#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/24/2232491.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2232491
loop_
_publ_author_name
'Chygorin, Eduard N.'
'Petrusenko, Svitlana R.'
'Kokozay, Volodymyr N.'
'Smal, Yuri O.'
'Omelchenko, Irina V.'
'Shishkin, Oleg V.'
_publ_section_title
;
 Hexakis(dimethylformamide-κO)manganese(II)
 μ-oxido-bis[trichloridoferrate(III)]
;
_journal_coeditor_code           WM2531
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1563
_journal_page_last               m1564
_journal_paper_doi               10.1107/S1600536811041523
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Mn (C3 H7 N O)6] [Fe2 Cl6 O]'
_chemical_formula_moiety         'C18 H42 Mn N6 O6 2+, Cl6 Fe2 O 2-'
_chemical_formula_sum            'C18 H42 Cl6 Fe2 Mn N6 O7'
_chemical_formula_weight         833.92
_chemical_name_systematic
;
Hexakis(dimethylformamide-κO)manganese(II)
μ-oxido-bis[trichloridoferrate(III)]
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
CrysAlis RED (Oxford Diffraction, 2010)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   14.0171(8)
_cell_length_b                   14.0171(8)
_cell_length_c                   15.3966(14)
_cell_measurement_reflns_used    2653
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.5139
_cell_measurement_theta_min      2.9005
_cell_volume                     2619.8(3)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2010)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2010)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2010)
;
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1827
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur/Sapphire3'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_sigmaI/netI    0.3499
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16066
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.0000
_diffrn_reflns_theta_min         2.9005
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.677
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2010)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1281
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.054
_refine_diff_density_min         -0.371
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     68
_refine_ls_number_reflns         1624
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0385
_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)+(0.0428P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0924
_reflns_number_gt                1323
_reflns_number_total             1624
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            wm2531.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               2232491
_cod_database_fobs_code          2232491
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+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+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, -z'
'y, -x+y, -z'
'x-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+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'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Mn Mn1 0.0000 0.0000 0.5000 0.02020(19) Uani d S 1 6
N N1 0.23962(14) -0.02345(15) 0.65588(11) 0.0223(4) Uani d . 1 1
Fe Fe1 0.0000 0.0000 0.88467(3) 0.02113(16) Uani d S 1 3
O O1 0.08798(13) -0.06054(12) 0.57785(10) 0.0262(4) Uani d . 1 1
Cl Cl1 0.03397(5) -0.12729(4) 0.82931(3) 0.02609(16) Uani d . 1 1
C C1 0.15838(18) -0.00668(18) 0.63362(15) 0.0232(4) Uani d . 1 1
H H1 0.1622(18) 0.0567(19) 0.6623(13) 0.015(6) Uiso d . 1 1
O O1S 0.0000 0.0000 1.0000 0.0282(8) Uani d S 1 6
C C2 0.2521(2) -0.1115(2) 0.61800(16) 0.0318(5) Uani d . 1 1
H H2A 0.1939 -0.1512 0.5750 0.048 Uiso calc R 1 1
H H2B 0.2467 -0.1626 0.6638 0.048 Uiso calc R 1 1
H H2C 0.3242 -0.0802 0.5897 0.048 Uiso calc R 1 1
C C3 0.3184(2) 0.0425(2) 0.72297(17) 0.0347(6) Uani d . 1 1
H H3A 0.3143 -0.0055 0.7709 0.052 Uiso calc R 1 1
H H3B 0.3010 0.0977 0.7446 0.052 Uiso calc R 1 1
H H3C 0.3929 0.0795 0.6985 0.052 Uiso calc R 1 1
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'
N N 0.0061 0.0033 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Mn1 O1 11_556 2 180.00(6)
O1 Mn1 O1 11_556 . 87.49(6)
O1 Mn1 O1 2 . 92.51(6)
O1 Mn1 O1 11_556 10_556 92.51(6)
O1 Mn1 O1 2 10_556 87.49(6)
O1 Mn1 O1 . 10_556 180.00(7)
O1 Mn1 O1 11_556 12_556 92.51(6)
O1 Mn1 O1 2 12_556 87.49(6)
O1 Mn1 O1 . 12_556 87.49(6)
O1 Mn1 O1 10_556 12_556 92.51(6)
O1 Mn1 O1 11_556 3 87.49(6)
O1 Mn1 O1 2 3 92.51(6)
O1 Mn1 O1 . 3 92.51(6)
O1 Mn1 O1 10_556 3 87.49(6)
O1 Mn1 O1 12_556 3 180.00(7)
C1 N1 C2 . . 121.94(18)
C1 N1 C3 . . 121.34(19)
C2 N1 C3 . . 116.65(18)
O1S Fe1 Cl1 . 2 112.438(17)
O1S Fe1 Cl1 . . 112.438(17)
Cl1 Fe1 Cl1 2 . 106.348(19)
O1S Fe1 Cl1 . 3 112.438(17)
Cl1 Fe1 Cl1 2 3 106.348(19)
Cl1 Fe1 Cl1 . 3 106.348(19)
C1 O1 Mn1 . . 125.35(15)
O1 C1 N1 . . 124.6(2)
O1 C1 H1 . . 122.4(13)
N1 C1 H1 . . 112.8(13)
Fe1 O1S Fe1 10_557 . 180.0
N1 C2 H2A . . 109.5
N1 C2 H2B . . 109.5
H2A C2 H2B . . 109.5
N1 C2 H2C . . 109.5
H2A C2 H2C . . 109.5
H2B C2 H2C . . 109.5
N1 C3 H3A . . 109.5
N1 C3 H3B . . 109.5
H3A C3 H3B . . 109.5
N1 C3 H3C . . 109.5
H3A C3 H3C . . 109.5
H3B C3 H3C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 O1 11_556 2.1736(15) ?
Mn1 O1 2 2.1736(15) ?
Mn1 O1 . 2.1736(15) y
Mn1 O1 10_556 2.1736(15) ?
Mn1 O1 12_556 2.1736(15) ?
Mn1 O1 3 2.1736(15) ?
N1 C1 . 1.318(3) ?
N1 C2 . 1.453(3) ?
N1 C3 . 1.456(3) ?
Fe1 O1S . 1.7758(5) y
Fe1 Cl1 2 2.2330(6) ?
Fe1 Cl1 . 2.2330(6) y
Fe1 Cl1 3 2.2330(6) ?
O1 C1 . 1.239(3) ?
C1 H1 . 0.97(2) ?
O1S Fe1 10_557 1.7758(5) ?
C2 H2A . 0.9800 ?
C2 H2B . 0.9800 ?
C2 H2C . 0.9800 ?
C3 H3A . 0.9800 ?
C3 H3B . 0.9800 ?
C3 H3C . 0.9800 ?
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_site_symmetry_1
_geom_torsion
O1 Mn1 O1 C1 11_556 169.64(18)
O1 Mn1 O1 C1 2 -10.36(18)
O1 Mn1 O1 C1 12_556 77.01(14)
O1 Mn1 O1 C1 3 -102.99(14)
Mn1 O1 C1 N1 . -152.23(16)
C2 N1 C1 O1 . -2.2(3)
C3 N1 C1 O1 . -179.2(2)
