# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Cameron J. Kepert' _publ_contact_author_address ;School of Chemistry University of Sydney NSW 2006 Australia ; _publ_contact_author_email c.kepert@chem.usyd.edu.au _publ_contact_author_phone +61-2-9351-5741 _publ_contact_author_fax +61-2-9351-3329 _publ_section_title ; Dehydration of the nanoporous coordination framework ErIII[CoIII(CN)6]4H2O: single crystal to single crystal transformation and negative thermal expansion in ErIII[CoIII(CN)6] ; loop_ _publ_author_name _publ_author_address T.Pretsch ;School of Chemistry University of Sydney NSW 2006 Australia ; K.W.Chapman ;School of Chemistry University of Sydney NSW 2006 Australia ; C.J.Kepert ;School of Chemistry University of Sydney NSW 2006 Australia ; data_er100 _database_code_depnum_ccdc_archive 'CCDC 296836' _audit_creation_method SHELXL-97 _chemical_name_systematic ; erbium(III)-hexacyanocobaltate(III) ; _chemical_name_common erbium(iii)-hexacyanocobaltate(iii) _chemical_melting_point ? _chemical_formula_moiety 'C6 Co Er N6' _chemical_formula_sum 'C6 Co Er N6' _chemical_formula_weight 382.31 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' N N 0.0061 0.0033 '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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M 'P 63/m m c' _symmetry_space_group_name_Hall '-P 6c 2c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 7.3887(2) _cell_length_b 7.3887(2) _cell_length_c 13.0436(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 616.69(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5618 _cell_measurement_theta_min 3.124 _cell_measurement_theta_max 30.828 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.059 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 346 _exptl_absorpt_coefficient_mu 8.074 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2963 _exptl_absorpt_correction_T_max 0.410 _exptl_absorpt_process_details 'SADABS, Sheldrick 1996' _exptl_special_details ; Mounted on a thin smear of grease in an open-ended glass capillary. ; _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 graphite _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8106 _diffrn_reflns_av_R_equivalents 0.0173 _diffrn_reflns_av_sigmaI/netI 0.0069 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 31.21 _reflns_number_total 415 _reflns_number_gt 397 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BrukerAXS, 1997)' _computing_cell_refinement 'SMART (BrukerAXS, 1997)' _computing_data_reduction 'SAINT+ (BrukerAXS, 1997)' _computing_structure_solution 'SHELXTL (BrukerAXS, 2000)' _computing_structure_refinement 'SHELXTL (BrukerAXS, 2000)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997), WebLab ViewerPro 3.7 (Accelrys, 2001)' _computing_publication_material XCIF _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^)+(0.0076P)^2^+0.7335P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 415 _refine_ls_number_parameters 17 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0117 _refine_ls_R_factor_gt 0.0103 _refine_ls_wR_factor_ref 0.0256 _refine_ls_wR_factor_gt 0.0253 _refine_ls_goodness_of_fit_ref 1.268 _refine_ls_restrained_S_all 1.268 _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 Er1 Er 0.3333 0.6667 0.2500 0.00689(6) Uani 1 12 d S . . Co1 Co 1.0000 1.0000 0.0000 0.00700(11) Uani 1 12 d S . . C1 C 0.7604(3) 0.88020(15) 0.08431(13) 0.0116(3) Uani 1 2 d S . . N1 N 0.6156(3) 0.80781(14) 0.13694(13) 0.0164(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 Er1 0.00764(7) 0.00764(7) 0.00540(9) 0.000 0.000 0.00382(3) Co1 0.00746(16) 0.00746(16) 0.0061(2) 0.000 0.000 0.00373(8) C1 0.0124(9) 0.0132(6) 0.0090(7) -0.0006(3) -0.0013(7) 0.0062(4) N1 0.0123(8) 0.0207(7) 0.0133(7) 0.0004(3) 0.0009(6) 0.0061(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 Er1 N1 2.3319(17) . ? Er1 N1 2.3319(17) 16_556 ? Er1 N1 2.3319(17) 3_565 ? Er1 N1 2.3319(17) 17_666 ? Er1 N1 2.3319(17) 2_665 ? Er1 N1 2.3319(17) 18_566 ? Co1 C1 1.8868(19) . ? Co1 C1 1.8868(19) 2_765 ? Co1 C1 1.8868(19) 3_675 ? Co1 C1 1.8868(19) 15_655 ? Co1 C1 1.8868(19) 13_775 ? Co1 C1 1.8868(19) 14_565 ? C1 N1 1.153(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Er1 N1 78.46(9) . 16_556 ? N1 Er1 N1 84.26(6) . 3_565 ? N1 Er1 N1 134.43(3) 16_556 3_565 ? N1 Er1 N1 134.43(3) . 17_666 ? N1 Er1 N1 84.26(6) 16_556 17_666 ? N1 Er1 N1 134.43(3) 3_565 17_666 ? N1 Er1 N1 84.26(6) . 2_665 ? N1 Er1 N1 134.43(3) 16_556 2_665 ? N1 Er1 N1 84.26(6) 3_565 2_665 ? N1 Er1 N1 78.46(8) 17_666 2_665 ? N1 Er1 N1 134.43(3) . 18_566 ? N1 Er1 N1 84.26(6) 16_556 18_566 ? N1 Er1 N1 78.46(9) 3_565 18_566 ? N1 Er1 N1 84.26(6) 17_666 18_566 ? N1 Er1 N1 134.43(3) 2_665 18_566 ? C1 Co1 C1 89.45(8) . 2_765 ? C1 Co1 C1 89.45(8) . 3_675 ? C1 Co1 C1 89.45(8) 2_765 3_675 ? C1 Co1 C1 90.55(8) . 15_655 ? C1 Co1 C1 90.55(8) 2_765 15_655 ? C1 Co1 C1 180.0 3_675 15_655 ? C1 Co1 C1 180.0 . 13_775 ? C1 Co1 C1 90.55(8) 2_765 13_775 ? C1 Co1 C1 90.55(8) 3_675 13_775 ? C1 Co1 C1 89.45(8) 15_655 13_775 ? C1 Co1 C1 90.55(8) . 14_565 ? C1 Co1 C1 180.0 2_765 14_565 ? C1 Co1 C1 90.55(8) 3_675 14_565 ? C1 Co1 C1 89.45(8) 15_655 14_565 ? C1 Co1 C1 89.45(8) 13_775 14_565 ? N1 C1 Co1 179.12(17) . . ? C1 N1 Er1 177.31(16) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 31.21 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.754 _refine_diff_density_min -0.537 _refine_diff_density_rms 0.074 data_er150 _database_code_depnum_ccdc_archive 'CCDC 296837' _audit_creation_method SHELXL-97 _chemical_name_systematic ; erbium(III)-hexacyanocobaltate(III) ; _chemical_name_common erbium(iii)-hexacyanocobaltate(iii) _chemical_melting_point ? _chemical_formula_moiety 'C6 Co Er N6' _chemical_formula_sum 'C6 Co Er N6' _chemical_formula_weight 382.31 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' N N 0.0061 0.0033 '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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M 'P 63/m m c' _symmetry_space_group_name_Hall '-P 6c 2c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 7.3863(2) _cell_length_b 7.3863(2) _cell_length_c 13.0391(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 616.07(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5552 _cell_measurement_theta_min 3.125 _cell_measurement_theta_max 30.840 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.061 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 346 _exptl_absorpt_coefficient_mu 8.082 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.299 _exptl_absorpt_correction_T_max 0.411 _exptl_absorpt_process_details 'SADABS, Sheldrick 1996' _exptl_special_details ; Mounted on a thin smear of grease in an open-ended glass capillary. