Fe1 O1 92.28(9) . . ? O3 Fe1 O1 87.81(9) 2 . ? O3 Fe1 O1 87.81(9) . 2 ? O3 Fe1 O1 92.28(9) 2 2 ? O1 Fe1 O1 179.88(10) . 2 ? O3 Fe1 O2 97.29(8) . . ? O3 Fe1 O2 162.13(8) 2 . ? O1 Fe1 O2 74.88(7) . . ? O1 Fe1 O2 105.03(7) 2 . ? O3 Fe1 O2 162.12(8) . 2 ? O3 Fe1 O2 97.29(8) 2 2 ? O1 Fe1 O2 105.03(7) . 2 ? O1 Fe1 O2 74.88(7) 2 2 ? O2 Fe1 O2 83.26(10) . 2 ? C1 O1 Fe1 117.62(16) . . ? C2 O2 Fe1 116.74(16) . . ? O1 C1 C3 125.5(2) . 7_455 ? O1 C1 C2 115.3(2) . . ? C3 C1 C2 119.2(2) 7_455 . ? O2 C2 C3 125.2(2) . . ? O2 C2 C1 114.9(2) . . ? C3 C2 C1 119.9(2) . . ? C2 C3 C1 120.5(2) . 7_455 ? C2 C3 Cl1 119.33(19) . . ? C1 C3 Cl1 120.0(2) 7_455 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 74.86 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.392 _refine_diff_density_min -0.538 _refine_diff_density_rms 0.099 #===END data_cdcanabs97 _audit_creation_method SHELXL-97 _chemical_name_systematic ; catena-diaqua-\M(O,O',O'',O'''chloranilato)cadmium(II) hydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H24 Cd4 Cl8 O28' _chemical_formula_weight 373.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cd' 'Cd' 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 4.8655(5) _cell_length_b 14.575(1) _cell_length_c 14.252(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.95(1) _cell_angle_gamma 90.00 _cell_volume 1009.34(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.7 _cell_measurement_theta_max 29.6 _exptl_crystal_description parallelipiped _exptl_crystal_colour black _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.014 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 22.451 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.2244 _exptl_absorpt_correction_T_max 0.7351 _exptl_absorpt_process_details 'SHELX-76 (Sheldrick, 1976)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method \w:2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 'no observable decay' _diffrn_reflns_number 1261 _diffrn_reflns_av_R_equivalents 0.0106 _diffrn_reflns_av_sigmaI/netI 0.0181 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 6.07 _diffrn_reflns_theta_max 74.93 _reflns_number_total 1043 _reflns_number_gt 1008 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Software' _computing_cell_refinement 'CAD4 Software' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+2.1723P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1043 _refine_ls_number_parameters 86 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0253 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.0684 _refine_ls_wR_factor_gt 0.0679 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.137 _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 Cd1 Cd 0.0000 0.11497(2) 0.2500 0.02540(14) Uani 1 2 d S . . Cl1 Cl 0.21447(15) 0.40030(5) 0.03841(5) 0.02570(18) Uani 1 1 d . . . O1 O -0.3271(5) 0.11960(16) 0.12965(18) 0.0281(5) Uani 1 1 d . . . O2 O 0.0949(4) 0.23582(16) 0.15319(15) 0.0246(5) Uani 1 1 d . . . C1 C -0.2963(6) 0.1770(2) 0.0657(2) 0.0190(6) Uani 1 1 d . . . C2 C -0.0628(6) 0.2478(2) 0.0817(2) 0.0189(6) Uani 1 1 d . . . C3 C -0.0404(6) 0.3188(2) 0.0178(2) 0.0202(6) Uani 1 1 d . . . O3 O 0.2275(7) 0.0025(2) 0.1805(3) 0.0485(8) Uani 1 1 d D . . H1 H 0.368(7) 0.009(4) 0.152(4) 0.065(18) Uiso 1 1 d D . . H2 H 0.202(14) -0.0507(16) 0.196(5) 0.08(2) Uiso 1 1 d D . . O4 O 0.5000 0.3449(3) 0.2500 0.0396(9) Uani 1 2 d S . . H3 H 0.391(10) 0.318(4) 0.218(4) 0.051(15) Uiso 1 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 Cd1 0.0349(2) 0.01996(19) 0.02020(19) 0.000 -0.00965(13) 0.000 Cl1 0.0254(4) 0.0236(3) 0.0274(4) 0.0003(3) -0.0055(3) -0.0063(3) O1 0.0303(12) 0.0295(13) 0.0235(12) 0.0086(9) -0.0084(9) -0.0074(9) O2 0.0270(11) 0.0266(11) 0.0194(10) 0.0036(9) -0.0071(9) -0.0046(9) C1 0.0199(13) 0.0201(13) 0.0166(13) 0.0007(11) -0.0015(10) 0.0006(11) C2 0.0190(13) 0.0216(13) 0.0158(13) -0.0018(10) -0.0028(10) 0.0007(11) C3 0.0191(13) 0.0216(14) 0.0195(14) -0.0007(11) -0.0033(10) -0.0030(11) O3 0.0456(17) 0.0387(16) 0.064(2) -0.0102(15) 0.0285(15) -0.0036(14) O4 0.043(2) 0.0247(18) 0.048(2) 0.000 -0.0229(19) 0.000 _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 Cd1 O3 2.238(3) . ? Cd1 O3 2.238(3) 2 ? Cd1 O1 2.280(3) . ? Cd1 O1 2.280(3) 2 ? Cd1 O2 2.299(2) . ? Cd1 O2 2.299(2) 2 ? Cl1 C3 1.731(3) . ? O1 C1 1.252(4) . ? O2 C2 1.256(3) . ? C1 C3 1.398(4) 7_455 ? C1 C2 1.543(4) . ? C2 C3 1.387(4) . ? C3 C1 1.398(4) 7_455 ? 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 O3 Cd1 O3 85.74(16) . 2 ? O3 Cd1 O1 91.77(12) . . ? O3 Cd1 O1 90.71(12) 2 . ? O3 Cd1 O1 90.71(12) . 2 ? O3 Cd1 O1 91.77(12) 2 2 ? O1 Cd1 O1 176.61(12) . 2 ? O3 Cd1 O2 100.18(11) . . ? O3 Cd1 O2 161.13(11) 2 . ? O1 Cd1 O2 71.33(8) . . ? O1 Cd1 O2 105.95(8) 2 . ? O3 Cd1 O2 161.13(11) . 2 ? O3 Cd1 O2 100.18(11) 2 2 ? O1 Cd1 O2 105.95(8) . 2 ? O1 Cd1 O2 71.33(8) 2 2 ? O2 Cd1 O2 79.97(11) . 2 ? C1 O1 Cd1 117.5(2) . . ? C2 O2 Cd1 117.41(19) . . ? O1 C1 C3 124.4(3) . 7_455 ? O1 C1 C2 117.0(3) . . ? C3 C1 C2 118.6(3) 7_455 . ? O2 C2 C3 124.9(3) . . ? O2 C2 C1 116.2(3) . . ? C3 C2 C1 118.9(3) . . ? C2 C3 C1 122.1(3) . 7_455 ? C2 C3 Cl1 118.7(2) . . ? C1 C3 Cl1 119.0(2) 7_455 . ? _diffrn_measured_fraction_theta_max 1.001 _diffrn_reflns_theta_full 74.93 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.757 _refine_diff_density_min -0.814 _refine_diff_density_rms 0.121 #===END data_fecankl2abs97 _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetraaquatris(chloranilato)diiron(III) tetrahydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H16 Cl6 Fe2 O20' _chemical_formula_weight 876.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.909(2) _cell_length_b 9.894(4) _cell_length_c 11.391(3) _cell_angle_alpha 74.91(2) _cell_angle_beta 78.45(2) _cell_angle_gamma 75.59(3) _cell_volume 720.5(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.8 _cell_measurement_theta_max 24.1 _exptl_crystal_description 'hexagonal prism' _exptl_crystal_colour 'black' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.021 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 438 _exptl_absorpt_coefficient_mu 14.039 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.2166 _exptl_absorpt_correction_T_max 0.4179 _exptl_absorpt_process_details 'SHELX-76 (G. Sheldrick, 1976)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method \w:2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 'No obsevable decay' _diffrn_reflns_number 3321 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.06 _diffrn_reflns_theta_max 75.17 _reflns_number_total 2852 _reflns_number_gt 2465 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD-4 Software' _computing_cell_refinement 'CAD-4 Software' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0887P)^2^+0.0959P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2852 _refine_ls_number_parameters 223 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1265 _refine_ls_wR_factor_gt 0.1204 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.049 _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 0.17939(8) 0.19912(5) 0.25406(5) 0.02048(17) Uani 1 1 d . . . Cl1 Cl 0.12616(13) 0.10044(11) -0.14700(9) 0.0318(2) Uani 1 1 d . . . O1 O 0.1617(4) 0.1624(3) 0.0906(2) 0.0242(5) Uani 1 1 d . . . O2 O 0.4612(4) 0.0770(3) 0.2137(2) 0.0222(5) Uani 1 1 d . . . C1 C 0.3136(5) 0.0852(4) 0.0426(3) 0.0197(6) Uani 1 1 d . . . C2 C 0.4935(5) 0.0356(3) 0.1140(3) 0.0202(7) Uani 1 1 d . . . C3 C 0.3298(5) 0.0464(4) -0.0680(3) 0.0215(7) Uani 1 1 d . . . Cl2 Cl 0.24254(15) 0.38110(10) 0.60799(9) 0.0321(2) Uani 1 1 d . . . Cl3 Cl 0.32021(16) 0.67676(10) 0.03912(9) 0.0332(2) Uani 1 1 d . . . O3 O 0.2636(4) 0.3817(3) 0.1634(2) 0.0262(5) Uani 1 1 d . . . O4 O 0.2452(4) 0.2573(3) 0.3924(2) 0.0249(5) Uani 1 1 d . . . O5 O 0.2407(5) 0.6911(3) 0.4898(3) 0.0356(7) Uani 1 1 d . . . O6 O 0.2945(5) 0.8114(3) 0.2500(3) 0.0337(6) Uani 1 1 d . . . C4 C 0.2758(5) 0.4610(4) 0.2339(3) 0.0214(7) Uani 1 1 d . . . C5 C 0.2637(5) 0.3888(4) 0.3683(3) 0.0215(7) Uani 1 1 d . . . C6 C 0.2646(5) 0.4631(4) 0.4540(3) 0.0229(7) Uani 1 1 d . . . C7 C 0.2631(5) 0.6130(4) 0.4186(4) 0.0246(7) Uani 1 1 d . . . C8 C 0.2894(5) 0.6840(4) 0.2796(4) 0.0246(7) Uani 1 1 d . . . C9 C 0.2990(6) 0.5998(4) 0.1936(3) 0.0238(7) Uani 1 1 d . . . O7 O -0.1133(4) 0.3030(3) 0.2698(3) 0.0306(6) Uani 1 1 d D . . H1 H -0.165(8) 0.309(6) 0.338(3) 0.054(12) Uiso 1 1 d D . . H2 H -0.124(9) 0.372(4) 0.215(4) 0.054(12) Uiso 1 1 d D . . O8 O 0.0906(4) 0.0269(3) 0.3620(3) 0.0270(6) Uani 1 1 d D . . H3 H 0.172(7) -0.044(4) 0.355(6) 0.064(14) Uiso 1 1 d D . . H4 H -0.025(5) 0.020(7) 0.376(6) 0.064(14) Uiso 1 1 d D . . O9 O 0.2872(5) -0.0062(4) 0.5865(3) 0.0408(7) Uani 1 1 d . . . O10 O 0.1885(6) 0.4507(4) 0.8972(3) 0.0472(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0284(3) 0.0180(3) 0.0159(3) -0.0053(2) -0.0030(2) -0.0048(2) Cl1 0.0280(4) 0.0436(5) 0.0254(5) -0.0122(4) -0.0130(3) 0.0016(3) O1 0.0275(13) 0.0262(12) 0.0200(13) -0.0095(10) -0.0066(10) -0.0005(10) O2 0.0276(12) 0.0230(11) 0.0178(13) -0.0084(10) -0.0053(9) -0.0032(9) C1 0.0217(15) 0.0195(14) 0.0182(18) -0.0028(13) -0.0044(12) -0.0050(11) C2 0.0277(17) 0.0193(15) 0.0148(17) -0.0011(12) -0.0060(13) -0.0076(12) C3 0.0235(16) 0.0232(15) 0.0197(18) -0.0054(13) -0.0062(13) -0.0048(12) Cl2 