#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:57:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179497 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/94/4339449.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_4339449
loop_
_publ_author_name
'Muñoz, M Carmen'
'Gaspar, Ana B.'
'Galet, Ana'
'Real, José A'
_publ_section_title
;
 Spin-crossover behavior in cyanide-bridged iron(II)-silver(I) bimetallic
 2D Hofmann-like metal-organic frameworks.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8182
_journal_page_last               8192
_journal_paper_doi               10.1021/ic700607x
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C56 H32 Ag8 Cl8 Fe4 N24'
_chemical_formula_weight         2411.02
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 99.437(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   9.2580(2)
_cell_length_b                   12.9500(3)
_cell_length_c                   16.5700(4)
_cell_measurement_temperature    270(2)
_cell_volume                     1959.71(8)
_computing_cell_refinement       'HKL DENZO'
_computing_data_collection       COLLECT
_computing_data_reduction        'HKL DENZO and SCALEPACK'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      270(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8628
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    2.990
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.043
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.946
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.260
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         4473
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0691P)²+2.3348P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1274
_reflns_number_gt                3179
_reflns_number_total             4473
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700607x-file002.cif
_cod_data_source_block           2_(270_K)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4339449
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Fe Fe 0.84540(7) 0.50319(5) 0.26385(3) 0.02268(17) Uani 1 1 d .
Ag2 Ag 0.76588(5) 0.77185(3) 0.02038(2) 0.04233(15) Uani 1 1 d .
Ag1 Ag 0.91477(5) 0.26682(3) 0.00966(2) 0.04148(15) Uani 1 1 d .
Cl1 Cl 0.2862(2) 0.47347(19) 0.05132(11) 0.0830(6) Uani 1 1 d .
Cl2 Cl 1.3895(2) 0.6063(3) 0.47710(12) 0.1189(11) Uani 1 1 d .
N1 N 0.6131(5) 0.4499(3) 0.2359(2) 0.0322(9) Uani 1 1 d .
N2 N 1.0760(5) 0.5650(3) 0.2899(3) 0.0377(10) Uani 1 1 d .
N3 N 0.8965(5) 0.4078(3) 0.1662(2) 0.0348(10) Uani 1 1 d .
N4 N 0.7900(5) 0.6269(3) 0.1769(2) 0.0353(10) Uani 1 1 d .
N5 N 0.7863(5) 0.5975(3) 0.3595(2) 0.0347(10) Uani 1 1 d .
N6 N 0.8972(5) 0.3832(3) 0.3541(2) 0.0349(10) Uani 1 1 d .
C1 C 0.5477(6) 0.4037(4) 0.2925(3) 0.0428(13) Uani 1 1 d .
H1 H 0.6022 0.3923 0.3440 0.061(7) Uiso 1 1 calc R
C2 C 0.4052(7) 0.3724(5) 0.2783(4) 0.0597(17) Uani 1 1 d .
H2 H 0.3649 0.3394 0.3192 0.061(7) Uiso 1 1 calc R
C3 C 0.3217(7) 0.3899(5) 0.2035(4) 0.0577(17) Uani 1 1 d .
H3 H 0.2246 0.3685 0.1921 0.061(7) Uiso 1 1 calc R
C4 C 0.3871(6) 0.4406(5) 0.1450(3) 0.0474(14) Uani 1 1 d .
C5 C 0.5310(6) 0.4670(4) 0.1623(3) 0.0390(12) Uani 1 1 d .
H5 H 0.5744 0.4980 0.1217 0.061(7) Uiso 1 1 calc R
C6 C 1.1356(7) 0.6093(5) 0.2305(4) 0.0500(15) Uani 1 1 d .
H6 H 1.0805 0.6110 0.1783 0.061(7) Uiso 1 1 calc R
C7 C 1.2729(8) 0.6526(5) 0.2413(4) 0.0609(17) Uani 1 1 d .
H7 H 1.3100 0.6817 0.1977 0.061(7) Uiso 1 1 calc R
C8 C 1.3520(7) 0.6514(5) 0.3171(4) 0.0618(18) Uani 1 1 d .
H8 H 1.4452 0.6802 0.3267 0.061(7) Uiso 1 1 calc R
C9 C 1.2955(7) 0.6083(5) 0.3788(4) 0.0544(16) Uani 1 1 d .
C10 C 1.1548(6) 0.5647(5) 0.3641(3) 0.0475(14) Uani 1 1 d .
H10 H 1.1164 0.5352 0.4072 0.061(7) Uiso 1 1 calc R
C11 C 0.9063(6) 0.3586(4) 0.1106(3) 0.0358(12) Uani 1 1 d .
C12 C 0.7717(6) 0.6817(4) 0.1240(3) 0.0364(12) Uani 1 1 d .
