#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:02:50 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180120 $
#$URL: svn://www.crystallography.net/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'
'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                 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       θ-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/[σ²(Fo²)+(0.0999P)²+9.0157P] where P=(Fo²+2Fc²)/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)
_cod_data_source_file            b615130b.txt
_cod_data_source_block           ber6_90
_cod_original_sg_symbol_H-M      'I 2/m'
_cod_database_code               7101818
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_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(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
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