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8085 _diffrn_reflns_av_R_equivalents 0.0168 _diffrn_reflns_av_sigmaI/netI 0.0068 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 31.22 _reflns_number_total 415 _reflns_number_gt 395 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BrukerAXS, 1997)' _computing_cell_refinement 'SMART (BrukerAXS, 1997)' _computing_data_reduction 'SAINT+ (BrukerAXS, 1997)' _computing_structure_solution 'SHELXTL (BrukerAXS, 2000)' _computing_structure_refinement 'SHELXTL (BrukerAXS, 2000)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997), WebLab ViewerPro 3.7 (Accelrys, 2001)' _computing_publication_material XCIF _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^)+(0.0083P)^2^+0.6365P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 415 _refine_ls_number_parameters 17 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0113 _refine_ls_R_factor_gt 0.0100 _refine_ls_wR_factor_ref 0.0254 _refine_ls_wR_factor_gt 0.0251 _refine_ls_goodness_of_fit_ref 1.263 _refine_ls_restrained_S_all 1.263 _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 Er1 Er 0.3333 0.6667 0.2500 0.00814(6) Uani 1 12 d S . . Co1 Co 1.0000 1.0000 0.0000 0.00817(11) Uani 1 12 d S . . C1 C 0.7603(3) 0.88014(15) 0.08420(13) 0.0138(3) Uani 1 2 d S . . N1 N 0.6157(3) 0.80785(14) 0.13698(13) 0.0200(4) 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 Er1 0.00893(7) 0.00893(7) 0.00656(9) 0.000 0.000 0.00446(3) Co1 0.00877(16) 0.00877(16) 0.0070(2) 0.000 0.000 0.00438(8) C1 0.0135(9) 0.0160(6) 0.0112(7) -0.0006(3) -0.0012(7) 0.0068(4) N1 0.0143(8) 0.0261(7) 0.0157(7) 0.0011(3) 0.0022(6) 0.0071(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 Er1 N1 2.3311(18) . ? Er1 N1 2.3311(17) 16_556 ? Er1 N1 2.3311(17) 3_565 ? Er1 N1 2.3311(17) 17_666 ? Er1 N1 2.3311(17) 2_665 ? Er1 N1 2.3311(17) 18_566 ? Co1 C1 1.8859(19) . ? Co1 C1 1.8860(19) 3_675 ? Co1 C1 1.8860(19) 15_655 ? Co1 C1 1.8860(19) 13_775 ? Co1 C1 1.8860(19) 14_565 ? Co1 C1 1.8860(19) 2_765 ? C1 N1 1.153(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Er1 N1 78.42(9) . 16_556 ? N1 Er1 N1 84.29(6) . 3_565 ? N1 Er1 N1 134.41(3) 16_556 3_565 ? N1 Er1 N1 134.41(3) . 17_666 ? N1 Er1 N1 84.29(6) 16_556 17_666 ? N1 Er1 N1 134.41(3) 3_565 17_666 ? N1 Er1 N1 84.29(6) . 2_665 ? N1 Er1 N1 134.41(3) 16_556 2_665 ? N1 Er1 N1 84.29(6) 3_565 2_665 ? N1 Er1 N1 78.42(9) 17_666 2_665 ? N1 Er1 N1 134.41(3) . 18_566 ? N1 Er1 N1 84.29(6) 16_556 18_566 ? N1 Er1 N1 78.42(9) 3_565 18_566 ? N1 Er1 N1 84.29(6) 17_666 18_566 ? N1 Er1 N1 134.41(3) 2_665 18_566 ? C1 Co1 C1 89.52(8) . 3_675 ? C1 Co1 C1 90.48(8) . 15_655 ? C1 Co1 C1 180.0 3_675 15_655 ? C1 Co1 C1 179.999(1) . 13_775 ? C1 Co1 C1 90.48(8) 3_675 13_775 ? C1 Co1 C1 89.52(8) 15_655 13_775 ? C1 Co1 C1 90.48(8) . 14_565 ? C1 Co1 C1 90.48(8) 3_675 14_565 ? C1 Co1 C1 89.52(8) 15_655 14_565 ? C1 Co1 C1 89.52(8) 13_775 14_565 ? C1 Co1 C1 89.52(8) . 2_765 ? C1 Co1 C1 89.52(8) 3_675 2_765 ? C1 Co1 C1 90.48(8) 15_655 2_765 ? C1 Co1 C1 90.48(8) 13_775 2_765 ? C1 Co1 C1 180.0 14_565 2_765 ? N1 C1 Co1 178.95(17) . . ? C1 N1 Er1 177.44(16) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 31.22 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.700 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.071 data_er225 _database_code_depnum_ccdc_archive 'CCDC 296838' _audit_creation_method SHELXL-97 _chemical_name_systematic ; erbium(III)-hexacyanocobaltate(III) ; _chemical_name_common erbium(iii)-hexacyanocobaltate(iii) _chemical_melting_point ? _chemical_formula_moiety 'C6 Co Er N6' _chemical_formula_sum 'C6 Co Er N6' _chemical_formula_weight 382.31 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' N N 0.0061 0.0033 '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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M 'P 63/m m c' _symmetry_space_group_name_Hall '-P 6c 2c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 7.3828(2) _cell_length_b 7.3828(2) _cell_length_c 13.0303(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 615.07(4) _cell_formula_units_Z 2 _cell_measurement_temperature 225(2) _cell_measurement_reflns_used 5449 _cell_measurement_theta_min 3.127 _cell_measurement_theta_max 30.861 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.064 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 346 _exptl_absorpt_coefficient_mu 8.095 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.297 _exptl_absorpt_correction_T_max 0.411 _exptl_absorpt_process_details 'SADABS, Sheldrick 1996' _exptl_special_details ; Mounted on a thin smear of grease in an open-ended glass capillary. ; _diffrn_ambient_temperature 225(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8085 _diffrn_reflns_av_R_equivalents 0.0175 _diffrn_reflns_av_sigmaI/netI 0.0072 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 31.24 _reflns_number_total 415 _reflns_number_gt 392 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BrukerAXS, 1997)' _computing_cell_refinement 'SMART (BrukerAXS, 1997)' _computing_data_reduction 'SAINT+ (BrukerAXS, 1997)' _computing_structure_solution 'SHELXTL (BrukerAXS, 2000)' _computing_structure_refinement 'SHELXTL (BrukerAXS, 2000)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997), WebLab ViewerPro 3.7 (Accelrys, 2001)' _computing_publication_material XCIF _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^)+(0.0078P)^2^+0.5842P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 415 _refine_ls_number_parameters 17 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0115 _refine_ls_R_factor_gt 0.0099 _refine_ls_wR_factor_ref 0.0248 _refine_ls_wR_factor_gt 0.0245 _refine_ls_goodness_of_fit_ref 1.248 _refine_ls_restrained_S_all 1.248 _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 Er1 Er 0.3333 0.6667 0.2500 0.01015(6) Uani 1 12 d S . . Co1 Co 1.0000 1.0000 0.0000 0.01018(11) Uani 1 12 d S . . C1 C 0.7603(3) 0.88016(16) 0.08427(14) 0.0175(4) Uani 1 2 d S . . N1 N 0.6158(3) 0.80792(15) 0.13681(14) 0.0268(4) 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 Er1 0.01098(7) 0.01098(7) 0.00848(9) 0.000 0.000 0.00549(3) Co1 0.01090(16) 0.01090(16) 0.0087(2) 0.000 0.000 0.00545(8) C1 0.0169(9) 0.0202(7) 0.0143(8) -0.0002(3) -0.0004(7) 0.0085(4) N1 0.0187(9) 0.0358(8) 0.0203(8) 0.0023(3) 0.0046(7) 0.0093(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 Er1 N1 2.3320(18) 16_556 ? Er1 N1 2.3320(18) 3_565 ? Er1 N1 2.3320(18) 17_666 ? Er1 N1 2.3320(18) 2_665 ? Er1 N1 2.3320(18) 18_566 ? Er1 