Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Matti Haukka' _publ_contact_author_address ; Department of Chemistry University of Joensuu PO Box 111 Joensuu FI-80101 FINLAND ; _publ_contact_author_email MATTI.HAUKKA@JOENSUU.FI _publ_section_title ; Use of Iron Containing Metal Surfaces for the Syntheses of Trinuclear [Ru2Cl2(m-Cl)4(CO)6FeL2] (L=H2O, EtOH) compounds ; loop_ _publ_author_name 'Matti Haukka' 'Minna Jakonen' 'Mirja Kallinen' 'Taina Nivajarvi' data_compound_1 _database_code_depnum_ccdc_archive 'CCDC 299525' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Fe H12 O6, 2(C3 Cl3 O3 Ru)' _chemical_formula_sum 'C6 H12 Cl6 Fe O12 Ru2' _chemical_formula_weight 746.85 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' 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' Ru Ru -1.2594 0.8363 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.2958(6) _cell_length_b 6.4156(4) _cell_length_c 13.9122(14) _cell_angle_alpha 87.513(5) _cell_angle_beta 77.295(4) _cell_angle_gamma 80.322(6) _cell_volume 540.36(8) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10445 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.295 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 360 _exptl_absorpt_coefficient_mu 2.832 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5035 _exptl_absorpt_correction_T_max 0.9232 _exptl_absorpt_process_details 'Xprep in Shelxtl v.6.14-1 (Sheldrick, 2005)' _publ_section_exptl_refinement ; The H2O hydrogens were located from the difference Fourier but constrained constrained to ride on their parent atoms (U~iso~ = 1.5 U~eq~(parent atom)). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10445 _diffrn_reflns_av_R_equivalents 0.0812 _diffrn_reflns_av_sigmaI/netI 0.0762 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2472 _reflns_number_gt 1782 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.0e (Crystal Impact GbR, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+0.4318P] 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 2472 _refine_ls_number_parameters 124 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.0865 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 Ru1 Ru 0.86984(7) 0.87401(6) 0.80968(3) 0.01988(14) Uani 1 1 d . . . Fe1 Fe 0.5000 0.5000 0.5000 0.0209(2) Uani 1 2 d S . . Cl1 Cl 0.8277(2) 0.57083(18) 0.72262(10) 0.0255(3) Uani 1 1 d . . . Cl2 Cl 1.0583(2) 1.01222(18) 0.65601(10) 0.0245(3) Uani 1 1 d . . . Cl3 Cl 0.5212(2) 1.05312(19) 0.78038(10) 0.0278(3) Uani 1 1 d . . . O1 O 0.9335(6) 1.2489(6) 0.9181(3) 0.0329(9) Uani 1 1 d . . . O2 O 0.5966(7) 0.7048(6) 0.9937(3) 0.0341(9) Uani 1 1 d . . . O3 O 1.2898(6) 0.6133(6) 0.8517(3) 0.0320(9) Uani 1 1 d . . . O4 O 0.5709(6) 0.7782(5) 0.5597(3) 0.0284(9) Uani 1 1 d . . . H4A H 0.6575 0.7605 0.6053 0.043 Uiso 1 1 d . . . H4B H 0.4591 0.8651 0.5804 0.043 Uiso 1 1 d . . . O5 O 0.3488(6) 0.4146(5) 0.6431(3) 0.0268(8) Uani 1 1 d . . . H5A H 0.4095 0.3009 0.6588 0.040 Uiso 1 1 d . . . H5B H 0.2037 0.4084 0.6641 0.040 Uiso 1 1 d . . . O6 O 0.8102(6) 0.3312(6) 0.5137(3) 0.0297(9) Uani 1 1 d . . . H6A H 0.8389 0.2718 0.5651 0.045 Uiso 1 1 d . . . H6B H 0.8724 0.2550 0.4664 0.045 Uiso 1 1 d . . . C1 C 0.9076(8) 1.1148(8) 0.8764(4) 0.0254(12) Uani 1 1 d . . . C2 C 0.7024(9) 0.7674(8) 0.9256(4) 0.0242(12) Uani 1 1 d . . . C3 C 1.1431(9) 0.7131(8) 0.8330(4) 0.0227(11) 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 Ru1 0.0203(2) 0.0187(2) 0.0211(2) -0.00034(16) -0.00619(18) -0.00213(16) Fe1 0.0235(6) 0.0185(5) 0.0208(6) 0.0006(4) -0.0062(5) -0.0022(4) Cl1 0.0271(7) 0.0217(6) 0.0287(8) -0.0028(5) -0.0085(6) -0.0032(5) Cl2 0.0273(7) 0.0216(6) 0.0243(7) 0.0011(5) -0.0060(6) -0.0027(5) Cl3 0.0248(7) 0.0249(6) 0.0341(8) 0.0002(6) -0.0096(6) -0.0013(5) O1 0.038(2) 0.030(2) 0.034(2) -0.0054(18) -0.0104(19) -0.0105(18) O2 0.038(2) 0.037(2) 0.027(2) 0.0032(19) -0.005(2) -0.0096(19) O3 0.030(2) 0.030(2) 0.037(3) 0.0014(18) -0.0115(19) -0.0040(18) O4 0.031(2) 0.0273(19) 0.029(2) -0.0031(16) -0.0124(18) -0.0008(16) O5 0.027(2) 0.0297(19) 0.023(2) 0.0053(16) -0.0058(17) -0.0036(16) O6 0.033(2) 0.035(2) 0.019(2) -0.0066(16) -0.0072(17) 0.0042(17) C1 0.020(3) 0.029(3) 0.024(3) 0.007(2) -0.003(2) 0.000(2) C2 0.025(3) 0.018(3) 0.035(4) -0.004(2) -0.018(3) -0.002(2) C3 0.030(3) 0.018(2) 0.022(3) -0.004(2) -0.006(2) -0.009(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 Ru1 C2 1.892(6) . ? Ru1 C1 1.910(6) . ? Ru1 C3 1.937(6) . ? Ru1 Cl3 2.4102(13) . ? Ru1 Cl2 2.4162(14) . ? Ru1 Cl1 2.4166(12) . ? Fe1 O5 2.102(4) . ? Fe1 O5 2.102(4) 2_666 ? Fe1 O6 2.111(4) . ? Fe1 O6 2.111(4) 2_666 ? Fe1 O4 2.153(3) 2_666 ? Fe1 O4 2.153(3) . ? O1 C1 1.112(6) . ? O2 C2 1.132(7) . ? O3 C3 1.106(6) . ? O4 H4A 0.9153 . ? O4 H4B 0.8257 . ? O5 H5A 0.8090 . ? O5 H5B 0.9029 . ? O6 H6A 0.8358 . ? O6 H6B 0.8213 . ? 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 C2 Ru1 C1 92.6(2) . . ? C2 Ru1 C3 92.3(2) . . ? C1 Ru1 C3 92.0(2) . . ? C2 Ru1 Cl3 85.88(15) . . ? C1 Ru1 Cl3 91.24(15) . . ? C3 Ru1 Cl3 176.32(14) . . ? C2 Ru1 Cl2 175.46(15) . . ? C1 Ru1 Cl2 89.56(16) . . ? C3 Ru1 Cl2 91.62(16) . . ? Cl3 Ru1 Cl2 90.09(5) . . ? C2 Ru1 Cl1 88.50(14) . . ? C1 Ru1 Cl1 178.87(17) . . ? C3 Ru1 Cl1 87.64(14) . . ? Cl3 Ru1 Cl1 89.12(4) . . ? Cl2 Ru1 Cl1 89.36(5) . . ? O5 Fe1 O5 180.0 . 2_666 ? O5 Fe1 O6 92.26(14) . . ? O5 Fe1 O6 87.74(14) 2_666 . ? O5 Fe1 O6 87.74(14) . 2_666 ? O5 Fe1 O6 92.26(14) 2_666 2_666 ? O6 Fe1 O6 179.999(2) . 2_666 ? O5 Fe1 O4 91.01(14) . 2_666 ? O5 Fe1 O4 88.99(14) 2_666 2_666 ? O6 Fe1 O4 89.39(13) . 2_666 ? O6 Fe1 O4 90.61(13) 2_666 2_666 ? O5 Fe1 O4 88.99(14) . . ? O5 Fe1 O4 91.01(14) 2_666 . ? O6 Fe1 O4 90.61(13) . . ? O6 Fe1 O4 89.39(13) 2_666 . ? O4 Fe1 O4 180.000(1) 2_666 . ? Fe1 O4 H4A 118.1 . . ? Fe1 O4 H4B 113.0 . . ? H4A O4 H4B 109.3 . . ? Fe1 O5 H5A 110.8 . . ? Fe1 O5 H5B 125.1 . . ? H5A O5 H5B 104.0 . . ? Fe1 O6 H6A 125.4 . . ? Fe1 O6 H6B 113.7 . . ? H6A O6 H6B 108.9 . . ? O1 C1 Ru1 176.9(5) . . ? O2 C2 Ru1 177.9(5) . . ? O3 C3 Ru1 174.7(5) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O4 H4A Cl1 0.92 2.34 3.186(4) 154.5 . yes O4 H4B Cl2 0.83 2.55 3.333(4) 159.7 1_455 yes O5 H5A Cl3 0.81 2.41 3.143(4) 151.7 1_545 yes O5 H5B Cl1 0.90 2.40 3.223(4) 152.0 1_455 yes O5 H5B Cl2 0.90 2.86 3.383(4) 118.5 1_445 no O6 H6A Cl2 0.84 2.47 3.237(4) 153.3 1_545 yes O6 H6A Cl1 0.84 2.96 3.378(4) 113.5 . no O6 H6B Cl2 0.82 2.39 3.177(4) 161.0 2_766 yes O6 H6B Cl1 0.82 3.16 3.662(4) 121.7 2_766 no _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.702 _refine_diff_density_min -0.855 _refine_diff_density_rms 0.166 #===END======================================================================== data_compound_1b _database_code_depnum_ccdc_archive 'CCDC 299526' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Fe H12 O6, 2(C3 Cl3 O3 Ru), 2(H2 O)' _chemical_formula_sum 'C6 H16 Cl6 Fe O14 Ru2' _chemical_formula_weight 782.88 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' 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' Ru Ru -1.2594 0.8363 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.2478(5) _cell_length_b 7.1825(7) _cell_length_c 14.7889(16) _cell_angle_alpha 92.023(4) _cell_angle_beta 97.730(4) _cell_angle_gamma 115.042(5) _cell_volume 592.65(10) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3545 _cell_measurement_theta_min 3.15 _cell_measurement_theta_max 25.98 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 380 _exptl_absorpt_coefficient_mu 2.594 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3882 _exptl_absorpt_correction_T_max 0.8813 _exptl_absorpt_process_details 'Xprep in Shelxtl v.6.14-1 (Sheldrick, 2005)' _publ_section_exptl_refinement ; The H2O hydrogens were located from the difference Fourier but constrained constrained to ride on their parent atoms (U~iso~ = 1.5 U~eq~(parent atom)). ; _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 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3545 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0452 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 25.98 _reflns_number_total 1972 _reflns_number_gt 1823 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.0e (Crystal Impact GbR, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+0.8814P] 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 1972 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0889 _refine_ls_wR_factor_gt 0.0857 