Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_codmf _audit_creation_method SHELXL-97 _chemical_name_systematic Cobalt(II)bisdimethylformamide Iron(II)Tetracyanodicarbonyl monohydrate ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H16 Co Fe N6 O5' _chemical_formula_weight 439.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M I2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 13.4386(17) _cell_length_b 7.4128(10) _cell_length_c 19.479(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.153(3) _cell_angle_gamma 90.00 _cell_volume 1925.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour pink _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 1.647 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3767 _exptl_absorpt_correction_T_max 0.4674 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4446 _diffrn_reflns_av_R_equivalents 0.0639 _diffrn_reflns_av_sigmaI/netI 0.0665 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 23.26 _reflns_number_total 1506 _reflns_number_gt 1078 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0587P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1506 _refine_ls_number_parameters 152 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1110 _refine_ls_wR_factor_gt 0.1012 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.969 _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 Co1 Co 0.23518(6) 0.0000 0.44655(4) 0.0301(3) Uani 1 2 d S . . Fe2 Fe 0.0000 0.5000 0.5000 0.0296(4) Uani 1 4 d S . . Fe1 Fe 0.5000 0.5000 0.5000 0.0332(4) Uani 1 4 d S . . O1 O 0.5672(5) 0.5000 0.3618(4) 0.104(2) Uani 1 2 d S . . C4 C 0.0778(3) 0.3148(5) 0.4633(2) 0.0322(11) Uani 1 1 d . . . C3 C 0.4023(3) 0.3130(6) 0.4730(2) 0.0370(12) Uani 1 1 d . . . O3 O 0.2407(4) 0.0000 0.5587(3) 0.0511(13) Uani 1 2 d S . . O4 O 0.2293(3) 0.0000 0.3379(2) 0.0467(12) Uani 1 2 d S . . N4 N 0.1253(3) 0.2013(5) 0.4440(2) 0.0390(10) Uani 1 1 d . . . N3 N 0.3462(3) 0.1996(4) 0.4580(2) 0.0386(10) Uani 1 1 d . . . N2 N 0.3088(6) 0.0000 0.2429(4) 0.073(2) Uani 1 2 d S . . N1 N 0.1575(6) 0.0000 0.6552(4) 0.080(2) Uani 1 2 d S . . C6 C 0.3043(7) 0.0000 0.3094(4) 0.054(2) Uani 1 2 d S . . C1 C 0.5405(6) 0.5000 0.4143(4) 0.051(2) Uani 1 2 d S . . C2 C 0.0883(6) 0.5000 0.5782(4) 0.0479(19) Uani 1 2 d S . . C5 C 0.1612(8) 0.0000 0.5878(5) 0.059(2) Uani 1 2 d S . . O2 O 0.1440(5) 0.5000 0.6263(3) 0.093(2) Uani 1 2 d S . . O5 O 0.4533(5) 0.0000 0.6119(4) 0.141(3) Uani 1 2 d S . . C9 C 0.2232(8) 0.0000 0.1947(5) 0.102(4) Uani 1 2 d S . . H9A H 0.2049 -0.1220 0.1824 0.153 Uiso 0.50 1 calc PR . . H9B H 0.2365 0.0646 0.1541 0.153 Uiso 0.50 1 calc PR . . H9C H 0.1693 0.0574 