#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:57:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179497 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/94/4339451.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_4339451
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 Br8 Fe4 N24'
_chemical_formula_weight         2766.70
_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                 101.2430(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   9.4500(3)
_cell_length_b                   12.5440(3)
_cell_length_c                   16.8530(5)
_cell_measurement_temperature    293(2)
_cell_volume                     1959.43(10)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0431
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7296
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    6.797
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.345
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.953
_refine_diff_density_min         -1.763
_refine_diff_density_rms         0.433
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         4484
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0359
_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)+(0.0557P)²+1.8744P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.1093
_reflns_number_gt                3444
_reflns_number_total             4484
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700607x-file002.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4339451
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 -0.14740(7) 0.49536(4) -0.23484(3) 0.02240(15) Uani 1 1 d .
Ag1 Ag -0.23577(5) 0.27702(3) 0.02139(2) 0.04240(14) Uani 1 1 d .
Ag2 Ag 0.07486(4) 0.22954(3) -0.01072(2) 0.04019(13) Uani 1 1 d .
Br1 Br 0.39765(8) 0.36852(11) -0.01262(4) 0.1069(4) Uani 1 1 d .
Br2 Br -0.71866(7) 0.51628(6) -0.45384(4) 0.0659(2) Uani 1 1 d .
N1 N 0.0793(4) 0.4323(3) -0.2087(2) 0.0317(9) Uani 1 1 d .
N2 N -0.3776(4) 0.5504(3) -0.2649(2) 0.0324(8) Uani 1 1 d .
N3 N -0.2052(5) 0.4001(3) -0.1401(2) 0.0367(9) Uani 1 1 d .
N6 N -0.2054(5) 0.3670(3) -0.3199(2) 0.0348(9) Uani 1 1 d .
N5 N -0.0983(4) 0.5916(3) -0.3321(2) 0.0336(9) Uani 1 1 d .
N4 N -0.0948(4) 0.6191(3) -0.1445(2) 0.0328(9) Uani 1 1 d .
C1 C 0.1355(6) 0.3929(4) -0.2691(3) 0.0418(12) Uani 1 1 d .
H1 H 0.0803 0.3953 -0.3211 0.059(7) Uiso 1 1 calc R
C2 C 0.2712(6) 0.3486(4) -0.2584(3) 0.0458(13) Uani 1 1 d .
H2 H 0.3068 0.3234 -0.3026 0.059(7) Uiso 1 1 calc R
C3 C 0.3526(6) 0.3420(4) -0.1825(3) 0.0440(13) Uani 1 1 d .
H3 H 0.4446 0.3124 -0.1735 0.059(7) Uiso 1 1 calc R
C4 C 0.2941(6) 0.3806(5) -0.1195(3) 0.0445(13) Uani 1 1 d .
C5 C 0.1600(6) 0.4255(4) -0.1345(3) 0.0394(11) Uani 1 1 d .
H5 H 0.1233 0.4523 -0.0912 0.059(7) Uiso 1 1 calc R
C6 C -0.4370(6) 0.5995(4) -0.2090(3) 0.0413(12) Uani 1 1 d .
H6 H -0.3799 0.6126 -0.1584 0.059(7) Uiso 1 1 calc R
C7 C -0.5783(6) 0.6314(5) -0.2232(3) 0.0508(14) Uani 1 1 d .
H7 H -0.6148 0.6665 -0.1829 0.059(7) Uiso 1 1 calc R
C8 C -0.6663(6) 0.6116(5) -0.2969(4) 0.0522(14) Uani 1 1 d .
H8 H -0.7626 0.6324 -0.3078 0.059(7) Uiso 1 1 calc R
C9 C -0.6045(5) 0.5590(4) -0.3542(3) 0.0388(11) Uani 1 1 d .
C10 C -0.4619(6) 0.5315(4) -0.3362(3) 0.0385(11) Uani 1 1 d .
H10 H -0.4220 0.4979 -0.3759 0.059(7) Uiso 1 1 calc R
C11 C -0.2252(5) 0.3572(4) -0.0843(3) 0.0359(11) Uani 1 1 d .
C14 C -0.2265(6) 0.1895(4) 0.1265(3) 0.0354(11) Uani 1 1 d .
C13 C 0.0855(5) 0.1390(4) -0.1123(3) 0.0344(11) Uani 1 1 d .
