#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2205204.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2205204 loop_ _publ_author_name 'Ilyukhin, Andrey B.' 'Kotov, Vitalii Yu.' _publ_section_title ; Dipotassium sodium hexacyanocobalt(III) ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first i26 _journal_page_last i27 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac 'K2 Na [Co (C N)6]' _chemical_formula_structural 'K2 Na [Co (C N)6]' _chemical_formula_sum 'C6 Co K2 N6 Na' _chemical_formula_weight 316.24 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 90 _cell_angle_beta 90.665(12) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 7.0276(7) _cell_length_b 7.5566(6) _cell_length_c 10.2883(8) _cell_measurement_reflns_used 24 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 14.9 _cell_measurement_theta_min 13.7 _cell_volume 546.32(8) _computing_cell_refinement 'CAD-4 EXPRESS' _computing_data_collection 'CAD-4 EXPRESS (Enraf--Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf--Nonius CAD-4' _diffrn_measurement_method 'non-profiled \w/2\q' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -2 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -3 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 3025 _diffrn_reflns_theta_full 29.97 _diffrn_reflns_theta_max 29.97 _diffrn_reflns_theta_min 3.35 _diffrn_standards_decay_% 3 _diffrn_standards_interval_time 120 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 2.348 _exptl_absorpt_correction_T_max 0.625 _exptl_absorpt_correction_T_min 0.534 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.922 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 308 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.439 _refine_diff_density_min -0.369 _refine_ls_extinction_coef 0.0093(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_matrix_type full _refine_ls_number_parameters 77 _refine_ls_number_reflns 1598 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.998 _refine_ls_R_factor_gt 0.0193 _refine_ls_shift/su_max 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.03P)^2^+0.2P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.0555 _reflns_number_gt 1461 _reflns_number_total 1598 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file br6179.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_database_code 2205204 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Co1 0 0.5 0.5 0.01692(8) Uani d S 1 Co K1 0.02605(5) 0.07903(4) 0.24778(3) 0.03779(10) Uani d . 1 K Na1 0 0.5 0 0.02363(15) Uani d S 1 Na N1 0.35585(18) 0.28980(17) 0.43703(13) 0.0380(3) Uani d . 