0.2143 0.153 Uiso 0.50 1 calc PR . . C8 C 0.0667(8) 0.0000 0.6854(6) 0.117(4) Uani 1 2 d S . . H8A H 0.0743 -0.0743 0.7261 0.176 Uiso 0.50 1 calc PR . . H8B H 0.0135 -0.0468 0.6528 0.176 Uiso 0.50 1 calc PR . . H8C H 0.0508 0.1211 0.6978 0.176 Uiso 0.50 1 calc PR . . C10 C 0.4043(9) 0.0000 0.2141(7) 0.171(7) Uani 1 2 d S . . H10A H 0.4223 0.1216 0.2041 0.256 Uiso 0.50 1 calc PR . . H10B H 0.3978 -0.0699 0.1723 0.256 Uiso 0.50 1 calc PR . . H10C H 0.4555 -0.0517 0.2471 0.256 Uiso 0.50 1 calc PR . . C7 C 0.2513(9) 0.0000 0.7004(6) 0.182(7) Uani 1 2 d S . . H7A H 0.2681 -0.1213 0.7147 0.273 Uiso 0.50 1 calc PR . . H7B H 0.2447 0.0727 0.7404 0.273 Uiso 0.50 1 calc PR . . H7C H 0.3033 0.0486 0.6762 0.273 Uiso 0.50 1 calc PR . . H1 H 0.101(6) 0.0000 0.562(4) 0.07(3) Uiso 1 2 d S . . H2 H 0.365(6) 0.05(2) 0.343(5) 0.27(6) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0266(5) 0.0243(5) 0.0402(6) 0.000 0.0070(4) 0.000 Fe2 0.0268(7) 0.0230(7) 0.0404(9) 0.000 0.0091(6) 0.000 Fe1 0.0293(7) 0.0269(7) 0.0429(9) 0.000 0.0027(6) 0.000 O1 0.124(6) 0.127(6) 0.070(5) 0.000 0.045(5) 0.000 C4 0.031(2) 0.023(2) 0.044(3) 0.004(2) 0.011(2) -0.005(2) C3 0.033(3) 0.028(3) 0.050(3) 0.005(2) 0.003(2) 0.009(2) O3 0.061(3) 0.051(3) 0.043(3) 0.000 0.011(3) 0.000 O4 0.043(3) 0.056(3) 0.042(3) 0.000 0.010(2) 0.000 N4 0.036(2) 0.029(2) 0.054(3) -0.0011(19) 0.014(2) 0.0036(18) N3 0.034(2) 0.023(2) 0.058(3) 0.0001(18) 0.0015(19) -0.0060(18) N2 0.108(6) 0.072(5) 0.042(5) 0.000 0.023(5) 0.000 N1 0.088(6) 0.101(6) 0.054(6) 0.000 0.022(5) 0.000 C6 0.064(6) 0.061(5) 0.038(5) 0.000 0.012(5) 0.000 C1 0.060(5) 0.041(4) 0.056(6) 0.000 0.021(4) 0.000 C2 0.050(5) 0.038(4) 0.055(5) 0.000 0.003(4) 0.000 C5 0.082(7) 0.053(5) 0.041(6) 0.000 0.002(5) 0.000 O2 0.098(5) 0.093(5) 0.079(5) 0.000 -0.027(4) 0.000 O5 0.097(6) 0.200(9) 0.119(7) 0.000 -0.010(5) 0.000 C9 0.162(11) 0.080(7) 0.055(7) 0.000 -0.019(7) 0.000 C8 0.109(9) 0.135(10) 0.118(10) 0.000 0.055(8) 0.000 C10 0.156(12) 0.263(18) 0.114(12) 0.000 0.100(10) 0.000 C7 0.141(12) 0.34(2) 0.052(8) 0.000 -0.053(8) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N3 2.093(4) . ? Co1 N3 2.093(4) 6 ? Co1 N4 2.096(4) 6 ? Co1 N4 2.096(3) . ? Co1 O4 2.108(5) . ? Co1 O3 2.177(5) . ? Fe2 C2 1.810(8) 5_566 ? Fe2 C2 1.810(8) . ? Fe2 C4 1.917(4) . ? Fe2 C4 1.917(4) 6_565 ? Fe2 C4 1.917(4) 2_556 ? Fe2 C4 1.917(4) 5_566 ? Fe1 C1 1.819(8) 5_666 ? Fe1 C1 1.819(8) . ? Fe1 C3 1.936(5) 5_666 ? Fe1 C3 1.936(5) . ? Fe1 C3 1.936(5) 2_656 ? Fe1 C3 1.936(5) 6_565 ? O1 C1 1.126(9) . ? C4 N4 1.147(5) . ? C3 N3 1.144(5) . ? O3 C5 1.270(10) . ? O4 C6 1.210(9) . ? N2 C6 1.305(10) . ? N2 C9 1.391(11) . ? N2 C10 1.463(11) . ? N1 C5 1.319(10) . ? N1 C8 1.420(10) . ? N1 C7 1.445(11) . ? C2 O2 1.124(8) . ? 