#------------------------------------------------------------------------------
#$Date: 2017-02-04 00:25:31 +0200 (Sat, 04 Feb 2017) $
#$Revision: 191245 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/50/4345098.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_4345098
loop_
_publ_author_name
'Mazzuca, Lidia'
'Cañadillas-Delgado, Laura'
'Rodríguez-Velamazán, J Alberto'
'Fabelo, Oscar'
'Scarrozza, Marco'
'Stroppa, Alessandro'
'Picozzi, Silvia'
'Zhao, Jiong-Peng'
'Bu, Xian-He'
'Rodríguez-Carvajal, Juan'
_publ_section_title
;
 Magnetic Structures of Heterometallic M(II)-M(III) Formate Compounds.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              197
_journal_page_last               207
_journal_paper_doi               10.1021/acs.inorgchem.6b01866
_journal_volume                  56
_journal_year                    2017
_chemical_formula_sum            'C8 H14 Fe Mn N O12'
_chemical_formula_weight         426.98
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           163
_space_group_name_Hall           '-P 3 2c'
_space_group_name_H-M_alt        'P -3 1 c'
_symmetry_space_group_name_Hall  '-P 3 2c'
_symmetry_space_group_name_H-M   'P -3 1 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   8.27550(10)
_cell_length_b                   8.27550(10)
_cell_length_c                   13.8942(2)
_cell_measurement_reflns_used    6464
_cell_measurement_temperature    55(2)
_cell_measurement_theta_max      32.3630
_cell_measurement_theta_min      2.7140
_cell_volume                     824.048(18)
_computing_cell_refinement       'CrysAlis PRO software program'
_computing_data_collection       'CrysAlis PRO software program'
_computing_data_reduction        'CrysAlis PRO software program'
_computing_molecular_graphics    'Mercury (McRae, 2006)'
_computing_publication_material  'WINGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      55(2)
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'CRISTAL beamline, SOLEIL synchrotron'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.66951
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 0.914
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10354
_diffrn_reflns_point_group_measured_fraction_full 0.914
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        23.685
_diffrn_reflns_theta_max         32.600
_diffrn_reflns_theta_min         2.762
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.436
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84225
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            dark-yellow
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_description       prism
_exptl_crystal_F_000             432
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.229
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         1123
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.229
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0262
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0289P)²+0.4955P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0793
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1060
_reflns_number_total             1123
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            FeMn_55K.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        824.05(2)
_cod_database_code               4345098
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_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, -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'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Mn2 Mn 0.6667 0.3333 0.2500 0.01150(11) Uani 1 6 d S T P
Fe1 Fe 1.0000 0.0000 0.0000 0.01090(11) Uani 1 6 d S T P
O1 O 0.88926(14) 0.34252(14) 0.16593(8) 0.0258(2) Uani 1 1 d . . .
O2 O 1.01604(12) 0.20795(13) 0.08174(7) 0.01883(18) Uani 1 1 d . . .
C1 C 0.87844(17) 0.21152(18) 0.11806(8) 0.0192(2) Uani 1 1 d . . .
H1 H 0.7606 0.1085 0.1082 0.041(6) Uiso 1 1 calc R . .
C2 C 1.3333 0.6667 0.1600(11) 0.203(7) Uani 1 3 d S T P
N1 N 1.2790(5) 0.5580(10) 0.2500 0.136(8) Uani 0.3333 2 d S T P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0010 '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 0.0050 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0090 0.0050 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3380 0.7620 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3240 0.6570 '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
O1 Mn2 O1 93.28(4) 4_665 6
O1 Mn2 O1 84.21(5) 4_665 3_665
O1 Mn2 O1 176.49(5) 6 3_665
O1 Mn2 O1 93.28(4) 4_665 5_655
O1 Mn2 O1 93.28(4) 6 5_655
O1 Mn2 O1 89.32(6) 3_665 5_655
O1 Mn2 O1 176.49(5) 4_665 2_655
O1 Mn2 O1 89.32(6) 6 2_655
O1 Mn2 O1 93.28(4) 3_665 2_655
O1 Mn2 O1 84.21(5) 5_655 2_655
O1 Mn2 O1 89.32(6) 4_665 .
O1 Mn2 O1 84.21(5) 6 .
O1 Mn2 O1 93.28(4) 3_665 .
O1 Mn2 O1 176.49(5) 5_655 .
O1 Mn2 O1 93.28(4) 2_655 .
O2 Fe1 O2 91.21(4) 7_755 9_545
O2 Fe1 O2 88.79(4) 7_755 3_765
O2 Fe1 O2 180.00(6) 9_545 3_765
O2 Fe1 O2 88.79(4) 7_755 2_645
O2 Fe1 O2 88.79(4) 9_545 2_645
O2 Fe1 O2 91.21(4) 3_765 2_645
O2 Fe1 O2 91.21(4) 7_755 8_665
O2 Fe1 O2 91.21(4) 9_545 8_665
O2 Fe1 O2 88.79(4) 3_765 8_665
O2 Fe1 O2 180.00(7) 2_645 8_665
O2 Fe1 O2 180.0 7_755 .
O2 Fe1 O2 88.79(4) 9_545 .
O2 Fe1 O2 91.21(4) 3_765 .
O2 Fe1 O2 91.21(4) 2_645 .
O2 Fe1 O2 88.79(4) 8_665 .
C1 O1 Mn2 125.17(9) . .
C1 O2 Fe1 124.96(8) . .
O1 C1 O2 124.48(12) . .
N1 C2 N1 54.5(7) 2_755 .
N1 C2 N1 54.5(7) 2_755 3_775
N1 C2 N1 54.5(7) . 3_775
N1 N1 N1 60.0 2_755 3_775
N1 N1 C2 62.7(3) 2_755 4_775
N1 N1 C2 62.7(3) 3_775 4_775
N1 N1 C2 62.7(3) 2_755 .
N1 N1 C2 62.7(3) 3_775 .
C2 N1 C2 116.2(8) 4_775 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn2 O1 2.1502(10) 4_665
Mn2 O1 2.1502(10) 6
Mn2 O1 2.1502(10) 3_665
Mn2 O1 2.1502(10) 5_655
Mn2 O1 2.1502(10) 2_655
Mn2 O1 2.1502(10) .
Fe1 O2 2.0101(9) 7_755
Fe1 O2 2.0101(9) 9_545
Fe1 O2 2.0101(9) 3_765
Fe1 O2 2.0101(9) 2_645
Fe1 O2 2.0101(9) 8_665
Fe1 O2 2.0102(9) .
O1 C1 1.2363(14) .
O2 C1 1.2593(14) .
C2 N1 1.473(14) 2_755
C2 N1 1.473(14) .
C2 N1 1.473(14) 3_775
N1 N1 1.349(13) 2_755
N1 N1 1.349(13) 3_775
N1 C2 1.473(14) 4_775