C12 C 0.0837(5) 0.3237(4) 0.0915(3) 0.0356(11) 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'
Br Br -0.2901 2.4595 '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
N3 Fe N6 90.60(15) .
N3 Fe N5 177.72(15) .
N6 Fe N5 88.68(15) .
N3 Fe N4 86.16(15) .
N6 Fe N4 176.70(14) .
N5 Fe N4 94.53(15) .
N3 Fe N1 91.69(15) .
N6 Fe N1 88.66(15) .
N5 Fe N1 90.45(15) .
N4 Fe N1 92.02(14) .
N3 Fe N2 87.88(15) .
N6 Fe N2 88.27(15) .
N5 Fe N2 89.94(15) .
N4 Fe N2 91.02(15) .
N1 Fe N2 176.90(13) .
C11 Ag1 C14 174.15(19) .
C11 Ag1 Ag2 74.93(14) .
C14 Ag1 Ag2 99.29(14) .
C13 Ag2 C12 174.80(19) .
C13 Ag2 Ag1 116.30(14) .
C12 Ag2 Ag1 68.75(13) .
C1 N1 C5 116.8(4) .
C1 N1 Fe 119.3(3) .
C5 N1 Fe 123.7(3) .
C10 N2 C6 117.4(4) .
C10 N2 Fe 122.3(3) .
C6 N2 Fe 120.3(3) .
C11 N3 Fe 172.1(4) .
C14 N6 Fe 168.2(4) 4_565
C13 N5 Fe 173.1(4) 2_554
C12 N4 Fe 168.8(4) 3_565
N1 C1 C2 123.4(5) .
N1 C1 H1 118.3 .
C2 C1 H1 118.3 .
C3 C2 C1 119.3(5) .
C3 C2 H2 120.4 .
C1 C2 H2 120.4 .
C2 C3 C4 117.7(5) .
C2 C3 H3 121.1 .
C4 C3 H3 121.1 .
C5 C4 C3 120.0(5) .
C5 C4 Br1 120.1(4) .
C3 C4 Br1 119.9(4) .
N1 C5 C4 122.7(5) .
N1 C5 H5 118.6 .
C4 C5 H5 118.6 .
N2 C6 C7 122.8(5) .
N2 C6 H6 118.6 .
C7 C6 H6 118.6 .
C6 C7 C8 120.1(5) .
C6 C7 H7 119.9 .
C8 C7 H7 119.9 .
C9 C8 C7 116.8(5) .
C9 C8 H8 121.6 .
C7 C8 H8 121.6 .
C10 C9 C8 119.7(5) .
C10 C9 Br2 119.5(4) .
C8 C9 Br2 120.6(4) .
N2 C10 C9 123.2(5) .
N2 C10 H10 118.4 .
C9 C10 H10 118.4 .
N3 C11 Ag1 173.3(4) .
N6 C14 Ag1 169.6(4) 4_566
N5 C13 Ag2 176.4(4) 2_544
N4 C12 Ag2 174.5(4) 3_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe N3 2.149(4) .
Fe N6 2.154(4) .
Fe N5 2.158(4) .
Fe N4 2.162(4) .
Fe N1 2.245(4) .
Fe N2 2.244(4) .
Ag1 C11 2.064(4) .
Ag1 C14 2.071(5) .
Ag1 Ag2 3.1438(6) .
Ag2 C13 2.073(4) .
Ag2 C12 2.077(4) .
Br1 C4 1.880(5) .
Br2 C9 1.888(5) .
N1 C1 1.331(6) .
N1 C5 1.335(6) .
N2 C10 1.328(6) .
N2 C6 1.337(6) .
N3 C11 1.131(6) .
N6 C14 1.135(6) 4_565
N5 C13 1.136(6) 2_554
N4 C12 1.135(6) 3_565
C1 C2 1.376(7) .
C1 H1 0.9300 .
C2 C3 1.360(7) .
C2 H2 0.9300 .
C3 C4 1.378(7) .
C3 H3 0.9300 .
C4 C5 1.365(7) .
C5 H5 0.9300 .
C6 C7 1.370(8) .
C6 H6 0.9300 .
C7 C8 1.377(8) .
C7 H7 0.9300 .
C8 C9 1.389(8) .
C8 H8 0.9300 .
C9 C10 1.367(7) .
C10 H10 0.9300 .
C14 N6 1.135(6) 4_566
C13 N5 1.136(6) 2_544
C12 N4 1.135(6) 3_565