1 N N2 0.20696(18) 0.83718(16) 0.42294(13) 0.0359(3) Uani d . 1 N N3 0.13619(19) 0.54771(18) 0.77915(11) 0.0345(2) Uani d . 1 N C1 0.22183(17) 0.36863(15) 0.46199(11) 0.0229(2) Uani d . 1 C C2 0.12688(16) 0.71142(15) 0.45273(11) 0.0226(2) Uani d . 1 C C3 0.08538(17) 0.52756(15) 0.67371(12) 0.0233(2) Uani d . 1 C loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co1 0.01640(12) 0.01479(11) 0.01958(11) 0.00040(6) 0.00015(7) 0.00050(6) K1 0.03516(17) 0.02944(16) 0.04877(18) 0.00337(11) 0.00082(13) -0.00071(12) Na1 0.0237(4) 0.0212(3) 0.0260(3) -0.0006(2) -0.0006(3) 0.0009(2) N1 0.0326(6) 0.0315(6) 0.0501(7) 0.0119(5) 0.0080(5) 0.0064(5) N2 0.0330(6) 0.0283(5) 0.0463(6) -0.0079(5) -0.0046(5) 0.0063(5) N3 0.0374(6) 0.0410(6) 0.0250(5) 0.0022(5) -0.0014(4) -0.0015(5) C1 0.0240(5) 0.0188(5) 0.0258(5) 0.0004(4) 0.0004(4) 0.0025(4) C2 0.0209(5) 0.0208(5) 0.0262(5) 0.0003(4) -0.0015(4) 0.0006(4) C3 0.0224(5) 0.0213(5) 0.0262(5) 0.0016(4) 0.0018(4) 0.0006(4) 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 1 7 0 -5 1 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C3 Co1 C3 3_566 . 180 n C3 Co1 C1 3_566 3_566 90.00(5) n C3 Co1 C1 . 3_566 90.00(5) n C3 Co1 C1 3_566 . 90.00(5) n C3 Co1 C1 . . 90.00(5) n C1 Co1 C1 3_566 . 180 n C3 Co1 C2 3_566 . 89.74(5) n C3 Co1 C2 . . 90.26(5) n C1 Co1 C2 3_566 . 90.11(5) n C1 Co1 C2 . . 89.89(5) n C3 Co1 C2 3_566 3_566 90.26(5) n C3 Co1 C2 . 3_566 89.74(5) n C1 Co1 C2 3_566 3_566 89.89(5) n C1 Co1 C2 . 3_566 90.11(5) n C2 Co1 C2 . 3_566 180 n N2 K1 N3 1_545 4_565 97.56(4) n N2 K1 N1 1_545 2_545 79.07(4) n N3 K1 N1 4_565 2_545 95.58(4) n N2 K1 N3 1_545 3_566 144.25(4) n N3 K1 N3 4_565 3_566 87.89(2) n N1 K1 N3 2_545 3_566 135.77(4) n N2 K1 C3 1_545 3_566 123.17(4) n N3 K1 C3 4_565 3_566 92.54(4) n N1 K1 C3 2_545 3_566 155.05(4) n N3 K1 C3 3_566 3_566 21.10(3) n N2 K1 C1 1_545 2_545 82.12(4) n N3 K1 C1 4_565 2_545 115.78(4) n N1 K1 C1 2_545 2_545 20.80(3) n N3 K1 C1 3_566 2_545 126.99(3) n C3 K1 C1 3_566 2_545 140.26(3) n N2 K1 N2 1_545 2_545 118.12(2) n N3 K1 N2 4_565 2_545 143.78(3) n N1 K1 N2 2_545 2_545 85.94(3) n N3 K1 N2 3_566 2_545 67.20(3) n C3 K1 N2 3_566 2_545 73.78(3) n C1 K1 N2 2_545 2_545 66.92(3) n N2 K1 C3 1_545 4_565 113.68(3) n N3 K1 C3 4_565 4_565 20.29(3) n N1 K1 C3 2_545 4_565 86.66(3) n N3 K1 C3 3_566 4_565 81.68(3) n C3 K1 C3 3_566 4_565 93.09(2) n C1 K1 C3 2_545 4_565 104.35(3) n N2 K1 C3 2_545 4_565 124.97(3) n N2 K1 C2 1_545 2_545 104.87(3) n N3 K1 C2 4_565 2_545 148.42(3) n N1 K1 C2 2_545 2_545 67.83(3) n N3 K1 C2 3_566 2_545 86.69(3) n C3 K1 C2 3_566 2_545 93.45(3) n C1 K1 C2 2_545 2_545 47.85(3) n N2 K1 C2 2_545 2_545 19.90(3) n C3 K1 C2 4_565 2_545 128.28(3) n N2 K1 C1 1_545 . 