#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:42:20 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180050 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/44/7034431.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_7034431
loop_
_publ_author_name
'Ciupa, Aneta'
'Mączka, Mirosław'
'Gągor, Anna'
'Sieradzki, Adam'
'Trzmiel, Justyna'
'Pikul, Adam'
'Ptak, Maciej'
_publ_section_title
;
 Temperature-dependent studies of [(CH3)2NH2][Fe(III)M(II)(HCOO)6]
 frameworks (M(II) = Fe and Mg): structural, magnetic, dielectric and
 phonon properties.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8846
_journal_page_last               8854
_journal_paper_doi               10.1039/c5dt00512d
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C8 H14 Fe Mg N O12'
_chemical_formula_weight         396.36
_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-2014/7
_audit_update_record
;
2015-03-10 deposited with the CCDC.
2015-03-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   8.2076(2)
_cell_length_b                   8.2076(2)
_cell_length_c                   13.8988(6)
_cell_measurement_reflns_used    3797
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.3896
_cell_measurement_theta_min      2.8603
_cell_volume                     810.85(4)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_molecular_graphics
'Diamond Version 3.2k Crystal Impact GbR, Bonn, Germany'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 8.4350
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire1, long nozzle'
_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  0.0368
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8337
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.656
_diffrn_reflns_theta_max         25.656
_diffrn_reflns_theta_min         2.931
_exptl_absorpt_coefficient_mu    1.027
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    1.623
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             406
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.295
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         518
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.244
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0320P)²+0.1100P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0604
_refine_ls_wR_factor_ref         0.0618
_reflns_Friedel_coverage         0.000
_reflns_number_gt                433
_reflns_number_total             518
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt00512d2.cif
_cod_data_source_block           model1
_cod_depositor_comments
'Adding full bibliography for 7034429--7034431.cif.'
_cod_original_cell_volume        810.85(5)
_cod_database_code               7034431
#BEGIN Tags that were not found in dictionaries:
_shelx_shelxl_version_number     2014/7
_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.
;
#END Tags that were not found in dictionaries
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
Fe1 Fe 0.3333 0.6667 0.2500 0.0157(3) Uani 0.300(3) 6 d S T P
Mg1 Mg 0.3333 0.6667 0.2500 0.0157(3) Uani 0.700(4) 6 d S T P
Fe2 Fe 0.0000 1.0000 0.0000 0.0134(2) Uani 0.702(3) 6 d S T P
Mg2 Mg 0.0000 1.0000 0.0000 0.0134(2) Uani 0.297(4) 6 d S T P
O1 O 0.12234(18) 0.6627(2) 0.16840(8) 0.0335(4) Uani 1 1 d . . .
O2 O -0.00803(18) 0.79308(17) 0.08205(9) 0.0294(3) Uani 1 1 d . . .
C1 C 0.1284(3) 0.7904(3) 0.11959(13) 0.0327(5) Uani 1 1 d . . .
H1 H 0.2464 0.8954 0.1097 0.039 Uiso 1 1 calc R U .