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 N3 Co1 N3 89.96(19) . 6 ? N3 Co1 N4 175.28(15) . 6 ? N3 Co1 N4 89.44(13) 6 6 ? N3 Co1 N4 89.44(13) . . ? N3 Co1 N4 175.28(15) 6 . ? N4 Co1 N4 90.77(19) 6 . ? N3 Co1 O4 92.51(14) . . ? N3 Co1 O4 92.51(14) 6 . ? N4 Co1 O4 92.20(14) 6 . ? N4 Co1 O4 92.20(14) . . ? N3 Co1 O3 87.62(15) . . ? N3 Co1 O3 87.62(15) 6 . ? N4 Co1 O3 87.67(15) 6 . ? N4 Co1 O3 87.67(15) . . ? O4 Co1 O3 179.81(18) . . ? C2 Fe2 C2 180.000(1) 5_566 . ? C2 Fe2 C4 90.9(2) 5_566 . ? C2 Fe2 C4 89.1(2) . . ? C2 Fe2 C4 90.9(2) 5_566 6_565 ? C2 Fe2 C4 89.1(2) . 6_565 ? C4 Fe2 C4 91.5(2) . 6_565 ? C2 Fe2 C4 89.1(2) 5_566 2_556 ? C2 Fe2 C4 90.9(2) . 2_556 ? C4 Fe2 C4 88.5(2) . 2_556 ? C4 Fe2 C4 180.00(16) 6_565 2_556 ? C2 Fe2 C4 89.1(2) 5_566 5_566 ? C2 Fe2 C4 90.9(2) . 5_566 ? C4 Fe2 C4 180.0(3) . 5_566 ? C4 Fe2 C4 88.5(2) 6_565 5_566 ? C4 Fe2 C4 91.5(2) 2_556 5_566 ? C1 Fe1 C1 180.000(1) 5_666 . ? C1 Fe1 C3 91.2(2) 5_666 5_666 ? C1 Fe1 C3 88.8(2) . 5_666 ? C1 Fe1 C3 88.8(2) 5_666 . ? C1 Fe1 C3 91.2(2) . . ? C3 Fe1 C3 180.0 5_666 . ? C1 Fe1 C3 91.2(2) 5_666 2_656 ? C1 Fe1 C3 88.8(2) . 2_656 ? C3 Fe1 C3 91.4(2) 5_666 2_656 ? C3 Fe1 C3 88.6(2) . 2_656 ? C1 Fe1 C3 88.8(2) 5_666 6_565 ? C1 Fe1 C3 91.2(2) . 6_565 ? C3 Fe1 C3 88.6(2) 5_666 6_565 ? C3 Fe1 C3 91.4(2) . 6_565 ? C3 Fe1 C3 180.0(3) 2_656 6_565 ? N4 C4 Fe2 177.1(4) . . ? N3 C3 Fe1 178.3(4) . . ? C5 O3 Co1 121.4(6) . . ? C6 O4 Co1 122.1(5) . . ? C4 N4 Co1 159.1(4) . . ? C3 N3 Co1 170.4(4) . . ? C6 N2 C9 122.3(8) . . ? C6 N2 C10 122.1(9) . . ? C9 N2 C10 115.6(9) . . ? C5 N1 C8 123.6(10) . . ? C5 N1 C7 118.0(9) . . ? C8 N1 C7 118.5(9) . . ? O4 C6 N2 126.8(9) . . ? O1 C1 Fe1 178.8(8) . . ? O2 C2 Fe2 179.2(7) . . ? O3 C5 N1 125.5(10) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.618 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.086 #===END data_fedmf _audit_creation_method SHELXL-97 _chemical_name_systematic Iron(II)bisdimethylforamide Iron(II)tetracyanodicarbonyl monohydrate ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H16 Fe2 N6 O5' _chemical_formula_weight 436.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 I2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 13.4721(10) _cell_length_b 7.4905(6) _cell_length_c 19.5630(15) _cell_angle_alpha 90.00 _cell_angle_beta 97.754(2) _cell_angle_gamma 90.00 _cell_volume 1956.