N1 2.3320(18) . ? Co1 C1 1.885(2) 3_675 ? Co1 C1 1.885(2) 15_655 ? Co1 C1 1.885(2) 13_775 ? Co1 C1 1.885(2) 14_565 ? Co1 C1 1.885(2) . ? Co1 C1 1.885(2) 2_765 ? C1 N1 1.150(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Er1 N1 134.43(3) 16_556 3_565 ? N1 Er1 N1 84.26(7) 16_556 17_666 ? N1 Er1 N1 134.43(3) 3_565 17_666 ? N1 Er1 N1 134.43(3) 16_556 2_665 ? N1 Er1 N1 84.26(7) 3_565 2_665 ? N1 Er1 N1 78.46(9) 17_666 2_665 ? N1 Er1 N1 84.26(7) 16_556 18_566 ? N1 Er1 N1 78.46(9) 3_565 18_566 ? N1 Er1 N1 84.26(7) 17_666 18_566 ? N1 Er1 N1 134.43(3) 2_665 18_566 ? N1 Er1 N1 78.47(9) 16_556 . ? N1 Er1 N1 84.26(7) 3_565 . ? N1 Er1 N1 134.43(3) 17_666 . ? N1 Er1 N1 84.26(7) 2_665 . ? N1 Er1 N1 134.43(3) 18_566 . ? C1 Co1 C1 180.0 3_675 15_655 ? C1 Co1 C1 90.51(8) 3_675 13_775 ? C1 Co1 C1 89.49(8) 15_655 13_775 ? C1 Co1 C1 90.51(8) 3_675 14_565 ? C1 Co1 C1 89.49(8) 15_655 14_565 ? C1 Co1 C1 89.49(8) 13_775 14_565 ? C1 Co1 C1 89.49(8) 3_675 . ? C1 Co1 C1 90.51(8) 15_655 . ? C1 Co1 C1 180.0 13_775 . ? C1 Co1 C1 90.51(8) 14_565 . ? C1 Co1 C1 89.49(8) 3_675 2_765 ? C1 Co1 C1 90.51(8) 15_655 2_765 ? C1 Co1 C1 90.51(8) 13_775 2_765 ? C1 Co1 C1 180.0 14_565 2_765 ? C1 Co1 C1 89.49(8) . 2_765 ? N1 C1 Co1 179.08(18) . . ? C1 N1 Er1 177.31(17) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 31.24 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.528 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.069 data_er300 _database_code_depnum_ccdc_archive 'CCDC 296839' _audit_creation_method SHELXL-97 _chemical_name_systematic ; erbium(III)-hexacyanocobaltate(III) ; _chemical_name_common erbium(iii)-hexacyanocobaltate(iii) _chemical_melting_point ? _chemical_formula_moiety 'C6 Co Er N6' _chemical_formula_sum 'C6 Co Er N6' _chemical_formula_weight 382.31 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' N N 0.0061 0.0033 '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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M 'P 63/m m c' _symmetry_space_group_name_Hall '-P 6c 2c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 7.3782(2) _cell_length_b 7.3782(2) _cell_length_c 13.0222(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 613.93(4) _cell_formula_units_Z 2 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 4170 _cell_measurement_theta_min 3.129 _cell_measurement_theta_max 30.684 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.068 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 346 _exptl_absorpt_coefficient_mu 8.111 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.309 _exptl_absorpt_correction_T_max 0.411 _exptl_absorpt_process_details 'SADABS, Sheldrick 1996' _exptl_special_details ; Mounted on a thin smear of grease in an open-ended glass capillary. ; _diffrn_ambient_temperature 300(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6345 _diffrn_reflns_av_R_equivalents 0.0185 _diffrn_reflns_av_sigmaI/netI 0.0082 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 30.85 _reflns_number_total 405 _reflns_number_gt 381 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BrukerAXS, 1997)' _computing_cell_refinement 'SMART (BrukerAXS, 1997)' _computing_data_reduction 'SAINT+ (BrukerAXS, 1997)' _computing_structure_solution 'SHELXTL (BrukerAXS, 2000)' _computing_structure_refinement 'SHELXTL (BrukerAXS, 2000)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997), WebLab ViewerPro 3.7 (Accelrys, 2001)' _computing_publication_material XCIF _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^)+(0.0071P)^2^+0.5473P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 405 _refine_ls_number_parameters 17 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0115 _refine_ls_R_factor_gt 0.0100 _refine_ls_wR_factor_ref 0.0265 _refine_ls_wR_factor_gt 0.0262 _refine_ls_goodness_of_fit_ref 1.331 _refine_ls_restrained_S_all 1.331 _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 Er1 Er 0.3333 0.6667 0.2500 0.01238(7) Uani 1 12 d S . . Co1 Co 1.0000 1.0000 0.0000 0.01218(13) Uani 1 12 d S . . C1 C 0.7599(4) 0.87997(18) 0.08450(16) 0.0209(4) Uani 1 2 d S . . N1 N 0.6155(3) 0.80776(17) 0.13684(16) 0.0334(5) 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 Er1 0.01330(8) 0.01330(8) 0.01053(10) 0.000 0.000 0.00665(4) Co1 0.01312(18) 0.01312(18) 0.0103(3) 0.000 0.000 0.00656(9) C1 0.0191(10) 0.0247(8) 0.0172(9) 0.0002(4) 0.0005(8) 0.0096(5) N1 0.0224(11) 0.0451(11) 0.0251(10) 0.0032(4) 0.0063(8) 0.0112(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 N1 2.329(2) 16_556 ? Er1 N1 2.329(2) 3_565 ? Er1 N1 2.329(2) 17_666 ? Er1 N1 2.329(2) 2_665 ? Er1 N1 2.329(2) 18_566 ? Er1 N1 2.329(2) . ? Co1 C1 1.888(2) 15_655 ? Co1 C1 1.888(2) 13_775 ? Co1 C1 1.888(2) 14_565 ? Co1 C1 1.888(2) 2_765 ? Co1 C1 1.888(2) 3_675 ? Co1 C1 1.888(2) . ? C1 N1 1.147(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Er1 N1 134.45(4) 16_556 3_565 ? N1 Er1 N1 84.22(8) 16_556 17_666 ? N1 Er1 N1 134.45(4) 3_565 17_666 ? N1 Er1 N1 134.45(4) 16_556 2_665 ? N1 Er1 N1 84.22(8) 3_565 2_665 ? N1 Er1 N1 78.52(11) 17_666 2_665 ? N1 Er1 N1 84.22(8) 16_556 18_566 ? N1 Er1 N1 78.52(11) 3_565 18_566 ? N1 Er1 N1 84.22(8) 17_666 18_566 ? N1 Er1 N1 134.45(4) 2_665 18_566 ? N1 Er1 N1 78.52(11) 16_556 . ? N1 Er1 N1 84.22(8) 3_565 . ? N1 Er1 N1 134.45(4) 17_666 . ? N1 Er1 N1 84.22(8) 2_665 . ? N1 Er1 N1 134.45(4) 18_566 . ? C1 Co1 C1 89.45(9) 15_655 13_775 ? C1 Co1 C1 89.45(9) 15_655 14_565 ? C1 Co1 C1 89.45(9) 13_775 14_565 ? C1 Co1 C1 90.55(9) 15_655 2_765 ? C1 Co1 C1 90.55(9) 13_775 2_765 ? C1 Co1 C1 180.0 14_565 2_765 ? C1 Co1 C1 180.00(8) 15_655 3_675 ? C1 Co1 C1 90.55(9) 13_775 3_675 ? C1 Co1 C1 90.55(9) 14_565 3_675 ? C1 Co1 C1 89.45(9) 2_765 3_675 ? C1 Co1 C1 90.55(9) 15_655 . ? C1 Co1 C1 180.0 13_775 . ? C1 Co1 C1 90.55(9) 14_565 . ? C1 Co1 C1 89.45(9) 2_765 . ? C1 Co1 C1 89.45(9) 3_675 . ? N1 C1 Co1 179.2(2) . . ? C1 N1 Er1 177.2(2) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 30.85 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.505 _refine_diff_density_min -0.530 _refine_diff_density_rms 0.072 data_er375 _database_code_depnum_ccdc_archive 'CCDC 296840' _audit_creation_method SHELXL-97 _chemical_name_systematic ; erbium(III)-hexacyanocobaltate(III) ; _chemical_name_common erbium(iii)-hexacyanocobaltate(iii) _chemical_melting_point ? _chemical_formula_moiety 'C6 Co Er N6' _chemical_formula_sum 'C6 Co Er N6' _chemical_formula_weight 382.31 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' N N 0.0061 0.0033 '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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M 'P 63/m m