#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:02:50 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180120 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/18/7101816.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_7101816
loop_
_publ_author_name
'Mukhopadhyay, Uday'
'Grunert, C Matthias'
'Kusz, Joachim'
'Reiman, Sergey'
'Gütlich, P'
'Bernal, Ivan'
_publ_section_title
;
 57Fe Mössbauer 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_paper_doi               10.1039/b615130b
_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                 104.17(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.786(2)
_cell_length_b                   13.998(5)
_cell_length_c                   14.643(2)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      8
_cell_volume                     1944.8(8)
_computing_cell_refinement       'KM4 KUMA Diffraction'
_computing_data_collection       'KM4 KUMA Diffraction'
_computing_data_reduction        'Omnibus-BLP (E.Galdecka,2002)'
_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      200(2)
_diffrn_detector_area_resol_mean 'point detector'
_diffrn_measured_fraction_theta_full 0.882
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_device_type  'KM4 KUMA Diffraction'
_diffrn_measurement_method       'profile data from θ/2θ 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  0.0223
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1661
_diffrn_reflns_theta_full        24.95
_diffrn_reflns_theta_max         24.95
_diffrn_reflns_theta_min         2.04
_diffrn_standards_interval_count 60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.649
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             937
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.689
_refine_diff_density_min         -1.140
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         1589
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0426P)²+21.6022P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1247
_refine_ls_wR_factor_ref         0.1408
_reflns_number_gt                1307
_reflns_number_total             1589
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b615130b.txt
_cod_data_source_block           ber6_200
_cod_original_sg_symbol_H-M      'I 2/m'
_cod_database_code               7101816
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 0.49712(9) 0.5000 1.18598(6) 0.0226(3) Uani 1 2 d S . .
Cl2 Cl 0.3124(3) 0.5000 1.0406(2) 0.0630(8) Uani 1 2 d S . .
N1 N 0.4110(5) 0.4125(4) 1.2685(4) 0.0386(13) Uani 1 1 d . . .
N2 N 0.6188(5) 0.3996(4) 1.1485(4) 0.0363(13) Uani 1 1 d . . .
H1N H 0.6276 0.4142 1.0890 0.044 Uiso 1 1 calc R . .
H2N H 0.7072 0.4045 1.1884 0.044 Uiso 1 1 calc R . .
C1 C 0.5746(8) 0.2988(5) 1.1481(6) 0.058(2) Uani 1 1 d . . .
H11 H 0.6479 0.2576 1.1325 0.070 Uiso 1 1 calc R . .
H21 H 0.4863 0.2896 1.0986 0.070 Uiso 1 1 calc R . .
C2 C 0.5515(8) 0.2698(5) 1.2402(7) 0.071(3) Uani 1 1 d . . .
H12 H 0.6316 0.2929 1.2906 0.085 Uiso 1 1 calc R . .
H22 H 0.5511 0.1991 1.2434 0.085 Uiso 1 1 calc R . .
C3 C 0.4154(8) 0.3071(5) 1.2592(6) 0.062(2) Uani 1 1 d . . .
H13 H 0.3356 0.2867 1.2072 0.075 Uiso 1 1 calc R A 2
H23 H 0.4023 0.2776 1.3180 0.075 Uiso 1 1 calc R A 2
C4 C 0.2639(7) 0.4451(6) 1.2558(5) 0.0474(18) Uani 1 1 d . . .
H14 H 0.2249 0.4208 1.3077 0.057 Uiso 1 1 calc R . .
H24 H 0.2048 0.4208 1.1955 0.057 Uiso 1 1 calc R . .
C8 C 0.4926(7) 0.4455(6) 1.3629(4) 0.059(2) Uani 1 1 d . . .
H18 H 0.5905 0.4212 1.3757 0.071 Uiso 1 1 calc R . .
H28 H 0.4487 0.4212 1.4124 0.071 Uiso 1 1 calc R . .
Fe1 Fe 0.0000 0.5000 0.5000 0.0206(4) Uani 1 4 d S . .
N3 N -0.2142(5) 0.6551(4) 0.5221(4) 0.0367(12) Uani 1 1 d . . .
N4 N 0.1358(8) 0.5000 0.7143(5) 0.044(2) Uani 1 2 d S . .
C5 C -0.1338(6) 0.5980(4) 0.5148(4) 0.0273(13) Uani 1 1 d . . .