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 1.515 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3017 _exptl_absorpt_correction_T_max 0.3744 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4556 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 23.28 _reflns_number_total 1540 _reflns_number_gt 1232 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0473P)^2^+0.0424P] 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 1540 _refine_ls_number_parameters 151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0848 _refine_ls_wR_factor_gt 0.0789 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 C1 C 0.9610(4) 1.0000 1.0855(3) 0.0460(12) Uani 1 2 d S . . C4 C 0.5757(2) 0.8168(4) 0.96135(15) 0.0327(7) Uani 1 1 d . . . O3 O 0.7380(2) 0.5000 1.05744(15) 0.0448(8) Uani 1 2 d S . . N4 N 0.62095(19) 0.7033(3) 0.94114(13) 0.0393(7) Uani 1 1 d . . . O4 O 0.7296(2) 0.5000 0.83683(15) 0.0454(8) Uani 1 2 d S . . N3 N 0.84582(19) 0.7027(3) 0.95785(13) 0.0402(6) Uani 1 1 d . . . C3 C 0.9024(2) 0.8158(4) 0.97302(15) 0.0334(7) Uani 1 1 d . . . O1 O 0.9350(4) 1.0000 1.1374(2) 0.0934(15) Uani 1 2 d S . . N1 N 0.6613(3) 0.5000 1.1544(2) 0.0668(13) Uani 1 2 d S . . C5 C 0.6606(4) 0.5000 1.0872(3) 0.0473(12) Uani 1 2 d S . . C6 C 0.8045(4) 0.5000 0.8098(3) 0.0541(14) Uani 1 2 d S . . C2 C 0.5924(4) 1.0000 1.0763(3) 0.0447(12) Uani 1 2 d S . . O2 O 0.6493(3) 1.0000 1.1242(2) 0.0896(14) Uani 1 2 d S . . C7 C 0.7544(6) 0.5000 1.1991(3) 0.162(5) Uani 1 2 d S . . H7A H 0.7435 0.4614 1.2443 0.243 Uiso 0.50 1 calc PR . . H7B H 0.7819 0.6185 1.2017 0.243 Uiso 0.50 1 calc PR . . H7C H 0.8004 0.4201 1.1812 0.243 Uiso 0.50 1 calc PR . . N2 N 0.8104(4) 0.5000 0.7432(2) 0.0637(13) Uani 1 2 d S . . C8 C 0.5690(5) 0.5000 1.1854(3) 0.094(2) Uani 1 2 d S . . H8A H 0.5142 0.5353 1.1516 0.141 Uiso 0.50 1 calc PR . . H8B H 0.5752 0.5824 1.2233 0.141 Uiso 0.50 1 calc PR . . H8C H 0.5569 0.3823 1.2018 0.141 Uiso 0.50 1 calc PR . . C10 C 0.9056(6) 0.5000 0.7164(4) 0.149(4) Uani 1 2 d S . . H10A H 0.9020 0.4211 0.6775 0.224 Uiso 0.50 1 calc PR . . H10B H 0.9574 0.4601 0.7517 0.224 Uiso 0.50 1 calc PR . . H10C H 0.9206 0.6187 0.7024 0.224 Uiso 0.50 1 calc PR . . C9 C 0.7223(6) 0.5000 0.6937(3) 0.096(2) Uani 1 2 d S . . H9A H 0.6668 0.5441 0.7148 0.143 Uiso 0.50 1 calc PR . . H9B H 0.7083 0.3805 0.6775 0.143 Uiso 0.50 1 calc PR . . H9C H 0.7326 0.5754 0.6556 0.143 Uiso 0.50 1 calc PR . . O5 O 0.9545(3) 0.5000 0.1111(2) 0.1193(17) Uani 1 2 d S . . Fe1 Fe 1.0000 1.0000 1.0000 0.0286(2) Uani 1 4 d S . . Fe2 Fe 0.5000 1.0000 1.0000 0.0289(3) Uani 1 4 d S . . Fe3 Fe 0.73328(4) 0.5000 0.94520(3) 0.0284(2) Uani 1 2 d S . . H1 H 0.596(4) 0.5000 1.062(2) 0.056(15) Uiso 1 2 d S . . H2 H 0.880(5) 0.5000 0.837(3) 0.10(2) Uiso 1 2 d S . . 