c' _symmetry_space_group_name_Hall '-P 6c 2c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' '-y, -x, z' '-x+y, y, z' 'x, x-y, z' 'y, x, z-1/2' 'x-y, -y, z-1/2' '-x, -x+y, z-1/2' _cell_length_a 7.3719(2) _cell_length_b 7.3719(2) _cell_length_c 13.0109(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 612.35(4) _cell_formula_units_Z 2 _cell_measurement_temperature 375(2) _cell_measurement_reflns_used 4398 _cell_measurement_theta_min 3.132 _cell_measurement_theta_max 30.675 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.073 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 346 _exptl_absorpt_coefficient_mu 8.132 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.299 _exptl_absorpt_correction_T_max 0.411 _exptl_absorpt_process_details 'SADABS, Sheldrick 1996' _exptl_special_details ; Mounted on a thin smear of grease in an open-ended glass capillary. ; _diffrn_ambient_temperature 375(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7336 _diffrn_reflns_av_R_equivalents 0.0185 _diffrn_reflns_av_sigmaI/netI 0.0081 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 31.10 _reflns_number_total 412 _reflns_number_gt 384 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BrukerAXS, 1997)' _computing_cell_refinement 'SMART (BrukerAXS, 1997)' _computing_data_reduction 'SAINT+ (BrukerAXS, 1997)' _computing_structure_solution 'SHELXTL (BrukerAXS, 2000)' _computing_structure_refinement 'SHELXTL (BrukerAXS, 2000)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997), WebLab ViewerPro 3.7 (Accelrys, 2001)' _computing_publication_material XCIF _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^)+(0.0059P)^2^+0.4185P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 412 _refine_ls_number_parameters 17 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0124 _refine_ls_R_factor_gt 0.0105 _refine_ls_wR_factor_ref 0.0236 _refine_ls_wR_factor_gt 0.0232 _refine_ls_goodness_of_fit_ref 1.305 _refine_ls_restrained_S_all 1.305 _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 Er1 Er 0.3333 0.6667 0.2500 0.01456(6) Uani 1 12 d S . . Co1 Co 1.0000 1.0000 0.0000 0.01448(12) Uani 1 12 d S . . C1 C 0.7596(3) 0.87981(17) 0.08451(15) 0.0249(4) Uani 1 2 d S . . N1 N 0.6161(3) 0.80804(16) 0.13674(15) 0.0406(5) 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 Er1 0.01543(7) 0.01543(7) 0.01282(9) 0.000 0.000 0.00772(3) Co1 0.01552(17) 0.01552(17) 0.0124(2) 0.000 0.000 0.00776(8) C1 0.0228(10) 0.0293(8) 0.0203(8) 0.0008(4) 0.0017(8) 0.0114(5) N1 0.0265(10) 0.0551(11) 0.0308(9) 0.0046(4) 0.0091(8) 0.0132(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Er1 N1 2.3303(19) 16_556 ? Er1 N1 2.3303(19) 3_565 ? Er1 N1 2.330(2) . ? Er1 N1 2.3303(19) 17_666 ? Er1 N1 2.3303(19) 2_665 ? Er1 N1 2.3303(19) 18_566 ? Co1 C1 1.888(2) 3_675 ? Co1 C1 1.888(2) 15_655 ? Co1 C1 1.888(2) 13_775 ? Co1 C1 1.888(2) . ? Co1 C1 1.888(2) 14_565 ? Co1 C1 1.888(2) 2_765 ? C1 N1 1.141(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Er1 N1 134.42(4) 16_556 3_565 ? N1 Er1 N1 78.46(10) 16_556 . ? N1 Er1 N1 84.27(8) 3_565 . ? N1 Er1 N1 84.27(8) 16_556 17_666 ? N1 Er1 N1 134.42(4) 3_565 17_666 ? N1 Er1 N1 134.42(4) . 17_666 ? N1 Er1 N1 134.42(4) 16_556 2_665 ? N1 Er1 N1 84.27(8) 3_565 2_665 ? N1 Er1 N1 84.27(8) . 2_665 ? N1 Er1 N1 78.46(10) 17_666 2_665 ? N1 Er1 N1 84.27(8) 16_556 18_566 ? N1 Er1 N1 78.46(10) 3_565 18_566 ? N1 Er1 N1 134.42(4) . 18_566 ? N1 Er1 N1 84.27(8) 17_666 18_566 ? N1 Er1 N1 134.42(4) 2_665 18_566 ? C1 Co1 C1 180.0 3_675 15_655 ? C1 Co1 C1 90.51(9) 3_675 13_775 ? C1 Co1 C1 89.49(9) 15_655 13_775 ? C1 Co1 C1 89.49(9) 3_675 . ? C1 Co1 C1 90.51(9) 15_655 . ? C1 Co1 C1 180.0 13_775 . ? C1 Co1 C1 90.51(9) 3_675 14_565 ? C1 Co1 C1 89.49(9) 15_655 14_565 ? C1 Co1 C1 89.49(9) 13_775 14_565 ? C1 Co1 C1 90.51(9) . 14_565 ? C1 Co1 C1 89.49(9) 3_675 2_765 ? C1 Co1 C1 90.51(9) 15_655 2_765 ? C1 Co1 C1 90.51(9) 13_775 2_765 ? C1 Co1 C1 89.49(9) . 2_765 ? C1 Co1 C1 180.0 14_565 2_765 ? N1 C1 Co1 179.07(19) . . ? C1 N1 Er1 177.33(19) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 31.10 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.445 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.068 data_er100w _database_code_depnum_ccdc_archive 'CCDC 296841' _audit_creation_method SHELXL-97 _chemical_name_systematic ; erbium(III)-hexacyanocobaltate(III)tetrahydrate ; _chemical_name_common erbium(iii)-hexacyanocobaltate(iii)tetrahydrate _chemical_melting_point ? _chemical_formula_moiety 'C6 H4 Co Er N6 O2, 2(H2 O)' _chemical_formula_sum 'C6 H8 Co Er N6 O4' _chemical_formula_weight 454.37 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'C m c m' _symmetry_space_group_name_Hall '-C 2c 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 7.2835(11) _cell_length_b 12.5836(19) _cell_length_c 13.462(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1233.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 729 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 27.96 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 8.115 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.217 _exptl_absorpt_correction_T_max 0.410 _exptl_absorpt_process_details 'SADABS, Sheldrick 1996' _exptl_special_details ; Mounted on a thin smear of grease in an open-ended glass capillary. ; _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 graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 85 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 4247 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0260 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.96 _reflns_number_total 835 _reflns_number_gt 791 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BrukerAXS, 1997)' _computing_cell_refinement 'SMART (BrukerAXS, 1997)' _computing_data_reduction 'SAINT+ (BrukerAXS, 1997)' _computing_structure_solution 'SHELXTL (BrukerAXS, 2000)' _computing_structure_refinement 'SHELXTL (BrukerAXS, 2000)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997), WebLab ViewerPro 3.7 (Accelrys, 2001)' _computing_publication_material XCIF _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^)+(0.0359P)^2^+10.2366P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 835 _refine_ls_number_parameters 58 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0297 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0701 _refine_ls_wR_factor_gt 0.0688 _refine_ls_goodness_of_fit_ref 1.172 _refine_ls_restrained_S_all 1.170 _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 Er1 Er 0.0000 0.32498(3) 0.7500 0.00749(14) Uani 1 4 d S . . Co1 Co 0.0000 0.0000 0.5000 0.0082(2) Uani 1 4 d S . . N1 N 0.0000 0.2185(4) 0.5974(4) 0.0139(11) Uani 1 2 d S . . C1 C 0.0000 0.1354(5) 0.5598(5) 0.0119(12) Uani 1 2 d S . . N2 N 0.2007(5) 0.4240(3) 0.6406(3) 0.0148(8) Uani 1 1 d . . . C2 C 0.3158(6) 0.4534(3) 0.5888(3) 0.0131(9) Uani 1 1 d . . . O1 O 0.2584(7) 0.2180(4) 0.7500 0.0198(10) Uani 1 2 d SD . . H1 H 0.342(8) 0.212(5) 0.701(4) 0.030 Uiso 1 1 d D . . O2 O 0.0000 0.6556(4) 0.6002(4) 0.0187(10) Uani 1 2 d SD . . H2 H 0.0000 0.695(6) 0.544(5) 0.028 Uiso 1 2 d SD . . H3 H 0.0000 0.584(4) 0.604(7) 0.028 Uiso 1 2 d SD . . 