#------------------------------------------------------------------------------
#$Date: 2018-01-01 05:20:54 +0200 (Mon, 01 Jan 2018) $
#$Revision: 204639 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/69/4126951.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_4126951
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         '2(Cl2 Fe0.5), C4 H9 N'
_chemical_formula_sum            'C4 H12 Cl4 Fe N'
_chemical_formula_weight         271.80
_space_group_crystal_system      orthorhombic
_space_group_IT_number           38
_space_group_name_Hall           'A 2 -2'
_space_group_name_H-M_alt        'A m m 2'
_symmetry_space_group_name_Hall  'A 2 -2'
_symmetry_space_group_name_H-M   'A m m 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.218(8)
_cell_length_b                   9.019(9)
_cell_length_c                   9.362(10)
_cell_measurement_reflns_used    1181
_cell_measurement_temperature    330
_cell_measurement_theta_max      27.346
_cell_measurement_theta_min      2.822
_cell_volume                     609.5(11)
_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      330
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4233
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.404
_diffrn_reflns_theta_min         2.822
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.059
_exptl_absorpt_correction_T_max  0.704102
_exptl_absorpt_correction_T_min  0.539113
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0896 before and 0.0400 after correction.
 The Ratio of minimum to maximum transmission is 0.77.
 The λ/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0898 before and 0.0424 after correction.
 The Ratio of minimum to maximum transmission is 0.77.
 The λ/2 correction factor is Not present

Final HKLF 4 output contains 4233 reflections, Rint = 0.0326
 (3725 with I > 3sig(I), Rint = 0.0324)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.481
_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         0.347
_refine_diff_density_min         -0.196
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.13(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     43
_refine_ls_number_reflns         803
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0638P)²+0.1268P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1008
_reflns_Friedel_coverage         0.885
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                776
_reflns_number_total             803
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja7b10539_si_004.cif
_cod_data_source_block           TMA_FeCl4_330K
_cod_original_cell_volume        609.4(11)
_cod_database_code               4126951
_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.
;
_shelx_estimated_absorpt_t_max   0.783
_shelx_estimated_absorpt_t_min   0.627
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.87(6)
 0.13(6)
2. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N1-C1 \\sim N1-C2 \\sim N1-C3
 with sigma of 0.02
4. 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
5. Others
 Fixed Sof: C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5) C2(0.25) H2C(0.25) H2A(0.25)
 H2B(0.25) C3(0.25) H3B(0.25) H3C(0.25) H3A(0.25)
6.a Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C3(H3B,H3C,H3A)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y, z'
'-x, y, z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x, -y+1/2, z+1/2'
'-x, y+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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Fe1 Fe 0.5000 0.0000 0.41366(6) 0.0644(4) Uani 1 4 d S TU P
Cl1 Cl 0.2475(3) 0.0000 0.5412(3) 0.1080(8) Uani 1 2 d S TU P
Cl2 Cl 0.5000 0.1979(3) 0.2777(3) 0.1252(9) Uani 1 2 d S TU P
N1 N 0.0000 0.5000 0.5003(8) 0.081(2) Uani 1 4 d DS TU P
C1 C 0.178(4) 0.560(3) 0.455(2) 0.180(11) Uani 0.5 1 d D U P
H1A H 0.2508 0.5852 0.5373 0.270 Uiso 0.5 1 calc R U P
H1B H 0.2427 0.4880 0.3986 0.270 Uiso 0.5 1 calc R U P
H1C H 0.1579 0.6480 0.3986 0.270 Uiso 0.5 1 calc R U P
C2 C 0.0000 0.446(4) 0.649(2) 0.160(11) Uani 0.5 2 d DS TU P
H2C H 0.1117 0.4770 0.6954 0.240 Uiso 0.25 1 calc R U P
H2A H -0.1052 0.4855 0.6982 0.240 Uiso 0.25 1 calc R U P
H2B H -0.0065 0.3395 0.6487 0.240 Uiso 0.5 2 calc R U P
C3 C 0.0000 0.354(2) 0.432(4) 0.158(9) Uani 0.5 2 d DS TU P
H3B H 0.1246 0.3176 0.4270 0.236 Uiso 0.25 1 calc R U P
H3C H -0.0744 0.2872 0.4872 0.236 Uiso 0.25 1 calc R U P
H3A H -0.0502 0.3627 0.3375 0.236 Uiso 0.25 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'
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 113.52(17) . 2_655
Cl1 Fe1 Cl2 108.56(7) 2_655 .
Cl1 Fe1 Cl2 108.56(7) . .
Cl1 Fe1 Cl2 108.56(7) . 2_655
Cl1 Fe1 Cl2 108.56(7) 2_655 2_655
Cl2 Fe1 Cl2 109.0(2) 2_655 .
C1 N1 C1 44(2) 2_565 4
C1 N1 C1 44(2) . 3_565
C1 N1 C1 146.1(19) 4 3_565
C1 N1 C1 146.1(19) 2_565 .
C1 N1 C1 123(2) 4 .
C1 N1 C1 123(2) 2_565 3_565
C1 N1 C2 113.5(11) 4 .
C1 N1 C2 98.7(11) . 3_565
C1 N1 C2 98.7(11) 2_565 .
C1 N1 C2 98.7(11) 3_565 .
C1 N1 C2 113.5(11) 3_565 3_565
C1 N1 C2 113.5(11) 2_565 3_565
C1 N1 C2 98.7(11) 4 3_565
C1 N1 C2 113.5(11) . .
C1 N1 C3 102.0(13) 2_565 3_565
C1 N1 C3 102.0(13) . .
C1 N1 C3 102.0(13) 3_565 3_565
C1 N1 C3 62.4(12) 4 3_565
C1 N1 C3 62.4(12) . 3_565
C1 N1 C3 62.4(12) 2_565 .
C1 N1 C3 102.0(13) 4 .
C1 N1 C3 62.4(12) 3_565 .
C2 N1 C2 39(3) 3_565 .
C3 N1 C2 135(2) 3_565 .
C3 N1 C2 96(2) 3_565 3_565
C3 N1 C2 96(2) . .
C3 N1 C2 135(2) . 3_565
C3 N1 C3 128(3) . 3_565
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 H2C 109.5 . .
N1 C2 H2A 109.5 . .
N1 C2 H2B 109.5 . .
H2C C2 H2A 109.5 . .
H2C C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
N1 C3 H3B 109.5 . .
N1 C3 H3C 109.5 . .
N1 C3 H3A 109.5 . .
H3B C3 H3C 109.5 . .
H3B C3 H3A 109.5 . .
H3C C3 H3A 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 2.179(3) .
Fe1 Cl1 2.179(3) 2_655
Fe1 Cl2 2.192(3) 2_655
Fe1 Cl2 2.192(3) .
N1 C1 1.46(2) 4
N1 C1 1.46(2) 3_565
N1 C1 1.46(2) .
N1 C1 1.46(2) 2_565
N1 C2 1.471(19) .
N1 C2 1.471(19) 3_565
N1 C3 1.46(2) .
N1 C3 1.46(2) 3_565
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 H2C 0.9600 .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C3 H3A 0.9600 .
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.87(6)
2 0.13(6)