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 0.050(3) 0.040(3) 0.049(3) 0.000 0.010(3) 0.000 C4 0.0266(17) 0.0303(17) 0.0421(18) 0.0031(14) 0.0081(14) -0.0052(14) O3 0.050(2) 0.051(2) 0.0346(18) 0.000 0.0080(16) 0.000 N4 0.0347(16) 0.0315(14) 0.0541(17) -0.0015(12) 0.0145(13) 0.0053(13) O4 0.0358(19) 0.060(2) 0.0413(19) 0.000 0.0095(16) 0.000 N3 0.0332(15) 0.0295(14) 0.0570(18) -0.0026(12) 0.0034(13) -0.0049(13) C3 0.0303(18) 0.0259(17) 0.0432(19) 0.0018(13) 0.0022(14) 0.0072(14) O1 0.110(4) 0.121(4) 0.055(3) 0.000 0.035(3) 0.000 N1 0.061(3) 0.098(4) 0.040(3) 0.000 0.005(2) 0.000 C5 0.055(4) 0.048(3) 0.038(3) 0.000 0.002(3) 0.000 C6 0.053(4) 0.071(4) 0.039(3) 0.000 0.007(3) 0.000 C2 0.049(3) 0.033(3) 0.052(3) 0.000 0.002(3) 0.000 O2 0.083(3) 0.098(3) 0.076(3) 0.000 -0.033(3) 0.000 C7 0.087(6) 0.344(15) 0.052(5) 0.000 -0.005(4) 0.000 N2 0.086(4) 0.069(3) 0.039(3) 0.000 0.017(3) 0.000 C8 0.088(5) 0.139(6) 0.062(4) 0.000 0.033(4) 0.000 C10 0.128(7) 0.250(11) 0.087(6) 0.000 0.077(6) 0.000 C9 0.138(7) 0.091(5) 0.051(4) 0.000 -0.012(4) 0.000 O5 0.077(3) 0.176(5) 0.100(4) 0.000 -0.005(3) 0.000 Fe1 0.0228(5) 0.0238(5) 0.0384(5) 0.000 0.0018(4) 0.000 Fe2 0.0242(5) 0.0235(5) 0.0400(5) 0.000 0.0078(4) 0.000 Fe3 0.0244(4) 0.0242(3) 0.0370(4) 0.000 0.0060(3) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.117(6) . ? C1 Fe1 1.820(5) . ? C4 N4 1.147(3) . ? C4 Fe2 1.924(3) . ? O3 C5 1.261(6) . ? O3 Fe3 2.188(3) . ? N4 Fe3 2.141(2) . ? O4 C6 1.201(6) . ? O4 Fe3 2.114(3) . ? N3 C3 1.151(4) . ? N3 Fe3 2.136(3) . ? C3 Fe1 1.930(3) . ? N1 C5 1.312(6) . ? N1 C7 1.429(8) . ? N1 C8 1.456(7) . ? C6 N2 1.317(6) . ? C2 O2 1.126(5) . ? C2 Fe2 1.811(5) . ? N2 C9 1.426(8) . ? N2 C10 1.450(8) . ? Fe1 C1 1.820(5) 5_777 ? Fe1 C3 1.930(3) 5_777 ? Fe1 C3 1.930(3) 6_575 ? Fe1 C3 1.930(3) 2_757 ? Fe2 C2 1.811(5) 5_677 ? Fe2 C4 1.924(3) 6_575 ? Fe2 C4 1.924(3) 2_657 ? Fe2 C4 1.924(3) 5_677 ? Fe3 N3 2.136(3) 6_565 ? Fe3 N4 2.141(2) 6_565 ? 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 Fe1 178.5(5) . . ? N4 C4 Fe2 176.8(3) . . ? C5 O3 Fe3 123.4(3) . . ? C4 N4 Fe3 157.0(2) . . ? C6 O4 Fe3 122.3(3) . . ? C3 N3 Fe3 171.0(3) . . ? N3 C3 Fe1 178.2(3) . . ? C5 N1 C7 120.0(5) . . ? C5 N1 C8 121.8(5) . . ? C7 N1 C8 118.2(5) . . ? O3 C5 N1 124.6(5) . . ? O4 C6 N2 127.0(5) . . ? O2 C2 Fe2 179.4(5) . . ? C6 N2 C9 121.1(5) . . ? C6 N2 C10 122.1(6) . . ? C9 N2 C10 116.8(5) . . ? C1 Fe1 C1 180.000(2) 5_777 . ? C1 Fe1 C3 88.91(14) 5_777 5_777 ? C1 Fe1 C3 91.09(14) . 5_777 ? C1 Fe1 C3 91.09(14) 5_777 . ? C1 Fe1 C3 88.91(14) . . ? C3 Fe1 C3 180.000(1) 5_777 . ? C1 Fe1 C3 91.09(14) 5_777 6_575 ? C1 Fe1 C3 88.91(14) . 6_575 ? C3 Fe1 C3 88.73(16) 5_777 6_575 ? C3 Fe1 C3 91.27(16) . 