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 C1 C 0.7191(7) 0.5972(7) 0.1061(3) 0.0267(9) Uani 1 1 d . . . C2 C 0.7660(7) 0.2389(6) 0.0653(3) 0.0270(9) Uani 1 1 d . . . C3 C 0.4167(8) 0.2243(6) 0.1634(3) 0.0244(9) Uani 1 1 d . . . O1 O 0.6991(6) 0.7210(5) 0.0657(2) 0.0377(8) Uani 1 1 d . . . O2 O 0.7788(6) 0.1498(5) 0.0043(2) 0.0358(7) Uani 1 1 d . . . O3 O 0.2213(6) 0.1180(5) 0.1555(2) 0.0331(7) Uani 1 1 d . . . O4 O 0.7447(6) -0.1306(5) 0.4875(2) 0.0299(7) Uani 1 1 d . . . H4A H 0.7658 -0.1696 0.4359 0.045 Uiso 1 1 d . . . H4B H 0.7403 -0.2212 0.5236 0.045 Uiso 1 1 d . . . O5 O 0.7580(5) 0.2932(4) 0.48018(19) 0.0253(6) Uani 1 1 d . . . H5A H 0.7825 0.3406 0.4288 0.038 Uiso 1 1 d . . . H5B H 0.7558 0.3870 0.5162 0.038 Uiso 1 1 d . . . O6 O 0.3561(6) -0.0667(5) 0.3593(2) 0.0360(8) Uani 1 1 d . . . H6A H 0.4632 -0.0446 0.3259 0.054 Uiso 1 1 d . . . H6B H 0.2290 -0.1680 0.3327 0.054 Uiso 1 1 d . . . O99 O 1.2753(5) 0.4227(5) 0.3979(2) 0.0304(7) Uani 1 1 d . . . H99A H 1.3839 0.4690 0.3648 0.046 Uiso 1 1 d . . . H99B H 1.1538 0.3592 0.3564 0.046 Uiso 1 1 d . . . Cl1 Cl 0.80657(18) 0.12746(15) 0.26103(7) 0.0267(2) Uani 1 1 d . . . Cl3 Cl 1.18460(17) 0.57741(15) 0.18430(7) 0.0270(2) Uani 1 1 d . . . Cl2 Cl 0.77765(18) 0.57963(15) 0.31463(7) 0.0262(2) Uani 1 1 d . . . Fe1 Fe 0.5000 0.0000 0.5000 0.0192(2) Uani 1 2 d S . . Ru1 Ru 0.75659(5) 0.38800(5) 0.17264(2) 0.02047(14) 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 C1 0.023(2) 0.030(2) 0.026(2) -0.0011(19) 0.0015(16) 0.0108(18) C2 0.023(2) 0.025(2) 0.034(2) 0.0097(19) 0.0032(17) 0.0111(17) C3 0.036(3) 0.025(2) 0.0175(19) -0.0026(16) 0.0030(16) 0.019(2) O1 0.0398(19) 0.0340(18) 0.0415(19) 0.0122(16) 0.0017(15) 0.0188(15) O2 0.049(2) 0.0364(18) 0.0259(16) -0.0005(14) 0.0113(14) 0.0203(15) O3 0.0232(17) 0.0297(16) 0.0448(19) -0.0029(14) 0.0066(14) 0.0101(14) O4 0.0383(18) 0.0303(16) 0.0288(16) 0.0028(13) 0.0065(13) 0.0219(14) O5 0.0240(15) 0.0218(14) 0.0262(15) 0.0017(12) 0.0060(12) 0.0055(12) O6 0.0354(18) 0.0329(17) 0.0234(15) 0.0012(13) -0.0018(13) 0.0012(14) O99 0.0280(16) 0.0362(17) 0.0288(15) 0.0016(13) 0.0011(12) 0.0168(13) Cl1 0.0280(5) 0.0244(5) 0.0294(5) 0.0070(4) 0.0047(4) 0.0129(4) Cl3 0.0210(5) 0.0263(5) 0.0311(5) 0.0025(4) 0.0030(4) 0.0083(4) Cl2 0.0283(5) 0.0262(5) 0.0246(5) -0.0012(4) 0.0014(4) 0.0134(4) Fe1 0.0166(4) 0.0180(4) 0.0217(4) 0.0002(3) 0.0016(3) 0.0069(3) Ru1 0.0203(2) 0.0206(2) 0.0203(2) 0.00163(14) 0.00118(14) 0.00941(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 C1 O1 1.129(5) . ? C1 Ru1 1.903(5) . ? C2 O2 1.120(5) . ? C2 Ru1 1.905(5) . ? C3 O3 1.119(5) . ? C3 Ru1 1.926(4) . ? O4 Fe1 2.128(3) . ? O4 H4A 0.8497 . ? O4 H4B 0.8502 . ? O5 Fe1 2.101(3) . ? O5 H5A 0.8499 . ? O5 H5B 0.8501 . ? O6 Fe1 2.104(3) . ? O6 H6A 0.8502 . ? O6 H6B 0.8499 . ? O99 H99A 0.8495 . ? O99 H99B 0.8505 . ? Cl1 Ru1 2.4219(10) . ? Cl3 Ru1 2.4106(10) . ? Cl2 Ru1 2.4269(10) . ? Fe1 O5 2.101(3) 2_656 ? Fe1 O6 2.104(3) 2_656 ? Fe1 O4 2.128(3) 2_656 ? 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 C1 Ru1 178.9(4) . . ? O2 C2 Ru1 177.1(4) . . ? O3 C3 Ru1 175.2(3) . . ? Fe1 O4 H4A 122.5 . . ? Fe1 O4 H4B 115.6 . . ? H4A O4 H4B 107.8 . . ? Fe1 O5 H5A 125.9 . . ? Fe1 O5 H5B 111.1 . . ? H5A O5 H5B 107.7 . . ? Fe1 O6 H6A 112.3 . . ? Fe1 O6 H6B 128.6 . . ? H6A O6 H6B 107.7 . . ? H99A O99 H99B 99.8 . . ? O5 Fe1 O5 180.0 . 2_656 ? O5 Fe1 O6 92.00(11) . . ? O5 Fe1 O6 88.00(11) 2_656 . ? O5 Fe1 O6 88.00(11) . 2_656 ? O5 Fe1 O6 92.00(11) 2_656 2_656 ? O6 Fe1 O6 179.999(1) . 2_656 ? O5 Fe1 O4 89.05(12) . 2_656 ? O5 Fe1 O4 90.95(12) 2_656 2_656 ? O6 Fe1 O4 86.75(13) . 2_656 ? O6 Fe1 O4 93.25(13) 2_656 2_656 ? O5 Fe1 O4 90.95(12) . . ? O5 Fe1 O4 89.05(12) 2_656 . ? O6 Fe1 O4 93.25(13) . . ? O6 Fe1 O4 86.75(13) 2_656 . ? O4 Fe1 O4 179.999(1) 2_656 . ? C1 Ru1 C2 93.16(18) . . ? C1 Ru1 C3 93.45(17) . . ? C2 Ru1 C3 91.65(17) . . ? C1 Ru1 Cl3 89.00(13) . . ? C2 Ru1 Cl3 86.79(12) . . ? C3 Ru1 Cl3 177.17(12) . . ? C1 Ru1 Cl1 178.49(13) . . ? C2 Ru1 Cl1 88.31(12) . . ? C3 Ru1 Cl1 86.85(12) . . ? Cl3 Ru1 Cl1 90.75(4) . . ? C1 Ru1 Cl2 89.45(13) . . ? C2 Ru1 Cl2 175.15(12) . . ? C3 Ru1 Cl2 92.27(11) . . ? Cl3 Ru1 Cl2 89.17(4) . . ? Cl1 Ru1 Cl2 89.06(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4A Cl2 0.85 2.53 3.322(3) 156.3 1_545 O4 H4A Cl1 0.85 3.38 3.870(3) 119.8 . O4 H4B O99 0.85 1.87 2.716(4) 179.0 2_756 O5 H5A Cl2 0.85 2.46 3.235(3) 152.6 . O5 H5A Cl1 0.85 2.92 3.509(3) 127.7 . O5 H5A O99 0.85 2.98 3.373(4) 110.4 . O5 H5B O99 0.85 1.92 2.767(4) 174.2 2_766 O6 H6A Cl1 0.85 2.33 3.146(3) 160.4 . O6 H6B Cl2 0.85 2.60 3.379(3) 153.5 1_445 O6 H6B Cl3 0.85 2.71 3.294(3) 126.9 1_445 O99 H99A Cl2 0.85 2.47 3.284(3) 160.2 1_655 O99 H99B Cl1 0.85 2.33 3.165(3) 168.0 . O99 H99B Cl3 0.85 3.02 3.441(3) 112.7 . O99 H99B Cl2 0.85 3.35 3.806(3) 116.3 . _diffrn_measured_fraction_theta_max 0.850 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.850 _refine_diff_density_max 0.708 _refine_diff_density_min -1.081 _refine_diff_density_rms 0.141 #===END======================================================================== data_compound_1c _database_code_depnum_ccdc_archive 'CCDC 299527' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Fe H12 O6, 2(C3 Cl3 O3 Ru), 2(H2 O)' _chemical_formula_sum 'C6 H16 Cl6 Fe O14 Ru2' _chemical_formula_weight 782.88 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' 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' Ru Ru -1.2594 0.8363 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.22440(10) _cell_length_b 13.0253(2) _cell_length_c 15.4469(4) _cell_angle_alpha 70.9850(10) _cell_angle_beta 85.5080(10) _cell_angle_gamma 89.0770(10) _cell_volume 1180.32(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 20364 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 2.605 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4625 _exptl_absorpt_correction_T_max 0.8187 _exptl_absorpt_process_details 'Xprep in Shelxtl v.6.14-1 (Sheldrick, 2005)' _publ_section_exptl_refinement ; The H2O hydrogens were located from the difference Fourier but constrained constrained to ride on their parent atoms (U~iso~ = 1.5 U~eq~(parent atom)). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13322 _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_sigmaI/netI 0.0344 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 27.44 _reflns_number_total 5342 _reflns_number_gt 4725 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.0e (Crystal Impact GbR, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0246P)^2^+0.5752P] 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 5342 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0273 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0631 _refine_ls_wR_factor_gt 0.0605 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 C1 C 1.1458(3) 0.25716(17) -0.10814(14) 0.0160(4) Uani 1 1 d . . . C2 C 1.2893(3) 0.47252(16) -0.16339(14) 0.0148(4) Uani 1 1 d . . . C3 C 0.8970(3) 0.41564(15) -0.06746(14) 0.0155(4) Uani 1 1 d . . . C4 C 0.3782(3) 0.24979(17) 0.10291(14) 0.0164(4) Uani 1 1 d . . . C5 C 0.6256(3) 0.09021(16) 0.06336(14) 0.0158(4) Uani 1 1 d . . . C6 C 0.2340(3) 0.03508(16) 0.16128(14) 0.0156(4) Uani 1 1 d . . . O1 O 1.2074(3) 0.17459(12) -0.06776(11) 0.0238(3) Uani 1 1 d . . . O2 O 1.4278(2) 0.52159(12) -0.15449(11) 0.0208(3) Uani 1 1 d . . . O3 O 0.8066(2) 0.42814(13) -0.00559(11) 0.0219(3) Uani 1 1 d . . . O4 O 0.3142(3) 0.33157(12) 0.06208(11) 0.0229(3) Uani 1 1 d . . . O5 O 0.7122(3) 0.07602(13) 0.00123(11) 0.0250(3) Uani 1 1 d . . . O6 O 0.0943(2) -0.01439(13) 0.15393(11) 0.0214(3) Uani 1 1 d . . . O7 O -0.3760(2) 0.08834(11) 0.52321(10) 0.0155(3) Uani 1 1 d . . . H7A H -0.3929 0.0373 0.5705 0.023 Uiso 1 1 d . . . H7B H -0.3142 0.0562 0.4826 0.023 Uiso 1 1 d . . . O8 O -0.1321(2) 0.40135(10) 0.48369(9) 0.0150(3) Uani 1 1 d . . . H8A H -0.1840 0.4313 0.5201 0.023 Uiso 1 1 d . . . H8B H -0.1266 0.4528 0.4301 0.023 Uiso 1 1 d . . . O9 O -0.5841(2) 0.30230(11) 0.51507(10) 0.0147(3) Uani 1 1 d . . . H9A H -0.6423 0.3018 0.5650 0.022 Uiso 1 1 d . . . H9B H -0.5949 0.3716 0.4773 0.022 Uiso 1 1 d . . . O10 O -0.3102(2) 0.28772(11) 0.36324(10) 0.0169(3) Uani 1 1 d . . . H10A H -0.3703 0.2474 0.3416 0.025 Uiso 1 1 d . . . H10B H -0.2000 0.3137 0.3253 0.025 Uiso 1 1 d . . . O11 O 0.0507(2) 0.18262(11) 0.49072(10) 0.0159(3) Uani 1 1 d . . . H11A H 0.0723 0.1213 0.5258 0.024 Uiso 1 1 d . . . H11B H 0.1595 0.2192 0.4825 