#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/22/4512252.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_4512252
loop_
_publ_author_name
'Piñeiro-López, Lucía'
'Arcís-Castillo, Zulema'
'Muñoz, M. Carmen'
'Real, José A.'
_publ_section_title
;
 Clathration of Five-Membered Aromatic Rings in the Bimetallic Spin
 Crossover Metal--Organic Framework [Fe(TPT)2/3{MI(CN)2}2]·G (MI=
 Ag, Au)
;
_journal_issue                   12
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              6311
_journal_paper_doi               10.1021/cg5010616
_journal_volume                  14
_journal_year                    2014
_chemical_formula_sum            'C18 H10 Ag2 Fe N8 O0.5'
_chemical_formula_weight         617.93
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           166
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   26.8761(8)
_cell_length_b                   26.8761(8)
_cell_length_c                   10.0456(4)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    300(1)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      12
_cell_volume                     6284.0(4)
_computing_cell_refinement       'HKL DENZO'
_computing_data_collection       COLLECT
_computing_data_reduction        'HKL DENZO and SCALEPACK'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      300(1)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.893
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7478
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.81
_diffrn_reflns_theta_min         3.75
_exptl_absorpt_coefficient_mu    1.919
_exptl_absorpt_correction_T_max  0.8616
_exptl_absorpt_correction_T_min  0.7618
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Empirical absorption correction:XABS2'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2682
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.396
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         2085
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1214P)²+10.5162P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1655
_refine_ls_wR_factor_ref         0.1914
_reflns_number_gt                1501
_reflns_number_total             2085
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5010616_si_002.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 4512243--4512254.cif.'
_cod_original_cell_volume        6284.1(4)
_cod_original_sg_symbol_H-M      R-3m
_cod_original_formula_sum        'C18 H10 Ag2 Fe N8 O0.50'
_cod_database_code               4512252
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'y+1/3, x+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z'
'x, x-y, z'
'-y, -x, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
'-y+1/3, -x+2/3, z+2/3'
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
C6 C 0.5869(11) 0.0921(10) 0.508(2) 0.071(6) Uiso 0.25 1 d PD
O O 0.5391(6) 0.0781(13) 0.576(3) 0.098(8) Uiso 0.25 2 d SP
C7 C 0.5834(11) 0.1205(11) 0.400(2) 0.084(7) Uiso 0.25 1 d PD
Ag Ag 0.6667 0.03506(3) 0.3333 0.0782(3) Uani 1 2 d S
Fe Fe 0.5000 0.0000 0.0000 0.0356(3) Uani 1 4 d S
N1 N 0.45257(10) -0.0949(2) 0.0040(5) 0.0434(10) Uani 1 2 d S
N2 N 0.55882(17) 0.00066(17) 0.1466(4) 0.0560(9) Uani 1 1 d .
N3 N 0.30391(10) -0.30391(10) 0.0044(5) 0.0396(9) Uani 1 2 d S
C1 C 0.48015(18) -0.12445(18) 0.0053(6) 0.0529(11) Uani 1 1 d .
H1 H 0.5201 -0.1041 0.0058 0.064 Uiso 1 1 calc R
C2 C 0.45279(18) -0.18326(17) 0.0059(5) 0.0498(10) Uani 1 1 d .
H2 H 0.4739 -0.2021 0.0082 0.060 Uiso 1 1 calc R
C3 C 0.39264(11) -0.2147(2) 0.0031(6) 0.0401(11) Uani 1 2 d S
C4 C 0.36149(11) -0.2770(2) 0.0031(5) 0.0378(11) Uani 1 2 d S
C5 C 0.5958(2) 0.0079(2) 0.2137(6) 0.0632(13) 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'
Fe Fe 0.3463 0.8444 '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'
O O 0.0106 0.0060 '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
O C6 C7 104(2) . .
C6 O C6 111(3) 22_655 .
C7 C7 C6 110.4(16) 22_655 .
C5 Ag C5 167.6(3) . 17_655
N2 Fe N2 86.3(2) 19_655 22_655
N2 Fe N2 180.0(2) 19_655 .
N2 Fe N2 93.7(2) 22_655 .
N2 Fe N2 93.7(2) 19_655 4
N2 Fe N2 180.0(2) 22_655 4
N2 Fe N2 86.3(2) . 4
N2 Fe N1 89.69(14) 19_655 19_655
N2 Fe N1 90.31(14) 22_655 19_655
N2 Fe N1 90.31(14) . 19_655
N2 Fe N1 89.69(14) 4 19_655
N2 Fe N1 90.31(14) 19_655 .
N2 Fe N1 89.69(14) 22_655 .
N2 Fe N1 89.69(14) . .
N2 Fe N1 90.31(14) 4 .
N1 Fe N1 180.00(14) 19_655 .
C1 N1 C1 117.7(5) . 22_655
C1 N1 Fe 121.2(2) . .
C1 N1 Fe 121.2(2) 22_655 .
C5 N2 Fe 169.7(5) . .
C4 N3 C4 115.6(5) . 2_545
N1 C1 C2 123.5(4) . .
N1 C1 H1 118.3 . .
C2 C1 H1 118.3 . .
C3 C2 C1 119.2(4) . .
C3 C2 H2 120.4 . .
C1 C2 H2 120.4 . .
C2 C3 C2 116.9(5) 22_655 .
C2 C3 C4 121.5(2) 22_655 .
C2 C3 C4 121.5(2) . .
N3 C4 N3 124.4(5) . 3_655
N3 C4 C3 117.8(3) . .
N3 C4 C3 117.8(3) 3_655 .
N2 C5 Ag 170.6(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C6 O 1.33(3) .
C6 C7 1.360(10) .
O C6 1.33(3) 22_655
C7 C7 1.24(5) 22_655
Ag C5 2.052(5) .
Ag C5 2.052(5) 17_655
Fe N2 2.154(4) 19_655
Fe N2 2.154(4) 22_655
Fe N2 2.154(4) .
Fe N2 2.154(4) 4
Fe N1 2.208(5) 19_655
Fe N1 2.208(5) .
N1 C1 1.331(5) .
N1 C1 1.331(5) 22_655
N2 C5 1.135(6) .
N3 C4 1.341(3) .
N3 C4 1.341(3) 2_545
C1 C2 1.370(6) .
C1 H1 0.9300 .
C2 C3 1.401(5) .
C2 H2 0.9300 .
C3 C2 1.401(5) 22_655
C3 C4 1.450(7) .
C4 N3 1.341(3) 3_655