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 Er1 0.0056(2) 0.0079(2) 0.0089(2) 0.000 0.000 0.000 Co1 0.0066(5) 0.0073(5) 0.0106(6) 0.0001(4) 0.000 0.000 N1 0.013(3) 0.014(3) 0.014(3) -0.003(2) 0.000 0.000 C1 0.011(3) 0.014(3) 0.010(3) 0.003(2) 0.000 0.000 N2 0.0108(18) 0.0196(19) 0.0140(18) 0.0004(15) -0.0011(15) -0.0035(15) C2 0.014(2) 0.011(2) 0.015(2) -0.0004(16) -0.0022(17) 0.0018(16) O1 0.017(2) 0.028(3) 0.015(2) 0.000 0.000 0.007(2) O2 0.019(3) 0.019(2) 0.018(2) 0.001(2) 0.000 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 Er1 O1 2.314(5) 3_556 ? Er1 O1 2.314(5) . ? Er1 N2 2.421(4) . ? Er1 N2 2.421(4) 10_557 ? Er1 N2 2.421(4) 12 ? Er1 N2 2.421(4) 3_556 ? Er1 N1 2.453(5) . ? Er1 N1 2.453(5) 10_557 ? Co1 C1 1.884(6) 9_556 ? Co1 C1 1.884(6) . ? Co1 C2 1.890(5) 16_545 ? Co1 C2 1.890(5) 8_456 ? Co1 C2 1.890(5) 5_445 ? Co1 C2 1.890(5) 13_556 ? N1 C1 1.162(9) . ? N2 C2 1.151(6) . ? C2 Co1 1.890(5) 5 ? O1 H1 0.90(5) . ? O2 H2 0.90(5) . ? O2 H3 0.90(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 Er1 O1 108.8(3) 3_556 . ? O1 Er1 N2 142.24(9) 3_556 . ? O1 Er1 N2 78.96(14) . . ? O1 Er1 N2 142.24(9) 3_556 10_557 ? O1 Er1 N2 78.96(14) . 10_557 ? N2 Er1 N2 74.98(18) . 10_557 ? O1 Er1 N2 78.96(14) 3_556 12 ? O1 Er1 N2 142.24(9) . 12 ? N2 Er1 N2 74.29(19) . 12 ? N2 Er1 N2 118.04(19) 10_557 12 ? O1 Er1 N2 78.96(14) 3_556 3_556 ? O1 Er1 N2 142.24(9) . 3_556 ? N2 Er1 N2 118.04(19) . 3_556 ? N2 Er1 N2 74.29(19) 10_557 3_556 ? N2 Er1 N2 74.98(18) 12 3_556 ? O1 Er1 N1 71.47(9) 3_556 . ? O1 Er1 N1 71.47(9) . . ? N2 Er1 N1 76.78(14) . . ? N2 Er1 N1 142.28(10) 10_557 . ? N2 Er1 N1 76.78(14) 12 . ? N2 Er1 N1 142.28(10) 3_556 . ? O1 Er1 N1 71.47(9) 3_556 10_557 ? O1 Er1 N1 71.47(9) . 10_557 ? N2 Er1 N1 142.28(10) . 10_557 ? N2 Er1 N1 76.78(14) 10_557 10_557 ? N2 Er1 N1 142.28(10) 12 10_557 ? N2 Er1 N1 76.78(14) 3_556 10_557 ? N1 Er1 N1 113.8(3) . 10_557 ? C1 Co1 C1 180.0 9_556 . ? C1 Co1 C2 89.41(19) 9_556 16_545 ? C1 Co1 C2 90.59(19) . 16_545 ? C1 Co1 C2 90.59(19) 9_556 8_456 ? C1 Co1 C2 89.41(19) . 8_456 ? C2 Co1 C2 180.0 16_545 8_456 ? C1 Co1 C2 89.41(19) 9_556 5_445 ? C1 Co1 C2 90.59(19) . 5_445 ? C2 Co1 C2 90.4(3) 16_545 5_445 ? C2 Co1 C2 89.6(3) 8_456 5_445 ? C1 Co1 C2 90.59(19) 9_556 13_556 ? C1 Co1 C2 89.41(19) . 13_556 ? C2 Co1 C2 89.6(3) 16_545 13_556 ? C2 Co1 C2 90.4(3) 8_456 13_556 ? C2 Co1 C2 180.0 5_445 13_556 ? C1 N1 Er1 148.9(5) . . ? N1 C1 Co1 179.5(6) . . ? C2 N2 Er1 166.8(4) . . ? N2 C2 Co1 178.0(4) . 5 ? Er1 O1 H1 126(4) . . ? H2 O2 H3 126(8) . . ? 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 H1 O2 0.90(5) 1.92(5) 2.789(5) 162(6) 5_545 O2 H2 N1 0.90(5) 2.19(5) 3.095(8) 176(8) 9_566 O2 H3 N2 0.90(5) 2.54(4) 3.306(6) 143(2) . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.96 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.009 _refine_diff_density_min -1.670 _refine_diff_density_rms 0.217 data_er150w _database_code_depnum_ccdc_archive 'CCDC 296842' _audit_creation_method SHELXL-97 _chemical_name_systematic ; erbium(III)-hexacyanocobaltate(III)tetrahydrate ; _chemical_name_common erbium(iii)-hexacyanocobaltate(iii)tetrahydrate _chemical_melting_point ? _chemical_formula_moiety 'C6 H4 Co Er N6 O2, 2(H2 O)' _chemical_formula_sum 'C6 H8 Co Er N6 O4' _chemical_formula_weight 454.37 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'C m c m' _symmetry_space_group_name_Hall '-C 2c 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 7.2858(12) _cell_length_b 12.601(2) _cell_length_c 13.469(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1236.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 713 _cell_measurement_theta_min 3.025 _cell_measurement_theta_max 27.714 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.441 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 8.097 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.214 _exptl_absorpt_correction_T_max 0.410 _exptl_absorpt_process_details 'SADABS, Sheldrick 1996' _exptl_special_details ; Mounted on a thin smear of grease in an open-ended glass capillary. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 85 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 4247 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.94 _reflns_number_total 833 _reflns_number_gt 787 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BrukerAXS, 1997)' _computing_cell_refinement 'SMART (BrukerAXS, 1997)' _computing_data_reduction 'SAINT+ (BrukerAXS, 1997)' _computing_structure_solution 'SHELXTL (BrukerAXS, 2000)' _computing_structure_refinement 'SHELXTL (BrukerAXS, 2000)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997), WebLab ViewerPro 3.7 (Accelrys, 2001)' _computing_publication_material XCIF _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^)+(0.0407P)^2^+7.5518P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 833 _refine_ls_number_parameters 58 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0740 _refine_ls_wR_factor_gt 0.0717 _refine_ls_goodness_of_fit_ref 1.190 _refine_ls_restrained_S_all 1.187 _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 Er1 Er 0.0000 0.32497(3) 0.7500 0.00849(15) Uani 1 4 d S . . Co1 Co 0.0000 0.0000 0.5000 0.0091(3) Uani 1 4 d S . . N1 N 0.0000 0.2178(5) 0.5985(4) 0.0163(11) Uani 1 2 d S . . C1 C 0.0000 0.1351(5) 0.5607(5) 0.0132(12) Uani 1 2 d S . . N2 N 0.2009(6) 0.4237(3) 0.6407(3) 0.0167(8) Uani 1 1 d . . . C2 C 0.3155(6) 0.4532(3) 0.5886(3) 0.0138(9) Uani 1 1 d . . . O1 O 0.2587(8) 0.2186(4) 0.7500 0.0227(11) Uani 1 2 d SD . . H1 H 0.344(8) 0.215(5) 0.697(4) 0.034 Uiso 1 1 d D . . O2 O 0.0000 0.6558(4) 0.6004(4) 0.0229(11) Uani 1 2 d SD . . H2 H 0.0000 0.689(7) 0.537(5) 0.034 Uiso 1 2 d SD . . H3 H 0.0000 0.581(4) 0.598(7) 0.034 Uiso 1 2 d SD . . 