0.024 Uiso 1 1 d . . . O12 O -0.2378(2) 0.21297(12) 0.64580(10) 0.0216(3) Uani 1 1 d . . . H12A H -0.3317 0.1717 0.6805 0.032 Uiso 1 1 d . . . H12B H -0.1917 0.2523 0.6748 0.032 Uiso 1 1 d . . . O98 O 0.6444(2) 0.49562(11) -0.39872(10) 0.0166(3) Uani 1 1 d . . . H98A H 0.5300 0.4615 -0.3722 0.025 Uiso 1 1 d . . . H98B H 0.7144 0.5075 -0.3474 0.025 Uiso 1 1 d . . . O99 O 0.8725(2) 0.02182(11) 0.39619(10) 0.0174(3) Uani 1 1 d . . . H99A H 0.8176 0.0243 0.3372 0.026 Uiso 1 1 d . . . H99B H 0.9871 0.0685 0.3783 0.026 Uiso 1 1 d . . . Cl1 Cl 0.90039(7) 0.57059(4) -0.26246(3) 0.01467(10) Uani 1 1 d . . . Cl2 Cl 0.70806(7) 0.30823(4) -0.18683(3) 0.01549(10) Uani 1 1 d . . . Cl3 Cl 1.18286(8) 0.37309(4) -0.31798(3) 0.01539(10) Uani 1 1 d . . . Cl4 Cl 0.62807(7) -0.06250(4) 0.25868(3) 0.01552(10) Uani 1 1 d . . . Cl5 Cl 0.34230(7) 0.13737(4) 0.31127(3) 0.01430(10) Uani 1 1 d . . . Cl6 Cl 0.81626(7) 0.20140(4) 0.18158(3) 0.01554(10) Uani 1 1 d . . . Fe1 Fe -0.25765(4) 0.244637(18) 0.503997(17) 0.00994(7) Uani 1 1 d . . . Ru1 Ru 1.03679(2) 0.396025(11) -0.174443(10) 0.01053(6) Uani 1 1 d . . . Ru2 Ru 0.48854(2) 0.112072(12) 0.169937(10) 0.01090(6) 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 C1 0.0154(9) 0.0206(10) 0.0150(10) -0.0099(8) -0.0002(7) -0.0012(8) C2 0.0160(10) 0.0164(9) 0.0123(10) -0.0056(8) 0.0004(7) 0.0051(8) C3 0.0155(9) 0.0122(9) 0.0182(11) -0.0038(8) -0.0030(8) -0.0004(7) C4 0.0151(9) 0.0215(10) 0.0144(10) -0.0084(8) -0.0005(7) -0.0036(8) C5 0.0157(9) 0.0126(9) 0.0173(11) -0.0023(8) -0.0028(8) 0.0006(7) C6 0.0181(10) 0.0156(9) 0.0134(10) -0.0054(8) -0.0004(7) 0.0051(8) O1 0.0280(8) 0.0164(7) 0.0247(9) -0.0027(6) -0.0072(7) 0.0060(6) O2 0.0143(7) 0.0257(8) 0.0263(9) -0.0142(7) 0.0006(6) -0.0027(6) O3 0.0250(8) 0.0238(8) 0.0171(8) -0.0085(6) 0.0048(6) 0.0005(6) O4 0.0273(8) 0.0159(7) 0.0237(9) -0.0028(6) -0.0069(6) 0.0040(6) O5 0.0305(9) 0.0262(8) 0.0180(8) -0.0089(7) 0.0060(6) 0.0015(7) O6 0.0151(7) 0.0265(8) 0.0280(9) -0.0165(7) 0.0011(6) -0.0037(6) O7 0.0206(7) 0.0106(6) 0.0148(7) -0.0034(5) -0.0003(5) -0.0019(5) O8 0.0199(7) 0.0108(6) 0.0139(7) -0.0035(5) -0.0004(5) -0.0017(5) O9 0.0135(7) 0.0142(7) 0.0162(7) -0.0054(6) 0.0020(5) 0.0014(5) O10 0.0189(7) 0.0189(7) 0.0127(7) -0.0048(6) -0.0007(5) -0.0052(6) O11 0.0100(6) 0.0137(6) 0.0229(8) -0.0048(6) -0.0003(5) -0.0001(5) O12 0.0288(8) 0.0223(7) 0.0135(7) -0.0054(6) -0.0008(6) -0.0094(6) O98 0.0162(7) 0.0173(7) 0.0164(7) -0.0057(6) -0.0005(5) -0.0013(5) O99 0.0176(7) 0.0174(7) 0.0174(8) -0.0054(6) -0.0028(6) -0.0002(6) Cl1 0.0144(2) 0.0118(2) 0.0167(2) -0.00304(18) -0.00117(17) 0.00053(17) Cl2 0.0142(2) 0.0149(2) 0.0177(2) -0.00570(18) -0.00132(17) -0.00181(17) Cl3 0.0168(2) 0.0171(2) 0.0128(2) -0.00610(18) 0.00059(17) 0.00189(17) Cl4 0.0160(2) 0.0125(2) 0.0169(2) -0.00326(18) -0.00108(17) 0.00102(17) Cl5 0.0146(2) 0.0159(2) 0.0133(2) -0.00622(18) 0.00012(17) 0.00001(17) Cl6 0.0136(2) 0.0150(2) 0.0178(2) -0.00495(18) -0.00101(17) -0.00188(17) Fe1 0.00997(14) 0.00921(14) 0.01104(15) -0.00386(11) -0.00061(11) -0.00027(11) Ru1 0.01072(9) 0.01099(9) 0.00995(10) -0.00353(6) -0.00071(6) 0.00057(6) Ru2 0.01099(9) 0.01142(9) 0.01034(10) -0.00360(6) -0.00093(6) 0.00038(6) _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 C1 O1 1.131(2) . ? C1 Ru1 1.909(2) . ? C2 O2 1.124(3) . ? C2 Ru1 1.922(2) . ? C3 O3 1.127(3) . ? C3 Ru1 1.896(2) . ? C4 O4 1.131(3) . ? C4 Ru2 1.903(2) . ? C5 O5 1.130(3) . ? C5 Ru2 1.896(2) . ? C6 O6 1.125(3) . ? C6 Ru2 1.925(2) . ? O7 Fe1 2.0966(13) . ? O7 H7A 0.8128 . ? O7 H7B 0.9190 . ? O8 Fe1 2.1145(13) . ? O8 H8A 0.8267 . ? O8 H8B 0.8772 . ? O9 Fe1 2.1682(13) . ? O9 H9A 0.8246 . ? O9 H9B 0.9064 . ? O10 Fe1 2.1117(14) . ? O10 H10A 0.8174 . ? O10 H10B 0.8622 . ? O11 Fe1 2.0913(13) . ? O11 H11A 0.8224 . ? O11 H11B 0.8119 . ? O12 Fe1 2.1060(15) . ? O12 H12A 0.8310 . ? O12 H12B 0.8492 . ? O98 H98A 0.8474 . ? O98 H98B 0.9887 . ? O99 H99A 0.9893 . ? O99 H99B 0.9104 . ? Cl1 Ru1 2.4174(5) . ? Cl2 Ru1 2.4104(5) . ? Cl3 Ru1 2.4370(5) . ? Cl4 Ru2 2.4281(5) . ? Cl5 Ru2 2.4189(5) . ? Cl6 Ru2 2.4120(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 C1 Ru1 178.81(19) . . ? O2 C2 Ru1 175.21(17) . . ? O3 C3 Ru1 177.28(18) . . ? O4 C4 Ru2 179.09(19) . . ? O5 C5 Ru2 178.02(18) . . ? O6 C6 Ru2 175.23(17) . . ? Fe1 O7 H7A 128.7 . . ? Fe1 O7 H7B 114.4 . . ? H7A O7 H7B 102.4 . . ? Fe1 O8 H8A 115.0 . . ? Fe1 O8 H8B 122.4 . . ? H8A O8 H8B 104.2 . . ? Fe1 O9 H9A 121.0 . . ? Fe1 O9 H9B 110.4 . . ? H9A O9 H9B 105.2 . . ? Fe1 O10 H10A 122.9 . . ? Fe1 O10 H10B 115.9 . . ? H10A O10 H10B 105.1 . . ? Fe1 O11 H11A 116.1 . . ? Fe1 O11 H11B 122.8 . . ? H11A O11 H11B 109.3 . . ? Fe1 O12 H12A 116.3 . . ? Fe1 O12 H12B 130.6 . . ? H12A O12 H12B 107.1 . . ? H98A O98 H98B 102.6 . . ? H99A O99 H99B 103.0 . . ? O11 Fe1 O7 86.98(5) . . ? O11 Fe1 O12 91.50(6) . . ? O7 Fe1 O12 92.81(6) . . ? O11 Fe1 O10 95.20(6) . . ? O7 Fe1 O10 89.07(5) . . ? O12 Fe1 O10 173.13(5) . . ? O11 Fe1 O8 91.89(5) . . ? O7 Fe1 O8 178.84(5) . . ? O12 Fe1 O8 87.48(6) . . ? O10 Fe1 O8 90.77(5) . . ? O11 Fe1 O9 176.91(5) . . ? O7 Fe1 O9 90.27(5) . . ? O12 Fe1 O9 90.06(6) . . ? O10 Fe1 O9 83.33(6) . . ? O8 Fe1 O9 90.85(5) . . ? C3 Ru1 C1 93.21(8) . . ? C3 Ru1 C2 91.52(8) . . ? C1 Ru1 C2 93.58(8) . . ? C3 Ru1 Cl2 86.28(6) . . ? C1 Ru1 Cl2 88.90(6) . . ? C2 Ru1 Cl2 176.78(6) . . ? C3 Ru1 Cl1 88.35(6) . . ? C1 Ru1 Cl1 178.34(6) . . ? C2 Ru1 Cl1 86.93(6) . . ? Cl2 Ru1 Cl1 90.655(16) . . ? C3 Ru1 Cl3 174.51(6) . . ? C1 Ru1 Cl3 89.77(6) . . ? C2 Ru1 Cl3 92.90(6) . . ? Cl2 Ru1 Cl3 89.171(17) . . ? Cl1 Ru1 Cl3 88.628(17) . . ? C5 Ru2 C4 93.35(8) . . ? C5 Ru2 C6 91.67(9) . . ? C4 Ru2 C6 93.30(8) . . ? C5 Ru2 Cl6 87.15(6) . . ? C4 Ru2 Cl6 88.96(6) . . ? C6 Ru2 Cl6 177.51(6) . . ? C5 Ru2 Cl5 175.26(6) . . ? C4 Ru2 Cl5 89.41(6) . . ? C6 Ru2 Cl5 92.01(6) . . ? Cl6 Ru2 Cl5 89.058(17) . . ? C5 Ru2 Cl4 87.90(6) . . ? C4 Ru2 Cl4 178.67(6) . . ? C6 Ru2 Cl4 87.09(6) . . ? Cl6 Ru2 Cl4 90.670(16) . . ? Cl5 Ru2 Cl4 89.307(17) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7A Cl5 0.81 2.44 3.2235(14) 161.2 2_556 O7 H7B O99 0.92 1.86 2.754(2) 163.2 1_455 O8 H8A O98 0.83 1.97 2.783(2) 170.1 1_456 O8 H8B Cl3 0.88 2.40 3.2373(14) 158.9 2_665 O9 H9A Cl3 0.82 2.46 3.2444(15) 158.6 1_356 O9 H9A Cl4 0.82 3.41 3.8484(14) 116.3 2_556 O9 H9B O98 0.91 1.80 2.7000(19) 173.5 2_565 O10 H10A Cl5 0.82 2.47 3.2545(15) 159.9 1_455 O10 H10B Cl1 0.86 2.35 3.1611(15) 155.8 2_665 O11 H11A O99 0.82 1.90 2.7257(19) 178.1 2_656 O11 H11B O9 0.81 2.12 2.893(2) 158.3 1_655 O12 H12A Cl4 0.83 2.29 3.1026(15) 165.3 2_556 O12 H12B Cl2 0.85 2.51 3.2059(16) 140.4 1_456 O98 H98A Cl3 0.85 2.42 3.2626(14) 171.7 1_455 O98 H98B Cl1 0.99 2.17 3.1365(15) 165.2 . O99 H99A Cl4 0.99 2.30 3.1802(15) 147.4 . O99 H99A Cl6 0.99 2.74 3.4185(15) 126.5 . O99 H99B Cl5 0.91 2.42 3.2850(15) 158.3 1_655 O99 H99B O11 0.91 2.68 3.173(2) 114.9 1_655 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.620 _refine_diff_density_min -1.065 _refine_diff_density_rms 0.102 #===END======================================================================= data_compound_2 _database_code_depnum_ccdc_archive 'CCDC 299528' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Cl2 Fe H8 O4' _chemical_formula_sum 'Cl2 Fe H8 O4' _chemical_formula_weight 198.