80.11(3) n N3 K1 C1 4_565 . 120.93(3) n N1 K1 C1 2_545 . 139.90(3) n N3 K1 C1 3_566 . 67.08(3) n C3 K1 C1 3_566 . 47.95(3) n C1 K1 C1 2_545 . 122.109(19) n N2 K1 C1 2_545 . 74.34(3) n C3 K1 C1 4_565 . 133.24(3) n C2 K1 C1 2_545 . 85.12(3) n N2 K1 N1 1_545 . 69.10(3) n N3 K1 N1 4_565 . 136.27(3) n N1 K1 N1 2_545 . 120.56(2) n N3 K1 N1 3_566 . 82.57(3) n C3 K1 N1 3_566 . 65.52(3) n C1 K1 N1 2_545 . 103.74(3) n N2 K1 N1 2_545 . 68.50(3) n C3 K1 N1 4_565 . 151.88(3) n C2 K1 N1 2_545 . 73.63(3) n C1 K1 N1 . . 19.43(3) n N2 K1 Na1 1_545 . 155.52(3) n N3 K1 Na1 4_565 . 106.80(3) n N1 K1 Na1 2_545 . 100.46(3) n N3 K1 Na1 3_566 . 37.72(2) n C3 K1 Na1 3_566 . 54.58(2) n C1 K1 Na1 2_545 . 89.27(2) n N2 K1 Na1 2_545 . 38.13(2) n C3 K1 Na1 4_565 . 90.63(2) n C2 K1 Na1 2_545 . 54.03(2) n C1 K1 Na1 . . 85.28(2) n N1 K1 Na1 . . 91.02(2) n N1 Na1 N1 2 4_565 180.00(6) n N1 Na1 N3 2 1_554 87.19(4) n N1 Na1 N3 4_565 1_554 92.81(4) n N1 Na1 N3 2 3_566 92.81(4) n N1 Na1 N3 4_565 3_566 87.19(4) n N3 Na1 N3 1_554 3_566 180 n N1 Na1 N2 2 4_575 88.91(4) n N1 Na1 N2 4_565 4_575 91.09(4) n N3 Na1 N2 1_554 4_575 87.92(4) n N3 Na1 N2 3_566 4_575 92.08(4) n N1 Na1 N2 2 2_545 91.09(4) n N1 Na1 N2 4_565 2_545 88.91(4) n N3 Na1 N2 1_554 2_545 92.08(4) n N3 Na1 N2 3_566 2_545 87.92(4) n N2 Na1 N2 4_575 2_545 180.00(5) n N1 Na1 K1 2 3_565 59.54(3) n N1 Na1 K1 4_565 3_565 120.46(3) n N3 Na1 K1 1_554 3_565 48.31(3) n N3 Na1 K1 3_566 3_565 131.69(3) n N2 Na1 K1 4_575 3_565 52.54(3) n N2 Na1 K1 2_545 3_565 127.46(3) n N1 Na1 K1 2 . 120.46(3) n N1 Na1 K1 4_565 . 59.54(3) n N3 Na1 K1 1_554 . 131.69(3) n N3 Na1 K1 3_566 . 48.31(3) n N2 Na1 K1 4_575 . 127.46(3) n N2 Na1 K1 2_545 . 52.54(3) n K1 Na1 K1 3_565 . 180.000(6) n N1 Na1 K1 2 2 53.41(3) n N1 Na1 K1 4_565 2 126.59(3) n N3 Na1 K1 1_554 2 103.26(3) n N3 Na1 K1 3_566 2 76.74(3) n N2 Na1 K1 4_575 2 139.22(3) n N2 Na1 K1 2_545 2 40.78(3) n K1 Na1 K1 3_565 2 107.566(8) n K1 Na1 K1 . 2 72.434(7) n N1 Na1 K1 2 4_565 126.59(3) n N1 Na1 K1 4_565 4_565 53.41(3) n N3 Na1 K1 1_554 4_565 76.74(3) n N3 Na1 K1 3_566 4_565 103.26(3) n N2 Na1 K1 4_575 4_565 40.78(3) n N2 Na1 K1 2_545 4_565 139.22(3) n K1 Na1 K1 3_565 4_565 72.434(7) n K1 Na1 K1 . 4_565 107.566(7) n K1 Na1 K1 2 4_565 180.000(9) n N1 Na1 K1 2 2_455 93.81(3) n N1 Na1 K1 4_565 2_455 86.19(3) n N3 Na1 K1 1_554 2_455 144.64(3) n N3 Na1 K1 3_566 2_455 35.36(3) n N2 Na1 K1 4_575 2_455 56.80(3) n N2 Na1 K1 2_545 2_455 123.20(3) n K1 Na1 K1 3_565 2_455 102.809(8) n K1 Na1 K1 . 