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 Er1 0.0070(2) 0.0090(2) 0.0095(2) 0.000 0.000 0.000 Co1 0.0084(5) 0.0084(5) 0.0106(6) 0.0001(4) 0.000 0.000 N1 0.018(3) 0.015(3) 0.016(3) -0.003(2) 0.000 0.000 C1 0.009(3) 0.017(3) 0.014(3) 0.002(2) 0.000 0.000 N2 0.0114(18) 0.021(2) 0.0177(19) 0.0021(16) -0.0005(15) -0.0045(15) C2 0.014(2) 0.012(2) 0.016(2) -0.0001(16) -0.0017(17) 0.0007(16) O1 0.018(3) 0.035(3) 0.015(2) 0.000 0.000 0.012(2) O2 0.023(3) 0.024(3) 0.021(3) 0.001(2) 0.000 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 Er1 O1 2.313(5) . ? Er1 O1 2.313(5) 3_556 ? Er1 N2 2.420(4) . ? Er1 N2 2.420(4) 10_557 ? Er1 N2 2.420(4) 12 ? Er1 N2 2.420(4) 3_556 ? Er1 N1 2.447(6) . ? Er1 N1 2.447(6) 10_557 ? Co1 C1 1.889(7) . ? Co1 C1 1.889(7) 9_556 ? Co1 C2 1.892(5) 16_545 ? Co1 C2 1.892(5) 8_456 ? Co1 C2 1.892(5) 5_445 ? Co1 C2 1.892(5) 13_556 ? N1 C1 1.160(9) . ? N2 C2 1.152(6) . ? C2 Co1 1.892(5) 5 ? O1 H1 0.94(5) . ? O2 H2 0.95(5) . ? O2 H3 0.95(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 Er1 O1 109.1(3) . 3_556 ? O1 Er1 N2 78.75(15) . . ? O1 Er1 N2 142.26(10) 3_556 . ? O1 Er1 N2 78.75(15) . 10_557 ? O1 Er1 N2 142.26(10) 3_556 10_557 ? N2 Er1 N2 74.92(19) . 10_557 ? O1 Er1 N2 142.26(10) . 12 ? O1 Er1 N2 78.75(15) 3_556 12 ? N2 Er1 N2 74.4(2) . 12 ? N2 Er1 N2 118.1(2) 10_557 12 ? O1 Er1 N2 142.26(10) . 3_556 ? O1 Er1 N2 78.75(15) 3_556 3_556 ? N2 Er1 N2 118.1(2) . 3_556 ? N2 Er1 N2 74.4(2) 10_557 3_556 ? N2 Er1 N2 74.92(19) 12 3_556 ? O1 Er1 N1 71.34(10) . . ? O1 Er1 N1 71.34(10) 3_556 . ? N2 Er1 N1 77.09(14) . . ? N2 Er1 N1 142.27(10) 10_557 . ? N2 Er1 N1 77.09(14) 12 . ? N2 Er1 N1 142.27(10) 3_556 . ? O1 Er1 N1 71.34(10) . 10_557 ? O1 Er1 N1 71.34(10) 3_556 10_557 ? N2 Er1 N1 142.27(10) . 10_557 ? N2 Er1 N1 77.09(14) 10_557 10_557 ? N2 Er1 N1 142.27(10) 12 10_557 ? N2 Er1 N1 77.09(14) 3_556 10_557 ? N1 Er1 N1 113.0(3) . 10_557 ? C1 Co1 C1 180.0 . 9_556 ? C1 Co1 C2 90.4(2) . 16_545 ? C1 Co1 C2 89.6(2) 9_556 16_545 ? C1 Co1 C2 89.6(2) . 8_456 ? C1 Co1 C2 90.4(2) 9_556 8_456 ? C2 Co1 C2 180.0(2) 16_545 8_456 ? C1 Co1 C2 90.4(2) . 5_445 ? C1 Co1 C2 89.6(2) 9_556 5_445 ? C2 Co1 C2 90.5(3) 16_545 5_445 ? C2 Co1 C2 89.5(3) 8_456 5_445 ? C1 Co1 C2 89.6(2) . 13_556 ? C1 Co1 C2 90.4(2) 9_556 13_556 ? C2 Co1 C2 89.5(3) 16_545 13_556 ? C2 Co1 C2 90.5(3) 8_456 13_556 ? C2 Co1 C2 180.0 5_445 13_556 ? C1 N1 Er1 149.5(5) . . ? N1 C1 Co1 179.6(6) . . ? C2 N2 Er1 167.1(4) . . ? N2 C2 Co1 178.4(4) . 5 ? Er1 O1 H1 124(4) . . ? H2 O2 H3 115(8) . . ? 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 H1 O2 0.94(5) 1.89(5) 2.789(6) 159(6) 5_545 O2 H2 N1 0.95(5) 2.17(5) 3.117(8) 173(8) 9_566 O2 H3 N2 0.95(5) 2.53(5) 3.315(6) 141(3) . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.94 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.526 _refine_diff_density_min -1.418 _refine_diff_density_rms 0.227 data_er225w _database_code_depnum_ccdc_archive 'CCDC 296843' _audit_creation_method SHELXL-97 _chemical_name_systematic ; erbium(III)-hexacyanocobaltate(III)tetrahydrate ; _chemical_name_common erbium(iii)-hexacyanocobaltate(iii)tetrahydrate _chemical_melting_point ? _chemical_formula_moiety 'C6 H4 Co Er N6 O2, 2(H2 O)' _chemical_formula_sum 'C6 H8 Co Er N6 O4' _chemical_formula_weight 454.37 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'C m c m' _symmetry_space_group_name_Hall '-C 2c 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 7.2828(12) _cell_length_b 12.623(2) _cell_length_c 13.471(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1238.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 225(2) _cell_measurement_reflns_used 687 _cell_measurement_theta_min 3.025 _cell_measurement_theta_max 27.712 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 8.085 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.218 _exptl_absorpt_correction_T_max 0.411 _exptl_absorpt_process_details 'SADABS, Sheldrick 1996' _exptl_special_details ; Mounted on a thin smear of grease in an open-ended glass capillary. ; _diffrn_ambient_temperature 225(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 80 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 4255 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.93 _reflns_number_total 834 _reflns_number_gt 786 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BrukerAXS, 1997)' _computing_cell_refinement 'SMART (BrukerAXS, 1997)' _computing_data_reduction 'SAINT+ (BrukerAXS, 1997)' _computing_structure_solution 'SHELXTL (BrukerAXS, 2000)' _computing_structure_refinement 'SHELXTL (BrukerAXS, 2000)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997), WebLab ViewerPro 3.7 (Accelrys, 2001)' _computing_publication_material XCIF _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^)+(0.0423P)^2^+10.2718P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 834 _refine_ls_number_parameters 58 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0765 _refine_ls_wR_factor_gt 0.0742 _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_restrained_S_all 1.147 _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 Er1 Er 0.0000 0.32494(3) 0.7500 0.01066(16) Uani 1 4 d S . . Co1 Co 0.0000 0.0000 0.5000 0.0110(3) Uani 1 4 d S . . N1 N 0.0000 0.2172(5) 0.5991(5) 0.0212(13) Uani 1 2 d S . . C1 C 0.0000 0.1343(5) 0.5611(5) 0.0170(13) Uani 1 2 d S . . N2 N 0.2007(6) 0.4235(3) 0.6403(3) 0.0215(9) Uani 1 1 d . . . C2 C 0.3151(7) 0.4530(4) 0.5883(4) 0.0158(9) Uani 1 1 d . . . O1 O 0.2590(8) 0.2192(5) 0.7500 0.0298(13) Uani 1 2 d SD . . H1 H 0.352(9) 0.214(6) 0.698(5) 0.045 Uiso 1 1 d D . . O2 O 0.0000 0.6561(5) 0.6000(5) 0.0301(13) Uani 1 2 d SD . . H2 H 0.0000 0.693(8) 0.535(6) 0.045 Uiso 1 2 d SD . . H3 H 0.0000 0.578(4) 0.606(8) 0.045 Uiso 1 2 d SD . . 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 Er1 0.0090(2) 0.0112(2) 0.0118(2) 0.000 0.000 0.000 Co1 0.0103(6) 0.0099(6) 0.0130(6) -0.0003(4) 0.000 0.000 N1 0.022(3) 0.020(3) 0.021(3) -0.008(3) 0.000 0.000 C1 0.017(3) 0.015(3) 0.018(3) 0.004(3) 0.000 0.000 N2 0.019(2) 0.027(2) 0.018(2) 0.0032(17) -0.0001(17) -0.0051(17) C2 0.017(2) 0.014(2) 0.017(2) 0.0006(17) -0.0030(18) -0.0016(17) O1 0.024(3) 0.041(3) 0.024(3) 0.000 0.000 0.016(3) O2 0.032(3) 0.031(3) 0.027(3) -0.001(2) 0.000 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 Er1 O1 2.311(6) . ? Er1 O1 2.311(6) 3_556 ? Er1 N2 2.423(4) 10_557 ? Er1 N2 2.423(4) 12 ? Er1 N2 2.423(4) 3_556 ? Er1 N2 2.423(4) . ? Er1 N1 2.446(6) . ? Er1 N1 2.446(6) 10_557 ? Co1 C1 1.885(7) 9_556 ? Co1 C1 1.885(7) . ? Co1 C2 1.892(5) 16_545 ? Co1 C2 1.892(5) 8_456 ? Co1 C2 1.892(5) 5_445 ? Co1 C2 1.892(5) 13_556 ? N1 C1 1.164(10) . ? N2 C2 1.150(7) . ? C2 Co1 1.892(5) 5 ? O1 H1 0.98(5) . ? O2 H2 0.99(5) . ? O2 H3 0.99(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 Er1 O1 109.4(3) . 3_556 ? O1 Er1 N2 78.71(17) . 10_557 ? O1 Er1 N2 142.12(11) 3_556 10_557 ? O1 Er1 N2 142.12(11) . 