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 '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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 5.8738(3) _cell_length_b 7.1006(5) _cell_length_c 8.4040(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.623(3) _cell_angle_gamma 90.00 _cell_volume 330.15(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2741 _cell_measurement_theta_min 3.72 _cell_measurement_theta_max 27.45 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.000 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 200 _exptl_absorpt_coefficient_mu 3.017 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4821 _exptl_absorpt_correction_T_max 0.6571 _exptl_absorpt_process_details 'Xprep in Shelxtl v.6.14-1 (Sheldrick, 2005)' _publ_section_exptl_refinement ; The H2O hydrogens were located from the difference Fourier map but refined with fixed O-H distance (with O---H = 0.85 \%A) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2741 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 27.45 _reflns_number_total 755 _reflns_number_gt 722 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.0e (Crystal Impact GbR, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+0.0859P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 755 _refine_ls_number_parameters 50 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0226 _refine_ls_R_factor_gt 0.0214 _refine_ls_wR_factor_ref 0.0518 _refine_ls_wR_factor_gt 0.0509 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.091 _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 Cl1 Cl 0.26455(6) 0.26095(5) 0.07774(4) 0.01351(13) Uani 1 1 d . . . Fe1 Fe 0.5000 0.0000 0.0000 0.01035(12) Uani 1 2 d S . . O1 O 0.29794(19) -0.20638(16) 0.06642(13) 0.0156(2) Uani 1 1 d D . . O2 O 0.2529(2) 0.00106(13) -0.24936(17) 0.0180(3) Uani 1 1 d D . . H1A H 0.1486(9) -0.209(3) 0.008(2) 0.035(6) Uiso 1 1 d D . . H2B H 0.129(3) 0.071(3) -0.286(3) 0.037(6) Uiso 1 1 d D . . H1B H 0.308(4) -0.212(4) 0.1696(8) 0.040(7) Uiso 1 1 d D . . H2A H 0.261(4) -0.068(3) -0.330(2) 0.041(6) 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 Cl1 0.01098(19) 0.0172(2) 0.0128(2) -0.00116(12) 0.00454(13) 0.00040(12) Fe1 0.00860(18) 0.01283(19) 0.00957(19) 0.00034(9) 0.00296(12) -0.00121(9) O1 0.0125(5) 0.0213(6) 0.0133(5) 0.0016(4) 0.0045(4) -0.0030(4) O2 0.0163(5) 0.0224(6) 0.0115(5) -0.0033(4) -0.0003(4) 0.0066(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 Cl1 Fe1 2.5258(4) . ? Fe1 O1 2.0767(11) . ? Fe1 O1 2.0767(11) 3_655 ? Fe1 O2 2.1107(13) 3_655 ? Fe1 O2 2.1107(13) . ? Fe1 Cl1 2.5258(4) 3_655 ? O1 H1A 0.850(11) . ? O1 H1B 0.850(9) . ? O2 H2B 0.85(2) . ? O2 H2A 0.850(19) . ? 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 Fe1 O1 180.0 . 3_655 ? O1 Fe1 O2 89.72(4) . 3_655 ? O1 Fe1 O2 90.28(4) 3_655 3_655 ? O1 Fe1 O2 90.28(4) . . ? O1 Fe1 O2 89.72(4) 3_655 . ? O2 Fe1 O2 180.0 3_655 . ? O1 Fe1 Cl1 92.07(3) . . ? O1 Fe1 Cl1 87.93(3) 3_655 . ? O2 Fe1 Cl1 89.97(3) 3_655 . ? O2 Fe1 Cl1 90.03(3) . . ? O1 Fe1 Cl1 87.93(3) . 3_655 ? O1 Fe1 Cl1 92.07(3) 3_655 3_655 ? O2 Fe1 Cl1 90.03(3) 3_655 3_655 ? O2 Fe1 Cl1 89.97(3) . 3_655 ? Cl1 Fe1 Cl1 180.0 . 3_655 ? Fe1 O1 H1A 115.6(16) . . ? Fe1 O1 H1B 117.2(17) . . ? H1A O1 H1B 107(2) . . ? Fe1 O2 H2B 125.5(16) . . ? Fe1 O2 H2A 125.6(17) . . ? H2B O2 H2A 109(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1A Cl1 0.85 2.317(7) 3.1377(11) 162(2) 3 O2 H2B Cl1 0.85 2.38(2) 3.2244(12) 172(2) 4_565 O2 H2B O2 0.85 3.12(2) 3.5505(13) 113.8(18) 2_554 O1 H1B Cl1 0.85 2.310(6) 3.1414(11) 166(2) 2_545 O2 H2A Cl1 0.85 2.371(18) 3.2160(13) 172(2) 2_544 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.342 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.110 #===END======================================================================== data_compound_3 _database_code_depnum_ccdc_archive 'CCDC 299529' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C3 H2 Cl2 O4 Ru' _chemical_formula_sum 'C3 H2 Cl2 O4 Ru' _chemical_formula_weight 274.02 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' 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 6.2164(3) _cell_length_b 10.2373(5) _cell_length_c 11.7124(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.922(3) _cell_angle_gamma 90.00 _cell_volume 738.25(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1603 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description colorless _exptl_crystal_colour block _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 520 _exptl_absorpt_coefficient_mu 2.797 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5321 _exptl_absorpt_correction_T_max 0.7153 _exptl_absorpt_process_details 'Xprep in Shelxtl v.6.14-1 (Sheldrick, 2005)' _publ_section_exptl_refinement ; The H2O hydrogens were located from the difference Fourier but constrained to ride on their parent atoms (U~iso~ = 1.5 U~eq~(parent atom)). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6605 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0359 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1677 _reflns_number_gt 1480 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.0e (Crystal Impact GbR, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0199P)^2^+0.0596P] 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 1677 _refine_ls_number_parameters 91 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0278 _refine_ls_R_factor_gt 0.0219 _refine_ls_wR_factor_ref 0.0456 _refine_ls_wR_factor_gt 0.0436 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.003 _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 Ru1 Ru 0.14635(3) 0.279065(17) 0.611068(14) 0.01154(8) Uani 1 1 d . . . Cl1 Cl -0.20271(9) 0.27774(5) 0.49264(5) 0.01688(13) Uani 1 1 d . . . Cl2 Cl 0.03739(8) 0.46036(5) 0.72033(4) 0.01568(13) Uani 1 1 d . . . O1 O 0.5858(3) 0.28425(15) 0.76217(14) 0.0203(4) Uani 1 1 d . . . O2 O 0.2734(3) 0.05102(16) 0.46735(14) 0.0257(4) Uani 1 1 d . . . O3 O -0.0373(2) 0.09119(16) 0.77118(13) 0.0197(4) Uani 1 1 d . . . O4 O 0.25183(10) 0.419006(13) 0.49452(3) 0.0158(3) Uani 1 1 d D . . H4A H 0.2590 0.4934 0.5188 0.024 Uiso 1 1 d D . . H4B H 0.1650 0.4270 0.4283 0.024 Uiso 1 1 d D . . C1 C 0.4244(4) 0.2825(2) 0.7055(2) 0.0153(5) Uani 1 1 d . . . C2 C 0.2305(3) 0.1365(2) 0.52060(18) 0.0173(5) Uani 1 1 d . . . C3 C 0.0367(3) 0.1604(2) 0.71259(19) 0.0145(5) 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 Ru1 0.01293(11) 0.00927(12) 0.01221(11) 0.00089(6) 0.00097(7) 0.00114(7) Cl1 0.0168(3) 0.0151(3) 0.0174(3) 0.0008(2) -0.0025(2) -0.0002(2) Cl2 0.0179(3) 0.0125(3) 0.0167(3) -0.0015(2) 0.0028(2) 0.0013(2) O1 0.0166(9) 0.0201(10) 0.0231(9) 0.0012(7) -0.0011(7) -0.0004(7) O2 0.0361(10) 0.0178(10) 0.0232(9) -0.0038(7) 0.0047(7) 0.0074(8) O3 0.0177(8) 0.0195(9) 0.0224(8) 0.0052(7) 0.0040(7) -0.0021(7) O4 0.0187(8) 0.0140(8) 0.0146(7) 0.0023(6) 0.0018(6) 0.0011(7) C1 0.0224(13) 0.0084(12) 0.0172(12) -0.0001(9) 0.0100(10) 0.0009(9) C2 0.0170(11) 0.0179(13) 0.0159(12) 0.0055(10) -0.0014(9) -0.0002(10) C3 0.0117(11) 0.0140(12) 0.0164(11) -0.0045(10) -0.0035(9) 0.0030(9) _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 Ru1 C3 1.891(2) . ? Ru1 C2 1.918(2) . ? Ru1 C1 1.919(2) . ? Ru1 O4 2.1430(6) . ? Ru1 Cl2 2.4041(5) . ? Ru1 Cl1 2.4089(6) . ? O1 C1 1.125(3) . ? O2 C2 1.128(3) . ? O3 C3 1.128(3) . ? O4 H4A 0.8120 . ? O4 H4B 0.8860 . ? 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 C3 Ru1 C2 90.47(10) . . ? C3 Ru1 C1 91.35(9) . . ? C2 Ru1 C1 92.27(9) . . ? C3 Ru1 O4 176.55(6) . . ? C2 Ru1 O4 91.49(7) . . ? C1 Ru1 O4 91.40(7) . . ? C3 Ru1 Cl2 90.49(7) . . ? C2 Ru1 Cl2 178.64(6) . . ? C1 Ru1 Cl2 88.66(6) . . ? O4 Ru1 Cl2 87.498(18) . . ? C3 Ru1 Cl1 89.09(6) . . ? C2 Ru1 Cl1 88.30(6) . . ? C1 Ru1 Cl1 179.28(6) . . ? O4 Ru1 Cl1 88.132(18) . . ? Cl2 Ru1 Cl1 90.766(18) . . ? Ru1 O4 H4A 114.2 . . ? Ru1 O4 H4B 114.6 . . ? H4A O4 H4B 102.6 . . ? O1 C1 Ru1 179.0(2) . . ? O2 C2 Ru1 177.7(2) . . ? O3 C3 Ru1 177.10(18) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4A Cl1 0.81 2.37 3.1251(6) 155.0 3_566 O4 H4B Cl2 0.89 2.31 3.1373(5) 155.3 3_566 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.573 _refine_diff_density_min -0.811 _refine_diff_density_rms 0.114 #===END======================================================================== data_compound_4 _database_code_depnum_ccdc_archive 'CCDC 299530' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H12 Cl6 Fe O8 Ru2' _chemical_formula_sum 'C10 H12 Cl6 Fe O8 Ru2' _chemical_formula_weight 730.89 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' 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.2270(7) _cell_length_b 10.9769(6) _cell_length_c 11.0272(8) _cell_angle_alpha 90.00 _cell_angle_beta 96.796(4) _cell_angle_gamma 90.00 _cell_volume 1109.03(13) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2969 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.189 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 2.745 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5207 _exptl_absorpt_correction_T_max 0.5951 _exptl_absorpt_process_details 'Xprep in Shelxtl v.6.14-1 (Sheldrick, 2005)' _publ_section_exptl_refinement ; The OH hydrogen was located from the difference Fourier map but refined with fixed O-H distance (with O---H = 0.85 \%A). All other hydrogens were positioned geometrically and allowed to ride on their parent atoms, with C---H = 0.98-0.99 \%A, and U~iso~ = 1.2-1.5 U~eq~(parent atom). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8311 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2522 _reflns_number_gt 2011 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.0e (Crystal Impact GbR, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+0.6251P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2522 _refine_ls_number_parameters 129 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0679 _refine_ls_wR_factor_gt 0.0619 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 Ru1 Ru 0.82659(3) 0.11006(2) 0.69059(2) 0.01519(10) Uani 1 1 d . . . Fe1 Fe 0.5000 0.0000 0.5000 0.01664(16) Uani 1 2 d S . . Cl1 Cl 0.74035(9) 0.09892(7) 0.47513(7) 0.01780(18) Uani 1 1 d . . . Cl2 Cl 0.57957(9) 0.05475(8) 0.72184(7) 0.02094(19) Uani 1 1 d . . . Cl3 Cl 0.89261(9) -0.10307(7) 0.69044(8) 0.02242(19) Uani 1 1 d . . . O1 O 0.9218(3) 0.1189(2) 0.9625(2) 0.0270(6) Uani 1 1 d . . . O2 O 1.1347(3) 0.1587(2) 0.6327(2) 0.0296(6) Uani 1 1 d . . . O3 O 0.7414(3) 0.3772(2) 0.6837(2) 0.0263(6) Uani 1 1 d . . . O4 O 0.3945(3) 0.1628(2) 0.4693(2) 0.0255(6) Uani 1 1 d D . . C1 C 0.8867(4) 0.1159(3) 0.8609(3) 0.0201(7) Uani 1 1 d . . . C2 C 1.0198(4) 0.1434(3) 0.6546(3) 0.0207(7) Uani 1 1 d . . . C3 C 0.7744(4) 0.2781(3) 0.6883(3) 0.0189(7) Uani 1 1 d . . . C4 C 0.4286(5) 0.2830(3) 0.5146(4) 0.0427(11) Uani 1 1 d . . . H4A H 0.5251 0.3068 0.4916 0.051 Uiso 1 1 calc R . . H4B H 0.4364 0.2812 0.6049 0.051 Uiso 1 1 calc R . . C5 C 0.3221(5) 0.3757(3) 0.4698(4) 0.0376(10) Uani 1 1 d . . . H5A H 0.3173 0.3815 0.3808 0.056 Uiso 1 1 calc R . . H5B H 0.3515 0.4545 0.5065 0.056 Uiso 1 1 calc R . . H5C H 0.2259 0.3532 0.4921 0.056 Uiso 1 1 calc R . . H4 H 0.321(3) 0.159(4) 0.415(3) 0.070(17) 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 Ru1 0.01529(15) 0.01458(14) 0.01537(15) 0.00005(11) 0.00044(10) 0.00012(10) Fe1 0.0158(4) 0.0138(3) 0.0197(4) 0.0007(3) -0.0003(3) 0.0011(3) Cl1 0.0182(4) 0.0198(4) 0.0152(4) 0.0002(3) 0.0014(3) -0.0007(3) Cl2 0.0178(4) 0.0261(4) 0.0192(4) 0.0013(4) 0.0033(3) -0.0012(3) Cl3 0.0213(4) 0.0153(4) 0.0289(5) 0.0012(3) -0.0043(4) 0.0023(3) O1 0.0297(15) 0.0315(14) 0.0187(13) 0.0003(11) -0.0015(11) 0.0033(11) O2 0.0222(15) 0.0303(14) 0.0378(15) -0.0128(12) 0.0097(12) -0.0051(11) O3 0.0360(16) 0.0193(13) 0.0228(13) -0.0010(10) 0.0005(11) 0.0070(11) O4 0.0218(14) 0.0164(12) 0.0352(15) -0.0024(11) -0.0094(12) 0.0031(10) C1 0.0163(18) 0.0151(16) 0.029(2) -0.0001(15) 0.0049(15) 0.0002(13) C2 0.029(2) 0.0155(16) 0.0174(17) -0.0046(14) -0.0005(15) 0.0036(14) C3 0.0167(17) 0.0237(18) 0.0161(17) 0.0007(14) 0.0019(13) -0.0007(14) C4 0.036(3) 0.0227(19) 0.066(3) -0.001(2) -0.008(2) 0.0033(18) C5 0.035(2) 0.0184(18) 0.060(3) -0.0008(19) 0.006(2) 0.0017(16) _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 Ru1 C1 1.895(4) . ? Ru1 C3 1.905(3) . ? Ru1 C2 1.907(4) . ? Ru1 Cl3 2.4176(8) . ? Ru1 Cl1 2.4178(8) . ? Ru1 Cl2 2.4224(8) . ? Fe1 O4 2.043(2) . ? Fe1 O4 2.043(2) 3_656 ? Fe1 Cl1 2.5132(8) 3_656 ? Fe1 Cl1 2.5132(8) . ? Fe1 Cl2 2.5415(8) 3_656 ? Fe1 Cl2 2.5415(8) . ? O1 C1 1.130(4) . ? O2 C2 1.128(4) . ? O3 C3 1.130(4) . ? O4 C4 1.433(4) . ? O4 H4 0.85(3) . ? C4 C5 1.459(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? 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 C1 Ru1 C3 91.38(13) . . ? C1 Ru1 C2 91.65(14) . . ? C3 Ru1 C2 93.01(14) . . ? C1 Ru1 Cl3 89.40(10) . . ? C3 Ru1 Cl3 179.20(10) . . ? C2 Ru1 Cl3 86.76(10) . . ? C1 Ru1 Cl1 177.60(10) . . ? C3 Ru1 Cl1 89.00(10) . . ? C2 Ru1 Cl1 90.69(10) . . ? Cl3 Ru1 Cl1 90.23(3) . . ? C1 Ru1 Cl2 92.14(10) . . ? C3 Ru1 Cl2 90.23(10) . . ? C2 Ru1 Cl2 174.95(10) . . ? Cl3 Ru1 Cl2 89.94(3) . . ? Cl1 Ru1 Cl2 85.49(3) . . ? O4 Fe1 O4 179.998(1) . 3_656 ? O4 Fe1 Cl1 89.23(7) . 3_656 ? O4 Fe1 Cl1 90.77(7) 3_656 3_656 ? O4 Fe1 Cl1 90.77(7) . . ? O4 Fe1 Cl1 89.23(7) 3_656 . ? Cl1 Fe1 Cl1 180.0 3_656 . ? O4 Fe1 Cl2 88.26(7) . 3_656 ? O4 Fe1 Cl2 91.74(7) 3_656 3_656 ? Cl1 Fe1 Cl2 81.07(3) 3_656 3_656 ? Cl1 Fe1 Cl2 98.93(3) . 3_656 ? O4 Fe1 Cl2 91.74(7) . . ? O4 Fe1 Cl2 88.26(7) 3_656 . ? Cl1 Fe1 Cl2 98.93(3) 3_656 . ? Cl1 Fe1 Cl2 81.07(3) . . ? Cl2 Fe1 Cl2 180.0 3_656 . ? Ru1 Cl1 Fe1 96.12(3) . . ? Ru1 Cl2 Fe1 95.27(3) . . ? C4 O4 Fe1 131.8(2) . . ? C4 O4 H4 114(3) . . ? Fe1 O4 H4 113(3) . . ? O1 C1 Ru1 179.6(3) . . ? O2 C2 Ru1 177.5(3) . . ? O3 C3 Ru1 178.1(3) . . ? O4 C4 C5 114.4(3) . . ? O4 C4 H4A 108.7 . . ? C5 C4 H4A 108.7 . . ? O4 C4 H4B 108.7 . . ? C5 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4 Cl3 0.85(3) 2.254(16) 3.073(3) 162(5) 3_656 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.944 _refine_diff_density_min -1.106 _refine_diff_density_rms 0.260 #===END======================================================================== data_compound_5 _database_code_depnum_ccdc_archive 'CCDC 299531' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H4 Cl6 Fe O8 Ru2' _chemical_formula_sum 'C6 H4 Cl6 Fe O8 Ru2' _chemical_formula_weight 674.78 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' 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 7.0444(4) _cell_length_b 15.6274(3) _cell_length_c 8.5003(7) _cell_angle_alpha 90.00 _cell_angle_beta 97.016(3) _cell_angle_gamma 90.00 _cell_volume 928.75(9) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 10764 _cell_measurement_theta_min 3.19 _cell_measurement_theta_max 27.48 _exptl_crystal_description 'greenish yellow' _exptl_crystal_colour block _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.413 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 3.267 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6080 _exptl_absorpt_correction_T_max 0.6318 _exptl_absorpt_process_details 'Xprep in Shelxtl v.6.14-1 (Sheldrick, 2005)' _publ_section_exptl_refinement ; The H2O hydrogens were located from the difference Fourier map but refined with fixed O-H distance (with O---H = 0.85 \%A) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10764 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2118 _reflns_number_gt 1806 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.0e (Crystal Impact GbR, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0258P)^2^+1.4287P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2118 _refine_ls_number_parameters 114 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0626 _refine_ls_wR_factor_gt 0.0596 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.103 _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 Ru1 Ru 0.60440(4) 0.154125(15) -0.29344(3) 0.01801(9) Uani 1 1 d . . . Fe1 Fe 0.5000 0.0000 0.0000 0.01598(13) Uani 1 2 d S . . Cl1 Cl 0.59557(12) 0.00006(5) -0.27418(9) 0.02453(17) Uani 1 1 d . . . O1 O 0.6137(4) 0.34815(14) -0.2945(3) 0.0292(5) Uani 1 1 d . . . C1 C 0.6097(5) 0.2761(2) -0.2964(3) 0.0224(6) Uani 1 1 d . . . Cl2 Cl 0.48321(12) 0.15620(4) -0.03718(8) 0.02194(17) Uani 1 1 d . . . O2 O 0.7649(4) 0.14577(16) -0.6091(3) 0.0340(6) Uani 1 1 d . . . C2 C 0.7055(5) 0.1490(2) -0.4924(4) 0.0238(7) Uani 1 1 d . . . Cl3 Cl 0.92516(12) 0.15415(5) -0.15457(9) 0.02709(18) Uani 1 1 d . . . O3 O 0.1955(4) 0.14510(17) -0.4523(3) 0.0342(6) Uani 1 1 d . . . C3 C 0.3460(5) 0.1501(2) -0.3949(4) 0.0223(7) Uani 1 1 d . . . O4 O 0.7864(3) 0.01279(14) 0.0950(3) 0.0298(5) Uani 1 1 d D . . H4A H 0.883(4) -0.016(3) 0.135(5) 0.060(15) Uiso 1 1 d D . . H4B H 0.839(6) 0.046(2) 0.034(4) 0.053(14) 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 Ru1 0.02088(15) 0.01615(13) 0.01697(13) 0.00101(9) 0.00213(9) -0.00042(9) Fe1 0.0204(3) 0.0114(3) 0.0162(3) 0.0014(2) 0.0027(2) 0.0005(2) Cl1 0.0338(4) 0.0166(3) 0.0240(4) -0.0008(3) 0.0069(3) 0.0013(3) O1 0.0430(15) 0.0199(12) 0.0245(12) 0.0004(9) 0.0026(11) -0.0025(10) C1 0.0244(16) 0.0275(17) 0.0153(14) 0.0013(12) 0.0020(12) -0.0020(13) Cl2 0.0306(4) 0.0152(3) 0.0211(4) 0.0002(3) 0.0072(3) 0.0014(3) O2 0.0357(14) 0.0409(15) 0.0270(13) -0.0055(10) 0.0111(11) -0.0107(11) C2 0.0216(16) 0.0192(15) 0.0299(17) -0.0020(13) 0.0000(13) -0.0051(12) Cl3 0.0231(4) 0.0320(4) 0.0254(4) 0.0003(3) -0.0001(3) -0.0015(3) O3 0.0236(14) 0.0490(16) 0.0290(13) 0.0006(11) -0.0010(11) -0.0008(11) C3 0.0299(19) 0.0204(15) 0.0174(14) 0.0017(12) 0.0062(13) 0.0001(13) O4 0.0299(14) 0.0261(13) 0.0337(14) 0.0002(10) 0.0044(11) 0.0001(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru1 C1 1.907(3) . ? Ru1 C2 1.915(3) . ? Ru1 C3 1.918(4) . ? Ru1 Cl1 2.4145(8) . ? Ru1 Cl3 2.4182(9) . ? Ru1 Cl2 2.4350(7) . ? Fe1 O4 2.089(2) . ? Fe1 O4 2.089(2) 3_655 ? Fe1 Cl2 2.4624(7) 3_655 ? Fe1 Cl2 2.4624(7) . ? Fe1 Cl1 2.5036(7) . ? Fe1 Cl1 2.5036(7) 3_655 ? O1 C1 1.126(4) . ? O2 C2 1.123(4) . ? O3 C3 1.115(4) . ? O4 H4A 0.85(4) . ? O4 H4B 0.85(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 C2 91.14(13) . . ? C1 Ru1 C3 92.63(13) . . ? C2 Ru1 C3 92.08(13) . . ? C1 Ru1 Cl1 176.81(9) . . ? C2 Ru1 Cl1 91.94(9) . . ? C3 Ru1 Cl1 88.11(9) . . ? C1 Ru1 Cl3 89.29(10) . . ? C2 Ru1 Cl3 90.29(10) . . ? C3 Ru1 Cl3 176.92(9) . . ? Cl1 Ru1 Cl3 89.85(3) . . ? C1 Ru1 Cl2 90.46(9) . . ? C2 Ru1 Cl2 177.92(10) . . ? C3 Ru1 Cl2 89.17(9) . . ? Cl1 Ru1 Cl2 86.44(2) . . ? Cl3 Ru1 Cl2 88.40(3) . . ? O4 Fe1 O4 180.0 . 