C6 C 0.0838(8) 0.5000 0.6351(6) 0.0272(18) Uani 1 2 d S . .
O1W O 0.3490(14) 0.1668(7) 1.4893(10) 0.133(5) Uani 0.92 1 d P B 1
K1 K 0.399(4) 0.188(3) 1.473(3) 0.080(11) Uiso 0.08 1 d P . 2
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_
_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(3) 6_565 .
N2 Cu2 N1 160.4(2) 6_565 .
N2 Cu2 N1 95.8(2) . .
N2 Cu2 N1 95.8(2) 6_565 6_565
N2 Cu2 N1 160.4(2) . 6_565
N1 Cu2 N1 73.7(3) . 6_565
N2 Cu2 Cl2 97.16(16) 6_565 .
N2 Cu2 Cl2 97.16(16) . .
N1 Cu2 Cl2 101.07(15) . .
N1 Cu2 Cl2 101.07(15) 6_565 .
Cu2 Cl2 K1 111.8(8) . 7_557
Cu2 Cl2 K1 111.8(8) . 4_557
K1 Cl2 K1 104.8(17) 7_557 4_557
C4 N1 C3 110.1(5) . .
C4 N1 C8 107.8(5) . .
C3 N1 C8 111.8(6) . .
C4 N1 Cu2 105.7(4) . .
C3 N1 Cu2 121.1(5) . .
C8 N1 Cu2 99.1(4) . .
C1 N2 Cu2 118.6(4) . .
N2 C1 C2 111.7(6) . .
C1 C2 C3 114.2(6) . .
N1 C3 C2 113.9(6) . .
N1 C3 K1 111.9(9) . .
C2 C3 K1 103.3(9) . .
N1 C4 C4 108.0(4) . 6_565
N1 C8 C8 108.0(4) . 6_565
C5 Fe1 C5 179.998(1) . 5_566
C5 Fe1 C5 90.3(3) . 2_556
C5 Fe1 C5 89.7(3) 5_566 2_556
C5 Fe1 C5 89.7(3) . 6_565
C5 Fe1 C5 90.3(3) 5_566 6_565
C5 Fe1 C5 179.999(1) 2_556 6_565
C5 Fe1 C6 89.1(2) . 5_566
C5 Fe1 C6 90.9(2) 5_566 5_566
C5 Fe1 C6 90.9(2) 2_556 5_566
C5 Fe1 C6 89.1(2) 6_565 5_566
C5 Fe1 C6 90.9(2) . .
C5 Fe1 C6 89.1(2) 5_566 .
C5 Fe1 C6 89.1(2) 2_556 .
C5 Fe1 C6 90.9(2) 6_565 .
C6 Fe1 C6 179.998(2) 5_566 .
C5 N3 K1 173.0(9) . 5_567
N3 C5 Fe1 178.8(5) . .
N4 C6 Fe1 178.7(8) . .
K1 K1 N3 125.4(14) 2_658 5_567
K1 K1 Cl2 125.6(10) 2_658 7_557
N3 K1 Cl2 102.8(12) 5_567 7_557
K1 K1 C3 95(2) 2_658 .
N3 K1 C3 80.1(11) 5_567 .
Cl2 K1 C3 118.3(13) 7_557 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu2 N2 2.003(5) 6_565
Cu2 N2 2.003(5) .
Cu2 N1 2.041(5) .
Cu2 N1 2.041(5) 6_565
Cu2 Cl2 2.432(3) .
Cl2 K1 3.32(4) 7_557
Cl2 K1 3.32(4) 4_557
N1 C4 1.478(8) .
N1 C3 1.484(10) .
N1 C8 1.489(8) .
N2 C1 1.475(9) .
C1 C2 1.478(12) .
C2 C3 1.519(12) .
C3 K1 3.59(4) .
C4 C4 1.537(16) 6_565
C8 C8 1.527(17) 6_565
Fe1 C5 1.945(6) .
Fe1 C5 1.945(6) 5_566
Fe1 C5 1.945(6) 2_556
Fe1 C5 1.945(6) 6_565
Fe1 C6 1.947(8) 5_566
Fe1 C6 1.947(8) .
N3 C5 1.145(7) .
N3 K1 2.85(5) 5_567
N4 C6 1.148(11) .
K1 K1 1.94(8) 2_658
K1 N3 2.85(5) 5_567
K1 Cl2 3.33(4) 7_557
