#------------------------------------------------------------------------------
#$Date: 2016-03-21 16:41:47 +0100 (lun 21 de mar de 2016) $
#$Revision: 178790 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/44/4104493.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_4104493
loop_
_publ_author_name
'Karl S. Hagen'
'Sunil G. Naik'
'Boi Hanh Huynh'
'Antonio Masello'
'George Christou'
_publ_contact_author_address
;
Department of Chemistry
Emory University
Atlanta, GA 30322
;
_publ_contact_author_email       khagen@emory.edu
_publ_contact_author_fax         1-404-727-6586
_publ_contact_author_name        'Karl S. Hagen'
_publ_contact_author_phone       1-404-727-6556
_publ_section_title
;
 Intensely Colored Mixed-Valence Iron(II) Iron(III) Formate Analogue of
 Prussian Blue Exhibits Néel N-Type Ferrimagnetism
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7516
_journal_page_last               7517
_journal_paper_doi               10.1021/ja901093b
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C3 H3 Fe O6, C2 H8 N1'
_chemical_formula_sum            'C5 H15 Fe N O6'
_chemical_formula_weight         241.03
_chemical_name_common            catena-(Me2NH2)[Fe(HCOO)3]
_chemical_name_systematic
catena-(dimethylammonium)-(tris(μ₂-Formato-O,O')-iron(ii)
_space_group_IT_number           167
_symmetry_cell_setting           rhombohedral
_symmetry_Int_Tables_number      167
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2009-01-05 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   8.2310(5)
_cell_length_b                   8.2310(5)
_cell_length_c                   22.399(3)
_cell_measurement_reflns_used    2430
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.00
_cell_measurement_theta_min      3.00
_cell_volume                     1314.2(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0180
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            3379
_diffrn_reflns_theta_full        32.00
_diffrn_reflns_theta_max         32.00
_diffrn_reflns_theta_min         2.73
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker D8 Apex'
_exptl_absorpt_coefficient_mu    1.722
_exptl_absorpt_correction_T_max  0.6827
_exptl_absorpt_correction_T_min  0.5683
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Xprep, Bruker'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.827
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.0034(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     27
_refine_ls_number_reflns         513
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0206
_refine_ls_R_factor_gt           0.0199
_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)+(0.0290P)²+0.9725P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0535
_reflns_number_gt                494
_reflns_number_total             513
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja901093b_si_001.cif
_cod_data_source_block           feofmf
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4104493
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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
Fe1 Fe 0.0000 0.0000 0.0000 0.01228(12) Uani 1 6 d S
O1 O -0.20692(9) -0.21893(10) 0.05440(3) 0.02138(17) Uani 1 1 d .
C1 C -0.3333 -0.21230(15) 0.0833 0.0179(2) Uani 1 2 d S
H1 H -0.3333 -0.0957 0.0833 0.022 Uiso 1 2 d SR
C2 C 0.0000 0.0000 0.19548(10) 0.0374(5) Uani 1 3 d S
H2 H -0.0162 0.1056 0.1875 0.045 Uiso 1 1 d R
N1 N 0.0870(4) 0.0000 0.2500 0.0211(6) Uani 0.33 2 d SP
H3 H 0.2194 0.1114 0.2541 0.025 Uiso 0.33 1 d P
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.01225(14) 0.01225(14) 0.01235(16) 0.000 0.000 0.00613(7)
O1 0.0191(3) 0.0200(3) 0.0248(3) 0.0041(2) 0.0076(2) 0.0096(2)
C1 0.0161(5) 0.0175(4) 0.0196(5) 0.0006(2) 0.0011(4) 0.0081(2)
C2 0.0449(8) 0.0449(8) 0.0223(8) 0.000 0.000 0.0225(4)
N1 0.0172(11) 0.0175(14) 0.0285(16) -0.0018(12) -0.0009(6) 0.0087(7)
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'
O O 0.0106 0.0060 '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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 0.00 1.00 0.2920
0.00 0.00 -1.00 0.2640
1.00 0.00 -2.00 0.1810
-1.00 0.00 2.00 0.2050
0.00 -1.00 -2.00 0.1240
0.00 1.00 2.00 0.1980
-1.00 3.00 2.00 0.1180
-1.00 1.00 -3.00 0.1960
1.00 -1.00 2.00 0.1940
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
O1 Fe1 O1 180.00(4) 20 2
O1 Fe1 O1 90.69(3) 20 21
O1 Fe1 O1 89.31(3) 2 21
O1 Fe1 O1 89.31(3) 20 3
O1 Fe1 O1 90.69(3) 2 3
O1 Fe1 O1 180.00(4) 21 3
O1 Fe1 O1 90.69(3) 20 19
O1 Fe1 O1 89.31(3) 2 19
O1 Fe1 O1 90.69(3) 21 19
O1 Fe1 O1 89.31(3) 3 19
O1 Fe1 O1 89.31(3) 20 .
O1 Fe1 O1 90.69(3) 2 .
O1 Fe1 O1 89.31(3) 21 .
O1 Fe1 O1 90.69(3) 3 .
O1 Fe1 O1 180.00(3) 19 .
C1 O1 Fe1 126.08(7) . .
O1 C1 O1 125.24(12) 18_444 .
O1 C1 H1 117.4 18_444 .
O1 C1 H1 117.4 . .
N1 C2 N1 52.0(2) 2 3
N1 C2 N1 52.0(2) 2 .
N1 C2 N1 52.0(2) 3 .
N1 C2 H2 70.5 2 .
N1 C2 H2 110.7 3 .
N1 C2 H2 117.3 . .
N1 N1 N1 60.0 3 2
N1 N1 C2 64.02(11) 3 4
N1 N1 C2 64.02(11) 2 4
N1 N1 C2 64.02(11) 3 .
N1 N1 C2 64.02(11) 2 .
C2 N1 C2 119.2(3) 4 .
N1 N1 H3 157.9 3 .
N1 N1 H3 98.5 2 .
C2 N1 H3 103.6 4 .
C2 N1 H3 113.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O1 2.1362(7) 20
Fe1 O1 2.1362(7) 2
Fe1 O1 2.1362(7) 21
Fe1 O1 2.1362(7) 3
Fe1 O1 2.1362(7) 19
Fe1 O1 2.1362(7) .
O1 C1 1.2500(8) .
C1 O1 1.2499(8) 18_444
C1 H1 0.9601 .
C2 N1 1.416(3) 2
C2 N1 1.416(3) 3
C2 N1 1.416(3) .
C2 H2 0.9600 .
N1 N1 1.240(6) 3
N1 N1 1.240(6) 2
N1 C2 1.416(3) 4
N1 H3 1.0187 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O1 Fe1 O1 C1 -60.62(4) 20 .
O1 Fe1 O1 C1 119.38(4) 2 .
O1 Fe1 O1 C1 -151.32(7) 21 .
O1 Fe1 O1 C1 28.68(7) 3 .
O1 Fe1 O1 C1 -32.31(5) 19 .
Fe1 O1 C1 O1 175.75(6) . 18_444
N1 C2 N1 N1 67.58(7) 2 3
N1 C2 N1 N1 -67.58(7) 3 2
N1 C2 N1 C2 33.79(3) 2 4
N1 C2 N1 C2 -33.79(3) 3 4