3_655 ? O4 Fe1 Cl2 90.93(6) . 3_655 ? O4 Fe1 Cl2 89.07(6) 3_655 3_655 ? O4 Fe1 Cl2 89.07(6) . . ? O4 Fe1 Cl2 90.93(6) 3_655 . ? Cl2 Fe1 Cl2 179.999(4) 3_655 . ? O4 Fe1 Cl1 90.17(7) . . ? O4 Fe1 Cl1 89.83(7) 3_655 . ? Cl2 Fe1 Cl1 96.07(2) 3_655 . ? Cl2 Fe1 Cl1 83.93(2) . . ? O4 Fe1 Cl1 89.83(7) . 3_655 ? O4 Fe1 Cl1 90.17(7) 3_655 3_655 ? Cl2 Fe1 Cl1 83.93(2) 3_655 3_655 ? Cl2 Fe1 Cl1 96.07(2) . 3_655 ? Cl1 Fe1 Cl1 180.0 . 3_655 ? Ru1 Cl1 Fe1 94.34(3) . . ? O1 C1 Ru1 178.4(3) . . ? Ru1 Cl2 Fe1 94.88(2) . . ? O2 C2 Ru1 179.8(3) . . ? O3 C3 Ru1 177.7(3) . . ? Fe1 O4 H4A 142(3) . . ? Fe1 O4 H4B 107(3) . . ? H4A O4 H4B 100(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4B Cl3 0.85 2.457(10) 3.293(2) 168(4) . O4 H4B O1 0.85 2.82(4) 3.224(3) 111(4) 4_666 O4 H4A Cl3 0.85 2.54(2) 3.307(2) 150(4) 3_755 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.923 _refine_diff_density_min -0.760 _refine_diff_density_rms 0.106 #===END======================================================================= data_compound_5b _database_code_depnum_ccdc_archive 'CCDC 299532' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H4 Cl6 Fe O8 Ru2, H2 O' _chemical_formula_sum 'C6 H6 Cl6 Fe O9 Ru2' _chemical_formula_weight 692.80 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' 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' Ru Ru -1.2594 0.8363 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.9100(2) _cell_length_b 11.7730(5) _cell_length_c 12.5560(5) _cell_angle_alpha 103.407(2) _cell_angle_beta 101.573(2) _cell_angle_gamma 95.605(2) _cell_volume 962.20(6) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7981 _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 26.00 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 660 _exptl_absorpt_coefficient_mu 3.160 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7408 _exptl_absorpt_correction_T_max 0.9056 _exptl_absorpt_process_details 'Xprep in Shelxtl v.6.14-1 (Sheldrick, 2005)' _publ_section_exptl_refinement ; The H2O hydrogens were located from the difference Fourier but only U~iso~ parameters were refined. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16410 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4377 _reflns_number_gt 3431 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.0e (Crystal Impact GbR, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+0.0000P] 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 refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4377 _refine_ls_number_parameters 241 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0679 _refine_ls_wR_factor_gt 0.0616 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Ru1 Ru 0.03577(4) 0.10249(2) 0.23074(2) 0.01551(8) Uani 1 1 d . . . Cl1 Cl -0.03605(12) 0.19387(7) 0.07510(7) 0.01956(19) Uani 1 1 d . . . O1 O 0.1248(4) -0.0107(2) 0.4242(2) 0.0243(6) Uani 1 1 d . . . C1 C 0.0947(5) 0.0329(3) 0.3533(3) 0.0165(7) Uani 1 1 d . . . Ru2 Ru 0.18563(4) 0.65047(2) 0.34885(2) 0.01502(8) Uani 1 1 d . . . Cl2 Cl 0.26847(12) 0.28108(7) 0.33117(7) 0.01820(18) Uani 1 1 d . . . O2 O -0.2775(4) -0.1106(2) 0.1051(2) 0.0304(6) Uani 1 1 d . . . C2 C -0.1588(5) -0.0329(3) 0.1497(3) 0.0216(8) Uani 1 1 d . . . Fe1 Fe 0.22826(7) 0.36874(4) 0.16619(4) 0.01716(12) Uani 1 1 d . . . Cl3 Cl -0.22126(13) 0.18931(8) 0.31049(7) 0.02244(19) Uani 1 1 d . . . O3 O 0.3690(4) 0.0034(2) 0.1293(2) 0.0307(6) Uani 1 1 d . . . C3 C 0.2458(5) 0.0379(3) 0.1671(3) 0.0202(8) Uani 1 1 d . . . Cl5 Cl -0.03838(12) 0.48045(7) 0.22336(7) 0.01916(18) Uani 1 1 d . . . O5 O 0.4812(4) 0.8657(2) 0.4914(2) 0.0271(6) Uani 1 1 d . . . C5 C 0.3714(5) 0.7848(3) 0.4403(3) 0.0190(8) Uani 1 1 d . . . Cl4 Cl 0.44703(12) 0.56318(7) 0.27165(7) 0.01911(18) Uani 1 1 d . . . O4 O -0.1603(4) 0.7565(2) 0.4276(2) 0.0272(6) Uani 1 1 d . . . C4 C -0.0321(5) 0.7164(3) 0.4004(3) 0.0189(8) Uani 1 1 d . . . Cl6 Cl 0.12674(12) 0.75389(7) 0.20221(7) 0.02084(19) Uani 1 1 d . . . O6 O 0.2462(4) 0.5207(2) 0.5328(2) 0.0298(6) Uani 1 1 d . . . C6 C 0.2261(5) 0.5684(3) 0.4647(3) 0.0215(8) Uani 1 1 d . . . O7 O 0.4722(3) 0.2899(2) 0.1335(2) 0.0232(6) Uani 1 1 d D . . O8 O 0.2049(4) 0.4135(2) 0.0109(2) 0.0261(6) Uani 1 1 d D . . O99 O 0.3854(3) 0.6417(2) 0.0321(2) 0.0266(6) Uani 1 1 d D . . H7A H 0.533(5) 0.301(4) 0.083(2) 0.051(15) Uiso 1 1 d D . . H7B H 0.547(7) 0.276(5) 0.190(3) 0.075(18) Uiso 1 1 d D . . H8B H 0.224(7) 0.4810(18) -0.002(4) 0.051(15) Uiso 1 1 d D . . H8A H 0.114(5) 0.378(3) -0.047(2) 0.046(14) Uiso 1 1 d D . . H99A H 0.315(6) 0.690(3) 0.061(4) 0.067(17) Uiso 1 1 d D . . H99B H 0.480(5) 0.646(5) 0.089(3) 0.08(2) 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 Ru1 0.01623(15) 0.01390(15) 0.01605(15) 0.00323(11) 0.00347(11) 0.00272(11) Cl1 0.0236(4) 0.0172(4) 0.0161(4) 0.0043(3) 0.0011(3) 0.0019(3) O1 0.0271(14) 0.0234(14) 0.0231(14) 0.0072(12) 0.0063(11) 0.0038(11) C1 0.0123(16) 0.0120(17) 0.0217(18) -0.0022(15) 0.0030(14) 0.0024(13) Ru2 0.01595(15) 0.01391(15) 0.01421(14) 0.00306(11) 0.00187(11) 0.00227(10) Cl2 0.0204(4) 0.0172(4) 0.0155(4) 0.0040(3) 0.0017(3) 0.0012(3) O2 0.0265(14) 0.0229(15) 0.0355(15) -0.0013(12) 0.0047(12) 0.0003(12) C2 0.0195(18) 0.022(2) 0.0256(19) 0.0074(16) 0.0068(16) 0.0087(16) Fe1 0.0194(3) 0.0151(3) 0.0160(2) 0.0038(2) 0.0025(2) 0.00209(19) Cl3 0.0209(4) 0.0254(5) 0.0215(4) 0.0039(4) 0.0067(3) 0.0075(3) O3 0.0255(14) 0.0285(15) 0.0353(16) -0.0008(12) 0.0104(12) 0.0049(12) C3 0.0227(19) 0.0148(18) 0.0184(18) 0.0031(14) -0.0016(15) -0.0031(14) Cl5 0.0170(4) 0.0160(4) 0.0213(4) 0.0019(3) 0.0010(3) 0.0015(3) O5 0.0224(13) 0.0208(14) 0.0336(15) 0.0044(12) 0.0009(12) -0.0002(11) C5 0.0162(17) 0.025(2) 0.0198(18) 0.0097(16) 0.0056(15) 0.0097(15) Cl4 0.0156(4) 0.0184(4) 0.0214(4) 0.0024(3) 0.0028(3) 0.0025(3) O4 0.0218(14) 0.0275(15) 0.0292(15) 0.0007(12) 0.0074(12) 0.0027(11) C4 0.0232(19) 0.0162(18) 0.0131(16) 0.0035(14) -0.0014(15) -0.0049(15) Cl6 0.0278(5) 0.0181(4) 0.0169(4) 0.0060(3) 0.0033(4) 0.0053(3) O6 0.0406(17) 0.0262(15) 0.0230(14) 0.0078(12) 0.0043(12) 0.0091(12) C6 0.0191(18) 0.0188(19) 0.0220(19) -0.0012(16) 0.0028(15) 0.0007(14) O7 0.0257(14) 0.0259(15) 0.0223(14) 0.0099(12) 0.0096(12) 0.0067(11) O8 0.0301(15) 0.0275(16) 0.0196(13) 0.0096(12) 0.0008(12) 0.0003(12) O99 0.0287(15) 0.0286(15) 0.0259(15) 0.0095(12) 0.0106(13) 0.0051(12) _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 Ru1 C1 1.898(4) . ? Ru1 C2 1.914(4) . ? Ru1 C3 1.930(4) . ? Ru1 Cl3 2.4073(9) . ? Ru1 Cl2 2.4275(9) . ? Ru1 Cl1 2.4316(9) . ? Cl1 Fe1 2.4935(9) . ? O1 C1 1.122(4) . ? Ru2 C5 1.907(4) . ? Ru2 C6 1.915(4) . ? Ru2 C4 1.916(4) . ? Ru2 Cl5 2.4164(8) . ? Ru2 Cl4 2.4210(9) . ? Ru2 Cl6 2.4236(9) . ? Cl2 Fe1 2.5000(10) . ? O2 C2 1.121(4) . ? Fe1 O7 2.068(2) . ? Fe1 O8 2.115(3) . ? Fe1 Cl5 2.4912(9) . ? Fe1 Cl4 2.5287(9) . ? O3 C3 1.120(4) . ? O5 C5 1.129(4) . ? O4 C4 1.119(4) . ? O6 C6 1.120(4) . ? O7 H7A 0.86(3) . ? O7 H7B 0.85(4) . ? O8 H8B 0.85(3) . ? O8 H8A 0.85(3) . ? O99 H99A 0.85(4) . ? O99 H99B 0.85(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ru1 C2 89.65(15) . . ? C1 Ru1 C3 92.08(14) . . ? C2 Ru1 C3 92.99(14) . . ? C1 Ru1 Cl3 88.88(10) . . ? C2 Ru1 Cl3 88.56(10) . . ? C3 Ru1 Cl3 178.18(11) . . ? C1 Ru1 Cl2 92.39(10) . . ? C2 Ru1 Cl2 176.81(10) . . ? C3 Ru1 Cl2 89.39(10) . . ? Cl3 Ru1 Cl2 89.03(3) . . ? C1 Ru1 Cl1 179.21(10) . . ? C2 Ru1 Cl1 91.14(11) . . ? C3 Ru1 Cl1 87.82(10) . . ? Cl3 Ru1 Cl1 91.20(3) . . ? Cl2 Ru1 Cl1 86.83(3) . . ? Ru1 Cl1 Fe1 94.34(3) . . ? O1 C1 Ru1 177.9(3) . . ? C5 Ru2 C6 92.12(14) . . ? C5 Ru2 C4 91.41(14) . . ? C6 Ru2 C4 91.66(15) . . ? C5 Ru2 Cl5 176.27(11) . . ? C6 Ru2 Cl5 90.26(10) . . ? C4 Ru2 Cl5 91.39(10) . . ? C5 Ru2 Cl4 91.32(10) . . ? C6 Ru2 Cl4 90.70(11) . . ? C4 Ru2 Cl4 176.32(10) . . ? Cl5 Ru2 Cl4 85.78(3) . . ? C5 Ru2 Cl6 88.54(10) . . ? C6 Ru2 Cl6 178.76(11) . . ? C4 Ru2 Cl6 87.27(10) . . ? Cl5 Ru2 Cl6 89.14(3) . . ? Cl4 Ru2 Cl6 90.33(3) . . ? Ru1 Cl2 Fe1 94.28(3) . . ? O2 C2 Ru1 177.2(3) . . ? O7 Fe1 O8 87.21(10) . . ? O7 Fe1 Cl5 173.50(7) . . ? O8 Fe1 Cl5 95.27(7) . . ? O7 Fe1 Cl1 98.15(7) . . ? O8 Fe1 Cl1 90.44(7) . . ? Cl5 Fe1 Cl1 87.86(3) . . ? O7 Fe1 Cl2 85.10(8) . . ? O8 Fe1 Cl2 169.73(7) . . ? Cl5 Fe1 Cl2 93.11(3) . . ? Cl1 Fe1 Cl2 83.94(3) . . ? O7 Fe1 Cl4 91.98(7) . . ? O8 Fe1 Cl4 91.65(7) . . ? Cl5 Fe1 Cl4 81.96(3) . . ? Cl1 Fe1 Cl4 169.75(3) . . ? Cl2 Fe1 Cl4 95.39(3) . . ? O3 C3 Ru1 177.9(3) . . ? Ru2 Cl5 Fe1 95.90(3) . . ? O5 C5 Ru2 177.8(3) . . ? Ru2 Cl4 Fe1 94.81(3) . . ? O4 C4 Ru2 177.7(3) . . ? O6 C6 Ru2 178.6(3) . . ? Fe1 O7 H7A 124(3) . . ? Fe1 O7 H7B 115(4) . . ? H7A O7 H7B 114(4) . . ? Fe1 O8 H8B 130(3) . . ? Fe1 O8 H8A 122(3) . . ? H8B O8 H8A 100(4) . . ? H99A O99 H99B 101(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O8 H8B O99 0.85 2.01(2) 2.779(4) 151(4) . O8 H8A Cl6 0.85 2.402(8) 3.241(2) 170(4) 2_565 O7 H7A O99 0.85 1.896(13) 2.718(4) 162(4) 2_665 O7 H7B Cl3 0.85 2.440(15) 3.263(3) 163(5) 1_655 O99 H99A Cl6 0.85 2.43(3) 3.192(3) 149(5) . