#------------------------------------------------------------------------------
#$Date: 2018-01-01 05:22:27 +0200 (Mon, 01 Jan 2018) $
#$Revision: 204641 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/69/4126953.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_4126953
loop_
_publ_author_name
'Harada, Jun'
'Yoneyama, Naho'
'Yokokura, Seiya'
'Takahashi, Yukihiro'
'Miura, Atsushi'
'Kitamura, Noboru'
'Inabe, Tamotsu'
_publ_section_title
;
 Ferroelectricity and Piezoelectricity in Free-Standing Polycrystalline
 Films of Plastic Crystals.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b10539
_journal_year                    2017
_chemical_formula_moiety         'Cl4 Fe, 0.5(C8 H12 N2)'
_chemical_formula_sum            'C4 H12 Cl4 Fe N'
_chemical_formula_weight         271.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           28
_space_group_name_Hall           'P 2 -2a'
_space_group_name_H-M_alt        'P m a 2'
_symmetry_space_group_name_Hall  'P 2 -2a'
_symmetry_space_group_name_H-M   'P m a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.268(5)
_cell_length_b                   6.442(2)
_cell_length_c                   6.451(2)
_cell_measurement_reflns_used    5996
_cell_measurement_temperature    300
_cell_measurement_theta_max      27.346
_cell_measurement_theta_min      2.855
_cell_volume                     592.9(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2 2014.1-1 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      300
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0154
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            8298
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.508
_diffrn_reflns_theta_min         2.855
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.117
_exptl_absorpt_correction_T_max  0.7041
_exptl_absorpt_correction_T_min  0.6083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.0873 before and 0.0412 after correction. The Ratio of minimum to maximum transmission is 0.8639. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       block
_exptl_crystal_F_000             274
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.170
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         1419
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0246
_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)+(0.0465P)²+0.0512P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0720
_reflns_Friedel_coverage         0.837
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                1397
_reflns_number_total             1419
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja7b10539_si_003.cif
_cod_data_source_block           TMA_FeCl4_300K
_cod_original_cell_volume        592.9(4)
_cod_database_code               4126953
_shelxl_version_number           2014/6
_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.
;
_shelx_estimated_absorpt_t_max   0.778
_shelx_estimated_absorpt_t_min   0.620
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.94(3)
 0.06(3)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C2(0.5) H2A(0.5) H2B(0.5)
 H2C(0.5) C3(0.5) H3A(0.5) H3B(0.5) H3C(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5)
5.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y, z'
'-x+1/2, y, z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.2500 0.42205(7) 0.41451(8) 0.05674(18) Uani 1 2 d S TU P . .
Cl1 Cl 0.37702(8) 0.54365(19) 0.55319(19) 0.0937(4) Uani 1 1 d . U . . .
Cl2 Cl 0.2500 0.0848(2) 0.4512(5) 0.1137(8) Uani 1 2 d S TU P . .
Cl3 Cl 0.2500 0.4954(4) 0.0849(2) 0.1074(5) Uani 1 2 d S TU P . .
N1 N 0.5000 0.0000 0.0011(7) 0.0683(9) Uani 1 2 d S TU P . .
C1 C 0.5971(15) -0.034(4) -0.095(4) 0.149(7) Uani 0.5 1 d . U P A -1
H1A H 0.5904 -0.0864 -0.2329 0.223 Uiso 0.5 1 calc R U P A -1
H1B H 0.6316 -0.1313 -0.0122 0.223 Uiso 0.5 1 calc R U P A -1
H1C H 0.6303 0.0961 -0.0985 0.223 Uiso 0.5 1 calc R U P A -1
C2 C 0.5019(19) 0.222(2) 0.067(4) 0.144(6) Uani 0.5 1 d . U P A -1
H2A H 0.4769 0.2341 0.2047 0.216 Uiso 0.5 1 calc R U P A -1
H2B H 0.4647 0.3036 -0.0266 0.216 Uiso 0.5 1 calc R U P A -1
H2C H 0.5653 0.2719 0.0656 0.216 Uiso 0.5 1 calc R U P A -1
C3 C 0.4469(18) 0.069(4) -0.166(3) 0.154(7) Uani 0.5 1 d . U P A -1
H3A H 0.4186 0.2001 -0.1319 0.232 Uiso 0.5 1 calc R U P A -1
H3B H 0.3988 -0.0304 -0.1963 0.232 Uiso 0.5 1 calc R U P A -1
H3C H 0.4866 0.0858 -0.2850 0.232 Uiso 0.5 1 calc R U P A -1
C4 C 0.4684(17) -0.149(3) 0.153(3) 0.155(7) Uani 0.5 1 d . U P A -1
H4A H 0.4031 -0.1279 0.1810 0.233 Uiso 0.5 1 calc R U P A -1
H4B H 0.5036 -0.1323 0.2788 0.233 Uiso 0.5 1 calc R U P A -1
H4C H 0.4777 -0.2874 0.1005 0.233 Uiso 0.5 1 calc R U P A -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'
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
Cl1 Fe1 Cl1 113.47(8) 4
Cl1 Fe1 Cl2 108.33(6) 4
Cl1 Fe1 Cl2 108.33(6) .
Cl1 Fe1 Cl3 108.93(5) .
Cl1 Fe1 Cl3 108.93(5) 4
Cl3 Fe1 Cl2 108.75(11) .
C2 N1 C1 103.5(14) .
C3 N1 C1 103.1(14) .
C3 N1 C2 85.6(16) .
C3 N1 C4 124.7(15) .
C4 N1 C1 117.4(11) .
C4 N1 C2 116.7(14) .
N1 C1 H1A 109.5 .
N1 C1 H1B 109.5 .
N1 C1 H1C 109.5 .
H1A C1 H1B 109.5 .
H1A C1 H1C 109.5 .
H1B C1 H1C 109.5 .
N1 C2 H2A 109.5 .
N1 C2 H2B 109.5 .
N1 C2 H2C 109.5 .
N1 C2 C3 45.0(9) .
H2A C2 H2B 109.5 .
H2A C2 H2C 109.5 .
H2B C2 H2C 109.5 .
C3 C2 H2A 126.9 .
C3 C2 H2B 64.6 .
C3 C2 H2C 122.5 .
N1 C3 C2 49.4(10) .
N1 C3 H3A 109.5 .
N1 C3 H3B 109.5 .
N1 C3 H3C 109.5 .
C2 C3 H3A 63.3 .
C2 C3 H3B 141.1 .
C2 C3 H3C 108.7 .
H3A C3 H3B 109.5 .
H3A C3 H3C 109.5 .
H3B C3 H3C 109.5 .
N1 C4 H4A 109.5 .
N1 C4 H4B 109.5 .
N1 C4 H4C 109.5 .
H4A C4 H4B 109.5 .
H4A C4 H4C 109.5 .
H4B C4 H4C 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 Cl1 2.1676(12) 4
Fe1 Cl1 2.1677(12) .
Fe1 Cl2 2.1854(16) .
Fe1 Cl3 2.1781(18) .
N1 C1 1.532(17) .
N1 C2 1.494(14) .
N1 C3 1.39(2) .
N1 C4 1.447(13) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C2 C3 1.96(3) .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
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
C1 N1 C2 C3 102.4(14)
C1 N1 C3 C2 -102.9(15)
C4 N1 C2 C3 -126.9(16)
C4 N1 C3 C2 119.7(16)
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.94(3)
2 0.06(3)
