#------------------------------------------------------------------------------ #$Date: 2014-03-15 13:45:36 +0200 (Sat, 15 Mar 2014) $ #$Revision: 106525 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/10/18/7101818.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7101818 loop_ _publ_author_name 'Mukhopadhyay, Uday' 'Grunert, C Matthias' 'Kusz, Joachim' 'Reiman, Sergey' 'G\"utlich, P' 'Bernal, Ivan' _publ_section_title ; 57Fe M\"ossbauer spectroscopy predicts superstructure for K0.08[Cu(II)(N,N'app)Cl]2[Fe(III)(CN)6].0.92H3O.3H2O. ; _journal_issue 14 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 1444 _journal_page_last 1446 _journal_year 2007 _chemical_formula_sum 'C26 H63.84 Cl2 Cu2 Fe K0.08 N14 O3.92' _chemical_formula_weight 892.43 _chemical_name_systematic ; ? ; _space_group_IT_number 12 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-I 2y' _symmetry_space_group_name_H-M 'I 1 2/m 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 103.930(16) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 9.8104(12) _cell_length_b 13.967(3) _cell_length_c 14.6291(16) _cell_measurement_reflns_used 7572 _cell_measurement_temperature 90(2) _cell_measurement_theta_max 32.64 _cell_measurement_theta_min 4.08 _cell_volume 1945.6(5) _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) ; _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET) (compiled Jan 20 2006,12:36:28) ; _computing_molecular_graphics 'PLATON (Spek,2003)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 90(2) _diffrn_detector_area_resol_mean 16.0328 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.927 _diffrn_measurement_device_type KM4_CCD_Sapphire3 _diffrn_measurement_method \q-scan _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_sigmaI/netI 0.0243 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 9683 _diffrn_reflns_theta_full 30.00 _diffrn_reflns_theta_max 32.65 _diffrn_reflns_theta_min 4.08 _exptl_absorpt_coefficient_mu 1.648 _exptl_absorpt_correction_type none _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_description polyhedron _exptl_crystal_F_000 937 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _refine_diff_density_max 1.681 _refine_diff_density_min -2.501 _refine_diff_density_rms 0.160 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 123 _refine_ls_number_reflns 3415 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.142 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0606 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0999P)^2^+9.0157P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1758 _refine_ls_wR_factor_ref 0.1790 _reflns_number_gt 3109 _reflns_number_total 3415 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file b615130b.txt _[local]_cod_data_source_block ber6_90 _[local]_cod_cif_authors_sg_H-M 'I 2/m' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' 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 Cu2 Cu 0.49790(4) 0.5000 1.18656(3) 0.01202(14) Uani 1 2 d S . . Cl2 Cl 0.31288(15) 0.5000 1.04096(10) 0.0391(3) Uani 1 2 d S . . N1 N 0.4113(3) 0.4120(2) 1.2697(2) 0.0327(7) Uani 1 1 d . . . N2 N 0.6202(3) 0.3991(2) 1.1494(2) 0.0319(6) Uani 1 1 d . . . H1N H 0.6287 0.4131 1.0896 0.038 Uiso 1 1 calc R . . H2N H 0.7083 0.4044 1.1889 0.038 Uiso 1 1 calc R . . C1 C 0.5752(4) 0.2975(3) 1.1503(5) 0.070(2) Uani 1 1 d . . . H11 H 0.6482 0.2557 1.1350 0.084 Uiso 1 1 calc R . . H21 H 0.4874 0.2881 1.1010 0.084 Uiso 1 1 calc R . . C2 C 0.5512(5) 0.2686(3) 1.2439(6) 0.076(2) Uani 1 1 d . . . H12 H 0.5509 0.1979 1.2479 0.092 Uiso 1 1 calc R . . H22 H 0.6300 0.2925 1.2945 0.092 Uiso 1 1 calc R . . C3 C 0.4153(4) 0.3065(4) 1.2602(5) 0.0671(19) Uani 1 1 d . . . H13 H 0.3375 0.2865 1.2069 0.081 Uiso 1 1 calc R . . H23 H 0.3989 0.2769 