#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:42:20 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180050 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/44/7034430.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_7034430
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                   8.2067(2)
_cell_length_b                   8.2067(2)
_cell_length_c                   13.8818(6)
_cell_measurement_reflns_used    4448
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      28.1861
_cell_measurement_theta_min      2.8596
_cell_volume                     809.68(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      190(2)
_diffrn_detector_area_resol_mean 8.4350
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0257
_diffrn_reflns_av_unetI/netI     0.0125
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7770
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.659
_diffrn_reflns_theta_max         25.659
_diffrn_reflns_theta_min         3.220
_exptl_absorpt_coefficient_mu    1.029
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, 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    1.626
_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         0.435
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         517
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0420P)²+0.4600P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0677
_reflns_Friedel_coverage         0.000
_reflns_number_gt                451
_reflns_number_total             517
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt00512d2.cif
_cod_data_source_block           190
_cod_depositor_comments
'Adding full bibliography for 7034429--7034431.cif.'
_cod_original_cell_volume        809.68(5)
_cod_database_code               7034430
#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 0.0092(3) Uani 0.315(4) 6 d S T P
Mg1 Mg 0.3333 0.6667 0.2500 0.0092(3) Uani 0.685(4) 6 d S T P
Fe2 Fe 0.0000 1.0000 0.0000 0.0073(2) Uani 0.687(4) 6 d S T P
Mg2 Mg 0.0000 1.0000 0.0000 0.0073(2) Uani 0.313(4) 6 d S T P
O1 O 0.12150(18) 0.66142(19) 0.16846(9) 0.0234(3) Uani 1 1 d . . .
O2 O -0.00985(18) 0.79207(17) 0.08225(9) 0.0198(3) Uani 1 1 d . . .
C1 C 0.1286(3) 0.7907(3) 0.11922(12) 0.0217(4) Uani 1 1 d . . .
H1 H 0.2466 0.8955 0.1089 0.026 Uiso 1 1 calc R U .
C2 C 0.3333 0.6667 0.8681(9) 0.076(4) Uani 0.5 3 d DS TU P
H2A H 0.4641 0.7612 0.8694 0.114 Uiso 0.1667 1 calc R U P
H2B H 0.3055 0.5828 0.9217 0.114 Uiso 0.1667 1 calc R U P
H2C H 0.2580 0.7258 0.8722 0.114 Uiso 0.1667 1 calc R U P
C21 C 0.3333 0.6667 0.6906(11) 0.090(5) Uani 0.5 3 d DS TU P
H21A H 0.3224 0.7764 0.7011 0.135 Uiso 0.1667 1 calc R U P
H21B H 0.2464 0.5903 0.6413 0.135 Uiso 0.1667 1 calc R U P
H21C H 0.4593 0.7043 0.6706 0.135 Uiso 0.1667 1 calc R U P
N1 N 0.291(2) 0.5605(19) 0.7783(7) 0.053(4) Uiso 0.1667 1 d D . P
H1A H 0.3551 0.4990 0.7781 0.064 Uiso 0.1667 1 calc R U P
H1B H 0.1695 0.4747 0.7781 0.064 Uiso 0.1667 1 calc R 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 88.91(8) . 4_665
O1 Fe1 O1 85.90(7) . 6_565
O1 Fe1 O1 92.62(5) 4_665 6_565
O1 Fe1 O1 92.62(5) . 3_565
O1 Fe1 O1 85.90(7) 4_665 3_565
O1 Fe1 O1 177.92(8) 6_565 3_565
O1 Fe1 O1 92.62(5) . 2_665
O1 Fe1 O1 177.92(8) 4_665 2_665
O1 Fe1 O1 88.91(8) 6_565 2_665
O1 Fe1 O1 92.62(5) 3_565 2_665
O1 Fe1 O1 177.92(8) . 5
O1 Fe1 O1 92.62(5) 4_665 5
O1 Fe1 O1 92.62(5) 6_565 5
O1 Fe1 O1 88.91(8) 3_565 5
O1 Fe1 O1 85.90(7) 2_665 5
O2 Fe2 O2 91.22(5) 7_575 8_455
O2 Fe2 O2 88.78(5) 7_575 2_675
O2 Fe2 O2 180.00(6) 8_455 2_675
O2 Fe2 O2 180.0 7_575 .
O2 Fe2 O2 88.78(5) 8_455 .
O2 Fe2 O2 91.22(5) 2_675 .
O2 Fe2 O2 91.22(5) 7_575 9_665
O2 Fe2 O2 91.22(5) 8_455 9_665
O2 Fe2 O2 88.78(5) 2_675 9_665
O2 Fe2 O2 88.78(5) . 9_665
O2 Fe2 O2 88.78(5) 7_575 3_465
O2 Fe2 O2 88.78(5) 8_455 3_465
O2 Fe2 O2 91.22(5) 2_675 3_465
O2 Fe2 O2 91.22(5) . 3_465
O2 Fe2 O2 180.0 9_665 3_465
C1 O1 Fe1 127.46(12) . .
C1 O2 Fe2 125.85(12) . .
O1 C1 O2 125.40(17) . .
O1 C1 H1 117.3 . .
O2 C1 H1 117.3 . .
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 116.7(13) . .
C21 N1 H1A 108.1 . .
C2 N1 H1A 108.1 . .
C21 N1 H1B 108.1 . .
C2 N1 H1B 108.1 . .
H1A N1 H1B 107.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O1 2.0568(12) .
Fe1 O1 2.0568(12) 4_665
Fe1 O1 2.0568(12) 6_565
Fe1 O1 2.0568(12) 3_565
Fe1 O1 2.0568(12) 2_665
Fe1 O1 2.0568(12) 5
Fe2 O2 2.0208(12) 7_575
Fe2 O2 2.0208(12) 8_455
Fe2 O2 2.0208(12) 2_675
Fe2 O2 2.0209(12) .
Fe2 O2 2.0209(12) 9_665
Fe2 O2 2.0209(12) 3_465
O1 C1 1.239(2) .
O2 C1 1.252(2) .
C1 H1 0.9300 .
C2 N1 1.460(9) .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C21 N1 1.435(9) .
C21 H21A 0.9600 .
C21 H21B 0.9600 .
C21 H21C 0.9600 .
N1 H1A 0.8900 .
N1 H1B 0.8900 .
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 0.89 2.43 3.175(15) 140.9 11_666
N1 H1A O1 0.89 2.48 3.211(17) 140.0 8_556
N1 H1B O1 0.89 2.20 3.029(17) 155.0 7_566
C2 H2C O2 0.96 2.53 3.421(3) 153.9 9_666