6_575 ? C1 Fe1 C3 88.91(14) 5_777 2_757 ? C1 Fe1 C3 91.09(14) . 2_757 ? C3 Fe1 C3 91.27(16) 5_777 2_757 ? C3 Fe1 C3 88.73(16) . 2_757 ? C3 Fe1 C3 180.000(1) 6_575 2_757 ? C2 Fe2 C2 180.000(1) 5_677 . ? C2 Fe2 C4 91.01(14) 5_677 6_575 ? C2 Fe2 C4 88.99(14) . 6_575 ? C2 Fe2 C4 91.01(14) 5_677 . ? C2 Fe2 C4 88.99(14) . . ? C4 Fe2 C4 90.99(16) 6_575 . ? C2 Fe2 C4 88.99(14) 5_677 2_657 ? C2 Fe2 C4 91.01(14) . 2_657 ? C4 Fe2 C4 180.0 6_575 2_657 ? C4 Fe2 C4 89.01(16) . 2_657 ? C2 Fe2 C4 88.99(14) 5_677 5_677 ? C2 Fe2 C4 91.01(14) . 5_677 ? C4 Fe2 C4 89.01(16) 6_575 5_677 ? C4 Fe2 C4 180.00(15) . 5_677 ? C4 Fe2 C4 90.99(16) 2_657 5_677 ? O4 Fe3 N3 92.09(9) . . ? O4 Fe3 N3 92.09(9) . 6_565 ? N3 Fe3 N3 90.58(13) . 6_565 ? O4 Fe3 N4 92.41(9) . 6_565 ? N3 Fe3 N4 175.50(10) . 6_565 ? N3 Fe3 N4 89.19(9) 6_565 6_565 ? O4 Fe3 N4 92.41(9) . . ? N3 Fe3 N4 89.19(9) . . ? N3 Fe3 N4 175.50(10) 6_565 . ? N4 Fe3 N4 90.69(13) 6_565 . ? O4 Fe3 O3 179.68(13) . . ? N3 Fe3 O3 87.69(10) . . ? N3 Fe3 O3 87.69(9) 6_565 . ? N4 Fe3 O3 87.82(9) 6_565 . ? N4 Fe3 O3 87.82(9) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.473 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.060 #===END data_coh2o _audit_creation_method SHELXL-97 _chemical_name_systematic Cobalt(II)diaquo Iron(II)tetracyanodicarbonyl octahydrate ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H20 Co Fe N4 O12' _chemical_formula_weight 455.02 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' '-x, -y, -z' 'x, -y, z' _cell_length_a 6.971(2) _cell_length_b 7.467(2) _cell_length_c 9.267(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.377(5) _cell_angle_gamma 90.00 _cell_volume 474.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour pink _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 213 _exptl_absorpt_coefficient_mu 1.682 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2402 _exptl_absorpt_correction_T_max 0.3574 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2183 _diffrn_reflns_av_R_equivalents 0.0851 _diffrn_reflns_av_sigmaI/netI 0.0703 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 23.32 _reflns_number_total 755 _reflns_number_gt 513 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0866P)^2^+0.1210P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 755 _refine_ls_number_parameters 65 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0759 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1532 _refine_ls_wR_factor_gt 0.1392 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.006 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 Co1 Co 0.5000 0.0000 0.5000 0.0303(5) Uani 1 4 d S . . Fe1 Fe 0.0000 0.5000 