12 ? O1 Er1 N2 78.71(17) 3_556 12 ? N2 Er1 N2 118.2(2) 10_557 12 ? O1 Er1 N2 142.12(11) . 3_556 ? O1 Er1 N2 78.71(17) 3_556 3_556 ? N2 Er1 N2 74.2(2) 10_557 3_556 ? N2 Er1 N2 75.2(2) 12 3_556 ? O1 Er1 N2 78.71(17) . . ? O1 Er1 N2 142.12(11) 3_556 . ? N2 Er1 N2 75.2(2) 10_557 . ? N2 Er1 N2 74.2(2) 12 . ? N2 Er1 N2 118.2(2) 3_556 . ? O1 Er1 N1 71.26(11) . . ? O1 Er1 N1 71.26(12) 3_556 . ? N2 Er1 N1 142.43(11) 10_557 . ? N2 Er1 N1 77.22(16) 12 . ? N2 Er1 N1 142.43(11) 3_556 . ? N2 Er1 N1 77.22(16) . . ? O1 Er1 N1 71.26(11) . 10_557 ? O1 Er1 N1 71.26(12) 3_556 10_557 ? N2 Er1 N1 77.22(16) 10_557 10_557 ? N2 Er1 N1 142.43(11) 12 10_557 ? N2 Er1 N1 77.22(16) 3_556 10_557 ? N2 Er1 N1 142.43(11) . 10_557 ? N1 Er1 N1 112.4(3) . 10_557 ? C1 Co1 C1 179.999(1) 9_556 . ? C1 Co1 C2 89.6(2) 9_556 16_545 ? C1 Co1 C2 90.4(2) . 16_545 ? C1 Co1 C2 90.4(2) 9_556 8_456 ? C1 Co1 C2 89.6(2) . 8_456 ? C2 Co1 C2 180.000(1) 16_545 8_456 ? C1 Co1 C2 89.6(2) 9_556 5_445 ? C1 Co1 C2 90.4(2) . 5_445 ? C2 Co1 C2 90.7(3) 16_545 5_445 ? C2 Co1 C2 89.3(3) 8_456 5_445 ? C1 Co1 C2 90.4(2) 9_556 13_556 ? C1 Co1 C2 89.6(2) . 13_556 ? C2 Co1 C2 89.3(3) 16_545 13_556 ? C2 Co1 C2 90.7(3) 8_456 13_556 ? C2 Co1 C2 180.0 5_445 13_556 ? C1 N1 Er1 149.8(6) . . ? N1 C1 Co1 179.9(6) . . ? C2 N2 Er1 167.0(4) . . ? N2 C2 Co1 178.5(4) . 5 ? Er1 O1 H1 127(4) . . ? H2 O2 H3 123(9) . . ? 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 H1 O2 0.98(5) 1.85(6) 2.793(6) 161(7) 5_545 O2 H2 N1 0.99(5) 2.14(5) 3.123(9) 176(9) 9_566 O2 H3 N2 0.99(5) 2.48(5) 3.324(7) 143.1(19) . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.93 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.178 _refine_diff_density_min -0.862 _refine_diff_density_rms 0.220 data_er300w _database_code_depnum_ccdc_archive 'CCDC 296844' _audit_creation_method SHELXL-97 _chemical_name_systematic ; erbium(III)-hexacyanocobaltate(III)tetrahydrate ; _chemical_name_common erbium(iii)-hexacyanocobaltate(iii)tetrahydrate _chemical_melting_point ? _chemical_formula_moiety 'C6 H4 Co Er N6 O2, 2(H2 O)' _chemical_formula_sum 'C6 H8 Co Er N6 O4' _chemical_formula_weight 454.37 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'C m c m' _symmetry_space_group_name_Hall '-C 2c 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 7.2765(10) _cell_length_b 12.6476(18) _cell_length_c 13.4804(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1240.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 991 _cell_measurement_theta_min 3.222 _cell_measurement_theta_max 27.828 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 8.071 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.215 _exptl_absorpt_correction_T_max 0.412 _exptl_absorpt_process_details 'SADABS, Sheldrick 1996' _exptl_special_details ; Mounted on a thin smear of grease in an open-ended glass capillary. ; _diffrn_ambient_temperature 300(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 80 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.01 _diffrn_reflns_number 4264 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.96 _reflns_number_total 836 _reflns_number_gt 785 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BrukerAXS, 1997)' _computing_cell_refinement 'SMART (BrukerAXS, 1997)' _computing_data_reduction 'SAINT+ (BrukerAXS, 1997)' _computing_structure_solution 'SHELXTL (BrukerAXS, 2000)' _computing_structure_refinement 'SHELXTL (BrukerAXS, 2000)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997), WebLab ViewerPro 3.7 (Accelrys, 2001)' _computing_publication_material XCIF _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^)+(0.0416P)^2^+6.5226P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 836 _refine_ls_number_parameters 58 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0311 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0735 _refine_ls_wR_factor_gt 0.0714 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.145 _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 Er1 Er 0.0000 0.32481(3) 0.7500 0.01232(15) Uani 1 4 d S . . Co1 Co 0.0000 0.0000 0.5000 0.0124(3) Uani 1 4 d S . . N1 N 0.0000 0.2160(5) 0.5997(5) 0.0237(12) Uani 1 2 d S . . C1 C 0.0000 0.1342(5) 0.5619(5) 0.0185(13) Uani 1 2 d S . . N2 N 0.2012(6) 0.4232(3) 0.6400(3) 0.0253(9) Uani 1 1 d . . . C2 C 0.3157(7) 0.4528(3) 0.5880(3) 0.0181(9) Uani 1 1 d . . . O1 O 0.2606(8) 0.2195(5) 0.7500 0.0342(13) Uani 1 2 d SD . . H1 H 0.338(10) 0.207(6) 0.694(5) 0.051 Uiso 1 1 d D . . O2 O 0.0000 0.6558(5) 0.5991(5) 0.0375(14) Uani 1 2 d SD . . H2 H 0.0000 0.693(8) 0.537(6) 0.056 Uiso 1 2 d SD . . H3 H 0.0000 0.581(5) 0.610(9) 0.056 Uiso 1 2 d SD . . 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 Er1 0.0103(2) 0.0132(2) 0.0134(2) 0.000 0.000 0.000 Co1 0.0111(5) 0.0113(5) 0.0148(6) 0.0000(4) 0.000 0.000 N1 0.029(3) 0.019(3) 0.024(3) -0.007(2) 0.000 0.000 C1 0.018(3) 0.020(3) 0.018(3) 0.001(3) 0.000 0.000 N2 0.019(2) 0.033(2) 0.024(2) 0.0043(17) 0.0032(17) -0.0058(17) C2 0.020(2) 0.016(2) 0.018(2) 0.0017(16) -0.0018(18) 0.0008(17) O1 0.029(3) 0.048(3) 0.026(3) 0.000 0.000 0.021(3) O2 0.040(4) 0.038(3) 0.034(3) 0.000(3) 0.000 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 Er1 O1 2.317(5) . ? Er1 O1 2.317(5) 3_556 ? Er1 N2 2.427(4) . ? Er1 N2 2.427(4) 10_557 ? Er1 N2 2.427(4) 12 ? Er1 N2 2.427(4) 3_556 ? Er1 N1 2.450(6) 10_557 ? Er1 N1 2.450(6) . ? Co1 C2 1.887(5) 16_545 ? Co1 C2 1.887(5) 8_456 ? Co1 C2 1.887(5) 13_556 ? Co1 C2 1.887(5) 5_445 ? Co1 C1 1.891(7) 9_556 ? Co1 C1 1.891(7) . ? N1 C1 1.153(9) . ? N2 C2 1.151(6) . ? C2 Co1 1.887(5) 5 ? O1 H1 0.95(5) . ? O2 H2 0.96(5) . ? O2 H3 0.96(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 Er1 O1 109.8(3) . 3_556 ? O1 Er1 N2 78.54(17) . . ? O1 Er1 N2 142.04(11) 3_556 . ? O1 Er1 N2 78.54(17) . 10_557 ? O1 Er1 N2 142.04(11) 3_556 10_557 ? N2 Er1 N2 75.3(2) . 10_557 ? O1 Er1 N2 142.04(11) . 12 ? O1 Er1 N2 78.54(17) 3_556 12 ? N2 Er1 N2 74.2(2) . 12 ? N2 Er1 N2 118.3(2) 10_557 12 ? O1 Er1 N2 142.04(11) . 3_556 ? O1 Er1 N2 78.54(17) 3_556 3_556 ? N2 Er1 N2 118.3(2) . 3_556 ? N2 Er1 N2 74.2(2) 10_557 3_556 ? N2 Er1 N2 75.3(2) 12 3_556 ? O1 Er1 N1 71.15(11) . 10_557 ? O1 Er1 N1 71.15(11) 3_556 10_557 ? N2 Er1 N1 142.51(11) . 