1.3181 0.081 Uiso 1 1 calc R . . C4 C 0.2633(3) 0.4452(4) 1.2564(2) 0.0409(10) Uani 1 1 d . . . H14 H 0.2236 0.4209 1.3081 0.049 Uiso 1 1 calc R . . H24 H 0.2051 0.4209 1.1960 0.049 Uiso 1 1 calc R . . C8 C 0.4910(4) 0.4451(4) 1.3639(2) 0.0543(14) Uani 1 1 d . . . H18 H 0.5886 0.4208 1.3771 0.065 Uiso 1 1 calc R . . H28 H 0.4463 0.4208 1.4132 0.065 Uiso 1 1 calc R . . Fe1 Fe 0.0000 0.5000 0.5000 0.01186(16) Uani 1 4 d S . . N3 N -0.2153(3) 0.65641(19) 0.52200(18) 0.0235(5) Uani 1 1 d . . . N4 N 0.1332(4) 0.5000 0.7153(2) 0.0257(7) Uani 1 2 d S . . C5 C -0.1340(3) 0.59828(18) 0.51425(17) 0.0165(4) Uani 1 1 d . . . C6 C 0.0822(4) 0.5000 0.6350(2) 0.0174(6) Uani 1 2 d S . . OW1 O 0.3439(10) 0.1661(5) 1.4772(7) 0.148(4) Uani 0.92 1 d P A 1 K1 K 0.4078(15) 0.1821(12) 1.4856(10) 0.044(3) Uiso 0.08 1 d P . 2 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 Cu2 0.0106(2) 0.0142(2) 0.0112(2) 0.000 0.00251(14) 0.000 Cl2 0.0372(6) 0.0460(7) 0.0361(6) 0.000 0.0128(5) 0.000 N1 0.0153(10) 0.0519(18) 0.0269(12) 0.0243(12) -0.0028(9) -0.0090(11) N2 0.0153(10) 0.0397(15) 0.0369(14) -0.0221(12) -0.0012(9) 0.0068(10) C1 0.0228(16) 0.0329(19) 0.131(5) -0.050(3) -0.027(2) 0.0128(15) C2 0.036(2) 0.0218(17) 0.142(6) 0.026(3) -0.034(3) -0.0056(15) C3 0.0288(17) 0.047(2) 0.106(4) 0.054(3) -0.022(2) -0.0202(17) C4 0.0145(11) 0.087(3) 0.0206(12) 0.0196(16) 0.0026(9) -0.0102(15) C8 0.0204(13) 0.118(4) 0.0193(13) 0.0286(19) -0.0043(11) -0.0135(19) Fe1 0.0124(3) 0.0119(3) 0.0097(3) 0.000 -0.0003(2) 0.000 N3 0.0240(11) 0.0224(11) 0.0227(10) -0.0024(9) 0.0028(9) 0.0039(9) N4 0.0256(16) 0.0316(18) 0.0160(14) 0.000 -0.0023(12) 0.000 C5 0.0173(10) 0.0166(10) 0.0142(9) -0.0007(8) 0.0014(8) -0.0005(8) C6 0.0180(15) 0.0174(14) 0.0150(14) 0.000 0.0008(11) 0.000 OW1 0.141(7) 0.060(4) 0.201(9) -0.048(5) -0.041(6) 0.060(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cu2 N2 2.008(3) 6_565 Cu2 N2 2.008(3) . Cu2 N1 2.052(3) . Cu2 N1 2.052(2) 6_565 Cu2 Cl2 2.4434(16) . Cl2 K1 3.302(15) 4_557 Cl2 K1 3.302(15) 7_557 N1 C3 1.483(7) . N1 C8 1.484(5) . N1 C4 1.492(5) . N2 C1 1.487(6) . C1 C2 1.500(10) . C2 C3 1.506(9) . C4 C4 1.530(10) 6_565 C8 C8 1.534(12) 6_565 Fe1 C6 1.946(3) . Fe1 C6 1.946(3) 5_566 Fe1 C5 1.947(3) . Fe1 C5 1.947(3) 2_556 Fe1 C5 1.947(3) 6_565 Fe1 C5 1.947(3) 5_566 N3 C5 1.162(4) . N3 K1 2.927(16) 5_567 N4 C6 1.160(5) . K1 K1 1.76(3) 2_658 K1 N3 2.927(16) 5_567 K1 Cl2 3.302(15) 7_557 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 N2 Cu2 N2 89.1(2) 6_565 . N2 Cu2 N1 160.09(13) 6_565 . N2 Cu2 N1 95.75(15) . . N2 Cu2 N1 95.75(15) 6_565 6_565 N2 Cu2 N1 160.09(13) . 6_565 N1 Cu2 N1 73.6(2) . 6_565 N2 Cu2 Cl2 97.51(8) 6_565 . N2 Cu2 Cl2 97.51(8) . . N1 Cu2 Cl2 100.97(8) . . N1 Cu2 Cl2 100.97(8) 6_565 . Cu2 Cl2 K1 115.5(3) . 4_557 Cu2 Cl2 K1 115.5(3) . 7_557 K1 Cl2 K1 100.8(6) 4_557 7_557 C3 N1 C8 112.2(3) . . C3 N1 C4 110.1(3) . . C8 N1 C4 107.6(3) . . C3 N1 Cu2 121.0(3) . . C8 N1 Cu2 99.4(2) . . C4 N1 Cu2 105.4(2) . . C1 N2 Cu2 118.0(3) . . N2 C1 C2 112.1(4) . . C3 C2 C1 112.9(4) . . N1 C3 C2 114.1(3) . . N1 C4 C4 108.1(2) . 6_565 N1 C8 C8 108.1(2) . 6_565 C6 Fe1 C6 180.0 . 5_566 C6 Fe1 C5 90.96(11) . . C6 Fe1 C5 89.04(11) 5_566 . C6 Fe1 C5 89.04(11) . 2_556 C6 Fe1 C5 90.96(11) 5_566 2_556 C5 Fe1 C5 90.31(15) . 2_556 C6 Fe1 C5 90.96(11) . 6_565 C6 Fe1 C5 89.04(11) 5_566 6_565 C5 Fe1 C5 89.69(15) . 6_565 C5 Fe1 C5 180.0 2_556 6_565 C6 Fe1 C5 89.04(11) . 5_566 C6 Fe1 C5 90.96(11) 5_566 5_566 C5 Fe1 C5 179.998(1) . 5_566 C5 Fe1 C5 89.69(15) 2_556 5_566 C5 Fe1 C5 90.31(15) 6_565 5_566 C5 N3 K1 170.4(4) . 5_567 N3 C5 Fe1 179.2(2) . . N4 C6 Fe1 179.0(4) . . K1 K1 N3 128.8(3) 2_658 5_567 K1 K1 Cl2 129.5(3) 2_658 7_557 N3 K1 Cl2 101.0(4) 5_567 7_557 _cod_database_code 7101818 _journal_paper_doi 10.1039/b615130b