2_455 77.191(8) n K1 Na1 K1 2 2_455 105.565(10) n K1 Na1 K1 4_565 2_455 74.435(10) n N1 Na1 K1 2 4_665 86.19(3) n N1 Na1 K1 4_565 4_665 93.81(3) n N3 Na1 K1 1_554 4_665 35.36(3) n N3 Na1 K1 3_566 4_665 144.64(3) n N2 Na1 K1 4_575 4_665 123.20(3) n N2 Na1 K1 2_545 4_665 56.80(3) n K1 Na1 K1 3_565 4_665 77.191(8) n K1 Na1 K1 . 4_665 102.809(8) n K1 Na1 K1 2 4_665 74.435(10) n K1 Na1 K1 4_565 4_665 105.565(10) n K1 Na1 K1 2_455 4_665 180 n C1 N1 Na1 . 2_545 136.90(10) n C1 N1 K1 . 2 89.86(9) n Na1 N1 K1 2_545 2 133.24(5) n C1 N1 K1 . . 79.37(9) n Na1 N1 K1 2_545 . 90.55(4) n K1 N1 K1 2 . 99.72(4) n C2 N2 Na1 . 2 136.20(10) n C2 N2 K1 . 1_565 118.84(10) n Na1 N2 K1 2 1_565 104.03(4) n C2 N2 K1 . 2 86.28(9) n Na1 N2 K1 2 2 89.33(4) n K1 N2 K1 1_565 2 107.45(4) n C3 N3 Na1 . 1_556 136.13(11) n C3 N3 K1 . 4_666 97.69(9) n Na1 N3 K1 1_556 4_666 114.96(4) n C3 N3 K1 . 3_566 85.70(9) n Na1 N3 K1 1_556 3_566 93.96(4) n K1 N3 K1 4_666 3_566 129.93(5) n N1 C1 Co1 . . 178.96(11) n N1 C1 K1 . 2 69.34(8) n Co1 C1 K1 . 2 109.86(5) n N1 C1 K1 . . 81.20(9) n Co1 C1 K1 . . 98.28(4) n K1 C1 K1 2 . 96.04(3) n N2 C2 Co1 . . 178.45(12) n N2 C2 K1 . 2 73.82(9) n Co1 C2 K1 . 2 104.66(4) n N3 C3 Co1 . . 178.66(12) n N3 C3 K1 . 3_566 73.20(9) n Co1 C3 K1 . 3_566 105.47(5) n N3 C3 K1 . 4_666 62.02(9) n Co1 C3 K1 . 4_666 118.75(5) n K1 C3 K1 3_566 4_666 113.89(4) n loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co1 C3 3_566 1.8901(12) n Co1 C3 . 1.8901(12) y Co1 C1 3_566 1.8928(12) n Co1 C1 . 1.8928(12) y Co1 C2 . 1.8958(12) y Co1 C2 3_566 1.8958(12) n K1 N2 1_545 2.8549(13) n K1 N3 4_565 2.9237(14) n K1 N1 2_545 3.0195(13) n K1 N3 3_566 3.0537(14) n K1 C3 3_566 3.1809(12) n K1 C1 2_545 3.2270(12) n K1 N2 2_545 3.2384(14) n K1 C3 4_565 3.2810(13) n K1 C2 2_545 3.3649(13) n K1 C1 . 3.3866(12) n K1 N1 . 3.4051(15) n K1 Na1 . 4.0793(4) n Na1 N1 2 2.4953(12) y Na1 N1 4_565 2.4953(12) n Na1 N3 1_554 2.5019(12) y Na1 N3 3_566 2.5019(12) n Na1 N2 4_575 2.5190(12) n Na1 N2 2_545 2.5190(12) y Na1 K1 3_565 4.0793(4) n Na1 K1 2 4.2407(6) n Na1 K1 4_565 4.2407(6) n Na1 K1 2_455 4.5804(6) n Na1 K1 4_665 4.5804(6) n N1 C1 . 1.1461(17) y N1 Na1 2_545 2.4953(12) n N1 K1 2 3.0195(13) n N2 C2 . 1.1479(17) y N2 Na1 2 2.5190(12) n N2 K1 1_565 2.8549(13) n N2 K1 2 3.2384(14) n N3 C3 . 1.1482(17) y N3 Na1 1_556 2.5019(12) n N3 K1 4_666 2.9237(14) n N3 K1 3_566 3.0537(14) n C1 K1 2 3.2270(12) n C2 K1 2 3.3649(13) n C3 K1 3_566 3.1809(12) n C3 K1 4_666 3.2810(13) n