C13 C 0.7703(6) 0.6435(4) 0.4158(3) 0.0382(12) Uani 1 1 d .
C14 C 0.9056(6) 0.3270(4) 0.4077(3) 0.0392(12) Uani 1 1 d .
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 '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'
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
N5 Fe N3 177.94(16) . .
N5 Fe N6 87.29(16) . .
N3 Fe N6 93.24(16) . .
N5 Fe N4 90.52(15) . .
N3 Fe N4 88.94(16) . .
N6 Fe N4 177.79(15) . .
N5 Fe N1 88.60(15) . .
N3 Fe N1 89.41(15) . .
N6 Fe N1 91.06(16) . .
N4 Fe N1 88.59(16) . .
N5 Fe N2 90.28(16) . .
N3 Fe N2 91.69(16) . .
N6 Fe N2 91.57(16) . .
N4 Fe N2 88.73(17) . .
N1 Fe N2 177.09(15) . .
C13 Ag2 C12 176.6(2) 4_575 .
C13 Ag2 Ag1 78.51(15) 4_575 3_765
C12 Ag2 Ag1 98.37(15) . 3_765
C11 Ag1 C14 175.5(2) . 4_565
C11 Ag1 Ag2 112.63(15) . 3_765
C14 Ag1 Ag2 71.85(15) 4_565 3_765
C1 N1 C5 117.1(5) . .
C1 N1 Fe 121.6(4) . .
C5 N1 Fe 121.3(3) . .
C10 N2 C6 117.1(5) . .
C10 N2 Fe 122.5(4) . .
C6 N2 Fe 120.3(4) . .
C11 N3 Fe 171.8(4) . .
C12 N4 Fe 169.1(4) . .
C13 N5 Fe 171.7(4) . .
C14 N6 Fe 168.2(4) . .
N1 C1 C2 123.2(5) . .
N1 C1 H1 118.4 . .
C2 C1 H1 118.4 . .
C3 C2 C1 119.6(6) . .
C3 C2 H2 120.2 . .
C1 C2 H2 120.2 . .
C2 C3 C4 117.7(6) . .
C2 C3 H3 121.2 . .
C4 C3 H3 121.2 . .
C5 C4 C3 119.7(5) . .
C5 C4 Cl1 119.6(5) . .
C3 C4 Cl1 120.7(5) . .
N1 C5 C4 122.6(5) . .
N1 C5 H5 118.7 . .
C4 C5 H5 118.7 . .
N2 C6 C7 124.4(6) . .
N2 C6 H6 117.8 . .
C7 C6 H6 117.8 . .
C8 C7 C6 117.8(6) . .
C8 C7 H7 121.1 . .
C6 C7 H7 121.1 . .
C9 C8 C7 119.7(6) . .
C9 C8 H8 120.1 . .
C7 C8 H8 120.1 . .
C8 C9 C10 120.0(6) . .
C8 C9 Cl2 121.9(5) . .
C10 C9 Cl2 118.1(5) . .
N2 C10 C9 121.0(6) . .
N2 C10 H10 119.5 . .
C9 C10 H10 119.5 . .
N3 C11 Ag1 177.4(5) . .
N4 C12 Ag2 171.0(5) . .
N5 C13 Ag2 173.7(5) . 4_576
N6 C14 Ag1 175.9(5) . 4_566
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe N5 2.142(4) .
Fe N3 2.149(4) .
Fe N6 2.155(4) .
Fe N4 2.160(4) .
Fe N1 2.234(4) .
Fe N2 2.255(4) .
Ag2 C13 2.057(5) 4_575
Ag2 C12 2.069(5) .
Ag2 Ag1 3.1180(6) 3_765
Ag1 C11 2.064(5) .
Ag1 C14 2.072(5) 4_565
Ag1 Ag2 3.1180(6) 3_765
Cl1 C4 1.729(6) .
Cl2 C9 1.716(6) .
N1 C1 1.338(6) .
N1 C5 1.345(6) .
N2 C10 1.323(7) .
N2 C6 1.333(7) .
N3 C11 1.136(6) .
N4 C12 1.119(6) .
N5 C13 1.137(6) .
N6 C14 1.141(6) .
C1 C2 1.363(8) .
C1 H1 0.9300 .
C2 C3 1.368(9) .
C2 H2 0.9300 .
C3 C4 1.388(8) .
C3 H3 0.9300 .
C4 C5 1.360(8) .
C5 H5 0.9300 .
C6 C7 1.373(8) .
C6 H6 0.9300 .
C7 C8 1.346(9) .
C7 H7 0.9300 .
C8 C9 1.343(9) .
C8 H8 0.9300 .
C9 C10 1.404(8) .
C10 H10 0.9300 .
C13 Ag2 2.057(5) 4_576
C14 Ag1 2.072(5) 4_566