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.746 _refine_diff_density_min -0.771 _refine_diff_density_rms 0.139 #===END======================================================================== data_compound_5c _database_code_depnum_ccdc_archive 'CCDC 299533' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H4 Cl6 Fe O8 Ru2' _chemical_formula_sum 'C6 H4 Cl6 Fe O8 Ru2' _chemical_formula_weight 674.78 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' 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.1193(2) _cell_length_b 6.40080(10) _cell_length_c 27.7787(8) _cell_angle_alpha 90.00 _cell_angle_beta 95.3390(9) _cell_angle_gamma 90.00 _cell_volume 1791.47(7) _cell_formula_units_Z 4 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 7981 _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 26.00 _exptl_crystal_description 'pale yellow' _exptl_crystal_colour block _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 3.387 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4212 _exptl_absorpt_correction_T_max 0.7136 _exptl_absorpt_process_details 'Xprep in Shelxtl v.6.14-1 (Sheldrick, 2005)' _publ_section_exptl_refinement ; The H2O hydrogens were located from the difference Fourier map but refined with fixed O-H distance (O---H = 0.85 \%A) and fixed U~iso~ (U~iso~ = 0.05) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7981 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0403 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -3 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3345 _reflns_number_gt 2918 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.0e (Crystal Impact GbR, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+2.2879P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3345 _refine_ls_number_parameters 220 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0316 _refine_ls_R_factor_gt 0.0242 _refine_ls_wR_factor_ref 0.0599 _refine_ls_wR_factor_gt 0.0578 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.155 _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 C2 C 0.4838(4) 0.8300(6) 0.44346(13) 0.0211(8) Uani 1 1 d . . . C1 C 0.4124(4) 0.4377(6) 0.40652(13) 0.0225(8) Uani 1 1 d . . . C3 C 0.3193(4) 0.8020(6) 0.35884(14) 0.0208(8) Uani 1 1 d . . . C4 C -0.2267(4) 0.8577(7) 0.24294(15) 0.0270(9) Uani 1 1 d . . . C5 C -0.3912(4) 0.6038(7) 0.28976(13) 0.0262(9) Uani 1 1 d . . . C6 C -0.1288(4) 0.5024(7) 0.28874(13) 0.0249(9) Uani 1 1 d . . . O2 O 0.5762(3) 0.9176(4) 0.45688(10) 0.0279(6) Uani 1 1 d . . . O1 O 0.4591(3) 0.2870(5) 0.39665(11) 0.0335(7) Uani 1 1 d . . . O3 O 0.3174(3) 0.8752(5) 0.32182(10) 0.0320(7) Uani 1 1 d . . . O4 O -0.2280(3) 0.9253(5) 0.20542(10) 0.0426(8) Uani 1 1 d . . . O5 O -0.4896(3) 0.5205(5) 0.28203(11) 0.0403(8) Uani 1 1 d . . . O6 O -0.0721(3) 0.3616(5) 0.27756(10) 0.0356(7) Uani 1 1 d . . . O7 O -0.0552(3) 0.7106(4) 0.48739(9) 0.0237(6) Uani 1 1 d D . . O8 O -0.1337(2) 1.0877(5) 0.43262(10) 0.0277(6) Uani 1 1 d D . . Cl2 Cl 0.11281(8) 0.50729(14) 0.40183(3) 0.0193(2) Uani 1 1 d . . . Cl1 Cl 0.19095(8) 0.98221(14) 0.44397(3) 0.0219(2) Uani 1 1 d . . . Cl3 Cl 0.31502(9) 0.56433(15) 0.50399(3) 0.0233(2) Uani 1 1 d . . . Cl4 Cl -0.22959(9) 0.60844(15) 0.38730(3) 0.0226(2) Uani 1 1 d . . . Cl5 Cl -0.02368(9) 0.92410(15) 0.33344(3) 0.0234(2) Uani 1 1 d . . . Cl6 Cl -0.34456(9) 1.04652(17) 0.32991(4) 0.0308(2) Uani 1 1 d . . . Fe1 Fe -0.02698(5) 0.80842(8) 0.418074(18) 0.01793(13) Uani 1 1 d . . . Ru1 Ru 0.32161(3) 0.68675(5) 0.422679(10) 0.01602(9) Uani 1 1 d . . . Ru2 Ru -0.22745(3) 0.74344(5) 0.306001(10) 0.01899(9) Uani 1 1 d . . . H7A H -0.128(2) 0.661(6) 0.4948(12) 0.050 Uiso 1 1 d D . . H7B H -0.013(3) 0.756(7) 0.5131(7) 0.050 Uiso 1 1 d D . . H8A H -0.168(3) 1.144(7) 0.4068(7) 0.050 Uiso 1 1 d D . . H8B H -0.191(3) 1.089(7) 0.4530(9) 0.050 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 C2 0.024(2) 0.020(2) 0.0199(19) 0.0000(16) 0.0067(16) 0.0073(17) C1 0.020(2) 0.026(2) 0.022(2) 0.0030(17) 0.0027(15) -0.0027(17) C3 0.014(2) 0.023(2) 0.025(2) -0.0014(17) 0.0024(15) 0.0011(15) C4 0.020(2) 0.033(2) 0.028(2) 0.0036(19) 0.0037(16) 0.0063(17) C5 0.026(3) 0.034(2) 0.019(2) -0.0010(17) 0.0011(16) 0.0074(19) C6 0.022(2) 0.034(3) 0.0176(19) 0.0075(18) 0.0006(15) -0.0033(19) O2 0.0221(16) 0.0276(16) 0.0333(16) -0.0029(13) -0.0007(12) -0.0027(13) O1 0.0339(18) 0.0269(17) 0.0406(18) -0.0046(14) 0.0079(13) 0.0111(13) O3 0.0323(17) 0.0400(19) 0.0236(16) 0.0103(14) 0.0018(12) -0.0009(13) O4 0.0382(18) 0.065(2) 0.0257(17) 0.0213(16) 0.0062(13) 0.0140(16) O5 0.0269(19) 0.052(2) 0.0404(18) -0.0023(16) -0.0060(13) -0.0073(15) O6 0.0411(19) 0.0323(18) 0.0350(17) 0.0030(14) 0.0124(14) 0.0124(14) O7 0.0231(16) 0.0294(16) 0.0187(13) -0.0002(12) 0.0029(11) -0.0030(12) O8 0.0236(15) 0.0308(17) 0.0294(16) 0.0032(13) 0.0066(12) 0.0072(12) Cl2 0.0178(5) 0.0185(5) 0.0214(4) -0.0020(4) 0.0004(3) 0.0001(4) Cl1 0.0175(5) 0.0187(5) 0.0291(5) -0.0052(4) 0.0008(4) 0.0017(4) Cl3 0.0221(5) 0.0300(5) 0.0176(5) 0.0047(4) 0.0009(4) -0.0011(4) Cl4 0.0195(5) 0.0315(5) 0.0167(4) 0.0025(4) 0.0009(3) -0.0045(4) Cl5 0.0185(5) 0.0297(5) 0.0219(5) 0.0066(4) 0.0005(4) -0.0021(4) Cl6 0.0262(6) 0.0347(6) 0.0314(5) -0.0031(4) 0.0023(4) 0.0113(4) Fe1 0.0165(3) 0.0201(3) 0.0172(3) -0.0002(2) 0.0014(2) 0.0010(2) Ru1 0.01472(18) 0.01746(17) 0.01595(15) 0.00009(12) 0.00186(11) 0.00123(12) Ru2 0.01525(18) 0.02614(19) 0.01547(16) 0.00142(13) 0.00091(12) 0.00299(12) _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 C2 O2 1.124(4) . ? C2 Ru1 1.921(4) . ? C1 O1 1.120(4) . ? C1 Ru1 1.914(4) . ? C3 O3 1.129(4) . ? C3 Ru1 1.919(4) . ? C4 O4 1.127(5) . ? C4 Ru2 1.899(4) . ? C5 O5 1.132(5) . ? C5 Ru2 1.900(4) . ? C6 O6 1.128(5) . ? C6 Ru2 1.922(4) . ? O7 Fe1 2.070(3) . ? O7 H7A 0.85(2) . ? O7 H7B 0.85(3) . ? O8 Fe1 2.146(3) . ? O8 H8A 0.85(3) . ? O8 H8B 0.85(3) . ? Cl2 Ru1 2.4273(9) . ? Cl2 Fe1 2.4573(10) . ? Cl1 Ru1 2.4125(9) . ? Cl1 Fe1 2.5145(10) . ? Cl3 Ru1 2.3974(9) . ? Cl4 Ru2 2.4201(9) . ? Cl4 Fe1 2.4994(10) . ? Cl5 Ru2 2.4243(9) . ? Cl5 Fe1 2.4681(10) . ? Cl6 Ru2 2.3990(10) . ? 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 O2 C2 Ru1 177.4(3) . . ? O1 C1 Ru1 176.3(3) . . ? O3 C3 Ru1 178.1(3) . . ? O4 C4 Ru2 179.1(4) . . ? O5 C5 Ru2 177.2(3) . . ? O6 C6 Ru2 178.4(3) . . ? Fe1 O7 H7A 123(2) . . ? Fe1 O7 H7B 125(3) . . ? H7A O7 H7B 108(3) . . ? Fe1 O8 H8A 112(3) . . ? Fe1 O8 H8B 121(3) . . ? H8A O8 H8B 108(3) . . ? Ru1 Cl2 Fe1 95.06(3) . . ? Ru1 Cl1 Fe1 93.97(3) . . ? Ru2 Cl4 Fe1 93.33(3) . . ? Ru2 Cl5 Fe1 94.01(3) . . ? O7 Fe1 O8 87.79(11) . . ? O7 Fe1 Cl2 93.74(8) . . ? O8 Fe1 Cl2 175.02(8) . . ? O7 Fe1 Cl5 172.87(8) . . ? O8 Fe1 Cl5 88.92(8) . . ? Cl2 Fe1 Cl5 90.08(3) . . ? O7 Fe1 Cl4 89.05(8) . . ? O8 Fe1 Cl4 94.57(8) . . ? Cl2 Fe1 Cl4 90.19(3) . . ? Cl5 Fe1 Cl4 84.91(3) . . ? O7 Fe1 Cl1 93.50(8) . . ? O8 Fe1 Cl1 91.21(8) . . ? Cl2 Fe1 Cl1 83.97(3) . . ? Cl5 Fe1 Cl1 92.90(3) . . ? Cl4 Fe1 Cl1 173.77(4) . . ? C1 Ru1 C3 93.92(15) . . ? C1 Ru1 C2 93.03(15) . . ? C3 Ru1 C2 91.77(16) . . ? C1 Ru1 Cl3 90.27(11) . . ? C3 Ru1 Cl3 175.80(11) . . ? C2 Ru1 Cl3 88.32(11) . . ? C1 Ru1 Cl1 175.10(11) . . ? C3 Ru1 Cl1 88.02(11) . . ? C2 Ru1 Cl1 91.41(11) . . ? Cl3 Ru1 Cl1 87.79(3) . . ? C1 Ru1 Cl2 88.62(11) . . ? C3 Ru1 Cl2 91.49(11) . . ? C2 Ru1 Cl2 176.24(11) . . ? Cl3 Ru1 Cl2 88.29(3) . . ? Cl1 Ru1 Cl2 86.83(3) . . ? C4 Ru2 C5 