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#$Date: 2016-03-23 01:24:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179139 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/00/4310068.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_4310068
loop_
_publ_author_name
'Ana Galet'
'M. Carmen Muñoz'
'Ana B. Gaspar'
'José A. Real'
_publ_section_title
;
Architectural Isomerism in the Three-Dimensional Polymeric Spin Crossover
System {Fe(pmd)2[Ag(CN)2]2}: Synthesis, Structure, Magnetic Properties,
and Calorimetric Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8749
_journal_page_last               8755
_journal_paper_doi               10.1021/ic0509074
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C48 H32 Ag8 Fe4 N32'
_chemical_formula_weight         2143.42
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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                90.00
_cell_formula_units_Z            1
_cell_length_a                   14.8950(2)
_cell_length_b                   8.1580(4)
_cell_length_c                   13.3480(5)
_cell_measurement_temperature    150(2)
_cell_volume                     1621.96(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      150(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0280
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3394
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.85
_exptl_absorpt_coefficient_mu    1.682
_exptl_crystal_colour            orange-yellow
_exptl_crystal_density_diffrn    2.194
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         1840
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0312P)²+0.3875P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0643
_reflns_number_gt                1572
_reflns_number_total             1840
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0509074si20050606_051018.cif
_cod_data_source_block           ja348
_cod_database_code               4310068
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z+1/2'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z-1/2'
'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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag Ag 0.294834(14) 1.08776(3) 0.196790(15) 0.01952(10) Uani 1 1 d . . .
Fe Fe 0.0000 1.0000 0.0000 0.01275(13) Uani 1 2 d S . .
C1 C 0.05012(18) 0.7029(4) -0.11301(19) 0.0191(6) Uani 1 1 d . . .
H1 H 0.0234 0.7563 -0.1668 0.019(4) Uiso 1 1 calc R . .
N3 N 0.10488(15) 1.0519(3) 0.07905(16) 0.0163(5) Uani 1 1 d . . .
N1 N 0.04912(14) 0.7743(3) -0.02163(15) 0.0149(5) Uani 1 1 d . . .
N4 N 0.12588(17) 0.5432(3) 0.04530(18) 0.0224(5) Uani 1 1 d . . .
N2 N -0.06513(15) 0.9332(3) 0.11965(15) 0.0155(5) Uani 1 1 d . . .
C5 C -0.1111(2) 0.9156(4) 0.1877(2) 0.0198(6) Uani 1 1 d . . .
C3 C 0.1280(2) 0.4760(4) -0.0462(2) 0.0249(7) Uani 1 1 d . . .
H3 H 0.1558 0.3749 -0.0548 0.019(4) Uiso 1 1 calc R . .
C6 C 0.1700(2) 1.0732(4) 0.1230(2) 0.0184(6) Uani 1 1 d . . .
C4 C 0.08665(19) 0.6895(4) 0.05283(18) 0.0180(6) Uani 1 1 d . . .
H4 H 0.0853 0.7370 0.1161 0.019(4) Uiso 1 1 calc R . .
C2 C 0.0901(2) 0.5522(4) -0.1280(2) 0.0237(7) Uani 1 1 d . . .
H2 H 0.0913 0.5038 -0.1911 0.019(4) 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'
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
_geom_angle_publ_flag
C6 Ag C5 159.77(11) 3_575 . ?
C5 Ag N4 105.50(10) 3_575 2_565 ?
C6 Ag N4 90.83(9) . 2_565 ?
C5 Ag Ag 108.35(8) 3_575 2_575 ?
C6 Ag Ag 69.68(8) . 2_575 ?
N4 Ag Ag 125.26(6) 2_565 2_575 ?
N3 Fe N3 180.0 5_575 . ?
N2 Fe N3 90.93(9) 5_575 5_575 ?
N2 Fe N3 89.07(9) . 5_575 ?
N2 Fe N3 89.07(9) 5_575 . ?
N2 Fe N3 90.93(9) . . ?
N2 Fe N2 180.0 5_575 . ?
N3 Fe N1 89.14(9) 5_575 5_575 ?
N3 Fe N1 90.86(9) . 5_575 ?
N2 Fe N1 92.47(9) 5_575 5_575 ?
N2 Fe N1 87.53(9) . 5_575 ?
N3 Fe N1 90.86(9) 5_575 . ?
N3 Fe N1 89.14(9) . . ?
N2 Fe N1 87.53(9) 5_575 . ?
N2 Fe N1 92.47(9) . . ?
N1 Fe N1 180.00(12) 5_575 . ?
N1 C1 C2 121.3(3) . . ?
N1 C1 H1 119.4 . . ?
C2 C1 H1 119.4 . . ?
C6 N3 Fe 175.2(2) . . ?
C4 N1 C1 116.3(2) . . ?
C4 N1 Fe 121.54(18) . . ?
C1 N1 Fe 122.05(19) . . ?
C4 N4 C3 116.5(2) . . ?
C4 N4 Ag 120.91(17) . 2_565 ?
C3 N4 Ag 122.4(2) . 2_565 ?
C5 N2 Fe 169.3(2) . . ?
N2 C5 Ag 171.7(3) . 3_475 ?
N4 C3 C2 121.9(3) . . ?
N4 C3 H3 119.1 . . ?
C2 C3 H3 119.1 . . ?
N3 C6 Ag 173.6(3) . . ?
N1 C4 N4 126.3(2) . . ?
N1 C4 H4 116.8 . . ?
N4 C4 H4 116.8 . . ?
C3 C2 C1 117.7(3) . . ?
C3 C2 H2 121.2 . . ?
C1 C2 H2 121.2 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag C5 2.083(3) 3_575 ?
Ag C6 2.107(3) . ?
Ag N4 2.574(2) 2_565 ?
Ag Ag 2.9649(5) 2_575 ?
Fe N3 1.932(2) 5_575 ?
Fe N3 1.932(2) . ?
Fe N2 1.946(2) 5_575 ?
Fe N2 1.946(2) . ?
Fe N1 2.002(2) 5_575 ?
Fe N1 2.002(2) . ?
C1 N1 1.352(3) . ?
C1 C2 1.380(4) . ?
C1 H1 0.9300 . ?
N3 C6 1.147(4) . ?
N1 C4 1.334(3) . ?
N4 C4 1.332(4) . ?
N4 C3 1.339(4) . ?
N4 Ag 2.574(2) 2_565 ?
N2 C5 1.147(4) . ?
C6 Ag 2.083(3) 3_475 ?
C3 C2 1.377(4) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C2 H2 0.9300 . ?