0.0416(5) 0.0365(5) 0.0190(5) -0.0045(4) -0.0070(4) -0.0093(4) Cl3 0.0495(6) 0.0255(4) 0.0213(5) -0.0007(3) -0.0009(4) -0.0098(4) O3 0.0401(15) 0.0227(12) 0.0177(13) -0.0053(10) -0.0024(10) -0.0108(10) O4 0.0381(14) 0.0190(11) 0.0190(13) -0.0025(10) -0.0072(10) -0.0079(10) O5 0.0478(17) 0.0346(15) 0.0309(17) -0.0187(13) 0.0005(13) -0.0131(13) O6 0.0496(17) 0.0214(13) 0.0329(17) -0.0065(11) -0.0040(13) -0.0135(11) C4 0.0250(16) 0.0197(15) 0.0183(18) -0.0037(13) -0.0027(13) -0.0036(12) C5 0.0252(16) 0.0213(15) 0.0185(18) -0.0053(13) -0.0058(13) -0.0024(12) C6 0.0289(17) 0.0265(17) 0.0153(18) -0.0044(14) -0.0036(13) -0.0091(13) C7 0.0258(17) 0.0257(17) 0.025(2) -0.0104(15) -0.0026(14) -0.0062(13) C8 0.0254(17) 0.0204(15) 0.029(2) -0.0073(14) -0.0022(14) -0.0054(12) C9 0.0316(18) 0.0223(16) 0.0167(18) -0.0050(14) -0.0001(13) -0.0063(13) O7 0.0333(14) 0.0311(14) 0.0226(16) -0.0048(12) -0.0018(11) -0.0008(11) O8 0.0336(14) 0.0200(12) 0.0258(15) -0.0028(11) -0.0016(11) -0.0071(10) O9 0.0436(17) 0.0515(18) 0.0316(17) -0.0077(14) -0.0104(13) -0.0152(14) O10 0.062(2) 0.0423(18) 0.0337(19) 0.0038(14) -0.0193(16) -0.0072(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O4 1.978(3) . ? Fe1 O8 1.980(3) . ? Fe1 O3 1.995(3) . ? Fe1 O1 2.020(3) . ? Fe1 O7 2.023(3) . ? Fe1 O2 2.055(3) . ? Cl1 C3 1.719(3) . ? O1 C1 1.254(4) . ? O2 C2 1.266(4) . ? C1 C3 1.386(5) . ? C1 C2 1.530(4) . ? C2 C3 1.377(5) 2_655 ? C3 C2 1.377(5) 2_655 ? Cl2 C6 1.724(4) . ? Cl3 C9 1.718(4) . ? O3 C4 1.287(4) . ? O4 C5 1.291(4) . ? O5 C7 1.223(4) . ? O6 C8 1.225(4) . ? C4 C9 1.369(5) . ? C4 C5 1.506(5) . ? C5 C6 1.368(5) . ? C6 C7 1.430(5) . ? C7 C8 1.550(5) . ? C8 C9 1.425(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 O4 Fe1 O8 92.92(11) . . ? O4 Fe1 O3 80.65(11) . . ? O8 Fe1 O3 173.15(11) . . ? O4 Fe1 O1 167.11(11) . . ? O8 Fe1 O1 98.34(12) . . ? O3 Fe1 O1 88.32(11) . . ? O4 Fe1 O7 95.64(12) . . ? O8 Fe1 O7 87.98(12) . . ? O3 Fe1 O7 90.28(12) . . ? O1 Fe1 O7 91.02(11) . . ? O4 Fe1 O2 95.43(11) . . ? O8 Fe1 O2 89.85(11) . . ? O3 Fe1 O2 93.11(11) . . ? O1 Fe1 O2 78.43(10) . . ? O7 Fe1 O2 168.81(11) . . ? C1 O1 Fe1 116.7(2) . . ? C2 O2 Fe1 115.7(2) . . ? O1 C1 C3 125.4(3) . . ? O1 C1 C2 115.1(3) . . ? C3 C1 C2 119.5(3) . . ? O2 C2 C3 126.0(3) . 2_655 ? O2 C2 C1 114.0(3) . . ? C3 C2 C1 120.0(3) 2_655 . ? C2 C3 C1 120.5(3) 2_655 . ? C2 C3 Cl1 120.2(3) 2_655 . ? C1 C3 Cl1 119.4(3) . . ? C4 O3 Fe1 113.7(2) . . ? C5 O4 Fe1 114.2(2) . . ? O3 C4 C9 124.3(3) . . ? O3 C4 C5 114.6(3) . . ? C9 C4 C5 121.1(3) . . ? O4 C5 C6 125.1(3) . . ? O4 C5 C4 114.2(3) . . ? C6 C5 C4 120.6(3) . . ? C5 C6 C7 120.5(3) . . ? C5 C6 Cl2 120.3(3) . . ? C7 C6 Cl2 118.9(3) . . ? O5 C7 C6 125.0(4) . . ? O5 C7 C8 116.8(3) . . ? C6 C7 C8 118.2(3) . . ? O6 C8 C9 123.6(4) . . ? O6 C8 C7 117.7(3) . . ? C9 C8 C7 118.7(3) . . ? C4 C9 C8 120.3(3) . . ? C4 C9 Cl3 119.8(3) . . ? C8 C9 Cl3 119.8(3) . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 75.17 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 0.871 _refine_diff_density_min -0.590 _refine_diff_density_rms 0.112 #===END