#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:36:54 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179669 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/22/4512249.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_4512249
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            'C24 H18 Au2 Fe N10'
_chemical_formula_weight         896.27
_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                   26.4590(10)
_cell_length_b                   26.4590(10)
_cell_length_c                   9.5783(5)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      12
_cell_volume                     5807.2(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      120(1)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.917
_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  0.0405
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6502
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.48
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    11.929
_exptl_absorpt_correction_T_max  0.5869
_exptl_absorpt_correction_T_min  0.3817
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Empirical absorption correction:XABS2'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3744
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.462
_refine_diff_density_min         -1.118
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         2269
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0461P)²+190.5547P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1314
_reflns_number_gt                1823
_reflns_number_total             2269
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5010616_si_007.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 4512243--4512254.cif.'
_cod_original_sg_symbol_H-M      R-3m
_cod_database_code               4512249
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
Au Au 0.373651(17) 0.3333 0.8333 0.03753(16) Uani 1 2 d S
Fe Fe 0.5000 0.5000 0.5000 0.0210(4) Uani 1 4 d S
N1 N 0.4548(2) 0.5452(2) 0.5027(10) 0.0321(19) Uani 1 2 d S
N2 N 0.4449(3) 0.4438(3) 0.6464(7) 0.0348(14) Uani 1 1 d .
N3 N 0.3924(3) 0.69619(17) 0.5024(9) 0.0298(18) Uani 1 2 d S
C1 C 0.4833(3) 0.6040(3) 0.5027(9) 0.0339(16) Uani 1 1 d .
H1 H 0.5238 0.6243 0.5024 0.041 Uiso 1 1 calc R
C2 C 0.4546(3) 0.6351(3) 0.5029(9) 0.0356(17) Uani 1 1 d .
H2 H 0.4757 0.6757 0.5039 0.043 Uiso 1 1 calc R
C3 C 0.3940(2) 0.6060(2) 0.5018(13) 0.035(2) Uani 1 2 d S
C4 C 0.3619(2) 0.6381(2) 0.4996(12) 0.034(2) Uani 1 2 d S
C5 C 0.4153(4) 0.4047(4) 0.7160(9) 0.0369(17) Uani 1 1 d .
N4 N 0.6042(7) 0.8021(4) 0.4283(18) 0.074(4) Uani 1 2 d S
C6 C 0.5854(7) 0.7526(6) 0.3622(15) 0.081(4) Uani 1 1 d .
H6 H 0.5941 0.7236 0.3852 0.097 Uiso 1 1 calc R
C7 C 0.5509(6) 0.7505(6) 0.2536(16) 0.083(4) Uani 1 1 d .
H7 H 0.5311 0.7197 0.1914 0.100 Uiso 1 1 calc R
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'
Au Au -2.0133 8.8022 '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
C5 Au C5 170.9(5) . 16_556
N2 Fe N2 180.0(4) 24_665 6_556
N2 Fe N2 87.2(4) 24_665 19_666
N2 Fe N2 92.8(4) 6_556 19_666
N2 Fe N2 92.8(4) 24_665 .
N2 Fe N2 87.2(4) 6_556 .
N2 Fe N2 180.0(4) 19_666 .
N2 Fe N1 89.8(3) 24_665 19_666
N2 Fe N1 90.2(3) 6_556 19_666
N2 Fe N1 90.2(3) 19_666 19_666
N2 Fe N1 89.8(3) . 19_666
N2 Fe N1 90.2(3) 24_665 .
N2 Fe N1 89.8(3) 6_556 .
N2 Fe N1 89.8(3) 19_666 .
N2 Fe N1 90.2(3) . .
N1 Fe N1 180.000(1) 19_666 .
C1 N1 C1 117.8(9) . 24_665
C1 N1 Fe 121.1(5) . .
C1 N1 Fe 121.1(5) 24_665 .
C5 N2 Fe 167.5(7) . .
C4 N3 C4 116.8(11) . 2_665
N1 C1 C2 122.5(7) . .
N1 C1 H1 118.8 . .
C2 C1 H1 118.8 . .
C1 C2 C3 120.0(7) . .
C1 C2 H2 120.0 . .
C3 C2 H2 120.0 . .
C2 C3 C2 117.3(10) . 24_665
C2 C3 C4 121.4(5) . .
C2 C3 C4 121.4(5) 24_665 .
N3 C4 N3 123.2(10) . 3_565
N3 C4 C3 118.4(5) . .
N3 C4 C3 118.4(5) 3_565 .
N2 C5 Au 170.8(8) . .
C6 N4 C6 108(2) . 23_565
N4 C6 C7 108.7(15) . .
N4 C6 H6 125.7 . .
C7 C6 H6 125.7 . .
C7 C7 C6 107.1(9) 23_565 .
C7 C7 H7 126.5 23_565 .
C6 C7 H7 126.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Au C5 1.990(8) .
Au C5 1.990(8) 16_556
Fe N2 2.033(7) 24_665
Fe N2 2.033(7) 6_556
Fe N2 2.033(7) 19_666
Fe N2 2.033(7) .
Fe N1 2.071(9) 19_666
Fe N1 2.071(9) .
N1 C1 1.349(8) .
N1 C1 1.349(8) 24_665
N2 C5 1.149(10) .
N3 C4 1.332(7) .
N3 C4 1.332(7) 2_665
C1 C2 1.369(11) .
C1 H1 0.9300 .
C2 C3 1.390(9) .
C2 H2 0.9300 .
C3 C2 1.390(9) 24_665
C3 C4 1.468(15) .
C4 N3 1.332(7) 3_565
N4 C6 1.310(16) .
N4 C6 1.310(16) 23_565
C6 C7 1.37(2) .
C6 H6 0.9300 .
C7 C7 1.32(3) 23_565
C7 H7 0.9300 .