C2 C 0.3333 0.6667 0.8736(8) 0.105(4) Uani 0.5 3 d DS TU P
H2A H 0.4511 0.7824 0.8698 0.158 Uiso 0.1667 1 calc R U P
H2B H 0.3390 0.5902 0.9242 0.158 Uiso 0.1667 1 calc R U P
H2C H 0.2342 0.6934 0.8867 0.158 Uiso 0.1667 1 calc R U P
C21 C 0.3333 0.6667 0.6905(10) 0.105(4) Uani 0.5 3 d DS TU P
H21A H 0.3234 0.7773 0.6998 0.158 Uiso 0.1667 1 calc R U P
H21B H 0.2434 0.5874 0.6431 0.158 Uiso 0.1667 1 calc R U P
H21C H 0.4579 0.7026 0.6689 0.158 Uiso 0.1667 1 calc R U P
N1 N 0.296(2) 0.5648(19) 0.7809(7) 0.067(4) Uiso 0.1667 1 d D . P
H1A H 0.3543 0.4950 0.7790 0.080 Uiso 0.1667 1 d . U P
H1B H 0.1671 0.4706 0.7790 0.080 Uiso 0.1667 1 d . U P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Mg Mg 0.0486 0.0363 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Fe1 O1 88.64(8) . 4_665
O1 Fe1 O1 86.36(7) . 6_565
O1 Fe1 O1 92.51(5) 4_665 6_565
O1 Fe1 O1 92.51(5) . 3_565
O1 Fe1 O1 86.36(7) 4_665 3_565
O1 Fe1 O1 178.42(8) 6_565 3_565
O1 Fe1 O1 92.51(5) . 2_665
O1 Fe1 O1 178.42(8) 4_665 2_665
O1 Fe1 O1 88.64(8) 6_565 2_665
O1 Fe1 O1 92.51(5) 3_565 2_665
O1 Fe1 O1 178.42(8) . 5
O1 Fe1 O1 92.51(5) 4_665 5
O1 Fe1 O1 92.51(5) 6_565 5
O1 Fe1 O1 88.64(8) 3_565 5
O1 Fe1 O1 86.36(7) 2_665 5
O2 Fe2 O2 88.77(5) . 8_455
O2 Fe2 O2 91.23(5) . 2_675
O2 Fe2 O2 180.00(6) 8_455 2_675
O2 Fe2 O2 88.77(5) . 9_665
O2 Fe2 O2 91.23(5) 8_455 9_665
O2 Fe2 O2 88.77(5) 2_675 9_665
O2 Fe2 O2 180.0 . 7_575
O2 Fe2 O2 91.23(5) 8_455 7_575
O2 Fe2 O2 88.77(5) 2_675 7_575
O2 Fe2 O2 91.23(5) 9_665 7_575
O2 Fe2 O2 91.23(5) . 3_465
O2 Fe2 O2 88.77(5) 8_455 3_465
O2 Fe2 O2 91.23(5) 2_675 3_465
O2 Fe2 O2 180.0 9_665 3_465
O2 Fe2 O2 88.77(5) 7_575 3_465
C1 O1 Fe1 128.06(13) . .
C1 O2 Fe2 126.86(12) . .
O1 C1 O2 126.39(18) . .
O1 C1 H1 116.8 . .
O2 C1 H1 116.8 . .
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 C21 H21A 109.5 . .
N1 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
N1 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C21 N1 C2 120.2(12) . .
C21 N1 H1A 108.0 . .
C2 N1 H1A 110.6 . .
C21 N1 H1B 106.0 . .
C2 N1 H1B 108.5 . .
H1A N1 H1B 102.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O1 2.0566(12) .
Fe1 O1 2.0566(12) 4_665
Fe1 O1 2.0566(12) 6_565
Fe1 O1 2.0566(12) 3_565
Fe1 O1 2.0566(12) 2_665
Fe1 O1 2.0566(12) 5
Fe2 O2 2.0192(12) .
Fe2 O2 2.0193(12) 8_455
Fe2 O2 2.0193(12) 2_675
Fe2 O2 2.0193(12) 9_665
Fe2 O2 2.0193(12) 7_575
Fe2 O2 2.0193(12) 3_465
O1 C1 1.229(2) .
O2 C1 1.245(2) .
C1 H1 0.9300 .
C2 N1 1.482(9) .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C21 N1 1.454(8) .
C21 H21A 0.9600 .
C21 H21B 0.9600 .
C21 H21C 0.9600 .
N1 H1A 0.9134 .
N1 H1B 0.9478 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A O1 0.91 2.43 3.202(14) 142.2 11_666
N1 H1A O1 0.91 2.48 3.195(17) 135.7 8_556
N1 H1B O1 0.95 2.18 3.058(17) 152.7 7_566