0.5000 0.0296(6) Uani 1 4 d S . . O2 O 0.4707(9) 0.0000 0.7263(6) 0.0502(17) Uani 1 2 d S . . N1 N 0.2871(7) 0.1992(7) 0.4623(6) 0.0430(13) Uani 1 1 d . . . C2 C 0.0987(14) 0.5000 0.6926(12) 0.051(3) Uani 1 2 d S . . C1 C 0.1848(8) 0.3145(8) 0.4734(6) 0.0350(14) Uani 1 1 d . . . O1 O 0.1692(13) 0.5000 0.8145(9) 0.089(3) Uani 1 2 d S . . O5 O 0.0000 0.2132(14) 0.0000 0.122(4) Uani 1 2 d S . . O4 O 0.3848(9) 0.3073(9) 0.1112(6) 0.106(2) Uani 1 1 d . . . O3 O 0.0771(11) 0.0000 0.7670(8) 0.084(3) Uani 1 2 d S . . 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 Co1 0.0287(9) 0.0123(9) 0.0516(10) 0.000 0.0121(7) 0.000 Fe1 0.0286(10) 0.0113(9) 0.0496(11) 0.000 0.0088(7) 0.000 O2 0.053(4) 0.042(4) 0.056(4) 0.000 0.012(3) 0.000 N1 0.037(3) 0.019(3) 0.076(4) -0.002(3) 0.020(3) 0.005(2) C2 0.055(6) 0.031(6) 0.066(7) 0.000 0.008(5) 0.000 C1 0.034(3) 0.018(3) 0.054(3) 0.000(3) 0.012(3) -0.009(3) O1 0.120(8) 0.079(6) 0.060(5) 0.000 -0.007(5) 0.000 O5 0.124(8) 0.124(9) 0.127(8) 0.000 0.048(6) 0.000 O4 0.103(5) 0.104(6) 0.104(5) 0.042(4) 0.005(4) 0.000(4) O3 0.077(6) 0.095(7) 0.085(5) 0.000 0.023(4) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 2.086(5) 4 ? Co1 N1 2.086(5) 2_656 ? Co1 N1 2.086(5) . ? Co1 N1 2.086(5) 3_656 ? Co1 O2 2.143(6) 3_656 ? Co1 O2 2.143(6) . ? Fe1 C2 1.794(11) 3_566 ? Fe1 C2 1.794(11) . ? Fe1 C1 1.937(6) 4_565 ? Fe1 C1 1.937(6) 2_556 ? Fe1 C1 1.937(6) . ? Fe1 C1 1.937(6) 3_566 ? N1 C1 1.135(8) . ? C2 O1 1.147(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 180.00(19) 4 2_656 ? N1 Co1 N1 91.0(3) 4 . ? N1 Co1 N1 89.0(3) 2_656 . ? N1 Co1 N1 89.0(3) 4 3_656 ? N1 Co1 N1 91.0(3) 2_656 3_656 ? N1 Co1 N1 180.000(1) . 3_656 ? N1 Co1 O2 91.50(18) 4 3_656 ? N1 Co1 O2 88.50(18) 2_656 3_656 ? N1 Co1 O2 91.50(18) . 3_656 ? N1 Co1 O2 88.50(18) 3_656 3_656 ? N1 Co1 O2 88.50(18) 4 . ? N1 Co1 O2 91.50(18) 2_656 . ? N1 Co1 O2 88.50(18) . . ? N1 Co1 O2 91.50(18) 3_656 . ? O2 Co1 O2 180.000(1) 3_656 . ? C2 Fe1 C2 180.000(2) 3_566 . ? C2 Fe1 C1 91.0(3) 3_566 4_565 ? C2 Fe1 C1 89.0(3) . 4_565 ? C2 Fe1 C1 89.0(3) 3_566 2_556 ? C2 Fe1 C1 91.0(3) . 2_556 ? C1 Fe1 C1 180.0 4_565 2_556 ? C2 Fe1 C1 91.0(3) 3_566 . ? C2 Fe1 C1 89.0(3) . . ? C1 Fe1 C1 91.3(3) 4_565 . ? C1 Fe1 C1 88.7(3) 2_556 . ? C2 Fe1 C1 89.0(3) 3_566 3_566 ? C2 Fe1 C1 91.0(3) . 3_566 ? C1 Fe1 C1 88.7(3) 4_565 3_566 ? C1 Fe1 C1 91.3(3) 2_556 3_566 ? C1 Fe1 C1 180.0(3) . 3_566 ? C1 N1 Co1 165.0(5) . . ? O1 C2 Fe1 177.2(9) . . ? N1 C1 Fe1 175.9(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.32 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.998 _refine_diff_density_min -0.663 _refine_diff_density_rms 0.143 #===END