92.32(17) . . ? C4 Ru2 C6 91.85(16) . . ? C5 Ru2 C6 91.43(16) . . ? C4 Ru2 Cl6 89.33(12) . . ? C5 Ru2 Cl6 90.21(12) . . ? C6 Ru2 Cl6 177.93(11) . . ? C4 Ru2 Cl4 178.24(13) . . ? C5 Ru2 Cl4 88.30(11) . . ? C6 Ru2 Cl4 89.78(11) . . ? Cl6 Ru2 Cl4 89.02(3) . . ? C4 Ru2 Cl5 91.71(12) . . ? C5 Ru2 Cl5 175.29(11) . . ? C6 Ru2 Cl5 90.86(12) . . ? Cl6 Ru2 Cl5 87.41(3) . . ? Cl4 Ru2 Cl5 87.60(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7A Cl3 0.85(2) 2.377(13) 3.191(3) 161(4) 3_566 O7 H7B O8 0.85(3) 2.248(9) 3.077(4) 165(3) 3_576 _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 0.515 _refine_diff_density_min -0.592 _refine_diff_density_rms 0.148 #===END======================================================================== data_compound_6 _database_code_depnum_ccdc_archive 'CCDC 299534' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Cl2 Fe H8 O4, C3 Cl3 O3 Ru, 2(H2 O)' _chemical_formula_sum 'C3 H12 Cl5 Fe O9 Ru' _chemical_formula_weight 526.30 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' 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' Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.7975(5) _cell_length_b 9.4944(2) _cell_length_c 15.1011(6) _cell_angle_alpha 90.00 _cell_angle_beta 107.635(2) _cell_angle_gamma 90.00 _cell_volume 1611.99(10) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'orange yellow' _exptl_crystal_colour block _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.169 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1028 _exptl_absorpt_coefficient_mu 2.693 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6802 _exptl_absorpt_correction_T_max 0.8749 _exptl_absorpt_process_details 'Xprep in Shelxtl v.6.14-1 (Sheldrick, 2005)' _publ_section_exptl_refinement ; The H2O hydrogens were located from the difference Fourier but constrained to ride on their parent atoms (U~iso~ = 1.5 U~eq~(parent atom)). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_method '\f scans and \w scans with \k offset' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11762 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.86 _diffrn_reflns_theta_max 27.47 _reflns_number_total 3676 _reflns_number_gt 3256 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo/Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond v.3.0e (Crystal Impact GbR, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+0.8994P] 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 3676 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0591 _refine_ls_wR_factor_gt 0.0567 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _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 Ru1 Ru -0.249867(16) 0.799622(18) 0.351637(13) 0.01223(7) Uani 1 1 d . . . Fe1 Fe -0.25743(3) 0.31816(3) 0.58816(2) 0.01357(9) Uani 1 1 d . . . Cl1 Cl -0.37545(5) 0.87211(6) 0.44453(4) 0.01687(13) Uani 1 1 d . . . Cl2 Cl -0.35450(5) 0.57728(6) 0.32322(4) 0.01804(13) Uani 1 1 d . . . Cl3 Cl -0.10963(5) 0.69791(6) 0.48843(4) 0.01603(12) Uani 1 1 d . . . Cl4 Cl -0.16241(5) 0.45906(6) 0.70734(4) 0.02059(13) Uani 1 1 d . . . Cl5 Cl -0.13625(5) 0.12381(6) 0.63111(4) 0.02051(13) Uani 1 1 d . . . O1 O -0.10404(16) 0.70228(18) 0.22932(13) 0.0244(4) Uani 1 1 d . . . O2 O -0.11923(17) 1.07824(19) 0.40380(13) 0.0266(4) Uani 1 1 d . . . O3 O -0.42598(16) 0.91261(19) 0.17633(13) 0.0241(4) Uani 1 1 d . . . O4 O -0.36918(15) 0.20466(16) 0.47938(12) 0.0180(4) Uani 1 1 d . . . H4A H -0.4311 0.2347 0.4461 0.027 Uiso 1 1 d . . . H4B H -0.3664 0.1196 0.4705 0.027 Uiso 1 1 d . . . O5 O -0.36474(15) 0.48039(16) 0.52069(12) 0.0180(4) Uani 1 1 d . . . H5A H -0.3899 0.5424 0.5464 0.027 Uiso 1 1 d . . . H5B H -0.3649 0.5131 0.4741 0.027 Uiso 1 1 d . . . O6 O -0.15841(15) 0.37345(16) 0.50155(12) 0.0191(4) Uani 1 1 d . . . H6A H -0.1461 0.4578 0.4968 0.029 Uiso 1 1 d . . . H6B H -0.0915 0.3386 0.5163 0.029 Uiso 1 1 d . . . O7 O -0.37714(15) 0.27134(19) 0.65391(12) 0.0214(4) Uani 1 1 d . . . H7A H -0.4423 0.2303 0.6316 0.032 Uiso 1 1 d . . . H7B H -0.3674 0.2715 0.7095 0.032 Uiso 1 1 d . . . O98 O -0.42095(16) 0.68128(17) 0.62919(12) 0.0206(4) Uani 1 1 d . . . H98A H -0.4266 0.6583 0.6820 0.031 Uiso 1 1 d . . . H98B H -0.3550 0.7331 0.6423 0.031 Uiso 1 1 d . . . O99 O -0.30560(17) 0.30361(16) 0.83592(12) 0.0218(4) Uani 1 1 d . . . H99A H -0.3031 0.3885 0.8514 0.033 Uiso 1 1 d . . . H99B H -0.3354 0.2561 0.8702 0.033 Uiso 1 1 d . . . C1 C -0.1545(2) 0.7396(2) 0.27678(17) 0.0164(5) Uani 1 1 d . . . C2 C -0.1665(2) 0.9750(3) 0.38241(16) 0.0169(5) Uani 1 1 d . . . C3 C -0.3611(2) 0.8731(2) 0.24287(18) 0.0171(5) 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 Ru1 0.01295(11) 0.01210(11) 0.01164(11) 0.00047(6) 0.00375(8) -0.00059(6) Fe1 0.01314(17) 0.01346(17) 0.01471(18) 0.00099(12) 0.00510(14) 0.00011(12) Cl1 0.0165(3) 0.0176(3) 0.0175(3) -0.0033(2) 0.0067(2) -0.0006(2) Cl2 0.0213(3) 0.0153(3) 0.0182(3) -0.0025(2) 0.0069(2) -0.0043(2) Cl3 0.0146(3) 0.0181(3) 0.0147(3) 0.0026(2) 0.0036(2) 0.0015(2) Cl4 0.0197(3) 0.0190(3) 0.0216(3) -0.0024(2) 0.0039(2) -0.0025(2) Cl5 0.0209(3) 0.0152(3) 0.0241(3) 0.0030(2) 0.0049(2) 0.0028(2) O1 0.0246(10) 0.0285(10) 0.0234(10) -0.0001(8) 0.0124(8) 0.0019(7) O2 0.0339(11) 0.0225(10) 0.0242(10) -0.0036(8) 0.0099(8) -0.0092(8) O3 0.0210(9) 0.0286(10) 0.0200(10) 0.0016(8) 0.0019(8) 0.0052(7) O4 0.0185(9) 0.0149(8) 0.0182(9) -0.0011(6) 0.0019(7) 0.0020(6) O5 0.0222(9) 0.0176(8) 0.0159(9) 0.0016(7) 0.0085(7) 0.0055(6) O6 0.0186(9) 0.0162(8) 0.0248(10) 0.0057(7) 0.0103(8) 0.0035(6) O7 0.0172(9) 0.0339(10) 0.0144(9) -0.0023(7) 0.0067(7) -0.0083(7) O98 0.0201(9) 0.0239(9) 0.0165(9) -0.0021(7) 0.0039(7) 0.0004(7) O99 0.0315(11) 0.0176(9) 0.0177(9) 0.0002(7) 0.0097(8) -0.0012(7) C1 0.0203(12) 0.0118(11) 0.0142(12) 0.0017(9) 0.0011(10) -0.0028(9) C2 0.0176(12) 0.0206(12) 0.0128(12) 0.0016(9) 0.0052(10) 0.0026(9) C3 0.0185(12) 0.0156(12) 0.0193(13) -0.0038(9) 0.0091(11) -0.0020(9) _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 Ru1 C3 1.898(3) . ? Ru1 C1 1.907(3) . ? Ru1 C2 1.918(2) . ? Ru1 Cl2 2.4173(6) . ? Ru1 Cl3 2.4220(6) . ? Ru1 Cl1 2.4281(6) . ? Fe1 O7 2.0069(17) . ? Fe1 O5 2.0571(16) . ? Fe1 O6 2.0680(17) . ? Fe1 O4 2.0702(17) . ? Fe1 Cl4 2.2501(7) . ? Fe1 Cl5 2.3038(6) . ? O1 C1 1.119(3) . ? O2 C2 1.125(3) . ? O3 C3 1.127(3) . ? O4 H4A 0.8035 . ? O4 H4B 0.8211 . ? O5 H5A 0.8095 . ? O5 H5B 0.7683 . ? O6 H6A 0.8205 . ? O6 H6B 0.8219 . ? O7 H7A 0.8364 . ? O7 H7B 0.8124 . ? O98 H98A 0.8493 . ? O98 H98B 0.8902 . ? O99 H99A 0.8371 . ? O99 H99B 0.8400 . ? 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 C3 Ru1 C1 88.54(10) . . ? C3 Ru1 C2 93.44(10) . . ? C1 Ru1 C2 92.98(10) . . ? C3 Ru1 Cl2 89.15(7) . . ? C1 Ru1 Cl2 89.70(7) . . ? C2 Ru1 Cl2 176.32(7) . . ? C3 Ru1 Cl3 178.07(7) . . ? C1 Ru1 Cl3 90.76(7) . . ? C2 Ru1 Cl3 88.39(7) . . ? Cl2 Ru1 Cl3 89.048(19) . . ? C3 Ru1 Cl1 90.72(7) . . ? C1 Ru1 Cl1 178.48(7) . . ? C2 Ru1 Cl1 88.39(7) . . ? Cl2 Ru1 Cl1 88.97(2) . . ? Cl3 Ru1 Cl1 89.94(2) . . ? O7 Fe1 O5 89.49(7) . . ? O7 Fe1 O6 170.45(7) . . ? O5 Fe1 O6 82.97(7) . . ? O7 Fe1 O4 84.42(7) . . ? O5 Fe1 O4 81.28(6) . . ? O6 Fe1 O4 88.64(7) . . ? O7 Fe1 Cl4 89.47(5) . . ? O5 Fe1 Cl4 91.93(5) . . ? O6 Fe1 Cl4 96.60(5) . . ? O4 Fe1 Cl4 170.88(5) . . ? O7 Fe1 Cl5 98.80(6) . . ? O5 Fe1 Cl5 167.28(5) . . ? O6 Fe1 Cl5 87.72(5) . . ? O4 Fe1 Cl5 89.90(5) . . ? Cl4 Fe1 Cl5 97.74(2) . . ? Fe1 O4 H4A 123.5 . . ? Fe1 O4 H4B 126.5 . . ? H4A O4 H4B 108.7 . . ? Fe1 O5 H5A 124.6 . . ? Fe1 O5 H5B 125.9 . . ? H5A O5 H5B 104.1 . . ? Fe1 O6 H6A 116.8 . . ? Fe1 O6 H6B 114.0 . . ? H6A O6 H6B 103.7 . . ? Fe1 O7 H7A 127.0 . . ? Fe1 O7 H7B 127.6 . . ? H7A O7 H7B 104.1 . . ? H98A O98 H98B 104.2 . . ? H99A O99 H99B 109.3 . . ? O1 C1 Ru1 176.3(2) . . ? O2 C2 Ru1 177.0(2) . . ? O3 C3 Ru1 177.3(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4A O98 0.80 1.94 2.744(2) 176.1 3_466 O4 H4B Cl1 0.82 2.38 3.1981(16) 175.2 1_545 O5 H5A O98 0.81 1.93 2.724(2) 168.0 . O5 H5B Cl2 0.77 2.40 3.1579(18) 170.4 . O6 H6A Cl3 0.82 2.33 3.1511(16) 178.2 . O6 H6B Cl3 0.82 2.42 3.1924(17) 156.8 3_566 O7 H7A Cl1 0.84 2.32 3.1551(17) 174.2 3_466 O7 H7B O99 0.81 1.85 2.637(2) 162.7 . O98 H98A O1 0.85 2.75 3.186(3) 113.7 4_576 O98 H98B O99 0.89 1.94 2.814(3) 166.0 2_456 O99 H99A Cl5 0.84 2.38 3.1886(17) 161.2 2_456 O99 H99B Cl3 0.84 2.47 3.2634(19) 156.9 2_446 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.430 _refine_diff_density_min -0.953 _refine_diff_density_rms 0.109