#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:17:56 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179475 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/72/4337220.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_4337220
loop_
_publ_author_name
'Han, Jing'
'Nishihara, Sadafumi'
'Inoue, Katsuya'
'Kurmoo, Mohamedally'
_publ_section_title
;
 On the Nature of the Structural and Magnetic Phase Transitions in the
 Layered Perovskite-Like (CH3NH3)2[Fe(II)Cl4].
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2068
_journal_page_last               2075
_journal_paper_doi               10.1021/ic402535u
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C0.13 H0.75 Cl0.25 Fe0.06 N0.13'
_chemical_formula_weight         16.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           139
_symmetry_space_group_name_Hall  '-I 4 2'
_symmetry_space_group_name_H-M   'I 4/m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            32
_cell_length_a                   5.117(3)
_cell_length_b                   5.117(3)
_cell_length_c                   19.260(12)
_cell_measurement_temperature    350(2)
_cell_volume                     504.3(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      350(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0158
_diffrn_reflns_av_sigmaI/netI    0.0123
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            1517
_diffrn_reflns_theta_full        27.98
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    2.487
_exptl_absorpt_correction_T_max  0.9519
_exptl_absorpt_correction_T_min  0.3168
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             264
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.328
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     17
_refine_ls_number_reflns         222
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.328
_refine_ls_R_factor_all          0.0163
_refine_ls_R_factor_gt           0.0163
_refine_ls_shift/su_max          0.831
_refine_ls_shift/su_mean         0.052
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0210P)²+0.0841P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0407
_refine_ls_wR_factor_ref         0.0407
_reflns_number_gt                222
_reflns_number_total             222
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            E-350k-I-4mmm.cif
_cod_data_source_block           E-350K-Pccn
_cod_original_cell_volume        504.3(6)
_cod_original_sg_symbol_H-M      '? I 4/mmm'
_cod_database_code               4337220
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'-y, -x, -z'
'y, x, -z'
'y, -x, z'
'-y, x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'-x, y, z'
'x, -y, z'
'y, x, z'
'-y, -x, z'
'-y, x, -z'
'y, -x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'y+1/2, -x+1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Fe1 Fe 0.0000 0.0000 0.0000 0.02603(16) Uani 1 16 d S
Cl1 Cl 0.0000 0.0000 0.12507(3) 0.0572(2) Uani 1 8 d S
Cl2 Cl 0.0000 -0.5000 0.0000 0.0451(2) Uani 1 8 d S
N1 N -0.5000 -0.5000 -0.11413(12) 0.0527(7) Uani 1 8 d S
H1 H -0.6442 -0.5781 -0.0987 0.079 Uiso 0.13 1 calc PR
H1A H -0.4955 -0.3361 -0.0987 0.079 Uiso 0.25 2 calc SPR
H1B H -0.3603 -0.5859 -0.0987 0.079 Uiso 0.13 1 calc PR
C1 C -0.5000 -0.5000 -0.18821(17) 0.0819(13) Uani 1 8 d S
H1C H -0.6751 -0.4750 -0.2048 0.123 Uiso 0.13 1 calc PR
H1D H -0.4341 -0.6641 -0.2048 0.123 Uiso 0.13 1 calc PR
H1E H -0.3908 -0.3609 -0.2048 0.123 Uiso 0.13 1 calc PR
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 0.02253(18) 0.02253(18) 0.0330(2) 0.000 0.000 0.000
Cl1 0.0699(3) 0.0699(3) 0.0317(3) 0.000 0.000 0.000
Cl2 0.0356(3) 0.0208(3) 0.0788(5) 0.000 0.000 0.000
N1 0.0586(10) 0.0586(10) 0.0411(12) 0.000 0.000 0.000
C1 0.102(2) 0.102(2) 0.0416(17) 0.000 0.000 0.000
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'
N N 0.0061 0.0033 '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'
Fe Fe 0.3463 0.8444 '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
Cl1 Fe1 Cl1 180.0 17 .
Cl1 Fe1 Cl2 90.0 17 5
Cl1 Fe1 Cl2 90.0 . 5
Cl1 Fe1 Cl2 90.0 17 .
Cl1 Fe1 Cl2 90.0 . .
Cl2 Fe1 Cl2 90.0 5 .
Cl1 Fe1 Cl2 90.0 17 1_565
Cl1 Fe1 Cl2 90.0 . 1_565
Cl2 Fe1 Cl2 90.0 5 1_565
Cl2 Fe1 Cl2 180.0 . 1_565
Cl1 Fe1 Cl2 90.0 17 5_455
Cl1 Fe1 Cl2 90.0 . 5_455
Cl2 Fe1 Cl2 180.0 5 5_455
Cl2 Fe1 Cl2 90.0 . 5_455
Cl2 Fe1 Cl2 90.0 1_565 5_455
Fe1 Cl2 Fe1 180.0 1_545 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 Cl1 2.4088(17) 17
Fe1 Cl1 2.4088(17) .
Fe1 Cl2 2.5585(17) 5
Fe1 Cl2 2.5585(17) .
Fe1 Cl2 2.5585(17) 1_565
Fe1 Cl2 2.5585(17) 5_455
Cl2 Fe1 2.5585(17) 1_545
N1 C1 1.427(4) .
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
Cl1 Fe1 Cl2 Fe1 180.0 17 1_545
Cl1 Fe1 Cl2 Fe1 0.0 . 1_545
Cl2 Fe1 Cl2 Fe1 90.0 5 1_545
Cl2 Fe1 Cl2 Fe1 0.0 1_565 1_545
Cl2 Fe1 Cl2 Fe1 -90.0 5_455 1_545