10_557 ? N2 Er1 N1 77.47(16) 10_557 10_557 ? N2 Er1 N1 142.51(11) 12 10_557 ? N2 Er1 N1 77.47(16) 3_556 10_557 ? O1 Er1 N1 71.15(11) . . ? O1 Er1 N1 71.15(11) 3_556 . ? N2 Er1 N1 77.47(16) . . ? N2 Er1 N1 142.51(11) 10_557 . ? N2 Er1 N1 77.47(16) 12 . ? N2 Er1 N1 142.51(11) 3_556 . ? N1 Er1 N1 111.6(3) 10_557 . ? C2 Co1 C2 180.0(2) 16_545 8_456 ? C2 Co1 C2 89.4(3) 16_545 13_556 ? C2 Co1 C2 90.6(3) 8_456 13_556 ? C2 Co1 C2 90.6(3) 16_545 5_445 ? C2 Co1 C2 89.4(3) 8_456 5_445 ? C2 Co1 C2 180.0 13_556 5_445 ? C2 Co1 C1 89.6(2) 16_545 9_556 ? C2 Co1 C1 90.4(2) 8_456 9_556 ? C2 Co1 C1 90.4(2) 13_556 9_556 ? C2 Co1 C1 89.6(2) 5_445 9_556 ? C2 Co1 C1 90.4(2) 16_545 . ? C2 Co1 C1 89.6(2) 8_456 . ? C2 Co1 C1 89.6(2) 13_556 . ? C2 Co1 C1 90.4(2) 5_445 . ? C1 Co1 C1 180.0 9_556 . ? C1 N1 Er1 150.4(6) . . ? N1 C1 Co1 179.9(6) . . ? C2 N2 Er1 167.2(4) . . ? N2 C2 Co1 178.5(4) . 5 ? Er1 O1 H1 125(5) . . ? H2 O2 H3 128(10) . . ? 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 H1 O2 0.95(5) 1.86(5) 2.797(6) 168(7) 5_545 O2 H2 N1 0.96(5) 2.18(5) 3.132(9) 177(10) 9_566 O2 H3 N2 0.96(5) 2.51(5) 3.331(7) 144.2(10) . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.96 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.425 _refine_diff_density_min -0.791 _refine_diff_density_rms 0.205 data_er375w _database_code_depnum_ccdc_archive 'CCDC 296845' _audit_creation_method SHELXL-97 _chemical_name_systematic ; erbium(III)-hexacyanocobaltate(III)tetrahydrate ; _chemical_name_common erbium(iii)-hexacyanocobaltate(iii)tetrahydrate _chemical_melting_point ? _chemical_formula_moiety 'C6 H4 Co Er N6 O2, 2(H2 O)' _chemical_formula_sum 'C6 H8 Co Er N6 O4' _chemical_formula_weight 454.37 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'C m c m' _symmetry_space_group_name_Hall '-C 2c 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 7.275(3) _cell_length_b 12.687(5) _cell_length_c 13.487(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1244.8(8) _cell_formula_units_Z 4 _cell_measurement_temperature 375(2) _cell_measurement_reflns_used 653 _cell_measurement_theta_min 3.212 _cell_measurement_theta_max 27.688 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 8.044 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.199 _exptl_absorpt_correction_T_max 0.413 _exptl_absorpt_process_details 'SADABS, Sheldrick 1996' _exptl_special_details ; Mounted on a thin smear of grease in an open-ended glass capillary. ; _diffrn_ambient_temperature 375(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 48 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.08 _diffrn_reflns_number 4247 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 28.01 _reflns_number_total 839 _reflns_number_gt 767 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (BrukerAXS, 1997)' _computing_cell_refinement 'SMART (BrukerAXS, 1997)' _computing_data_reduction 'SAINT+ (BrukerAXS, 1997)' _computing_structure_solution 'SHELXTL (BrukerAXS, 2000)' _computing_structure_refinement 'SHELXTL (BrukerAXS, 2000)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997), WebLab ViewerPro 3.7 (Accelrys, 2001)' _computing_publication_material XCIF _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^)+(0.0582P)^2^+12.5501P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 839 _refine_ls_number_parameters 51 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1139 _refine_ls_wR_factor_gt 0.1079 _refine_ls_goodness_of_fit_ref 1.238 _refine_ls_restrained_S_all 1.236 _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 Er1 Er 0.0000 0.32460(4) 0.7500 0.0161(2) Uani 1 4 d S . . Co1 Co 0.0000 0.0000 0.5000 0.0165(4) Uani 1 4 d S . . N1 N 0.0000 0.2141(7) 0.6012(7) 0.030(2) Uani 1 2 d S . . C1 C 0.0000 0.1326(7) 0.5622(8) 0.0208(19) Uani 1 2 d S . . N2 N 0.2014(10) 0.4220(5) 0.6396(5) 0.0314(15) Uani 1 1 d . . . C2 C 0.3158(10) 0.4518(5) 0.5879(5) 0.0217(14) Uani 1 1 d . . . O1 O 0.2612(13) 0.2198(8) 0.7500 0.046(2) Uani 1 2 d SD . . H1 H 0.3487 0.2211 0.6950 0.069 Uiso 1 1 d D . . O2 O 0.0000 0.6546(7) 0.5974(8) 0.049(2) Uani 1 2 d SD . . H2 H 0.0000 0.6864 0.5311 0.074 Uiso 1 2 d SD . . H3 H 0.0000 0.5773 0.5935 0.074 Uiso 1 2 d SD . . 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 Er1 0.0154(3) 0.0160(3) 0.0170(3) 0.000 0.000 0.000 Co1 0.0169(9) 0.0144(8) 0.0183(9) 0.0008(6) 0.000 0.000 N1 0.037(5) 0.023(4) 0.031(5) -0.010(4) 0.000 0.000 C1 0.027(5) 0.014(4) 0.022(5) -0.003(4) 0.000 0.000 N2 0.034(4) 0.033(3) 0.028(3) 0.006(3) 0.002(3) -0.003(3) C2 0.021(3) 0.020(3) 0.024(4) 0.003(3) 0.000(3) -0.005(3) O1 0.041(5) 0.059(6) 0.038(5) 0.000 0.000 0.025(5) O2 0.047(6) 0.056(6) 0.044(6) -0.002(5) 0.000 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 Er1 O1 2.319(9) 3_556 ? Er1 O1 2.319(9) . ? Er1 N2 2.427(7) . ? Er1 N2 2.427(7) 10_557 ? Er1 N2 2.427(7) 12 ? Er1 N2 2.427(7) 3_556 ? Er1 N1 2.448(9) 10_557 ? Er1 N1 2.448(9) . ? Co1 C1 1.880(9) . ? Co1 C1 1.880(9) 9_556 ? Co1 C2 1.891(7) 16_545 ? Co1 C2 1.891(7) 8_456 ? Co1 C2 1.891(7) 5_445 ? Co1 C2 1.891(7) 13_556 ? N1 C1 1.160(14) . ? N2 C2 1.150(10) . ? C2 Co1 1.891(7) 5 ? O1 H1 0.9776 . ? O2 H2 0.9811 . ? O2 H3 0.9828 . ? 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 Er1 O1 110.0(6) 3_556 . ? O1 Er1 N2 141.86(17) 3_556 . ? O1 Er1 N2 78.3(3) . . ? O1 Er1 N2 141.86(17) 3_556 10_557 ? O1 Er1 N2 78.3(3) . 10_557 ? N2 Er1 N2 75.7(3) . 10_557 ? O1 Er1 N2 78.3(3) 3_556 12 ? O1 Er1 N2 141.86(17) . 12 ? N2 Er1 N2 74.3(3) . 12 ? N2 Er1 N2 118.8(3) 10_557 12 ? O1 Er1 N2 78.3(3) 3_556 3_556 ? O1 Er1 N2 141.86(17) . 3_556 ? N2 Er1 N2 118.8(3) . 3_556 ? N2 Er1 N2 74.3(3) 10_557 3_556 ? N2 Er1 N2 75.7(3) 12 3_556 ? O1 Er1 N1 70.83(19) 3_556 10_557 ? O1 Er1 N1 70.83(19) . 10_557 ? N2 Er1 N1 142.61(17) . 10_557 ? N2 Er1 N1 77.8(3) 10_557 10_557 ? N2 Er1 N1 142.61(17) 12 10_557 ? N2 Er1 N1 77.8(3) 3_556 10_557 ? O1 Er1 N1 70.83(19) 3_556 . ? O1 Er1 N1 70.83(18) . . ? N2 Er1 N1 77.8(3) . . ? N2 Er1 N1 142.61(17) 10_557 . ? N2 Er1 N1 77.8(3) 12 . ? N2 Er1 N1 142.61(18) 3_556 . ? N1 Er1 N1 110.1(5) 10_557 . ? C1 Co1 C1 179.998(1) . 9_556 ? C1 Co1 C2 90.5(3) . 16_545 ? C1 Co1 C2 89.5(3) 9_556 16_545 ? C1 Co1 C2 89.5(3) . 8_456 ? C1 Co1 C2 90.5(3) 9_556 8_456 ? C2 Co1 C2 180.000(1) 16_545 8_456 ? C1 Co1 C2 90.5(3) . 5_445 ? C1 Co1 C2 89.5(3) 9_556 5_445 ? C2 Co1 C2 90.3(4) 16_545 5_445 ? C2 Co1 C2 89.7(4) 8_456 5_445 ? C1 Co1 C2 89.5(3) . 13_556 ? C1 Co1 C2 90.5(3) 9_556 13_556 ? C2 Co1 C2 89.7(4) 16_545 13_556 ? C2 Co1 C2 90.3(4) 8_456 13_556 ? C2 Co1 C2 180.000(1) 5_445 13_556 ? C1 N1 Er1 151.9(9) . . ? N1 C1 Co1 179.5(10) . . ? C2 N2 Er1 167.6(6) . . ? N2 C2 Co1 178.5(7) . 5 ? Er1 O1 H1 121.6 . . ? H2 O2 H3 111.2 . . ? 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 O1 H1 O2 0.98 1.91 2.817(10) 152.8 5_545 O2 H2 N1 0.98 2.19 3.154(14) 168.9 9_566 O2 H3 N2 0.98 2.53 3.344(10) 139.8 . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.01 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.535 _refine_diff_density_min -1.418 _refine_diff_density_rms 0.296